CN1603298A - Process for extracting lactic acid from fermentation liquid - Google Patents
Process for extracting lactic acid from fermentation liquid Download PDFInfo
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- CN1603298A CN1603298A CN 200410041622 CN200410041622A CN1603298A CN 1603298 A CN1603298 A CN 1603298A CN 200410041622 CN200410041622 CN 200410041622 CN 200410041622 A CN200410041622 A CN 200410041622A CN 1603298 A CN1603298 A CN 1603298A
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Abstract
This invention relates to a technical proposal of producing lactic acid by deep layer fermentation, that is the proposal of extracting lactic acid from fermentation liquor. The features are that desugarization and decoloration are done by using granular active carbon and H-103 resin column. Two times consumption of heat is adopted, that is the temperature reduces from 300C to 15, then from 150C to 40C, and calcium lactate is extracted through once crystallization. The loss of lactic acid is much reduced and the technology continuance is realized by this invention. The extraction rate and purity are raised, the percent crystallinity can reach 80%, purity 97.2%, the extraction rate of lactic acid exceeds 70% and stability of finished product lactic acid is good.
Description
Technical field
The present invention relates to submerged fermentation and produce the processing method of lactic acid, specifically from fermented liquid, extract the processing method of lactic acid.
Background technology
Lactic acid is one of three big organic acids of generally acknowledging in the world, is widely used in fields such as food, medicine, chemical industry.In recent years, along with the L-lactic acid polymerizes becomes carrying out of Biodegradable Polymers research, production, the applied research of L-lactic acid started new climax at home and abroad, the market requirement of the L-lactic acid of high-optical-purity is very good.
At present, the production of the L-lactic acid of high-optical-purity is based on microbial fermentation, and fermented bacterium comprises Bacterium lacticum, Rhizopus oryzae etc.It is raw material with starch that China has a lot of fairly large enterprises now, and lactic acid is produced in submerged fermentation.These enterprises are with regard to fermentation level, approaching even part surpasses world level, but extract from downstream separation, the calcium lactate crystallization that China generally adopts at present-acidolysis process exists serialization, the level of automation extracted low, extraction yield is low, finished product purity is not high, problems such as shelf stability difference.
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 concentrates through suitable, crystallization under certain condition, and mother liquor is removed in centrifugation, obtains the white crystal of calcium lactate.Behind the heating redissolution calcium lactate crystal, carry out acidolysis, add an amount of gac and decolour, separate and remove calcium sulfate and gac residue, obtain crude lactic acid solution with sulfuric acid.Then crude lactic acid solution is passed through anion and cation exchange resin respectively, remove foreign ion wherein, through being concentrated into more than 80%, gained solution gets product lactic acid solution again.
Advantages such as this technology has the control of being easy to, and equipment requirements is simple, but unit operation is many, labour intensity is big, and environmental pollution is serious, and 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 carbohydrate in the fermented liquid, major impurity remarkably influenceds such as protein and pigment calcium lactate percent crystallization in massecuite and purity; The repeatedly activated carbon decolorizing that adopts makes calcium lactate and lactic acid rate of loss up to 30%, and causes the serialization of technology, level of automation low; It is insufficient to remove sugar in the technology, the quality that causes residual sugar in the finished product lactic acid or other reducing substances to influence product; In addition, calcium lactate crystallization processes conditional request harshness, wayward.
Summary of the invention
The objective of the invention is: by to the processing method of existing technical process, the improvement of condition, provide a kind of extraction yield and purity higher, percent crystallization in massecuite can reach 80%, purity reaches 97.2% the novel process of extracting lactic acid from fermented liquid.
The technical solution that realizes above-mentioned purpose is as follows:
1, from fermented liquid, extract the novel process of lactic acid, comprise fermented liquid sterilization, deproteinated, desugar, decolouring, condensing crystal, acidolysis, ion exchange resin and concentrate the finished product operation, it is characterized in that: concrete operations operation and processing condition are as follows:
In A, the 10 liters of fermented liquids after sterilization, add calcium hydroxide 37 grams and regulate pH value to 13, left standstill 6-7 hour under 45 ℃ of temperature condition;
B, leave standstill after liquid filters, add the Adlerikas of 10 grams, left standstill 3-4 hour under 90 ℃ of temperature condition above-mentioned;
C, will put into bleacher behind the B operation liquid filtering, add 0.2 kilogram of granular active carbon, 50 ℃ of-60 ℃ of temperature, vibration is 4-5 hour in the vibrator of 140rpm rotating speed;
After D, the liquid that will vibrate filter, adopt weak base anion-exchange resin to carry out the post decolouring, generate crude lactic acid calcium liquid, processing parameter is 40 ℃ of column temperatures, and the decolouring flow velocity is 2.5BV/h, and the volume ratio of upper prop resin and fermented liquid is 1: 5 (decolorization condition)
Described weak base anion-exchange resin is the H-103 macroporous adsorbent resin;
E, the crude lactic acid calcium liquid that generates is concentrated into 20% after, add 60～70 gram crystal seeds; Crystallization is carried out in twice cooling, and cooling for the first time is to drop to 15 ℃ from 30 ℃, and 12 hours time, cooling is for to drop to 4 ℃, 12 hours time from 15 ℃ for the second time;
F, after 24 hours, wash crystal with water, redissolve, add concentration and be lower than 50% sulphur and carry out acidolysis and get crude lactic acid in being lower than under 80 ℃ the temperature heating;
G, anion and cation exchange resin desalination; The weak base anion-exchange resin decolouring, processing condition are: 20 ℃ of column temperatures, the volume ratio of upper column quantity and resin are 5: 1, dynamic flow rate is 3BV/h;
Described weak base anion-exchange resin is the AB-8 polymeric adsorbent;
H, concentrate finished product lactic acid, its purity is 87～91%.
By regulate pH value with alkali, heat, add mode such as flocculation agent and remove major impurity such as protein, starch in the fermented liquid; Adopt granular active carbon and H-103 resin column associating desugar decolouring, can significantly reduce the loss of calcium lactate, and effect is better than powdered active carbon; Use falling temperature method twice, to the calcium lactate solution primary crystallization after the removal of impurities; Further adopt the AB-8 resin column dynamically to decolour to the lactic acid after acidolysis, the ion-exchange desalination, finally obtain high-purity lactic acid.
Inventive point: the desugar decolouring adsorption-edulcoration operation of fermented liquid is to the clearance height of major impurities such as sugar, protein; Changed the progressively decrease temperature crystalline method in the traditional technology, used falling temperature method twice, promptly dropped to 15 ℃ from 30 ℃, drop to 4 ℃ from 15 ℃ again, extract calcium lactate by primary crystallization technology, and its extraction yield and and purity higher, percent crystallization in massecuite can reach 80%, and purity reaches 97.2%; The dynamic H-103 of fixed bed, the AB-8 macroporous adsorptive resins decoloration process decolorizing effect that adopt are remarkable, and the loss of lactic acid reduces greatly, has realized the serialization of technology, has improved the extraction yield of finished product.
The useful technique effect that lactic acid extraction novel process of the present invention is compared with former technology is embodied in the following aspects:
1. the improvement of fermented liquid pretreatment procedure.Former technology removal of impurities is insufficient, cause repeatedly crystallization and percent crystallization in massecuite not high, the purity and the extraction yield of product have finally been influenced, pretreatment procedure after the optimization can fully remove major impurities such as desaccharification, protein, pigment sugared clearance is reached 91%, the protein removal rate reaches 93%, and remove most pigments, for later separation has alleviated burden.
2. the improvement of decoloring method.Repeatedly use the powdered active carbon decolouring in the former technology, decolour the lactic acid rate of loss more than 10% at every turn, difficulty is reclaimed in desorb, has seriously reduced the extraction yield of lactic acid.Technology after the improvement is used the dynamic post decolouring of AB-8 resin, reduces the rate of loss in the lactic acid decoloration process greatly, and effect obviously is better than gac.
3. crystallization method and crystallization condition have been improved.Use secondary crystal even repeatedly crystallization in the former technology, and the crystallization condition harshness, the calcium lactate percent crystallization in massecuite is low and purity is not high.Technology after the improvement has reduced the influence of impurity to calcium lactate solubleness because removal of impurities is abundant, only uses the cooling of two steps, just makes the calcium lactate crystal reach high purity by primary crystallization, has shortened process cycle, has saved the consumption of the energy.
4. realized by product CaSO
4Recycling.Because abundant to the fermented liquid removal of impurities, crystalline product calcium lactate purity height, so the CaSO that obtains of acidolysis
4By product purity is higher, can directly reclaim.
5 adopt the loss of this technology lactic acid to reduce greatly, have realized the serialization of technology, have improved the extraction yield of finished product.The lactic acid extraction rate is stable to surpass 70%, and finished product lactic acid stability better.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Below in conjunction with technical process Fig. 1, the present invention is done to describe further by embodiment.
Embodiment 1:
Get 10 liters of fermented liquids after the sterilization, about 37 grams of adding calcium hydroxide are regulated pH to 13, left standstill 6 hours in 45 ℃, add sal epsom quiet putting 3 hours under 90 ℃ of 10 grams after the filtration again, filter the back adds 0.2 kilogram in filtrate granular active carbon, the rotating speed that changes in 70 ℃, per minute 140 was placed on the vibrator vibration 4 hours with bleacher, filtering the back adopts H-103 macroporous adsorbent resin (weak base anion-exchange resin) to carry out the post decolouring, processing parameter is 40 ℃ of column temperatures, the decolouring flow velocity is 2.5BV/h, and the volume ratio of upper prop resin and fermented liquid is 1: 5.After the crude lactic acid calcium liquid that generates is concentrated into 20%, add 60～70 gram crystal seeds, crystallization is carried out in twice cooling, promptly earlier dropping to 15 ℃ from 30 ℃ left standstill 12 hours, dropping to 4 ℃ from 15 ℃ again left standstill 12 hours, wash crystal with water, redissolve, add concentration and be lower than 50% sulphur and carry out acidolysis and get crude lactic acid in being lower than under 80 ℃ the temperature heating; Crude lactic acid, after the anion and cation exchange resin desalination, the decolouring of AB-8 polymeric adsorbent (weak base anion-exchange resin) post, its processing condition are: 20 ℃ of column temperatures, the volume ratio of upper prop crude lactic acid and resin is 5: 1, and dynamic flow rate is 3BV/h, concentrate finished product lactic acid.
Claims (1)
1, from fermented liquid, extract the novel process of lactic acid, comprise fermented liquid sterilization, deproteinated, desugar, decolouring, condensing crystal, acidolysis, ion exchange resin and concentrate the finished product operation, it is characterized in that: concrete operations operation and processing condition are as follows:
In A, the 10 liters of fermented liquids after sterilization, add calcium hydroxide 37 grams and regulate pH value to 13, left standstill 6-7 hour under 45 ℃ of temperature condition;
B, leave standstill after liquid filters, add the Adlerikas of 10 grams, left standstill 3-4 hour under 90 ℃ of temperature condition above-mentioned;
C, will put into bleacher behind the B operation liquid filtering, add 0.2 kilogram of granular active carbon, 50 ℃ of-60 ℃ of temperature, vibration is 4-5 hour in the vibrator of 140rpm rotating speed;
After D, the liquid that will vibrate filter, adopt weak base anion-exchange resin to carry out the post decolouring, generate crude lactic acid calcium liquid, processing parameter is 40 ℃ of column temperatures, and the decolouring flow velocity is 2.5BV/h, and the volume ratio of upper prop resin and fermented liquid is 1: 5 (decolorization condition)
Described weak base anion-exchange resin is the H-103 macroporous adsorbent resin;
E, the crude lactic acid calcium liquid that generates is concentrated into 20% after, add 60～70 gram crystal seeds; Crystallization is carried out in twice cooling, and cooling for the first time is to drop to 15 ℃ from 30 ℃, and 12 hours time, cooling is for to drop to 4 ℃, 12 hours time from 15 ℃ for the second time;
F, after 24 hours, wash crystal with water, redissolve, add concentration and be lower than 50% sulphur and carry out acidolysis and get crude lactic acid in being lower than under 80 ℃ the temperature heating;
G, anion and cation exchange resin desalination; The weak base anion-exchange resin decolouring, processing condition are: 20 ℃ of column temperatures, the volume ratio of upper column quantity and resin are 5: 1, dynamic flow rate is 3BV/h;
Described weak base anion-exchange resin is the AB-8 polymeric adsorbent;
H, concentrate finished product lactic acid, its purity is 87～91%.
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| CN 200410041622 CN1241894C (en) | 2004-08-03 | 2004-08-03 | Process for extracting lactic acid from fermentation liquid |
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| CN 200410041622 CN1241894C (en) | 2004-08-03 | 2004-08-03 | Process for extracting lactic acid from fermentation liquid |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100339351C (en) * | 2005-08-26 | 2007-09-26 | 江南大学 | Method for separating remaining sugar and extracting organic acid from organic acid fermentation liquor and corresponding organic acid mother liquor |
| CN102516063A (en) * | 2011-12-30 | 2012-06-27 | 南京工业大学 | Method for extracting D-lactic acid from fermentation liquid |
| CN102864187A (en) * | 2012-09-29 | 2013-01-09 | 武汉三江航天固德生物科技有限公司 | L-lactic acid fermenting filtrate recycling method |
| CN105646193A (en) * | 2014-12-05 | 2016-06-08 | 中国石油化工股份有限公司 | Method used for separating and extracting lactic acid from fermentation broth |
| 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 |
| CN114478231A (en) * | 2020-10-27 | 2022-05-13 | 河北圣雪大成制药有限责任公司 | Method for recovering lactic acid from nisin waste liquid |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PT2794544T (en) | 2011-12-23 | 2018-05-18 | Purac Biochem Bv | Lactic acid extraction |
-
2004
- 2004-08-03 CN CN 200410041622 patent/CN1241894C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100339351C (en) * | 2005-08-26 | 2007-09-26 | 江南大学 | Method for separating remaining sugar and extracting organic acid from organic acid fermentation liquor and corresponding organic acid mother liquor |
| CN102516063A (en) * | 2011-12-30 | 2012-06-27 | 南京工业大学 | Method for extracting D-lactic acid from fermentation liquid |
| CN102864187A (en) * | 2012-09-29 | 2013-01-09 | 武汉三江航天固德生物科技有限公司 | L-lactic acid fermenting filtrate recycling method |
| CN105646193A (en) * | 2014-12-05 | 2016-06-08 | 中国石油化工股份有限公司 | Method used for separating and extracting lactic acid from fermentation broth |
| CN105646193B (en) * | 2014-12-05 | 2018-04-10 | 中国石油化工股份有限公司 | A kind of method of the separation and Extraction lactic acid from zymotic fluid |
| 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 |
| CN114478231A (en) * | 2020-10-27 | 2022-05-13 | 河北圣雪大成制药有限责任公司 | Method for recovering lactic acid from nisin waste liquid |
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| CN1241894C (en) | 2006-02-15 |
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