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Method for refining dodecanedioic acid

A dodecanedioic acid and refining method technology, which is applied in the field of chemical product preparation, can solve the problems of low total acid content, low product purity, and poor quality of dodecanedioic acid products, so as to increase the content and reduce the ester content Effect

Active Publication Date: 2012-11-28
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

[0005] The production of dodecanedioic acid by using alcohol as a solvent to refine biological fermentation or enzymatic method has been of poor quality for a long time. Titration) is low at 97.8wt.%, and the product contains a small amount of long-chain dibasic acid ethyl ester, which is 1.2wt.%, which affects the use of polyamide as a raw material

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 400kg of common dodecanedioic acid and 3kg of coconut shell activated carbon into 1000L90wt.% edible alcohol, in 2m 3 Mix slurry in glass-lined decolorization kettle, heat up to 65°C, 30m 2 Box-type undercurrent plate and frame pressure filtration, the filtrate is filtered through a precision filter to the crystallization tank, cooled to crystallize, cooled to 25°C, centrifuged, and the centrifuged material is put into a clean glass-lined low-temperature washing tank, and 200L95wt.%, 15°C alcohol is added , stirred evenly, and centrifuged twice, and the centrifuged material was put into a double-cone vacuum dryer for drying, the material temperature was controlled at 45°C±1°C, the vacuum degree was -0.085~-0.10MPa, and dried until the moisture content was lower than 0.1wt.%. After drying, 328kg of refined acid was obtained. Gas chromatographic determination of product single acid content 99.17wt.%, neutralization titration determination of total acid content 99.5wt...

Embodiment 2

[0025] Add 200kg of common dodecanedioic acid and 1.5kg of coconut shell activated carbon into 500L 95wt.% edible alcohol, in 1m 3 Mix slurry in glass-lined decolorization kettle, heat up to 72°C, 30m 2 Box-type undercurrent plate and frame pressure filtration, the filtrate is filtered through a precision filter to the crystallization tank, cooled to crystallize, cooled to 25°C, centrifuged, and the centrifuged material is put into a clean glass-lined low-temperature washing tank, and 100L 90wt.% is newly distilled Cool down to 20°C with alcohol, stir evenly, and centrifuge twice. The centrifuged material is put into a double-cone vacuum dryer for drying. The material temperature is controlled at 50°C±1°C, the vacuum degree is -0.085~-0.10MPa, and dried until the moisture content is lower than 0.1 wt.%, finish drying, get refined acid 161kg. The single acid content of the product was determined by gas chromatography to be 99.10wt.%, the total acid content was determined to be...

Embodiment 3

[0027] Add 800kg of common dodecanedioic acid and 5kg of coconut shell activated carbon into 2000L 95wt.% edible alcohol, in 3m 3 Mix slurry in glass-lined decolorization kettle, heat up to 75°C, 30m 2 Box-type undercurrent plate and frame pressure filtration, the filtrate is filtered through a precision filter to the crystallization tank, cooled to crystallize, cooled to 25°C, centrifuged, and the centrifuged material is put into a clean glass-lined low-temperature washing tank, and 400L95wt.%, 18°C ​​alcohol is added , stirred evenly, centrifuged twice, and the centrifuged material was put into a double-cone vacuum dryer for drying. The temperature of the material was controlled at 48°C±1°C, and the vacuum was -0.085~-0.10MPa. Dry until the moisture content was lower than 0.1wt.%, and the drying was completed. , 661kg of refined acid was obtained. The single acid content of the product was determined by gas chromatography to be 99.10%, the total acid content was determined ...

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Abstract

The invention relates to a method for refining dodecanedioic acid and belongs to the technical field of preparation of chemical products. According to the method, the dodecanedioic acid is refined by using dodecanedioic acid produced by a biological fermentation method or an enzyme method as a raw material and alcohol as a solvent. The method particularly comprises the following steps: mixing the dodecanedioic acid and the alcohol; heating and decoloring, wherein heat is not preserved after heating to a certain temperature in the decoloring process; directly filtering; cooling, crystallizing and centrifuging the filtrate to obtain a centrifugal material; washing the centrifugal material with the alcohol; performing secondary centrifugation; and vacuum drying to obtain the dodecanedioic acid refined product. According to the method, the problem about the product quality of the dodecanedioic acid refined by the alcohol is solved, the single acid content and the total acid content of the dodecanedioic acid product are increased, and the ester content is reduced.

Description

technical field [0001] The invention relates to a method for refining dodecanedioic acid, which belongs to the technical field of chemical product preparation. Background technique [0002] Long-chain dibasic acid is an important fine chemical raw material, which can be used in the synthesis of spices, hot melt adhesives, engineering plastics and liquid crystals, etc., and is widely used. [0003] At present, long-chain dibasic acids are mainly produced by microbial fermentation, and the refining methods include refining with glacial acetic acid as a solvent and refining with alcohol as a solvent. [0004] A small amount of monobasic acid remains in the refined dodecanedioic acid product of glacial acetic acid, which will cause yellowing of the product and short chains during polymerization when producing polyamide products. [0005] The production of dodecanedioic acid by using alcohol as a solvent to refine biological fermentation or enzymatic method has been of poor qual...

Claims

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Application Information

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IPC IPC(8): C07C55/21C07C51/42
Inventor 苏庆旺尹海顺高丽丽
Owner 山东广通新材料有限公司
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