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Method for synthesizing block HTPE copolymer

A copolymer and block type technology, applied in the direction of adhesive types, polyether adhesives, adhesives, etc., to achieve the effect of low temperature, simple and easy method, and easy engineering enlargement

Active Publication Date: 2013-07-17
HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Pure BuNENA plasticizer will crystallize at -8°C, but no low-temperature embrittlement has been found in HTPE propellants added with BuNENA plasticizer

Method used

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  • Method for synthesizing block HTPE copolymer
  • Method for synthesizing block HTPE copolymer
  • Method for synthesizing block HTPE copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Add 200g (0.3mol) of PTMEG650 and 120g (0.3mol) ) of PEG400, blow nitrogen and stir, keep the nitrogen flow at 0.1Mpa, stir for 1 hour, add dropwise a mixture of 5g (0.05mol) of concentrated sulfuric acid with a concentration of 96% and 10g of tetrahydrofuran, after the addition, the reaction temperature is raised to 110°C, and divided Moisture begins to appear in the water tank, raise the temperature to 135°C for 4 hours, continue to maintain nitrogen protection, collect 35ml of tetrahydrofuran fraction in the water separator, slowly add 300ml of distilled water as a chain terminator to quench the reaction, and keep the hydrolysis reaction at 100°C until the water is separated After 50ml of water was collected by the device, the reaction was stopped.

[0037] (2) Add water 1 to 10 times the volume of the metered distillate in step (1) as a chain terminator, hydrolyze at 100°C, and the reaction is quenched;

[0038] Pour the reaction solution into a 500ml beaker, a...

Embodiment 2

[0051] Add 200g (0.3mol) of PTMEG650 and 120g (0.3mol) of PEG400 into a 1000ml four-necked round-bottomed reaction flask equipped with a reflux condenser (with bubbler, water separator), stirrer, thermometer, and airway , pass nitrogen and stir, keep the nitrogen flow at 0.1Mpa, after stirring for 1h, add dropwise a mixture of 5g (0.05mol) concentrated sulfuric acid with a concentration of 96% and 14.2g distilled water, after the addition, the reaction temperature rises to 115°C, and continue to maintain nitrogen Protection, there is moisture in the water separator, raise the temperature to 135°C for 4 hours, collect 30ml of tetrahydrofuran fraction in the water separator, slowly add 300ml of distilled water dropwise to quench the reaction, keep the hydrolysis reaction at 100°C, until the water separator collects 50ml of water, Stop responding.

[0052] Pour the reaction solution into a 500ml beaker, add 3.6gCa(OH) 2 After fully stirring, add 300ml tetrahydrofuran (anhydrous)...

Embodiment 3

[0057] Add 200g (0.3mol) of PTMEG650 and 60g (0.3mol) of PEG200 into a 1000ml four-necked round-bottomed reaction flask equipped with a DC condenser (equipped with a vacuum tailpiece and a receiving bottle), a stirrer, a thermometer, and an airway, After stirring for 1 hour, add 5 g (0.05 mol) of a mixture of concentrated sulfuric acid with a concentration of 96% and 10 g of tetrahydrofuran dropwise. After the addition, stop the nitrogen flow. The reaction pressure is reduced to 10 mmHg and the temperature is raised to 120 ° C. React for 3 hours. Collect water and 30ml of tetrahydrofuran fraction in the receiving bottle; after enough fractions are collected, stop the decompression, protect with nitrogen, slowly add 300ml of distilled water dropwise to quench the reaction, and keep the hydrolysis reaction at 100°C until the water separator collects 50ml of water, then stop the reaction.

[0058] Pour the reaction solution into a 500ml beaker, add 3.6gCa(OH) 2 After fully stirri...

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Abstract

The invention provides a method for synthesizing a block HTPE copolymer. Polytetrahydrofuran and polyol are adopted as raw materials, the main chain of polytetrahydrofuran cracks at 90-150DEG C to obtain tetrahydrofuran monomers, and a coupling reaction of obtained tertiary oxonium ions and terminal hydroxyl groups of polyol is rapidly carried out to obtain the block HTPE copolymer. Compared with the prior art, the method provided by the invention allows the structure and performances of the block HTPE copolymer synthesized through a copolymerization technology to be controlled through experiment designs, and the main chain structure and the molecular weight distribution of a target polymer to be controlled and changed in advance, enables the polytetrahydrofuran and polyethylene glycol block copolymer having a number-average molecular weight of about 3000 to be synthesized under the protection of a nitrogen flow through a simple synthetic reaction apparatus without pressure reduction, and has the advantages of simplicity of the required synthetic apparatus, simple and easily implemented post-treatment method, and easy realization of the engineered amplification of the synthetic technology.

Description

technical field [0001] The present invention relates to the synthesis technology of block copolymer hydroxyl-terminated polyether (English writing: the hydroxyl-terminated polyether, English abbreviation is HTPE). The copolymers synthesized by this method are mainly used as binders for solid propellants. Background technique [0002] With the large-scale application of high-tech in war, the role of missile weapons in war is becoming more and more important, which requires that the propellant can greatly increase the energy; however, with the increase of propellant energy, its manufacturing, storage, transportation and The danger during use also increases accordingly. For this reason, extensive and in-depth research on insensitive solid propellants has been carried out at home and abroad in recent years, and great progress has been made. New insensitive propellants such as HTPB, NEPE, HTPE, and XLDB have been developed. [0003] Hydroxy-terminated polyether prepolymer (HTP...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/34C09J171/08
Inventor 哈恒欣黄浩南朱朝阳王素芳孙忠祥王宏志张素敏
Owner HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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