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Preparation method of anti-atomic oxygen polyimide hybrid films containing octamer cage-shaped silsesquioxane structures

An anti-atomic polyimide and silsesquioxane technology, applied in the direction of silicon organic compounds, can solve the problems of inconvenient operation, high cost, cumbersome synthesis steps, etc., and achieve low cost, outstanding heat resistance, and advanced technology. simple effect

Inactive Publication Date: 2015-02-18
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, unfortunately, the bisamine-based POSS used in this research is prepared by a multi-step chemical synthesis method. The synthesis steps are cumbersome, the operation is inconvenient, and the cost of the monomers used in the synthesis is relatively high. Therefore, the production of POSS polyimide is difficult for industrialization. It's a tricky subject

Method used

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  • Preparation method of anti-atomic oxygen polyimide hybrid films containing octamer cage-shaped silsesquioxane structures
  • Preparation method of anti-atomic oxygen polyimide hybrid films containing octamer cage-shaped silsesquioxane structures
  • Preparation method of anti-atomic oxygen polyimide hybrid films containing octamer cage-shaped silsesquioxane structures

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Experimental program
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Effect test

Embodiment 1

[0052] (1) Synthesis of diamine octapolycage silsesquioxane (diamine POSS)

[0053] Add 50mL tetrahydrofuran, 4mL distilled water, 9.26mL APSM, 30.74mL PTMS and 1mL benzyltrimethylammonium hydroxide (20wt% methanol solution) successively into a reaction vessel equipped with a magnetic stirrer and a thermometer, stir for 2 to 5 minutes, and keep The temperature of the system was kept at 25° C., and the reaction was carried out for 4 days. Then the temperature of the system was raised to 50° C., and the reaction was refluxed for 2 days under magnetic stirring. After the end, it was cooled in a low-temperature environment of -10°C for 24 hours, and a white crude product was precipitated, which was filtered to obtain a white crude product D. Product D was washed twice with 30 mL of acetonitrile / diethyl ether mixture at 0°C (the volume ratio of acetonitrile and diethyl ether was 3:2) to obtain product E. Product E was dissolved in 30 mL of DMAc, then precipitated with 200 mL of d...

Embodiment 2

[0057] (1) Synthesis of diamine octapolycage silsesquioxane (diamine POSS)

[0058] Add 50mL tetrahydrofuran, 5mL distilled water, 9.39mL APSE, 30.61mL PTES and 1.5mL tetraethylammonium hydroxide (25wt% methanol solution) to the reaction vessel equipped with magnetic stirring and thermometer, and stir for 2-5 minutes to maintain the system The temperature was 25°C, and the reaction was carried out for 5 days. Then the temperature of the system was raised to 60° C., and the reaction was refluxed for 3 days under magnetic stirring. After the end, it was cooled in a low-temperature environment of -10°C for 24 hours, and a white crude product was precipitated, which was filtered to obtain a white crude product D. Product D was washed twice with 40 mL of acetonitrile / diethyl ether mixture at 0°C (the volume ratio of acetonitrile and diethyl ether was 3:1) to obtain product E. Product E was dissolved in 20 mL of DMAc, then precipitated with 200 mL of distilled water and filtered. ...

Embodiment 3

[0062] (1) Synthesis of diamine octapolycage silsesquioxane (diamine POSS)

[0063] Add 50mL tetrahydrofuran, 4mL distilled water, 13.72mL ABSM, 26.28mL MTMS and 0.5mL tetramethylammonium hydroxide (20wt% aqueous solution) successively into the reaction vessel equipped with magnetic stirring and thermometer, stir for 2-5 minutes, and maintain the temperature of the system At 25°C, react for 3 days. Then the temperature of the system was raised to 60° C., and the reaction was refluxed for 2 days under magnetic stirring. After the end, it was cooled in a low-temperature environment of -10°C for 24 hours, and a white crude product was precipitated, which was filtered to obtain a white crude product D. Product D was washed twice with 50 mL of acetonitrile / diethyl ether mixture at 0°C (the volume ratio of acetonitrile and diethyl ether was 3:2) to obtain product E. Product E was dissolved in 20 mL of DMAc, then precipitated with 200 mL of distilled water and filtered. This opera...

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Abstract

The invention relates to a preparation method of anti-atomic oxygen polyimide hybrid films containing octamer cage-shaped silsesquioxane structures. In order to obtain a POSS polyimide hybrid film with excellent anti-atomic oxygen (AO) performance with low cost and keep the thermal performance and the mechanical performance of the polyimide, the preparation method adopts tetrahydrofuran as a solvent and alkali as a catalyst to synthesize tetrahydrofuran-diamine POSS containing two active amino groups by adopting a hydrolysis co-condensation method which is simple to operate, low in cost and gentle in reaction condition; and introducing the diamine POSS into a polyimide molecular main chain by adopting a co-condensation method to finally obtain the POSS polyimide hybrid films with excellent anti-AO performances. The preparation method disclosed by the invention is gentle in conditions of a reaction process, low in cost, simple in process, capable of greatly lowering the production cost and beneficial to realizing industrial production.

Description

technical field [0001] The invention relates to the preparation of diamine-based octapolycage silsesquioxane (diamine POSS) and a preparation method of an anti-atomic oxygen polyimide hybrid film containing a POSS structure. Background technique [0002] Low Earth Orbit (LEO) is the main operating area for Earth observation satellites, meteorological satellites, space stations and other spacecraft. The LEO environment is extremely harsh, and there are mainly space factors such as atomic oxygen (Atomic Oxygen, AO), meteorites, space debris, ultraviolet radiation, and cold and heat cycles. Among these factors, the steric effect of AO is the most significant, second only to the strong oxidizing properties of fluorine on the physical and chemical erosion of the surface materials of low-orbit vehicles. Micrometeorites, space debris, etc. are much more serious. Polyimide has become an important class of materials in the aerospace field due to its excellent thermal properties, me...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08L79/08C08K5/549C08G73/10C07F7/21
Inventor 张秋禹雷星锋乔明涛田力冬
Owner NORTHWESTERN POLYTECHNICAL UNIV
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