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Method for purifying and refining brassylic acid

A tridecanedioic acid and refining method technology, applied in the separation/purification of carboxylic acid compounds, carboxylate preparation, chemical instruments and methods, etc., can solve the problem of acetic acid and methanol being volatile, increasing the load of purification, and product yield. It can improve the purity, reduce the generation of salt, and improve the color and luster.

Active Publication Date: 2015-04-08
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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  • Method for purifying and refining brassylic acid
  • Method for purifying and refining brassylic acid
  • Method for purifying and refining brassylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] A kind of refining method of improving tridecanedioic acid purity and yield of the present invention comprises the following steps:

[0064] ①.. Adsorption decolorization

[0065] In the dissolution reactor, put 1000 parts by weight of deionized water, add 180 parts by weight of crude tridecanedioic acid in dry weight 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, and keep warm for 20 minutes for decolorization;

[0066] ②..oxidative decolorization

[0067] Filter the material treated in step ① while it is hot, rinse the filter cake with hot water at 90°C, put the filtrate and flushing liquid into the oxidation decolorization reaction kettle, raise the temperature to 98°C, and control it at 5~ Within 10 minutes, add hydrogen peroxide w...

Embodiment 2

[0078] A kind of refining method of improving tridecanedioic acid purity and yield of the present invention comprises the following steps:

[0079] ①.. Adsorption decolorization

[0080] In the dissolution reactor, put 1000 parts by weight of deionized water, add 180 parts by weight of crude tridecanedioic acid in dry weight under stirring, add 110 parts by weight of sodium hydroxide aqueous solution with a mass concentration of 30.3%, and heat up 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, and keep warm for 30 minutes for decolorization;

[0081] ②..oxidative decolorization

[0082] Filter the material treated in step ① while it is hot, rinse the filter cake with hot water at 85°C, put the filtrate and flushing liquid into the oxidation decolorization reaction kettle, raise the temperature to 99°C, and control it at 5~ Within 10 minutes, add hydrogen peroxide w...

Embodiment 3

[0093] A kind of refining method of improving tridecanedioic acid purity and yield of the present invention comprises the following steps:

[0094] ①.. Adsorption decolorization

[0095] In the dissolution reactor, put 1000 parts by weight of deionized water, add 180 parts by weight of crude tridecanedioic acid in dry weight 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, and keep warm for 25 minutes for decolorization;

[0096] ②..oxidative decolorization

[0097] Filter the material treated in step ① while it is hot, rinse the filter cake with hot water at 88°C, put the filtrate and flushing liquid into the oxidation decolorization reaction kettle, raise the temperature to 100°C, and control the temperature at 5~ Within 10 minutes, add hydro...

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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 tridecanedioic acid. Purification of acyclic dicarboxylic acids with 13 carbon atoms. Background technique [0002] Tridecanedioic acid is an industrial product developed earlier among long-chain dibasic acids. It is mainly used in the synthesis of polymer materials, spices, medicines, etc. For example, as the main raw material for the synthesis of musk ketone, the raw material for the synthesis of high-performance lubricants with long carbon chain dibasic acid dibasic esters with special performance requirements, the synthesis of high-performance polyamide hot-melt adhesive condensation monomers, and as polycondensation monomers Polycondensation reaction with diamine to synthesize long carbon chain nylon (also known as polyamide resin) engineering plastics, etc., which have been applied in many fields. [0003] Nylon is a class of polymer compounds containing amide groups (-NHCO-) ​​in the main chain of the m...

Claims

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Application Information

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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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