CN101633634A - Method for extracting L-proline from fermentation liquor by membrane separation technology - Google Patents
Method for extracting L-proline from fermentation liquor by membrane separation technology Download PDFInfo
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- CN101633634A CN101633634A CN200910017941A CN200910017941A CN101633634A CN 101633634 A CN101633634 A CN 101633634A CN 200910017941 A CN200910017941 A CN 200910017941A CN 200910017941 A CN200910017941 A CN 200910017941A CN 101633634 A CN101633634 A CN 101633634A
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Abstract
The invention discloses a method for extracting L-proline from fermentation liquor by a membrane separation technology. The method comprises the following steps: firstly performing microfiltration, ultrafiltration and reverse osmosis concentration on the fermentation liquor of the L-proline to obtain reverse osmosis dialyzate, evaporating and concentrating the reverse osmosis dialyzate by a conventional method, and then crystallizing at the reduced temperature to obtain a crude product L-proline. The method helps fundamentally solve the problem of environmental pollution during the extraction process of the L-proline, reduce production cost, increase economic benefit, improve the product grade and promote sustainable development of production of the L-proline.
Description
Technical field
The invention belongs to the amino acid production technical field, relate to a kind of method of utilizing membrane separation technique from fermented liquid, to extract the L-proline(Pro).
Background technology
The L-proline(Pro) is the neutral amino acids that contains imino-, belongs to heterocycle family amino acid, is to constitute one of proteinic 20 kinds of primary amino acids, belongs to the human body non-essential amino acid.The L-proline(Pro) has important purposes in industries such as medicine, chemical industry and agriculturals.Pharmaceutically mainly as one of raw material of amino acid, be used for malnutrition, hypoproteinosis, serious intestines and stomach illness is scalded and surgical operation after protein replenish, the L-proline(Pro) uses in the research and development of new drug widely as medicine synthetic intermediate in recent years; Characteristics such as on compound probability, the L-proline(Pro) can participate in inducing asymmetric reaction, as catalyst for reaction such as hydrogenation, polymerization, water Jie, has activity by force, and stereospecificity is good; On agricultural, report was also once arranged with " tonic " of L-proline(Pro) as farm crop, improve the quality of farm crop.
At present, the extracting and purifying method of common L-proline(Pro) mainly contains Pentachlorophenol and becomes salt precipitation method, alumina column chromatography and ion exchange method.It is to utilize L-proline(Pro) and Pentachlorophenol salify that Pentachlorophenol becomes salt precipitation method, separates out precipitation, with after ammoniacal liquor is resolved precipitation, obtain the L-proline(Pro), but Pentachlorophenol is a violent in toxicity, and operating environment is difficult to guarantee; The alumina column chromatography method generally is used for the purifying of the refining and crude product of product, because of small scale, only is confined to laboratory scope, at present can't industrialized production; Adopt ion exchange method to realize the extraction of L-proline(Pro) on the present industrial production mostly, still because the wastewater flow rate that ion exchange method extraction L-proline(Pro) produces is too big, environmental issue is difficult to solve.
Summary of the invention
The objective of the invention is in order to solve the deficiency of above-mentioned L-proline(Pro) extracting and purifying method, thereby provide a kind of method of utilizing membrane separation technique from fermented liquid, to extract the L-proline(Pro), both improved the purification effect of L-proline(Pro), improved economic benefit, reduce the discharging of waste water again, increased environmental benefit.
To achieve these goals, the present invention is undertaken by following processing step:
1) micro-filtration filters: L-proline(Pro) fermented liquid is passed through microfiltration membrane, the used film of micro-filtration is ceramic membrane or organic membrane, its aperture is at 0.05-10 μ m, service temperature is 10-90 ℃, operating pressure: entrance pressure is 2-8bar, go out to press to be 0-5bar, obtain the micro-filtration dialyzate and the tropina of fermented liquid, after the tropina drying as high-quality feed;
2) ultra-filtration filters: the micro-filtration dialyzate in the step 1) is passed through ultra-filtration membrane, the used mould material of ultrafiltration is selected a kind of in PAN, PVDF, PC, PES, PP, the PE composite membrane for use, its molecular weight cut-off is 10000-100000, service temperature is 30-50 ℃, operating pressure: entrance pressure is 1-8bar, go out to press, obtain ultrafiltration dialysis liquid and concentrated solution, be used for producing biological fermentation fertilizer after the concentrated solution drying to 0.5-3bar;
3) the ultrafiltration dialysis liquid reverse osmosis concentration: with step 2) passes through reverse osmosis membrane, the used mould material of reverse osmosis membrane is selected a kind of in PAN, PVDF, PC, PES, PP, the PE composite membrane for use, to the NaCl rejection is more than 95%, service temperature is 30-50 ℃, operating pressure: entrance pressure is 11-50bar, go out to press to 10.5-30bar, obtain reverse osmosis dialyzate and pure water, pure water is back to production;
4) decrease temperature crystalline after the reverse osmosis dialyzate evaporation concentration in the step 3) is obtained crude product L-proline(Pro), promptly obtain L-proline(Pro) product after the crude product L-proline(Pro) of gained is molten through alcohol, decolouring, crystallization, centrifugal, the oven dry.
The present invention utilizes membrane separation technique to extract the method for L-proline(Pro) from fermented liquid, compared with prior art has the following advantages:
Need not add flocculating aids or flocculation agent when 1, micro-filtration removes albumen, the bacterium slag is made feed does not have other side effect, compliance with environmental protection requirements; Need not sheet frame etc. device, supporting cost is low; The rate of recovery of tropina will exceed 30% up to more than 95% than traditional method, and convection drying can get highly purified tropina;
2, the filtering accuracy height of ultra-filtration membrane, filtration rear filtrate quality is good, helps subsequent extractions, improves the product crystalline quality;
3, carry out pre-concentration with reverse osmosis, realize cold concentration, reduce steam consumption, reduce production costs;
4, the present invention does not adopt ion exchange process, has controlled the generation of L-proline(Pro) production process middle and high concentration waste water on the source, reduces the consumption of sulfuric acid and liquefied ammonia, has reduced discharge of wastewater, has alleviated environmental protection pressure, and effects of energy saving and emission reduction is remarkable.
In a word, the present invention has fundamentally solved the problem of environmental pollution in the L-proline(Pro) leaching process, and has reduced production cost, has improved economic benefit, has promoted product specification, promotes the sustainable development that the L-proline(Pro) is produced.
Embodiment
Further set forth the present invention below by the detailed description of specific embodiment of the present invention being utilized membrane separation technique from fermented liquid, extract the method for L-proline(Pro), but embodiment not a limitation of the present invention.
Embodiment
1) micro-filtration filters: with content is that 6% L-proline(Pro) fermented liquid 1500Kg filters by micro-filtration, it is that the aperture is the ceramic membrane of 0.05 μ m that micro-filtration filters used mould material, service temperature is 55 ℃, entrance pressure is 3.0bar, go out to press and be with 600Kg albumen wash water, to obtain the micro-filtration dialyzate 1900Kg of L-proline(Pro) and the tropina of 200Kg by 1.0bar, the transmittance of dialyzate is 80%, and albumen is after drying as feed;
2) ultra-filtration filters: the micro-filtration dialyzate of step 1) gained is passed through ultra-filtration filters, the used mould material of ultrafiltration is that molecular weight cut-off is the ultra-filtration membrane of 30000 PVDF, service temperature is 40 ℃, entrance pressure is 7bar, go out to press to be 2bar, with 600Kg albumen wash water, get ultrafiltration dialysis liquid 2300Kg and 200Kg ultrafiltration and concentration liquid, the transmittance of dialyzate is 93%;
3) reverse osmosis concentration: with step 2) the ultrafiltration dialysis liquid of gained passes through osmosis filtration, the used mould material of reverse osmosis is that to hold back NaCl be 97% PVDF reverse osmosis membrane, service temperature is 40 ℃, entrance pressure is 18bar, go out to press to be 17bar, get the pure water of reverse osmosis dialyzate 750Kg and 1550Kg, the pure water reuse is produced;
4) with decrease temperature crystalline after the reverse osmosis dialyzate evaporation concentration in the step 3), obtain containing the thick product 90Kg of L-proline(Pro) of moisture 20%, obtain high-quality L-proline(Pro) 60Kg after the crude product L-proline(Pro) of gained is molten through alcohol, decolouring, crystallization, centrifugal, the oven dry.
Evaporation concentration, decrease temperature crystalline, alcohol are molten, decolouring, crystallization, centrifugal, baking operation, belong to amino acid purification common process.
Claims (1)
1, a kind of method of utilizing membrane separation technique to extract the L-proline(Pro) from fermented liquid is characterized in that being undertaken by following processing step:
1) micro-filtration filters: by microfiltration membrane, the used film of micro-filtration is ceramic membrane or organic membrane with L-proline(Pro) fermented liquid, and its aperture is at 0.05-10 μ m, service temperature is 10-90 ℃, operating pressure: entrance pressure is 2-8bar, goes out to press to be 0-5bar, obtains the micro-filtration dialyzate and the tropina of fermented liquid;
2) ultra-filtration filters: the micro-filtration dialyzate in the step 1) is passed through ultra-filtration membrane, the used mould material of ultrafiltration is selected a kind of in PAN, PVDF, PC, PES, PP, the PE composite membrane for use, its molecular weight cut-off is 10000-100000, service temperature is 30-50 ℃, operating pressure: entrance pressure is 1-8bar, go out to press, obtain ultrafiltration dialysis liquid and concentrated solution to 0.5-3bar;
3) the ultrafiltration dialysis liquid reverse osmosis concentration: with step 2) passes through reverse osmosis membrane, the used mould material of reverse osmosis membrane is selected a kind of in PAN, PVDF, PC, PES, PP, the PE composite membrane for use, to the NaCl rejection is more than 95%, service temperature is 30-50 ℃, operating pressure: entrance pressure is 11-50bar, go out to press, can obtain reverse osmosis dialyzate and pure water to 10.5-30bar;
4) decrease temperature crystalline after the reverse osmosis dialyzate evaporation concentration in the step 3) is obtained crude product L-proline(Pro), promptly obtain L-proline(Pro) product after the crude product L-proline(Pro) of gained is molten through alcohol, decolouring, crystallization, centrifugal, the oven dry.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200910017941A CN101633634A (en) | 2009-08-16 | 2009-08-16 | Method for extracting L-proline from fermentation liquor by membrane separation technology |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102675180A (en) * | 2012-05-31 | 2012-09-19 | 精晶药业有限公司 | Method for extracting proline |
| CN103265467A (en) * | 2013-05-06 | 2013-08-28 | 华南理工大学 | Method for cooling, crystallizing and refining L-proline |
| CN105777603A (en) * | 2016-04-01 | 2016-07-20 | 天津市敬业精细化工有限公司 | Method for extracting L-hydroxyproline from L-hydroxyproline fermentation liquor |
| CN105831734A (en) * | 2016-03-25 | 2016-08-10 | 中国农业科学院农产品加工研究所 | Method of gradient in-series membrane concentration for bone extract liquid |
| CN105837488A (en) * | 2016-03-31 | 2016-08-10 | 天津市敬业精细化工有限公司 | Hydroxyproline fermentation production technology |
| CN106336370A (en) * | 2016-08-11 | 2017-01-18 | 山东阜丰发酵有限公司 | Extraction and purification process of proline |
| CN106543063A (en) * | 2016-09-23 | 2017-03-29 | 合肥信达膜科技有限公司 | A kind of proline extraction element and method |
| CN106966945A (en) * | 2017-03-29 | 2017-07-21 | 沁浩膜技术(厦门)有限公司 | A kind of full embrane method extracting method of L hydroxyprolines zymotic fluid |
| CN106966946A (en) * | 2017-03-29 | 2017-07-21 | 沁浩膜技术(厦门)有限公司 | A kind of full embrane method extracting method of L proline Fermentation Broths |
| CN107619740A (en) * | 2017-09-25 | 2018-01-23 | 河南省金路达食品科技有限公司 | A kind of preparation method of pure fermented honey moderate wine |
| CN109265337A (en) * | 2018-10-30 | 2019-01-25 | 徐州绿油油生物肥料有限公司 | A kind of embrane method extraction process for extracting succinic acid from bio-fermented liquid |
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2009
- 2009-08-16 CN CN200910017941A patent/CN101633634A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102675180A (en) * | 2012-05-31 | 2012-09-19 | 精晶药业有限公司 | Method for extracting proline |
| CN103265467A (en) * | 2013-05-06 | 2013-08-28 | 华南理工大学 | Method for cooling, crystallizing and refining L-proline |
| CN105831734A (en) * | 2016-03-25 | 2016-08-10 | 中国农业科学院农产品加工研究所 | Method of gradient in-series membrane concentration for bone extract liquid |
| CN105831734B (en) * | 2016-03-25 | 2020-03-10 | 中国农业科学院农产品加工研究所 | Method for concentrating bone extract by gradient series membrane |
| CN105837488A (en) * | 2016-03-31 | 2016-08-10 | 天津市敬业精细化工有限公司 | Hydroxyproline fermentation production technology |
| CN105837488B (en) * | 2016-03-31 | 2019-02-15 | 天津市敬业精细化工有限公司 | A kind of hydroxyproline fermentation manufacturing technique |
| CN105777603A (en) * | 2016-04-01 | 2016-07-20 | 天津市敬业精细化工有限公司 | Method for extracting L-hydroxyproline from L-hydroxyproline fermentation liquor |
| CN105777603B (en) * | 2016-04-01 | 2019-02-15 | 天津市敬业精细化工有限公司 | A method of extracting L- hydroxyproline from L- hydroxyproline fermentation liquid |
| CN106336370B (en) * | 2016-08-11 | 2018-07-27 | 山东阜丰发酵有限公司 | A kind of extraction and purification process of proline |
| CN106336370A (en) * | 2016-08-11 | 2017-01-18 | 山东阜丰发酵有限公司 | Extraction and purification process of proline |
| CN106543063A (en) * | 2016-09-23 | 2017-03-29 | 合肥信达膜科技有限公司 | A kind of proline extraction element and method |
| CN106966946A (en) * | 2017-03-29 | 2017-07-21 | 沁浩膜技术(厦门)有限公司 | A kind of full embrane method extracting method of L proline Fermentation Broths |
| CN106966945A (en) * | 2017-03-29 | 2017-07-21 | 沁浩膜技术(厦门)有限公司 | A kind of full embrane method extracting method of L hydroxyprolines zymotic fluid |
| CN107619740A (en) * | 2017-09-25 | 2018-01-23 | 河南省金路达食品科技有限公司 | A kind of preparation method of pure fermented honey moderate wine |
| CN109265337A (en) * | 2018-10-30 | 2019-01-25 | 徐州绿油油生物肥料有限公司 | A kind of embrane method extraction process for extracting succinic acid from bio-fermented liquid |
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