CN101172945A - Method for concentration of lactic acid in fermentation liquor - Google Patents

Method for concentration of lactic acid in fermentation liquor Download PDF

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Publication number
CN101172945A
CN101172945A CNA2007100562511A CN200710056251A CN101172945A CN 101172945 A CN101172945 A CN 101172945A CN A2007100562511 A CNA2007100562511 A CN A2007100562511A CN 200710056251 A CN200710056251 A CN 200710056251A CN 101172945 A CN101172945 A CN 101172945A
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lactic acid
phase
polymkeric substance
salt
rich
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陈继
邓岳锋
张冬丽
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Changchun Institute of Applied Chemistry of CAS
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Changchun Institute of Applied Chemistry of CAS
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Abstract

The invention relates to a method for collecting lactic acid from zymotic fluid, and comprises the steps as follows: the proper double aqueous phase system is selected to adjust the distribution of the lactic acid and the lactobacillus in the double aqueous phase system, the lactic acid is distributed at a polymer-rich phase, and the lactobacillus is distributed at a salt-rich phase to achieve the lactic acid collecting. The selected double aqueous phase system is a neutral extracting system close to the PH valve of 5.5 to 6.0 required by zymolysis of the lactic acid, the finished product is separated from the reacting matters. The phase separation provides a reaction power for the zymolysis of the lactic acid, so that the invention is beneficial to improve the productivity of the lactic acid. Moreover, the method disclosed in the invention can be coupled with the zymotic method of the lactic acid to reform the prior separating method of the lactic acid.

Description

A kind of method of enrichment Lactic Acid from Fermentation Broth
Technical field
The present invention relates to a kind of method of enrichment Lactic Acid from Fermentation Broth.
Background technology
Lactic acid is one of widely used in the world three big organic acids, has another name called lactic acid.Lactic acid is mainly used in industries such as food, medicine, medicine, light industry, chemical industry, is that raw material can obtain a series of lactic acid derivativess with important use with lactic acid.In recent years, along with the growing tension of resource and people growing interest, be that raw material synthetic degradable polymer poly(lactic acid) has caused world scientific research personnel's extensive concern with lactic acid to environmental issue.At present, the main stream approach of synthesizing lactic acid is a fermentation method.The extraction of lactic acid is refining to be the important step of thick product being produced finished product lactic acid, and in the lactic fermentation method, the expense that extraction fine purification of lactic acid process expends is the over half of whole lactic acid-producing cost.Therefore, be the research focus for the refining improvement technology of the extraction of lactic acid-producing always.Traditional lactic acid-producing adopts calcium salt method, and this method changes lactic acid into calcium lactate with lime carbonate earlier, by crystallization calcium lactate is proposed from fermented liquid.Calcium lactate is a lactic acid with vitriol oil acidolysis, and lactic acid obtains product after purifying through operations such as further decolouring, ion-exchanges.This method extraction treating process is various, and labour intensity and production cost are very big, and quality product is also unstable.The synthetic bottleneck that has become the lactic acid industrial development of lactic acid, however lactic acid synthetic gordian technique is that lactic acid separates from fermented liquid.Owing to have shortcomings such as efficient is low, cost is high, separation is difficult, method steps is many in the traditional zymotic production process, many fermentation novel methods have appearred, as methods such as ion exchange method, distillation method, electrodialysis fermentation, film fermentation, extractive fermentations, wherein Yan Jiu focus is an extractive fermentation.Extractive fermentation is to utilize organic solvent continuous extraction separate fermentation product during the fermentation, thereby eliminates the restraining effect of product, and its fermenting process energy consumption is low, the good and no bacteria pollution of selectivity.The extraction agent that the research of bibliographical information extractive fermentation is used mainly is divided three classes: oxygen-hydrogen bond extraction agent that (1) is traditional, as methyl iso-butyl ketone (MIBK) (MIBK), octanol etc.; (2) phosphorus extractant is as tributyl phosphate (TBP) etc.; (3) amine extractant is as Aliquat 336 and Alamine etc.(G.Kyuchoukov such as G.Kyuchoukov, et al.Ind.Eng.Chem.Res.2005,44,5733-5739.) studied with Aliquat 336 as extraction agent, dodecane and positive certain herbaceous plants with big flowers alcohol are the extraction system of thinner, and the pH value is to the influence of lactic acid partition ratio.The advantage of this method is that energy consumption is low, selectivity is high, separation efficiency is high, the industrialization technology maturation, but also exist extraction agent and zymophyte to require height and extraction agent to have shortcomings such as toxicity to environment PH.
Double-aqueous phase system refers to that polymer/polymer, polymkeric substance/salt or salt/salt surpass certain threshold concentration in the aqueous solution, and the system of upper and lower two waters that form.The application of double water-phase aspect biomacromolecule has the characteristics of natural green, because most of protein, nucleic acid and various organoid and cell be easily inactivation sex change in organic solvent system, and double water-phase itself is the aqueous solution system by 85-95%, become the polymkeric substance of phase, and inorganic salts all has Bc, can keep the activity of biological substance.In addition, but double water-phase is easy to amplification and serialization, and working conditions is gentle, saves energy consumption, has been applied in the recovery of cell widely, extracts protein and enzyme and the bio-transformation that combines with the extracting and separating of product from fermented liquid.Therefore, this technology is the focus that people pay close attention at biological technical field in the time of the nearly half a century till now of coming out always, and no matter from basic theories, fundamental research, to novel method technology and industrialization aspect, development is also quite ripe.(Chen Ji etc. such as Chen Ji and Liu Huizhou, the three phase extraction single stage method is extracted process to purify penicillin, Chinese invention patent number: ZL00107655.8) on the basis of aqueous two-phase extraction penicillin research,, invented the novel method of three phase extraction single stage method in conjunction with present traditional method is innovated improvement.(J.K.Yun, et al.Biotechnol.Bioeng.1996,50 such as Yun, 280-290.) reported and utilized polyethylene diamines/hydroxy ethers Mierocrystalline cellulose double-aqueous phase system extracting and separating lactic acid, lactic acid is distributed in phase, and milk-acid bacteria is distributed in down phase, obtains higher percentage extraction.
Summary of the invention
The objective of the invention is to overcome in the existing lactic fermentation process, there are problems such as efficient is low, cost is high, separation is difficult, method steps is many in the extraction of lactic acid, proposes to utilize the method for the lactic acid in polymkeric substance/salt double-aqueous phase system enrichment fermented liquid.By selecting suitable double-aqueous phase system to regulate lactic acid and the distribution of milk-acid bacteria in double-aqueous phase system, make lactic acid be distributed in polymer-rich phase, milk-acid bacteria is distributed in rich salt face, reaches the lactic acid enrichment.The present invention has set up the lactic acid method of utilizing in polyoxyethylene glycol/salt double-aqueous phase system enrichment fermented liquid, has studied the influence to the lactic acid partition ratio of the concentration of inorganic salt and lactic acid concn.Because the double-aqueous phase system that adopts is neutral extraction system, close with lactic acid fermented appropriate pH=5.5~6.0, and make product and reactants separate, this being separated provides a kind of lactic acid fermented reaction power, improved the productivity of lactic acid, therefore this technology can be in the fermentation process coupling of lactic acid, and the method for a kind of green, efficient, easy, energy-conservation enrichment Lactic Acid from Fermentation Broth is provided.
The method of a kind of enrichment Lactic Acid from Fermentation Broth of the present invention, step and condition are as follows:
(1) is that to add massfraction in the aqueous solution of 10000ug/mL~30000ug/mL be 20% polymkeric substance at lactic acid concn, stirs polymkeric substance is dissolved fully, form homogeneous system;
(2) adding massfraction in above-mentioned homogeneous system is 9.09%~37.5% inorganic salt, stirs inorganic salt are dissolved fully, forms double-aqueous phase system, leaves standstill phase-splitting, and the lactic acid in the aqueous solution is enriched in polymer-rich phase;
(3) separate two-phase, polymer-rich phase goes out lactic acid by fractionation by distillation, and polymkeric substance of Hui Shouing and salt reusable edible descend mutually rich salt face reusable edible in fermentation process simultaneously;
Described polymkeric substance is a polyoxyethylene glycol, preferentially selects Macrogol 4000 for use;
Described inorganic salt are dipotassium hydrogen phosphate, ammonium sulfate or sodium sulfate.
Utilize the concentration of lactic acid in the high-performance liquid chromatogram determination upper and lower phase, by formula 1 dispensed ratio.
Figure S2007100562511D00041
Formula 1
Compared with the prior art, the advantage of the lactic acid method in a kind of enrichment fermented liquid provided by the invention is:
1. double-aqueous phase system has and can design and modulability, select different double-aqueous phase systems can control reactant and the distribution of product in double water-phase, being separated provides a kind of fermentation reaction motivating force, can improve the productivity of lactic acid, reaches the separation and the enrichment of lactic acid.
In the double-aqueous phase system partition ratio of lactic acid near 10.
3. double-aqueous phase system is neutral extraction system, close with lactic acid fermented appropriate pH=5.5~6.0, double water-phase becomes phase component to have low toxicity, the advantage of low volatility and biodegradability, and zymophyte is had no side effect, and is a kind of green and separation method efficiently.
4. but double-aqueous phase system is easy to amplify and serialization, and working conditions is gentle, can save energy consumption.
Description of drawings
Fig. 1 three hypophosphite monohydrate hydrogen dipotassium massfractions are to the figure that influences of lactic acid partition ratio.
Fig. 2 ammonium sulfate massfraction is to the figure that influences of lactic acid partition ratio.
Fig. 3 sodium sulfate quality mark is to the figure that influences of lactic acid partition ratio.
Fig. 4 PEG/K 2HPO 4Lactic acid concn is to the figure that influences of partition ratio in the double-aqueous phase system.
Embodiment
Embodiment 1
(1) get the aqueous solution that the 5mL lactic acid concn is 20000ug/mL respectively, all add the 1.25g Macrogol 4000, stirring is dissolved it fully, forms homogeneous system.
(2) in above-mentioned homogeneous system, add the K of 0.5g, 1.0g, 1.5g, 2.0g, 2.5g, 3.0g different mass respectively 2HPO 43H 2O, stirring is dissolved inorganic salt fully, forms double-aqueous phase system.Leave standstill phase-splitting, the lactic acid in the aqueous solution is enriched in rich polyoxyethylene glycol phase.
(3) separate two-phase, rich polyoxyethylene glycol goes out lactic acid by fractionation by distillation, and polyoxyethylene glycol of Hui Shouing and salt reusable edible descend mutually rich salt face reusable edible in fermentation process simultaneously.
According to the partition ratio of above-mentioned formula 1 calculating lactic acid, the result as shown in Figure 1.
Embodiment 2
According to the method for embodiment 1, but the salt that adds is ammonium sulfate.According to the partition ratio of above-mentioned formula 1 calculating lactic acid, the result as shown in Figure 2.
Embodiment 3
According to the method for embodiment 1, but the salt that adds is sodium sulfate.According to the partition ratio of above-mentioned formula 1 calculating lactic acid, the result as shown in Figure 3.
Embodiment 4
(1) getting concentration respectively is 10000 μ g/mL, 15000 μ g/mL, 20000 μ g/mL, 25000 μ g/mL, 30000 μ g/mL lactic acid solution 5mL, adds the 1.25g Macrogol 4000 respectively, stirs it is dissolved fully, forms homogeneous system.
(2) in above-mentioned homogeneous system, add 2g K respectively 2HPO 43H 2O, stirring is dissolved inorganic salt fully, forms double-aqueous phase system.Leave standstill phase-splitting, the lactic acid in the aqueous solution is enriched in rich polyoxyethylene glycol phase.
(3) separate two-phase, rich polyoxyethylene glycol goes out lactic acid by fractionation by distillation, and polyoxyethylene glycol of Hui Shouing and salt reusable edible descend mutually rich salt face reusable edible in fermentation process simultaneously.
According to the partition ratio of above-mentioned formula 1 calculating lactic acid, the result as shown in Figure 4.

Claims (2)

1. the method for an enrichment Lactic Acid from Fermentation Broth is characterized in that, step and condition are:
(1) is that to add massfraction in the aqueous solution of 10000ug/mL~30000ug/mL be 20% polymkeric substance at lactic acid concn, stirs polymkeric substance is dissolved fully, form homogeneous system;
(2) adding massfraction in above-mentioned homogeneous system is 9.09%~37.5% inorganic salt, stirs inorganic salt are dissolved fully, forms double-aqueous phase system, leaves standstill phase-splitting, and the lactic acid in the aqueous solution is enriched in polymer-rich phase;
(3) separate two-phase, polymer-rich phase goes out lactic acid by fractionation by distillation, and polymkeric substance of Hui Shouing and salt reusable edible simultaneously, time mutually rich salt face reusable edible are in fermentation process:
Described polymkeric substance is a polyoxyethylene glycol;
Described inorganic salt are dipotassium hydrogen phosphate, ammonium sulfate or sodium sulfate.
2. the method for a kind of enrichment Lactic Acid from Fermentation Broth as claimed in claim 1 is characterized in that, described polymkeric substance is a Macrogol 4000.
CNA2007100562511A 2007-10-30 2007-10-30 Method for concentration of lactic acid in fermentation liquor Pending CN101172945A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112194721A (en) * 2019-10-29 2021-01-08 西北农林科技大学 Double-solution mixed extraction system and application thereof in ostrich liver
CN113336639A (en) * 2021-06-11 2021-09-03 万华化学(四川)有限公司 Method for purifying lactic acid by aqueous two-phase extraction
CN115097037A (en) * 2022-06-22 2022-09-23 华润双鹤药业股份有限公司 Method for detecting lactic acid in pentazocine injection

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112194721A (en) * 2019-10-29 2021-01-08 西北农林科技大学 Double-solution mixed extraction system and application thereof in ostrich liver
CN112194721B (en) * 2019-10-29 2022-12-23 西北农林科技大学 Double-solution mixed extraction system and application thereof in ostrich liver
CN113336639A (en) * 2021-06-11 2021-09-03 万华化学(四川)有限公司 Method for purifying lactic acid by aqueous two-phase extraction
CN113336639B (en) * 2021-06-11 2023-12-19 万华化学(四川)有限公司 Method for purifying lactic acid by aqueous two-phase extraction
CN115097037A (en) * 2022-06-22 2022-09-23 华润双鹤药业股份有限公司 Method for detecting lactic acid in pentazocine injection
CN115097037B (en) * 2022-06-22 2024-03-29 华润双鹤药业股份有限公司 Method for detecting lactic acid in pentazocine injection

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