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Thermally reversible covalent cross-linked PGN-based elastomer and preparation method thereof

A technology of covalent cross-linking and elastomer, applied in the field of solid propellants, can solve the problems of unsatisfactory mechanical properties and no self-healing function of PGN cured film, and achieve the effects of excellent mechanical properties and good storage properties.

Active Publication Date: 2020-11-10
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the mechanical properties of the PGN cured film prepared in this study are still unsatisfactory (the tensile strength is 0.912 MPa, the elongation at break is 354%), and there is no self-healing function, which needs further improvement

Method used

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  • Thermally reversible covalent cross-linked PGN-based elastomer and preparation method thereof
  • Thermally reversible covalent cross-linked PGN-based elastomer and preparation method thereof
  • Thermally reversible covalent cross-linked PGN-based elastomer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] This example provides a thermally reversible covalently crosslinked PGN-based elastomer, which is prepared according to the following method:

[0030] (1) In a 100mL three-necked round-bottom flask equipped with mechanical stirring, a thermometer and a reflux device, add PGN (15g, 7.5mmol) with a molecular weight of 2000Da, glycidyl furfuryl ether (3.47g, 22.5mmol) and 40mg of catalyst N 'N-Dimethylaniline forms a mixed solution, put the mixed solution in an oil bath at 100°C, and stir for 6 hours; after the reaction, wash the mixed solution with ether at 0°C for three times, and dry it under vacuum at 40°C to obtain furan modified sexual PGN;

[0031] (2) 12g of furan-modified PGN synthesized above and tris(2-maleimidoethyl)amine crosslinking agent (1.53g, 3.96mmol) were mixed uniformly and added to the polytetrafluoroethylene mold , put the mold in an oven at 75°C, and cure for 12 hours. After the reaction time is up, demould the mold to obtain a light yellow film. ...

Embodiment 2

[0039] This example provides a thermally reversible covalently crosslinked PGN-based elastomer, which is prepared according to the following method:

[0040] (1) In a 100mL three-neck round bottom bottle equipped with mechanical stirring, a thermometer and a reflux device, add PGN (22.5g, 7.5mmol) with a molecular weight of 3000Da, glycidyl furfuryl ether (4.16g, 27mmol) and 45mg of catalyst N 'N-Dimethylaniline forms a mixed solution, put the mixed solution in an oil bath at 110°C, and stir for 8 hours; after the reaction, wash the mixed solution with ether at 0°C three times, and dry it under vacuum at 40°C to obtain furan modified sexual PGN;

[0041] (2) 18g of furan-modified PGN synthesized above and tris(2-maleimidoethyl)amine crosslinking agent (1.57g, 4.07mmol) were mixed uniformly and added to the polytetrafluoroethylene mold , put the mold in an oven at 80°C, and cure for 16 hours. After the reaction time is up, remove the mold to obtain a light yellow film.

Embodiment 3

[0043] This example provides a thermally reversible covalently crosslinked PGN-based elastomer, which is prepared according to the following method:

[0044] (1) In a 100mL three-neck round bottom bottle equipped with mechanical stirring, a thermometer and a reflux device, add PGN (30g, 7.5mmol) with a molecular weight of 4000Da, glycidyl furfuryl ether (4.62g, 30mmol) and 50mg of catalyst N' N-dimethylaniline forms a mixed solution, put the mixed solution in an oil bath at 115°C, and stir for 10 hours; after the reaction, wash the mixed solution with ether at 0°C three times, and dry it in vacuum at 40°C to obtain a furan-terminated the PGN;

[0045] (2) Mix 24g of the above-mentioned furan-modified PGN and tris(2-maleimidoethyl)amine crosslinking agent (1.62g, 4.20mmol) and add them into the polytetrafluoroethylene mold , place the mold in an oven at 85°C, and cure for 12 hours. After the reaction time is up, remove the mold to obtain a light yellow film.

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Abstract

The invention discloses a thermally reversible covalent cross-linked PGN-based elastomer and a preparation method thereof, and aims at solving the problems that a traditional PGN thermosetting film ispoor in storage stability and difficult to repair after cracking. The molecular structural formula of the thermally reversible covalent cross-linked PGN-based elastomer is shown in the specification,and n is an integer of 8 to 60. The preparation method comprises the following steps: firstly, taking PGN and glycidyl furfuryl ether as raw materials, and preparing furyl-terminated modified PGN through a ring-opening reaction; and then carrying out DielsAlder reaction by taking furyl-terminated modified PGN as a prepolymer and tri(2-maleimidylethyl)amine as a cross-linking agent, so as to prepare the thermally reversible covalent cross-linked PGN-based elastomer. The thermally reversible covalent cross-linked PGN-based elastomer is simple and feasible in synthetic route and good in storagestability, has a self-repairing function, and has a wide application value in the field of solid propellants.

Description

technical field [0001] The invention relates to a thermally reversible covalently crosslinked PGN-based elastomer, which is suitable for the field of solid propellants. Background technique [0002] Polyglycidyl ether (PGN) is a kind of high-energy adhesive with nitrate ester group in the side chain. It has the characteristics of high energy, high density, oxygen-rich, etc., and has good compatibility with nitrate ester. It is used in high-energy propulsion It is expected to increase the energy level of the propellant, reduce its risk level, and improve its safety in use. The current curing system of solid propellants is mostly isocyanate curing system, which is sensitive to moisture and prone to bubbles during the curing process. Moreover, the degradation activation energy of the PGN polyurethane network is low, and the proximity effect between the terminal hydroxyl group and the nitrate group can easily cause the polyurethane network to lose its mechanical properties due ...

Claims

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Application Information

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IPC IPC(8): C08J3/24C08L71/02C08K5/3415C08G65/331
CPCC08J3/24C08G65/26C08J2371/02C08K5/3415
Inventor 徐明辉卢先明莫洪昌段秉蕙刘宁张倩陈淼汪伟
Owner XIAN MODERN CHEM RES INST