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A kind of separation and extraction method of 1,3-propanediol in fermented liquid

A technology of propylene glycol and fermentation broth, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of long separation time, long process route, membrane fouling, etc., to avoid excessive volatilization loss and improve the operating environment. , the effect of simplifying the separation process

Active Publication Date: 2018-06-19
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

[0038] 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 78.5 g / L, and the pH value at the end of fermentation is is 7.0.

[0039] Take 20 L of the above-mentioned fermentation broth, filter to remove the bacteria and sediment, and obtain the fermentation supernatant.

[0040] Add 3.9kg of benzaldehyde, 54.7g of aluminum sulfate and 273.5g of PEG600 to the above fermentation liquid under stirring, and carry out acetalization reaction under rapid stirring, and 1,3-propanediol is converted into benzaldehyde acetal 1,3-propanediol acetal . The reaction temperature was 60 °C, and the reaction time was 5.5 h. After the reaction is over, let it stand for stratification. The acetal product and unreacted benzaldehyde are located in the upper organic phase layer, and the original fermentation broth, together with impurities such as salts, proteins, a...

Embodiment 2

[0044] The 1,3-propanediol fermentation broth used in this example is the same as in Example 1.

[0045] Take 20 L of the above-mentioned fermentation broth, filter to remove the bacteria and sediment, and obtain the fermentation supernatant.

[0046] Add 4.95 kg of phenylacetaldehyde, 32.0 g of D72 strong acid resin, and 130.0 g of dodecyltrimethylammonium chloride into the above-mentioned fermented liquid under stirring for acetalization reaction, and 1,3-propanediol is converted into Phenylacetaldehyde acetal 1,3-propanediol acetal. The reaction temperature is 50° C., and the reaction time is 8.0 h. After the reaction is over, let it stand for stratification. The acetal product and unreacted benzaldehyde are located in the upper organic phase layer, and the original fermentation broth, together with impurities such as salts, proteins, and sugars, are located in the lower aqueous phase layer. Water is removed by phase separation. Layers.

[0047] Under the pressure of 30 ...

Embodiment 3

[0050] The 1,3-propanediol fermentation broth used in this example is the same as in Example 1.

[0051] Take 20 L of the above-mentioned fermentation broth, filter to remove the bacteria and sediment, and obtain the fermentation supernatant.

[0052] Add 7.19kg of phenylpropanal, 131.0g of 001×7 strong acid resin, and 700.0g of tetrabutylammonium bromide to the above-mentioned fermented liquid under stirring for acetalization reaction, and 1,3-propanediol is converted into phenylpropanoid Aldehyde 1,3-propanediol acetal. The reaction temperature is 85°C, and the reaction time is 3.5h. After the reaction is over, let it stand for stratification. The acetal product and unreacted benzaldehyde are located in the upper organic phase layer, and the original fermentation broth, together with impurities such as salts, proteins, and sugars, are located in the lower aqueous phase layer. Water is removed by phase separation. Layers.

[0053] Under the pressure of 45 kPa, carry out va...

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PUM

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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) separating 1,3-propylene glycol fermentation broth to remove insoluble solids; (2) adding an aromatic aldehyde solvent, an acetalation catalyst, and a phase transfer catalyst into the fermentation broth, and carrying out acetalation reactions of 1,3-propylene glycol under stirring; (3) allowing the reaction liquid to stand still for a while to carry out layering, wherein the aromatic aldehyde solvent and acetalation products are in the upper layer (organic phase layer), and the lower layer (water phase layer) is removed through phase separation; (4) subjecting the obtained organic phase layer to distillation to obtain acetalation products; (5) adding pure water and a hydrolysis catalyst to carry out hydrolysis of the acetalation products, allowing the system to stand still for a while to carry out layering, wherein the aromatic aldehyde solvent is the organic phase layer, and 1,3-propylene glycol enters the water phase layer, and filtering the water phase layer or subjecting the water phase layer to centrifugation to remove the catalyst; (6) subjecting the obtained water phase layer to rectification and dehydration, and carrying out rectification to collect the 1,3-propylene glycol fraction. The extraction method has the advantages that the technology is simple, no toxic extracting agent is used, and the purity and yield of product are high.

Description

technical field [0001] The invention belongs to the field of biotechnology, and relates to a separation technology of microbial fermentation products, in particular to a method for separating and extracting 1,3-propanediol in a 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 characteris...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/20C07C29/80C07C29/92
Inventor 王崇辉孙启梅高大成
Owner CHINA PETROLEUM & CHEM CORP
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