A kind of method of continuous production polyether amide

A technology of polyetheramide and caprolactam, which is applied in the field of continuous production of polyetheramide, can solve the problems of poor product uniformity, cost, quality and product disadvantage, achieve high structural uniformity, eliminate the concentration of terminal carboxyl groups, and reduce the risk of esterification reaction Effect

Active Publication Date: 2021-03-02
CHINA TEXTILE ACADEMYTIANJINSCI & TECH DEV CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] It can be seen that at present, the preparation of polyetheramide usually adopts a batch method. Although this method has the advantage of high production flexibility, the uniformity of the produced product is poor, and it is at an obvious disadvantage in terms of cost, quality and product.

Method used

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  • A kind of method of continuous production polyether amide
  • A kind of method of continuous production polyether amide
  • A kind of method of continuous production polyether amide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069]A1. Mix the caprolactam melt, capping agent adipic acid and water uniformly and enter the pre-polymerization reactor to carry out the pre-polymerization reaction. The mass ratio of caprolactam melt, capping agent adipic acid and water is 92.6wt%:4.7 wt%: 2.7 wt%, the reaction temperature is 265° C., the reaction pressure is 200 kPa, and the reaction time is 4 h to obtain a carboxyl-terminated caprolactam prepolymer with a molecular weight of 3000.

[0070]A2. The carboxyl-terminated caprolactam prepolymer prepared in step A1 is mixed with the polyethylene glycol added online and the catalyst tetraisopropyl titanate through the high-shear homogenizing pump of the dynamic mixer, and then enters the falling film tower reaction The pre-polycondensation reaction is carried out in the reactor, wherein the molecular weight of the polyethylene glycol added online is 2000, the polyethylene glycol injection amount is 10wt% of the mass of the caprolactam prepolymer, and the injection amount...

Embodiment 2

[0074]A1. Mix the caprolactam melt, capping agent adipic acid and water uniformly and enter the pre-polymerization reactor for pre-polymerization reaction. The mass ratio of caprolactam melt, capping agent adipic acid and water is 75wt%:20wt% : 5wt%, the reaction temperature is 235°C, the reaction pressure is 600kPa, and the reaction time is 3h to obtain a carboxyl-terminated caprolactam prepolymer with a molecular weight of 550.

[0075]A2. The carboxyl-terminated caprolactam prepolymer prepared in step A1, the polypropylene glycol added online and the catalyst tetrapropyl zirconate are mixed uniformly through the high-shear homogenization pump of the dynamic mixer, and then enters the falling film tower reactor to proceed. Pre-polycondensation reaction, where the molecular weight of the polypropylene glycol added online is 4000, the injection amount of polypropylene glycol is 20wt% of the mass of the caprolactam prepolymer, the injection amount of the catalyst tetrapropyl zirconate i...

Embodiment 3

[0079]A1. Mix the caprolactam melt, capping agent adipic acid and water uniformly and enter the pre-polymerization reactor for the pre-polymerization reaction. The mass ratio of caprolactam melt, capping agent adipic acid and water is 98.0wt%: 1.5 wt%: 0.5wt%, the reaction temperature is 300° C., the reaction pressure is 100 kPa, and the reaction time is 10 h to obtain a carboxyl-terminated caprolactam prepolymer with a molecular weight of 10,000.

[0080]A2. The carboxyl-terminated caprolactam prepolymer prepared in step A1 is mixed with the polyethylene glycol added online and the catalyst tetrabutyl titanate uniformly through the dynamic mixer screw extruder, and then enters the falling film tower reactor for pretreatment. Polycondensation reaction, where the molecular weight of the polyethylene glycol added online is 10,000, the polyethylene glycol injection amount is 40wt% of the mass of the caprolactam prepolymer, and the injection amount of the catalyst tetraisopropyl titanate i...

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Abstract

The invention relates to a method for continuously producing polyether amide. The method mainly comprises the following steps: uniformly mixing lactam melt, an end capping agent, i.e., a dibasic acid,and water, and then, enabling the mixture to enter a pre-polymerization reactor for a pre-polymerization reaction, so as to obtain a carboxyl-terminated lactam prepolymer; uniformly mixing the obtained carboxyl-terminated lactam prepolymer, polyalkaneneglycol which is added on line and a catalyst by a shearing homogenizer, and then, enabling the mixture to enter a pre-polycondensation reactor fora pre-polycondensation reaction, so as to obtain polyether amide prepolymer melt; subjecting the obtained polyether amide prepolymer to a final polycondensation reaction in a final polycondensation reactor, so as to obtain polyether amide melt; and subjecting the obtained polyether amide melt to pelleting, extracting and drying sequentially, thereby obtaining polyether amide slices. According tothe method, through innovation of processing technologies, the accurate proportional adding of a modifier, i.e., polyalkaneneglycol in a continuous polyether amide production process and effective regulation and control on a polymerization reaction process are achieved, and the continuously produced polyether amide has high structural homogeneity.

Description

Technical field[0001]The invention relates to a method for continuously producing polyetheramide.Background technique[0002]Polyetheramide is a multi-block copolymer composed of polyamide hard segment and polyether soft segment. It has excellent processing properties, moisture absorption properties, mechanical properties, chemical resistance and other excellent comprehensive properties. It has been widely used in the automotive industry. , Machinery, textiles, electronic appliances, electrical precision instruments, sporting goods, medical, telecommunications and other fields.[0003]Patent CN200910200344.6 discloses a specific preparation process of a polyether block-containing polyamide thermoplastic elastomer: adding 100 minutes of amino-terminated polyether into a reaction vessel, heating to 140-180°C, and heating at 50-200 r / min Add 0.1-1 part of anionic catalyst under stirring at a speed of 0.5 to 1 hour after the catalyst reacts with the amino-terminated polyether, then add 50 t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/00C08G69/40
CPCC08G69/40C08G81/00
Inventor 邱志成李鑫曲希明姜峰金剑
Owner CHINA TEXTILE ACADEMYTIANJINSCI & TECH DEV CO LTD
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