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Melt direct processing caprolactam polymerization method

A technology of caprolactam and polymerization method, which is applied in the field of nylon materials, can solve the problems of low polymer number average molecular weight, slow reaction speed, and oligomer control, and achieve the effects of reducing energy consumption, improving utilization rate, and simple process

Active Publication Date: 2020-07-10
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 nylon 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 disadvantage of low temperature polymerization , that is, the reaction speed is slow, and the number-average molecular weight of the polymer obtained is relatively low; while the polymerization process at a lower temperature is actually divided into two parts, one part is a mel

Method used

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  • Melt direct processing caprolactam polymerization method
  • Melt direct processing caprolactam polymerization method
  • Melt direct processing caprolactam polymerization method

Examples

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Embodiment 1

[0063] The first step: at a temperature of 75°C, caprolactam, HOOC (CH 2 ) 4 COOH, deionized water and NH 2 (CH 2 ) 4 COOH was mixed in proportion, and stirred for 60min under the condition of mechanical stirring (60r / min); the amount of deionized water added was 1.5wt% relative to caprolactam, and HOOC(CH 2 ) 2 The amount of COOH added is 0.4wt%, NH 2 (CH 2 ) 4 The amount of COOH added is 0.8wt%;

[0064] The second step: After the mixture obtained in the first step is heated by the melt pump and the pre-heater, it is transported to the ring-opening kettle for ring-opening reaction. The polymerization temperature is controlled at 213 ° C, and the polymerization pressure is controlled at 1.8 MPa; the reaction time is The 0.7h prepolymer is transported to the top of the tower by a melt pump, mixed with fresh caprolactam, and the reflux flow is 1.8wt% of the caprolactam flow. When the following conditions are met, the reaction is terminated: the number average molecular...

Embodiment 2

[0069] The first step: at a temperature of 138°C, caprolactam, HOOC (CH 2 ) 8 COOH, deionized water and nylon 66 salt were mixed in proportion, and stirred for 15 minutes under the condition of mechanical stirring (200r / min); the amount of deionized water added was 3.5wt% relative to caprolactam, HOOC(CH 2 ) 8 The amount of COOH added is 0.12wt%, and the amount of nylon 66 salt added is 0.03wt%;

[0070] The second step: After the mixture obtained in the first step is heated by the melt pump and the pre-heater, it is transported to the ring-opening kettle for ring-opening reaction. The polymerization temperature is controlled at 258 ° C, and the polymerization pressure is controlled at 0.3 MPa; the reaction time is The 1.4h prepolymer is transported to the top of the tower by a melt pump, mixed with fresh caprolactam, and the reflux flow is 0.48wt% of the caprolactam flow. When the following conditions are met, the reaction is terminated: the number average molecular weight...

Embodiment 3

[0075] The first step: at a temperature of 95°C, caprolactam, terephthalic acid, deionized water and NH 2 (CH 2 ) 4 COOH was mixed in proportion, and stirred for 45 minutes under the condition of mechanical stirring (120r / min); among them, relative to caprolactam, the amount of deionized water added was 2.3wt%, the amount of terephthalic acid added was 0.33wt%, and the amount of NH 2 (CH 2 ) 4 The amount of COOH added is 0.47wt%;

[0076] The second step: After the mixture obtained in the first step is heated by the melt pump and the pre-heater, it is transported to the ring-opening kettle for ring-opening reaction. The polymerization temperature is controlled at 228 ° C, and the polymerization pressure is controlled at 0.9 MPa; the reaction time is The 1.3h prepolymer is transported to the top of the tower by a melt pump, mixed with fresh caprolactam, and the reflux rate is 1.5wt% of the caprolactam flow rate. When the following conditions are met, the reaction is termin...

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Abstract

The invention relates to the field of nylon materials, and discloses a melt direct processing caprolactam polymerization method which comprises the following steps: (1) burdening: heating and mixing caprolactam, an end-capping reagent, water and a catalyst to obtain a mixture; (2) ring opening: heating the mixture to carry out a ring opening reaction; (3) pre-polycondensation: heating the productobtained through ring opening to conduct pre-polycondensation reaction and devolatilization; and (4) final polycondensation: heating the product obtained through pre-polycondensation to conduct finalpolycondensation reaction and devolatilization. By means of the method, direct processing of a nylon melt after polymerization can be achieved, and the content of hot water extractable substances andthe content of cyclic dimers in the nylon melt can be effectively controlled.

Description

technical field [0001] The invention relates to the field of nylon materials, in particular to a caprolactam polymerization method capable of direct melt processing. Background technique [0002] Nylon is widely used in various fields, for example, it can be processed into fibers, films and plastic products, etc. [0003] Among them, taking nylon fiber as an example, because of its excellent physical and mechanical properties and textile processing properties, nylon fiber (PA fiber, nylon) has ranked first in the synthetic fiber family in terms of output for a long time since its inception. However, due to the limitation of price and production cost and the rapid development of polyester fiber, it is now the second largest output of synthetic fiber. In 2018, my country's nylon output exceeded 3.3 million tons. Nylon 6 fiber has excellent physical properties unmatched by polyester fiber. For example, nylon 6 fiber has high breaking strength, wear resistance is the crown of ge...

Claims

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Application Information

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IPC IPC(8): C08G69/16C08G69/14B01J19/18
CPCC08G69/16C08G69/14B01J19/0053B01J19/1862
Inventor 汤廉徐锦龙王松林何宁艳黄家鹏王华平王朝生
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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