Purification method for long-chain dicarboxylic acid

A long-chain dibasic acid and emulsifier technology, applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carboxylic acid compounds, etc., can solve the problem of reducing the yield of long-chain dibasic acids and increasing the cost of sewage treatment , limit the scope of application and other issues, to achieve the effect of improving the purity of single acid, reducing loss and reducing pollution

Active Publication Date: 2015-05-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantages are: the pH value during stripping is 9-12, which will make the ester solvent in the solvent phase easier to hydrolyze, and the amount of alkali used is large, and the amount of acid used in acid analysis is also large, resulting in sewage The higher salt content in the medium increases the cost of sewage treatment
This method adopts high-concentration acetic acid as a solvent, and the amount of solvent used is very large, so that when cooling and crystallization, some acetic acid will remain in the product, which limits the scope of application of the product. There is still a certain solubility, which will reduce the yield of long-chain dibasic acids

Method used

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  • Purification method for long-chain dicarboxylic acid

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Embodiment 1

[0041] Take 2000ml and get C by fermenting Candida tropicalis 12 h 22 o 4 Fermented liquid, concentration is the fermented liquid of 160g / L. Heat the terminated fermentation broth at 85°C, let it stand for about 2 hours, then remove the residual liquid wax in the upper layer, then lower the temperature to 70°C, and filter through microfiltration to remove impurities such as bacteria cells to obtain the filtrated liquid. Add H to the filtrate 2 SO 4 Adjust the pH to 2.5 and heat to 90 °C to give C 12 h 22 o 4 The crystallized aqueous solution was cooled to room temperature and filtered to obtain a filter cake.

[0042] Put C 12 h 22 o 4 Filter cake and isobutyl ether (isobutyl ether and C 12 h 22 o 4 The weight ratio is 7:1) mixed, heated to 90°C, stood still for 30min, and separated the lower aqueous phase; then added 300mL deionized water to the solvent phase to wash the organic phase, and separated the aqueous phase again; then added to the organic phase 0.3g o...

Embodiment 2

[0045] Take 2000ml and get C by fermenting Candida tropicalis 12 h 22 o 4 Fermented liquid, concentration is the fermented liquid of 160g / L. The fermented liquid is heated to 85°C, and enters a microfiltration device to remove bacterial cells and liquid wax, etc., to obtain a clarified filtrate containing long-chain dibasic acid salts. Add H to the filtrate 2 SO 4 Adjust the pH to 3.0 and heat to 95 °C to give C 12 h 22 o 4 The crystallized aqueous solution was cooled to room temperature and filtered to obtain a filter cake.

[0046] Will C 12 h 22 o 4 Filter cake and n-butyl ether (n-butyl ether and C 12 h 22 o 4 The weight ratio is 6:1) mixed, heated to 95°C, stood still for 30min, and the lower aqueous phase was separated; 280mL deionized water was added to the solvent phase to wash the organic phase, and the aqueous phase was separated again; 0.2g was added to the organic phase Activated carbon was decolorized by heat preservation for 30 minutes, and then fil...

Embodiment 3

[0049] Take 2000ml and get C by fermenting Candida tropicalis 13 h 24 o 4 Fermented liquid, concentration is the fermented liquid of 154g / L. Heat to 70°C, filter through a ceramic microfiltration membrane, remove bacteria and residual liquid wax to obtain a filtrate. Add H to the filtrate 2 SO 4 Adjust the pH to 2.4 and heat to 95 °C to give C 13 h 24 o 4 The crystallized aqueous solution was cooled to room temperature and filtered to obtain a filter cake.

[0050] Put the obtained C 13 h 24 o 4 Filter cake and n-butyl ether (n-butyl ether and C 13 h 22 o 4 The weight ratio is 4:1), mix, mix and heat to 105°C, stand still for 45min, and remove the lower aqueous phase; then add 310mL deionized water to the solvent phase to wash the organic phase, and then separate the aqueous phase; add 0.15 g activated carbon was decolorized by heat preservation for 30min, and then the activated carbon was removed by filtration.

[0051] Add 130 μg / g of octylphenol polyoxyethyle...

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Abstract

The invention discloses a purification method for long-chain dicarboxylic acid. The method comprises the following steps: subjecting terminated long-chain dicarboxylic acid fermentation broth to pretreatment and acidification; carrying out extraction with an organic solvent and adsorption, adding an emulsifier and an alkaline solution and carrying out treatment; and adding acetic acid into the obtained water phase and then carrying out cooling crystallization so as to obtain a long-chain dicarboxylic acid product. Compared with the prior art, the method of the invention has the following advantages: a small amount of raw materials are used; loss and cost are low; the purity of the obtained long-chain dicarboxylic acid is high; total nitrogen content meets requirements of the polymer grade; and the method is suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for purifying long-chain dibasic acids, in particular to a method for obtaining high-purity long-chain dibasic acids from fermentation broth. Background technique [0002] The long-chain dibasic acid molecule general formula that the present invention refers to is C n h 2n-2 o 4 , where n is 10-18, which is a metabolite obtained by fermentation of microorganisms using liquid wax, etc. Its fermentation broth is a complex multiphase system, which contains unreacted carbon sources, microbial cells and debris, unused medium and metabolites, and microbial secretions, etc., especially containing a large amount of impurities such as proteins and pigments. It affects the purity and application of the product, and brings difficulties to the extraction and purification of this type of long-chain dibasic acid. [0003] At present, the market has very high requirements on the purity of this type of long-chain dibasic acid, esp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/42C07C55/21C07C55/02
CPCC07C51/42C07C51/48C07C51/487C07C55/21C07C55/02
Inventor 高大成李晓姝
Owner CHINA PETROLEUM & CHEM CORP
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