Preparation method and preparation device of semi-aromatic polyamide

A semi-aromatic polyamide and lactam technology, applied in feeding devices, chemical instruments and methods, chemical/physical/physical-chemical stationary reactors, etc., can solve the problem of gel particles losing melt processability, semi-aromatic Deterioration of polyamide resin performance, degradation and crosslinking of nylon resin, etc.

Active Publication Date: 2021-03-12
SHANDONG GUANGYIN NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high melting temperature, the long residence time of semi-aromatic polyamide at high temperature will lead to the degradation and crosslinking of nylon

Method used

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  • Preparation method and preparation device of semi-aromatic polyamide
  • Preparation method and preparation device of semi-aromatic polyamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] Example 1: PA6T / 6I / 66=65:25:10

[0082] (1) In the 50L salt forming kettle, add 4.648kg hexamethylenediamine, 0.5846kg adipic acid, 4.319kg terephthalic acid, 1.661kg isophthalic acid, 20g sodium hypophosphite and 16.82kg deionized water, the mixture is in Stir at 80°C to form a salt for 30 minutes to obtain a salt solution.

[0083] (2) After the salt is formed, the salt solution is added to the conical high-pressure polymerization kettle for polymerization reaction. The reaction temperature is 250° C. and the pressure is 3.5 MPa; after the salt solution is added to the reactor, close the reactor feed valve, The gas in the kettle was replaced by nitrogen, and the temperature in the kettle was raised to 250° C. within 85 minutes, and the pressure in the kettle reached 3.5 MPa. The stirring state was kept during the whole heating process, and the stirring rate was 5 r / min.

[0084] (3) After the polymerization reaction is over, the pressure in the kettle is gradually re...

Embodiment 2

[0086] Embodiment 2: PA6T / 6I / 66=60:15:25

[0087] (1) In the 50L salt forming kettle, add 4.648kg hexamethylenediamine, 1.461kg adipic acid, 3.987kg terephthalic acid, 0.9968kg isophthalic acid, 20g sodium hypophosphite and 16.64kg deionized water, the mixture is in Stir at 80°C to form a salt for 30 minutes to obtain a salt solution.

[0088] (2) After the salt is formed, the salt solution is added to the conical high-pressure polymerization kettle for polymerization reaction. The reaction temperature is 230°C and the pressure is 2.5MPa; the effective volume of the polymerization kettle is 100L, the height of the reaction kettle is 1800mm, and the polymerization kettle is equipped with The jacket is used to heat the polymerization kettle through heat-conducting oil. The reactor is equipped with a ribbon-type stirring paddle with a width of 82 mm. After the salt solution is added to the reactor, the feed valve of the reactor is closed, and the gas in the reactor is replaced by...

Embodiment 3

[0091] Embodiment 3: PA6T / 6I=65:35

[0092] (1) Add 4.648kg of hexamethylenediamine, 4.319kg of terephthalic acid, 2.326kg of isophthalic acid, 20g of sodium hypophosphite and 16.94kg of deionized water into a 50L salt-forming kettle, and stir the mixture at 80°C to form a salt 30min to obtain a saline solution.

[0093] (2) After the salt is formed, the salt solution is added to the conical high-pressure polymerization kettle for polymerization reaction. The reaction temperature is 250°C and the pressure is 3.5MPa; the effective volume of the polymerization kettle is 100L, the height of the reaction kettle is 1800mm, and the polymerization kettle is equipped with The jacket is used to heat the polymerization kettle through heat-conducting oil. The reactor is equipped with a ribbon-type stirring paddle with a width of 82 mm. After the salt solution is added to the reactor, the feed valve of the reactor is closed, and the gas in the reactor is replaced by nitrogen. The tempera...

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Abstract

The invention relates to the technical field of semi-aromatic polyamide, in particular to a preparation method and a preparation device of semi-aromatic polyamide. The preparation method of the semi-aromatic polyamide comprises the following steps: under the action of a catalyst, salifying a diacid monomer and one or more of a diamine monomer, lactam and omega-amino acid in a water phase to obtaina salt solution; conveying the salt solution into a polymerization kettle through a pipeline to carry out polymerization reaction; after the polymerization reaction is finished, subjecting the polymerization kettle to pressure relief and cooling, and then crushing prepolymer solids through stirring in the kettle; and drying the crushed prepolymer solid in the polymerization kettle, and carrying out solid-phase polymerization to obtain the semi-aromatic polyamide. The preparation method is short in technological process and high in synthesis efficiency, and the prepared semi-aromatic polyamideis low in terminal amino group and terminal carboxyl group content and high in intrinsic viscosity. According to the preparation device, the number of equipment in the production process is reduced,and the investment cost and the operation cost of the equipment are remarkably reduced.

Description

technical field [0001] The invention relates to the technical field of semi-aromatic polyamides, in particular to a preparation method and a preparation device of semi-aromatic polyamides. Background technique [0002] Polyamide refers to a class of polymers containing amide bonds in the main chain. Due to the hydrogen bond interaction and crystallization characteristics of amide bonds, it has excellent mechanical strength, wear resistance, and solvent resistance. Therefore, polyamides are usually used in plastic pipes and profiles. , Parts, films and fibers are used in many fields. [0003] Due to the large amount of fatty structure, common polyamide resins have low melting points, which limits their application in high temperature fields. By partially introducing aromatic structures, such as aromatic diacids or aromatic diamines, the melting temperature of polyamide resins can be further increased, thereby increasing the use temperature of polyamide resins. A common way ...

Claims

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Application Information

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IPC IPC(8): C08G69/30C08G69/12B01J4/00B01J19/00B01J19/20
CPCC08G69/30C08G69/265C08G69/12B01J4/007B01J19/0053B01J19/20
Inventor 程圣利李雪婷孔祥福刘建明
Owner SHANDONG GUANGYIN NEW MATERIALS
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