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Method for preparing long-chain dicarboxylic acid by aqueous phase method

A long-chain dibasic acid, water-phase technology, applied in the preparation of carboxylate, separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of poor quality of acidified crystalline products, waste of resources, environment, and high processing costs, Achieve the effect of reducing safety and environmental protection hidden dangers, saving resources and costs, and achieving good quality

Inactive Publication Date: 2020-08-14
羊晓磊
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] The purpose of the present invention is to overcome the complex process of preparing long-chain dibasic acids by microbial fermentation in the prior art, which requires the use of organic solvents to refine and purify the crude products, resulting in high processing costs, resulting in resource waste and environmental pollution, and the quality of acidified crystallization products. The problems of poor and low yields provide a method for preparing long-chain dibasic acids by aqueous phase method. The method has simple process flow, avoids the waste of resources and costs caused by the large use of organic solvents, and can obtain refined products at one time, and The prepared product has high purity, good quality, high yield and light color

Method used

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  • Method for preparing long-chain dicarboxylic acid by aqueous phase method
  • Method for preparing long-chain dicarboxylic acid by aqueous phase method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] (1) Take the fermented dodecane dibasic acid fermentation broth, heat the fermentation broth to 80°C through a steam heat exchanger, then add caustic soda to adjust the pH value of the fermentation broth to 10, and filter through ceramic membrane and ultrafiltration membrane Carrying out solid-liquid separation on the fermentation liquid to obtain a fermentation treatment liquid;

[0062] (2) The fermentation treatment liquid obtained in step (1) is decolorized at 30° C. with granular coal-based activated carbon decolorization column, and the filtration speed is controlled to be 3ml / min. After separation, the decolorized fermented liquid is obtained, and the pH of the decolorized fermented liquid Control is 6.8;

[0063] (3) Heating the decolorized fermented liquid obtained in step (2) to 90° C., adding sulfuric acid, adjusting the pH value to 3.2 for acidification and crystallization, and obtaining dodecanedibasic acid after filtration.

Embodiment 2

[0065] (1) Take the fermented tridecanedibasic acid fermentation broth, heat the fermentation broth to 90°C through a steam heat exchanger, then add caustic soda to adjust the pH value of the fermentation broth to 9.5, and filter the fermentation broth through a ceramic membrane Solid-liquid separation to obtain a fermentation treatment liquid;

[0066] (2) The fermentation treatment liquid obtained in step (1) is decolorized at 50° C. with a granular wood activated carbon decolorization column, and the filtration speed is controlled to be 1ml / min. After separation, the decolorized fermented liquid is obtained, and the pH value of the decolorized fermented liquid is controlled is 6.5;

[0067] (3) Heating the decolorized fermented liquid obtained in step (2) to 85° C., adding nitric acid, adjusting the pH value to 2 for acidification and crystallization, and obtaining tridecanedibasic acid after filtration.

Embodiment 3

[0069] (1) Take the fermented sebacic acid fermentation broth, heat the fermentation broth to 70°C through a steam heat exchanger, then add caustic soda to adjust the pH value of the fermentation broth to 10.5, and filter the fermentation broth through ultrafiltration membrane to perform solid-liquid Separation to obtain a fermentation treatment liquid;

[0070] (2) The fermentation treatment liquid obtained in step (1) is decolorized at 20° C. with granular coal-based activated carbon decolorization column, and the filtration speed is controlled to be 5ml / min. Control is 6.7;

[0071] (3) Heating the decolorized fermented liquid obtained in step (2) to 87° C., adding hydrochloric acid, adjusting the pH value to 5 for acidification and crystallization, and obtaining sebacic acid after filtration.

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Abstract

The invention relates to the technical field of preparation of long-chain dicarboxylic acid, and discloses a method for preparing long-chain dicarboxylic acid by an aqueous phase method. The method comprises the following steps: (1) carrying out solid-liquid separation on a fermentation liquid to obtain a fermentation treatment liquid, (2) decolorizing the fermentation treatment liquid obtained inthe step (1) at 20-50 DEG C, separating to obtain a decolorized fermentation liquid, and controlling the pH value of the decolorized fermentation liquid to be less than 7, and (3) acidifying and crystallizing the decolorized fermentation liquid obtained in the step (2), and carrying out after-treatment to obtain the long-chain dicarboxylic acid. The method is simple in technological process, avoids waste of resources and cost due to the fact that a large amount of organic solvent is used and can obtain refined products at a time, and the prepared products are high in purity, good in quality,high in yield and light in color.

Description

technical field [0001] The invention relates to the technical field of preparation of long-chain dibasic acids, in particular to a method for preparing long-chain dibasic acids by an aqueous phase method. Background technique [0002] Long chain dicarboxylic acids (Long chain dicarboxy acids) refer to aliphatic dicarboxylic acids (n=9-18) containing more than 9 carbon atoms in the carbon chain, including saturated and unsaturated dicarboxylic acids. Fine chemical products with a wide range of industrial uses 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, such as sebacic acid and dodecanedioic acid, can be synthesized chemically. In addition, ...

Claims

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Application Information

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IPC IPC(8): C07C51/42C07C51/47C07C51/02C07C55/21C07C55/02C07C57/13C07C55/20
CPCC07C51/02C07C51/42C07C51/47C07C55/21C07C55/02C07C57/13C07C55/20
Inventor 羊晓磊
Owner 羊晓磊
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