A kind of preparation method of nylon 65 salt

A technology of nylon and solution, which is applied in the field of preparation of nylon 65 salt, can solve the problems of concentration and purification that are difficult to judge the reaction end point, and achieve the effects of easy control of the reaction end point, convenient storage and transportation, and reduction of oxidative deterioration

Active Publication Date: 2020-04-03
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Aiming at the problems existing in the prior art, the present invention provides a preparation method of nylon 65 salt, which solves the technical problems of the difficult judgment of the reaction end point and the concentration and purification of the salt

Method used

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  • A kind of preparation method of nylon 65 salt
  • A kind of preparation method of nylon 65 salt

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Experimental program
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Effect test

Embodiment 1

[0030] The preparation method of the nylon 65 salt of the present embodiment, the steps are as follows:

[0031] (1) Weigh 13.20g (0.10mol) of glutaric acid and dissolve it in water to make a glutaric acid solution with a concentration of 45%, and heat it to 45°C; then take 11.60g (0.10mol) of hexamethylenediamine and dissolve it in water , form a hexamethylenediamine solution with a concentration of 55%, and heat to 45°C;

[0032] (2) Add the hexamethylenediamine solution dropwise to the glutaric acid solution at 1.2mL / min under stirring at a constant rate of 110r / min. During this process, the air is replaced three times by vacuuming and filling with nitrogen, and nitrogen is introduced for protection. Use a pH meter to monitor the pH in real time, control the pH to be stable at 7.30-7.50, and maintain the reaction time at 2.5 hours to make it fully react;

[0033] (3) After fully reacting, vacuum distillation was carried out under airtight conditions, and then nylon 65 salt...

Embodiment 2

[0036] The preparation method of the nylon 65 salt of the present embodiment, the steps are as follows:

[0037] (1) Weigh 13.20g (0.10mol) of glutaric acid and dissolve it in water to make a glutaric acid solution with a concentration of 50%, and heat it to 50°C; then take 11.68g (0.10mol) of hexamethylenediamine and dissolve it in water , form a hexamethylenediamine solution with a concentration of 55%, and heat to 50°C;

[0038] (2) Add the hexamethylenediamine solution dropwise to the glutaric acid solution at 1.3mL / min under stirring at a constant rate of 110r / min. During this process, the air in the solution is replaced three times by vacuuming and filling with nitrogen, and nitrogen is introduced for protection. Use a pH meter to monitor the pH in real time. The reaction time is maintained at 2.5 hours to allow it to fully react, and then the pH is stabilized at 7.30~7.50;

[0039](3) After fully reacting, vacuum distillation was carried out under airtight conditions, ...

Embodiment 3

[0042] The preparation method of the nylon 65 salt of the present embodiment, the steps are as follows:

[0043] (1) Weigh 39.60g (0.30mol) of glutaric acid and dissolve it in water to make a glutaric acid solution with a concentration of 45%, and heat it to 45°C; then take 34.80g (0.30mol) of hexamethylenediamine and dissolve it in In water, a hexamethylenediamine solution with a concentration of 55% is formed and heated to 45°C;

[0044] (2) Add the hexamethylenediamine solution dropwise to the glutaric acid solution at 1.2mL / min under stirring at a constant rate of 110r / min. During this process, the air in the solution is replaced by vacuuming and filling with nitrogen for three times and nitrogen is introduced for protection. Use a pH meter to monitor the pH in real time, control the pH to be stable at 7.30-7.50, and maintain the reaction time at 2.5 hours to make it fully react;

[0045] (3) After fully reacting, vacuum distillation was carried out under airtight conditi...

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Abstract

The invention discloses a preparation method of nylon 65 salt. Glutarate is dissolved in a solvent, the mixture is heated to 30-50 DEG C, and a glutarate solution is prepared; hexamethylendiamine is dissolved in a solvent, the mixture is heated to 30-50 DEG C, and a hexamethylendiamine solution is prepared; the hexamethylendiamine solution is dropwise added into the glutarate solution under constant rate stirring at the temperature of 30-50 DEG C, inert gas is introduced for protection, the pH value is monitored by a pH meter in real time, the pH value is controlled to range from 7.20 to 7.90,and the reaction is carried out for 1.5 h to 5.0 h; after the material completely reacts, reduced pressure distillation or direct suction filtration is carried out, and then nylon 65 salt is dried ina vacuum drying box for 24 h at the temperature of 60 DEG C; the dried nylon 65 salt is purified through a purification solvent, the nylon 65 salt is dried, and the pure nylon 65 salt sample is obtained. The prepared nylon 65 salt is high in yield, the pH value is monitored by the pH meter in real time in the reaction process, reaction monitoring is convenient, the reaction conditions are moderate, and operation is easy.

Description

technical field [0001] The invention belongs to the technical field of nylon salt preparation, and in particular relates to a preparation method of nylon 65 salt. Background technique [0002] Nylon resin (PA), also known as polyamide, is the most widely used material among the five major engineering plastics at home and abroad. Now the world's annual consumption has exceeded 10,000 tons. Nylon has good comprehensive properties, its strength is higher than that of metal, it has good mechanical properties, heat resistance, wear resistance, chemical resistance, flame retardancy and self-lubricating property, and it is easy to process, low friction coefficient, and is also suitable for glass Filled with fibers and other materials. [0003] In the automobile industry, nylon is used to manufacture radiator parts, engine cover parts, cylinder end covers, oil seal covers, fuel filters, water tank shells, heat-resistant radiator covers, water pump boxes, etc., which is in line with...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/26C08G69/28C08G69/46
CPCC08G69/26C08G69/28C08G69/46
Inventor 王训遒卢晶晶张雷
Owner ZHENGZHOU UNIV
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