High-purity nylon 5X salt and purification method thereof

A purification method and nylon technology, applied in the separation/purification of carboxylic acid compounds, amino compound purification/separation, organic chemistry, etc., can solve problems such as affecting the mechanical properties of nylon and limiting the growth of nylon molecular weight.

Pending Publication Date: 2020-10-27
CATHAY R&D CENT CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method uses ethanol as a solvent, and alcohols and dibasic acids inevitably undergo esterification reactions to generate dibasic acid esters. This impurity is difficult to remove from nylon salts, and residual

Method used

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  • High-purity nylon 5X salt and purification method thereof
  • High-purity nylon 5X salt and purification method thereof

Examples

Experimental program
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Example Embodiment

[0073] Preparation Example 1

[0074] Refer to CN201410004636.3 and CN201810022432.0, pass the lysine fermentation broth through a ceramic membrane to obtain a pure lysine collection solution. After deamination, react with adipic acid and lysine to form a lysine adipate solution , Control the pH of the reaction solution between 5-7. The lysine decarboxylase fermentation broth after the culture is added to the processed lysine adipate feed solution, and the added amount of the lysine decarboxylase fermentation broth is 8 wt.% of the lysine adipate. The pH of the conversion process was controlled at 7.1, and it was controlled by adding adipic acid solid to convert it into an aqueous solution of pentanediamine adipate. The aqueous solution of pentanediamine adipate was filtered through a ceramic membrane to obtain nylon 56 salt feed solution. Then, the nylon 56 salt feed liquid was added to the activated carbon of 3 wt.% of the total lysine in the lysine fermentation broth for deco...

Example Embodiment

[0076] Preparation Example 2

[0077] With reference to CN201410790873.7, the crude nylon 56 salt was prepared using commercially available 1,5-pentanediamine and adipic acid as raw materials.

Example Embodiment

[0078] Example 1

[0079] The crude nylon 56 prepared in Preparation Example 1 was added to a 100-liter enamel reactor, and 95 wt.% ethanol aqueous solution was added to obtain a nylon 56 salt mixture. The weight of the nylon 56 salt crude product in the nylon 56 salt mixture The fraction is 54%. The temperature is increased to 66℃ to dissolve the above mixture, and it is kept at this temperature for 0.5h until the solution becomes transparent. The temperature is lowered at a rate of 5min / ℃ to the precipitation temperature of 60℃. At this time, solid particles are precipitated in the solution by naked eyes After the temperature is kept for 1 hour, the particles in the solution continue to increase. After the temperature is kept, the temperature is reduced to 30 degrees at a rate of 5 min / ℃. After the temperature is kept for 1 hour, the crystal slurry is directly centrifuged. After liquid-solid separation, double the amount (relative to nylon 56 salt crude product weight) 95% etha...

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Abstract

The invention relates to a high-purity nylon 5X salt and a preparation method thereof, wherein the purity of the nylon 5X salt reaches 99.5% or above, and the nylon 5X salt can be directly used for polymerization. According to the preparation method of the nylon 5X salt provided by the invention, pentamethylene diamine and nylon salt production processes are coupled together, and the nylon salt isproduced by a one-step method, so that the tedious and complex process flow is omitted, the equipment investment is reduced, and the production cost is saved; and the method provided by the inventionsolves the problem of low yield of nylon salt crystallization products by an aqueous solution method, the crystallization process is more effectively controlled, and explosion nucleation is avoided.

Description

technical field [0001] The invention belongs to the technical field of industrial crystallization, and in particular relates to a high-purity nylon 5X salt and a preparation method thereof. Background technique [0002] Polyamide, commonly known as nylon, is an important engineering plastic and textile fiber material. It is widely used in machinery, automobiles, electrical appliances, textile equipment, chemical equipment, aviation, metallurgy and other fields due to its excellent mechanical properties. At present, the monomers used in the production of nylon are mainly prepared by chemical methods, and the raw materials are derived from fossil energy. However, with the increasing shortage of fossil energy and the increasing awareness of environmental protection, the development of new chemical materials that use biomass as raw materials , in line with the overall goal of sustainable human development. In recent years, the technology of biological production of long-chain d...

Claims

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Application Information

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IPC IPC(8): C07C211/09C07C209/84C07C51/42C07C51/43C07C55/10C07C55/14C07C55/20C07C55/21C07C55/02
CPCC07C211/09C07C209/84C07C51/42C07C51/43C07C55/10C07C55/14C07C55/20C07C55/21C07C55/02
Inventor 董华董筱雯杨晨刘修才
Owner CATHAY R&D CENT CO LTD
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