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Long-chain binary acid continuous crystallization method

A long-chain dibasic acid and long-chain dibasic carboxylic acid technology, applied in solution crystallization, separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve low production efficiency, high production cost, unstable product quality, etc. question

Inactive Publication Date: 2015-03-18
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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  • Long-chain binary acid continuous crystallization method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0099] DC12 fermentation broth was prepared according to the method disclosed in patent document ZL200410018255.7, adding sulfuric acid with a weight concentration of 97% to the fermentation broth to adjust the pH value to 3.0, and heating 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. Keep at 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 the clear liquid.

[0100] 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 contr...

Embodiment 2

[0103] According to the membrane filtration method disclosed in the patent document ZL200410018255.7, the DC12 membrane supernatant was prepared, and the solution was added with 97% sulfuric acid by weight 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.

[0104] 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...

Embodiment 3

[0107] 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 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.

[0108] 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 long-chain binary acid continuous crystallization method and an application thereof. The continuous crystallization method comprises the step that multi-stage crystallization, preferably three-stage crystallization, is sequentially carried out on an organic solution containing a binary acid. Compared with a batch crystallization device, the crystallization method disclosed by the invention is high in industrial automatic degree, and stable in product quality on the premise that the same product quality is obtained; meanwhile, the operating personnel are greatly reduced; and the investment cost is reduced by over 50% (on the product scale of 10,000t / year) in comparison with a batch crystallization device, and therefore, the high-quality long-chain binary acid crystal can be efficiently obtained through the continuous crystallization equipment; the equipment investment is reduced; the fluctuation in production is reduced; and the long-chain binary acid continuous crystallization method is an ideal long-chain binary acid crystallization method, and can be suitable for 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 (Long chain dicarboxy acids) refer to aliphatic dicarboxylic acids (DCn for short) containing 9 or more carbon atoms in the carbon chain, including saturated and unsaturated dicarboxylic acids. Fine chemical products for industrial use 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-chain dibasic acids can be synt...

Claims

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Application Information

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IPC IPC(8): C07C51/43C07C55/18C07C55/20C07C55/02C07C57/13B01D9/02C08G63/16C08G63/52C08G69/26
Inventor 秦兵兵杨希伟高冰刘驰李乃强
Owner CATHAY R&D CENT CO LTD
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