Purification and refining method of tridecanedioic acid

A technology of tridecanedioic acid and purification method, which is applied in the separation/purification of carboxylic acid compounds, preparation of carboxylate salts, chemical instruments and methods, etc. It can improve the purity, reduce the generation of salt, and achieve the effect of good color and luster.

Active Publication Date: 2016-08-24
山东广通新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] ①.Because methanol is easy to undergo esterification reaction with the solute tridecanedioic acid under acidic and heating conditions, adding new impurities and increasing the load of purification
[0011] 3. Using acetic acid as a solvent, there is a problem that acetic acid remains relatively large in the filtrate and the product yield is not high
[0012] 4. Both acetic acid and methanol are volatile and cause environmental pollution

Method used

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  • Purification and refining method of tridecanedioic acid
  • Purification and refining method of tridecanedioic acid
  • Purification and refining method of tridecanedioic acid

Examples

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Embodiment 1

[0063] The refining method for improving the purity and yield of tridecanedioic acid of the present invention includes the following operation steps:

[0064] ①.. Adsorption and decolorization

[0065] Put 1000 parts by weight of deionized water into the dissolving reactor, add 180 parts by weight of crude tridecanedioic acid in a dry amount under stirring, add 110 parts by weight of sodium hydroxide aqueous solution with a mass concentration of 30.3%, and heat up to 100°C , The pH value is controlled between 6.0, after the material is completely dissolved, add 3 parts by weight of coconut shell-type activated carbon, keep the temperature and decolorize for 20 minutes;

[0066] ②.. Decolorization by oxidation

[0067] The material after step ① is filtered while it is hot, the filter cake is washed with 90℃ hot water, the filtrate and the washing liquid are put into the oxidation decolorization reactor together, and the temperature is raised to 98℃, and at this temperature, the tempera...

Embodiment 2

[0078] The refining method for improving the purity and yield of tridecanedioic acid of the present invention includes the following operation steps:

[0079] ①.. Adsorption and decolorization

[0080] In the dissolution reactor, put in 1000 parts by weight of deionized water, add 180 parts by weight of crude tridecanedioic acid in a dry amount under stirring, and add 110 parts by weight of sodium hydroxide aqueous solution with a mass concentration of 30.3%, and heat to 101°C , The pH value is controlled between 6.1, after the material is completely dissolved, add 4 parts by weight of coconut shell-type activated carbon, keep heat and decolorize for 30 minutes;

[0081] ②.. Decolorization by oxidation

[0082] Filter the material processed in step ① while it is hot, and rinse the filter cake with 85°C hot water. Put the filtrate and the rinse solution into the oxidation decolorization reactor, and heat to 99°C, and at this temperature, control the temperature to 5~ Within 10 minutes...

Embodiment 3

[0093] The refining method for improving the purity and yield of tridecanedioic acid of the present invention includes the following operation steps:

[0094] ①.. Adsorption and decolorization

[0095] In the dissolution reactor, put in 1000 parts by weight of deionized water, add 180 parts by weight of crude tridecanedioic acid on a dry basis under stirring, add 110 parts by weight of sodium hydroxide aqueous solution with a mass concentration of 30.3%, and heat up to 102°C , The pH value is controlled between 6.2, after the material is completely dissolved, add 5 parts by weight of coconut shell type activated carbon, heat preservation and decolorization for 25 minutes;

[0096] ②.. Decolorization by oxidation

[0097] The material treated in step ① is filtered while it is hot, the filter cake is rinsed with 88°C hot water, the filtrate and the rinse solution are put into the oxidation decolorization reactor, the temperature is raised to 100°C, and at this temperature, the temperatu...

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Abstract

The invention discloses a method for purifying and refining brassylic acid, and belongs to purification treatment of loop-free dicarboxylic acid with 13 carbon atoms. The method is characterized by comprising the following steps: with a brassylic acid crude product produced by a microbiological fermentation method as an initial raw material, and water as a dissolving solvent, carrying out alkali dissolution at 100-102 DEG C under the condition that the pH value is 6.0-6.2, so as to prepare a brassylic acid crude product water solution; after double decoloration of adsorption and oxidation, carrying out acid precipitation and crystallization at 98-102 DEG C; and finally preparing a cataphracted high-purity brassylic acid product. The method for purifying and refining the brassylic acid disclosed by the invention is good in color and luster, high in purity, high in refining yield, low in equipment investment, and simple and convenient to operate; resources are saved; environmental protection is facilitated; the purifying yield of the brassylic acid is greater than or equal to 98.4%; and the brassylic acid is suitable for condensation polymerization together with diamine as a polycondensation monomer, so as to synthesize long carbon chain nylon, and also is suitable for raw materials of synthesizing spices and medicines.

Description

Technical field [0001] The invention is a method for purifying and refining tridecanedioic acid. It belongs to the purification treatment of acyclic dicarboxylic acids with 13 carbon atoms. Background technique [0002] Tridecanedioic acid is an industrial product developed earlier in the long-chain dibasic acid. Mainly used to synthesize polymer materials, spices, medicines, etc. For example, as the main raw material for the synthesis of muscone, the raw material for the synthesis of high-performance lubricants with special performance requirements and long carbon chain dibasic acid dibasic esters, the synthesis of high-performance polyamide hot-melt adhesive condensation monomers, and as condensation monomers Polycondensation reaction with diamines to synthesize long carbon chain nylon (also known as polyamide resin) engineering plastics, etc., which are used in many fields. [0003] Nylon is a type of polymer compound containing amide group (-NHCO-) ​​on the molecular backbon...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C55/02C07C51/42C07C51/47C07C51/487C07C51/43
CPCC07C51/43C07C51/47C07C51/487C07C55/02
Inventor 郝本清
Owner 山东广通新材料有限公司
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