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Method for synthesizing semi-aromatic nylon salt by using mixed solvent

A semi-aromatic nylon and mixed solvent technology is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc. The effect of high usage and high purity

Active Publication Date: 2015-05-20
JIANGMEN DENGZHONGTAI ENG PLASTICS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the use of organic solvents can effectively avoid the possibility of salt-encapsulated acid, the long carbon chain semi-aromatic nylon salts produced by the reaction are in powder form, which brings troubles to the separation and purification of nylon salts and organic solvents in the later stage.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Mix 116g (1mol) of hexamethylenediamine with 50g of water and heat up to 60°C for later use;

[0023] (2) Take 166g (1mol) of terephthalic acid and 350g DMSO and raise the temperature to 80°C, dissolve and clarify for later use;

[0024] (3) Slowly add the solution obtained in step (2) into the solution obtained in step (1), and control the reaction temperature at 75°C;

[0025] (4) Use a small amount of terephthalic acid or hexamethylenediamine dissolved in DMSO to adjust the pH value of the solution to 7.0-7.2, and stabilize for 1 hour;

[0026] (5) Cool down to room temperature, perform centrifugation, wash the obtained solid with deionized water, and dry to obtain 274g of 6T salt with a yield of 97.2%.

Embodiment 2

[0028] (1) Mix 172g (1mol) of decanediamine with 500g of water and heat up to 60°C for later use;

[0029] (2) Mix 166g (1mol) isophthalic acid with 300g DMF and heat up to 80°C, dissolve and clarify for later use;

[0030] (3) Slowly add the solution obtained in step (2) into the solution obtained in step (1), and control the reaction temperature at 65°C;

[0031] (4) Adjust the pH value to 7.0-7.2 with a small amount of terephthalic acid or decanediamine dissolved in DMF, and stabilize for 1 hour;

[0032] (5) Cool down to room temperature, perform centrifugation, wash the obtained solid with deionized water, and dry to obtain 324 g of 10I salt with a yield of 95.9%.

Embodiment 3

[0034] (1) Mix 202g (1.01mol) of dodecanediamine with 550g of water and raise the temperature to 95°C for later use;

[0035] (2) Take 166g (1mol) of terephthalic acid and 200g of NMP and raise the temperature to 80°C, dissolve and clarify for later use;

[0036] (3) Slowly add the solution obtained in step (2) into the solution obtained in step (1), and control the reaction temperature at 95°C;

[0037] (4) Adjust the pH value of the solution to 7.0-7.2 with a small amount of terephthalic acid or dodecanediamine dissolved in NMP, and stabilize for 1 hour;

[0038] (5) Cool down to room temperature, perform centrifugation, wash the obtained solid with deionized water, and dry to obtain 355.71 g of 12T salt, with a yield of 97.19%.

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Abstract

The invention discloses a method for synthesizing a semi-aromatic nylon salt by using a mixed solvent composed of water and an organic solvent. The method comprises the steps: mixing aliphatic diamine and water, pulping, and heating the aliphatic diamine solution to 60-98 DEG C, and remaining the aliphatic diamine solution for later use; mixing aliphatic diacid and an organic solution, heating the aliphatic diacid solution to 60-120 DEG C until the aliphatic diacid is completely dissolved, and remaining the aliphatic diacid solution for later use; slowly adding the aliphatic diacid solution into the aliphatic diamine solution, and carrying out neutral reaction at the temperature of 60-98 DEG C; and regulating the pH value to 7.0-7.5, then, cooling, centrifugally separating, washing by using deionized water, and drying to obtain the semi-aromatic nylon salt. The semi-aromatic nylon salt prepared by using the method disclosed by the invention is high in purity, favorable in particle crystal form, easy to separate and purify, low in consumption of organic solvent, mild in reaction condition and low in energy consumption. The organic solvent used in the method can be recycled.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for synthesizing semi-aromatic nylon salts using a mixed solvent. Background technique [0002] Semi-aromatic nylon resin has excellent mechanical strength, self-lubrication, wear resistance, heat resistance, and good corrosion resistance to chemicals. It is between general engineering plastic nylon and high temperature resistant nylon plastic PEEK. High thermal resin. [0003] In recent years, in order to meet the higher performance requirements in the fields of automobiles, electronics, and electrical appliances, polyamides with high heat resistance such as PA46, PA6T, PA9T, PA10T, and PA12T have been developed. With the enhancement of people's awareness of environmental protection and the relevant national regulations on automobile exhaust emissions, automobile manufacturers are required to reduce exhaust emissions and improve engine efficiency to reduce...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/12C07C211/09C07C209/00C07C63/28C07C63/24C07C51/41C08G69/26
Inventor 曾建平金良文严燕
Owner JIANGMEN DENGZHONGTAI ENG PLASTICS CO LTD
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