CN102976923A - 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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- CN102976923A CN102976923A CN2012105500936A CN201210550093A CN102976923A CN 102976923 A CN102976923 A CN 102976923A CN 2012105500936 A CN2012105500936 A CN 2012105500936A CN 201210550093 A CN201210550093 A CN 201210550093A CN 102976923 A CN102976923 A CN 102976923A
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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 the separation and the technique of purification of lactic acid, specifically relate to and a kind ofly from lactic acid fermentation liquid, separating and the technique of purification of lactic acid with film.
Background technology
Lactic acid extensively is present in human body, animal body and the plant as a kind of important organic acid.Lactic acid, lactic acid salt and derivative thereof have widely application in food, feed, chemical industry and medicine and other fields.In recent years, the poly (l-lactic acid) that the Pfansteihl polymerization generates is as type material, biodegradable plastic, environmentally friendly packing material and the family expenses film etc. made, solved day by day serious problem of environmental pollution, caused the extensive concern in the world, be considered to the most rising novel material of new millennium, 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 take microbial fermentation as main, and fermented bacterium is Bacterium lacticum, Rhizopus oryzae etc.The problems such as the extraction to lactic acid fermentation liquid separates, and calcium lactate crystallization-acidolysis process that China generally adopts at present exists extraction yield low, and finished product purity is not high, and shelf stability is poor.
The flow process of calcium lactate crystallization-acidolysis process is roughly as follows:
The upstream fermented liquid is removed thalline, protein isocolloid impurity after intensification, alkalinisation treatment.The calcium lactate mash that obtains is through condensing crystal, and mother liquor is removed in centrifugation, obtains the calcium lactate crystal.Heating is carried out acidolysis with sulfuric acid after redissolving, and adds the proper amount of active carbon decolouring, separates and removes calcium sulfate and gac residue, obtains crude lactic acid solution.Then crude lactic acid solution is passed through respectively anion and cation exchange resin, remove foreign ion wherein, through being concentrated into more than 80%, gained solution gets product lactic acid solution again.
The advantages such as this technique has the control of being easy to, and equipment requirements is simple, but the product extraction yield is low, and purity is not high.Cause the low and not high reason of purity of present lactic acid extraction rate to have: the major impurities such as the carbohydrate in the fermented liquid, protein and pigment can not effectively be removed, remarkably influenced calcium lactate percent crystallization in massecuite and purity; Adopt repeatedly activated carbon decolorizing to make the rate of loss of calcium lactate and lactic acid up to 30%; Insufficient except sugar in the technique, the quality that causes residual sugar in the finished product lactic acid or other reducing substances to affect product.
Summary of the invention
Based on the deficiency of calcium lactate crystallization-acidolysis process, the invention provides a kind of novel process of from lactic acid fermentation liquid, extracting lactic acid.
Its technical solution is:
A kind of novel process of from lactic acid fermentation liquid, extracting lactic acid, it may further comprise the steps:
(1) lactic acid fermentation liquid is heated to 80～90 ℃, adds calcium hydroxide and regulate pH to 10～12, insulated and stirred is filtered after 15～60 minutes and is obtained feed liquid 1;
(2) add the flocculation agent polyacrylamide in the feed liquid 1, leave standstill 1～6 hour after, filter and obtain filtrate 2;
(3) with gac filtrate 2 is decoloured, the mass ratio of gac and lactic acid fermentation liquid is 0.05: 100～1: 100, and bleaching temperature is 65～80OC, and bleaching time is 30～70min, successively obtains filtrate 3 with sheet frame and inorganic ceramic membrane filtration again;
(4) with plate-type heat exchanger filtrate 3 is lowered the temperature, made the temperature of filtrate 3 drop to 45～60 ℃ by 60～80 ℃, then filter with organic nanofiltration membrane and obtain filtrate 4;
(5) to filtrate 4 take successively to concentrate, decrease temperature crystalline, centrifugal, wash crystalline substance, drying, make the calcium lactate crystal;
(6) the heavy molten calcium lactate crystal of adding distil water, heating is redissolved it fully under being lower than 80 ℃, and adding sulfuric acid carries out acidolysis and gets crude lactic acid;
(7) with the foreign ion in the anion and cation exchange resin removal crude lactic acid;
(8) concentrate to get finished product lactic acid, its purity is 95%～98%.
Preferably, in the step (5): in the triple effect concentrating pan, concentrate; In the crystallization cylinder, carry out decrease temperature crystalline.
Preferably, in the step (6): the weight percent concentration of sulfuric acid is 40%～98%.
Useful technique effect of the present invention is:
The calcium lactate crystallization-the acidolysis process removal of impurities is insufficient based on existing, cause repeatedly crystallization and percent crystallization in massecuite not high, purity and the extraction yield of product have finally been affected, technique of the present invention is optimized it, before crystallization, increased membrane filtration twice, be that inorganic ceramic membrane filtration and organic nanofiltration membrane filter, wherein, the inorganic ceramic membrane filtration has been removed the impurity such as insoluble solid impurities, thalline, colloidalmaterial and macromolecular carbohydrate small in the filtrate 2; Organic nanofiltration membrane filters low molecular sugar part and the polyvalent ion of having removed in the filtrate 3, thereby can fully remove the major impurities such as sugar, protein, pigment, make the finished product lactic acid purity that finally makes up to 95%～98%, and the lactic acid crystallization yield is brought up to more than 85% by original 70%, greatly reduce production cost.In addition, technique gained waste liquid of the present invention is because containing the monose of high density, and the raw material that can be used as the other products fermentation is utilized, and has reduced the discharging of waste liquid.Technique of the present invention adopted activated carbon decolorizing before crystal redissolves simultaneously, had 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 → the inorganic ceramic membrane filtration → plate-type heat exchanger cooling → organic nanofiltration membrane filters → the concentrate primary crystallization → centrifugal drying → weight molten → acidolysis → ion exchange resin column → concentrated finished product that to get.
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 make inorganic ceramic film and organic nanofiltration membrane can give full play to its filter effect, and making the finished product lactic acid that finally makes can obtain high purity and high crystallization yield, technique of the present invention is being carried out the again to some extent difference of twice existing calcium lactate crystallization-acidolysis process of the pretreatment procedure before the membrane filtration.Regulate pH to 10～12, insulated and stirred 15～60 minutes as adding calcium hydroxide in the pretreatment procedure; And for example preferred flocculation agent polyacrylamide left standstill 1～6 hour; Mass ratio such as active carbon for decolorization and lactic acid fermentation liquid is 0.05: 100～1.5: 100, and bleaching temperature is 65～80 ℃, and bleaching time is 30～70min etc.
The below enumerates several embodiment and more specifically illustrates:
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 adds calcium carbonate as neutralizing agent, and fermentation makes lactic acid fermentation liquid.Be heated to 85 ℃, add calcium hydroxide and regulate pH to 11, insulated and stirred is after 20 minutes, and the insolubless such as calcium carbonate of removing in the lactic acid fermentation liquid with filter-cloth filtering obtain feed liquid 1.Add the flocculation agent polyacrylamide in the feed liquid 1, leave standstill 4 hours after, filter and obtain filtrate 2.Then under 65 ℃ temperature condition, be to add the gac 40min that in feed liquid 1, decolours at 0.05: 100 by the mass ratio of gac and feed liquid 1, successively obtain filtrate 3 with sheet frame and inorganic ceramic membrane filtration again.With plate-type heat exchanger filtrate 3 is cooled to 55 ℃, then filters with organic nanofiltration membrane and obtain filtrate 4.It is 160g/L that filtrate 4 is concentrated to calcium lactate concentration through the triple effect concentrating pan first, decrease temperature crystalline in the crystallization cylinder again, and last centrifugal drying obtains the calcium lactate crystal.The heavy molten crystal of adding distil water redissolves it 70 ℃ of lower heating fully, adds weight percent concentration and is 45% sulfuric acid and carry out acidolysis and get crude lactic acid.Remove wherein foreign ion with anion and cation exchange resin, concentrated purity is 95% finished product lactic acid.
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 adds calcium carbonate as neutralizing agent, and fermentation makes lactic acid fermentation liquid.Be heated to 80 ℃, add calcium hydroxide and regulate pH to 12, insulated and stirred is after 30 minutes, and the insolubless such as calcium carbonate of removing in the lactic acid fermentation liquid with filter-cloth filtering obtain feed liquid 1.Add the flocculation agent polyacrylamide in the feed liquid 1, leave standstill 3.5 hours after, filter and obtain filtrate 2.Then under 70 ℃ temperature condition, be to add the gac 40min that in feed liquid 1, decolours at 0.1: 100 by the mass ratio of gac and feed liquid 1, successively obtain filtrate 3 with sheet frame and inorganic ceramic membrane filtration again.With plate-type heat exchanger filtrate 3 is cooled to 60 ℃, then filters with organic nanofiltration membrane and obtain filtrate 4.It is 140g/L that filtrate 4 is concentrated to calcium lactate concentration through the triple effect concentrating pan first, decrease temperature crystalline in the crystallization cylinder again, and last centrifugal drying obtains the calcium lactate crystal.The heavy molten crystal of adding distil water redissolves it 70 ℃ of lower heating fully, adds weight percent concentration and is 65% sulfuric acid and carry out acidolysis and get crude lactic acid.Use activated carbon decolorizing, anion and cation exchange resin is removed foreign ion wherein, and concentrated purity is 98% finished product lactic acid.
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 adds calcium carbonate as neutralizing agent, and fermentation makes lactic acid fermentation liquid.Be heated to 90 ℃, add calcium hydroxide and regulate pH to 10, insulated and stirred is after 40 minutes, and the insolubless such as calcium carbonate of removing in the lactic acid fermentation liquid with filter-cloth filtering obtain feed liquid 1.Add the flocculation agent polyacrylamide in the feed liquid 1, leave standstill 3.5 hours after, filter and obtain filtrate 2.Then under 80 ℃ temperature condition, be to add the gac 35min that in feed liquid 1, decolours at 1: 100 by the mass ratio of gac and feed liquid 1, successively obtain filtrate 3 with sheet frame and inorganic ceramic membrane filtration again.With plate-type heat exchanger filtrate 3 is cooled to 50 ℃, then filters with organic nanofiltration membrane and obtain filtrate 4.It is 120g/L that filtrate 4 is concentrated to calcium lactate concentration through the triple effect concentrating pan first, decrease temperature crystalline in the crystallization cylinder again, and last centrifugal drying obtains the calcium lactate crystal.The heavy molten crystal of adding distil water redissolves it 70 ℃ of lower heating fully, adds weight percent concentration and is 60% sulfuric acid and carry out acidolysis and get crude lactic acid.Use activated carbon decolorizing, anion and cation exchange resin is removed foreign ion wherein, and concentrated purity is 97% finished product lactic acid.
Claims (3)
1. novel process of extracting lactic acid from lactic acid fermentation liquid is characterized in that may further comprise the steps:
(1) lactic acid fermentation liquid is heated to 80～90 ℃, adds calcium hydroxide and regulate pH to 10～12, insulated and stirred is filtered after 15～60 minutes and is obtained feed liquid 1;
(2) add the flocculation agent polyacrylamide in the feed liquid 1, leave standstill 1～6 hour after, filter and obtain filtrate 2;
(3) with gac filtrate 2 is decoloured, the mass ratio of gac and lactic acid fermentation liquid is 0.05: 100～1: 100, and bleaching temperature is 65～80OC, and bleaching time is 30～70min, successively obtains filtrate 3 with sheet frame and inorganic ceramic membrane filtration again;
(4) with plate-type heat exchanger filtrate 3 is lowered the temperature, made the temperature of filtrate 3 drop to 45～60 ℃ by 60～80 ℃, then filter with organic nanofiltration membrane and obtain filtrate 4;
(5) to filtrate 4 take successively to concentrate, decrease temperature crystalline, centrifugal, wash crystalline substance, drying, make the calcium lactate crystal;
(6) the heavy molten calcium lactate crystal of adding distil water, heating is redissolved it fully under being lower than 80 ℃, and adding sulfuric acid carries out acidolysis and gets crude lactic acid;
(7) with the foreign ion in the anion and cation exchange resin removal crude lactic acid;
(8) concentrate to get finished product lactic acid, its purity is 95%～98%.
2. a kind of novel process of extracting lactic acid from lactic acid fermentation liquid according to claim 1 is characterized in that, in the step (5): concentrate in the triple effect concentrating pan; In the crystallization cylinder, carry out decrease temperature crystalline.
3. a kind of novel process of extracting lactic acid from lactic acid fermentation liquid according to claim 1 is characterized in that in the step (6): the weight percent concentration of sulfuric acid is 40%～98%.
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Cited By (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 |
| CN103641872A (en) * | 2013-11-18 | 2014-03-19 | 宁夏泰瑞制药股份有限公司 | Method for producing aseptic bulk drug tylosin salt by utilizing tylosin fermentation broth |
| 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 |
| 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 |
| 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 |
| CN109956859A (en) * | 2017-12-22 | 2019-07-02 | 广州中国科学院先进技术研究所 | A method of the separating-purifying lactic acid from lactic fermentation liquid |
| 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 |
| 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 |
| 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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Cited By (16)
| 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 |
| CN103641872A (en) * | 2013-11-18 | 2014-03-19 | 宁夏泰瑞制药股份有限公司 | Method for producing aseptic bulk drug tylosin salt by utilizing tylosin fermentation broth |
| 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 |
| CN109956859A (en) * | 2017-12-22 | 2019-07-02 | 广州中国科学院先进技术研究所 | A method of the separating-purifying lactic acid from lactic fermentation liquid |
| 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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