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A kind of caprolactam hydrolysis polymer and its hydrolysis polymerization method

A technology of caprolactam and hydrolysis polymerization, applied in the field of polymer polymerization, can solve the problems of inability to control oligomers, low polymer molecular weight, slow reaction speed, etc., and achieve the effects of reducing energy consumption, improving utilization rate, and reducing possibility

Active Publication Date: 2016-10-19
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to ensure that the polymerization process is carried out in a liquid state, the polymerization temperature must be at least 10°C higher than the melting point of polyamide 6. At this time, the polymerization temperature still cannot control the oligomer in the range of direct spinning of the melt, and there is another low-temperature polymerization. Disadvantages, that is, the reaction speed is slow, and the molecular weight of the obtained polymer is low; and the polymerization process at a lower temperature is actually divided into two parts, one is a melt polymerization process, and the other is a solid phase polymerization process. The process is to obtain a polymer with sufficient molecular weight for product development, but there is no effective way to turn the solid polymer formed at low temperature into a suitable spinning method. If fibers are spun from low-temperature polymers, they must be The polymer is melted first, however, at this time, with the balance related to time and temperature, low-molecular compounds are formed, the amount of which is adapted to the temperature of melting, and is always more than that of low-temperature polymerization. In this way, Compared with the normal aggregation method, there is no advantage

Method used

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  • A kind of caprolactam hydrolysis polymer and its hydrolysis polymerization method
  • A kind of caprolactam hydrolysis polymer and its hydrolysis polymerization method
  • A kind of caprolactam hydrolysis polymer and its hydrolysis polymerization method

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Embodiment 1

[0038] A method for hydrolytic polymerization of a caprolactam hydrolyzed polymer, the specific steps comprising:

[0039] The first step: at a temperature of 80°C, caprolactam, capping agent HOOC (CH 2 ) 2 COOH, deionized water and catalyst nylon 66 salt were mixed in proportion, mechanically stirred for 10min, and the rotating speed was 60r / min; wherein relative to caprolactam, the amount of deionized water added was 2wt%, and the capping agent HOOC(CH 2 ) 2 The addition of COOH is 5%, and the addition of catalyst nylon 66 salt is 0.1wt%;

[0040] The second step: pre-polymerize the mixture obtained in the first step under nitrogen atmosphere, the polymerization temperature is controlled at 150 ° C, and the polymerization pressure is controlled at 0.1 MPa; when the following conditions are met, the reaction is terminated: the molecular weight of the obtained prepolymer is 1000 , the content of terminal amino groups is ≤1mmol / kg, the content of extractables is ≤10wt%, and ...

Embodiment 2

[0045] The first step: at a temperature of 140°C, caprolactam, HOOC (CH 2 ) 10 COOH, deionized water and NH 2 (CH 2 ) 4 COOH was mixed in proportion, mechanically stirred for 60min, and the rotating speed was 240r / min; wherein relative to caprolactam, the amount of deionized water added was 5wt%, HOOC(CH 2 ) 10 The amount of COOH added is 30%, NH 2 (CH 2 ) 4 The amount of COOH added is 5wt%;

[0046] The second step: pre-polymerize the mixture obtained in the first step under a nitrogen atmosphere, the polymerization temperature is controlled at 200 ° C, and the polymerization pressure is controlled at 3 MPa; when the following conditions are met, the reaction is terminated: the molecular weight of the obtained prepolymer is 5000, Amino-terminal content ≤ 1mmol / kg, extractables content ≤ 10wt%, and cyclic dimer content ≤ 0.3wt%;

[0047] The third step: adding tetrabutyl titanate as a transesterification catalyst, the addition amount is 500ppm of the caprolactam mass ...

Embodiment 3

[0052] A method for hydrolytic polymerization of a caprolactam hydrolyzed polymer, the specific steps comprising:

[0053] The first step: under the condition of temperature of 100 ℃, caprolactam, capping agent HOOC (CH 2 ) 5 COOH, deionized water and catalyst NH 2 (CH 2 ) 10 COOH was mixed in proportion, mechanically stirred for 30min, and the rotating speed was 100r / min; wherein relative to caprolactam, the amount of deionized water added was 3wt%, and the capping agent HOOC(CH 2 ) 5 The amount of COOH added is 10%, the catalyst NH 2 (CH 2 ) 10 The amount of COOH added is 0.1-5wt%;

[0054] The second step: pre-polymerize the mixture obtained in the first step under nitrogen atmosphere, the polymerization temperature is controlled at 180 ° C, and the polymerization pressure is controlled at 0.5 MPa; when the following conditions are met, the reaction is terminated: the molecular weight of the obtained prepolymer is 3000 , the content of terminal amino groups is ≤1mm...

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Abstract

The invention relates to a caprolactam hydrolytic polymer and a hydrolytic polymerization method thereof. The hydrolytic polymerization method is characterized by pre-controlling the content of oligomers in a melt by firstly preparing a polyamide 6 prepolymer at low temperature, simultaneously adopting binary acid for termination in an auxiliary manner to reduce the content of amino end groups in a system, then adopting ethylene glycol for termination and carrying out chain propagation later by gylcol ester removal exchange, wherein in the obtained product, the content of extractable matters is not more than 2wt% and the content of cyclic dimmers is not more than 0.3wt%. The hydrolytic polymerization method has the beneficial effects that the polymerization process is simple, can be carried out on the basis of traditional polymerization equipment and also has the effect of reducing the energy consumption while the use ratio of caprolactam is increased; the obtained melt can directly undergo melt spinning, easily achieves high-capacity large-scale production and can be applied in the fields of fibers for clothes, industrial yarns, engineering plastics, and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer polymerization, and relates to a caprolactam hydrolysis polymer and a hydrolysis polymerization method thereof. Background technique [0002] Due to its excellent physical and mechanical properties and textile processing properties, nylon fiber has ranked first in the synthetic fiber family for a long period of time since its inception. However, due to price and production cost constraints and polyester fiber The rapid development of the synthetic fiber is now the second largest output. In 2013, my country's nylon output was 2.1128 million tons, a year-on-year increase of 12.44%, accounting for about 6.3% of the total synthetic fiber output. Nylon fiber has excellent physical properties unmatched by polyester fiber. For example, nylon fiber has high breaking strength, wear resistance ranks first among general textile fibers, good hygroscopicity, excellent elastic recovery rate and fatigue resista...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/16C08G69/14
Inventor 汤廉王朝生王华平江振林吉鹏赵晓敏黄庆
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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