CN106336370B - A kind of extraction and purification process of proline - Google Patents
A kind of extraction and purification process of proline Download PDFInfo
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- CN106336370B CN106336370B CN201610655336.0A CN201610655336A CN106336370B CN 106336370 B CN106336370 B CN 106336370B CN 201610655336 A CN201610655336 A CN 201610655336A CN 106336370 B CN106336370 B CN 106336370B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/04—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members
- C07D207/10—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/16—Carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
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- Organic Chemistry (AREA)
- Pyrrole Compounds (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention belongs to amino acid technical field of purification, disclose a kind of extraction and purification process of proline comprising following steps：Step 1）Prepare flocculant, step 2）Flocculation purification and filtering, step 3）Ultrafiltration, flocculation and micro-filtration, step 4）Decrease temperature crystalline.The present invention substantially increases the purity of proline by filtering, flocculation and crystallization.
Description
Technical field
The invention belongs to amino acid technical field of purification, and in particular to a kind of extraction and purification process of proline.
Background technology
Proline（proline；Pro）Chemical name be 2-pyrrolidone-5-carboxylic acid, it is a kind of cricoid imino acid.Dried meat
Propylhomoserin is the nonessential amino acid of human body.Proline is the base unit for constituting protein, is form human body protein 21 kinds
One of amino acid, for amino acid other than dried meat amino acid is imino acid, other amino acid are alpha amino acid.Proline purposes is wide
It is general, it can be used for amino acid injection, compound amino acid infusion, food additives, nutritional supplement liquid etc.；For Biochemical Research, doctor
For malnutrition, the supplement etc. of hypoproteinosis, gastrointestinal disease, scald and postoperative protein on medicine；Nutritional supplement, wind
Taste agent, heat generation amino-carbonyl reacts altogether with sugar, produces special fragrance matter.It is available by China GB 2760-86 regulations
Make fragrance；Branchamin.For one of big infusion raw material of amino acid, it is used for malnutritive, hypoproteinosis, sternly
The Protein intake of weight intestines and stomach illness, scald and surgical site infections；Medical material and food additives.
As amino acid industry gradually develops, microbe fermentation method becomes the most promising production technology of amino acids production,
In terms of proline production, microbe fermentation method also shows potential advantage, but in microbial fermentation solution extraction process, dried meat
It is not high that propylhomoserin shows as yield.Proline product level is different, and difference in selling prices is very big, and how to improve the purity of proline is us
The technical issues that need to address.
Invention content
In order to overcome the defects such as prior art proline extraction and purification process is cumbersome, purity is low, the present invention provides one kind
The extraction and purification process of proline.
The present invention is achieved by the following technical solution：
A kind of extraction and purification process of proline comprising following steps：Step 1）Prepare flocculant, step 2）Flocculation removes
Miscellaneous and filtering, step 3）Ultrafiltration, flocculation and micro-filtration, step 4）Decrease temperature crystalline.
Specifically, the technique includes the following steps：
Step 1）Prepare flocculant：
（1）Add the purified water for accounting for twice of mass of starch into starch, be uniformly mixing to obtain suspension, then addition and starch
Etc. quality sodium carboxymethylcellulose, 200 turns/min stir 30min, be subsequently placed in 80 DEG C and be dried to moisture 5%（Quality hundred
Divide ratio）Hereinafter, obtaining modified starch；
（2）According to 5:1:0.2 mass ratio takes chitosan, sodium humate and pectin, is mixed evenly, and then adds
The sodium hydrate aqueous solution of the 2M of twice of mass of chitosan, the ultrasonic 10min of 30KHz are accounted for, last 500 turns/min stirs 3min,
Obtain modification of chitosan；
（3）Corn stalk powder, sepiolite are crushed respectively and obtain corn stalk powder and sepiolite powder, by corn stalk powder, sea
Afrodite powder and diatomite are according to 3:1:1 mass ratio is mixed evenly, and is added to a concentration of 1M for accounting for 5 times of weight of diatomite
Sodium hydroxide solution in, 200 turns/min stirs 120min, then filters, dry, and it is 10-20 mesh powders to be ground into grain size；
（4）By modified starch, modification of chitosan and step（3）Gained powder is according to 5:3:2 mass ratio is mixed
Uniformly, it is subsequently placed in closed reactor, rises to 150 DEG C with the heating rate of 2 DEG C/s, keep the temperature 30min, take out, put into and stir
It mixes in device, 500 turns/min stirs 3min, obtains mixture, is placed in baking oven, and 80 DEG C of drying 90min take out, crush to obtain the final product；
Step 2）Flocculation purification and filtering：Proline crude product is dissolved in deionized water, 200 turns/min stirs 10min, so
Addition accounts for proline crude product 1% afterwards（w/w）Flocculant, continue to stir 3min with 500 turns/min, stand 30min, then use micro-filtration
Film once filters, and collects a filtered solution；
Step 3）Ultrafiltration, flocculation and micro-filtration：Ultrafiltration dialysis liquid is obtained by ultrafiltration membrance filter by filtered solution is dense, toward ultrafiltration
Addition accounts for proline crude product 0.5% in dialyzate（w/w）Flocculant, 500 turns/min stirs 2min, stands 30min, then with micro-
Filter membrane secondary filter collects secondary filtered solution；
Step 4）Decrease temperature crystalline：Secondary filtered solution is concentrated in vacuo to the one third of original volume, subsequently into crystallizing tank
Decrease temperature crystalline is carried out, cooling rate is 10 DEG C/h, is stirred in cooling, stops cooling when temperature is down to 10 DEG C, obtain wet
Crystal is collected by centrifugation in fine work, is subsequently placed in 50-60 DEG C and is dried in vacuo 2 hours, obtains proline product.
Preferably,
The microfiltration membranes once filter, the condition of secondary filter is：Microfiltration membranes are inorganic ceramic membrane, and molecular cut off is
10000Da, micro-filtration temperature are 40 DEG C.
The condition of the ultrafiltration membrance filter is：Ultrafiltration retaining molecular weight is 300Da, and ultrafiltrate temperature is 40 DEG C.
The advantageous effect that the present invention obtains includes mainly：
The present invention provides a kind of novel flocculant, is suitble to coarse amino acid purifying, avoids chemical substance, flocculation purification effect
It is good, it is of low cost, it is environment friendly and pollution-free；Flocculant of the present invention is using agricultural wastes and natural mineral matter as primary raw material, this original
Material derives from a wealth of sources and at low cost, and prepares porous material, and flocculation purification effect is good, realizes agricultural wastes recycling profit
With；Flocculant of the present invention is modified starch and chitosan so that aperture, adsorption capacity and specific surface area carry significantly
It is high；Using flocculant process twice in proline purifying crude technique, operating procedure is simplified, saves cost, and make
More preferably, the flocculant after use is also used as fertilizer preparation to purification effect, turns waste into wealth.
Specific implementation mode
The present invention will be further explained using specific embodiment, but be should not be construed as to this hair below
The limitation of bright initiative spirit.
Embodiment 1
A kind of extraction and purification process of proline comprising following steps：
Step 1）Prepare flocculant：
（1）Add the purified water for accounting for twice of mass of starch into starch, be uniformly mixing to obtain suspension, then addition and starch
Etc. quality sodium carboxymethylcellulose, 200 turns/min stir 30min, be subsequently placed in 80 DEG C and be dried to moisture 5%（Quality hundred
Divide ratio）Hereinafter, obtaining modified starch；
（2）According to 5:1:0.2 mass ratio takes chitosan, sodium humate and pectin, is mixed evenly, and then adds
The sodium hydrate aqueous solution of the 2M of twice of mass of chitosan, the ultrasonic 10min of 30KHz are accounted for, last 500 turns/min stirs 3min,
Obtain modification of chitosan；
（3）Corn stalk powder, sepiolite are crushed respectively and obtain corn stalk powder and sepiolite powder, by corn stalk powder, sea
Afrodite powder and diatomite are according to 3:1:1 mass ratio is mixed evenly, and is added to a concentration of 1M for accounting for 5 times of weight of diatomite
Sodium hydroxide solution in, 200 turns/min stirs 120min, then filters, dry, and it is 10-20 mesh powders to be ground into grain size；
（4）By modified starch, modification of chitosan and step（3）Gained powder is according to 5:3:2 mass ratio is mixed
Uniformly, it is subsequently placed in closed reactor, rises to 150 DEG C with the heating rate of 2 DEG C/s, keep the temperature 30min, take out, put into and stir
It mixes in device, 500 turns/min stirs 3min, obtains mixture, is placed in baking oven, and 80 DEG C of drying 90min take out, crush to obtain the final product.
Step 2）Flocculation purification and filtering：By proline crude product 1150g（Purity is 59.6%）It is dissolved in 1000ml deionized waters
In, 200 turns/min stirs 10min, and then addition accounts for proline crude product 1%（w/w）Flocculant, continue with 500 turns/min stir
3min stands 30min, then is once filtered with microfiltration membranes, collects a filtered solution；Filter condition of the microfiltration membranes is：It is micro-
Filter membrane is inorganic ceramic membrane, and molecular cut off 10000Da, micro-filtration temperature is 40 DEG C；
Step 3）Ultrafiltration, flocculation and micro-filtration：Ultrafiltration dialysis liquid is obtained by ultrafiltration membrance filter by filtered solution is dense, toward ultrafiltration
Addition accounts for proline crude product 0.5% in dialyzate（w/w）Flocculant, 500 turns/min stirrings, 2min stands 30min, then with micro-
Filter membrane secondary filter collects secondary filtered solution；
The condition of the ultrafiltration membrance filter is：Ultrafiltration retaining molecular weight is 300Da, and ultrafiltrate temperature is 40 DEG C；
The condition of the microfiltration membranes secondary filter is：Microfiltration membranes are inorganic ceramic membrane, molecular cut off 10000Da,
Micro-filtration temperature is 40 DEG C；
Step 4）Decrease temperature crystalline：Secondary filtered solution is concentrated in vacuo to the one third of original volume, subsequently into crystallizing tank
Decrease temperature crystalline is carried out, cooling rate is 10 DEG C/h, is stirred in cooling, stops cooling when temperature is down to 10 DEG C, obtain wet
Crystal is collected by centrifugation in fine work, is subsequently placed in 50-60 DEG C and is dried in vacuo 2 hours, obtains proline product 597g, detected through HPLC
Purity is 98.3%.
Finally, it should also be noted that it is listed above be only the present invention several specific embodiments.Obviously, this hair
Bright to be not limited to above example, acceptable there are many deformations.Those skilled in the art can be from present disclosure
All deformations for directly exporting or associating, are considered as protection scope of the present invention.
Claims (2)
1. a kind of extraction and purification process of proline, which is characterized in that the technique includes the following steps：
Step 1）Prepare flocculant：
（1）Add the purified water for accounting for twice of mass of starch into starch, be uniformly mixing to obtain suspension, is then added and the matter such as starch
The sodium carboxymethylcellulose of amount, 200 turns/min stir 30min, are subsequently placed in 80 DEG C and are dried to moisture 5% hereinafter, being changed
Property starch；
（2）According to 5:1:0.2 mass ratio takes chitosan, sodium humate and pectin, is mixed evenly, and then addition accounts for shell
The sodium hydrate aqueous solution of the 2M of twice of mass of glycan, the ultrasonic 10min of 30KHz, last 500 turns/min stir 3min, obtain
Modification of chitosan；
（3）Corn stalk powder, sepiolite are crushed respectively and obtain corn stalk powder and sepiolite powder, by corn stalk powder, sepiolite
Powder and diatomite are according to 3:1:1 mass ratio is mixed evenly, and is added to the hydrogen for a concentration of 1M for accounting for 5 times of weight of diatomite
In sodium hydroxide solution, 200 turns/min stirs 120min, then filters, dry, and it is 10-20 mesh powders to be ground into grain size；
（4）By modified starch, modification of chitosan and step（3）Gained powder is according to 5:3:2 mass ratio is mixed evenly,
It is subsequently placed in closed reactor, rises to 150 DEG C with the heating rate of 2 DEG C/s, keep the temperature 30min, take out, put into blender
In, 500 turns/min stirs 3min, obtains mixture, is placed in baking oven, and 80 DEG C of drying 90min take out, crush to obtain the final product；
Step 2）Flocculation purification and filtering：Proline crude product is dissolved in deionized water, 200 turns/min stirs 10min, then adds
It is mass ratio to add the flocculant for accounting for proline crude product 1%, the ratio, continues to stir 3min with 500 turns/min, stands 30min,
It is once filtered with microfiltration membranes again, collects a filtered solution；
Step 3）Ultrafiltration, flocculation and micro-filtration：Ultrafiltration dialysis liquid is obtained by ultrafiltration membrance filter by a filtered solution is dense, toward ultrafiltration
Add flocculant in dialyzate, 500 turns/min stirrings, 2min stands 30min, then with microfiltration membranes secondary filter, collects secondary filter
Cross liquid；
Step 4）Decrease temperature crystalline：Secondary filtered solution is concentrated in vacuo to the one third of original volume, is carried out subsequently into crystallizing tank
Decrease temperature crystalline, cooling rate are 10 DEG C/h, are stirred in cooling, stop cooling when temperature is down to 10 DEG C, obtain wet essence
Crystal is collected by centrifugation in product, is subsequently placed in 50-60 DEG C and is dried in vacuo 2 hours, obtains proline product.
2. technique according to claim 1, it is characterised in that：
The microfiltration membranes once filter, the condition of secondary filter is：Microfiltration membranes are inorganic ceramic membrane, and molecular cut off is
10000Da, micro-filtration temperature are 40 DEG C；The condition of the ultrafiltration membrance filter is：Ultrafiltration retaining molecular weight is 300Da, ultrafiltration temperature
Degree is 40 DEG C.
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| CN201610655336.0A CN106336370B (en) | 2016-08-11 | 2016-08-11 | A kind of extraction and purification process of proline |
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| CN201610655336.0A CN106336370B (en) | 2016-08-11 | 2016-08-11 | A kind of extraction and purification process of proline |
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| CN106336370A CN106336370A (en) | 2017-01-18 |
| CN106336370B true CN106336370B (en) | 2018-07-27 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101348453A (en) * | 2008-08-29 | 2009-01-21 | 广东肇庆星湖生物科技股份有限公司 | Method for purifying proline |
| CN101633634A (en) * | 2009-08-16 | 2010-01-27 | 山东阜丰生物科技开发有限公司 | Method for extracting L-proline from fermentation liquor by membrane separation technology |
| WO2010071129A1 (en) * | 2008-12-17 | 2010-06-24 | セントラル硝子株式会社 | Method for manufacturing hydroxyl group substitution product |
| CN103265467A (en) * | 2013-05-06 | 2013-08-28 | 华南理工大学 | Method for cooling, crystallizing and refining L-proline |
-
2016
- 2016-08-11 CN CN201610655336.0A patent/CN106336370B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101348453A (en) * | 2008-08-29 | 2009-01-21 | 广东肇庆星湖生物科技股份有限公司 | Method for purifying proline |
| WO2010071129A1 (en) * | 2008-12-17 | 2010-06-24 | セントラル硝子株式会社 | Method for manufacturing hydroxyl group substitution product |
| CN101633634A (en) * | 2009-08-16 | 2010-01-27 | 山东阜丰生物科技开发有限公司 | Method for extracting L-proline from fermentation liquor by membrane separation technology |
| CN103265467A (en) * | 2013-05-06 | 2013-08-28 | 华南理工大学 | Method for cooling, crystallizing and refining L-proline |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Extraction and purification process of proline Effective date of registration: 20211018 Granted publication date: 20180727 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: 20180727 Pledgee: China Construction Bank Corporation Junan sub branch Pledgor: SHANDONG FUFENG FERMENTATION CO.,LTD. Registration number: Y2021370000120 |
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