Component Project 1 "Combating the effects of CBRN aggression using new multi-decontamination systems POLIDEC"

PARTNERS: IC ICECHIM; P1 CCSA-CBRNE; P2 CCO; P3 CCSFN

TOTAL BUDGET PC. 1: 925.000 RON

PROJECT PERIOD: 19.03.2018-18.08.2021 (according to additional document)

By this project, the partners bring new contributions to the fight against the effects of CBRN agents through the implementation of new multi-purpose decontamination systems. Enhanced surfactant-based decontamination solutions with a high foaming agent will be provided, facilitating intimate contact with toxic agent particles on contaminated surfaces, and favouring chemical reactions and the impregnation with CBRN-related chemicals. The innovative solution is based on the selection of surfactants that not only increase the solubility of the agents in the aqueous medium but actually contribute to the decontamination process. Such decontamination systems are needed to respond to the demands imposed by social, economic and political factors following events such as the terrorist attacks that took place in the Tokyo subway in 1995 in the US on September 11, 2001, the accident at the nuclear plant in Fukushima in March 2011 and culminating with repeated threats to use nuclear weapons proliferated in the recent years by North Korea and progress in the nuclear field undertaken by Iran, forcing the international community to reassess its capabilities to intervene in order to prevent and annihilate terrorist CBRN actions. Consequently, there must be a steady preparation for the possibility of using CBRN assets, which would have devastating consequences and would be destabilizing the political, economical and social context. Increasing the efficiency and effectiveness of institutions that have attributions in the field of environmental protection, civil protection and emergency response are requirements that are imposed both nationally and internationally.\

PHASE I: Studies and experimental models

BUDGET PC. 1, PHASE I: 276,575 RON

PHASE PERIOD: 19.03.2018-31.12.2018

 SPECIFIC OBJECTIVES:

 Activity 1.1. Determination of decontamination requirements and methods, depending on the types of biological, chemical and radiological agents used predominantly in CBRN aggressions, and types of decontamination agents

Activity 1.2. Establishing the performance criteria for surfactants and decontamination systems in relation to contaminant types and decontamination modalities. Synthesis and characterization of surfactants used in CBRN decontamination, selection of optimal structures

Activity 1.3. Establishing the performance criteria for polymer gels and decontamination systems in relation to contaminant types and decontamination modalities. Synthesis and characterization of polymer gels used in CBRN decontamination, selection of optimal structures

Activity 1.4. Dissemination of results

SUMMARY

 At this stage, the types of contaminants and the nature of the contaminants were established, creating a material database for starting the procedures for preparing the two types of decontaminants. Amino acid surfactants (sodium lauroyl glycinate and sodium lauroyl prolinate) have been synthesized for use in decontamination systems against chemical and biological agents. The work will continue in the next stage with diversification of the surfactants range and elaboration of the experimental model for the conditioning of surfactant decontamination products. Also at this stage, APV basic polymer gels were successfully prepared for use in the decontamination of surfaces and (radio)chemical contaminated objects. The films detach easily from the tested surfaces and have excellent dry elasticity. Polymer gels are to be improved by staining to make them more visible on the surfaces that are deposited. The samples were tested for decontamination and the results were being promising. Following decontamination tests, a decontamination percentage of more than 80% was obtained for sample 1 and over 85% for sample 2. The results of the research were communicated through poster communications or oral presentations. In addition to the 6 communications, 3 ISI indexed articles were also published based on the background material used for within the concerned component project. An active link of Project 2 "POLIDEC" was made on the site of the Complex Project SECURE-NET. The research team composed of (ICECHIM, CCSA-CBRNE, CCO and CCSFN) met the proposed objectives for Phase 1 of PC 1 POLIDEC with a total degree of achievement.

DISSEMINATION

Scientific Communications:

1. Florica Adriana Jerca, Valentin Victor Jerca, Richard Hoogenboom, ”pH-Degradable thermoresponsive copolymers starting from well-defined poly(2-isopropenyl-2-oxazoline)”, 7th EuCheMS Chemistry Congress, Liverpool, Marea Britanie, 26-30 Aug 2018, poster.
   1. Emilian Ghibu, Valentin Victor Jerca, Verona Tanta Iordache, Dumitru Mircea Vuluga, Raluca Stan, Florica Adriana Jerca, “New drug release systems based on poly(2-isopropenyl-2-oxazoline) hydrogels”, Oral Comunication
   2. Emilian Ghibu, Valentin Victor Jerca, Verona Tanta Iordache, Dumitru Mircea Vuluga, Raluca Stan, Florica Adriana Jerca, “Poly(2-isopropenyl-2-oxazoline) based hydrogels for drug release systems” PRIOCHEM, Bucharest, Romania, 10-12 Oct 2018, poster
   3. Irina Elena Chican, Dana V?r??teanu, Sanda Maria Doncea, Raluca Somoghi, Ana-Maria G?lan,  The influence of hydrocarbon chain length on the surface properties of gluconolactone-based surfactants, Simpozionul International SICHEM 2018, Bucharest, Romania, 6-7 Sept. 2018, Oral Comunication
   4. Dana V?r??teanu , Irina Elena Chican, Elena Dimitriu, Ioan Dorel Buriu, Stability assessment of additivated formulations containing surfactants and oxidizing agents, Simpozionul International PRIOCHEM editia XIV, Bucharest, Romania, 10-12 Oct 2018, poster
   5. Iordache Tanta-Verona,  Chican Irina, Varasteanu Dana, Florea Ana Mihaela, Contingenta Hazardurilor CBRN si imbunatatirea mijloacelor de securitate nationala SECURE-NET, Simpozion Stiintific Aniversar Performanta, rigurozitate si competenta in cercetare stiintifica, 18 octombrie 2018, Centrul de Cercetare Stiintifica pentru Fortele Navale, Constanta, Romania, Oral Presentation

Articles:

1. Florica Adriana Jerca, Valentin Victor Jerca, Alina Maria Anghelache, Dumitru Mircea Vuluga, Richard Hoogenboom, “Poly(2-Isopropenyl-2-Oxazoline) as a Versatile Platform Towards Thermoresponsive Copolymers”, Polymer Chemistry, 2018, 9, 3473-3478.
2. Florica Adriana Jerca, Valentin Victor Jerca, Richard Hoogenboom, “Well-Defined Thermoresponsive Polymethacrylamide Copolymers with Ester Pendent Groups through One-Pot Statistical Postpolymerization Modification of Poly(2-Isopropenyl-2-Oxazoline) with Multiple Carboxylic Acids”, Journal of Polymer Science Part A: Polymer Chemistry, 2018, DOI:10.1002/pola.29188.
3. Florica Adriana Jerca, Alina Maria Anghelache, Emilian Ghibu, Sergiu Cecoltan, Izabela-Cristina Stancu, Roxana Trusca, Eugeniu Vasile, Mircea Teodorescu, Dumitru Mircea Vuluga, Richard Hoogenboom, Valentin Victor Jerca, “Poly(2-isopropenyl-2-oxazoline) hydrogels for biomedical applications”, Chemistry of Materials, 2018, 30, 7938−7949.

Activ Link of Project 1 "POLIDEC", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro 

PHASE II: Development of Functional Models and Technologies

BUDGET PC. 1, PHASE II: 291.375 RON

PHASE PERIOD: 01.01.2019-31.12.2019

SPECIFIC OBJECTIVES:

Activity 2.1. Synthesis and characterization of amino acid-based surfactants used in CBRN decontamination, selection of optimal structures. Elaboration of the conditioning experimental model of the decontamination products based on surfactants.

Activity 2.2. Synthesis and characterization of polymer gels used in CBRN decontamination, selection of optimal structures. Elaboration of the conditioning experimental model of the decontamination products based on polymer gels.

Activity 2.3. Testing the efficiency of decontamination products within the premises of the National Defence System.

Activity 2.4. Identification and protection of intellectual property rights

Activity 2.5. Dissemination of results

SUMMARY

At this stage, an N-acylated surfactant (sodium lauroyl-sarcozinate NaLSar) has been synthesized for use in decontamination systems against chemical and biological agents. The synthesized surfactant has been tested from the point of view of the surfactant properties, but also considering the evaluation of its stability in oxidizing agents. Taking into account the results obtained at this stage, the laboratory technology was developed to obtain the surfactant decontamination solution containing an aqueous system consisting of three surfactants (one amino acid surfactant and two non-ionic surfactants), two glycols (polyethylene glycol and propylene glycol), a corrosion inhibitor and oxygenated water as an oxidizing agent. In Phase II, the samples of APV polymer gels were optimized/ improved in terms of drying time of the deposited films and to be tested in multi-component chemical decontamination. Thus, optimized APV polymer gels were successfully prepared for use in the decontamination of surfaces and (radio) chemical contaminated objects. The films dry much faster and have the same efficiency to detach easily from the tested surfaces. The surfactants and the polymer gels were sent to the CBRN partner for testing. Following decontamination tests, it was concluded that the both the surfactants and the hydrogels have a great potential for use in the incorporation and decontamination of contaminated surfaces (with approximately 100% efficiency), using simple and safe procedures. Within the SECURE-NET project, Project component 1-POLIDEC, Phase 2, 4 trips were made in the country and 4 in Bucharest, which were aimed at disseminating the preliminary results through a Poster communication. The results of the research were communicated through poster communications or oral presentations. In addition to the 8 communications, 2 articles indexed ISI were also published (reported in the previous phase as being accepted) and 1 ISI paper proceedings accepted for publication, based on the background material used for within the concerned component project but also results obtained in the first phase. The research team composed of (ICECHIM, CCSA-CBRNE, CCO and CCSFN) met the proposed objectives for Phase 2 of PC 1 POLIDEC with a total degree of achievement.

DISSEMINATION

Scientific Communications:

1. Surface properties în surfactant systems containing amino acid-based surfactants, I. E. Chican, D. V?r??teanu, I.Fier?scu, R.C. Fier?scu, M. Deaconu, EUROINVENT International Conference on Innovative Research EUROINVENT International Conference on Innovative Research, Ia?i, România, 16-17 May 2019, Poster

2. Contingen?a hazardurilor CBRN ?i imbun?t??irea mijloacelor de securitate na?ionala – SECURE-NET (Proiectul 70PCCDI /2018), T.-V. Iordache, C. Lazaroaie, T. Rotariu, A. Jerca, A. Ghebaur, G. Surdu, I. E. Chican, A.-M. Florea, V. Raditoiu, E. Bartha, Expozi?ia European? a Creativit??ii ?i Inov?rii EUROINVENT, Ia?i, România 16-18 may 2019 (Diploma of excellence of the Salon and Diploma of excellence from the UMF Carol Davila Bucharest), Poster

3. Poly(2-Isopropenyl-2-Oxazoline) Hydrogels as Drug Delivery Systems, Ghibu, E., Banu, N.D., Iordache, T.V., Vuluga, D.M., Stan, R., Jerca, V.V., Jerca, F.A, 21st Romanian International Conference on Chemistry and Chemical Engineering (RICCCE 21) Constanta-Mamaia, Romania, 4-7.09.2019, Oral Communication

4. Cercetari privind noi sisteme de decontaminare polivalent? a suprafe?elor, I. E. Chican, R. Petre, A. Jerca, L. Calancea, WORKSHOP ”Noi Materiale si Metode privind Contingenta Hazardurilor CBRN si Imbunatatirea Mijloacelor de Securitate Nationala”, ICECHIM, Bucure?ti, Romania, 23.09. 2019, Oral Communication

5. Rezultatele obtinute la etapa I a proiectului ”Contingenta Hazardurilor CBRN si Îmbun?t?tirea Mijlozacelor de Securitate National? – SECURE-NET”, G. Surdu, L. Calancea, S. Popa, E. Curc?, A. Savastre, Simpozion Stiintific ”Performant?, rigurozitate si competent? în cercetarea stiintific?”, Centrul de Cercetare Stiintific? pentru Fortele Navale, Constanta, Romania, 18.10.2019 Oral Communication

6. Evaluation of peroxide-based compositions containing amino acid surfactants, I. E. Chican, I.-L. Calancea, D. V?r?steanu, R. Petre, I. Fier?scu, E.-G. Curca, G. Surdu, Simpozionul International “Priorit?tile Chimiei pentru o Dezvoltare Durabila” PRIOCHEM editia XV, Bucharest, Romania, 31.10 – 1.11.2019, Poster

7. Future perspective for incorporation and removal of chemical agents from contaminated surfaces, R. Petre, R. Ginghin?, L. Rece, N. Petrea, I. E. Chican, A. Jerca, Simpozionul International “Priorit?tile Chimiei pentru o Dezvoltare Durabila” PRIOCHEM editia XV, Bucharest, Romania 31.10 – 1.11.2019, Poster

8. Poly(2-Isopropenyl-2-Oxazoline) as Versatile Platform for Multi-Functional Materials, Jerca, F.A., Jerca, V.V., Vuluga, D.M., Hoogenboom, R. Simpozionul International “Priorit?tile Chimiei pentru o Dezvoltare Durabila” PRIOCHEM editia XV, Bucuresti, România 31 Octombrie – 1 Noiembrie 2019, Invited oral communication

Published articles or sent for publication:

1. Florica Adriana Jerca, Valentin Victor Jerca, Richard Hoogenboom, “Well-Defined Thermoresponsive Polymethacrylamide Copolymers with Ester Pendent Groups through One-Pot Statistical Postpolymerization Modification of Poly(2-Isopropenyl-2-Oxazoline) with Multiple Carboxylic Acids”, Journal of Polymer Science Part A: Polymer Chemistry, 2019.

2. Jerca Adriana, Anghelache Alina, Ghibu Emilian, Cecoltan Sergiu, Stancu Izabela, Trusca Roxana, Vasile Eugeniu, Teodorescu Mircea, Vuluga Dumitru Mircea, Hoogenboom Richard , Jerca Valentin Victor „Poly(2-isopropenyl-2-oxazoline) Hydrogels for Biomedical Applications” CHEMISTRY OF MATERIALS, 2018.

3. Surface properties în surfactant systems containing amino acid-based surfactants, I. E. Chican, D. V?r??teanu, I.Fier?scu, R.C. Fier?scu, M. Deaconu, EUROINVENT International Conference on Innovative Research EUROINVENT International Conference on Innovative Research, Conference Proceedings.

 Activ Link of Project 1 "POLIDEC", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro 

PHASE III: Development of Functional Models and Technologies

BUDGET PC. 1, PHASE III: 321.141 RON

PHASE PERIOD: 01.01.2020-31.12.2020

SPECIFIC OBJECTIVES:

Activity 3.1. Optimization of technologies for obtaining decontamination products based on surfactants – Part 1.

Achievement indicators: Optimized preparation protocols;

Activity 3.2. Optimization of technologies for obtaining decontamination products based on polymer gels – Part 1.

Achievement indicators: Optimized preparation protocols;

Activity 3.3. Selection of products with optimal decontamination efficiency on a wide range of CBRN agents – Part 1.

Achievement indicators: Technical specifications;

Activity 3.4. Elaboration of scientific papers.

Achievement indicators: 1 published proceedings article;

Activity 3.5. Dissemination of results

Achievement indicators: 2 Scientific Communications

SUMMARY

At this stage, a ternary system of surfactants has been proposed, which includes an amino acid-based surfactant (sodium lauroyl sarcosinate) that can be used in decontamination systems. The synergism of nonionic surfactants (polyethoxylated derivatives, amine oxides) over sodium lauryl sarcoosinate (NaLSar) in the behavior of mixed micelles was studied. Corrosivity tests were performed on ferrous metal surfaces (cast iron plate and steel plate used in ship building) and the painted steel surface used in ship building to assess the corrosion effect of decontamination solutions. The solutions were tested on a metal surface contaminated with DMMP (dimethyl methylphosphonate) with a concentration of 8.61µL DMMP/100 mL DCM. The tested solutions performed a decontamination >99.99%. Films based on APV and CMC, HPMC, respectively poloxamers were successfully obtained. It was observed that the films based on PVA containing poloxamers showing improved texture and elasticity. Polymeric films based on PVA have been successfully obtained, and respond in a visible way to contaminants, by changing the color. Samples tested in chemical decontamination of metal surfaces show fast drying time and color in contact with DMMP applied to the surface. The degree of decontamination determined is > 99.99%. The decontamination kit components based on polymer gels and surfactants (namely, the solutions for films based on APV/poloxamer films with the addition of pyrogalol and additive surfactants based on sodium lauroyl sarcosinate) was established. Within the SECURE-NET project, Component project 1-POLIDEC, Stage 3, the communication of the research results was made at various events in the form of Poster type communications. Besides the two communications, a proceedings paper was also published. The research team composed of ICECHIM, CCSA-CBRNE, CCO and CCSFN met the objectives proposed for stage III of PC 1 POLIDEC with a total degree of achievement.

DISSEMINATION

Scientific Communications:

1. I.E. Chican, D. V?r??teanu, I. Fier?scu, R.C. Fier?scu, I-L. Calancea, R. Petre, Corrosion Protection of Metallic Surfaces in Peroxide – Surfactant Formulation, EUROINVENT International Conference on Innovative  Research, Iasi, 21-22 May 2020. Poster
2. N.D. Banu, E. Ghibu, D.M. Vuluga, V.T. Iordache, I.E. Chican, R. Petre, V.V. Jerca, F.A. Jerca, Polyvinyl alcohol materials for chemically contaminated surfaces, Congresul International al Universitatii “APOLLONIA”, Editia a XXX-a, Iasi, Romania, 27 February – 1 March 2020. Poster

            Published articles or sent for publication:

1. I.E. Chican, D. V?r??teanu, I. Fier?scu, R.C. Fier?scu, I-L. Calancea, R. Petre, Corrosion Protection of Metallic Surfaces in Peroxide – Surfactant Formulations, IOP Conference Series: Materials Science and Engineering, 2020, 877(1), 012009.

Activ Link of Project 1 "POLIDEC", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro 

PHASE IV: Completion of Demonstration Studies

PARTNERS: IC ICECHIM; P1 CCSA-CBRNE; P2 CCO; P3 CCSFN

TOTAL BUDGET PC. 1: 951.200 RON (according to the additional document)

PROJECT PERIOD: 19.03.2018-18.08.2021 (according to the additional document)

PHASE IV: Completion of Demonstration Studies

PHASE PERIOD: 01.01.2021-18.08.2021

BUDGET PC. 1, PHASE IV:  62.109 RON

SPECIFIC OBJECTIVES:

Activity 4.1. Optimization of technologies for obtaining decontamination products based on surfactants – Part 2.

Achievement indicators: Demonstrator of the efficiency of surfactant decontamination products;

Activity 4.2. Optimization of technologies for obtaining decontamination products based on polymer gels – Part 2.

Achievement indicators: Demonstrator of the efficiency of decontamination products based on polymer gels;

Activity 4.3. Selection of products with optimal decontamination efficiency on a wide range of CBRN agents – Part 2

Achievement indicators: The appearance of the offer of research / technological services on erris.gov.ro; 2 patent applications registered, 1 proceeding paper published and 1 scientific communication. Another scientific communication will be presented at PRIOCHEM 2021 symposium.

SUMMARY:

         In this stage, the laboratory technology was optimized in order to obtain the surfactant-based decontamination solution, containing an aqueous system based on three surfactants (one amino acid surfactant and two nonionic surfactants), two glycols (polyethylene glycol and propylene glycol), an inhibitor of corrosion and hydrogen peroxide as an oxidizing agent.

The results obtained after the evaluation of the surfaces of steel or painted steel subjected to the attack of the decontamination solutions 9 and SD10 show an effective anticorrosive effect of the solutions SD9 and SD10. The decontamination solutions SD9 and SD10 were tested on a metallic surface contaminated with DMMP (dimethyl methylphosphonate) with a concentration of 8.61µL DMMP/100 mL DCM. The degree of decontamination using the SD9 solution was 99.98% and for the SD10 solution 99.99%. The testing of the polymeric gels obtained in stage III was extended to other chemical control agents with neurotoxic effect such as soman (GD) or with blistering action such as mustard gas (HD). Decontamination tests show an efficiency of over 85% for GD and over 99% for HD. Samples S3 and S5 were selected as products with optimal decontamination efficiency. The exact component of the decontamination kit based on polymer gels and surfactants was established, as well as a way to use the 3 components to maximize the degree of decontamination up to 100%. Within the component Project 1-POLIDEC, Phase IV, the communication of the research results was made within a scientific event in the form of a Poster communication type and two patent applications were filed. Moreover, a new research offer on erris.gov.ro was realized.

The research team composed of ICECHIM, CCSA-CBRNE, CCO and CCSFN met the objectives proposed for stage IV of PC 1 POLIDEC with a total degree of achievement.

RESEARCH OFFER

Conditioning and characterization of surfactant based products and auxiliaries https://eeris.eu/ERIF-2000-000X-4110  

DISSEMINATION

Scientific Communications:

1. Photocrosslinkable polymeric coatings for surface decontamination, Nicoleta Doriana Banu, Emilian Ghibu, Dumitru Mircea Vuluga, Verona Tanta Iordache, Irina Elena Chican, Razvan Petre, Valentin Victor Jerca, Florica Adriana Jerca, at International Congress: 2^nd Bucharest Polymer Conference, Bucharest, Romania, 9-11 June 2021 (Poster).

      INNOVATION:

1. Patent application A202100130/26.03.2021, Solu?ii polimerice pentru decontaminarea chimic? ?i radiochimic? ?i procedeu de ob?inere al acestora, Inventors: Florica Adriana Jerca, Valentin Victor Jerca, Nicoleta Doriana Banu, Emilian Ghibu

2. Patent application A202100484/13.08.2021, Solu?ii pe baz? de surfactan?i ecologici pentru neutralizarea agen?ilor chimici de r?zboi, Inventors: Irina Chican, Dana Varasteanu, Irina Fierascu, Radu Fierascu, Tanta-Verona Iordache

 Active Link of Project 1 "POLIDEC", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en and

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro

Component Project 2 " Counteraction of shock waves targeting marine vessels using synergic polymer materials MAUS"

PARTNERS: IC CCO; P1 ICECHIM; P2 UPB; P3 CCSFN

TOTAL BUDGET PC. 2: 1.090.000 RON

PROJECT PERIOD: 19.03.2018-18.08.2020 (according to the additional document)

The most likely danger that threatens military vessels is non-contact explosions, when shock waves in the form of high-pressure waves are launched to ships. Even if such explosions do not cause catastrophic damage to the structure or superstructure, the shock and associated vibrations can cause the ship's inability by damaging critical components and systems. An additional protection to that achieved during the design phase, especially for vessels which are most vulnerable to destruction due to repeated submarine explosions, can be achieved by placing on the inside of the ship's shell a layer consisting of wave shock absorption modules (MAUS), capable of dissipating within the internal structure and absorbing the shock wave energy, and thus, balancing the elastic pulsation of the ship's shell. It is imperative to the MAUS elements to be aligned with the internal rules for shipbuilding and, in addition, to have specific properties appropriate to their intended purpose, namely: durability, chemical stability, temperature and dimensional stability, open flame stability, mechanical strength, elasticity, compressibility and others and, last but not least, low price. Designing materials and structures resistant to shocks caused by explosions is a critical engineering problem. Hence, the overall objective of the project is to develop wave shock absorption modules (MAUS) consisting of composite sandwich systems with metallic faces and multilayer polyurethane foam filling of different chemical compositions and densities, consisting of: rigid nano foam -composite, containing phyllosilicates nanoparticle and semi-rigid / flexible foam containing mesogenic structural units.

PHASE I: Studies and experimental models

BUDGET PC. 2, PHASE I: 325.910 RON

PHASE PERIOD: 19.03.2018-31.12.2018

SPECIFIC OBJECTIVES:

Activity 1.5. Experiments for the synthesis of MAUS precursors

Activity 1.6. Elaboration of experimental models and realization of the MAUS theoretical concept

Activity 1.7. Elaboration of functional model for obtaining polyols containing mesogenic units

Activity 1.8. Developing the functional model for obtaining the polyols / filosilicate composites

Activity 1.9. Characterization of polyols containing mesogenic structural units and polyols / filosilicate composites, obtained by developing the experimental models

Activity 1.10. Disseminationof results

SUMMARY

During this stage, a material and data base was obtained for MAUS, consisting in the systematization of the theoretical considerations underlying the MAUS concept; its verification by preliminary experiments; synthesis of 4 ionic liquid catalysts, of which 2 original structures, used in the synthesis of polyols containing mesogenic units; 4 experimental models consisting of 3 experimental laboratory models on the synthesis of polyols with mesolite units, the polyols / filosilicate composites and the production of foams polyurethane and 1 experimental design model for MAUS configurations, using numerical modeling and simulation methods; a functional model for obtaining polyols with mesogenic units consisting of their synthesis recipes, a functional model for obtaining the polyols / filosilicate composites, consisting of recipes for their obtaining, 4 variants of chemical structures of polyols with mesogenic structural units (4 Selected samples) and 8 variants of polyol / filosilicate composite chemical structures (3 selected samples), results of their physico-chemical characterization by chemical methods, viscosity measurements, FT-IT and NMR spectroscopy and X-ray diffractometry, which have revealed their main features and allowed conclusions  to be drawn as to how chemical reactions and phyllosilicated polyols interact-useful for selecting optimal variants and improving the methods of obtaining the next steps. The scientific results obtained were disseminated by publishing an article in an ISI rated journal in Romania and developing and sustaining an oral presentation and a poster at a national conference with international participation. An active link of Project 2 "MAUS" was also constructed on the main website of the SECURE-NET Complex Project. Three young researchers were hired and several trips were made to participate at scientific events. The research team composed of (CCO, ICECHIM, UPB and CCSFN) met the proposed objectives for the PHASE 1 of PC 2 MAUS with a total degree of achievement.

DISSEMINATION

Scientific Communications:

1.Robert-Andrei Tincu, Andrei Slabu, Maria Maganu, Monica Duldner, Bogdan Cursaru, Emeric Bartha” Tailored synthesis of aromatic polyesterpolyols from PET wastes, using metal containing ionic liquids as catalysts” - a XXXV-a Conferinta Nationala de Chimie, 02-05 octombrie 2018, calimanesti-Caciulata, Valcea, Romania- Oral Comunication;

2.Robert-Andrei Tincu, Mihai Deleanu, Andrei Slabu, Monica Duldner, Cristina Stavrache, Emeric Bartha  “Modified ionic liquids as PET depolymerisation catalysts: synthesys and characterization” - a XXXV-a Conferinta Nationala de Chimie, 02-05 octombrie 2018, calimanesti-Caciulata, Valcea, Romania-  poster

Articles:

1. Simona Nica, Sorana Ionescu, Anamaria Hanganu, Monica Duldner, Stela Iancu, Andrei Sarbu, Petru Filip, Emeric Bartha “Mechanistic Investigations of the Organocatalytic Depolymerization of PET Waste with Isosorbide”  Rev. Chim. 69, 6, 2018, 1319-1326     

Activ Link of Project 2 "MAUS", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro 

PHASE II: Development of Functional Models and Technologies

BUDGET PC. 2, PHASE II: 343.350 RON

PHASE PERIOD: 01.01.2019-31.12.2019

 SPECIFIC OBJECTIVES:

Activity 2.6. Elaboration of the functional model for obtaining the nanocomposites PUR foams

Activity 2.7. Elaboration of the functional model for obtaining the PUSR / PUF foams

Activity 2.8. Characterization of nanocomposite PUR foams and PUSR / PUF foams containing mesogenic structural units obtained by developing experimental models

Activity 2.9. Elaboration and testing of the composite MAUS modules at shock wave action

Activity 2.10. Identification and protection of intellectual property rights

Activity 2.11. Disseminationof results

SUMMARY

As a result of the research work carried out in the second phase of the project, the following results were obtained: 1 Protocol for the obtaining of the PUR foams and Protocol for the obtaining of PUSR / PUF foams, for which experimental models have been developed previously. Both precursors and polyurethane foams have been characterized in terms of chemical structure (FT-IR, NMR), degree of intercalation of montmorilonite, and for the (nano) composite foams, thermal stability (TGA), viscoelastic behavior in dynamic regime (DMA) and physical-mechanical characteristics (traction, compression). Analysis bulletins were released. A MAUS sandwich module was developed by depositing two layers of polyurethane foams of different types, with a total thickness of 50 mm, between two metal plates, of thicknesses 10 and 5 mm, which was submitted for testing at shock wave action. A MAUS Preparation Protocol was developed. A testing stand of the MAUS module was designed and developed. A viable Sandwich material solution was investigated to improve the behaviour of impact structures, using the finite element method. An unconventional Sandwich-type structure was designed and tested using direct finite element analysis for elastic and plastic behaviour. Thus, the MAUS module was evaluated at shock wave action. Two patent applications were developed and registered at OSIM and 1 scientific ISI article was published. Moreover, the scientific results obtained were disseminated through 7 Scientific Communications at international and national events. A Workshop on the obtained results within the project was organized and held at the University Politehnica of Bucharest. For the presentation of the Scientific Communications, several were trips were made to: 1. 9th International Conference of the Chemical Societies of the South-East European Countries (ICOSECS9), Târgovi?te, Romania, 2. 21st Romanian International Conference on Chemistry and Chemical Engineering (RICCCE21), Mamaia, Romania, 3. 13th Students' Congress of SCTM, Skopje, Macedonia, 4. International Conference "Achievements and Perspectives of Modern Chemistry", Chisinau, Republic of Moldova. The research team composed of (CCO, ICECHIM, UPB and CCSFN) met the proposed objectives for the PHASE 2 of PC 2 MAUS with a total degree of achievement.

 DISSEMINATION

Scientific Communications:

1. Monica Duldner, Alina Elena Coman, Anita Radu, Emeric Bartha, Robert Tincu, Tanta-Verona Iordache, Andrei Sarbu, Adi Ghebaur, Celina Damian “(Nano)composite polyurethane foams from PET wastes and renewable raw materials“ 21-st Romanian International Conference on Chemistry and Chemical Engineering (RICCCE), Constanta- Mamaia Romania, September 4-7 2019 -poster

2. Robert-Andrei ?incu, Constantin Dr?ghici, Andrei Slabu, Monica Duldner, Alina Elena Coman, Emeric Bartha “5-Hydroxymethylfurfural Synthesis in Biphasic Solvent Systems” 21st Romanian International Conference on Chemistry and Chemical Engineering (RICCCE), Constanta- Mamaia, ROMANIA - September 4 – 7, 2019 -poster

3. Robert ?incu, Andrei Slabu, Maria Maganu, Constantin Dr?ghici, Monica Duldner, Alina Coman, Emeric Bartha “Attempts to obtain 5-Hydroxymethylfurfural” International Conference “ACHIEVEMENTS AND PERSPECTIVES OF MODERN CHEMISTRY”October 9-11, 2019, Chisinau, Republic of Moldova -poster

4. Robert-Andrei ?incu, Andrei Slabu, Maria Maganu, Cristina Stavarache, Monica Duldner, Emeric Bartha “Metal containing ionic liquids as catalysts for synthesis of polyester-polyols from PET wastes” 13th Students' Congress of The Society of Chemists and Technologists of Macedonia, Skopje, Macedonia, 19-21 septembrie 2019.- oral communication

5. Robert ?incu, Andrei Slabu, Maria Maganu, Constantin Dr?ghici, Monica Duldner, Alina Coman, Emeric Bartha “PET wasts recycling using various glycols and metal containing ionic liquids” International Conference “ACHIEVEMENTS AND PERSPECTIVES OF MODERN CHEMISTRY” October 9-11, 2019, Chisinau, Republic of Moldova- poster

6. Robert-Andrei ?incu, Constantin Dr?ghici, Andrei Slabu, Monica Duldner, Alina Elena Coman, Emeric Bartha „Towards an imporved synthesis of 5-hydroxymethylfurfural from fructose” 9th International Conference of the Chemical Societies of the South-East European Countries (ICOSECS)” 8- 11 May 2019 Targoviste, Romania- oral communication

7. Participare la Workshop-ul: “Noi Materiale si Metode privind Contingenta Hazardurilor CBRN si Imbunatatirea Mijloacelor de Securitate Nationala” Facultatea de Chimie Aplicata si Stiinta Materialelor, Universitatea Politehnica Bucuresti, 23 Septembrie 2019, cu prezentarea: Experimentari de obtinere a precursorilor pentru realizarea Modulelor de amortizare a undelor de soc (MAUS); Proiectarea testelor experimentale privind impactul socului de presiune asupra modulelor MAUS

 Articles:

1. Monica-Mirela Duldner, Emeric Bartha, Stanca Capitanu, Simona Nica, Alina Elena Coman , Robert Tincu, Andrei Sarbu, Petru Filip, Steluta Apostol, Sorina Garea “Attempts to Upcycle PET Wastes into Bio-based Long-lasting Insulating Materials” Rev. Chim. 70(7), 2301 (2019)

Patent applications:

1. Compozite Poliester-Eter Polioli/Montmorilonit Pentru Spume Poliuretanice Semiflexibile (Nano)Compozite Si Procedeu De Obtinere A Acestora (Polyester-Ether Polyols / Montmorilonite Composites for (Nano) Composite Semiflexible Polyurethane Foams and Process for Obtaining Them). Authors: Duldner Monica- Mirela, Coman Alina-Elena, Iordache Tanta Verona, Sarbu Andrei, Bartha Emeric, Tincu Robert-Andrei, Ghebaur Adi, Damian Celina, Surdu George, Savastre Alexandru, Patent Claim A2019-00845/03.12.2019.

2.  Polioli Cu Structura Poliester-Amidica Continand Unitati Structurale Mezogene Pentru Spume Poliuretanice Semiflexibile Si Procedeu De Obtinere A Acestora (Polyols with Polyester-Amid Structure Containing Mesogenic Structural Units for Semiflexible Polyurethane Foams and Process for Obtaining Them). Authors: Duldner Monica-Mirela, Coman Alina-Elena, Iordache Tanta Verona, Sarbu Andrei, Bartha Emeric, Teodorescu Florina, Ghebaur Adi, Chitulescu Victor- Ioan, Surdu George, Popa Sterica,Patent Claim A2019-00849/03.12.2019.

Activ Link of Project 2 "MAUS", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro 

PHASE III: Development of Functional Models and Technologies

BUDGET PC. 2, PHASE III: 382.206 RON

PHASE PERIOD: 01.01.2020-31.12.2020

SPECIFIC OBJECTIVES:

Activity 3.6. Improving and verifying the reproducibility of the procedures for obtaining MAUS precursor foams

Achievement indicators: Advanced processes for precursor synthesis; Physico-chemical analysis;

Activity 3.7. Characterization of polyols containing mesogenic structural units, polyol/phyllosilicate composites, nanocomposite PUR foams and PUF/PUSR foams obtained by perfecting experimental procedures - Part 1

Achievement indicators: Partial analysis bulletin;

Activity 3.8. Development of laboratory technologies for the preparation of polyols containing mesogenic structural units, polyol/phyllosilicate composites, nanocomposite PUR foams and PUF/PUSR foams.

Achievement indicators: Improved protocol for obtaining MAUS precursor foams; the appearance of the offer for research/technological services on erris.gov.ro;

Activity 3.9. Making the MAUS compact composite made up of precursor modules - Part 1

Achievement indicators: Foam compaction protocol for obtaining MAUS;

Activity 3.10. Elaboration of scientific papers

Achievement indicators:  1 ISI paper sent for publication;

Activity 3.11. Disseminationof results

Achievement indicators: 1 scientific communication (conference postponed for 2021);

SUMMARY

As a result of the research works carried out in Stage III of the project, the following results were obtained: 4 laboratory technologies for the preparation of Maus precursors, namely Technology for the preparation of polyols containing mesogenic structural units; Technology for the preparation of polyol/montmorillonite composites; PUF/PUSR foam preparation technology with content of mesogenic units; PUR (nano) composite foam preparation technology. For the elaboration of the technologies, 2 variants of polyols containing mesogenic units and 6 variants of polyol / montmorillonite composites were synthesized, which were characterized from a physico-chemical and structural point of view (NMR, FT-IR, XRD), and used in obtaining PUR / PUSR foams, which were characterized from a thermal and mechanical point of view by TGA and DMA. The aim was to improve and verify the reproducibility of the processes for obtaining MAUS precursor foams, to formulate the improved procedures for synthesizing precursors, to obtain data on the properties of precursors (Analysis Bulletins) and to draft the improved Protocol for obtaining MAUS precursor foams. The MAUS compact composite was further finalized. The obtaining of the compact composite which contains MAUS precursors consisted in compacting the two types of PUR/PUSR foams, with different chemical structures and densities obtained using precursor polyols, between two steel plates of 10 and 5 mm thickness, respectively. In this respect, a Foam Compaction Protocol was elaborated for obtaining MAUS and a Protocol for testing MAUS modules at the action of shock waves. Dissemination of the results consisted in: Elaboration of scientific papers - 1 article accepted for publication in the journal Materiale Plastice (ISI listed) and 1 paper submitted to the "2nd Bucharest Polymer Conference Bucharest, ROMANIA - June 10-12, 2020, which, due to the postponement of the Conference will be presented in 2021. The research works will continue in 2021, for the elaboration of the Technical Specifications for the realization of the MAUS compact composite. The research team composed of (CCO, ICECHIM, UPB and CCSFN) met the objectives proposed for stage III of PC 2 MAUS with a total degree of achievement.

DISSEMINATION

Offer of research services erris.gov.ro:

S17. Preparation of composite sandwich modules made of steel / polyurethane foams (with different degrees of flexibility) / steel

Articles:

1. Robert ?incu, Florina Teodorescu, Andrei Slabu, Monica-Mirela Duldner, Alina Elena Coman, Emeric Bartha " PET glycolysis using metal-containing ionic liquids as catalyst", Materiale Plastice, 2020.

Scientific Communications:

1. During the summary of 2020, a Poster was registered at the “2nd Bucharest Polymer Conference Bucharest, ROMANIA - June 10-12, 2020, which was postponed for June 9-11, 2021: M. Duldner, A. Coman, A. Miron, V. Iordache, A. Sarbu, E. Bartha, F. Teodorescu, R.Tincu, A. Ghebaur, C. Damian „Polyols with polyester-amidic structure containing mesogenic moieties, for semiflexible polyurethane foams, from PET wastes ”

Activ Link of Project 2 "MAUS", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro 

PHASE IV: Completion of Demonstration Studies 

PARTNERS: IC CCO; P1 ICECHIM; P2 UPB; P3 CCSFN

TOTAL BUDGET PC. 2: 1.108.200 RON (according to the additional document)

PROJECT PERIOD: 19.03.2018-18.08.2021 (according to the additional document)

PHASE IV: Completion of Demonstration Studies

PHASE PERIOD: 01.01.2021-18.08.2021

BUDGET PC. 2, PHASE IV:  56.734 RON

SPECIFIC OBJECTIVES:

Activity 4.4 - Characterization of polyols containing mesogenic structural units, polyol/phyllosilicate composites, nanocomposite PUR foams and PUF/PUSR foams obtained by perfecting experimental procedures - Part 2

            Achievement indicators: Final analysis bulletin;

Activity 4.5 – Obtaining the MAUS compact composite made up of precursor modules - Part 2

 Achievement indicators: Technical specifications for obtaining MAUS compact composite; 1 ISI article published and 1 scientific communication. Another scientific communication will be presented at PRIOCHEM 2021 symposium and an article in progress will be submitted for publication by the end of 2021.

SUMMARY

In the final stage, the aim was to complete the demonstration studies starting from the preparation of two types of phyllosilicate polyol composites and two compact MAUS modules. In order to obtain the composites, the sequence of process steps was varied, and the addition of MM suspended in water was tested, to the advantage of the degree of intercalation/exfoliation of montmorillonite. The composite experiments obtained in this stage and the variants obtained in the previous stages were ultrasonicated in order to favor the intercalation of the phyllosilicate. Ultrasonic polyol/phyllosilicate composites were characterized from physical-chemical point of view according to the standards described in the previous steps, as well as from a structural point of view by 1H-NMR and FT-IR spectroscopy. It was highlighted that there are no structural changes between the ultrasonic and non-ultrasonic composites. Ultrasonic composite samples were tested for the formation of polyurethane foams, which were characterized by thermal (TGA) and physical-mechanical (DMA, mechanical tests - traction and compression). The results revealed a compression behavior characteristic of semi-rigid polyurethane foams. Two compact MAUS modules were made by pouring the two types of polyurethane foams (nano) composites and containing mesogenic units - designed to present high densities between two outer steel plates, separated by another median steel plate, obtaining two compact sandwich composites. The modules were impact tested on a test stand designed and built for this purpose in the previous stages, highlighting a reduction of 57.69% - 64.61% of the maximum material displacement. Neither the outer metal plates nor the polyurethane foams cracked during the tests, which indicates a satisfactory mechanical strength of the modules for the intended application in the naval field. During this stage, results were disseminated through a communication and a scientific article published. The research team composed of (CCO, ICECHIM, UPB and CCSFN) met the objectives proposed for stage IV of PC 2 MAUS with a total degree of achievement.

DISSEMINATION

Article published: 

1. Alina Elena Coman, Julien Peyrton, Gheorghe Hubca, Andrei Sarbu, Augusta Raluca Gabor, Cristian Andi Nicolae, T.V. Iordache, L. Averous, Synthesis and characterization of renewable polyurethane foams using different biobased polyols from olive oil, European Polymer Journal, 2021, 110363.

Scientific communication:

1. Alina Elena Coman, Monica Mirela Duldner, Tanta Verona Iordache, Gheorghe Hubca, Florin Dîrloman, Ana Mihaela Gavrila, Ana-Lorena Ciurlic?, Synthesis of different polyols from polyester polyols obtained from renewable resources and recycled materials, used for PU production, 4^th European Chemistry Conference’, ECC-2021 Virtual, 12.04.2021 (oral communication)

Active Link of Project 2 "MAUS", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en and

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro 

Component Project 3 "Detection of persistent warfare chemical agents with specific screen-printed sensors ACLSENSE"

PARTNERS: IC ICECHIM; P1 CCSA-CBRNE; P2 ATM; P3 CCO; P4 CCSFN

TOTAL BUDGET PC. 3: 1.115.000 RON

PROJECT PERIOD: 19.03.2018-18.08.2021 (according to the additional document)

Chemical weapons are a means of mass destruction of personnel, the destruction of crops, or the deterioration of some military equipment, and the debilitation of combat troops by the contamination of air, land, fighting techniques, and various materials with warfare chemical agents (ACLs). Given that ACLs are very toxic (producing irritations, temporary physiological effects, serious illness or even death when used in combat concentrations) it is relevant to emphasize the development of small portable devices that can quickly and efficiently detect ACL traces. Although conventional analytical techniques for detecting ACLs (HPLC, LC, GC) are sensitive and specific, some drawbacks can be identified, namely extensive preparation and extraction steps, high organic solvent consumption, and expensive equipment. Therefore, literature provides important information on a simple and inexpensive method which can be applied for detecting ACLs in the atmosphere. This particular technique is based on the use of molecular imprinted polymers (MIPs) for sensors development. MIPs are synthetic materials that have specific complementary cavities of same shape, size and electronic entourage with a target molecule called template. Sensors with MIP recognition elements can identify and quantify the target molecules by transforming the MIP-analyte re-binding event into information, and thereafter, into a measurable physical signal. Thus, the overall objective of the project is to develop a new electrochemical sensor based on MIPs and sol-gel technologies to develop a simple, fast and efficient detection method for persistent ACLs.

PHASE I: Studies and experimental models

BUDGET PC. 3, PHASE I: 333.875 RON

PHASE PERIOD: 19.03.2018-31.12.2018

SPECIFIC OBJECTIVES:

Activity 1.11 Determination of precursor monomers and synthesis conditions for obtaining ACL-MIPs particles, depending on the approached method, and selection of ACLs of interest

Activity 1.12 Studies for obtaining imprinted ACL-MIPs and control ACL-NIPs by various chemical processes (mass polymerization / precipitation)

Activity 1.13 Structural and Morphological Characterization of ACL-MIPs and ACL-NIPs by FTIR, TGA, SEM, AFM, BET

Activity 1.14 Research for the simulation of extracted ACL-MIPs action from ACL vapours

Activity 1.15 Dissemination of results

SUMMARY

In Phase 1, the precursor monomers, the ACLs of interest and the synthesis conditions for obtaining ACL-MIPs particles were established, taking into account the data base resulting from the study of the ACL literature. Following the findings of the study, ACLs of interest were selected through: a study of vesicant agents, physicochemical properties, sulphur-mustard and detection methods, mechanisms proposed for vesicant action; a study conducted on MIP for ACL contributing to the establishment of the polymerization system. The experimental work has led to the successful production of four pairs of ACL-MIPs and non-implied NIPs homologues based on methacrylic acid and methylene bisacrylamide with ethylene glycol dimethacrylate by the two proposed polymerization methods, precipitation and mass. The ACL-MIPs particles were synthesized in order to be incorporated into an ACL-MIP / sol-gel ACL-sensed electrochemical sensor for ACL detection. For molecular imprinting with ACL, the simulant of the vesicant agent sulphur-mustard, i.e. thiodiglycol (TDG) was synthesized and characterized by GC / MS and FTIR. The new ACL-MIPs and NIPs particles were analyzed structurally and thermally by appropriate methods, such as FTIR and TGA, and morphologically, by SEM and BET. Finally, research was carried out to simulate the action of two types of imprinted ACL-MIP particles in the presence of ACL. New scientific results have been disseminated by presenting 2 poster-based scientific communications and 1 oral communication. Besides the dissemination of the results in the component project, a new young researcher was hired and an active link of Project 3 "ACLSENSE" was built on the website of SECURE-NET Complex Project. The research team composed of (ICECHIM, CCSA-CBRNE, ATM, CCO and CCSFN) met the proposed objectives for Phase 1 of ACLSENSE PC 3 with a total degree of achievement.

DISSEMINATION

Scientific Communications:

1. Ana-Mihaela Florea, Anamaria Zaharia, Anita-Laura Radu, Steluta Apostol, Bianca Georgescu, Traian Rotariu, Tudor-Viorel Tiganescu, Andreea-Elena Voicu, Andrei Sarbu, Tan?a-Verona Iordache, “Molecularly imprinted elements for the recognition of 2,4,6-trinitrotoluene”, EUPOC 2018, Como (Italy), 20-24 May 2018 (Poster)

2. Ana-Mihaela Florea, Tan?a-Verona Iordache, Bianca E. Georgescu, Anamaria Zaharia, Anita-Laura Radu, Steluta Apostol and Andrei Sârbu, “Novel Molecularly Imprinted Films: A Comparative Study For Ephedrine And Bisphenol A Recognition”, Bucharest Polymer Conference (BPC), 6-8 June 2018, Bucharest, Romania (Oral Communication)

3. Valentin Victor Jerca, Florica Adriana Jerca, Richard Hoogenboom, ”Poly(2-isopropenyl-2-oxazoline)-A versatile platform for advanced multifunctional materials” 7th EuCheMS Chemistry Congress, Liverpool, UK, 26-30 Aug 2018 (Poster).

Activ Link of Project 3 "ACL-SENSE", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro 

PHASE II: Development of Functional Models and Technologies

BUDGET PC. 3, PHASE II: 350.906 RON

PHASE PERIOD: 01.01.2019-31.12.2019

SPECIFIC OBJECTIVES:

Activity 2.12 Developing of ACL-MIPs/sol-gel-ECS screen-printed sensors by deposition of the organosilane sensitive layer with inserts of MIP particles, by sol-gel technique, on screen-printed carbon electrodes

Activity 2.13 Structural and Morphological Characterization of ACL-MIPs/sol-gel-ECS screen-printed sensors by FTIR, TGA, SEM, AFM, BET

Activity 2.14 Establishing the analytical performance of the sensors with ACL in order to select the most efficient sensors. Testing of the electrochemical properties by cyclic voltammetry. Elaboration of the Functional Model

Activity 2.15 Testing of sensitivity, selectivity and determination of sensors response time in the presence of ACL vapors

Activity 2.16 Identification and protection of intellectual property rights

Activity 2.17 Dissemination of results

SUMMARY

In Phase II/2019, functional models were elaborated for the developing of ACL-MIPs/sol-gel-ECS screen-printed sensors by deposition of the organosilane sensitive layer with inserts of MIP particles, by sol-gel technique, on screen-printed carbon electrodes (ECS). Micro- and nanoparticles of molecularly imprinted polymers (MIPs) were synthesized by precipitation polymerization, using several functional monomers, namely methacrylic acid, 4-vinylpyridine, methylenbisacrylamide (MBA) as well as monomers with electroactive properties of the ferrocene class (acetylferrocene, AcF). Imprinted MIP particles and non-imprinted NIP particles as well as MIPs/sol-gel-ECS si NIPs/sol-gel-ECS screen-printed sensors were characterized by specific morpho-structural and thermal methods using FTIR, TGA, SEM, AFM, BET and respectively electrochemical methods via cyclic voltammetry. The best results were obtained for the MIP based on MBA and AcF. The linear range of the most performant screen-printed sensors with inserts MIP particles is 10^-7 M, for those modified with MIP nanoparticles based on AcF and 10^-6 M, respectively, for those based on MBA, which are highly recommended for thiodiglycol detection as ACL. Screen-printed sensors with AcF have been proved to be selective against another ACL, dimethyl methylphosphonate. One patent application was developed and registered at OSIM and 1 scientific ISI article was sent for publication. Moreover, the scientific results obtained were disseminated through 7 Scientific Communications at international and national events. Within the Project Component 3-ACLSENSE, 2 trips were made abroad, which aimed to disseminate the results through Poster-type communication. Dr. Eng. Ana-Mihaela Gavrila sustained two communications in the country at the NeXT-Chem Exploratory Workshop, Bucharest and Early Career Scientists (ECS) STO NATO Bucharest. In addition, Mr.dr.ing. Constantin Toader traveled to Turkey at the APMAS 2019 conference, with the purpose of disseminating the results and Dr. Ing. Jerca Valentin Victor made 1 trip locally in order to disseminate the results through a guest oral communication. The research team composed of (ICECHIM, CCSA-CBRNE, ATM, CCO and CCSFN) met the proposed objectives for PHASE 2 of PC 3 ACLSENSE with a total degree of achievement.

DISSEMINATION

Scientific Communications:

1. Tanta-Verona Iordache, Ana-Mihaela Gavrila, Andrei Sarbu, Ana Lorena Ciurlica, Constantin Nicolae Toader, Anamaria Zaharia, Anita-Laura Radu, Alina Coman, Stoica Elena-Bianca, “A selective receptor based on a molecularly imprinted polymer for sulphur mustard”, World Congress on Functional Materials and Nanotechnology (WCFMN), 13-14 May 2019, Spain (Poster)

2. Ana-Mihaela Gavrila, Ana Lorena Ciurlica, Andrei Sârbu, Anamaria Zaharia, Anita-Laura Radu, Steluta Apostol, Elena-Bianca Stoica, Constantin Nicolae Toader and Tan?a-Verona Iordache, “Preparation and characterization of molecularly imprinted particles for sulphur mustard determination”, 8th Graduate Student Symposium on Molecular Imprinting, 28-30.08.2019, Berlin, Germany (Poster)

3. Ana-Lorena CIURLIC?, Tan?a-Verona IORDACHE, Andrei SÂRBU, Anamaria ZAHARIA, Anita-Laura RADU, Teodor SANDU, Bianca STOICA, Alina COMAN, Nicolae MARUNTELU si Ana-Mihaela GAVRIL?, “Molecularly imprinted films and particles”, NeXT-Chem Workshop Exploratoriu, 6-7 May 2019, Bucharest, Romania (Oral Communication)

4. Ana-Mihaela Gavrila, Andrei Sârbu, Ana Lorena Ciurlica, Anamaria Zaharia, Anita-Laura Radu, Constantin Nicolae Toader, Tan?a-Verona Iordache, “Advanced Materials for Sulphur Mustard Recognition and Retention Prepared by Molecular Imprinting Techniques”, Selected for participation at Early Career Scientists (ECS) STO NATO Bucharest, Palace of Parliament, 18 September 2019, Bucharest, Romania (Poster)

5. WORKSHOP Proiect Component 3 “ACLSENSE“, Ana-Mihaela Gavrila, Constantin Toader, Jerca Victor, Andreea Voicu, Elena Curca, “Realizarea senzorilor serigrafiati specifici cu agenti chimici de lupta“, in cadrul Workshop Proiect Complex SECURE-NET “Noi Materiale si Metode privind Contingenta Hazardurilor CBRN si Imbunatatirea Mijloacelor de Securitate Nationala”, 23.09.2019, Universitatea Politehnica Bucuresti (Oral Communication).

6. N. Grigoriu, C.N. Toader, T.V. ?ig?nescu, G. Epure, C. L?z?roaie, N. Sc?ri?oreanu, C. Viespe, R. E. Ginghin?, N. Petrea, “Testing the sensitivity, selectivity and time of response of some polymeric sensors in the presence of toxic compounds vapours”, 9th International Advances in Applied Physics and Materials Science Congress & Exhibition (APMAS 2019), 22-28.10.2019, Fethiye - Mugla, Turkey (poster)

7. Jerca, V.V., Jerca, F.A., Spiridon, M.C., Banu, N.D., Ghibu, E., Vuluga, D.M., Non-Linear Optical Applications or Drug Controlled Release from Poly-2-Oxazoline Matrix, Sixth International Workshop on Advanced Nano- and Biomaterials and Their Device Applications, 12-16 Mai, 2019 Cluj, Romania, Invited Oral Communication.

Article sent for publication:

1. Tanta-Verona Iordache, Nicoleta Doriana Banu, Elena Diana Giol, Dumitru Mircea Vuluga, Florica Adriana Jerca, Valentin Victor Jerca, “Factorial Design Optimization of Polystyrene Microspheres Obtained by Aqueous Dispersion Polymerization in the Presence of Poly(2-ethyl-2-oxazoline) Reactive Stabilizer”, Polymer International, 2019, Submitted manuscript for special issue

Patent applications

1. Filme hibride senzitive imprentate molecular cu tiodiglicol depuse pe electrozi serigrafia?i de carbon ?i procedeu pentru ob?inerea acestora/Sensitive hybrid molecularly imprinted films with thiodiglycol deposited on carbon-screen printed electrodes and process for obtaining them. Authors: Ana Mihaela Gavril?, Tan?a Verona Iordache, Andrei Sârbu, Ana Lorena Ciurlic?, Anamaria Zaharia, Anita Laura Chiriac, Teodor Sandu, Elena Bianca Stoica, Stelu?a Apostol, Patent Claim A 2019 -000779/22.11.2019.

Activ Link of Project 3 "ACL-SENSE", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro 

PHASE III: Development of Functional Models and Technologies

BUDGET PC. 3, PHASE III: 395.793 RON

PHASE PERIOD: 01.01.2020-31.12.2020

SPECIFIC OBJECTIVES:

Activity 3.12 Technology Development for obtaining the screen-printed sensor with the property of detecting ACLs

Performance indicators: Advanced sensor preparation protocol;

Activity 3.13 Structural and morphological characterization of ACL-MIPs/sol-gel-ECS sensors by FTIR, TGA, SEM, AFM, BET - Part 1

Achievement indicators: Partial analysis bulletin;

Activity 3.14 Tests to demonstrate the functionality and reproducibility of ACL-MIPs/sol-gel-ECS sensors in the laboratory (Cyclic voltammetry)

Achievement indicators: Appearance of the offer of research/technological services on erris.gov.ro;

Activity 3.15 Elaboration of scientific papers

Achievement indicators: 2 ISI articles published

Activity 3.16 Dissemination of results

Achievement indicators: 1 scientific communication;

SUMMARY

In stage III/2020 of the ACLSENSE project, the Optimization and Start of Demonstration Studies was carried out, which resulted in: Laboratory technology for the production of screen-printed sensors specific for ACL detectors and the Sensor Prototype. In this sense, the synthesis of particles based on MBA and AcF, respectively, imprinted with TDG MIP and non-imprinted NIP, was optimized. TDG-MIP particles and NIP control polymers and MIPs/sol-gel-ECS specific screen-printed sensors were subjected to physico-chemical characterization, namely morphological, thermal, porosimetric and structural-compositional analysis, to establish a correct correlation between their structure and TDG recognition properties. The SEM morphological results are similar for all MIP/NIP/sol-gel-ECS sensors, confirming that MIP/NIP particle inserts improve the properties of the organosilane sensitive layer deposited on the ECS. AFM analysis demonstrated that TDG influences the formation and size of particles and sols on the surface of sensors; the obtained results are reproductible and validate the results of the SEM morphological analyzes of the specific screen-printed sensors. Specific optimized screen-printed carbon sensors MIPs/sol-gel-ECS and NIPs/sol-gel-ECS tested electrochemically by cyclic voltammetry, in the presence and absence of TDG template, proved to be reproductible; the best results being obtained for the sensor system based on acetylferocene and ethylene glycol methacrylate, imprinted MIP 13 extracted/sol-gel-ECS (sensitivity obtained for the sensor with extracted MIP 13 of 1.86 * 10-5 A/μM (R2 = 0.9952)) and a response time only a few seconds and non-imprinted NIP 13/sol-gel-ECS (sensitivity 1.67 * 10-5 A/μM (R2 = 0.9866)). Within the SECURE-NET project, Component Project 3-ACLSENSE, Stage 3, the members of PC3 Project team did not performed any trips. The presentation of the obtained results was made through the following dissemination actions: 2 published articles and 1 oral communication at a national conference. The research team composed of (ICECHIM, CCSA-CBRNE, ATM, CCO and CCSFN) met the objectives proposed for stage III of PC 3 ACLSENSE with a total degree of achievement.

DISSEMINATION

Offer of research services on erris.gov.ro:

S16. Preparation of electrochemical sensors for the detection of chemical warfare agents simulant and voltametric methods

Article sent for publication:

1. 1.             Gavrila, A.-M., Iordache T. V., Lazau C., Rotariu T., Cernica I., Stroescu H., Stoica M., Orha C., Bandas C. E., Sarbu A., “Biomimetic Sensitive Elements for 2,4,6-Trinitrotoluene Tested on Multi-Layered Sensors”, Coatings 2020, 10, 273; doi:10.3390/coatings10030273 (Open Access article).

Scientific Communications:

1. 1.      Ana-Lorena CIURLIC?, Tan?a-Verona IORDACHE, Andrei SÂRBU, Constantin Nicolae TOADER, Teodor SANDU, Bianca STOICA, Alina COMAN, Andreea MIRON si Ana-Mihaela GAVRIL?, “Detection of Sulphur Mustard Simulant using MIP-based Screen-Printed Electrodes”, NeXT-Chem Workshop Exploratoriu, 2^nd Edition, May 2020, Bucharest, Romania (Oral communication)

Activ Link of Project 3 "ACL-SENSE", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro 

PHASE IV: Completion of Demonstration Studies

PARTNERS: IC ICECHIM; P1 CCSA-CBRNE; P2 ATM; P3 CCO; P4 CCSFN

TOTAL BUDGET PC. 3: 1.121.600 RON (according to the additional document)

PROJECT PERIOD: 19.03.2018-18.08.2021 (according to the additional document)

PHASE IV: Completion of Demonstration Studies

PHASE PERIOD: 01.01.2021-18.08.2021

BUDGET PC. 3, PHASE IV:  41.026 RON

SPECIFIC OBJECTIVES:

Activity 4.6 - Structural and morphological characterization of ACL-MIPs/sol-gel-ECS sensors by FTIR, TGA, SEM, AFM, BET - Part 2

Achievement indicators: Final analysis bulletin;

Activity 4.7 - Tests to demonstrate the functionality and reproducibility of ACL-MIPs/sol-gel-ECS sensors in the laboratory (Cyclic voltammetry)

Achievement indicators: Demonstrator of the sensor analytical performance; 1 article written that will be sent for publication by the end of 2021 (proposed Journal: Sensors and Actuators).

SUMMARY

         Phase IV/2021 of the project took into account the reproducibility of the recipes and the properties of the screen-printed sensors ACL-MIPs/sol-gel-ECS following the morpho-structural parameters: structural, thermal and morphological characterization of TDG-MIP particles, as well as the specific screen-printed sensors TDG-MIPs / sol-gel-ECS using FTIR, TGA, SEM, BET analyzes (Part 2); Tests to demonstrate the functionality and reproducibility of ACL-MIPs/sol-gel-ECS sensors in real conditions by cyclic voltammetry. The electrochemical sensors printed with TDG were built in three stages to reproduce the preparation protocol. Experimental work has led to the successful reproducibility of two series of MIP sensors [MIP 4 (MBA-EDMA) and MIP 13 (AcF-EDMA)] for TDG recognition. Thermogravimetric analysis revealed very good thermostability for all synthesized polymers and BET textural analyzes demonstrated the formation of microporous and mesoporous structures with comparable diameters and small specific surfaces that lead to small polymer particle sizes. The FTIR spectra of the MIP and control NIP particles showed the characteristic peaks of the polymer and also confirmed the presence of the TDG template in the matrix (especially in the case of MIP 13). The deposition of the organosilane layer with MIP 13 particle inserts allowed a sensitive detection of TDG with a detection limit (LOD) of only 0.33 μM and a response time of a few seconds, sensitivity of 1.98 * 10-5 A / μM and 2.01 * 10-5 A / μM, respectively. The selectivity results showed a significant difference between the electrochemical behavior of MIP 13/sol-gel-ECS for TDG compared to that obtained for dimethyl methylphosphonate (DMMP) and diisopropyl methylphosphonate (DIIP), leading to a decrease in the corresponding anodic current around ~ 8µA (28% TDG), ~ 5 µA (18% DMMP) and ~ 4µA (14% DIIP), respectively.

The research team composed of (ICECHIM, CCSA-CBRNE, ATM, CCO and CCSFN) met the objectives proposed for phase IV of PC 3 ACLSENSE with a total degree of achievement.

DISSEMINATION

Article draft:

Gavrila, A.-M., Ciurlica, A.L., Branger C., Brisset H., Toader, C., Stoica B.E., Sarbu A., Iordache T. V., A voltametric assay for the detection of sulfur mustard simulant based on screen-printed electrodes modified with molecularly imprinted microinsertions.

Active Link of Project 3 "ACL-SENSE", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en and

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro 

Component Project 4 "Smart polymeric composites for new generations of solid rocket fuel RAKETCOMB"

PARTNERS: IC ATM; P1 ICECHIM; P2 CCSA-CBRNE; P3 UPB;

TOTAL BUDGET PC. 4: 1.020.000 RON

PROJECT PERIOD: 19.03.2018-18.08.2021 (according to the additional document)

According to the specialists in the field, artillery and land missiles will continue to be the basis of the land-strike system while for missile and air forces missiles have been the main attack and defence systems for a long time. Spatial applications are also entirely based on rocket propulsion for launch and power generation. The main trend in the development of missiles is clearly linked to the increase in performance and traction. At the same time, in the context of the rapid tightening of international law, especially at European Union level, on the impact of military activities and, in particular, on environmental munitions, there is an important trend to develop new generations of propellants with low environmental  impact (green) throughout the lifetime, from manufacture to demilitarization / neutralization / use. At present, no solid rocket fuel producer exists in Romania, and their number is extremely low and decreasing at European level due to the tightening of environmental legislation (REACH regulation, air, water, and soil directives) and the disappearance of traditional raw material producers, respectively. In this context, of diminishing the production capacities of solid ingredients for solid rocket fuels at national and European level and, at the same time, of the explosion of knowledge generated in materials science and technology, the main objective of the project refers to development of new powder composites as solid rocket fuel with increased performance, reduced environmental impact and reduced cost price for the benefit of the national defence industry and, secondarily, the National Defence and Security System, the National Anti-hailstone System and the Precipitation Growth System.

PHASE I: Studies and experimental models

BUDGET PC. 4, PHASE I: 304.980 RON

PHASE PERIOD: 19.03.2018-31.12.2018

SPECIFIC OBJECTIVES:

Activity 1.16 Study on the requirements for new rocket propellants

Activity 1.17. Theoretical and experimental study on modern oxidants and fuel for rocket engines

Activity 1.18. Theoretical and experimental study of polymer binders with potential applications in the field of solid rocket fuels

SUMMARY

In Phase 1 of Component project 4, a database was developed from which can be easily extracted the types of precursor materials for the preparation of new solid rocket fuels. The technical specifications (minimum requirements) for potential oxidants and fuels were determined. An oxidant, i.e. NTO, has been synthesized using an original method that delivered higher yields compared to the reported studies. In parallel, with the patented methodology, 12 experiments were carried out. As a result three types of polyols were synthesized starting from recycled PET for their later use in the polyurethane structure of the solid rocket composite. Two polyurethane syntheses were performed with commercial polyols, considered evidence in the internal benchmarking study. Using only 2 polyol recipes, 3 experimental models of polyurethane were obtained, as follows: 1 composite obtained without vacuum and 2 obtained using vacuum and temperature. These proposed polyurethane models will be loaded in the next stage with the oxidant and the fuel components (simulants) for testing the binding and homogenization properties, in order to develop functional solid fuel models. Although there were no dissemination activities in Stage 1 of the Component 4 Project, basic results used in the Project were presented at two international conferences, in the form of an oral communication (1^st prize award) and a poster presentation. Moreover, a study using these methods for obtaining flexible fireproof composites has been sent for publication in an indexed ISI journal. Finally, an active link to Project 4 "RAKETCOMB" was constructed on the main website of SECURE-NET. The research team composed of (ATM, ICECHIM, CCSA-CBRNE and UPB) met the proposed objectives for Stage 1 of PC 4 RAKETCOMB with a total degree of achievement.

DISSEMINATION

Scientific Communications:

1. Coman Alina Elena, Gabor Raluca Augusta, Stoian Sergiu, Nicolae Andi, Raditioiu Valentin, Iordache Tanta Verona, Hubca Gheorghe, „The influence of fillers and flame retardant agents upon low-smoke and flame-retardant properties of PVC-based composites”– PRIOCHEM – XIV Ed, Bucharest, Romania, 10 - 12 October 2018, 1st prize awarded for the Best Oral Presentation.

2. Coman Alina Elena, Gabor Raluca Augusta, Raditioiu Valentin, Hubca Gheorghe, Mihailescu Mona‚Structural, optical and thermal properties of flexible Polyvinylchloride compounds’, The 6^th international colloquim ‚PHYSICS OF MATERIALS’ (PM6), Bucharest, Romania, 15-16 November 2018, Poster.

  Articles:

1. Coman Alina Elena, Gabor Raluca Augusta, Stoian Sergiu, Nicolae Andi, Raditioiu Valentin, Iordache Tanta Verona, Hubca Gheorghe, New formulations of flame-retardant flexible polyvinylchloride composites, Journal of Thermal Analysis and Calorimetry, Under Review.

Activ Link of Project 4 "RAKETCOMB", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro

PHASE II: Development of Functional Models and Technologies

BUDGET PC. 4, PHASE II: 321.300 RON

PHASE PERIOD: 01.01.2019-31.12.2019

SPECIFIC OBJECTIVES:

Activity 2.18 Synthesis, processing and evaluation the performance of oxidizing and fuel compounds / materials for solid rocket propellant of rocket engine

Activity 2.19 Synthesis, processing and characterization of intelligent binders for solid rocket propellant of rocket engine

Activity 2.20 Development of the laboratory technologies for obtaining the oxidizing and fuel compounds / materials and intelligent binders for solid rocket engine fuels

Activity 2.21 Determination of physical, explosive, performance and safety characteristics of the composite for solid rocket fuels.

Activity 2.22 Establishing the technical specifications and designing the functional model of the composite for the solid rocket propellant used for rocket engine.

Activity 2.23 Establishing and distribution of intellectual property rights

Activity 2.24 Dissemination of results

SUMMARY

Research on the synthesis of stabilized ammonium nitrate has allowed obtaining a cheap and efficient oxidant without crystalline form transitions at temperatures that can be reached in the environment. Laboratory technologies for obtaining polyols by PET degradation have been developed. Composite materials from polyols obtained from recycled PET were successfully obtained, which together with MDI form the binder of the composite material, and in combination with the fuel (aluminum powder) and the oxidant (stabilized ammonium nitrate) led to the development of propellants. Tests were performed regarding the properties of the new propellants synthesized by evaluating the performance characteristics (combustion speed, compression and tensile strength). The safety characteristics of the energetic composites were determined by differential thermal analysis (temperature sensitivity) and by friction stress with various pressing forces (friction sensitivity). Energetic composites have low temperature sensitivity and are not sensitive to friction. The samples containing TEGDN are much more homogeneous than the others, meaning a better compatibility of the materials; the material was much more compact before solidification as the binder incorporating the oxidant-fuel mixture was more efficient. Following the burning of the composites, the percentage of ash remaining was between 12-14%. In order to carry out the dissemination activities, the results obtained within the Project at two international conferences and two national events were presented, in the form of oral presentations or posters. In fact, a study using methods for the obtaining of flexible fireproof composites has been published in an indexed ISI journal. The research team composed of (ATM, ICECHIM, CCSA-CBRNE and UPB) met the proposed objectives for PHASE 2 of PC 4 RAKETCOMB with a total degree of achievement.

DISSEMINATION

Scientific Communications:

1. ‘6th Nano Today Conference (Nano Today 2019)’, Iunie 2019 in Lisabona, Portugalia, “New polyurethane formulations for rocket propellants based on polyols from recycled PET”, poster.

2. Workshop ‘Contingenta Hazardurilor CBRN si Imbunatatirea Mijloacelor de Securitate Nationala SECURE-NET’: Studii experimentale privind realizarea unor compozite polimerice destinate motoarelor rachet?’, Oral Communication.

3. The International Conference “Education And Reativity For A Knowledge Based Society”14-16 Noiembrie - Universitatea “Titu Maiorescu”, BUCURE?TI , Concerns on reducing the environmental impact of solid propellants; ISSN 2248-0064; ISBN 978-3-9503145 Oral Communication.

4. Conference Defence Technology Forum 2019 - “Vasil Levski” National Military University Artilery, Air Defense And Cis Faculty-Scumen, Bulgaria, 01-02.10.2019, Eco–Friendly Oxidizers: Minireview; ISSN 2367-7902, Oral Communication.

Articles:

1. New Formulations of Flame-retardant Flexible Polyvinylchloride Composites, Revista Materiale Plastice, COMAN Alina Elena, GABOR Raluca Augusta, STOIAN Sergiu, NICOLAE Andi, RADITIOIU Valentin, IORDACHE Tanta Verona, HUBCA Gheorghe, Materiale Plastice, nr.3, 2019.

Patent applications:

1. Lianti polimerici cu solubilitate selectiva pentru materiale compozite energetice “verzi” si procedeu pentru obtinerea acestora/ Polymer binders with selective solubility for "green" energy composite materials and process for obtaining them. Authors: Traian Rotariu, Elena Andreea Moldovan, Gabriela Toader, Tanta-Verona Iordache, Ana-Mihaela Gavrila, Anamaria Zaharia, Andrei Sarbu, Patent Claim A-00805/28.11.2019.

 2. Compozitii poliester-poliolice pentru poliuretani elastomeri, metoda de obtinere a acestora si materiale compozite pentru combustibili solizi de rachete incorporand respectivele compozitii poliester-poliolice/Polyester-polyol compositions for elastomeric polyurethanes, their method of obtaining and composite materials for solid rocket fuels incorporating the respective polyester-polyol compositions. Authors: Duldner Monica- Mirela, Coman Alina-Elena, Zaharia Anamaria, Iordache Tanta Verona, Sarbu Andrei, Rotariu Traian, Dirloman Florin-Marian, Hubca Gheorghe, Damian Celina Maria, Patent Claim A-00848/03.12.2019.

Activ Link of Project 4 "RAKETCOMB", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro

PHASE III: Development of Functional Models and Technologies

BUDGET PC. 4, PHASE III: 355.713 RON

PHASE PERIOD: 01.01.2020-31.12.2020

SPECIFIC OBJECTIVES:

Activity 3.17 Validation of the synthesis methodology and reproducibility of characteristics for the new polymer composite structure for solid rocket engine fuels

Achievement indicators: Recipes for the synthesis of validated precursors; Analysis bulletin;

Activity 3.18 Optimization of technologies for production of composite polymer for solid rocket engines fuel, Part 1

Performance indicators: Optimized composite preparation protocol;

Activity 3.19 Evaluation of the loading performance of composites and start of studies to determine the explosive characteristics, performance of solid rocket engines fuels by firing in manometric bombs or on the bench

Performance indicators: Protocol for loading the solid rocket engines fuels;

Activity 3.20 Determination of sensitivity and stability characteristics of solid rocket engine fuels

Achievement indicators: Technical specifications;

Activity 3.21 Elaboration of scientific papers

Achievement indicators: 3 ISI articles published

Activity 3.22 Dissemination of results

Achievement indicators: 3 scientific communications;

SUMMARY

In stage III/2020, the synthesis methodology and the reproducibility of the synthesized materials and their characteristics were validated, optimizing a technology for preparing the new solid fuel. Samples from the new solid fuel and a technology for loading intelligent polymer composites were also achived. Once the selection of the substances that will be used in the process of making the composite polymer mixture was completed, both production technologies of the materials that make up the composite and the compaction technology of the composite itself were developed. The technological process of making a solid polymeric composite fuel, which must be as simple as possible and allow series production, has been described. This stage encompasses the most complex activities, from the synthesis of the components to the arrangement of the mixture in the mold. In this respect, some basic steps were described as follows: admission of raw materials and establishing the necessary quantities; steps required to prepare the composite mixture and arrangement of the composite polymer mixture in the mold followed by polymerization to obtain composite bars that were subsequently tested by firing on manometric bombs. In the last stage, the chemical stability of the polymer composites was determined by the vacuum method, the temperature sensitivity of the polymer composites and the friction sensitivity of the polymer composite fuels. In order to carry out dissemination activities, the results obtained within the Project were presented at three international conferences in the form of oral or poster presentations. Furthermore, three papers have been published in ISI indexed journals. The research team composed of (ATM, ICECHIM, CCSA-CBRNE and UPB) met the objectives proposed for stage III of FP 4 RAKETCOMB with a total degree of achievement.

DISSEMINATION

            Published articles:

1. Daniela Pulpea, Traian Rotariu, Gabriela Toader, Gheorghe Bogdan Pulpea, Valentina Neculae, Mircea Teodorescu, Decontamination of radioactive hazardous materials by using novel biodegradable strippable coatings and new generation complexing agents Chemosphere, Volume 258, November 2020, 127227.
2. Alina Elena Coman, Augusta Raluca Gabor, Valentin Raditoiu, Cristian Andi Nicolae, Gheorghe Hubca, Mona Mihailescu, Sergiu Stoian, Tanta Verona IORDACHE, A Study For A Class Of Flame Retardant Systems Based On Thermal, Optical And Mechanical Analysis, U.P.B. Sci. Bull., Series A, Vol. 81, Iss. 4, 2019
3. Alina Elena Coman, Augusta Raluca Gabor, Cristian Andi Nicolae, Valentin Raditoiu,  Gheorghe Hubca, Tanta-Verona Iordache, The Influence of Plasticizer Nature and of Processing Mode Upon the Characteristics of Flexible Poly(vinyl chloride) Composites, 2020, MATERIALE PLASTICE, 56(4).

Scientific Communications:

1. Alina Elena Coman, Julien Peyrton, Luc Averous, Tanta Verona Iordache, Gheorghe Hubca, Andrei Sarbu, Augusta Raluca Gabor, Cristian Andi Nicolae, Synthesis of “green” polyurethanes starting from polyester polyols obtained from bio sourced polyols’, in cadrul conferin?ei ‘3rd European Chemistry Conference, ‘3rd European Chemistry Conference’, ECC-2020 Virtual, 12.10.2020. Oral communication.
2. 2.      Florin-Marian Dîrloman, Traian Rotariu, Tudor-Viorel ?ig?nescu, Andreea Elena Moldovan, Ovidiu George Iorga, Alina Elena Coman, Teodora Zecheru, Development of eco-friendly solid rocket propellant, a 23-a editie a conferintei internationale New Trends in Research of Energetic Materials, April 1–3, 2020, Pardubice, Czech Republic, proceeding ISBN 978-80-7560-286-2.
3. 3.      F.M. Dîrloman, T. Rotariu, T.V. ?ig?nescu, G. Toader, and T.V. Iordache, Phase stabilized ammonium nitrate for future green rocket propellants, 8th International Conference on Materials Science and Technologies – RoMat 2020, Bucharest, Romania, 26-27.11. 2020

Activ Link of Project 4 "RAKETCOMB", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro    

PHASE IV: Completion of Demonstration Studies

PARTNERS: IC ATM; P1 ICECHIM; P2 CCSA-CBRNE; P3 UPB;

TOTAL BUDGET PC. 4: 1.035.200 RON (according to the additional document)

PROJECT PERIOD: 19.03.2018-18.08.2021 (according to the additional document)

PHASE IV: Completion of Demonstration Studies

PHASE PERIOD: 01.01.2021-18.08.2021

BUDGET PC. 4, PHASE IV:  53.207 RON

SPECIFIC OBJECTIVES:

Activity 4.8 - Optimization of technologies for production of composite polymer for solid rocket engines fuel, Part 2

Achievement indicators: The appearance of the offer of research / technological services on erris.gov.ro; 1 scientific communication and 1 ISI article accepted for publication; Draft PhD thesis of PhD student Florin Dirloman, Military Technical Academy (proposed for presentation in 2021).

Activity 4.9 - Completion of studies to determine the explosive characteristics, performance of solid rocket engine fuels by firing in manometric bombs or on the bench.

Achievement indicators: Demonstrator of the performance of solid rocket engine fuels;

SUMMARY

            During this stage, reproducibility and optimization studies were successfully performed. Recycled PET polyols with reproducible characteristics were obtained, as well as polyol composite materials, which together with diisocyanates form the binder from the composite material and mixed with the fuel (aluminum powder) and the oxidant (stabilized ammonium nitrate) lead to propellants synthesis. Moreover, during this stage, laboratory technology was optimized to obtain PSAN (phase-stabilized ammonium nitrate), GAP (glycidylazidopolymer) and environmentally friendly solid rocket fuels. Studies performed by Scanning Electron Microscopy (SEM) and Micro Computer-Tomography (CT) have shown a proper morphology and a good dispersion of the composite, without cracks or other hidden defects. Compressive strength tests and dynamic mechanical analysis have allowed the mechanical characterization of composites and have shown that they have very good mechanical properties at usual ambient temperatures. The results of the tests for determining the performance characteristics are consistent with the objectives proposed in the project and may support the hypothesis that the performance of the new composites is comparable to that of homogeneous solid propellants based on nitrocellulose and nitroglycerin (double base), but lower than that of heterogeneous solid propellants based on ammonium and aluminum perchlorate. In addition to good performance, it is also observed that the new compositions have a low smoke emission which is another important advantage over the established compositions. The results obtained within the Project were disseminated through the research offer created on erris.gov.ro, a communication and an article accepted for publication. In fact, the Doctoral Thesis of PhD student Florin Dirloman, Military Technical Academy, is being drafted and is proposed for defense until the end of 2021.

The research team composed of (ATM, ICECHIM, CCSA-CBRNE and UPB) met the objectives proposed for stage IV of PC 4 RAKETCOMB with a total degree of achievement.

RESEARCH OFFER:

 „Subscale rocket propellant testing stand” https://eeris.eu/ ERIF-2000-000H-1369.

DISSEMINATION

Article accepted for publication:

1. Phase Stabilized Ammonium Nitrate For Future Green Rocket Propellants/ Scientific Bulletin of UPB Series B/ 2021/ F.M. Dîrloman, T. Rotariu, T.V. ?ig?nescu, G. Toader, T. Zecheru, T.V. Iordache.
2. The Doctoral Thesis entitled ‘Polymer composite materials for new generations of rocket fuels’ of PhD student Florin Dirloman is being drafted and is proposed for defense until the end of 2021. Coordinator: Prof. Viorel Tiganescu

Scientific communications:

1. Modern Technologies in Industrial Engineering - ModTech 2021, June 23-26, Eforie Nord, Romania, Computational fluid dynamics simulations for composite rocket propellant optimization, Florin-Marian Dirloman, Liviu-Cristian Matache, Tudor-Viorel Tiganescu, Traian Rotariu, Daniel Zvincu, Mihai-Ionut Ungureanu, Ovidiu Iorga, Paper 3077

Active Link of Project 4 "RAKETCOMB", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=enand

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro    

Component Project 5 "Passive systems for multi-spectral camouflage based on hybrid organic-inorganic chromogen-polymer structures MULTICAM"

PARTNERS: IC ICECHIM; P1 CCSA-CBRNE; P2 UPB; P3 ATM;

TOTAL BUDGET PC. 5: 965.000 RON

PROJECT PERIOD: 19.03.2018-18.08.2021 (according to the additional document)

The overall objective of the project is to achieve successive masking coatings on flexible (textile) or rigid supports (metal, composites), depending on the depth of electromagnetic radiation penetration (which is inversely proportional to its frequency) by: designing a model that provides visual protection by reducing differences with the environment in which it operates, contraction of the contrast to the background for infrared sensors, reducing the thermal print to the environmental limit for thermal sensors and absorbing microwaves in the case of radar detection. The current systems that ensure the camouflage in this field consist of organic and inorganic pigments and thereof mixtures dispersed in film-forming materials, together with fillers, specific for each type of backing and background (the main disadvantage being the limited range of nuances and profiles reflectance that can be obtained by film deposition on any type of support) Limited, bathtubs dyes, dispersion or reagent are used for dyeing the camouflage models, but exclusively on textiles. Therefore, it is intended to use some of these dyes by incorporating them into fillers or acromatic pigments to be used together with the actual (inorganic or organic) pigments to obtain camouflage filler materials that can be applied further on any type of support. For camouflage in snow-covered areas, it is necessary to achieve increased reflectivity in the UV field (350 nm). As a result, another innovative system based on hybrid materials obtained by incorporating optical bleaching agents into matrices transparent is also proposed for areas where the reflection obtained with white acromatic pigments is small.

PHASE I: Studies and experimental models

BUDGET PC. 5, PHASE I: 288.535 RON

PHASE PERIOD: 19.03.2018-31.12.2018

SPECIFIC OBJECTIVES:

Activity 1.19. Establishing the minimum requirements and specifications for the camouflage of equipment and military techniques according to the type of land and to the specific detection means

Activity 1.20. Tests for the evaluation of properties for chromogenic and auxiliary materials for camouflage from commercial sources and for the compatibility of chromogenic materials with inorganic substrates

Activity 1.21. The spectral design of chromogenic materials, the determination of the characteristics for the coating materials constituents and the reports between them, and the elaboration of the recipes

Activity 1.22. Communication of results

SUMMARY 

Based on the existing standards and documentation regarding the reflection / absorption / emission properties of environmental constituents, as well as the existing data on the influence of the disturbing factors (illumination, season, temperature, neighborhoods, etc.) on the behaviour of specific backgrounds (forest, desert, polar, air / water), the main characteristics that must be met by camouflage materials were elaborated, by determining the technical specifications. Experimental studies on the establishment of laboratory recipes for the preparation of camouflage coating materials focused on two main directions: 1. For textile fabrics - chromogenic materials were designed based on cationic dyes adsorbed on chromium substrates such as aluminosilicates; and 2. For metallic substrates - the research study aimed at finding appropriate formulations for obtaining water-based, green paints that comply with NATO standards. The communication of the results was done by participating in two international conferences, an indicator stipulated in the project implementation plan. In this respect, members of the working group, including the newly employed ICECHIM, presented the results in the form of poster-type communications at international conferences organized in Bucharest. An active link to Project 5 "MULTICAM" was built on the website of SECURE-NET and a new research service was developed and posted on the erris.gov.ro website. The research team composed of (ICECHIM, CCSA-CBRNE, ATM and UPB) met the proposed objectives for Stage 1 of PC 5 MULTICAM with a total degree of achievement. 

DISSEMINATION

Scientific Communications:

1. M. Raduly, A. Raditoiu, V. Raditoiu, V. Purcar, L. Wagner, C. Nicolae, „Optical Properties Of Some Textiles Dyed With Curcuminoid Hybrid Systems”, The International Symposium "Priorities Of Chemistry For A Sustainable Development" – Priochem XIVth Edition, Icechim - Bucharest – Romania October 10 - 12, 2018

2. G. Ispas, M. Raduly, A. Raditoiu, V. Raditoiu, V. Purcar, L. Wagner, R. Manea, C. A. Nicolae, “Hybrid Materials Based On Diketone Derivatives And Palygorskite With Luminescent Properties”, The 6-Th International Colloquium  “Physics Of Materials” (PM 6), 15-16 November 2018, Bucharest, Romania

Research Service Offer: 

In addition to the indicators provided for this stage, a research service offer was also accomplished, namely Testing camouflage properties by spectrometric methods (for the resulting service Spectrometry-assisted camouflage testing the link is: https://erris.gov.ro/FUNCTIONAL-DYES). 

Activ Link of Project 5 "MULTICAM", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro

PHASE II: Development of Functional Models and Technologies

BUDGET PC. 5, PHASE II: 303.975 RON

PHASE PERIOD: 01.01.2019-31.12.2019

SPECIFIC OBJECTIVES:

Activity 2.25. Evaluation of the component materials compatibility with the surface coating and developing of application tests on different types of surfaces. Evaluation of the limits of reflectance / emittance in the areas of interest and the resistance of the coatings

Activity 2.26. Elaborating the UV-VIS-NIR camouflage models specific to the types of support and background (operating environment) and evaluating their efficiency in relation to the reflectance models of the standard operating environment types.

Activity 2.27. Establishing the characteristics of the multispectral camouflage materials and coatings and elaborating the technical specifications.

Activity 2.28. Dissemination of results

SUMMARY

At this stage, two obtaining technologies for the materials used in screen printing of camouflage patterns on textile substrate, respectively for painting the fighting technique with water-soluble films were elaborated. The developed materials were analyzed from the point of view of the technical characteristics and of the application properties for the targeted field, according to the military and civil standards. Regarding the obtaining of the materials for textile printing, two methods have been developed: the adsorption of dyes mixed in an aqueous solution and the obtaining of colored materials for the fundamental colors and subsequent mixing of them in the printing paste. Protocols for the obtaining of camouflages for different types of media (textile and metal) and operating environments (snow, forest, water) were developed and characteristics and technical specifications for each case were elaborated, including the observations obtained from the training polygon. The communication of the results was attained by participating at two international conferences and two other national events, an indicator stipulated in the project implementation plan. For that purpose, members of the working group, including the newly employed ICECHIM, presented the results with Poster-type communications at international conferences organized in Bucharest. The research team composed of (ICECHIM, CCSA-CBRNE, ATM and UPB) met the proposed objectives for PHASE 2 of PC 5 MULTICAM with a total degree of achievement.

DISSEMINATION

Scientific Communications:

1. Hybrid colored materials with UV-Vis-NIR controlled reflectance for coating textile substrates, Georgiana Cornelia Ispas, Valentin Raditoiu, Alina Raditoiu, Florentina Monica Raduly, Violeta Purcar, Raluca Manea, Luminita Eugenia Wagner, Workshop exploratoriu NeXT Chem, ICECHIM, 6-7 may 2019, Bucharest-Romania

2. The effect of hybrid pigments on reflectance profile of printed cellulose fabrics in visible-near infrared spectral regions, Georgiana Cornelia Ispas, Valentin Raditoiu, Alina Raditoiu, Florentina Monica Raduly, Violeta Purcar, Raluca Manea, Luminita Eugenia Wagner, 21st Romanian International Conference on Chemistry and Chemical Engineering Constanta-Mamaia, ROMANIA – 4-7 september 2019

3. Coloured materials with controlled absorption and emission for military camouflage, Diana-Ioana Buliga, Aurelian Cristian Boscornea, Ioana Asofiei, Stefan Tomas, Cristina Pop, 21st Romanian International Conference on Chemistry and Chemical Engineering Constanta-Mamaia, ROMANIA - 4-7 september 2019

4. Colored coating materials with spectrally selective reflectance for woodland camouflage textile fabrics, Georgiana Cornelia Ispas, Valentin Raditoiu, Alina Raditoiu, Florentina Monica Raduly, Violeta Purcar, Raluca Manea, Luminita Eugenia Wagner, The International Symposium "Priorities of Chemistry for a Sustainable Development" – PRIOCHEM XV-th Edition, ICECHIM - Bucuresti – ROMANIA, 30.10- 1.11.2019

5. Workshop ‘Contingenta Hazardurilor CBRN si Imbunatatirea Mijloacelor de Securitate Nationala SECURE-NET’: Materiale colorante filmogene cu proprietati spectrale UV-Vis-NIR adaptate pentru camuflajul echipamentului individual si al tehnicii militare, Valentin Raditoiu, Cristian Boscornea, Cristiana Epure, Traian Rotariu, Oral Communication.

Published articles or sent for publication:

1. Monica Florentina Raduly, Alina Raditoiu, Valentin Raditoiu, Luminita Wagner, Violeta Purcar, Georgiana Cornelia Ispas, Raluca Manea, Cristian-Andi Nicolae, “Synthesis and characterization of some hybrid materials based on curcumin derivatives embedded in modified palygorskite”, U.P.B. Sci. Bull., Series B, Vol. 81, Iss. 3, 2019, 87-96.

2. Diana-Ioana Buliga, Aurelian Cristian Boscornea, Ioana Asofiei, Stefan Tomas, Cristina Pop, Aurel Diacon ”Coloured materials with controlled absorption and emission for military camouflage”, Dyes and Pigments (ISSN: 0143-7208, FI = 4,018) – Sent for publication

Activ Link of Project 5 "MULTICAM", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro

PHASE III: Development of Functional Models and Technologies

BUDGET PC. 5, PHASE III: 334.795 RON

PHASE PERIOD: 01.01.2020-31.12.2020

SPECIFIC OBJECTIVES:

Activity 3.23. Realization of MIR-FIR-MW camouflage models and experimentation of laboratory technologies for multispectral camouflage systems - Part 1.

Achievement indicators: Multilayer coated fabric model;

Activity 3.24. Evaluation of detection time and distance for each type of support/camouflage material depending on the background and analysis of the degree of utility in military applications - Part 1.

Achievement indicators: Analysis bulletin

Activity 3.25. Establishment of industrial property rights.

Achievement indicators: 1 Patent application.

Activity 3.26. Elaboration of scientific papers.

Achievement indicators: 2 ISI articles published

Activity 3.27. Act 3.27 - Communication of Results.

Achievement indicators: 1 Scientific communications; Dissertation - DISPERSED COATING SYSTEMS, DERMATOLOGICAL USE, FOR MILITARY CAMOUFLAGE- Georgiana Cornelia Ispas, UPB

SUMMARY

In this stage of the project, the technology of obtaining textile materials for multispectral camouflage by screen printing on textile substrate was optimized by reducing the differences in relation to the elements of the environment in which it operates in the visible field, attenuating the contrast against the background in infrared and reducing thermal footprint near the boundary of the environment. The developed materials were analyzed from the point of view of the technical characteristics and of the application properties for the targeted field, according to the military and civil standards. Protocols for evaluating the time and distance of detection were developed based on the observations obtained in the training polygon, for the "forest" model with five colors in the visible, near infrared field and in the thermal footprint area, the model within the limits accepted by military regulations. It can be appreciated that the use of conductive polymers in the composition of textile inks and camouflage paints can substantially increase their effectiveness in the near, medium and far infrared. Future studies from stage IV/2021 will also verify the impact of these materials in terms of radar waves and the possibility of using such materials in this field. According to the most efficient individual detection methods, 90% of the targets are detected in a maximum of 3 seconds for visible images, respectively 80% of the targets in 5 seconds for wide-field thermal imaging. The detection in case of using the sea in a narrow field, the same performances are obtained in about 10 seconds in both cases. Based on the results obtained from the optimization of the technology, a patent application was filed at OSIM. The dissemination of the results was achieved by participating in international conferences and the public presentation of a dissertation, respectively the publication of two ISI articles. The research team composed of ICECHIM, CCSA-CBRNE, ATM and UPB met the objectives proposed for stage III of FP 5 MULTICAM with a total degree of achievement.

DISSEMINATION

IPR – Application patent

1. PROCEDEU DE OBTINERE A UNOR TESATURI TEXTILE IMPRIMATE PENTRU CAMUFLAJ MULTISPECTRAL/ PROCESS FOR OBTAINING PRINTED TEXTILE FABRICS FOR MULTISPECTRAL CAMOUFLAGE, Raditoiu Valentin, Raditoiu Alina, Raduly Monica Florentina, Wagner Luminita Eugenia, Ispas Georgiana Cornelia, Purcar Violeta, Manea Raluca, OSIM 2020 00794 / 27.11.2020

Published articles:

1)      Ioana Asofiei, Aurelian Cristian Boscornea, Diana-Ioana Buliga, Aurel Diacon, Stefan Theodor Tomas, Cristina Viorica Pop, Mixture design experiments applied for the formulation of a textile ink with reproduction of the NATO IRR green color used in military camouflage, Textile Research Journal. July 2020 https://doi.org/10.1177/0040517520938152

2)      Cristiana Epure, Teodora Zecheru, Gabriel Epure, Claudiu Lazaroaie, Ovidiu Iorga, Razvan Petre, Gabriela Nita, Mihail Munteanu, Dan Stoica, Albert Plosnita, Valentin Raditoiu, Composite materials for passive antiradar camouflage, Mater. Plast., 2020, Volume 57, Issue 2, https://doi.org/10.37358/MP.20.2.5346

Scientific Communications:

1)      Georgiana Cornelia ISPAS, Sisteme disperse de acoperire, de uz dermatologic, pentru camuflaj militar , Universitatea POLITEHNICA din Bucuresti - Sesiunea de Comunicari Stiintifice Studentesti 2020 (https://upb.ro/wp-content/uploads/2020/03/SCSS-2020-CASM.pdf)

2)      Lucrare de dizertatie - Sisteme disperse de acoperire, de uz dermatologic, pentru camuflaj militar, Georgiana Cornelia ISPAS, anul II Master Produse Farmaceutice si Cosmetice, Facultatea de Chimie Aplicata si Stiinta Materialelor Conducatori stiintifici: Conf.dr.ing. Alina SIMION, Departamentul Chimie Organica „Costin Nenitescu”, C.S.I.Dr.ing. Valentin RADITOIU, Institutul National de Cercetare-Dezvoltare pentru Chimie si Petrochimie-ICECHIM

Activ Link of Project 5 "MULTICAM", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro

PHASE IV: Completion of Demonstration Studies

PARTNERS: IC ICECHIM; P1 CCSA-CBRNE; P2 UPB; P3 ATM;

TOTAL BUDGET PC. 5: 971.600 RON (according to the additional document)

PROJECT PERIOD: 19.03.2018-18.08.2021 (according to the additional document)

PHASE IV: Completion of Demonstration Studies

PHASE PERIOD: 01.01.2021-18.08.2021

BUDGET PC. 5, PHASE IV:  44.295 RON

SPECIFIC OBJECTIVES:

Activity 4.10 - Realization of MIR-FIR-MW camouflage models and experimentation of laboratory technologies for multispectral camouflage systems - Part 2

            Achievement indicators: Technical data sheet; 1 scientific communication

Activity 4.11 - Evaluation of detection time and distance for each type of support/camouflage material depending on the background and analysis of the degree of utility in military applications - Part 2

Achievement indicators: Utility study; 1 ISI article in evaluation.

SUMMARY

In the final stage of the project, the technology of obtaining textile materials for multispectral camouflage by screen printing on textile substrate was experienced. Camouflage in the visible field of the spectrum consists in diminishing the differences in relation to the elements of the environment in which it operates, attenuating the contrast with the background in the infrared field and reducing the thermal footprint near the limit of the environment. For the "forest" type camouflage, the reflectance limits imposed for achieving the lowest possible contrast with a landscape of this type, characteristic of the region in which our country is located, have been established. The five-color model falls within the limits accepted by NATO military regulations, for which the Technical Data Sheet is prepared. The properties of these materials were also verified in terms of radar waves and the possibility of using such materials in this field, in this sense being determined an attenuation of the radar signal which largely depends on the number of layers and the thickness of the coatings used. According to the utility study, the detection methods using computerized analysis of the obtained images lead to the detection of 90% of the targets camouflaged in static landscape reduced in 5 seconds for visible images, and 80% respectively of the targets in 8 seconds for thermal imaging images with large field. The results show an increase in camouflage efficiency of about 65% in the first case and 60% in the second, compared to the classic camouflage currently used. In this stage, the results were disseminated during a conference and through an article sent for publication, which is being evaluated.

The research team composed of ICECHIM, CCSA-CBRNE, ATM and UPB met the objectives proposed for stage IV of PC 5 MULTICAM with a total degree of achievement.

DISSEMINATION

Article in evaluation:

1. Organic coating with low IR emission, 2021, Revista Materiale plastice, in evaluation, Cristiana Epure, Viorel ?ig?nescu, Teodora Zecheru, Gabriel Epure, Ovidiu Iorga, Andrei ?chiopu, Mihail Munteanu, Alexandru Marin, Raluca Ginghin?, Daniel ?urcanu, Cornel Todiric?

Scientific communication:

1. NeXT-Chem „INNOVATIVE CROSS-SECTORAL TECHNOLOGIES”, third edition/ Workshop/, Diana-Ioana BULIGA, Aurelian Cristian BOSCORNEA, Ioana POPA, Ana-Maria DRAGHICI-POPA, Ioan CALINESCU - PHYCOCYANIN – A POSSIBLE SOLUTION FOR NATURAL BLUE PIGMENTS, 27-28 May 2021, Bucharest, Romania

Active Link of Project 5 "MULTICAM", on the SECURE-NET website

in English http://icechim-rezultate.ro/proiect.php?id=33&lang=en and

in Romanian http://icechim-rezultate.ro/proiect.php?id=40&lang=ro.