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Long chain diprotic acid refining method

A long-chain dibasic acid and inorganic acid technology, applied in the separation/purification of carboxylic acid compounds, organic chemistry, fermentation, etc., can solve the problems of expensive equipment, low purity, low recovery rate of alkanes, etc., and achieve complete crystal form rules , Simplify the operation steps, the effect of large particles

Active Publication Date: 2007-10-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The equipment used in this method is expensive, and because there is no decolorization treatment, the purity of the product obtained is lower, the highest is not more than 96%, and the recovery rate of alkane is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Using n-dodecane as a substrate, use Candida tropicalis to ferment and produce dodecane dibasic acid. After the fermentation, the cell concentration was 12.3g / L, the dibasic acid concentration was 124.5g / L, and the pH was 8.0. Take 1000 ml of fermentation broth, add 10 g of urea, heat to 98 ° C, then slowly cool to 20 ° C, let stand for 1 hour, and then separate and recover unreacted alkanes. Then add 550 milliliters of water for dilution, add 70 g of activated carbon, stir and decolorize at a temperature of 20° C. for 20 minutes, and then filter. After the filtration, the carbon cake was washed with 4000 ml of water at 70° C., and the washing liquid was recovered in the filtrate. Heat the above liquid to 95°C, adjust the pH to 3.5 with 6N sulfuric acid, and slowly cool to room temperature for crystallization. Filter again, and then wash the acid cake with water to neutrality. Finally, dry it at 80°C to obtain white dibasic acid crystals. The results are shown in Ta...

Embodiment 2

[0026] Using n-tridecane as substrate, use Candida tropicalis to ferment and produce dodecane dibasic acid. After the fermentation, the cell concentration was 14.1g / L, the dibasic acid concentration was 144.5g / L, and the pH was 9.3. Take 1000 ml of fermentation broth, add 12 g of urea, heat to 100°C, then slowly cool to 30°C, let stand for 1 hour, and then separate and recover unreacted alkanes. Then add 800 milliliters of water to dilute, add 72 g of activated carbon, stir and decolorize at a temperature of 30° C. for 30 minutes, and then filter. After the filtration, wash the carbon cake with 6000 ml of water at 60° C., and recycle the washing liquid into the filtrate. Heat the above liquid to 90°C, adjust the pH to 3.0 with 6N sulfuric acid, and slowly cool to room temperature. Filter again, and then wash the acid cake with water to neutrality. Finally, dry it at 75°C to obtain white dibasic acid crystals. The results are shown in Table 1.

Embodiment 3

[0028] Get 1000ml of dibasic acid fermentation broth mixed with dodecane and thirteen carbons. The bacterial cell concentration is 11.5g / L, the dibasic acid concentration is 124.7g / L, and the pH is 8.5. Add 5g of urea to the fermentation broth, heat to 100°C, slowly cool to 30°C, let stand for 1 hour, and then separate and recover unreacted alkanes. Add 650 milliliters of water to dilute, add 55 g of activated clay, stir and decolorize at a temperature of 30° C. for 20 minutes, and then filter. After the filtration, wash the carbon cake with 5000 ml of water at 50° C., and recycle the washing liquid into the filtrate. Heat the above liquid to 95°C, adjust the pH to 3.0 with 6N hydrochloric acid, and slowly cool to room temperature. Filter again, and then wash the acid cake with water to neutrality. Finally, dry it at 80°C to obtain the dibasic acid in white crystals. The results are shown in Table 1.

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Abstract

The invention relates to a method to extract and refine long-chain diacid from normal alkane fermentation liquor in water-phase, which comprises: adding proper urea when heating and breaking emulsion to overcome heavy emulsification and increase recycle yield of un-reacted alkane, decolourizing with adsorbent before degerming to save filter step and reduce cost.

Description

technical field [0001] The invention relates to a method for refining long-chain dibasic acids from normal alkane fermentation broth, especially from C 10 ~C 18 A method for refining long-chain dibasic acids in n-alkane fermentation broth. Background technique [0002] Long-chain dibasic acids are metabolites obtained from microbial fermentation of long-chain n-alkanes. Its fermentation broth is a complex multiphase system, which contains water, unreacted alkanes and various medium components, microbial cells, autolyzed cell fragments and proteins, pigments, various metabolites, long-chain dibasic acids , as well as emulsions of oil, water, and cells. This complex heterogeneous system increases the difficulty of extracting dibasic acids and affects the purity and yield of products. [0003] At present, the methods for extracting long-chain dibasic acids are generally divided into solvent method and aqueous method. Although the solvent method can solve the above problems...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C55/02C07C55/21C07C51/47C12P7/44
Inventor 范峰佟明友
Owner CHINA PETROLEUM & CHEM CORP
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