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Purification method of dodecanedioic acid

A technology for crude dodecanedioic acid and dodecanedioic acid, which is applied in the field of purification of dodecanedioic acid, and can solve the problems of reducing the yield of dodecanedioic acid, volatilization of acetic acid and methanol, and increasing the load of purification, etc. Problems, to achieve the effect of environmental protection, improve purity, reduce the generation of salt

Active Publication Date: 2016-03-02
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

[0010] ①.Because methanol is easy to undergo esterification reaction with solute dodecanedioic acid under acidic and heating conditions, adding new impurities and increasing the load of purification
Reduced yield of dodecanedioic acid
[0011] ②. Due to the high solubility of dodecanedioic acid in methanol, a small amount of dodecanedioic acid product is always dissolved in the solvent during the recrystallization process, resulting in low product yield and high production cost
[0012] 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
[0013] 4. Both acetic acid and methanol are volatile and cause environmental pollution

Method used

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  • Purification method of dodecanedioic acid
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  • Purification method of dodecanedioic acid

Examples

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Effect test

Embodiment 1

[0064] A kind of refining method of improving dodecanedioic acid purity and yield of the present invention comprises the following steps:

[0065] ①.. Adsorption decolorization

[0066] In the dissolution reactor, put 1000 parts by weight of deionized water, add 180 parts by weight of crude dodecanedioic 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;

[0067] ②..oxidative decolorization

[0068] 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 with...

Embodiment 2

[0079] A kind of refining method of improving dodecanedioic acid purity and yield of the present invention comprises the following steps:

[0080] ①.. Adsorption decolorization

[0081] In the dissolution reactor, put 1000 parts by weight of deionized water, add 180 parts by weight of crude dodecanedioic 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;

[0082] ②..oxidative decolorization

[0083] 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 wit...

Embodiment 3

[0094] A kind of refining method of improving dodecanedioic acid purity and yield of the present invention comprises the following steps:

[0095] ①.. Adsorption decolorization

[0096] In the dissolution reactor, put 1000 parts by weight of deionized water, add 180 parts by weight of crude dodecanedioic 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;

[0097] ②..oxidative decolorization

[0098] 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 hydroge...

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Abstract

The invention relates to a purification method of dodecanedioic acid, belonging to purification treatment of cycle-free dicarboxylic acid with 12 carbon atoms. The method is characterized by comprising the following steps: by using a dodecanedioic acid crude product produced by microbial fermentation as an initial raw material and water as a dissolving solvent, carrying out alkali fusion at 100-102 DEG C under the condition of pH value of 6.0-6.2 to prepare a dodecanedioic acid crude product water solution; and after carrying out adsorption-oxidation dual decolorization, acidifying at 98-102 DEG C to crystallize, and finally, drying to obtain the scale-like high-purity dodecanedioic acid crystal product. The purification method of dodecanedioic acid has the advantages of favorable product color, high product purity, high refinement yield, equipment investment saving and resource saving, and is simple to operate and beneficial to environmental protection. The purification yield of the dodecanedioic acid is greater than or equal to 98.4%. The dodecanedioic acid is suitable to be used as a polycondensation monomer to perform polycondensation reaction with diamine to synthesize the long-carbon-chain nylon, and is also suitable to be used as a raw material of synthetic perfume and drugs.

Description

technical field [0001] The invention is a method for purifying dodecanedioic acid. It belongs to the purification treatment of acyclic dicarboxylic acids with 12 carbon atoms. Background technique [0002] Dodecanedioic acid (Dodecanedioic Acid) is also known as lauric acid. It is an industrial product developed earlier among long-chain dibasic acids. It is mainly used in the synthesis of polymer materials, spices, medicines, etc. Among them, it is one of the most important uses to synthesize long carbon chain nylon (also known as polyamide resin) engineering plastics through polycondensation reaction between polycondensation monomer and diamine. [0003] Nylon is a class of polymer compounds containing amide groups (-NHCO-) ​​in the main chain of the molecule. Because the molecular structure of nylon contains a large number of amide groups, and the end of the macromolecule is an amino or carboxyl group, it is a kind of crystalline polymer with strong polarity, hydrogen ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C55/21C07C51/42
CPCC07C51/42C07C51/43C07C51/47C07C55/21
Inventor 郝本清房宁
Owner 山东广通新材料有限公司
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