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Method for separating 1,3-propanediol from fermentation liquor

A fermentation broth, propylene glycol technology, applied in the biological field, can solve the problems of long separation time, hindered by salt crystallization and viscous substances, low primary recovery rate, etc., to achieve the effect of strengthening flocculation effect, and the sterilization process is simple and effective.

Active Publication Date: 2008-08-27
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 and clogging, etc.
The primary recovery rate of this method is not high, the efficiency of the whole process is not high, the purity of the separated product is only 50% to 90%, and the regeneration treatment of the resin will produce a large amount of waste water, and there are many practical difficulties in large-scale production.
Aiming at the problems existing in the subsequent separation and purification of 1,3-propanediol produced by the current fermentation method, such as high cost, low separation capacity, salt crystallization and viscous substances hindering evaporation in vacuum distillation, etc., Chinese patent CN1460671A proposes a method for separating 1,3-propanediol from fermentation broth The method for recovering 1,3-propanediol is to directly evaporate and concentrate the fermented liquid containing bacteria to 1 / 2 to 1 / 20 of the original volume, and add a certain proportion of alcohol solvents such as methanol, ethanol, propanol or acetone, etc., Filtration or centrifugation to obtain the clear liquid, after distillation to recover the solvent, and then rectification under reduced pressure to obtain the product 1,3-propanediol
In this method, due to the existence of a considerable amount of water in the concentrated solution, and the used solvent part is hydrophilic, the properties of bacteria and proteins in this alcohol (ketone) water system have not changed greatly. Or filter sterilization is still very difficult, the color of the obtained clear liquid is darker, and the salt present in the fermented liquid has not been completely removed, and the problem of salt crystallization and viscous substances occurring in the vacuum distillation process hindering evaporation has not been effectively solved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The fermented liquid treated in this embodiment is 1,3-propanediol fermented liquid obtained by using glycerol as a substrate and fermented by Klebsiella, the content of 1,3-propanediol is 70.7g / L, and the pH value at the end of fermentation is 7.0.

[0026] Take 500ml of the above-mentioned fermentation broth, adjust the pH value to 4.0 with 8N sulfuric acid, add 1.2wt% powdered activated carbon, heat to 95°C under stirring, keep the temperature at a constant temperature for 0.8h, let it cool down naturally and let it settle, and filter it after the flocculation is completely settled to obtain Colorless and transparent fermented serum. Atmospheric pressure distillation removes the water in the clear liquid, and the salt contained in it precipitates out in the form of crystals, and the salt is removed by filtration to obtain a concentrated liquid containing 1,3-propanediol, which is then distilled under reduced pressure at a vacuum of 10mmHg to collect 100-108 ℃ of 1,3...

Embodiment 2

[0028] In the 1,3-propanediol fermentation broth used in this example, the content of 1,3-propanediol was 51.2 g / L, and the pH value at the end of fermentation was 7.0.

[0029] Take 500ml of the above-mentioned fermentation broth, adjust the pH value to 3.0 with 6N hydrochloric acid, add 2.0wt% powdered activated carbon, heat to 90°C with stirring, keep the temperature for 1h, let it cool down naturally and let it settle, and filter it after the flocculation is completely settled to obtain Clear fermented liquid. Remove the water in the clear liquid by distillation under reduced pressure, the operating vacuum is 200mmHg, the operating temperature is 65-70°C, and then filter to remove the crystallized salt to obtain a concentrated solution containing 1,3-propanediol, which is decompressed under a vacuum of 10mmHg Distill and collect the 1,3-propanediol fraction at 100-108°C to obtain a product with a purity of 99.3wt% and a recovery rate of 84.5wt%.

Embodiment 3

[0031]In the 1,3-propanediol fermentation broth used in this example, the content of 1,3-propanediol was 63.3 g / L, and the pH value at the end of fermentation was 7.4.

[0032] Take 500ml of the above-mentioned fermentation broth, adjust the pH value to 5.0 with 4N sulfuric acid, add 4.0wt% powdered activated clay, heat to 82°C under stirring, keep the temperature for 3.5h, let it cool down naturally, let it settle, and filter after the flocculation is completely settled. Obtain the fermented serum. Distill water under reduced pressure, operate at a vacuum of 100 mmHg, and operate at a temperature of 51 to 56 ° C, then filter to remove the crystallized salt to obtain a concentrated solution containing 1,3-propanediol, distill under reduced pressure at a vacuum of 6 mmHg, and collect 95 The 1,3-propanediol fraction at ~98°C has a purity of 99.0wt% and a recovery rate of 81.5wt%.

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Abstract

The invention discloses a removing method of 1, 3-propylene glycol from ferment liquid of 1, 3-propylene glycol, which comprises the following steps: adjusting pH value of ferment liquid not more than 5.5; heating; stewing; sedimenting; fetching supernatant; heating the supernatant; condensing; dehydrating; separating to remove evolved salt; decompressing; rectifying; collecting the fraction of 1, 3-propylene glycol. The invention reinforces flocculation effect, which is convenient to separate.

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 1,3-propanediol from fermentation liquid. Background technique [0002] 1,3-Propanediol (1,3-PD) is an important chemical raw material, which is widely used in the manufacture of polyester fibers, polyurethanes, hot melt adhesives, powder coatings, antifreeze agents, packaging materials and organic synthesis intermediates. 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 characteristics has bec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/74C07C31/20
Inventor 王崇辉
Owner CHINA PETROLEUM & CHEM CORP
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