CN1241894C - Process for extracting lactic acid from fermentation liquid - Google Patents
Process for extracting lactic acid from fermentation liquid Download PDFInfo
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- CN1241894C CN1241894C CN 200410041622 CN200410041622A CN1241894C CN 1241894 C CN1241894 C CN 1241894C CN 200410041622 CN200410041622 CN 200410041622 CN 200410041622 A CN200410041622 A CN 200410041622A CN 1241894 C CN1241894 C CN 1241894C
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- lactic acid
- liquid
- exchange resin
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- decolouring
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- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000004310 lactic acid Substances 0.000 title claims abstract description 38
- 235000014655 lactic acid Nutrition 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000007788 liquid Substances 0.000 title claims description 31
- 238000000855 fermentation Methods 0.000 title abstract description 7
- 230000004151 fermentation Effects 0.000 title abstract description 7
- 238000002425 crystallisation Methods 0.000 claims abstract description 21
- 230000008025 crystallization Effects 0.000 claims abstract description 20
- 239000011347 resin Substances 0.000 claims abstract description 14
- 229920005989 resin Polymers 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000003957 anion exchange resin Substances 0.000 claims description 14
- 239000013078 crystal Substances 0.000 claims description 12
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000003463 adsorbent Substances 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 6
- SMHNUIFHMAGAFL-UHFFFAOYSA-N calcium;2-hydroxypropanoic acid Chemical compound [Ca].CC(O)C(O)=O SMHNUIFHMAGAFL-UHFFFAOYSA-N 0.000 claims description 5
- 230000001954 sterilising effect Effects 0.000 claims description 5
- 238000004659 sterilization and disinfection Methods 0.000 claims description 5
- 150000001450 anions Chemical class 0.000 claims description 4
- 239000003729 cation exchange resin Substances 0.000 claims description 4
- 238000010612 desalination reaction Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 239000005864 Sulphur Substances 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- -1 acidolysis Substances 0.000 claims description 2
- 238000004042 decolorization Methods 0.000 claims description 2
- 239000003456 ion exchange resin Substances 0.000 claims description 2
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 2
- MKJXYGKVIBWPFZ-UHFFFAOYSA-L calcium lactate Chemical compound [Ca+2].CC(O)C([O-])=O.CC(O)C([O-])=O MKJXYGKVIBWPFZ-UHFFFAOYSA-L 0.000 abstract description 16
- 239000001527 calcium lactate Substances 0.000 abstract description 16
- 229960002401 calcium lactate Drugs 0.000 abstract description 16
- 235000011086 calcium lactate Nutrition 0.000 abstract description 16
- 238000000605 extraction Methods 0.000 abstract description 13
- 238000010924 continuous production Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 13
- 239000012535 impurity Substances 0.000 description 10
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 description 8
- 239000002585 base Substances 0.000 description 6
- 102000004169 proteins and genes Human genes 0.000 description 6
- 108090000623 proteins and genes Proteins 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 239000000049 pigment Substances 0.000 description 3
- 238000003672 processing method Methods 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- FRXSZNDVFUDTIR-UHFFFAOYSA-N 6-methoxy-1,2,3,4-tetrahydroquinoline Chemical compound N1CCCC2=CC(OC)=CC=C21 FRXSZNDVFUDTIR-UHFFFAOYSA-N 0.000 description 1
- 240000005384 Rhizopus oryzae Species 0.000 description 1
- 235000013752 Rhizopus oryzae Nutrition 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229920002988 biodegradable polymer Polymers 0.000 description 1
- 239000004621 biodegradable polymer Substances 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明涉及深层发酵生产乳酸的工艺方法，具体地说是从发酵液中提取乳酸的工艺方法。其特点是：采用颗粒状活性炭与H-103树脂柱联合脱糖脱色；采用两次降温法，即从30℃降到15℃，再从15℃降到4℃，通过一次结晶工艺提取乳酸钙。采用本工艺乳酸的损失大大降低，实现了工艺的连续化，提高了成品的提取率和和纯度较高，结晶率可达80%，纯度达97.2%，乳酸提取率稳定超过70%，且成品乳酸稳定性较好。
The invention relates to a process for producing lactic acid by submerged fermentation, in particular to a process for extracting lactic acid from fermentation broth. Its characteristics are: use granular activated carbon and H-103 resin column to desugar and decolorize; use two cooling methods, that is, drop from 30°C to 15°C, and then drop from 15°C to 4°C, and extract calcium lactate through a crystallization process . The loss of lactic acid is greatly reduced by this process, the continuous process is realized, the extraction rate and purity of the finished product are improved, the crystallization rate can reach 80%, the purity can reach 97.2%, the lactic acid extraction rate is stable over 70%, and the finished product Lactic acid is more stable.
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%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410041622 CN1241894C (en) | 2004-08-03 | 2004-08-03 | Process for extracting lactic acid from fermentation liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410041622 CN1241894C (en) | 2004-08-03 | 2004-08-03 | Process for extracting lactic acid from fermentation liquid |
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| CN1603298A CN1603298A (en) | 2005-04-06 |
| CN1241894C true CN1241894C (en) | 2006-02-15 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10017451B2 (en) | 2011-12-23 | 2018-07-10 | Purac Biochem B.V. | Lactic acid extraction |
Families Citing this family (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 liquor |
| 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 |
| 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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10017451B2 (en) | 2011-12-23 | 2018-07-10 | Purac Biochem B.V. | Lactic acid extraction |
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