CN102976923B - New process for extracting lactic acid from lactic acid fermentation liquid - Google Patents
New process for extracting lactic acid from lactic acid fermentation liquid Download PDFInfo
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Abstract
The invention discloses a new process for extracting lactic acid from lactic acid fermentation liquid. The process flow comprises the following steps: preparing the fermentation liquid, deproteinizing, removing bacteria, decolorizing with activated carbon, performing plate and frame filtration, filtering with an inorganic ceramic membrane, cooling by a plate type heat exchanger, filtering with an organic nano-filtration membrane, concentrating and performing primary crystallization, performing centrifugal drying, performing resolvation, performing acidolysis, passing through an ion exchange resin column and concentrating to obtain a finished product. The process flow performs membrane filtration twice, namely the filtration with the inorganic ceramic membrane and the filtration with the organic ceramic membrane, wherein the filtration with the inorganic ceramic membrane can remove small insoluble solid impurities, bacteria, colloidal substances, macromolecular sugars and other impurities in filtrate; the filtration with the organic nano-filtration membrane can remove low-molecular weight sugars and multivalent ions in the filtrate; and the purity of the finally prepared finished product lactic acid is as high as 95%-98%, the crystallization yield of the lactic acid is improved from original 70% to above 85%, and the production cost is greatly reduced.
Description
Technical field
The present invention relates to a kind of technique of isolation andpurification lactic acid, specifically relate to the technique of a kind of film isolation andpurification lactic acid from lactic acid fermentation liquid.
Background technology
Lactic acid, as a kind of important organic acid, is extensively present in human body, animal body and plant.Lactic acid, lactic acid salt and derivative thereof, have a wide range of applications in food, feed, chemical industry and medicine and other fields.In recent years, the poly (l-lactic acid) that Pfansteihl polymerization generates is as type material, the biodegradable plastic manufactured, environmentally friendly packing material and family expenses film etc., solve day by day serious problem of environmental pollution, cause the extensive concern in the world, be considered to new millennium the most rising novel material, application prospect is boundless.
The production method of lactic acid comprises fermentation method, chemical synthesis and enzyme process.At present, the production of the Pfansteihl of high-optical-purity is based on fermentable, and fermented bacterium is Bacterium lacticum, Rhizopus oryzae etc.The problems such as to the extraction and isolation of lactic acid fermentation liquid, that crystallization-acidolysis process exists extraction yield to the calcium lactate that China generally adopts at present is low, and finished product purity is not high, shelf stability difference.
The flow process of calcium lactate crystallization-acidolysis process is roughly as follows:
Upstream fermentation liquid, after intensification, alkalinisation treatment, removes thalline, protein isocolloid impurity.The calcium lactate mash obtained is through condensing crystal, and centrifugation removing mother liquor, obtains calcium lactate crystal.Heating carries out acidolysis with sulfuric acid after redissolving, and adds proper amount of active carbon decolouring, is separated and removes calcium sulfate and gac residue, obtain crude lactic acid solution.Then by crude lactic acid solution respectively by anion and cation exchange resin, remove foreign ion wherein, gained solution is again through being concentrated into more than 80%, and get product lactic acid solution.
This technique has and is easy to control, and advantages such as equipment requirements is simple, but product extraction yield is low, purity is not high.The reason that current lactic acid extraction rate is low and purity is not high is caused to have: the major impurities such as the carbohydrate in fermented liquid, protein and pigment can not effectively be removed, and significantly affects calcium lactate percent crystallization in massecuite and purity; Repeatedly activated carbon decolorizing is adopted to make the rate of loss of calcium lactate and lactic acid up to 30%; Except sugar is insufficient in technique, the residual sugar in finished product lactic acid or other reducing substances is caused to affect the quality of product.
Summary of the invention
Based on the deficiency of calcium lactate crystallization-acidolysis process, the invention provides a kind of novel process extracting lactic acid from lactic acid fermentation liquid.
Its technical solution is:
From lactic acid fermentation liquid, extract a novel process for lactic acid, it comprises the following steps:
(1) lactic acid fermentation liquid is heated to 80 ~ 90 DEG C, add calcium hydroxide and regulate pH to 10 ~ 12, insulated and stirred is filtered after 15 ~ 60 minutes and is obtained feed liquid 1;
(2) in feed liquid 1, add flocculation agent polyacrylamide, leave standstill after 1 ~ 6 hour, filter and obtain filtrate 2;
(3) decolour to filtrate 2 with gac, the mass ratio of gac and lactic acid fermentation liquid is 0.05: 100 ~ 1: 100, and bleaching temperature is 65 ~ 80 DEG C, and bleaching time is 30 ~ 70min, then priority sheet frame and inorganic ceramic membrane filtration obtain filtrate 3;
(4) with plate-type heat exchanger, filtrate 3 is lowered the temperature, make the temperature of filtrate 3 drop to 45 ~ 60 DEG C by 60 ~ 80 DEG C, then filter with organic nanofiltration membrane and obtain filtrate 4;
(5) take successively to concentrate to filtrate 4, decrease temperature crystalline, centrifugal, wash crystalline substance, drying, obtained calcium lactate crystal;
(6) the heavy molten calcium lactate crystal of adding distil water, heating makes it redissolve completely at lower than 80 DEG C, adds sulfuric acid and carries out acidolysis and obtain crude lactic acid;
(7) foreign ion in crude lactic acid is removed by anion and cation exchange resin;
(8) concentrate to obtain finished product lactic acid, its purity is 95% ~ 98%.
Preferably, in step (5): concentrate in triple effect concentrating pan; Decrease temperature crystalline is carried out in crystallization cylinder.
Preferably, in step (6): the weight percent concentration of sulfuric acid is 40% ~ 98%.
Advantageous Effects of the present invention is:
Insufficient based on existing calcium lactate crystallization-acidolysis process removal of impurities, cause needing repeatedly crystallization and percent crystallization in massecuite is not high, finally have impact on purity and the extraction yield of product, present invention process is optimized it, add twice membrane filtration before crystallization, namely inorganic ceramic membrane filtration and organic nanofiltration membrane filter, and wherein, inorganic ceramic membrane filtration eliminates the impurity such as insoluble solid impurities small in filtrate 2, thalline, colloidalmaterial and macromolecular carbohydrate; Organic nanofiltration membrane filters low molecular sugar part and polyvalent ion of eliminating in filtrate 3, thus can fully remove the major impurities such as sugar, protein, pigment, make final obtained finished product lactic acid high purity 95% ~ 98%, and make lactic acid crystallization yield bring up to more than 85% by original 70%, greatly reduce production cost.In addition, present invention process gained waste liquid is because of the monose containing high density, and the raw material that can be used as other products fermentation is utilized, and decreases the discharge of waste liquid.Present invention process adopted activated carbon decolorizing before crystal redissolves simultaneously, simplified the technical process of lactic acid separation and Extraction.
Embodiment
Technical process of the present invention comprises:
Fermented liquid → deproteinated → removal thalline → activated carbon decolorizing → Plate Filtration → inorganic ceramic membrane filtration → plate-type heat exchanger cooling → organic nanofiltration membrane filters → concentrate primary crystallization → centrifugal drying → weight molten → acidolysis → ion exchange resin column → concentrated to obtain finished product.
In order to obtain the lactic product of high quality, high yield, it is critical step that inorganic ceramic membrane filtration and organic nanofiltration membrane filter.Simultaneously in order to enable inorganic ceramic film and organic nanofiltration membrane give full play to its filter effect, and enabling final obtained finished product lactic acid obtain high purity and high crystallization yield, present invention process is distinguished again to some extent carrying out the more existing calcium lactate crystallization-acidolysis process of the pretreatment procedure before twice membrane filtration.PH to 10 ~ 12 are regulated, insulated and stirred 15 ~ 60 minutes as added calcium hydroxide in pretreatment procedure; And for example preferred flocculation agent polyacrylamide, leaves standstill 1 ~ 6 hour; Mass ratio as active carbon for decolorization and lactic acid fermentation liquid is 0.05: 100 ~ 1.5: 100, and bleaching temperature is 65 ~ 80 DEG C, and bleaching time is 30 ~ 70min etc.
Enumerate several embodiment below and carry out more specific detail:
Embodiment 1
Containing glucose, yeast extract, peptone, K
2hPO
4, sodium acetate, MgSO
47H
2o, MnSO
4h
2the inoculation of medium milk-acid bacteria of O, add calcium carbonate as neutralizing agent, fermentation obtains lactic acid fermentation liquid.Be heated to 85 DEG C, add calcium hydroxide and regulate pH to 11, insulated and stirred, after 20 minutes, obtains feed liquid 1 with insolubless such as the calcium carbonate in filter-cloth filtering removing lactic acid fermentation liquid.In feed liquid 1, add flocculation agent polyacrylamide, leave standstill after 4 hours, filter and obtain filtrate 2.Then under the temperature condition of 65 DEG C, be add gac and to decolour in feed liquid 1 40min at 0.05: 100 by the mass ratio of gac and feed liquid 1, then priority sheet frame and inorganic ceramic membrane filtration obtain filtrate 3.With plate-type heat exchanger, 55 DEG C are cooled to filtrate 3, then filter with organic nanofiltration membrane and obtain filtrate 4.It is 160g/L that filtrate 4 is first concentrated to lactate concentration through triple effect concentrating pan, then in crystallization cylinder decrease temperature crystalline, last centrifugal drying obtains calcium lactate crystal.The heavy molten crystal of adding distil water, at 70 DEG C, heating makes it redissolve completely, add weight percent concentration be 45% sulfuric acid carry out acidolysis and obtain crude lactic acid.Remove foreign ion wherein by anion and cation exchange resin, concentrated purity is the finished product lactic acid of 95%.
Embodiment 2
Containing glucose, yeast extract, peptone, K
2hPO
4, sodium acetate, MgSO
47H
2o, MnSO
4h
2the inoculation of medium milk-acid bacteria of O, add calcium carbonate as neutralizing agent, fermentation obtains lactic acid fermentation liquid.Be heated to 80 DEG C, add calcium hydroxide and regulate pH to 12, insulated and stirred, after 30 minutes, obtains feed liquid 1 with insolubless such as the calcium carbonate in filter-cloth filtering removing lactic acid fermentation liquid.In feed liquid 1, add flocculation agent polyacrylamide, leave standstill after 3.5 hours, filter and obtain filtrate 2.Then under the temperature condition of 70 DEG C, be add gac and to decolour in feed liquid 1 40min at 0.1: 100 by the mass ratio of gac and feed liquid 1, then priority sheet frame and inorganic ceramic membrane filtration obtain filtrate 3.With plate-type heat exchanger, 60 DEG C are cooled to filtrate 3, then filter with organic nanofiltration membrane and obtain filtrate 4.It is 140g/L that filtrate 4 is first concentrated to lactate concentration through triple effect concentrating pan, then in crystallization cylinder decrease temperature crystalline, last centrifugal drying obtains calcium lactate crystal.The heavy molten crystal of adding distil water, at 70 DEG C, heating makes it redissolve completely, add weight percent concentration be 65% sulfuric acid carry out acidolysis and obtain crude lactic acid.With activated carbon decolorizing, anion and cation exchange resin removes foreign ion wherein, and concentrated purity is the finished product lactic acid of 98%.
Embodiment 3
Containing glucose, yeast extract, peptone, K
2hPO
4, sodium acetate, MgSO
47H
2o, MnSO
4h
2the inoculation of medium milk-acid bacteria of O, add calcium carbonate as neutralizing agent, fermentation obtains lactic acid fermentation liquid.Be heated to 90 DEG C, add calcium hydroxide and regulate pH to 10, insulated and stirred, after 40 minutes, obtains feed liquid 1 with insolubless such as the calcium carbonate in filter-cloth filtering removing lactic acid fermentation liquid.In feed liquid 1, add flocculation agent polyacrylamide, leave standstill after 3.5 hours, filter and obtain filtrate 2.Then under the temperature condition of 80 DEG C, be add gac and to decolour in feed liquid 1 35min at 1: 100 by the mass ratio of gac and feed liquid 1, then priority sheet frame and inorganic ceramic membrane filtration obtain filtrate 3.With plate-type heat exchanger, 50 DEG C are cooled to filtrate 3, then filter with organic nanofiltration membrane and obtain filtrate 4.It is 120g/L that filtrate 4 is first concentrated to lactate concentration through triple effect concentrating pan, then in crystallization cylinder decrease temperature crystalline, last centrifugal drying obtains calcium lactate crystal.The heavy molten crystal of adding distil water, at 70 DEG C, heating makes it redissolve completely, add weight percent concentration be 60% sulfuric acid carry out acidolysis and obtain crude lactic acid.With activated carbon decolorizing, anion and cation exchange resin removes foreign ion wherein, and concentrated purity is the finished product lactic acid of 97%.
Claims (1)
1. from lactic acid fermentation liquid, extract a technique for lactic acid, it is characterized in that comprising the following steps:
(1) lactic acid fermentation liquid is heated to 80 ~ 90 DEG C, add calcium hydroxide and regulate pH to 10 ~ 12, insulated and stirred is filtered after 15 ~ 60 minutes and is obtained feed liquid 1;
(2) in feed liquid 1, add flocculation agent polyacrylamide, leave standstill after 1 ~ 6 hour, filter and obtain filtrate 2;
(3) decolour to filtrate 2 with gac, the mass ratio of gac and lactic acid fermentation liquid is 0.05: 100 ~ 1: 100, and bleaching temperature is 65 ~ 80 DEG C, and bleaching time is 30 ~ 70min, then priority sheet frame and inorganic ceramic membrane filtration obtain filtrate 3;
(4) with plate-type heat exchanger, filtrate 3 is lowered the temperature, make the temperature of filtrate 3 drop to 45 ~ 60 DEG C by 60 ~ 80 DEG C, then filter with organic nanofiltration membrane and obtain filtrate 4;
(5) take successively to concentrate to filtrate 4, decrease temperature crystalline, centrifugal, wash crystalline substance, drying, obtained calcium lactate crystal;
(6) the heavy molten calcium lactate crystal of adding distil water, heating makes it redissolve completely at lower than 80 DEG C, adds sulfuric acid and carries out acidolysis and obtain crude lactic acid;
(7) foreign ion in crude lactic acid is removed by anion and cation exchange resin;
(8) concentrate to obtain finished product lactic acid, its purity is 95% ~ 98%;
In step (5): concentrate in triple effect concentrating pan; Decrease temperature crystalline is carried out in crystallization cylinder;
In step (6): the weight percent concentration of sulfuric acid is 40% ~ 98%.
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| CN102976923B true CN102976923B (en) | 2015-06-10 |
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103482813A (en) * | 2013-10-08 | 2014-01-01 | 绍兴市元盛化工有限公司 | Production method for recovering calcium lactate and lactic acid from lactic acid degumming waste liquid |
| CN103641872B (en) * | 2013-11-18 | 2016-03-23 | 宁夏泰瑞制药股份有限公司 | A kind of method utilizing tylosin broth to produce sterile bulk drug tylosin salt |
| CN105218352A (en) * | 2015-10-27 | 2016-01-06 | 安徽中粮生化格拉特乳酸有限公司 | A kind of method extracting lactic acid from lactic acid fermentation liquid |
| CN109956859B (en) * | 2017-12-22 | 2021-10-19 | 广州中国科学院先进技术研究所 | Method for separating and purifying lactic acid from lactic acid fermentation liquor |
| CN107986956A (en) * | 2017-12-28 | 2018-05-04 | 九江科院生物化工有限公司 | A kind of method for preparing calcium lactate crystal and the method by the calcium lactate crystal production lactic acid of resistance to thermal level |
| CN110857445A (en) * | 2018-08-23 | 2020-03-03 | 滨州市华康梦之缘生物科技有限公司 | High-purity low-energy-consumption lactic acid production process |
| CN110857446A (en) * | 2018-08-23 | 2020-03-03 | 滨州市华康梦之缘生物科技有限公司 | Production process of high-purity lactic acid |
| CN109678696A (en) * | 2019-01-31 | 2019-04-26 | 华熙福瑞达生物医药有限公司 | A method of extracting lactic acid from hyaluronic acid fermentation liquor |
| CN113292418A (en) * | 2021-05-28 | 2021-08-24 | 郑州运维生物技术有限公司 | Method for preparing high-purity lactic acid by taking heavy-phase lactic acid as raw material |
| CN113773189A (en) * | 2021-08-02 | 2021-12-10 | 合肥信达膜科技有限公司 | Application of membrane process in lactic acid production |
| CN113912488A (en) * | 2021-11-17 | 2022-01-11 | 浙江新银象生物工程有限公司 | Method for extracting lactic acid from nisin extraction mother liquor |
| CN114014752A (en) * | 2021-12-07 | 2022-02-08 | 河南星汉生物科技有限公司 | Process for decoloring crude lactic acid by using activated carbon |
| CN114181070A (en) * | 2021-12-28 | 2022-03-15 | 普立思生物科技有限公司 | Method for extracting high-purity L-lactic acid by using molecular distillation heavy phase and nanofiltration membrane concentrated solution |
| CN114804387A (en) * | 2022-05-06 | 2022-07-29 | 四川绿沃创新环保工程有限公司 | Method for recovering lactic acid evaporation condensate water |
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