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Method for adsorbing and extracting 1,3-propanediol from zymotic fluid by using cationic resin

A cationic resin, adsorption and extraction technology, applied in the field of separation of microbial fermentation products, can solve the problems of 1,3-propanediol recovery research that has not yet been carried out, existing methods are complicated, and the amount of fermentation liquid is large, so as to reduce material consumption, low cost, The effect of large adsorption capacity

Active Publication Date: 2012-11-28
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the low concentration of 1,3-propanediol in the fermentation broth, the amount of fermentation broth to be processed is relatively large, so the problem of this method is that the process energy consumption is relatively high, and pretreatment processes such as desalination and deproteinization are required
Although this method can realize the simultaneous separation of microbial cells and 1,3-propanediol and simplify the separation process, the problem is that the recovery of the target product 1,3-propanediol after extraction has not yet been carried out.
[0011] In the above extraction and separation methods, either the method is too complicated, or the reagents used are toxic, the cost is high, or there are problems such as large energy consumption and serious environmental pollution, which are not conducive to the large-scale production of fermented 1,3-propanediol

Method used

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  • Method for adsorbing and extracting 1,3-propanediol from zymotic fluid by using cationic resin
  • Method for adsorbing and extracting 1,3-propanediol from zymotic fluid by using cationic resin
  • Method for adsorbing and extracting 1,3-propanediol from zymotic fluid by using cationic resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The fermented broth treated in this example uses waste glycerol as a substrate, and is fermented by Clostridium butyricum to produce 1,3-propanediol fermented broth, with a pH of 7.0 at the end of fermentation; wherein the concentration of 1,3-propanediol is 52 g / L, glycerin The concentration is 2g / L.

[0042] (1) Take the above fermentation broth, add 1wt% flocculant and 0.2wt% powdered activated carbon, stir for 60min, let stand and settle naturally;

[0043] (2) Remove bacteria and protein by plate and frame filtration to obtain supernatant;

[0044] (3) At 25°C, add 1.0g of wet resin and an appropriate amount of supernatant to a 250mL Erlenmeyer flask, place the Erlenmeyer flask on a constant temperature shaker, and perform adsorption at 150r / min. When 1,3- When the concentration of propylene glycol no longer changes, it means that the resin has reached saturation; then measure the concentration of 1,3-propanediol in the solution, and calculate the saturated adsorp...

Embodiment 2

[0049] The fermented broth treated in this example uses waste glycerol as a substrate, and is fermented by Clostridium butyricum to produce 1,3-propanediol fermented broth. The pH at the end of fermentation is 7.0, and the concentration of 1,3-propanediol is 52 g / L.

[0050] (1) Take a certain amount of the above fermentation broth, adjust the pH to 1.0 with 2moL / L sulfuric acid, add 3wt% chitosan and 0.3wt% powdered activated carbon, stir at 150r / min for 30min, and let it settle.

[0051] (2) Centrifuge at 3000r / min after the flocs are completely precipitated to obtain a colorless and transparent supernatant.

[0052] (3) Take 20g of 001×4 resin and fill it in a glass column with an inner diameter of 1.0cm to prepare the adsorption column I, put the supernatant on the column, control the flow rate at 0.5mL / min, and reach saturation after 90min of adsorption, it can be known that 001× 4 The equilibrium adsorption capacity of the resin is 105.2 mg / g.

[0053] (4) Wash away imp...

Embodiment 3

[0058] The fermented broth treated in this example uses waste glycerol as a substrate, and is fermented by Clostridium butyricum to produce 1,3-propanediol fermented broth. The pH of the fermentation end is 7.0, and the concentration of 1,3-propanediol is 56.5 g / L.

[0059] (1) Take a certain amount of the above-mentioned fermentation broth, adjust it to pH 3.0 with 2moL / L hydrochloric acid, add 5wt% chitosan and 0.5wt% powdered activated carbon, stir at 150r / min for 30min, and let it settle;

[0060] (2) After the flocs are completely precipitated, they are filtered through a plate frame to obtain a colorless and transparent supernatant;

[0061] (3) Take 20g of D101 resin and fill it into a glass column with an inner diameter of 1.0cm to prepare an adsorption column II. Put the supernatant on the column for adsorption, the flow rate is controlled at 2.0mL / min, and it reaches saturation after 30 minutes of adsorption. It can be seen that the D101 resin The equilibrium adsorpt...

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Abstract

The invention discloses a method for adsorbing and extracting 1,3-propanediol from a zymotic fluid by using cationic resin, which relates to a method for separating a microbial fermentation product. The method comprises the following steps of: adjusting the pH of a 1,3-propanediol zymotic fluid to 1-7, adding a flocculating agent and active carbon, stirring, standing and naturally settling; removing thalli, proteins and other insoluble solid particles in the obtained zymotic fluid with a centrifuging or filtering method to obtain a supernatant; adsorbing 1,3-propanediol in the obtained supernatant by using cationic resin, and loading onto a column at the flow speed of 0.5-2.0mL / min; adsorbing with a resin column to a saturated state, washing, eluting, and collecting an eluent; and distilling the obtained eluent which contains 1,3-propanediol under reduced pressure to obtain a 1,3-propanediol product of which the purity is 98-99.6 percent. The method has the advantages of freeness from pollution, small investment, reduction in the separating cost of 1,3-propanediol, saving in time and increase in production efficiency.

Description

technical field [0001] The invention relates to a method for separating microbial fermentation products, in particular to a method for extracting 1,3-propanediol in fermentation broth by adsorption with cationic resin. Background technique [0002] 1,3-Propanediol (1,3-PD) is an important chemical raw material widely used in cosmetics, liquid detergents, antifreeze, clothing, interior decoration materials, engineering polymers and many other fields. As a diol containing two functional groups, 1,3-propanediol can be used in a variety of organic synthesis reactions, especially as a monomer for the synthesis of polyesters, polyethers and polyurethanes. One of its most important uses Polytrimethylene terephthalate (PTT) is formed with terephthalic acid. PTT has excellent performance and broad application prospects. The national chemical fiber department has included the development of PTT in the "Tenth Five-Year Plan" synthetic fiber product structure adjustment plan. At prese...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/76C07C29/94
Inventor 方柏山代洪飞王世珍彭雅娟
Owner XIAMEN UNIV
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