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Method of isolating 1,3-propanediol, acetic acid and butyric acid from fermentation liquor

A technology of propylene glycol and fermentation broth, applied in the field of bioengineering, can solve the problems of high separation cost, difficult recovery of by-products, etc., and achieve the effects of simple operation, easy recovery and utilization, and cost reduction.

Active Publication Date: 2019-04-05
DALIAN UNIV OF TECH
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  • Claims
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Problems solved by technology

[0009] The object of the present invention is to provide a method for extracting and separating 1,3-propanediol, acetic acid and butyric acid in the fermentation broth, aiming at the problems that 1,3-propanediol in the fermentation broth is difficult to extract and separate, the recovery of by-products is difficult, and the separation cost is high. new method

Method used

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  • Method of isolating 1,3-propanediol, acetic acid and butyric acid from fermentation liquor
  • Method of isolating 1,3-propanediol, acetic acid and butyric acid from fermentation liquor
  • Method of isolating 1,3-propanediol, acetic acid and butyric acid from fermentation liquor

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preparation example Construction

[0034] 1. Preparation of 1,3-propanediol fermentation broth

[0035] The 1,3-propanediol fermentation broth is a fermentation broth prepared by a conventional method and contains 1,3-propanediol, acetic acid and butyric acid.

[0036] The fermentation liquid of the following examples is obtained by using the batch flow of Clostridium butyricum (Clostridium butyricum) to ferment crude glycerol. By adjusting the substrate concentration or feeding time, 1,3-propanediol fermentation with appropriate component content is obtained. Liquid, in which the concentrations of 1,3-propanediol (1,3-PD), acetic acid (HAc) and butyric acid (BA) are 50-100g / L, 6-15g / L and 10-20g / L, respectively. Filter the 1,3-PD fermentation broth through a hollow fiber membrane to remove bacteria and some proteins to obtain a fermentation serum.

[0037] 2. Analysis method

[0038] In the aqueous solution, the content of 1,3-PD, HAc and BA was detected by high performance liquid chromatography. Aminex HPX...

Embodiment 1

[0042] The method for separating 1,3-propanediol, acetic acid and butyric acid from 1,3-PD fermented liquid comprises the steps of microfiltration, ultrafiltration-concentration-precipitation under acidic conditions-organic solvent extraction-rectification, and the specific steps are as follows :

[0043] 1) The fermented liquid is removed by microfiltration and ultrafiltration to remove impurities such as bacteria and protein to obtain a fermented clear liquid;

[0044] 2) Distilling, concentrating and dehydrating the fermented clear liquid obtained in step 1) to obtain concentrated fermented liquid;

[0045] 3) adding an inorganic acid to the concentrated fermentation broth obtained in step 2), adjusting the pH to acidity, and then filtering to obtain a solid precipitate and a supernatant;

[0046] 4) adding methanol to the solid precipitate obtained in step 3), stirring, washing, and filtering, distilling the filtrate to recover methanol, and retaining the residual liquid;...

Embodiment 2

[0053] Example 2 Membrane Filtration

[0054] The concentrations of 1,3-PD, HAc, BA and glycerol in 1,3-PD fermentation broth were 87.97g / L, 8.59g / L, 16.62g / L, 6.76g / L, respectively.

[0055] 5L of fermented broth was passed through microfiltration membrane and ultrafiltration membrane at flow rates of 18mL / min and 16mL / min, respectively, to remove 99.90% of bacteria and 79.07% of protein in the fermented broth. Add 400mL of water to the last remaining bacteria-carrying liquid, filter again, and repeat three times to reduce product loss. The results are shown in Table 1. The recoveries of 1,3-PD, HAc, BA and glycerol were 99.10%, 98.82%, 96.05%, 75.52%, respectively. The lower recovery of glycerol may be due to its utilization and consumption by microorganisms surviving in the broth. The membrane liquid was mixed with the washing liquid three times to obtain the fermentation supernatant.

[0056] Table 1. Yield of main products after fermentation broth is filtered by membr...

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Abstract

The invention belongs to the technical field of bioengineering and provides a method of isolating 1,3-propanediol, acetic acid and butyric acid from a fermentation liquor. The method includes: performing micro-filtering and ultrafiltering on the fermentation liquor to obtain a fermentation supernatant, and removing nearly all bacteria and most miscellaneous proteins; concentrating the fermentationsupernatant, and removing part of water; using an acid to adjust the concentrate to acidity, and filtering to remove precipitate; using a hydrophobic organic solvent to extract acetic acid and butyric acid from the supernatant, using an alkali or an alkaline inorganic salt solution to back-extract the organic acid from the extract, and rectifying raffinate to recycle 1,3-propanediol. The method herein is simple to perform and has high recovery rate; the problems that 1,3-propanediol and byproducts are difficult to separate and the cost is high are solved; the method is a separation method having a promising industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of bioengineering, and relates to the separation technology of microbial fermentation liquid, in particular to a method for separating and extracting 1,3-propanediol, acetic acid and butyric acid from the fermentation liquid. Background technique [0002] 1,3-Propanediol is an important chemical raw material that can be used in many industries such as solvents, coatings, cosmetics, medicine and animal feed. Because there are two hydroxyl functional groups in the molecule, it can be used as a monomer to participate in various polycondensation reactions to synthesize polyester, polyether and polyurethane, etc. Among them, polytrimethylene terephthalate (PTT) synthesized with terephthalic acid is not easy to produce With the advantages of static electricity, good resilience, stain resistance and biodegradability, it has great application prospects in industries such as fiber and engineering plastics. [0003] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/74C07C29/86C07C31/20
CPCC07C29/74C07C29/86C07C31/202
Inventor 修志龙李震鄢凌孙亚琴牟英
Owner DALIAN UNIV OF TECH
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