CN102367255B - Method for extracting riboflavin from riboflavin fermentation liquor - Google Patents
Method for extracting riboflavin from riboflavin fermentation liquor Download PDFInfo
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- CN102367255B CN102367255B CN 201110401426 CN201110401426A CN102367255B CN 102367255 B CN102367255 B CN 102367255B CN 201110401426 CN201110401426 CN 201110401426 CN 201110401426 A CN201110401426 A CN 201110401426A CN 102367255 B CN102367255 B CN 102367255B
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Abstract
The invention discloses a method for extracting riboflavin from riboflavin fermentation liquor. The method comprises the following steps: 1) filtering; 2) acidizing; 3) separating; 4) performing hydrolysis and crystallization; and 5) filtering and drying the obtained riboflavin crystals to obtain feed-grade riboflavin with the content of 80%. The method has the advantages that: the characteristicthat the solubility of riboflavin is low under the acidic condition is utilized to precipitate riboflavin, form heavy phase suspension and realize separation, thus the extraction process of riboflavin is simplified, the dosage of acid is reduced, the chemical raw materials such as caustic soda solution and hydrogen peroxide are not used and the production cost is reduced.
Description
Technical field
The present invention relates to a kind of method of from Lactochrome fermentation liquor, extracting riboflavin.
Background technology
The separating and extracting method of riboflavin mainly contains: the heavy metallic salt precipitator method, Morehouse method, acid pasting and alkali solution technique.The rear two kinds of methods of many employings in the industrial production also have the extraction process of utilizing alkali solution technique and acid pasting to combine at present, and its operational path is: alkali is molten---separate---crystallization---filter (---acid molten---recrystallize---dehydration)---drying.Separate after the producer that also has utilizes high efficiency separation equipment with the Lactochrome fermentation liquor pre-treatment, and utilize the oxidation-reduction quality of riboflavin to separate, crystallization.
Although it is numerous to extract the riboflavin method from fermented liquid, processing step is complicated, yield is not very high, and also has following problem: 1) separation of solid impurity is very difficult, and this difficulty is through whole leaching process.In the impurity sepn process, because the molten rear somatic cells of alkali breaks, produce a lot of colloidalmaterials, cause soltion viscosity to rise, and thalline itself is tiny, and is very difficult with traditional Plate Filtration, easily stops up fenestra with the method for membrane sepn, concentration ratio is low, and film cleans and restores difficulty, causes cost very high.2) owing to the chemical process that is that adopts at present; used a large amount of bronsted lowry acids and bases bronsted lowries; residual salt in a large number in producing waste liquid; waste liquid can not directly carry out biochemical treatment; although the technology of extracting the thalline crude protein is arranged; but too high salt has limited the thalline crude protein and has used, and is unfavorable for environment protection and comprehensive utilization of resources.
Summary of the invention
For the problems of the prior art, the objective of the invention is to provide a kind of method of from Lactochrome fermentation liquor, extracting riboflavin, thereby reduce the riboflavin extraction step.
In order to achieve the above object, technical scheme of the present invention is: a kind of method of extracting riboflavin from Lactochrome fermentation liquor may further comprise the steps:
1) filters, Lactochrome fermentation liquor is removed thick impurity by 40～80 order spin vibration sieves;
2) acidifying, with the filtrate heating that step 1) obtains, temperature is controlled at 35 ℃～65 ℃, uses the salt acid for adjusting pH value, is controlled between 5.0～5.5, obtains acidification hydrolization liquid;
3) separating step 2) the acidification hydrolization liquid that obtains carries out centrifugation, obtains the underflow material, and the volume ratio of acidification hydrolization liquid and underflow material is 7: 1 ~ 9: 1;
4) hydrolysis crystallization, 3 ~ 5 times of the underflow material dilute with waters that step 3) is obtained, then with between nitric acid or hydrochloric acid adjust pH to 1.4～1.7, with steam treatment solution is heated to boiling, then airtight, pass into pressurized air and boost to 0.14-～0.17MPa, and pressurize was rushed down pressure after 4 hours, be cooled to 35 ℃～45 ℃, obtain the riboflavin crystal slurry;
5) filter, with the tap water washing, wash to the washing lotion pH value more than 5.0, the content that obtains is the feed grade riboflavin that the riboflavin crystal namely obtains content 80% after drying.
Further, step 2) adopt plate-type heat exchanger that filtrate is heated.
Further, the isolated supernatant liquor of step 3) is delivered to sewage treatment plant.
Further, step 3) adopts bipyramid three-phase decanter whizzer to carry out centrifugation.
Further, step 5) adopts flame filter press that the riboflavin crystal slurry is filtered.
The present invention utilizes the low characteristic of riboflavin solubleness under the acidic conditions, riboflavin is separated out form the heavy phase suspension and realize separating, simplified riboflavin extraction process step, reduced sour usage quantity, eliminate the use of the chemical feedstockss such as liquid caustic soda, hydrogen peroxide, reduced production cost; Riboflavin yield of the present invention is compared traditional technology and has been improved about 10%.
Embodiment
Below in conjunction with embodiment the present invention is further specified.
Embodiment 1
Lactochrome fermentation liquor is removed thick impurity by 40 order spin vibration sieves, then with plate-type heat exchanger filtrate is heated, temperature is controlled at 35 ℃, uses the salt acid for adjusting pH value, is controlled between 5.0, obtains acidification hydrolization liquid; Then with bipyramid three-phase decanter whizzer acidification hydrolization liquid is carried out centrifugation, obtain the underflow material, the volume ratio of acidification hydrolization liquid and underflow material is 7: 1, with 3 times of underflow material dilute with waters, then uses between the hydrochloric acid adjust pH to 1.4, with steam treatment solution is heated to boiling, then airtight, pass into pressurized air and boost to 0.14-MPa, and pressurize was rushed down pressure after 4 hours, be cooled to 35 ℃, obtain the riboflavin crystal slurry; The riboflavin crystal slurry after flame filter press filters, with the tap water washing, wash to the washing lotion pH value more than 5.0, the riboflavin crystal that obtains namely obtains the feed grade riboflavin of content 80% after drying.
Embodiment 2
Lactochrome fermentation liquor is removed thick impurity by 80 order spin vibration sieves, then with plate-type heat exchanger filtrate is heated, temperature is controlled at 65 ℃, uses the salt acid for adjusting pH value, is controlled between 5.5, obtains acidification hydrolization liquid; Then with bipyramid three-phase decanter whizzer acidification hydrolization liquid is carried out centrifugation, obtain the underflow material, the volume ratio of acidification hydrolization liquid and underflow material is 9: 1, with 5 times of underflow material dilute with waters, then uses between the nitric acid adjust pH to 1.7, with steam treatment solution is heated to boiling, then airtight, pass into pressurized air and boost to 0.17MPa, and pressurize was rushed down pressure after 4 hours, be cooled to 45 ℃, obtain the riboflavin crystal slurry; The riboflavin crystal slurry after flame filter press filters, with the tap water washing, wash to the washing lotion pH value more than 5.0, the riboflavin crystal that obtains namely obtains the feed grade riboflavin of content 80% after drying.
Embodiment 3
Lactochrome fermentation liquor is removed thick impurity by 50 order spin vibration sieves, then with plate-type heat exchanger filtrate is heated, temperature is controlled at 45 ℃, uses the salt acid for adjusting pH value, is controlled between 5.2, obtains acidification hydrolization liquid; Then with bipyramid three-phase decanter whizzer acidification hydrolization liquid is carried out centrifugation, obtain the underflow material, the volume ratio of acidification hydrolization liquid and underflow material is 8: 1, with 4 times of underflow material dilute with waters, then uses between the hydrochloric acid adjust pH to 1.3, with steam treatment solution is heated to boiling, then airtight, pass into pressurized air and boost to 0.15MPa, and pressurize was rushed down pressure after 4 hours, be cooled to 40 ℃, obtain the riboflavin crystal slurry; The riboflavin crystal slurry after flame filter press filters, with the tap water washing, wash to the washing lotion pH value more than 5.0, the riboflavin crystal that obtains namely obtains the feed grade riboflavin of content 80% after drying.
Embodiment 4
Lactochrome fermentation liquor is removed thick impurity by 60 order spin vibration sieves, then with plate-type heat exchanger filtrate is heated, temperature is controlled at 55 ℃, uses the salt acid for adjusting pH value, is controlled between 5.4, obtains acidification hydrolization liquid; Then with bipyramid three-phase decanter whizzer acidification hydrolization liquid is carried out centrifugation, obtain the underflow material, the volume ratio of acidification hydrolization liquid and underflow material is 8: 1, with 3 ~ 5 times of underflow material dilute with waters, then uses between the nitric acid adjust pH to 1.6, with steam treatment solution is heated to boiling, then airtight, pass into pressurized air and boost to 0.16MPa, and pressurize was rushed down pressure after 4 hours, be cooled to 42 ℃, obtain the riboflavin crystal slurry; The riboflavin crystal slurry after flame filter press filters, with the tap water washing, wash to the washing lotion pH value more than 5.0, the riboflavin crystal that obtains namely obtains the feed grade riboflavin of content 80% after drying.
Embodiment 5
Lactochrome fermentation liquor is removed thick impurity by 70 order spin vibration sieves, then with plate-type heat exchanger filtrate is heated, temperature is controlled at 50 ℃, uses the salt acid for adjusting pH value, is controlled between 5.5, obtains acidification hydrolization liquid; Then with bipyramid three-phase decanter whizzer acidification hydrolization liquid is carried out centrifugation, obtain the underflow material, the volume ratio of acidification hydrolization liquid and underflow material is 7: 1, with 5 times of underflow material dilute with waters, then uses between the nitric acid adjust pH to 1.4, with steam treatment solution is heated to boiling, then airtight, pass into pressurized air and boost to 0.17MPa, and pressurize was rushed down pressure after 4 hours, be cooled to 40 ℃, obtain the riboflavin crystal slurry; The riboflavin crystal slurry after flame filter press filters, with the tap water washing, wash to the washing lotion pH value more than 5.0, the riboflavin crystal that obtains namely obtains the feed grade riboflavin of content 80% after drying.
Embodiment 6
Lactochrome fermentation liquor is removed thick impurity by 80 order spin vibration sieves, then with plate-type heat exchanger filtrate is heated, temperature is controlled at 35 ℃ ℃, uses the salt acid for adjusting pH value, is controlled between 5.0, obtains acidification hydrolization liquid; Then with bipyramid three-phase decanter whizzer acidification hydrolization liquid is carried out centrifugation, obtain the underflow material, the volume ratio of acidification hydrolization liquid and underflow material is 8: 1, with 4 times of underflow material dilute with waters, then uses between the hydrochloric acid adjust pH to 1.5, with steam treatment solution is heated to boiling, then airtight, pass into pressurized air and boost to 0.14-MPa, and pressurize was rushed down pressure after 4 hours, be cooled to 45 ℃, obtain the riboflavin crystal slurry; The riboflavin crystal slurry after flame filter press filters, with the tap water washing, wash to the washing lotion pH value more than 5.0, the riboflavin crystal that obtains namely obtains the feed grade riboflavin of content 80% after drying.
All in the situation that do not break away from the simple distortion that core of the present invention makes or revise and all fall into protection scope of the present invention.
Claims (4)
1. method of extracting riboflavin from Lactochrome fermentation liquor may further comprise the steps:
1) filters, Lactochrome fermentation liquor is removed thick impurity by 40～80 order spin vibration sieves;
2) acidifying, with the filtrate heating that step 1) obtains, temperature is controlled at 35 ℃～65 ℃, uses the salt acid for adjusting pH value, is controlled between 5.0～5.5, obtains acidification hydrolization liquid;
3) separating step 2) the acidification hydrolization liquid that obtains adopts bipyramid three-phase decanter whizzer to carry out centrifugation, obtains the underflow material, and the volume ratio of acidification hydrolization liquid and underflow material is 7: 1 ~ 9: 1;
4) hydrolysis crystallization, 3 ~ 5 times of the underflow material dilute with waters that step 3) is obtained, then with between nitric acid or hydrochloric acid adjust pH to 1.4～1.7, with steam treatment solution is heated to boiling, then airtight, pass into pressurized air and boost to 0.14-～0.17MPa, and pressurize pressure release after 4 hours, be cooled to 35 ℃～45 ℃, obtain the riboflavin crystal slurry;
5) filter, with the tap water washing, wash to washing lotion pH value more than 5.0, the riboflavin crystal that obtains namely obtains the feed grade riboflavin of content 80% after drying.
2. a kind of method of extracting riboflavin from Lactochrome fermentation liquor according to claim 1 is characterized in that step 2) adopt plate-type heat exchanger that filtrate is heated.
3. a kind of method of extracting riboflavin from Lactochrome fermentation liquor according to claim 1 is characterized in that, the isolated supernatant liquor of step 3) is delivered to sewage treatment plant.
4. a kind of method of extracting riboflavin from Lactochrome fermentation liquor according to claim 1 is characterized in that, step 5) adopts flame filter press that the riboflavin crystal slurry is filtered.
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| CN 201110401426 CN102367255B (en) | 2011-12-07 | 2011-12-07 | Method for extracting riboflavin from riboflavin fermentation liquor |
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| CN 201110401426 CN102367255B (en) | 2011-12-07 | 2011-12-07 | Method for extracting riboflavin from riboflavin fermentation liquor |
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Citations (4)
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|---|---|---|---|---|
| CN1146455A (en) * | 1995-03-03 | 1997-04-02 | 弗·哈夫曼-拉罗切有限公司 | Purification for riboflavin |
| CN1765897A (en) * | 2004-10-27 | 2006-05-03 | 上海凯赛生物技术研发中心有限公司 | Lactochrome fermentation liquor extraction process |
| CN101205230A (en) * | 2007-12-10 | 2008-06-25 | 南京九思高科技有限公司 | Method for extracting high-purity riboflavin directly from fermentation liquor |
| CN101412716A (en) * | 2008-11-28 | 2009-04-22 | 山东恩贝生物工程有限公司 | Method for extracting lactoflavin |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1146455A (en) * | 1995-03-03 | 1997-04-02 | 弗·哈夫曼-拉罗切有限公司 | Purification for riboflavin |
| CN1765897A (en) * | 2004-10-27 | 2006-05-03 | 上海凯赛生物技术研发中心有限公司 | Lactochrome fermentation liquor extraction process |
| CN101205230A (en) * | 2007-12-10 | 2008-06-25 | 南京九思高科技有限公司 | Method for extracting high-purity riboflavin directly from fermentation liquor |
| CN101412716A (en) * | 2008-11-28 | 2009-04-22 | 山东恩贝生物工程有限公司 | Method for extracting lactoflavin |
Non-Patent Citations (5)
| Title |
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| 双锥三相卧螺离心机及其应用;铃木庄六;《化工装备技术》;19921231;第12卷(第1期);38-42 * |
| 李家洲.维生素及辅酶嘞药物.《生物制药工艺学》.2007,187-188. * |
| 李文钊.核黄素结晶分离纯化研究.《中国博士学位论文全文数据库 工程科技I辑》.2009,(第4期),5-7. |
| 核黄素结晶分离纯化研究;李文钊;《中国博士学位论文全文数据库 工程科技I辑》;20090415(第4期);5-7 * |
| 铃木庄六.双锥三相卧螺离心机及其应用.《化工装备技术》.1992,第12卷(第1期),38-42. |
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Owner name: GUANGJI PHARMA (MENGZHOU) CO., LTD. Effective date: 20131220 Owner name: HUBEI GUANGJI PHARMACEUTICAL CO., LTD. Free format text: FORMER OWNER: GUANGJI PHARMA (MENGZHOU) CO., LTD. Effective date: 20131220 |
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Effective date of registration: 20131220 Address after: Wuxue City, Hubei Province, 435400 River Road No. 1 Patentee after: Hubei Guangji Pharmaceutical Co., Ltd. Patentee after: Guangji Pharmaceutical (Mengzhou) Co., Ltd. Address before: Mengzhou City, Henan province 454791 Jiaozuo dadin Road South (Guangji pharmaceutical) Patentee before: Guangji Pharmaceutical (Mengzhou) Co., Ltd. |