CN106995398A - L proline novel technology for extracting - Google Patents
L proline novel technology for extracting Download PDFInfo
- Publication number
- CN106995398A CN106995398A CN201710377903.5A CN201710377903A CN106995398A CN 106995398 A CN106995398 A CN 106995398A CN 201710377903 A CN201710377903 A CN 201710377903A CN 106995398 A CN106995398 A CN 106995398A
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- China
- Prior art keywords
- proline
- liquid
- cleaner liquid
- ion exchange
- novel technology
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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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
The present invention relates to a kind of chemical process, i.e., a kind of L proline novel technology for extracting obtains cleaner liquid there is provided a kind of L proline novel technology for extracting, including zymotic fluid by ceramic membrane filter, is characterized in：The cleaner liquid carries out decolorization, then by being not more than ion exchange twice, obtains finished product.Its advantage is：Soda acid consumption and displacement are reduced, energy-conservation, consumption reduction, emission reduction, cost are greatly reduced, and finished product yield is high, and quality is good.
Description
Technical field
The present invention relates to a kind of chemical process, i.e., a kind of L-PROLINE novel technology for extracting.
Background technology
L-PROLINE (Pro) molecular formula：C5H9NO2, molal weight：115.13g/mol, be phytoprotein component it
One, it is possible to which free state is widely present in plant.In terms of being widely used in experiment reagent, medicine, cold resistant plant breeding,
Tooth enamel reparation etc..At present, L-PROLINE production generally uses microbe fermentation method, and its extraction process is zymotic fluid through ceramics
After membrane filtration, cleaner liquid is carried out continuously three step ion exchanges.Ion exchange needs a large amount of soda acids to make resin regeneration, also with a large amount of
Clear water rinse, increase environmental pressure, increase loss part proline among cost of sewage disposal, waste water.Because material is miscellaneous
Matter is more, and the product printing opacity value after ion exchange is relatively low, influences product quality.
The content of the invention
It is an object of the invention to provide a kind of soda acid consumption is small, few with water, ambient influnence is small, and product yield is high, and quality is good
L-PROLINE novel technology for extracting.
Above-mentioned purpose is realized by following technical scheme：A kind of L-PROLINE novel technology for extracting, including zymotic fluid are provided
Cleaner liquid is obtained by ceramic membrane filter, is characterized in：The cleaner liquid carries out decolorization, then through being not more than twice from
Son is exchanged, and obtains finished product.
The decolorization is using one of activated carbon, diatomite, PVPP, aluminium polychloride, Sodium Polyacrylate.
The new technology comprises the following steps：
1st, zymotic fluid is through ceramic membrane filter, 55-65 DEG C of membrane filtration temperature, pressure 2.0-4.0MPa.Generate cleaner liquid and cut
Liquid is stayed, thalline enters composite fertilizer's system with trapped fluid；Proline enters next procedure with cleaner liquid.
2nd, cleaner liquid is through activated carbon decolorizing, printing opacity value >=60%；Again through cation and anion exchange, ammonium sulfate etc. is removed inorganic miscellaneous
Matter, obtains the pure proline solution of comparison；Zwitterion resin makes regeneration treatment, wherein acid solution pH=of acid solution, alkali lye respectively
1.0,25-30 DEG C of temperature；Alkali lye pH=14.0,25-30 DEG C of temperature, is rinsed after processing with clear water, can be continued cycling through and be used；Processing
Acid solution after resin contains ammonium sulfate, extracts ammonium sulfate into composite fertilizer's system, alkali lye and wash water enter sewage disposal system.
3rd, the proline solution after resin treatment is concentrated by evaporation 50-70 DEG C of temperature through being concentrated by evaporation, and concentrates liquid hold-up
48-52%；2.5% activated carbon decolorizing 30min is added, by plate-frame filtering, proline decolouring cleaner liquid, sheet frame pressure is isolated
0.1-0.3MPa, plate-frame filtering liquid is further concentrated into single-action, crystallizes, is evaporated, then uses 95% ethanol, is cooled to 10
DEG C, isolate part proline wet product and a mother liquor.
4th, a mother liquor is back to single-action processing same with proline decolouring cleaner liquid and obtains proline wet product and secondary mother
Liquid, secondary mother liquid is back to that second step ion exchange is same with first step ion exchange collection liquid to be handled.
5th, proline wet product is put into double conic rotary vacuum dryer maintains 65 DEG C of drying to obtain proline finished product.
The separation of plate-frame filtering centrifuge or slide plate sedimentation separation or belt separation are substituted.
The beneficial effects of the invention are as follows：Once above ion exchange process is reduced, soda acid consumption and displacement is greatly reduced,
Energy-conservation, emission reduction, consumption reduction, cost are significantly reduced, and finished product yield is high, and quality is good.
Brief description of the drawings
Fig. 1 is a kind of process chart of embodiment；
Fig. 2 is the process chart of prior art.
Embodiment
The first embodiment：Fig. 1 describes visible following processing step in a kind of new technology, figure：
1st, zymotic fluid is through ceramic membrane filter, 55-65 DEG C of membrane filtration temperature, pressure 2.0-4.0MPa.Generate cleaner liquid and cut
Liquid is stayed, thalline enters composite fertilizer's system with trapped fluid；Proline enters next procedure with cleaner liquid, so as to be separated with thalline.
2nd, cleaner liquid is through activated carbon decolorizing, activated carbon decolorizing cleaner liquid printing opacity value >=60%；Again through cation and anion exchange, go
The inorganic impurities such as sulfuric acid ammonium, obtain the pure proline solution of comparison；Zwitterion resin is made at regeneration of acid solution, alkali lye respectively
Reason, then rinsed with clear water, used with continuing cycling through；Acid solution after processing resin contains ammonium sulfate, is extracted into composite fertilizer's system
Ammonium sulfate；Alkali lye and wash water enter sewage disposal system.Acid solution pH=1.0 in processing procedure, 25-30 DEG C of temperature；Alkali lye pH
=14.0,25-30 DEG C of temperature.
3rd, the proline solution after resin treatment is concentrated by evaporation 50-70 DEG C of temperature through being concentrated by evaporation, and concentrates liquid hold-up
50% or so；2.5% activated carbon decolorizing 30min is added, by plate-frame filtering, proline decolouring cleaner liquid, sheet frame pressure is isolated
Power 0.1-0.3MPa.Plate-frame filtering liquid is further concentrated into single-action, crystallizes, is evaporated, then uses 95%7 alcohol, is cooled to 10
DEG C, isolate part proline wet product and a mother liquor.
4th, a mother liquor is back to single-action processing same with proline decolouring cleaner liquid and obtains proline wet product and secondary mother
Liquid, secondary mother liquid is back to that second step ion exchange is same with first step ion exchange collection liquid to be handled.
5th, proline wet product is put into double conic rotary vacuum dryer maintains 65 DEG C of drying to obtain proline finished product.
In order to illustrate the superiority of above-mentioned technique, one kind is introduced than more typical existing process in conjunction with Fig. 2.The technique is walked
It is rapid as follows：
1st, zymotic fluid is through ceramic membrane filter, generation cleaner liquid and trapped fluid, and thalline enters composite fertilizer's system with trapped fluid；Dried meat
Propylhomoserin enters next procedure with cleaner liquid, so as to be separated with thalline.
2nd, cleaner liquid is exchanged through three secondary ions, is removed the inorganic impurities such as ammonium sulfate, is obtained the pure proline solution of comparison；Will
Seek first step ion exchange collection liquid printing opacity value >=40%；Zwitterion resin does regeneration treatment with acid solution, alkali lye respectively, then uses
Clear water is rinsed, and can be continued cycling through and be used；Acid solution after processing resin contains ammonium sulfate, and ammonium sulfate is extracted into composite fertilizer's system；
Alkali lye and wash water enter sewage disposal system.
3rd, the proline solution after resin treatment is concentrated by evaporation 50-70 DEG C of temperature through being concentrated by evaporation, and concentrates liquid hold-up
50% or so；2.5% activated carbon decolorizing 30min is added, by plate-frame filtering, proline decolouring cleaner liquid, sheet frame pressure is isolated
Power 0.1-0.3MPa.Plate-frame filtering liquid is further concentrated into single-action, crystallizes, is evaporated, then uses 95% ethanol, is cooled to 10
DEG C, isolate part proline wet product and a mother liquor.
4th, a mother liquor is back to single-action processing same with proline decolouring cleaner liquid and obtains proline wet product and secondary mother
Liquid, secondary mother liquid is back to that the 3rd step ion exchange is same with first step ion exchange collection liquid to be handled.
5th, proline wet product is put into double conic rotary vacuum dryer maintains 65 DEG C of drying to obtain proline finished product.
Obviously, the existing proline extraction processes of L mono- have the following disadvantages：
1st, soda acid consumption is big, and taking and discharging amount is big, and environmental protection pressure is big
Because using three step ion exchange techniques, it is necessary to substantial amounts of acid, alkali to resin regeneration, also rushed with substantial amounts of clear water
Wash.Particularly first step ion exchange, which often produces 1 ton of proline, needs sulfuric acid 1.7t, alkali lye 1.2t, water 40m3.Discharge density wastewater
16m3, dilute waste water 11m3, high-sulfate waste water 13m3, except containing ammonium sulfate in high-sulfate waste water, there is recycling to be worth
Outside, density wastewater and dilute waste water can only go organic fertilizer slurry-spraying pelletizing and sewage disposal system all without recovery value, and sewage disposal is difficult
Degree is very big.
2nd, yield is low, wastes serious
Also contain a small amount of dried meat ammonia in a certain amount of proline of first step ion exchange regenerant process losses, efflux wastewater
Acid, content 0.5% or so.These proline all Qu Liao composite fertilizers systems, are lost in vain, cause to waste.Because these waste existing
The presence of elephant, first step ion exchange yield only has 90%, and yield is low.
3rd, first step ion exchange collection liquid printing opacity value is unstable
When the first step ion exchange of traditional handicraft just starts to collect material, feed liquid printing opacity value is 90% or so, reaches and collects
During terminal, feed liquid printing opacity is 40%, and pigment impurity content difference is big, influences larger to second step ion exchange.
New technology substitutes first step ion exchange using activated carbon decolorizing, with obvious advantage：
1st, soda acid consumption, taking and discharging amount are reduced.New technology is by removing first step ion exchange, it is no longer necessary to regenerate first
Walk ion exchange resin and expend soda acid and taking and discharging.
2nd, energy-conservation, consumption reduction, emission reduction.Traditional handicraft uses three step ion exchanges, and the waste water of generation is by after sewage disposal
Discharge.And new technology removal first step ion exchange, only two-step solution, reduce energy consumption, soda acid consumption, taking and discharging
Amount, is consistent with national relevant policies, and the yield of activated carbon decolorizing is 99.7%, far above the receipts of first step ion exchange 90%
Rate.
3rd, second step ion exchange upper prop liquid steady quality.Cleaner liquid printing opacity value after activated carbon decolorizing is >=60%, surely
The qualitative quality better than first step ion exchange collection liquid.
Second of embodiment：The plate-frame filtering mode of this technique has a variety of alternative solutions, is such as separated with centrifuge, slide plate
Sedimentation separation, belt separation etc. also can reach same effect.
The third embodiment：The decoloring material activated carbon of this technique also has a variety of alternative materials, such as：It is PVPP, diatomite, poly-
Aluminium chloride, Sodium Polyacrylate etc. are closed, satisfied effect can be obtained.It is expected therefore further reduces cost.This technique is adopted
Plate and frame separation can also with or centrifuge separation or slide plate sedimentation separation or belt separation substitute.
Claims (4)
1. a kind of L-PROLINE novel technology for extracting, including zymotic fluid obtain cleaner liquid by ceramic membrane filter, it is characterised in that：Institute
State cleaner liquid and carry out decolorization, then by being not more than ion exchange twice, obtain finished product.
2. L-PROLINE novel technology for extracting according to claim 1, it is characterised in that：The decolorization is using activity
One of charcoal, diatomite, PVPP, aluminium polychloride, Sodium Polyacrylate.
3. L-PROLINE novel technology for extracting according to claim 1, it is characterised in that：The new technology includes following step
Suddenly：
(1) zymotic fluid is through ceramic membrane filter, 55-65 DEG C of membrane filtration temperature, pressure 2.0-4.0MPa.Generate cleaner liquid and retention
Liquid, thalline enters composite fertilizer's system with trapped fluid；Proline enters next procedure with cleaner liquid.
(2) cleaner liquid is through activated carbon decolorizing, printing opacity value >=60%；Again through cation and anion exchange, the inorganic impurities such as ammonium sulfate are removed,
Obtain the pure proline solution of comparison；Zwitterion resin makes regeneration treatment, wherein acid solution pH=1.0 of acid solution, alkali lye respectively,
25-30 DEG C of temperature；Alkali lye pH=14.0,25-30 DEG C of temperature, the resin after soda acid processing is rinsed with clear water, you can continued cycling through
Use；Acid solution after processing resin contains ammonium sulfate, and ammonium sulfate is extracted into composite fertilizer's system, and alkali lye and wash water enter at sewage
Reason system.
(3) the proline solution after resin treatment is concentrated by evaporation 50-70 DEG C of temperature, concentration liquid hold-up 48- through being concentrated by evaporation
52%；2.5% activated carbon decolorizing 30min is added, by plate-frame filtering, proline decolouring cleaner liquid, sheet frame pressure is isolated
0.1-0.3MPa, plate-frame filtering liquid is further concentrated into single-action, crystallizes, is evaporated, then uses 95% ethanol, is cooled to 10
DEG C, isolate part proline wet product and a mother liquor.
(4) mother liquors are back to single-action processing same with proline decolouring cleaner liquid and obtain proline wet product and secondary mother liquid,
Secondary mother liquid is back to that second step ion exchange is same with first step ion exchange collection liquid to be handled.
(5) proline wet product is put into double conic rotary vacuum dryer maintains 65 DEG C of drying to obtain proline finished product.
4. L-PROLINE novel technology for extracting according to claim 3, it is characterised in that：Plate-frame filtering centrifuge point
From or slide plate sedimentation separation or belt separation substitute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710377903.5A CN106995398A (en) | 2017-05-10 | 2017-05-10 | L proline novel technology for extracting |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710377903.5A CN106995398A (en) | 2017-05-10 | 2017-05-10 | L proline novel technology for extracting |
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| CN106995398A true CN106995398A (en) | 2017-08-01 |
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ID=59436072
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| CN201710377903.5A Pending CN106995398A (en) | 2017-05-10 | 2017-05-10 | L proline novel technology for extracting |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640865A (en) * | 2018-07-02 | 2018-10-12 | 无锡晶海氨基酸股份有限公司 | A kind of preparation method of medicinal proline |
| CN108658827A (en) * | 2018-07-02 | 2018-10-16 | 无锡晶海氨基酸股份有限公司 | A kind of preparation method of proline crude product |
| CN108707084A (en) * | 2018-07-02 | 2018-10-26 | 无锡晶海氨基酸股份有限公司 | A kind of preparation method of pharmaceutical grade Serine |
| CN112608266A (en) * | 2020-12-30 | 2021-04-06 | 南通紫琅生物医药科技有限公司 | Preparation method of L-proline |
| CN114085160A (en) * | 2021-10-30 | 2022-02-25 | 新泰市佳禾生物科技有限公司 | Method for separating and purifying L-serine from fermentation liquor |
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| CN102675180A (en) * | 2012-05-31 | 2012-09-19 | 精晶药业有限公司 | Method for extracting proline |
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| 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 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640865A (en) * | 2018-07-02 | 2018-10-12 | 无锡晶海氨基酸股份有限公司 | A kind of preparation method of medicinal proline |
| CN108658827A (en) * | 2018-07-02 | 2018-10-16 | 无锡晶海氨基酸股份有限公司 | A kind of preparation method of proline crude product |
| CN108707084A (en) * | 2018-07-02 | 2018-10-26 | 无锡晶海氨基酸股份有限公司 | A kind of preparation method of pharmaceutical grade Serine |
| CN112608266A (en) * | 2020-12-30 | 2021-04-06 | 南通紫琅生物医药科技有限公司 | Preparation method of L-proline |
| CN114085160A (en) * | 2021-10-30 | 2022-02-25 | 新泰市佳禾生物科技有限公司 | Method for separating and purifying L-serine from fermentation liquor |
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Application publication date: 20170801 |