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Method for separating and purifying 1,3-propylene glycol from fermentation liquor

A fermentation broth, propylene glycol technology, applied in the biological field, can solve the problems of low separation and extraction yield, small separation capacity, serious equipment corrosion, etc., and achieve the effect of strengthening flocculation effect and high separation degree.

Active Publication Date: 2014-01-08
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.
In these processes, concentration and water removal are all indispensable steps no matter before or after. When concentrating, because the water content of the fermentation broth is high (more than 80%) and the product concentration is very low, when concentrating with the method of direct evaporation, a large amount of The steam will carry the product and steam out together. The experimental results show that the carrying phenomenon is more serious especially in the later stage of concentration when the water content is low, and the loss is as high as 7% to 15%.
Such as CN1460671A adopts the concentration method of direct evaporation, and CN1887835A adopts a rotary evaporator to concentrate under reduced pressure, which will cause a large loss of 1,3-propanediol. Although the steamed water is large and of good quality, it can be returned to the fermentation system for reuse, but from It is very uneconomical economically, which is one of the main reasons for the low yield of 1,3-propanediol separation and extraction
Moreover, in the above method, except that the first step is carried out under non-acidic conditions, the subsequent steps are all carried out under strong acidic conditions, and the equipment is seriously corroded, which is not conducive to large-scale application.
The disclosed method of CN1880290A adopts rectification tower operation to concentrate and remove water, and the main problem of existence is that the concentration efficiency is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The fermented liquid that present embodiment is processed is to be substrate with glycerol, adopts Klebsiella fermentation, Ca(OH) 2 The 1,3-propanediol fermentation liquid obtained by neutralizing the carbon dioxide produced in the fermentation process has a content of 1,3-propanediol of 78.5 g / L and a pH value of 7.0 at the end of fermentation.

[0036] Take 20L of the above-mentioned fermentation broth, filter to remove bacteria and sediment, the filtration rate is 7.4l / h, the filtrate is clear and transparent, then adjust the pH value to 4.6 with 8mol / L sulfuric acid, heat to 95°C under stirring, and keep the temperature for 0.5h. Naturally cool down to room temperature and then filter to obtain a transparent fermented serum. The pH was adjusted to 6.8 with NaOH, and the precipitate was removed by filtration. Atmospheric pressure falling film-scraping film evaporation method is adopted, and packing columns are installed on the gas phase pipeline after vapor-liquid ...

Embodiment 2

[0039] The 1,3-propanediol fermentation broth used in this example is the same as that in Example 1.

[0040] Take 50L of fermentation broth, filter to remove bacteria and sediment, adjust the pH value of the clear liquid to 3.0 with 6mol / L hydrochloric acid, heat to 85°C with stirring, keep the temperature for 1 hour, naturally cool down to room temperature, and filter to obtain a transparent fermentation clear liquid . with Ca(OH) 2 Adjust the pH to 6.2, and remove the precipitate by filtration. The vacuum falling film-scraping film evaporation method is adopted, and the packing column is installed on the gas phase pipeline after the vapor-liquid separation. The vacuum degree is 200mmHg, and the operating temperature is 40-60°C. Concentrate first the water that accounts for 72.3% (mass fraction) of the water amount in the clear liquid, then filter to remove the precipitated salt, continue to concentrate according to the above conditions to remove the remaining water, and ...

Embodiment 3

[0043] The 1,3-propanediol fermentation broth used in this example is the same as that in Example 1.

[0044] The difference with Example 1 is: no packing column is added to concentrate the fermented supernatant in two steps, the first step concentrates the water amount to 58.4% (mass fraction) of the total water amount, the second step evaporates to remove the remaining water, and evaporates the water with The amount of 1,3-propanediol is 9.3% of the total content. Other processes and conditions are the same as in Example 1.

[0045] Distill under reduced pressure at a vacuum of 6mmHg to obtain a concentrated solution containing 1,3-propanediol, collect 1,3-propanediol fractions at 95-98°C, and obtain a product with a purity of 98.1wt% and a recovery rate of 77.1wt%.

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Abstract

The invention discloses a method for separating and purifying 1,3-propylene glycol from 1,3-propylene glycol fermentation liquor. The fermentation liquor treated by the method is calcium salt fermentation liquor. The method comprises the following steps of: removing microbial thalli and calcium salt; regulating to reach acidity and removing protein and insoluble solid matters; regulating to reach alkalinity and removing insoluble solid matters; heating, concentrating and dehydrating and separating crystallization salt out; and rectifying to obtain the 1,3-propylene glycol product, wherein heating and concentrating are performed in two steps, so that a large number of solid precipitates are prevented from being produced due to one-time concentration, solid-liquid separation is easier to perform, and an organic acid byproduct can be effectively recycled. The fermentation liquor treated by the method is the calcium salt fermentation liquor, and calcium ions can form calcium carbonate precipitates with carbon dioxide produced due to metabolism of microorganisms in the fermentation process, so that the normal proceeding of the fermentation process is facilitated; and when the product is separated, the calcium carbonate precipitates can serve as filter aids, so that the separation and removal of the microbial thalli are facilitated.

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): C07C31/20C07C29/74C07C29/78C12P7/18C07C55/10C07C59/08C07C51/02C07C51/43C12R1/22
Inventor 王崇辉
Owner CHINA PETROLEUM & CHEM CORP
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