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Semi-aromatic transparent polyamide preparation method and semi-aromatic transparent polyamide

A semi-aromatic and polyamide technology, applied in the field of polyamide preparation, can solve problems such as difficulty in controlling the molar ratio of raw materials

Inactive Publication Date: 2017-07-04
CHANGSHU RES INST OF DALIAN UNIV OF TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of semi-aromatic transparent polyamide, which can solve the technical problem that it is difficult to control the molar ratio of raw materials in the preparation of polyamide by direct condensation polymerization in the prior art

Method used

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Examples

Experimental program
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preparation example Construction

[0018] The present invention provides a kind of preparation method of semi-aromatic transparent polyamide, it is characterized in that, comprises the following steps:

[0019] (1) dissolving the aromatic dicarboxylic acid and the alicyclic diamine in a polar aprotic solvent and carrying out an acid-base neutralization reaction to obtain a mixed solution containing polyamide salt;

[0020] (2) separating and purifying the mixed solution containing polyamide salt to obtain powdered polyamide salt;

[0021] (3) Polymerize the powdered polyamide salt to obtain a semi-aromatic transparent polyamide,

[0022] Wherein, the polymerization reaction is divided into three stages, and the reaction conditions are respectively:

[0023] In the first stage, the pressure is 0.5-2MPa, the temperature is 175-245°C, and the reaction time is 1-5h;

[0024] In the second stage, the pressure is 0.1-1.2MPa, the temperature is 185-260℃, and the reaction time is 1-5h;

[0025] In the third stage, t...

Embodiment approach

[0030] As a more preferred embodiment of the present invention, the above-mentioned alicyclic diamines are cyclohexanediamine and 4,4-diamino-dicyclohexylmethane, and cyclohexanediamine and 4,4-dicyclohexylmethane The molar ratio of amino-dicyclohexylmethane is preferably 1:(4-10). In this preferred embodiment, the alicyclic polycyclic diamine 4,4-diamino-dicyclohexylmethane and the alicyclic monocyclic diamine cyclohexanediamine are used together to obtain two semi-aromatic The semi-aromatic transparent polyamide obtained by condensation polymerization of these two polyamide salts has high light transmittance and good heat resistance.

[0031] In the preparation method according to the present invention, first make aromatic dicarboxylic acid and alicyclic diamine dissolve in polar aprotic solvent and carry out acid-base neutralization reaction, wherein aromatic dicarboxylic acid and alicyclic The aromatic diamines can be dissolved in the same or different polar aprotic solve...

Embodiment 1

[0040] This example is used to illustrate the preparation method of the present invention and the prepared semi-aromatic transparent polyamide.

[0041] Dissolve 0.5mol of terephthalic acid in dimethyl sulfoxide at 50°C; then dissolve 0.5mol of 3,3-dimethyl-4,4-diamino-dicyclohexylmethane in dimethylsulfoxide at 50°C Add the terephthalic acid solution into the reaction kettle, stir, keep the temperature at 50°C, then add the diamine solution, react for 4 hours, cool down, filter, wash and dry to obtain the semi-aromatic poly Amide salt, yield 96.9%.

[0042] Put the obtained semi-aromatic polyamide salt into a stirred reactor, blow argon to 0.5Mpa, stir and raise the temperature to 245°C, react for 5 hours, slowly release the gas to a pressure of 0.1MPa, and raise the temperature to 260°C. React for 1 hour, vacuumize the system until the vacuum degree is 0.1Mpa, react for 0.5h, pressurize and discharge, and the colorless transparent melt flowing out is the semi-aromatic trans...

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Abstract

The present invention discloses a semi-aromatic transparent polyamide preparation method and semi-aromatic transparent polyamide. According to the present invention, an acid-alkali neutralization reaction is performed in a polar aprotic solvent, the reaction product semi-aromatic polyamide salt has poor solubility in the polar aprotic solvent, and the product polyamide salt can be precipitated from the reaction mixing liquid after the reaction, such that the semi-aromatic transparent polyamide salt is easily separated from the reaction mixing liquid, and the purity of the semi-aromatic transparent polyamide salt is high; the solid semi-aromatic transparent polyamide salt is subjected to the polymerization reaction, such that the problem that the reaction raw material ratio is difficult to control in the prior art is solved; and the polymerization reaction of the invention is divided into three stages such as the pressurization reaction stage, the normal pressure reaction stage and the pressure reducing reaction stage, wherein the condensation polymerization reaction by-product can be smoothly removed from the reaction system in the pressure reducing reaction stage, such that the reaction balance can easily move to the forward direction so as to obtain the high molecular weight semi-aromatic transparent polyamide.

Description

technical field [0001] The invention relates to the field of polyamide preparation, in particular to a method for preparing semi-aromatic transparent polyamide and the prepared semi-aromatic transparent polyamide. Background technique [0002] Polyamide (polyamide, PA), commonly known as nylon, has a history of more than 80 years since its industrialization in the 1930s. In the early stage, it was mainly used as raw material for spinning, and it was used as engineering plastics after the 1950s. With the rapid development of the automotive industry, electronics, transportation, machinery, aerospace and various daily industries, its production and demand The volume already ranks first among the five major engineering plastics. General transparent polymers are difficult to meet the requirements when they are used in harsh conditions, such as high temperature, high pressure, and the presence of organic solvents. Transparent polyamides are characterized by their excellent mechan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/26C08G69/28
CPCC08G69/26C08G69/28
Inventor 郑玉斌李丽丽
Owner CHANGSHU RES INST OF DALIAN UNIV OF TECH CO LTD
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