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Dual-cured nitrate polyether and synthesis method thereof

A nitrate ester and dual curing technology, applied in the direction of attacking equipment, compressed gas generation, etc., can solve the problems of low mechanical properties such as film tensile strength and elongation at break, and achieve moderate curing rate, wide adjustment range, high The effect of mechanical properties

Active Publication Date: 2020-08-25
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The mechanical properties such as tensile strength and elongation at break of the film are low

Method used

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  • Dual-cured nitrate polyether and synthesis method thereof
  • Dual-cured nitrate polyether and synthesis method thereof
  • Dual-cured nitrate polyether and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] At room temperature, add 30g (10mmol) hydroxyl-terminated poly-3-nitrate methyl-3-methyloxetane and 60mL dichloromethane into the reaction flask, stir well, then add 1.42g (10mmol) trifluoro Boronium ether complex, reacted for 30min under stirring, cooled to 0°C, began to slowly add 3.68g (20mmol) of 3-methacryloyloxymethyl-3-ethyloxetane dropwise, and the dropwise addition was completed Afterwards, the reaction was continued for 24 hours, neutralized with aqueous sodium carbonate solution, washed with water until neutral, the oil phase was separated and dichloromethane was distilled off under reduced pressure to obtain a light yellow viscous liquid.

[0027] Structure Identification:

[0028] IR, ν max (cm -1 ): 3651 (-OH), 2941, 2863, 2804 (-CH 2 -, -CH 3 ), 1719 (-COO-), 1637 (C=C-), 1632, 1281, 869 (-ONO 2 ), 1114 (C-O-C).

[0029] 1 HNMR (CDCl 3 ,500MHz): δ6.13, 5.60, 4.39, 4.25, 3.23~3.30, 1.96, 1.76, 0.90.

[0030] 13 C NMR (CDCl 3 ,500MHz): δ167.9, 13...

Embodiment 2

[0034] At room temperature, add 30g (10mmol) hydroxyl-terminated poly-3-nitrate methyl-3-methyloxetane and 60mL dichloromethane into the reaction flask, stir well, then add 1.42g (10mmol) trifluoro Boronium ether complex, reacted for 30min under stirring, cooled to 0°C, began to slowly add 7.36g (40mmol) of 3-methacryloyloxymethyl-3-ethyloxetane dropwise, and the dropwise addition was completed Afterwards, the reaction was continued for 28 hours, neutralized with aqueous sodium carbonate solution, washed with water until neutral, the oil phase was separated and dichloromethane was distilled off under reduced pressure to obtain a light yellow viscous liquid.

[0035] Molecular weight and distribution: Mn=3675, Mw=5733, Mw / Mn=1.56.

Embodiment 3

[0037] At room temperature, add 40g (10mmol) hydroxyl-terminated poly-3-nitrate methyl-3-methyloxetane and 80mL dichloromethane into the reaction flask, stir well, then add 1.42g (10mmol) trifluoro Boronium ether complex, reacted for 30min under stirring, cooled to 0°C, began to slowly add 5.52g (30mmol) of 3-methacryloyloxymethyl-3-ethyloxetane dropwise, and the dropwise addition was completed Afterwards, the reaction was continued for 28 hours, neutralized with aqueous sodium carbonate solution, washed with water until neutral, the oil phase was separated and dichloromethane was distilled off under reduced pressure to obtain a light yellow viscous liquid.

[0038] Molecular weight and distribution: Mn=4548, Mw=7186, Mw / Mn=1.58.

[0039] Dual curing type nitrate ester polyether application performance of the present invention

[0040] (1) Miscibility and reactivity evaluation with curing agent

[0041]Ethylene glycol diazide acetate (EGBAA), 1,5-diazido-3-nitroazapentane (D...

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Abstract

The invention discloses dual-cured type nitrate polyether and a synthesis method thereof. The structural formula of the dual-cured nitrate polyether is shown as a formula (I). The synthesis process ofthe dual-cured nitrate polyether comprises the following steps of: taking hydroxyl-terminated poly (3-nitrate methyl-3-methyloxetane) as a raw material and acrylate substituted oxetane as a monomer,carrying out cationic ring-opening polymerization reaction to obtain the dual-cured nitrate polyether. The double-cured type nitrate polyether disclosed by the invention is simple in synthesis methodand easy to amplify, contains two active reaction groups, namely hydroxyl and acrylate groups, can be cured by adopting a polyazide compound, and can also be cured by adopting a polyisocyanate compound. The dual-cured type nitrate polyether of the invention is mainly used for composite solid propellants. According to the structural formula, R1 is H or CH3, R2 is CH3 or CH2CH3, n is an integer ranging from 10 to 60, x is an integer ranging from 1 to 3, y is an integer ranging from 1 to 3, and y is an integer ranging from 1 to 3.

Description

technical field [0001] The invention relates to a dual-curing nitrate polyether and a synthesis method thereof. The compound is mainly used as a binder for solid propellants and belongs to the field of solid propellants. Background technique [0002] Hydroxy-terminated oxirane-tetrahydrofuran copolyether (PET) adhesive has the characteristics of good miscibility with nitrate plasticizers, good main chain flexibility, low viscosity, and low glass transition temperature. Polyether (NEPE) propellants have been widely used. PET generally forms an isocyanate curing system with a polyisocyanate curing agent. Polyurethane elastomers are prepared through the curing reaction between terminal hydroxyl groups and isocyanate groups. However, the curing conditions of the isocyanate curing system are harsh and sensitive to moisture. The isocyanate group can quickly react with water or organic acids. Generate CO 2 , It is easy to form pores in the propellant, which affects its mechanical...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/332C06D5/00
CPCC08G65/3328C06D5/00C08G2650/50
Inventor 莫洪昌卢先明徐明辉刘宁张倩葛忠学
Owner XIAN MODERN CHEM RES INST
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