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## Study of synthesis carboxyl-terminated polybutadiene

### Patrycja Kamila Piecyk

#### Abstract

Polymers, the termination of which can be further modified, are used in many technologies of copolymer synthesis, thermoplastic elastomers and others. Polybutadiene terminated with hydroxyl groups (HTPB) has many chemical and physical properties that allow its use in the armaments and civilian industry. HTPB is used in rocket and rocket technology as a phlegmatizer for explosives, but is most often used as a binder of heterogeneous solid rocket fuels [1]. Another material used for this purpose is CTPB, carboxyl-terminated polybutadiene [2]. CTPB can be obtained by the synthesis of HTPB with anhydride, in which maleic anhydride is most commonly used. The reaction is carried out at 80 °C for 24 hours under a nitrogen atmosphere [2]. Methods of CTPB production by means of other reactions (often polymerization) require more substrates and complicated procedures. Due to the fact that the conditions of this process are quite easy to maintain, it is worth optimizing the synthesis of CTPB with other anhydrides. The purpose of the presented work is to investigate CTPB synthesis and optimize this process. In this work, HTPB reacts with glutaric or hexahydrophthalic anhydride to form CTPB under argon for 24 hours. The process temperature was 50, 70 or 90 ° C. These reactions were not described in the literature, and the assumption was to determine the most favorable temperature for a given anhydride, the best molar ratio of hydroxyl groups to moles of anhydride and the choice of the optimal time to carry out the process. 18 samples were obtained, 9 from glutaric anhydride and 9 from hexahydrophthalic anhydride (4 samples at 70 and 90° C and one at 50 °C). The CTPB characteristics were based on the FTIR and 1HNMR methods, the COOH values was determined by titration and the viscosity of the resulting polymer was tested. The analysis showed that the most preferred ratio of OH groups to moles of anhydride is 1:1. For lower, product has a lower content of carboxylic groups and was a mixture of HTPB and CTPB. The temperature which was the best for both anhydrides was the highest in the conducted work, i.e. 90 °C. The polymers obtained at the lower temperature showed a lower COOH value and the carbonyl band was less intense. Due to the described synthesis of HTPB with maleic anhydride, the synthesis was carried out for 24 hours, however, the sample was taken after 4 hours to compare it with the final product. After analysis of FTIR, 1HNMR and the COOH value, it turned out that the reaction can be completed after only 4 hours without significant effect on the polymer properties.
Diploma type
Engineer's / Bachelor of Science
Diploma type
Engineer's thesis
Author
Patrycja Kamila Piecyk (FC) Patrycja Kamila Piecyk,, Faculty of Chemistry (FC)
Title in Polish
Supervisor
Michał Chmielarek (FC/DH-EM) Michał Chmielarek,, Department Of High-Energetic Materials (FC/DH-EM)Faculty of Chemistry (FC)
Certifying unit
Faculty of Chemistry (FC)
Affiliation unit
Department Of High-Energetic Materials (FC/DH-EM)
Study subject / specialization
, Technologia Chemiczna
Language
(pl) Polish
Status
Finished
Defense Date
31-01-2019
Issue date (year)
2019
Reviewers
Michał Chmielarek (FC/DH-EM) Michał Chmielarek,, Department Of High-Energetic Materials (FC/DH-EM)Faculty of Chemistry (FC) Krzysztof Krawczyk (FC/CChT) Krzysztof Krawczyk,, Chair of Chemical Technology (FC/CChT)Faculty of Chemistry (FC)
Keywords in Polish
Keywords in English
Abstract in Polish
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praca_inż-Piecyk_Patrycja-278441.pdf
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Identyfikator pracy APD: 30170

Uniform Resource Identifier
https://repo.pw.edu.pl/info/bachelor/WUTdd703484b141427b824bafd55f30bac1/
URN
urn:pw-repo:WUTdd703484b141427b824bafd55f30bac1

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