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A kind of nylon salt and preparation method thereof

A technology of nylon salt and dibasic acid, which is applied in the field of nylon salt preparation, can solve the problems of high solubility of nylon salt, mild reaction conditions, and affecting the color of nylon, so as to speed up the rate of neutralization reaction, facilitate storage and transportation, The effect of increasing the degree of response

Active Publication Date: 2020-06-19
CATHAY R&D CENT CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, the above-mentioned existing solution-based nylon salt preparation technology has the following problems: when water is used as a solvent to prepare a nylon salt solution, because the solubility of nylon salt in an aqueous solution is relatively large, it is difficult to effectively obtain a nylon salt solid by cooling and crystallization. , and if concentrated crystallization is used, the product quality of nylon salt will deteriorate due to high temperature
Thereby the cost of preparing nylon salt by the aqueous solution of nylon salt is high and the quality is not stable
However, when organic solvents are used to prepare solid nylon salt, it is easy to cause organic solvent residues and involve the recovery of organic solvents, high energy consumption, large pollution, high cost, and is not a very ideal process.
[0008] Patent application CN 103201314A discloses a method for preparing nylon salt by reacting liquid diamine and powdery solid diacid under the condition of low water content. However, this method needs to mix the diamine and diacid at 100-210°C above the melting point of pentamethylenediamine. The reaction is carried out in the temperature range of ℃, the reaction conditions are not mild, and the nylon salt obtained under high temperature reaction will cause yellowing of nylon in the subsequent polymerization, affecting the color of nylon
In addition, this preparation method has restrictions on the reaction system, stirring method, reaction temperature, and diacid addition method. The process is cumbersome, and is limited by its liquid-solid reaction method. There are still amine residues in the final product
[0009] In summary, the existing methods for the preparation of nylon salts are difficult to directly obtain nylon salts with low diamine and diacid residues and no influence on subsequent nylon polymerization.

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0024] In order to achieve the above object, a preparation method of nylon salt comprises the following steps: mixing 1,5-pentanediamine, water and dibasic acid at 65-120°C to prepare the nylon salt, wherein the water The weight is 2-12wt% of the total weight of the 1,5-pentanediamine and the dibasic acid.

[0025] The invention prepares the nylon salt with less free amine content by adding a specific amount of water when preparing the nylon salt. If too little water is added, the nylon salt cannot be fully mixed and reacted, and there are too many residual amines, which will affect the quality of nylon. If too much water is added, after the salt formation is completed, the nylon salt solid cannot be directly obtained after cooling down, or the obtained solid is easy to harden, resulting in difficulty in transportation.

[0026] Wherein, the amount of water is such that the nylon salt is in a molten state at 65-120°C. The preparation method does not limit the order and manne...

Embodiment 1

[0050] The 100 liters of enamel salt-forming kettle was replaced by vacuuming and filling the air three times with nitrogen, and protected with nitrogen, and 22kg of 1,5-pentanediamine (purity 99.5%) and 1.3kg of water (accounting for 1 , 2.4% of the total weight of 5-pentamethylenediamine and adipic acid), the mixed solution of pentamethylenediamine and water is heated to 112°C, and 31.6kg of adipic acid (China Petroleum Liaoyang Petrochemical Company) is added thereto to keep the above temperature And under vigorous stirring, the reaction system becomes viscous, and the stirring is continued for 3 hours, and acid and amine are added in small amounts, so that the final pH of the nylon salt is 7.3.

[0051] Fill the polymerization kettle with nitrogen to a pressure of 0.2 MPa (gauge pressure), start to melt and discharge, and slice with a slicer to cool down, and the sample does not have the characteristic odor of pentamethylenediamine.

Embodiment 2

[0053] A 500 milliliter three-neck flask was replaced with air three times by vacuumizing and filling with nitrogen, and protected with nitrogen, and added 110 g of 1,5-pentanediamine (Shandong Kaisai Biotechnology Materials Co., Ltd.) and 8 g of water ( Accounting for 1,5-pentanediamine, 3% of the total weight of adipic acid), at 80°C, add 158g of adipic acid (China Petroleum Liaoyang Petrochemical Company), keep the above temperature and under strong stirring, the reaction system becomes viscous , Stirring continuously for 1 hour, the salt formation reaction is completed, and the nylon salt product is a viscous paste. Pour out the reaction product, let it stand to cool to room temperature, and slice it to obtain a solid nylon salt product. The sample does not have the characteristic odor of pentamethylenediamine.

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PUM

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Abstract

The present invention provides a method for preparing nylon salt, which comprises mixing 1,5-pentanediamine, water and dicarboxylic acid at a temperature of 65 to 120°C to obtain a nylon salt, wherein the amount of the water is 2% to 12% by weight based on the total weight of the 1,5-pentanediamine and the dicarboxylic acid. The present invention also provides a nylon salt. According to the present method for preparing nylon salt, the incomplete reaction between the 1,5-pentanediamine and the dicarboxylic acid, which is caused by the nylon salt present during the preparation in a solid state, can be avoided; the reaction between the 1,5-pentanediamine and the dicarboxylic acid can be significantly speeded up, and the reaction time is accordingly shorten. Consequently, the content of diamine and dicarboxylic acid remained in the resulting nylon salt is very low. In addition, the final nylon salt product, which present in a solid state, makes it easier to be stored and transported.

Description

technical field [0001] The invention relates to a nylon salt and a preparation method thereof, in particular to a preparation method of a nylon salt with less residual diamine and diacid. Background technique [0002] In the prior art, nylon is mainly synthesized by the polycondensation reaction of dibasic acid and diamine. In order to ensure the equimolar ratio of dibasic acid and diamine raw materials as much as possible, the dibasic acid and diamine are usually made into nylon salt first. , and then undergo polycondensation. Therefore, as the precursor of nylon polymer, the product quality of nylon salt has a great influence on the quality of nylon polymer. Qualified nylon salt is the basic prerequisite for producing high-quality nylon polymer. [0003] Nylon salts currently on the market include nylon salt solutions and nylon salt solids. Due to the high water content, long-distance transportation is economically uneconomical, and the nylon salt solution has poor stab...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/28C08G69/30
CPCC08G69/28C08G69/26
Inventor 杨晨秦兵兵郑毅刘驰李乃强刘修才
Owner CATHAY R&D CENT CO LTD
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