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Method for producing alpha-calcium sulfate hemihydrate whiskers and synchronously recovering lactic acid monomers by taking fermentation liquor for producing lactic acid by calcium salt method as raw material

A technology of calcium sulfate hemihydrate and lactic acid monomer, which is applied in the separation/purification of calcium/strontium/barium sulfate, carboxylic acid compounds, organic chemistry, etc. Insufficient green environmental protection and other problems, to achieve the effect of reducing the input of lactic acid production

Active Publication Date: 2021-03-26
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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Problems solved by technology

[0013] The above methods for preparing α-calcium sulfate hemihydrate whiskers all use calcium sulfate dihydrate as the starting material, and most of the production process needs to be carried out at a temperature higher than 120°C, and some methods also need to add different compounds. Not only increase the manufacturing cost, but also increase the generation of by-products
It can be seen that the production technology of the existing α-calcium sulfate hemihydrate whiskers cannot directly prepare lactic acid monomers from the lactic acid fermentation liquid of the calcium salt method while preparing α-calcium sulfate hemihydrate whiskers
In addition, too high reaction temperature and the addition of crystallization agent will significantly affect the recovery of lactic acid monomer
[0014] So far, the release process of lactic acid in the calcium lactate produced in the process of producing lactic acid by the calcium salt method is based on the formation of calcium sulfate by-products, and the synchronization of the formation of lactic acid release and the preparation of α-calcium sulfate hemihydrate whiskers has not been realized. It is necessary to further process calcium sulfate "solid waste" in subsequent production, which not only increases production costs but also makes the production process not green enough

Method used

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  • Method for producing alpha-calcium sulfate hemihydrate whiskers and synchronously recovering lactic acid monomers by taking fermentation liquor for producing lactic acid by calcium salt method as raw material
  • Method for producing alpha-calcium sulfate hemihydrate whiskers and synchronously recovering lactic acid monomers by taking fermentation liquor for producing lactic acid by calcium salt method as raw material
  • Method for producing alpha-calcium sulfate hemihydrate whiskers and synchronously recovering lactic acid monomers by taking fermentation liquor for producing lactic acid by calcium salt method as raw material

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preparation example Construction

[0032] 1. Preparation of lactic acid fermentation broth by calcium salt method

[0033] The preparation of calcium salt method lactic acid fermentation liquid is carried out according to the method of the previous invention authorized patent (Wang Zhengxiang et al., ZL201580000781.7). The fermentation strain is CGMCC 11059 or CGMCC11060, and the strain CGMCC 11059 is used for the fermentation production of D-lactic acid. CGMCC11060 is used for the fermentative production of L-lactic acid (Wang Zhengxiang et al., ZL201580000781.7). In the initial stage of fermentation, add glucose to the basic fermentation medium to a final concentration of 10-50 g / L, culture at 30°C-37°C, pH 5.5-7.5, ventilation 0.1-2.0 vvm, 100-1000 r / min stirring The culture time is 5-15 h, and the bacterial volume reaches 10-50OD; close the ventilation, reduce the stirring speed to 0-300 r / min, increase the fermentation temperature to 37°C-50°C, and add a final concentration of 16%-25 % glucose solution, t...

Embodiment 1

[0048] Embodiment 1: the preparation of lactic acid fermentation broth

[0049]Inoculate the glycerol tube frozen storage of D-lactic acid-producing strain CGMCC 11059 or L-lactic acid-producing strain CGMCC 11060 into 50 mL of LB liquid medium, and culture it on a shaker at 37°C and 200 r / min for 12 h. First-class seed liquid. The primary seed solution was inoculated in 150 mL of M9 liquid medium with glucose as the carbon source, the initial sugar concentration was 0.5%, and cultured on a shaker at 37°C and 200 r / min for 10 h as the secondary seed solution. The secondary seed liquid was inoculated into a fermenter containing M9 liquid medium according to the inoculation amount of the initial OD value of 0.3. After inoculation, the initial volume of the 50 L fermenter was 25 L, and the initial addition of invert syrup was 3%. Body fermentation production. The initial temperature of the fermentation was controlled at 37°C, and the pH was maintained at 6.5 with ammonia water....

Embodiment 2

[0052] Embodiment 2: the preparation of α-calcium sulfate hemihydrate whisker

[0053] The lactic acid fermentation liquid obtained in the above-mentioned Example 1 was heated to 88° C. in the reactor and maintained at this temperature, and 5 mol / L sulfuric acid solution was added under stirring at 20 r / min. The total amount of sulfuric acid was controlled so that the molar ratio of lactic acid to sulfuric acid was 1:0.5, the time limit for adding all the sulfuric acid solution is controlled at 1 h / ton of fermentation broth; after adding all the sulfuric acid solution, keep the reaction for 15 min; The collected solid part is the α-calcium sulfate hemihydrate whisker, and the obtained α-calcium sulfate hemihydrate whisker is washed with absolute ethanol and flash-dried by steam at 120°C, and it is α-calcium sulfate hemihydrate crystal The finished product; the collected liquid part is the free lactic acid liquid containing lactic acid monomer, which is filtered through a plate...

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Abstract

The invention discloses a method for producing alpha-calcium sulfate hemihydrate whiskers and synchronously recovering lactic acid monomers by taking fermentation liquor for producing lactic acid by calcium salt method as a raw material The method comprises the following steps: 1) after lactic acid fermentation is finished, heating fermentation liquor; 2) starting stirring, and adding sulfuric acid for reaction; 3) after the reaction is finished, filtering and collecting a solid part, namely alpha-calcium sulfate hemihydrate whiskers, and collecting a liquid part, namely free lactic acid liquid containing lactic acid monomers; and 4) washing and drying the obtained alpha-calcium sulfate hemihydrate whiskers to obtain a finished product of the alpha-calcium sulfate hemihydrate whiskers, filtering and concentrating the obtained free lactic acid liquid to obtain a lactic acid crude product, and refining to obtain the high-purity lactic acid monomer. The method can replace lactic acid efficient separation and high added value conversion of calcium sulfate by-products in existing calcium salt method lactic acid production, significantly reduces lactic acid refining cost and waste formation, and is beneficial to lactic acid production quality improvement and post-extraction process technology simplification.

Description

technical field [0001] The invention belongs to the fields of fermentation engineering and chemical engineering, and in particular relates to the direct transformation of calcium lactate fermented liquid into α-calcium sulfate hemihydrate whiskers and free lactic acid under the action of sulfuric acid during lactic acid fermentation production. Background technique [0002] Lactic acid is an important three-carbon organic acid, which has two optical configurations of L-type and D-type, namely: L-lactic acid and D-lactic acid. Both L-lactic acid and D-lactic acid are monomer raw materials for polylactic acid synthesis and are important components of biodegradable materials. In addition, L-lactic acid and D-lactic acid are also used as raw materials for the synthesis of various esters (such as methyl lactate, ethyl lactate, propyl lactate, butyl lactate) and lactate. L-lactic acid is also widely used as an acidulant It is used in the production of food, beverage, condiment, w...

Claims

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Application Information

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IPC IPC(8): C01F11/46C07C51/42C07C51/47C07C59/08
CPCC01F11/46C07C51/42C07C51/47C01P2004/10C01P2004/01C07C59/08C12P7/00C07C51/02
Inventor 王正祥牛丹丹田康明路福平申春莉
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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