Method for continuously crystallizing long chain dicarboxylic acid

A long-chain dibasic acid and crystallization technology, applied in the field of chemical purification, can solve problems such as low production efficiency, unstable product quality, and high production costs

Pending Publication Date: 2019-06-28
CATHAY R&D CENT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The crystallization process in the prior art is generally directly linear or naturally cooled to the target temperature, and these methods have disadvantages such as low production efficiency, high production cost, and unstable product quality.

Method used

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  • Method for continuously crystallizing long chain dicarboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0101] According to the method disclosed in the patent document ZL200410018255.7, DC12 fermented liquid was prepared, the fermented liquid was added with 97% sulfuric acid by weight to adjust the pH value to 3.0, and heated to 80°C. Add butyl acetate containing 4 times the weight of the long-chain dibasic acid, stir, and directly extract the long-chain dibasic acid in the fermentation broth to the organic phase. Maintain 80° C., separate the organic phase, add 3% activated carbon to the organic phase for decolorization (relative to the weight ratio of the dibasic acid), and filter to obtain a clear liquid.

[0102] The butyl acetate solution enters the continuous crystallization device. The continuous crystallization device is equipped with stirring, and the stirring speed is 50 rpm. The first stage of the continuous crystallization device controls 68±1°C, with an average residence time of 2 hours; the second stage of the continuous crystallization device controls 60±2°C, wit...

Embodiment 2

[0105] According to the membrane filtration method disclosed in the patent document ZL200410018255.7, the DC12 membrane supernatant was prepared, and the liquid was added with 97% sulfuric acid to adjust the pH value to 3.0, filtered, and dried to obtain the crude long-chain dibasic acid. Add isoamyl acetate with 3 times the weight of long-chain dibasic acid, stir, keep the temperature at 90° C., add 3% activated carbon for decolorization (relative to the weight ratio of long-chain dibasic acid), and filter to obtain clear liquid.

[0106] The isoamyl acetate solution enters the continuous crystallization device. The continuous crystallization device is equipped with stirring, and the stirring speed is 50 rpm. The first-stage control of the continuous crystallization device is 72±1°C, with an average residence time of 2 hours; the second-stage control of the continuous crystallization device is 57±2°C, with an average residence time of 1 hour; the third-stage control of the co...

Embodiment 3

[0109] According to the membrane filtration method disclosed in the patent document ZL200410018255.7, the DC12 membrane supernatant was prepared, the solution was added with 97% sulfuric acid by weight to adjust the pH value to 3.0, filtered, washed, and dried to obtain the crude long-chain dibasic acid. Add isoamyl alcohol with 2.5 times the weight of long-chain dibasic acid, stir, keep the temperature at 75° C., add 3% activated carbon for decolorization (relative to the weight ratio of long-chain dibasic acid), and filter to obtain clear liquid.

[0110] The isoamyl alcohol solution enters the continuous crystallization device. The continuous crystallization device is equipped with stirring, and the stirring speed is 40 rpm. The first stage of the continuous crystallization device is controlled at 55±1°C, with an average residence time of 3 hours; the second stage of the continuous crystallization device is controlled at 48±2°C, with an average residence time of 1 hour; the...

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Abstract

The invention provides a method for continuously crystallizing long chain dicarboxylic acid and application of the method. The continuous crystallization method comprises the following steps: sequentially performing multi-stage crystallization, optimally three-stage crystallization, on an organic solution containing binary acid. Compared with an intermittent crystallization device, the crystallization method has the advantages of high industrial automatic degree and stable product quality on the premise that the same product quality is obtained; and the number of operators is greatly reduced,and the investment is saved by over 50 percent (1000 tons / annual product scale) than that of the intermittent crystallization device. Therefore, the method can be used for efficiently producing high-quality long chain binary acid crystal through continuous crystallization equipment to reduce equipment investment and production fluctuation, is an ideal long-chain binary acid crystallization method,and is applicable to large-scale industrial production.

Description

technical field [0001] The invention relates to a purification method of chemicals, in particular to a method for refining long-chain dibasic acids in the production process of long-chain dibasic acids, especially a method for refining long-chain dibasic acids produced by biological fermentation. Background technique [0002] Long chain dicarboxylic acids (Longchain dicarboxyacids) refer to aliphatic dicarboxylic acids (DCn for short) containing 9 or more carbon atoms in the carbon chain, including saturated and unsaturated dibasic acids, which are a class of important and widely used industrial Fine chemical products are important raw materials for the synthesis of high-grade spices, high-performance engineering plastics, high-temperature dielectrics, high-grade hot-melt adhesives, cold-resistant plasticizers, high-grade lubricating oils, high-grade paints and coatings in the chemical industry. [0003] Long-chain dibasic acids do not exist in nature, and some types of long...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/43C07C55/02C07C57/13C08G63/16C08G63/78C08G69/28
Inventor 秦兵兵杨希伟高冰刘驰李乃强刘修才
Owner CATHAY R&D CENT CO LTD
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