Preparation method of long-carbon-chain nylon elastomer and application of dicarboxylic acid

A technology of nylon elastomer and dicarboxylic acid, which is applied in the field of dicarboxylic acid, can solve the problems of harsh synthesis conditions, difficult equimolar ratio, low molecular weight of nylon elastomer, etc., and achieve high molecular weight, mild reaction conditions, The effect of excellent comprehensive performance

Active Publication Date: 2021-10-01
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis method of nylon elastomer generally adopts polycondensation reaction, which needs to be carried out under high temperature, high vacuum and special catalyst conditions, and the synthesis conditions are relatively harsh.
In addition, this method needs to control the equimolar ratio of the specific functional groups between the soft segment and the hard segment, but in the actual reaction process, it is extremely difficult to achieve the equimolar ratio of the specific functional groups, resulting in the molecular weight of the produced nylon elastomer being different. High, the performance of nylon elastomer needs to be further improved

Method used

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  • Preparation method of long-carbon-chain nylon elastomer and application of dicarboxylic acid
  • Preparation method of long-carbon-chain nylon elastomer and application of dicarboxylic acid
  • Preparation method of long-carbon-chain nylon elastomer and application of dicarboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 100 parts by weight of long carbon chain nylon 1210 salt, 10 parts by weight of sebacic acid, 60 parts by weight of deionized water, and 0.22 parts by weight of antioxidant 1098 are placed in the reactor, and the gas in the reactor is replaced with an inert gas, and then the temperature is raised to React at 190°C for 2 hours, and then release the system to normal pressure.

[0049] Add 100 parts by weight of polytetrahydrofuran ether glycol (number average molecular weight: 2000), 1.17 parts by weight of succinic acid and 0.42 parts by weight of tetrabutyl titanate into the reaction kettle; heat up to 200° C. for 3 hours.

[0050] Add 0.42 parts by weight of tetrabutyl titanate to the reaction kettle, heat up to 245°C, and then vacuumize, so that the absolute pressure slowly drops below 100 Pa within 30 minutes, continue the reaction for 4 hours, then stop heating, return the system to normal pressure and release The materials are cooled, pelletized and dried to obtain...

Embodiment 2

[0054] 100 parts by weight of long carbon chain nylon 1210 salt, 10 parts by weight of sebacic acid, 60 parts by weight of deionized water, and 0.22 parts by weight of antioxidant 1098 are placed in the reactor, and the gas in the reactor is replaced with an inert gas, and then the temperature is raised to React at 190°C for 2 hours, and then release the system to normal pressure.

[0055] Add 100 parts by weight of polytetrahydrofuran ether glycol (number average molecular weight: 2000), 3.01 parts by weight of sebacic acid and 0.43 parts by weight of tetrabutyl titanate into the reaction kettle; heat up to 200° C. for 3 hours.

[0056] Add 0.43 parts by weight of tetrabutyl titanate to the reaction kettle, heat up to 245°C, and then vacuumize, so that the absolute pressure slowly drops below 100 Pa within 30 minutes, continue the reaction for 4 hours, then stop heating, return the system to normal pressure and release The materials are cooled, pelletized and dried to obtain ...

Embodiment 3

[0059] 100 parts by weight of long carbon chain nylon 1210 salt, 10 parts by weight of sebacic acid, 60 parts by weight of deionized water, and 0.22 parts by weight of antioxidant 1098 are placed in the reactor, and the gas in the reactor is replaced with an inert gas, and then the temperature is raised to React at 190°C for 2 hours, and then release the system to normal pressure.

[0060] Add 83 parts by weight of polytetrahydrofuran ether glycol (number average molecular weight: 1000), 1.17 parts by weight of succinic acid and 0.40 parts by weight of tetrabutyl titanate into the reaction kettle; heat up to 200° C. for 3 hours.

[0061] Add 0.40 parts by weight of tetrabutyl titanate to the reaction kettle, heat up to 245°C, and then vacuumize, so that the absolute pressure slowly drops below 100 Pa within 30 minutes, continue the reaction for 4 hours, then stop heating, return the system to normal pressure and release The materials are cooled, pelletized and dried to obtain ...

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Abstract

The invention discloses a preparation method of a long-carbon-chain nylon elastomer. The preparation method comprises the following steps of: reacting long carbon chain nylon salt with C10-C20 dicarboxylic acid for 2-3 hours at 180-190 DEG C in the presence of a solvent under the protection of inert gas to obtain carboxyl-terminated polyamide; reacting the carboxyl-terminated polyamide, polytetrahydrofuran ether glycol, C4-C10 dicarboxylic acid and a first catalyst under the protection of inert gas at 200-210 DEG C for 2-4 hours to obtain a prepolymer; and adding a second catalyst into the reaction system, then heating to 230-250 DEG C, vacuumizing to reduce the absolute pressure of the reaction system to 100 Pa or below within 30 minutes, and continuing to react for 3-6 hours to enable the prepolymer to generate terminal carboxyl ester exchange, thereby obtaining the long-carbon-chain nylon elastomer. According to the invention, the long-carbon-chain nylon elastomer with higher molecular weight can be prepared.

Description

technical field [0001] The invention relates to a preparation method of a long carbon chain nylon elastomer, and also relates to a use of a dibasic carboxylic acid. Background technique [0002] Nylon elastomers are newly developed alternating block copolymers consisting of polyamide hard segments and polyether or polyester soft segments. Due to its excellent low-temperature impact resistance, good heat resistance, good flexibility, high elastic recovery and good processing performance, nylon elastomer is widely used in gas separation membranes, permanent antistatic agents, industrial products, new electronic devices, etc. The field shows great application potential, thus becoming a kind of elastomer material that has attracted much attention. [0003] At present, the synthesis method of nylon elastomer generally adopts polycondensation reaction, which needs to be carried out under high temperature, high vacuum and special catalyst conditions, and the synthesis conditions a...

Claims

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Application Information

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IPC IPC(8): C08G69/44
CPCC08G69/44
Inventor 潘凯龚舜陈向阳
Owner BEIJING UNIV OF CHEM TECH
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