Epoxy-terminated polyether compound as well as preparation method and application thereof

A technology of epoxy-terminated polyether and polyether compounds, which is applied in the field of epoxy-terminated polyether compounds and their preparation, can solve problems such as large safety risks, and achieve the effects of short curing time, high purity and low curing temperature

Active Publication Date: 2017-07-18
HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Li Na et al. have prepared epoxy-terminated polybutadiene. The method is to use boron trifluoride ether as a catalyst, and epichlorohydrin undergoes cationic ring-opening polymerization to form a polyether intermediate with chlorinated polyether at both ends. After the intermediate is released, the ring is closed under alkaline conditions to form epoxy-terminated polybutadiene. This method needs to use boron trifluoride ether as a catalyst and needs to be re-distilled before use. Distilling boron trifluoride ether has a large At the same time, under alkaline conditions, while the elimination ring closure reaction of halogenated hydrocarbons occurs, the nucleophilic substitution reaction of hydroxide to chlorine is prone to occur, so that a small amount of hydroxyl is introduced into the product

Method used

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  • Epoxy-terminated polyether compound as well as preparation method and application thereof
  • Epoxy-terminated polyether compound as well as preparation method and application thereof
  • Epoxy-terminated polyether compound as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The epoxy-terminated polyoxyethylene ether of synthetic PEG-6000, concrete method is as follows:

[0030] A 2000 mL four-necked flask was equipped with a mechanical stirrer, a condenser and a thermometer, and 600 g (0.10 mol) of polyethylene glycol (PEG-6000) and 800 mL of dichloromethane were added to the four-necked flask. Add 6.00g of sodium hydride (0.25mol) in batches, control the reaction temperature at 0-10°C, slowly add 23.2g (0.25mol) of epichlorohydrin dropwise, raise the temperature to 40°C and reflux for 4h after the addition, remove the solid by filtration, and wash the filtrate with water To neutrality, dry with anhydrous magnesium sulfate, and remove the dichloromethane solvent by rotary evaporation to obtain 504.2 g of epoxy-terminated polyether of PEG-6000 with a yield of 82.5%.

[0031] The epoxy-terminated polyether of PEG-6000 is used as a binder to prepare a solid propellant, and the specific method is as follows:

[0032] Add 25g PEG-6000 epoxy-te...

Embodiment 2

[0037] The epoxy-terminated polyoxyethylene ether of synthetic PEG-10200, specific method is as follows:

[0038] A 2000 mL four-necked flask was equipped with a mechanical stirrer, a condenser and a thermometer, and 510 g (0.05 mol) of polyethylene glycol (PEG-10200) and 800 mL of dichloromethane were added to the four-necked flask. Add 3.10g of sodium hydride (0.13mol) in batches, control the reaction temperature at 0-10°C, slowly add 12.1g (0.13mol) of epichlorohydrin dropwise, raise the temperature to 40°C and reflux for 4h after the addition, remove the solid by filtration, and wash the filtrate with water To neutrality, dry with anhydrous magnesium sulfate, and remove the dichloromethane solvent by rotary evaporation to obtain 432.6 g of epoxy-terminated polyether of PEG-10200 with a yield of 83.9%.

[0039] The epoxy-terminated polyether of PEG-10200 is used as a binder to prepare a solid propellant, and the specific method is as follows:

[0040] Add 25g PEG-10200 epo...

Embodiment 3

[0045] Synthesize epoxy-terminated polytetrahydrofuran-ethylene oxide copolyether of PET-5500, the specific method is as follows:

[0046] A 1000mL four-necked flask was equipped with a mechanical stirrer, a condenser and a thermometer, and 550g (0.10mol) of polytetrahydrofuran-ethylene oxide copolyether (PET-5500) and 350mL of benzene were added to the four-necked flask. Add 6.20g of sodium hydride (0.25mol) in batches, control the reaction temperature at 0-10°C, slowly add 20.08g (0.26mol) of epichlorohydrin dropwise, raise the temperature to 70±5°C and reflux for 4h after the addition, and remove the solid by filtration. The filtrate was washed with water until neutral, dried over anhydrous magnesium sulfate, and the benzene solvent was removed by rotary evaporation to obtain 466.9 g of epoxy-terminated polyether of polytetrahydrofuran-ethylene oxide copolyether (PET-5500), with a yield of 83.2%.

[0047] The solid propellant is prepared by using epoxy-terminated polytetrah...

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Abstract

The invention relates to an epoxy-terminated polyether compound as well as a preparation method and application thereof and belongs to the field of solid propellants. The compound comprises two epoxy-terminated groups; the preparation method of the epoxy-terminated polyether compound comprises the following steps: taking polyether diol and metal sodium or sodium hydride to react to generate polyether diol sodium; continually taking the polyether diol sodium and epoxy chloropropane to react and removing sodium chloride, so as to synthesize epoxy-terminated polyether. The epoxy-terminated polyether compound keeps good structure and performance of a traditional adhesive and is not sensitive to impurities including water and the like; meanwhile, the epoxy-terminated polyether compound has chemical inertness on novel energy-containing materials including ADN (Ammonium Dinitramide), CL-20, AlH3 and the like and good compatibility; after the compound is solidified, a propellant medicine block has no air pores and relatively good mechanical properties. The preparation method of the epoxy-terminated polyether compound is simple and feasible; a catalyst is not needed and an intermediate does not need to be separated; the epoxy value of the product is easy to control and large-scale production is convenient to realize.

Description

technical field [0001] The invention belongs to the field of solid propellants, in particular to an epoxy-terminated polyether compound and its preparation method and application. Background technique [0002] At present, the composite solid propellant curing system mainly adopts the method of preparing polyurethane elastomer with hydroxyl-terminated adhesive / isocyanate, such as HTPB, PEG, PAMMO, PET, GAP, PGN and other adhesive propellants. These adhesives are evenly mixed with oxidants, metal fuels and additives, and finally isocyanate reacted with terminal hydroxyl groups is added. After the adhesive / curing agent system is cured, the oxidants, fuels and other components in the propellant can be effectively fully Bond together to form a high solids elastomer. [0003] At present, the development of curing agents is almost all concentrated on isocyanate compounds. The propellants made of such compounds have stable performance, so they have been widely used. However, isocy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/337C06B33/08C06D5/02
CPCC06B23/001C06B33/08C06D5/00C06D5/02C08G65/337C08G65/338C08G2650/06C08G2650/08C08G2650/58
Inventor 任晓婷卢艳华何金选雷晴叶丹阳郭滢媛丁宁杜涛
Owner HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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