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Preparation method of long-chain semi-aromatic nylon salt

A semi-aromatic nylon, long-chain technology, used in the preparation of carboxylates, the preparation of amino compounds from amines, organic chemistry, etc., can solve the problems of difficulty in obtaining nylon salts, difficult to determine the reaction end point, and low solubility, and achieve easy separation. and purification, reducing energy consumption, and the effect of low reaction temperature

Inactive Publication Date: 2010-11-10
ZHUZHOU TIMES NEW MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There are following problems in the existing nylon salt preparation technology: 1. when using water or ethanol as solvent to prepare semi-aromatic nylon salt, aromatic dibasic acid and nylon salt have less solubility in these solvents, and it is difficult to obtain the required molar ratio. Nylon salt; 2. When dimethylformamide or N-methylpyrrolidone is selected as the solvent to prepare semi-aromatic nylon salt, because the prepared nylon salt is insoluble in the solvent within the neutralization reaction temperature range, it is difficult to determine the end point of the reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Dissolve 1.661Kg (10mol) terephthalic acid in 1.661Kg dimethyl sulfoxide solvent at 70°C; then dissolve 1.723Kg (10mol) decanediamine in 1.378Kg dimethyl sulfoxide solvent at 70°C ;First add the terephthalic acid solution into the reaction kettle, start stirring, and keep the temperature at 70°C, then gradually add the decanediamine solution into the reaction kettle, after the addition, react for 1 hour, adjust the pH to 7.2~7.4, After reacting for another 0.5h, it was cooled to room temperature (~25°C), centrifuged, washed, and dried to obtain 3.196Kg of 10T salt, with a yield of 94.3%.

Embodiment 2

[0026] Dissolve 1.661Kg (10mol) isophthalic acid in 1.661Kg dimethyl sulfoxide solvent at 60°C; then dissolve 1.723Kg (10mol) decanediamine in 1.378Kg dimethyl sulfoxide solvent at 70°C ; First add the isophthalic acid solution into the reaction kettle, start stirring, and keep the temperature at 60°C, then gradually add the decane diamine solution into the reaction kettle, after the addition, react for 1 hour, adjust the pH to 7.2~7.4, After reacting for another 0.5h, it was cooled to room temperature (~25°C), centrifuged, washed, and dried to obtain 3.264Kg of 10I salt, with a yield of 96.4%.

Embodiment 3

[0028] Dissolve 1.942Kg (10mol) terephthalic acid in 2.531Kg dimethyl sulfoxide solvent at 75°C; then dissolve 1.723Kg (10mol) decanediamine in 1.378Kg dimethyl sulfoxide solvent at 70°C ; First add the terephthalic acid solution into the reaction kettle, start stirring, and keep the temperature at 70°C, then gradually add the decane diamine solution into the reaction kettle, after the addition, react for 1 hour, adjust the pH to 7.2-7.4, After reacting for another 0.5h, it was cooled down to room temperature (~25°C), centrifuged, washed and dried to obtain 3.384Kg of 10P salt with a yield of 97.1%.

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PUM

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Abstract

The invention discloses a preparation method of long-chain semi-aromatic nylon salt. The method comprises the following steps: firstly, respectively dissolving aromatic dibasic acid and long-chain diamine in an organic solvent under the temperature of 60-80 DEG C, then slowly adding the long-chain diamine into aromatic dibasic acid solution to carry out neutral reaction under the temperature of 60-80 DEG C, adjusting pH value to 7.2-7.4, cooling, separating, washing with the organic solvent, and drying to obtain the long-chain semi-aromatic nylon salt. The long-chain semi-aromatic nylon salt prepared by the invention has higher purity, the speed of the neutral reaction can be controlled, and simultaneously the molar ratio of dibasic acid and diamine can be controlled; the neutral reaction temperature of the organic solvent selected by the invention is lower, the obtained long-chain semi-aromatic nylon salt can be partially dissolved in the organic solvent at the neutral reaction temperature, and is not dissolved in the organic solvent under normal temperature, so as to be convenient to adjust the pH value, separate and purify; and the used organic solvent can be used circularly.

Description

technical field [0001] The invention relates to a preparation and production method of long-chain semi-aromatic nylon salt. Background technique [0002] Nylon has excellent mechanical strength, wear resistance, self-lubrication and good corrosion resistance. It is widely used in electronic appliances, automobile industry, construction machinery, fiber and other fields. It is one of the important engineering plastics, and its output ranks among the top five projects. Plastic first. [0003] In recent years, in order to meet the higher performance requirements in the fields of electronics, electrical appliances, automobiles, etc., especially the rapid development of surface mount technology and the promotion of lead-free soldering, PBT and PA66 cannot meet the requirements, high temperature resistant nylon PA46, PA6T , HTN and PA9T, PA10T, PA12T, etc. have been developed one after another. [0004] When synthesizing nylon, in order to facilitate the control of the molar rat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/68C07C51/41C07C211/09C07C63/28C07C63/24C07C57/34C07C63/333C07C63/38C08G69/26
Inventor 王文志刘爱学宋传江邓凯桓张英伟
Owner ZHUZHOU TIMES NEW MATERIALS TECH
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