CN104817452A - Method for extracting abscisic acid from abscisic acid fermentation liquor - Google Patents
Method for extracting abscisic acid from abscisic acid fermentation liquor Download PDFInfo
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- CN104817452A CN104817452A CN201410799073.1A CN201410799073A CN104817452A CN 104817452 A CN104817452 A CN 104817452A CN 201410799073 A CN201410799073 A CN 201410799073A CN 104817452 A CN104817452 A CN 104817452A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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Abstract
The invention discloses a method for extracting an abscisic acid from an abscisic acid fermentation liquor. The method comprises the following steps: successively performing pH regulation, preprocessing, ceramic membrane filtration, rolling type ultrafiltration, concentration of concentration membranes, menstruum extraction, evaporation concentration, crystallization and drying on the abscisic acid fermentation liquor so as to obtain a finished product of the abscisic acid. The method disclosed by the invention simplifies the process of extracting the abscisic acid from the abscisic acid fermentation liquor and improves production efficiency, meanwhile the purity of the obtained abscisic acid product conforms to requirements.
Description
Technical field
The invention belongs to dormin purification techniques field, be specifically related to a kind of method extracting dormin from dormin fermented liquid.
Background technology
In prior art, the dormin extracted in fermented liquid mainly first passes through Plate Filtration, tubular membrane filtration, spiral wound and concentrated membrane concentration successively, obtain dormin concentrated solution, again by this dormin concentrated solution successively after solvent extraction, evaporation concentration, crystallization and drying, obtain finished product, adopt aforesaid method to extract dormin, complex steps, efficiency are lower, and the foreign matter content of products obtained therefrom is higher.
Summary of the invention
The object of the invention is to overcome prior art defect, a kind of method extracting dormin from dormin fermented liquid is provided.
Concrete technical scheme of the present invention is as follows:
From dormin fermented liquid, extract a method for dormin, comprise the steps:
(1) pre-treatment is carried out by behind dormin fermented liquid adjust ph to 5.5 ~ 7.0;
(2) be that the ceramic membrane of 50 ~ 60nm filters pretreated dormin fermented liquid with filtering accuracy, obtain the first ceramic membrane concentrated solution and the first ceramic membrane dialyzate, the design parameter of this step is as follows: normal-temperature operation, average entrance pressure 2 ~ 3bar, on average go out pressure 2 ~ 3bar, circulating pressure 2 ~ 3bar, circular flow 10 ~ 12m
3/ h, cycles of concentration is 2 times, and average flux is 160 ~ 172LMH;
(3) continue to add water, with above-mentioned ceramic membrane, 1000ppm is less than to the content that above-mentioned first ceramic membrane concentrated solution carries out wash-out process dormin extremely wherein, obtains the second ceramic membrane dialyzate and the second ceramic membrane concentrated solution;
(4) after the first ceramic membrane dialyzate and the second ceramic membrane dialyzate being merged, with the rolling ultrafiltration membrane process that molecular weight cut-off is 5000 ~ 6000, obtain ultrafiltration and concentration liquid and ultrafiltration permeate, the design parameter of this step is as follows: normal-temperature operation, on average go out pressure 18 ~ 21bar, average flux 55 ~ 73LMH, cycles of concentration is 11 ~ 13 times;
(5) by ultrafiltration membrane permeate liquid molecular weight cut-off be 50 ~ 60 concentrated film process, obtain dormin concentrated solution, this step design parameter is as follows: normal-temperature operation, on average goes out pressure 18 ~ 21bar, average flux 22 ~ 29LMH;
(6) by the dormin concentrated solution of gained successively after solvent extraction, evaporation concentration, crystallization and drying, get product.
In a preferred embodiment of the invention, the pre-treatment in described step (1) is for using Plate Filtration.
Preferred further, the average flux of described step (2) is 170 ~ 172LMH.
In a preferred embodiment of the invention, the pre-treatment in described step (1) is: by dormin fermented liquid in 60 ~ 80 DEG C, deactivation 20 ~ 40min.
Preferred further, the average flux of described step (2) is 163 ~ 167LMH.
In a preferred embodiment of the invention, the filtering accuracy of described ceramic membrane is 50nm;
In a preferred embodiment of the invention, the model of described rolling ultrafiltration membrane is S-274, and molecular weight cut-off is 5000.
In a preferred embodiment of the invention, the model of described concentrated film is S-400, and molecular weight cut-off is 50.
The invention has the beneficial effects as follows: method of the present invention simplifies the process extracting dormin from dormin fermented liquid, improves production efficiency, and the purity of the dormin product of gained meets the requirements.
Embodiment
Be further detailed below by way of embodiment technical scheme of the present invention and describe.
Embodiment 1
(1) by the rear Plate Filtration of dormin fermented liquid adjust ph to 6.5;
(2) be that the ceramic membrane of 50nm filters the dormin fermented liquid after Plate Filtration with filtering accuracy, obtain the first ceramic membrane concentrated solution and the first ceramic membrane dialyzate, the design parameter of this step is as follows: normal-temperature operation, average entrance pressure 2.3bar, on average go out to press 2.3bar, circulating pressure 3bar, circular flow 10.8m
3/ h, cycles of concentration is 2 times, and average flux is 171.8LMH;
(3) continue the water of the volume 1.5 times adding dormin fermented liquid, be 699ppm with the content that above-mentioned ceramic membrane carries out wash-out process dormin extremely wherein to above-mentioned first ceramic membrane concentrated solution, obtain the second ceramic membrane dialyzate and the second ceramic membrane concentrated solution;
(4) the second ceramic membrane concentrated solution in ceramic membrane is discharged, after rinsing well with clear water, with the first scavenging solution containing sodium hydroxide and clorox in 60 DEG C, to above-mentioned ceramic membrane cleaning 60min, then to rinse the first scavenging solution in ceramic membrane to pH well with clear water be neutral;
(5) after the first ceramic membrane dialyzate and the second ceramic membrane dialyzate being merged, with the S-274 rolling ultrafiltration membrane process that molecular weight cut-off is 5000, obtain ultrafiltration and concentration liquid and ultrafiltration permeate, the design parameter of this step is as follows: normal-temperature operation, on average go out to press 18.7bar, average flux 58LMH, cycles of concentration is 11 times;
(6) the ultrafiltration and concentration liquid in rolling ultrafiltration membrane is discharged, after rinsing well with clear water, with pH be second scavenging solution with the preparation of 90# clean-out system of 10 in 40 DEG C, to above-mentioned spiral wound Membrane cleaning 40min, then to rinse the second scavenging solution in rolling ultrafiltration membrane to pH well with clear water be neutral;
(7) by ultrafiltration membrane permeate liquid molecular weight cut-off be 50 S-400 concentrate film process, obtain dormin concentrated solution, this step design parameter is as follows: normal-temperature operation, on average goes out to press 18bar, average flux 22.5LMH, and cycles of concentration is 3.1;
(8) the dormin concentrated solution in concentrated film is discharged, after rinsing well with clear water, with described pH be second scavenging solution with the preparation of 90# clean-out system of 10 in 40 DEG C, to above-mentioned concentrated Membrane cleaning 40min, then to rinse the second scavenging solution in concentrated film to pH well with clear water be neutral;
(9) by the dormin concentrated solution of gained successively after solvent extraction, evaporation concentration, crystallization and drying, obtain the finished product that purity is 98.2%.
Embodiment 2
(1) carry out pre-treatment by after dormin fermented liquid adjust ph to 6.5, this pre-treatment is by dormin fermented liquid in 60 DEG C, deactivation 30min;
(2) be that the ceramic membrane of 50nm filters the dormin fermented liquid after Plate Filtration with filtering accuracy, obtain the first ceramic membrane concentrated solution and the first ceramic membrane dialyzate, the design parameter of this step is as follows: normal-temperature operation, average entrance pressure 2.1bar, on average go out to press 2.1bar, circulating pressure 2.9bar, circular flow 11m
3/ h, cycles of concentration is 2 times, and average flux is 166.7LMH;
(3) continue the water of the volume 2 times adding dormin fermented liquid, be 341ppm with the content that above-mentioned ceramic membrane carries out wash-out process dormin extremely wherein to above-mentioned first ceramic membrane concentrated solution, obtain the second ceramic membrane dialyzate and the second ceramic membrane concentrated solution;
(4) the second ceramic membrane concentrated solution in ceramic membrane is discharged, after rinsing well with clear water, with the first scavenging solution containing sodium hydroxide and clorox in 60 DEG C, to above-mentioned ceramic membrane cleaning 60min, then to rinse the first scavenging solution in ceramic membrane to pH well with clear water be neutral;
(5) after the first ceramic membrane dialyzate and the second ceramic membrane dialyzate being merged, with the S-274 rolling ultrafiltration membrane process that molecular weight cut-off is 5000, obtain ultrafiltration and concentration liquid and ultrafiltration permeate, the design parameter of this step is as follows: normal-temperature operation, on average go out to press 18.1bar, average flux 72.6LMH, cycles of concentration is 13 times;
(6) the ultrafiltration and concentration liquid in rolling ultrafiltration membrane is discharged, after rinsing well with clear water, with pH be second scavenging solution with the preparation of 90# clean-out system of 10 in 40 DEG C, to above-mentioned spiral wound Membrane cleaning 40min, then to rinse the second scavenging solution in rolling ultrafiltration membrane to pH well with clear water be neutral;
(7) by ultrafiltration membrane permeate liquid molecular weight cut-off be 50 S-400 concentrate film process, obtain dormin concentrated solution, this step design parameter is as follows: normal-temperature operation, on average goes out to press 18bar, average flux 23.1LMH, and cycles of concentration is 3;
(8) the dormin concentrated solution in concentrated film is discharged, after rinsing well with clear water, with described pH be second scavenging solution with the preparation of 90# clean-out system of 10 in 40 DEG C, to above-mentioned concentrated Membrane cleaning 40min, then to rinse the second scavenging solution in concentrated film to pH well with clear water be neutral;
(9) by the dormin concentrated solution of gained successively after solvent extraction, evaporation concentration, crystallization and drying, obtaining purity is 99.7% finished product.
Embodiment 3
(1) carry out pre-treatment by after dormin fermented liquid adjust ph to 6.5, this pre-treatment is by dormin fermented liquid in 60 DEG C, deactivation 30min;
(2) be that the ceramic membrane of 50nm filters the dormin fermented liquid after Plate Filtration with filtering accuracy, obtain the first ceramic membrane concentrated solution and the first ceramic membrane dialyzate, the design parameter of this step is as follows: normal-temperature operation, average entrance pressure 2.3bar, on average go out to press 2.3bar, circulating pressure 3bar, circular flow 10.8m
3/ h, cycles of concentration is 2 times, and average flux is 163.3LMH;
(3) continue the water of the volume 3 times adding dormin fermented liquid, be 65ppm with the content that above-mentioned ceramic membrane carries out wash-out process dormin extremely wherein to above-mentioned first ceramic membrane concentrated solution, obtain the second ceramic membrane dialyzate and the second ceramic membrane concentrated solution;
(4) the second ceramic membrane concentrated solution in ceramic membrane is discharged, after rinsing well with clear water, with the first scavenging solution containing sodium hydroxide and clorox in 60 DEG C, to above-mentioned ceramic membrane cleaning 60min, then to rinse the first scavenging solution in ceramic membrane to pH well with clear water be neutral;
(5) after the first ceramic membrane dialyzate and the second ceramic membrane dialyzate being merged, with the S-274 rolling ultrafiltration membrane process that molecular weight cut-off is 5000, obtain ultrafiltration and concentration liquid and ultrafiltration permeate, the design parameter of this step is as follows: normal-temperature operation, on average go out to press 18.3bar, average flux 70.6LMH, cycles of concentration is 13 times;
(6) the ultrafiltration and concentration liquid in rolling ultrafiltration membrane is discharged, after rinsing well with clear water, with pH be second scavenging solution with the preparation of 90# clean-out system of 10 in 40 DEG C, to above-mentioned spiral wound Membrane cleaning 40min, then to rinse the second scavenging solution in rolling ultrafiltration membrane to pH well with clear water be neutral;
(7) by ultrafiltration membrane permeate liquid molecular weight cut-off be 50 S-400 concentrate film process, obtain dormin concentrated solution, this step design parameter is as follows: normal-temperature operation, on average goes out to press 20bar, average flux 27LMH, and cycles of concentration is 9;
(8) the dormin concentrated solution in concentrated film is discharged, after rinsing well with clear water, with described pH be second scavenging solution with the preparation of 90# clean-out system of 10 in 40 DEG C, to above-mentioned concentrated Membrane cleaning 40min, then to rinse the second scavenging solution in concentrated film to pH well with clear water be neutral;
(9) by the dormin concentrated solution of gained successively after solvent extraction, evaporation concentration, crystallization and drying, obtaining purity is 99.9% finished product.
The above, be only preferred embodiment of the present invention, therefore can not limit scope of the invention process according to this, the equivalence change namely done according to the scope of the claims of the present invention and description with modify, all should still belong in scope that the present invention contains.
Claims (8)
1. from dormin fermented liquid, extract a method for dormin, it is characterized in that: comprise the steps:
(1) pre-treatment is carried out by behind dormin fermented liquid adjust ph to 5.5 ~ 7.0;
(2) be that the ceramic membrane of 50 ~ 60nm filters pretreated dormin fermented liquid with filtering accuracy, obtain the first ceramic membrane concentrated solution and the first ceramic membrane dialyzate, the design parameter of this step is as follows: normal-temperature operation, average entrance pressure 2 ~ 3bar, on average go out pressure 2 ~ 3bar, circulating pressure 2 ~ 3bar, circular flow 10 ~ 12m3/h, cycles of concentration is 2 times, and average flux is 160 ~ 172LMH;
(3) continue to add water, with above-mentioned ceramic membrane, 1000ppm is less than to the content that above-mentioned first ceramic membrane concentrated solution carries out wash-out process dormin extremely wherein, obtains the second ceramic membrane dialyzate and the second ceramic membrane concentrated solution;
(4) after the first ceramic membrane dialyzate and the second ceramic membrane dialyzate being merged, with the rolling ultrafiltration membrane process that molecular weight cut-off is 5000 ~ 6000, obtain ultrafiltration and concentration liquid and ultrafiltration permeate, the design parameter of this step is as follows: normal-temperature operation, on average go out pressure 18 ~ 21bar, average flux 55 ~ 73LMH, cycles of concentration is 11 ~ 13 times;
(5) by ultrafiltration membrane permeate liquid molecular weight cut-off be 50 ~ 60 concentrated film process, obtain dormin concentrated solution, this step design parameter is as follows: normal-temperature operation, on average goes out pressure 18 ~ 21bar, average flux 22 ~ 29LMH;
(6) by the dormin concentrated solution of gained successively after solvent extraction, evaporation concentration, crystallization and drying, get product.
2. a kind of method extracting dormin from dormin fermented liquid as claimed in claim 1, is characterized in that: the pre-treatment in described step (1) is for using Plate Filtration.
3. a kind of method extracting dormin from dormin fermented liquid as claimed in claim 2, is characterized in that: the average flux of described step (2) is 170 ~ 172LMH.
4. a kind of method extracting dormin from dormin fermented liquid as claimed in claim 1, is characterized in that: the pre-treatment in described step (1) is: by dormin fermented liquid in 60 ~ 80 DEG C, deactivation 20 ~ 40min.
5. a kind of method extracting dormin from dormin fermented liquid as claimed in claim 4, is characterized in that: the average flux of described step (2) is 163 ~ 167LMH.
6. a kind of method extracting dormin from dormin fermented liquid as claimed in claim 1, is characterized in that: the filtering accuracy of described ceramic membrane is 50nm.
7. a kind of method extracting dormin from dormin fermented liquid as claimed in claim 1, is characterized in that: the model of described rolling ultrafiltration membrane is S-274, and molecular weight cut-off is 5000.
8. a kind of method extracting dormin from dormin fermented liquid as claimed in claim 1, is characterized in that: the model of described concentrated film is S-400, and molecular weight cut-off is 50.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439847A (en) * | 2015-12-23 | 2016-03-30 | 江西新瑞丰生化有限公司 | Separation purification method for natural abscisic acid |
| CN105439846A (en) * | 2015-12-23 | 2016-03-30 | 江西新瑞丰生化有限公司 | Purification method for natural abscisic acid |
| CN105541603A (en) * | 2015-12-23 | 2016-05-04 | 江西新瑞丰生化有限公司 | Method for separating natural abscisic acid crude product from abscisic acid fermentation broth |
| CN106905142A (en) * | 2017-04-18 | 2017-06-30 | 四川龙蟒福生科技有限责任公司 | A kind of isolation and purification method of S abscisic acids |
| CN107047552A (en) * | 2017-04-18 | 2017-08-18 | 四川龙蟒福生科技有限责任公司 | The recoverying and utilizing method of accessory substance in a kind of S abscisic acids production |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56160996A (en) * | 1980-05-15 | 1981-12-11 | Kyowa Hakko Kogyo Co Ltd | Preparation of abscisic acid by fermentation method |
| CN1749401A (en) * | 2004-09-14 | 2006-03-22 | 中国科学院成都生物研究所 | A kind of extracting method of PBI 58 |
| CN101691349A (en) * | 2009-10-20 | 2010-04-07 | 山东恩贝生物工程有限公司 | Process for extracting tryptophan from fermentation liquid |
| CN102399686A (en) * | 2011-09-18 | 2012-04-04 | 淮北市三和诺生物工程有限责任公司 | After-extraction production line for fermentation liquid of enzymic preparation |
| CN102586088A (en) * | 2011-09-18 | 2012-07-18 | 淮北市三和诺生物工程有限责任公司 | Sterile ultrafiltration concentration enzymic preparation fermentation broth post-extraction production line |
| CN104109181A (en) * | 2014-06-30 | 2014-10-22 | 北大医药重庆大新药业股份有限公司 | Membrane filtration process method of meleumycin |
-
2014
- 2014-12-19 CN CN201410799073.1A patent/CN104817452B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56160996A (en) * | 1980-05-15 | 1981-12-11 | Kyowa Hakko Kogyo Co Ltd | Preparation of abscisic acid by fermentation method |
| CN1749401A (en) * | 2004-09-14 | 2006-03-22 | 中国科学院成都生物研究所 | A kind of extracting method of PBI 58 |
| CN101691349A (en) * | 2009-10-20 | 2010-04-07 | 山东恩贝生物工程有限公司 | Process for extracting tryptophan from fermentation liquid |
| CN102399686A (en) * | 2011-09-18 | 2012-04-04 | 淮北市三和诺生物工程有限责任公司 | After-extraction production line for fermentation liquid of enzymic preparation |
| CN102586088A (en) * | 2011-09-18 | 2012-07-18 | 淮北市三和诺生物工程有限责任公司 | Sterile ultrafiltration concentration enzymic preparation fermentation broth post-extraction production line |
| CN104109181A (en) * | 2014-06-30 | 2014-10-22 | 北大医药重庆大新药业股份有限公司 | Membrane filtration process method of meleumycin |
Non-Patent Citations (1)
| Title |
|---|
| 郑珩等: "灰绿葡萄孢发酵液中天然型脱落酸的分离纯化", 《中国抗生素杂志》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439847A (en) * | 2015-12-23 | 2016-03-30 | 江西新瑞丰生化有限公司 | Separation purification method for natural abscisic acid |
| CN105439846A (en) * | 2015-12-23 | 2016-03-30 | 江西新瑞丰生化有限公司 | Purification method for natural abscisic acid |
| CN105541603A (en) * | 2015-12-23 | 2016-05-04 | 江西新瑞丰生化有限公司 | Method for separating natural abscisic acid crude product from abscisic acid fermentation broth |
| CN105541603B (en) * | 2015-12-23 | 2019-04-19 | 江西新瑞丰生化有限公司 | A method of separating natural falls off acid crude from abscisic acid fermentation liquid |
| CN106905142A (en) * | 2017-04-18 | 2017-06-30 | 四川龙蟒福生科技有限责任公司 | A kind of isolation and purification method of S abscisic acids |
| CN107047552A (en) * | 2017-04-18 | 2017-08-18 | 四川龙蟒福生科技有限责任公司 | The recoverying and utilizing method of accessory substance in a kind of S abscisic acids production |
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