CN106278919A - A kind of method preparing L isoleucine propylhomoserin - Google Patents
A kind of method preparing L isoleucine propylhomoserin Download PDFInfo
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- CN106278919A CN106278919A CN201610655172.1A CN201610655172A CN106278919A CN 106278919 A CN106278919 A CN 106278919A CN 201610655172 A CN201610655172 A CN 201610655172A CN 106278919 A CN106278919 A CN 106278919A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/01—Separation of suspended solid particles from liquids by sedimentation using flocculating agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/08—Cellulose derivatives
- C08L1/26—Cellulose ethers
- C08L1/28—Alkyl ethers
- C08L1/286—Alkyl ethers substituted with acid radicals, e.g. carboxymethyl cellulose [CMC]
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L3/00—Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
- C08L3/02—Starch; Degradation products thereof, e.g. dextrin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Organic Chemistry (AREA)
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to aminoacid preparation field, disclose a kind of method preparing L isoleucine, it comprises the steps: step 1) micro-filtrate membrane filtration and flocculation purification, step 2) ultrafiltration membrance filter, step 3) condensing crystallizing.The inventive method simple possible, the yield of L isoleucine and purity are high, have a extensive future.
Description
Technical field
The invention belongs to aminoacid preparation field, specifically provide a kind of method preparing ILE.
Background technology
Isoleucine, formal name used at school 2-amino-3 methylvaleric acid, call isoleucine, be wherein the one of 20 kinds of primary amino acids
Kind, almost it is present in the structure of all proteins.Isoleucine has 2 asymmetric carbon atoms, therefore it exists 4 kinds of stereoisomerisms
Body and the diastereomer of 2 ILEs, but nature only exists ILE one type.Due to the different bright ammonia of L-
Acid can not synthesize in human body, so it is essential amino acid, is referred to as branched-amino with L-Leu, Valine
Acid, because of the 26S Proteasome Structure and Function that it is special, has important function in human life metabolism.
At present, the production method of ILE has extraction method, chemical synthesis, fermentation method.Implement in commercial production
Major part is fermentation method.The method extracting ILE from fermentation liquid typically uses sedimentation, ion exchange and embrane method
Deng.The consumable goods of extraction process and the purity of product decide the profit of enterprise.How to reduce production cost, alleviate environment pressure
Power, and then improve the competitiveness of enterprise self, it is the matter of utmost importance of industry competition.
Summary of the invention
In order to overcome the defects such as prior art ILE extraction process is loaded down with trivial details, purity is low, the invention provides one
The method preparing ILE.
The present invention is achieved by the following technical solution:
A kind of method preparing ILE, it comprises the steps: step 1) micro-filtrate membrane filtration and flocculation purification, step 2)
Ultrafiltration membrance filter, step 3) condensing crystallizing.
Specifically, described method comprises the steps:
Step 1) micro-filtrate membrane filtration and flocculation purification: ILE fermentation liquid is once filtered by micro-filtration membrane, is fermented
The microfiltration dialysis solution of liquid and tropina, sell as high-quality tropina after tropina drying；Then add and account for microfiltration
Dialysis solution 1%(w/w) flocculant, 200 turns/min stirs 10min, then stands 120min, micro-filtration membrane secondary filter, and it is heavy to collect
Form sediment and supernatant；
Step 2) ultrafiltration membrance filter: by the supernatant in step 1) by ultrafiltration membrance filter, obtain ultrafiltration dialysis liquid and concentrated solution,
The precipitation mixing of concentrated solution and step 1), is used for after drying producing forage protein；
Step 3) condensing crystallizing: ultrafiltration dialysis liquid is condensed into 1/4th of original volume, and then slow cooling is to 20 DEG C, regulation
The pH of solution is 6, settles 5 hours, centrifugal, collects precipitate, is put into by precipitate in purified water, then adds accounting for precipitate
Flocculant 1.5%(w/w), 200 turns/min stirs 10min, then filters for three times by micro-filtration membrane, removes precipitation, collect supernatant,
Being condensed into 1/3rd of original volume, then the pH regulating solution is 6, temperature controls at 18 DEG C, settles 6 hours；Centrifugal acquisition is tied
Brilliant ILE.
Described flocculant is prepared according to following technique:
1) toward starch adds the purified water accounting for starch twice quality, it is uniformly mixing to obtain suspension, is subsequently adding and the matter such as starch
The sodium carboxymethyl cellulose of amount, 200 turns/min stirs 30min, is subsequently placed in 80 DEG C and dries to moisture 5%(percent mass
Than) below, obtain modified starch；
2) take chitosan, sodium humate and pectin, mixing and stirring according to the mass ratio of 5:1:0.2, then add and account for shell
The sodium hydrate aqueous solution of the 2M of polysaccharide twice quality, the ultrasonic 10min of 30KHz, last 500 turns/min stir 3min, obtain
Modification of chitosan；
3) corn stalk powder, meerschaum are pulverized respectively obtain corn stalk powder and sepiolite powder, by corn stalk powder, sepiolite powder
And kieselguhr according to the quality of 3:1:1 than mixing and stirring, add the hydrogen-oxygen that concentration is 1M accounting for 5 times of weight of kieselguhr to
Changing in sodium solution, 200 turns/min stirs 120min, then filters, and is dried, grinds to form the powder that particle diameter is 10-20 mesh；
4) by modified starch, modification of chitosan and step 3) gained powder according to the quality of 5:3:2 than mixing and stirring, so
It is placed in closed reactor, rises to 150 DEG C with the heating rate of 2 DEG C/s, be incubated 30min, take out, put in agitator,
500 turns/min stirs 3min, obtains compound, is placed in baking oven, dries 90min for 80 DEG C, takes out, pulverize and get final product.
Preferably,
The condition that described micro-filtration membrane once filters, secondary filter and three times are filtered is: micro-filtration membrane is inorganic ceramic film, retains
Molecular weight is 10000Da, and microfiltration temperature is 40 DEG C；The condition of described ultrafiltration membrance filter is: ultrafilter membrane molecular cut off is
200Da, ultrafiltrate temperature is 40 DEG C.
The beneficial effect that the present invention obtains specifically includes that
The present invention combines novel flocculant remove impurity by membrane technology, and technique simple possible, relative to the patent skill before applicant
Art, substantially increases yield and purity, it is thus achieved that high-quality product, and enterprise income increases accordingly；The present invention provides a kind of novel
Flocculant, is suitable for amino acid zymotic fluid purification, it is to avoid chemical substance, flocculation purification is effective, with low cost, environment friendly and pollution-free；
More than 20% can be improved by adding flocculant purity of the present invention；
The present invention provides a kind of novel flocculant, is suitable for amino acid zymotic fluid purification, it is to avoid chemical substance, flocculation purification effect
Good, with low cost, environment friendly and pollution-free；Flocculant of the present invention is with agricultural wastes and natural mineral matter as primary raw material, this former
Material wide material sources and low cost, and prepare porous material, flocculation purification is effective, it is achieved that agricultural wastes reclaim profit
With；Aminoacid extraction process uses twice flocculant process, simplify operating procedure, provide cost savings, and make purification
Better, the flocculant after using is also used as fertilizer to be prepared, and turns waste into wealth.
Detailed description of the invention
Hereinafter the present invention is further explained by employing specific embodiment, but should not be construed as the present invention is created
The restriction of new spirit.
Embodiment 1
A kind of method preparing ILE, it comprises the steps:
Step 1) micro-filtrate membrane filtration and flocculation purification: the 1170kg ILE fermentation liquid that mass content is 1.69% is passed through
Micro-filtration membrane once filters, and obtains microfiltration dialysis solution and the tropina of fermentation liquid, as high-quality thalline after tropina drying
Albumen is sold；Then add account for microfiltration dialysis solution 1%(w/w) flocculant, 200 turns/min stirs 10min, then stands
120min, micro-filtration membrane secondary filter, collect precipitation and supernatant；
Step 2) ultrafiltration membrance filter: by the supernatant in step 1) by ultrafiltration membrance filter, obtain ultrafiltration dialysis liquid and concentrated solution,
The precipitation mixing of concentrated solution and step 1), is used for after drying producing forage protein；The condition that described supermembrane filters is: ultrafilter membrane
Molecular cut off is 200Da, and ultrafiltrate temperature is 40 DEG C；
Step 3) condensing crystallizing: ultrafiltration dialysis liquid is condensed into 1/4th of original volume, and then slow cooling is to 20 DEG C, regulation
The pH of solution is 6；Settle 5 hours, centrifugal, collect precipitate, precipitate is put in the purified water of double weight, then add
Account for precipitate 1.5%(w/w) flocculant, 200 turns/min stirs 10min, and then micro-filtration membrane filters for three times, removes precipitation, collects
Supernatant, is condensed into 1/3rd of original volume, then the pH regulating solution is 6；Temperature controls at 18 DEG C, settles 6 hours；Centrifugal
Obtain the ILE of crystallization, dry and obtain ILE product 16.39kg.After testing: the extraction ratio of ILE
Being 82.9%, HPLC detection purity is 99.1%.
The condition that described micro-filtration membrane once filters, secondary filter and three times are filtered is: micro-filtration membrane is inorganic ceramic film,
Molecular cut off is 10000Da, and microfiltration temperature is 40 DEG C；
Described flocculant is prepared according to following technique:
1) toward starch adds the purified water accounting for starch twice quality, it is uniformly mixing to obtain suspension, is subsequently adding and the matter such as starch
The sodium carboxymethyl cellulose of amount, 200 turns/min stirs 30min, is subsequently placed in 80 DEG C and dries to moisture 5%(percent mass
Than) below, obtain modified starch；
2) take chitosan, sodium humate and pectin, mixing and stirring according to the mass ratio of 5:1:0.2, then add and account for shell
The sodium hydrate aqueous solution of the 2M of polysaccharide twice quality, the ultrasonic 10min of 30KHz, last 500 turns/min stir 3min, obtain
Modification of chitosan；
3) corn stalk powder, meerschaum are pulverized respectively obtain corn stalk powder and sepiolite powder, by corn stalk powder, sepiolite powder
And kieselguhr according to the quality of 3:1:1 than mixing and stirring, add the hydrogen-oxygen that concentration is 1M accounting for 5 times of weight of kieselguhr to
Changing in sodium solution, 200 turns/min stirs 120min, then filters, and is dried, grinds to form the powder that particle diameter is 10-20 mesh；
4) by modified starch, modification of chitosan and step 3) gained powder according to the quality of 5:3:2 than mixing and stirring, so
It is placed in closed reactor, rises to 150 DEG C with the heating rate of 2 DEG C/s, be incubated 30min, take out, put in agitator,
500 turns/min stirs 3min, obtains compound, is placed in baking oven, dries 90min for 80 DEG C, takes out, pulverize and get final product.
Finally, in addition it is also necessary to be only several specific embodiments of the present invention it is noted that listed above.Obviously, this
Bright it is not limited to above example, it is also possible to have many deformation.Those of ordinary skill in the art can be from present disclosure
The all deformation directly derived or associate, are all considered as protection scope of the present invention.
Claims (4)
1. the method preparing ILE, it comprises the steps: step 1) micro-filtrate membrane filtration and flocculation purification, step
2) ultrafiltration membrance filter, step 3) condensing crystallizing.
Method the most according to claim 1, it is characterised in that described method comprises the steps:
Step 1) micro-filtrate membrane filtration and flocculation purification: ILE fermentation liquid is once filtered by micro-filtration membrane, is fermented
The microfiltration dialysis solution of liquid and tropina, sell as high-quality tropina after tropina drying；Then add and account for microfiltration
Dialysis solution 1%(w/w) flocculant, 200 turns/min stirs 10min, then stands 120min, then micro-filtration membrane secondary filter, collect
Precipitation and supernatant；
Step 2) ultrafiltration membrance filter: by the supernatant in step 1) by ultrafiltration membrance filter, obtain ultrafiltration dialysis liquid and concentrated solution,
The precipitation mixing of concentrated solution and step 1), is used for after drying producing forage protein；
Step 3) condensing crystallizing: ultrafiltration dialysis liquid is condensed into 1/4th of original volume, and then slow cooling is to 20 DEG C, regulation
The pH of solution is 6；Settle 5 hours, centrifugal, collect precipitate, precipitate is put in purified water, then add accounting for precipitate
Flocculant 1.5%(w/w), 200 turns/min stirs 10min, then filters for three times by micro-filtration membrane, removes precipitation, collect supernatant,
Being condensed into 1/3rd of original volume, then the pH regulating solution is 6, temperature controls at 18 DEG C, settles 6 hours；Finally it is centrifuged and obtains
The ILE that must crystallize.
Method the most according to claim 2, it is characterised in that described flocculant is prepared according to following technique:
1) toward starch adds the purified water accounting for starch twice quality, it is uniformly mixing to obtain suspension, is subsequently adding and the matter such as starch
The sodium carboxymethyl cellulose of amount, 200 turns/min stirs 30min, is subsequently placed in 80 DEG C and dries to moisture 5%(percent mass
Than) below, obtain modified starch；
2) take chitosan, sodium humate and pectin, mixing and stirring according to the mass ratio of 5:1:0.2, then add and account for shell
The sodium hydrate aqueous solution of the 2M of polysaccharide twice quality, the ultrasonic 10min of 30KHz, last 500 turns/min stir 3min, obtain
Modification of chitosan；
3) corn stalk powder, meerschaum are pulverized respectively obtain corn stalk powder and sepiolite powder, by corn stalk powder, sepiolite powder
And kieselguhr according to the quality of 3:1:1 than mixing and stirring, add the hydrogen-oxygen that concentration is 1M accounting for 5 times of weight of kieselguhr to
Changing in sodium solution, 200 turns/min stirs 120min, then filters, and is dried, grinds to form the powder that particle diameter is 10-20 mesh；
4) by modified starch, modification of chitosan and step 3) gained powder according to the quality of 5:3:2 than mixing and stirring, so
It is placed in closed reactor, rises to 150 DEG C with the heating rate of 2 DEG C/s, be incubated 30min, take out, put in agitator,
500 turns/min stirs 3min, obtains compound, is placed in baking oven, dries 90min for 80 DEG C, takes out, pulverize and get final product.
Method the most according to claim 2, it is characterised in that
The condition that described micro-filtration membrane once filters, secondary filter and three times are filtered is: micro-filtration membrane is inorganic ceramic film, retains
Molecular weight is 10000Da, and microfiltration temperature is 40 DEG C；The condition of described ultrafiltration membrance filter is: ultrafilter membrane molecular cut off is
200Da, ultrafiltrate temperature is 40 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610655172.1A CN106278919B (en) | 2016-08-11 | 2016-08-11 | A kind of method for preparing L isoleucines |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610655172.1A CN106278919B (en) | 2016-08-11 | 2016-08-11 | A kind of method for preparing L isoleucines |
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| CN106278919A true CN106278919A (en) | 2017-01-04 |
| CN106278919B CN106278919B (en) | 2018-01-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610655172.1A Active CN106278919B (en) | 2016-08-11 | 2016-08-11 | A kind of method for preparing L isoleucines |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108926875A (en) * | 2018-05-25 | 2018-12-04 | 湖北省联投生物科技股份有限公司 | A kind of quick sinking cooling device of tyrosine processing |
| WO2024191247A1 (en) * | 2023-03-14 | 2024-09-19 | 씨제이제일제당 (주) | Amino acid production method having improved filtration flow rate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654413A (en) * | 2009-09-17 | 2010-02-24 | 山东阜丰生物科技开发有限公司 | Method for extracting and separating L-isoleucine employing three-stage film cascade |
| CN102040531A (en) * | 2010-11-23 | 2011-05-04 | 五洲明珠股份有限公司 | Method for extracting L-isoleucine |
| CN102505027A (en) * | 2011-12-27 | 2012-06-20 | 开原市天慕生物科技有限公司 | Isoleucine fermenting process |
-
2016
- 2016-08-11 CN CN201610655172.1A patent/CN106278919B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654413A (en) * | 2009-09-17 | 2010-02-24 | 山东阜丰生物科技开发有限公司 | Method for extracting and separating L-isoleucine employing three-stage film cascade |
| CN102040531A (en) * | 2010-11-23 | 2011-05-04 | 五洲明珠股份有限公司 | Method for extracting L-isoleucine |
| CN102505027A (en) * | 2011-12-27 | 2012-06-20 | 开原市天慕生物科技有限公司 | Isoleucine fermenting process |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108926875A (en) * | 2018-05-25 | 2018-12-04 | 湖北省联投生物科技股份有限公司 | A kind of quick sinking cooling device of tyrosine processing |
| WO2024191247A1 (en) * | 2023-03-14 | 2024-09-19 | 씨제이제일제당 (주) | Amino acid production method having improved filtration flow rate |
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| CN106278919B (en) | 2018-01-16 |
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Denomination of invention: A method for preparing L-isoleucine Effective date of registration: 20211018 Granted publication date: 20180116 Pledgee: China Construction Bank Corporation Junan sub branch Pledgor: SHANDONG FUFENG FERMENTATION Co.,Ltd. Registration number: Y2021370000120 |
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Date of cancellation: 20230414 Granted publication date: 20180116 Pledgee: China Construction Bank Corporation Junan sub branch Pledgor: SHANDONG FUFENG FERMENTATION CO.,LTD. Registration number: Y2021370000120 |
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