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Six-arm type hydroxyl-terminated glycidyl azide polymer preparation method

A technology of glycidyl ether and terminal hydroxyl group, which is applied in the field of organic chemical synthesis, can solve the problem of few types of multi-arm type ester-terminated polyazido glycidyl ethers, etc., and achieves good thermal stability and improves the effect of thermal stability.

Inactive Publication Date: 2016-02-03
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the problem of fewer types of existing multi-arm type ester-terminated polyazide glycidyl ethers, and provide a six-arm type hydroxyl-terminated polyazide glycidyl ether preparation method

Method used

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  • Six-arm type hydroxyl-terminated glycidyl azide polymer preparation method

Examples

Experimental program
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Embodiment 1

[0022] Add sorbitol and catalyst to the solvent dichloromethane, stir, keep a constant temperature of 30°C, add epichlorohydrin dropwise, and react for 3 hours after the dropwise addition to obtain a polyepichlorohydrin solution; the mixture of sorbitol and epichlorohydrin The molar ratio is 1:90; the mass fraction of the catalyst is 2.5% of the total mass of sorbitol and epichlorohydrin.

[0023] Wash the polyepichlorohydrin solution with deionized water, discard the upper aqueous solution, and distill the organic matter in the lower layer under reduced pressure to obtain six-arm polyepichlorohydrin; under nitrogen protection, at a temperature of 120 ° C, the six-arm polyepoxychlorohydrin Propane and sodium azide were synthesized in N,N-dimethylformamide solvent for 12 hours, and the molar ratio of polyepichlorohydrin to sodium azide was 1:1.1; polyepichlorohydrin was based on theoretical epichlorohydrin Mole count. After the reaction, most of the N,N-dimethylformamide solve...

Embodiment 2

[0033]Add sorbitol and the catalyst into the solvent dichloromethane, stir, and keep a constant temperature of 30°C; add epichlorohydrin dropwise, and react for 3 hours after the dropwise addition to obtain polyepichlorohydrin solution B. The molar ratio of sorbitol and epichlorohydrin is 1:60, and the mass fraction of the catalyst is 2.5% of the total mass of sorbitol and epichlorohydrin.

[0034] Wash the polyepichlorohydrin solution with deionized water, discard the upper aqueous solution, and distill the organic matter in the lower layer under reduced pressure to obtain six-arm polyepichlorohydrin; Propane and sodium azide were synthesized in N,N-dimethylformamide solvent for 16 hours, and the molar ratio of polyepichlorohydrin to sodium azide was 1:1.1; polyepichlorohydrin was based on theoretical epichlorohydrin In terms of moles, after the reaction, most of the N,N-dimethylformamide solvent was evaporated under reduced pressure at 50°C, then washed with deionized water,...

Embodiment 3

[0038] Add sorbitol and catalyst to the solvent dichloromethane, stir, keep a constant temperature of 30°C, add epichlorohydrin dropwise, and react for 3 hours after the dropwise addition to obtain a polyepichlorohydrin solution; the mixture of sorbitol and epichlorohydrin The molar ratio is 1:48, and the mass fraction of the catalyst is 2.5% of the total mass of sorbitol and epichlorohydrin.

[0039] Wash the polyepichlorohydrin solution with deionized water, discard the upper aqueous solution, and distill the organic matter in the lower layer under reduced pressure to obtain six-arm polyepichlorohydrin; Propane and sodium azide were synthesized in N,N-dimethylformamide solvent for 12 hours, and the molar ratio of polyepichlorohydrin to sodium azide was 1:1.0; polyepichlorohydrin was based on theoretical epichlorohydrin In terms of moles, after the reaction, most of the N,N-dimethylformamide solvent was evaporated under reduced pressure at 50°C, then washed with deionized wat...

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Abstract

The present invention relates to an energy-containing plasticizer preparation method, specifically to a six-arm type glycidyl azide polymer preparation method, wherein sorbitol and epichlorohydrin are subjected to a cationic polymerization reaction to synthesize six-arm type poly epichlorohydrin, and under the protection of nitrogen gas, sodium azide and the poly epichlorohydrin are subjected to a substitution reaction so as to synthesize the six-arm type hydroxyl-terminated glycidyl azide polymer. According to the present invention, the initial decomposition temperature is 227.3 DEG C, the azido strong heat release absorption peak appears at the thermal decomposition temperature of 255.7 DEG C, and the 2459 J / g energy is provided; compared with the commonly used energetic plasticizer nitroglycerin, the material of the present invention has good thermal stability, and can significantly improve the thermal stability of the system of the energetic material when being adopted as the plasticizer; and the low molecular weight six-arm type hydroxyl-terminated glycidyl azide polymer can be adopted as the chain extender and the reaction raw material for preparation of the branched glycidyl azide polyurethane.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and relates to a preparation method of an energetic plasticizer, in particular to a preparation method of a six-arm type hydroxyl-terminated polyazide glycidyl ether. Background technique [0002] Glycidyl polyazide (GAP) is an energetic binder with excellent performance, which is used in rocket propellants, pyrotechnics and high-energy aggregate bonded explosives (PBX), which can improve its energy release characteristics. Due to the high viscosity and rigid molecular chain of linear GAP, its process and low temperature mechanical properties are not good. Most of the GAP used at present is a mixture of low viscosity and high viscosity, so the structure of GAP needs to be improved. [0003] The synthesis of branched GAP (B-GAP) and multi-armed GAP is an important aspect of its structure improvement. At the same molecular weight, the viscosity of B-GAP decreases significantly, and its d...

Claims

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Application Information

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IPC IPC(8): C08G65/325C08G65/28C08G18/50
Inventor 王树民舒远杰吴卫东
Owner SOUTHWEAT UNIV OF SCI & TECH
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