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Method for separating and purifying acetoin in fermentation liquor

A technology of fermented liquid and acetoin, which is applied in the field of bioengineering, can solve the problems of unfavorable rectification and excessive organic acids, and achieve the effects of less water content, less fouling, and lower energy consumption

Active Publication Date: 2017-04-26
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The present invention aims at the problems that the upper phase obtained when acetoin in the fermentation broth is extracted by two aqueous phases formed by a hydrophilic organic solvent-salt contains more water, pigments, residual sugars, organic acids, and is unfavorable for subsequent rectification. A new method for extracting and separating acetoin in fermentation broth based on multi-stage countercurrent salting-out extraction technology with weakly polar organic solvents

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  • Method for separating and purifying acetoin in fermentation liquor
  • Method for separating and purifying acetoin in fermentation liquor
  • Method for separating and purifying acetoin in fermentation liquor

Examples

Experimental program
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Embodiment 1

[0033]The impact of different organic solvents of embodiment 1 on the distribution of acetoin

[0034] Add 17.2 g of anhydrous sodium carbonate or 120 g of dipotassium hydrogen phosphate to 100 mL of fermentation clear liquid containing 35 g / L acetoin, stir and dissolve to obtain a salt solution. Take 4 mL each of the salt solution and the organic solvent (shown in Table 1), put them in a graduated 20 mL stoppered test tube, vortex for 1 minute, and then put them in a water bath at 20°C for 8 hours to separate the layers. The upper phase is acetoin-rich The organic phase, the lower phase is a salt-rich aqueous phase. The distribution data of acetoin are shown in Table 1. As can be seen from the data in the table, for structurally similar organic solvents, such as alcohols and acetates, the recovery rate of acetoin decreases as the polarity of the solvent decreases. When organic solvents with high polarity (propanol and butanol) are used, the ratio is relatively large, and th...

Embodiment 2

[0037] The influence of ethanol content on the distribution of acetoin in the solvent of embodiment 2

[0038] Put 4mL of fermentation broth containing 60.5g / L acetoin, 2g of inorganic salts and 4mL of solvent into a 20mL stoppered test tube, vortex for 1min, then place it in a water bath at 24°C for 12h, separate layers, and the upper phase is rich in The organic phase of acetoin, the lower phase and the aqueous phase rich in salt, wherein the inorganic salt is dipotassium hydrogen phosphate or potassium pyrophosphate, the solvent is ethyl acetate or methyl tert-butyl ether, and the solvent contains 0~ 100% ethanol, detect the ratio (R) of the upper and lower phases in different extraction systems, the distribution coefficient (K) and the recovery (Y) of acetoin, such as figure 1 shown. figure 1 The salting-out extraction systems of A to D are as follows: A, methyl tert-butyl ether-ethanol / potassium pyrophosphate; B, methyl tert-butyl ether-ethanol / dipotassium hydrogen phosp...

Embodiment 3

[0039] The impact of embodiment 3 salt dosage on the distribution of acetoin

[0040] Place 4 mL of fermentation clear liquid containing 60.5 g / L acetoin, inorganic salts and 4 mL of organic solvent in a 20 mL stoppered test tube, vortex for 1 min, then place in a 24°C water bath for 12 h, and separate layers. The organic phase of dioxin, the lower phase is rich in salt water phase, wherein the inorganic salt is dipotassium hydrogen phosphate or potassium pyrophosphate, and the organic solvent is ethyl acetate or methyl tert-butyl containing 20% ​​or 30% ethanol according to the volume percentage base ether, and detect the ratio (R) of the upper and lower phases, the distribution coefficient (K) and recovery (Y) of acetoin in different salting-out extraction systems, such as figure 2 shown. figure 2 The abscissa in A~D of A~D is the mass volume percentage content of the addition amount of inorganic salt (m, g) to the fermentation broth volume (v, mL), figure 2 The salting...

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Abstract

The invention discloses a method for separating and purifying acetoin in fermentation liquor. The method includes the step of adding inorganic salt and a weak polar organic solvent are added into the fermentation liquor for extraction, wherein the addition amount of the inorganic salt accounts for 25-125% of the volume of the fermentation liquor, and the volume ratio of the organic solvent and the fermentation liquor is (1-2):1. The weak polar organic solvent is one of ethyl acetate, methyl tertiary-butyl ether, butyl acetate, dimethyl carbonate and diethyl carbonate. By means of the method, an extraction phase containing acetoin hardly contains pigment, residual sugar and organic acid impurities, an extraction solution can be directly rectified, and the scaling phenomenon is not likely to happen to a column reactor in the rectification process. Polarity of the solvent in use is small, the specific heat capacity is low, the upper phase water content is low, energy consumption for recycling is low, and acetoin loss in the recycling process is small. Operation is easy, and the method is an acetoin separation and extraction technology with industrial application prospects.

Description

technical field [0001] The invention belongs to the technical field of bioengineering, and relates to a separation technology of products in microbial fermentation liquid, in particular to a method for separating acetoin in fermentation liquid by using a multistage countercurrent salting-out extraction technology. Background technique [0002] Acetoin (3-hydroxy-2-butanone) is a natural fragrance widely present in nature and an important platform compound, which can be used in the synthesis of fragrance diacetyl and tetramethylpyrazine, optically active α-hydroxy ketone derivatives and a variety of pharmaceutical intermediates. [0003] Acetoin has two optical isomers, R- and S-. At present, the commercialized acetoin products are mostly synthesized by chemical methods, which are racemic mixtures of two optical isomers, while the products prepared by biological methods are mostly one of the isomers. Therefore, in recent years, fermentation methods Research on the productio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/80C07C45/78C07C49/17
CPCC07C45/78C07C45/80C07C49/17
Inventor 戴建英关文天马林会修志龙
Owner DALIAN UNIV OF TECH
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