Method for separating and extracting 1,3-propylene glycol from fermentation broth

A technology of propylene glycol and fermentation liquid, applied in the biological field, can solve the problems of incomplete sterilization, long separation time, and long process route, and achieve the effects of avoiding the use and extraction process, avoiding excessive volatilization loss, and simplifying the separation process

Active Publication Date: 2016-06-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Centrifugal sterilization requires high-speed centrifugal equipment, which cannot be completely sterilized, and the product loss is large
The problems of membrane filtration are small separation capacity, long separation time, prone to membrane fouling, clogging, etc., frequent replacement of membrane modules, and large losses
This method uses low-carbon aldehyde, the process route is long, the loss of solvent is large, and it needs to use highly toxic benzene extractant, and there are 5 steps of rectification in the process, so the energy consumption is very high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The fermented broth treated in this example is a 1,3-propanediol fermented broth obtained by using glycerol as a substrate and fermented by Klebsiella. The content of 1,3-propanediol is 78.5g / L, and the pH value at the end of fermentation is is 7.0.

[0041] Take 20L of the above-mentioned fermentation liquid, filter to remove bacteria and sediment, obtain the filtered clear liquid, then use the normal pressure falling film-scraped film evaporation method to concentrate and remove water, concentrate and remove 82wt% of water in the clear liquid, most of the salt Precipitate in the form of crystals, some macromolecular proteins and polysaccharides are concentrated and precipitated, and the precipitates are removed by centrifugation to obtain a concentrated solution containing 1,3-propanediol.

[0042] Add 2.65 kg of benzaldehyde to the concentrated solution under stirring, continue heating and concentrating to remove water until the water is completely removed, and filte...

Embodiment 2

[0046] The 1,3-propanediol fermentation broth used in this example is the same as in Example 1.

[0047] Take 20L of the above-mentioned fermentation liquid, filter to remove bacteria and sediment, obtain the filtered clear liquid, and then use the reduced-pressure falling film-scraped film evaporation method to concentrate and remove water, concentrate and remove 90wt% of water in the clear liquid, and the operating pressure is 50kPa , most of the salts are precipitated in the form of crystals, and some macromolecular proteins and polysaccharides are concentrated and precipitated, and the crystallized salts and precipitates are removed by centrifugation to obtain a concentrated solution containing 1,3-propanediol.

[0048] Add 4.2 kg of phenylacetaldehyde to the concentrated solution under stirring, continue to concentrate to remove the remaining water, and centrifuge to remove the precipitated insoluble matter. 70.0 g of D72 strong acid resin was added to the filtrate for ac...

Embodiment 3

[0052] The 1,3-propanediol fermentation broth used in this example is the same as in Example 1.

[0053] Take 20L of the above-mentioned fermented liquid, filter to remove the bacteria and sediment, and obtain the filtered clear liquid. The clear liquid is sent to a batch distillation tower to concentrate and remove water, and concentrate to remove 86wt% of water in the clear liquid. It is operated under normal pressure, and the number of theoretical plates is 10. Most of the salts, polysaccharides and proteins are precipitated in the form of crystallization and precipitation, and these insoluble solids are removed by centrifugation to obtain a concentrated solution containing 1,3-propanediol.

[0054] Add 4.1 kg of phenylpropanal to the concentrated solution under stirring, continue to concentrate to remove the remaining water, and centrifuge to remove the precipitated insoluble matter. Add 46.0g of D62 strong acid resin to the filtrate to carry out acetalization reaction, a...

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Abstract

The invention discloses a method for separating and extracting 1,3-propylene glycol from fermentation broth. The method comprises the following steps: (1) removing solids in fermentation broth; (2) heating fermentation broth to concentrate and evaporate fermentation broth, and removing precipitated solids to obtain 1,3-propylene glycol concentrated liquid; (3) adding an aromatic aldehyde solvent into the concentrated liquid, and keeping on heating the concentrated liquid until all water is removed to obtain an organic solution containing 1,3-propylene glycol; (4) adding a catalyst into the organic solution to carry out acetalation reactions; (5) distilling the reaction liquid obtained in the step (4) to evaporate unreacted aromatic aldehyde solvent; (6) adding pure water and catalyst into the product obtained in the step (5) to carry out hydrolysis, wherein the aromatic aldehyde solvent forms an organic phase layer, 1,3-propylene glycol is dissolved in the lower-layer water phase, and the water phase layer is filtered to remove catalyst; (7) subjecting the water phase layer obtained in the step (6) to rectification dehydration, and collecting the 1,3-propylene glycol fraction. The method has the advantages that the technology is simple, toxic extracting agent is not used, and the product purity and yield are high.

Description

technical field [0001] The invention belongs to the field of biotechnology, and relates to the separation technology of microbial fermentation products, in particular to a method for separating and extracting 1,3-propanediol from fermentation liquid. Background technique [0002] 1,3-Propanediol (1,3-PDO) is an important chemical raw material, which is used in the manufacture of polyester fibers, polyurethanes, hot melt adhesives, powder coatings, antifreeze agents, packaging materials and organic synthesis intermediates, etc. A wide range of applications, among which the manufacture of high-performance polyester fiber PTT is currently the main application. 1,3-propanediol can be produced through chemical and biological routes, and biotechnology is used to produce 1,3-propanediol, which is characterized by its green chemistry, with mild reaction conditions, easy operation, less by-products, less environmental pollution, and The use of renewable resources and other character...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/74
Inventor 王崇辉孙启梅高大成
Owner CHINA PETROLEUM & CHEM CORP
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