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Polyalkenyl-terminated copolyether bonding agent and synthesis method thereof

A technology of alkenyl copolyether and synthesis method, which is applied in the direction of polyether adhesives, adhesive types, adhesives, etc., can solve the problems of harsh curing conditions, high curing temperature, and water sensitivity, so as to improve regularity, The effect of high mechanical properties and high flexibility

Active Publication Date: 2018-02-27
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

HTPB adhesives can be cured with isocyanate curing agents to form polyurethane elastomers. However, when curing isocyanate curing agents, there are problems such as harsh curing conditions, sensitivity to water, and high curing temperature.

Method used

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  • Polyalkenyl-terminated copolyether bonding agent and synthesis method thereof
  • Polyalkenyl-terminated copolyether bonding agent and synthesis method thereof
  • Polyalkenyl-terminated copolyether bonding agent and synthesis method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] (1) Synthesis of MHPET

[0029] In a 250ml four-necked flask equipped with mechanical stirring, reflux condenser, thermometer and dropping funnel, 50g (0.02mol) of hydroxyl-terminated oxirane-tetrahydrofuran copolyether (PET), 100ml of dichloromethane and 1.68g Boron trifluoride·tetrahydrofuran complex, stirred for 0.5h, cooled to 2°C, began to slowly add 4.08g of 3-hydroxymethyl-3-methyloxetane dropwise, the dropping time was 4h, and the dropwise addition was completed After that, continue the insulation reaction for 24h, and use Na 2 CO 3 The aqueous solution was neutralized, then washed 3 times with distilled water, poured into a separatory funnel, the organic phase was separated, and the solvent was evaporated under reduced pressure to obtain 52.7 g of light yellow viscous transparent liquid with a yield of 97.4%.

[0030] Structural identification: IR, ν max (cm -1 ): 3440(-OH), 2846, 2965(-CH 3 、-CH 2 ), 1101 (C-O-C).

[0031] 1 H NMR (CDCl 3 , 500MHz): 1...

Embodiment 2

[0040] (1) Synthesis of MHPET

[0041] In a 250ml four-neck flask equipped with mechanical stirring, reflux condenser, thermometer and dropping funnel, 50g (0.02mol) of hydroxyl-terminated oxirane-tetrahydrofuran copolyether (PET), 100ml of dichloromethane and 2.24g Boron trifluoride·tetrahydrofuran complex, stirred for 0.5h, cooled to 3°C, began to slowly add 6.12g of 3-hydroxymethyl-3-methyloxetane dropwise, the dropping time was 5h, and the dropwise addition was completed After that, continue the insulation reaction for 28h, and use Na 2 CO 3 The aqueous solution was neutralized, then washed 3 times with distilled water, poured into a separatory funnel, the organic phase was separated, and the solvent was evaporated under reduced pressure to obtain 54.5 g of light yellow viscous transparent liquid with a yield of 97.1%.

[0042] The number average molecular weight is 2810, and the hydroxyl value is 96.8 mgKOH / g.

[0043] (2) Synthesis of MAPET

[0044] In a 250ml four-n...

Embodiment 3

[0047] (1) Synthesis of MHPET

[0048] In a 250ml four-necked flask equipped with mechanical stirring, reflux condenser, thermometer and dropping funnel, 60g (0.02mol) of hydroxyl-terminated oxirane-tetrahydrofuran copolyether (PET), 100ml of dichloromethane and 2.24g Boron trifluoride tetrahydrofuran complex, stirred for 0.5h, cooled to 4°C, began to slowly add 6.12g of 3-hydroxymethyl-3-methyloxetane dropwise, the dropping time was 5h, and the dropwise addition was completed After that, continue the insulation reaction for 28h, and use Na 2 CO 3 The aqueous solution was neutralized, then washed three times with distilled water, poured into a separatory funnel, the organic phase was separated, and the solvent was evaporated under reduced pressure to obtain 64.5 g of light yellow viscous transparent liquid with a yield of 97.5%.

[0049] The number average molecular weight was 3320, and the hydroxyl value was 83.1 mgKOH / g.

[0050] (2) Synthesis of MAPET

[0051] In a 250m...

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Abstract

The invention provides a polyalkenyl-terminated copolyether bonding agent and a synthesis method thereof. The polyalkenyl-terminated copolyether bonding agent is shown as a structural formula (I). Thesynthesis process comprises the following steps of (1) using hydroxyl-terminated oxirane-tetrahydrofuran copolyether as an initiator and 3-hydroxymethyl-3-methyloxetane as monomers to perform cationic ring-opening polymerization reaction to obtain polyalkenyl-terminated oxirane-tetrahydrofuran copolyether; (2) using the polyalkenyl-terminated oxirane-tetrahydrofuran copolyether and allyl bromideas raw materials and potassium tert-butoxide as a catalyst to obtain the polyalkenyl-terminated copolyether bonding agent through etherification reaction. The synthesis method is simple; the polyalkenyl-terminated copolyether bonding agent can give strong mechanical property to polyisoxazoline elastomers. The formula I is shown in the description, wherein x+y is equal to1 to 6, and is an integer;m is 10 to 60, and is an integer; n is 10 to 60, and is an integer.

Description

technical field [0001] The invention relates to a polyene-terminated copolyether adhesive and a synthesis method thereof. The compound can be used as an adhesive for solid propellants and belongs to the technical field of polymer materials. Background technique [0002] Hydroxyl-terminated polybutadiene (HTPB) is a "telechelic" polymer compound with active terminal hydroxyl groups. It has good physical and chemical properties, low glass transition temperature and viscosity, good process and mechanical properties, and high capacity. It is the most widely researched and applied binder for solid propellants at present. HTPB adhesives can be cured with isocyanate curing agents to form polyurethane elastomers. However, when curing isocyanate curing agents, there are problems such as harsh curing conditions, sensitivity to water, and high curing temperature. [0003] In order to solve the above-mentioned problems in the curing of HTPB adhesives, researchers have developed a polyi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J171/02C08G65/337C08G65/20C08G65/28
CPCC08G65/20C08G65/2609C08G65/337C09J171/02
Inventor 莫洪昌卢先明徐明辉刘宁舒远杰葛忠学
Owner XIAN MODERN CHEM RES INST
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