Method for refining long-chain biatomic acid

A technology of long-chain dibasic acid and dibasic acid, applied in chemical instruments and methods, preparation of carboxylate, preparation of organic compounds, etc., can solve the problems of increasing dibasic acid and increasing processing cost, etc.

Inactive Publication Date: 2005-05-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN1255483A also proposes three methods for refining long-chain dibasic acid, only using the crystallization technology of long-chain dibasic acid monosodium salt, and under the condition of not reclaiming the dibasic acid in the single-salt filtrate, the yield of the product is 90wt% Below, the yield of product is lower; And under the situation of recovering the dibasic acid in the monosalt filtrate, the yield of product can reach 92wt%, but this step has increased the dibasic acid in the monosalt filtrate of recycling , which increases the processing cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 200mL fermented tridecanedibasic acid obtained by Candida tropicalis, with a concentration of 130g / l and a pH value of 7.6, heat it to 80°C, let it rest for 30min, remove the remaining alkanes in the solution, and filter it out Bacteria, the filtrate with 3mol / L of H 2 SO 4 Adjust the pH value to 4.0, keep it warm at 80°C for 30 minutes, then lower it to room temperature, filter and wash to obtain a rough filter cake of tridecanedioic acid.

[0025] Mix 130mL of water with the crude acid filter cake, then adjust the pH value to 6.2 with 10mol / L NaOH solution, add 26g of NaCl at the same time, heat to 95°C to fully dissolve it, then cool down to 80°C for 30min, then Slowly cool to room temperature, and filter to obtain tridecanedioic acid monosodium salt filter cake. At 50°C, add 10 mol / L NaOH to the filter cake to prepare a solution with a pH value of 10, filter to obtain a clear long-chain dibasic acid double salt solution, and add 3 mol / L H to the solution 2 S...

Embodiment 2

[0027] Take 200mL of thirteen-carbon and fourteen-carbon mixed dibasic acid fermentation broth with a concentration of 120g / l and a pH value of 7.6, heat it to 80°C, let it stand still for 30 minutes, and remove the residual thirteen-carbon and tetradecane in the solution. Use 3mol / L H2SO4 to adjust the pH value to 3.4, keep it at 80°C for 30min, then cool to room temperature, filter and wash to obtain the mixed dibasic acid filter cake.

[0028] Mix 300mL of water with the crude acid filter cake, then adjust the pH value to 6.0 with 10mol / L NaOH solution, add 72g of NaCl at the same time, heat to 90°C to fully dissolve, then cool down to 78°C for 30min, then Slowly cool to room temperature, filter to obtain mixed dibasic acid monosodium salt filter cake. At 60°C, add 10 mol / L NaOH to the filter cake to prepare a solution with a pH value of 9, filter to obtain a clear long-chain dibasic acid double salt solution, and add 3 mol / L H to the solution 2 SO 4 , adjust the pH value...

Embodiment 3

[0030] Take 200mL octadecanedibasic acid fermentation broth with a concentration of 90g / l and a pH value of 7.6, heat it to 80°C, let it rest for 30min, remove the residual alkanes in the solution, remove the bacteria by filtration, and then use 3mol / L h 2 SO 4 Adjust the pH value to 3.4, keep it warm at 80°C for 30 minutes, then cool to room temperature, filter and wash to obtain octadecanedioic acid filter cake.

[0031]Mix 200mL of water with the crude acid filter cake, then adjust the pH value to 6.0 with 10mol / L NaOH solution, add 36g of NaCl at the same time, heat to 95°C to fully dissolve it, then cool down to 80°C for 30min, then Slowly cool to room temperature, filter to obtain mixed dibasic acid monosodium salt filter cake. At 70°C, add 10 mol / L NaOH to the filter cake to prepare a solution with a pH value of 10, filter to obtain a clear long-chain dibasic acid double salt solution, and add 3 mol / L H to the solution 2 SO 4 , adjust the pH value to 3.0, heat to 95...

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PUM

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Abstract

The invention relates to a kind of method for abstracting and refining long chain binary acid by water phase from C10-C18 regular normal-structure alkane or mixed normal-structure alkane fermenting liquor. The invention solves the disadvantages of low purity and high chroma in the production made by existing water phase. The method can decline the content of impurity such as protein and chroma effectively, and can be combined with the steps of thalline separation, acid-out and crystallization, drying and so on, to manufacture long chain binary acid product with total acid content more than 99wt% and white appearance. It uses the technique combining long chain binary mono-salt crystallization and salting-out, so it can leave the step of binary acid recovering treatment with salting-out mother liquor and mono-salt filter liquor out, save treatment cost, and improve product yield.

Description

technical field [0001] The invention relates to a method for extracting and refining long-chain dibasic acids from fermentation broth, especially from one or more C 10 ~C 18 A method for extracting and refining long-chain dibasic acids from n-alkane fermentation broth. Background technique [0002] Long-chain dibasic acids are metabolites obtained from the fermentation of normal alkanes by microorganisms. Its fermentation broth is a complex multiphase system, which contains unreacted normal alkanes, microbial cells and debris, unused medium and metabolites, and microbial secretions, etc., especially containing a large amount of impurities such as proteins and pigments , affecting the purity and appearance quality of the product. [0003] At present, the methods for refining long-chain dibasic acids are generally divided into two categories: solvent method and aqueous method. Although the solvent method can solve the above problems, the use of the method is greatly restri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/487C07C55/02C07C55/21
Inventor 高大成刘树臣
Owner CHINA PETROLEUM & CHEM CORP
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