CN107868011A - A kind of glycine production technology - Google Patents
A kind of glycine production technology Download PDFInfo
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- CN107868011A CN107868011A CN201610852146.8A CN201610852146A CN107868011A CN 107868011 A CN107868011 A CN 107868011A CN 201610852146 A CN201610852146 A CN 201610852146A CN 107868011 A CN107868011 A CN 107868011A
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- glycine
- solution
- ammonium chloride
- ceramic membrane
- production technology
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
-
- 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
- C07C227/04—Formation of amino groups in compounds containing carboxyl groups
- C07C227/06—Formation of amino groups in compounds containing carboxyl groups by addition or substitution reactions, without increasing the number of carbon atoms in the carbon skeleton of the acid
- C07C227/08—Formation of amino groups in compounds containing carboxyl groups by addition or substitution reactions, without increasing the number of carbon atoms in the carbon skeleton of the acid by reaction of ammonia or amines with acids containing functional groups
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of glycine production technology, by using Chloroacetic Aminolysis production the glycine crude product containing glycine and inorganic salts be configured to mixed solution with deionized water dissolving, by ceramic membrane separation, continuous chromatography separate, concentration, crystallization, centrifugation, crystal it is dry Glycine crystals and ammonia chloride crystal.Using above-mentioned technical proposal, glycine production technology of the present invention, by using ceramic membrane separation and continuous chromatography piece-rate system, the production of glycine is carried out, is had the advantage that as target product glycine, ammonium chloride product purity is high, yield is big and energy consumption is low.
Description
Technical field
The present invention relates to glycine field, more particularly to a kind of glycine production technology.
Background technology
Glycine (Gly) also known as amion acetic acid, it is that structure is the simplest in amino acid series, a kind of nonessential ammonia of human body
Base acid, has acid and basic functionality, is in aqueous strong electrolyte, is dissolved in intensive polar solvent simultaneously in the molecule
Spend larger, be substantially insoluble in non-polar solven, and there is higher boiling point and fusing point, can by the regulation of aqueous solution acid-base property
So that different molecular conformations is presented in glycine.The glycine of wherein technical grade is mainly used as pesticides, is herbicide glyphosate
Primary raw material.At present, the technology path of industrialized production glycine mainly has Chloroacetic Aminolysis, applies special rake method
(cstercker methods), hydrogen cyanogen method synthesize glycine and biological synthesis process etc., wherein the country is mainly with the monoxone ammonia of traditional handicraft
Based on solution.The traditional handicraft is to be closed in alcohol phase with methenamine, monoxone, ammoniacal liquor (ammonia or liquefied ammonia) for raw material
Into.The advantages of Chloroacetic Aminolysis is that raw material is easy to get, and synthesis technique is simple, not high to equipment requirement, easy to operate, substantially without public affairs
Evil；Shortcoming is that the reaction time is longer, and by-product ammonium chloride inorganic salts material is difficult to remove, poor product quality, refines cost height,
Meanwhile the technique produces the largely waste water rich in inorganic salts (ammonium chloride) and formaldehyde, required environmental protection treatment is costly, and
And be difficult to recycle as the methenamine of catalyst, the significant wastage of raw material is caused, increases production cost.
The Chinese invention patent application in Application No. 201210331472.6 such as Zhao Jingwei, Xie Baiming《A kind of glycine
Process for cleanly preparing》In disclose a kind of process for cleanly preparing of glycine, it is produced based on Chloroacetic Aminolysis
Glycine and the mixed solution of ammonium chloride be raw material, using electrodialytic method separation of glycine and ammonium chloride.It is with tradition
Based on Chloroacetic Aminolysis, using the cleaning preparation technology of electrodialytic technique progress, compared with traditional handicraft, have quality good
The advantages that, but its shortcoming is exactly that purity is low, disposable yield is low, and energy consumption is very high.
The content of the invention
It is an object of the invention to provide the glycine production technology that a kind of purity is high, high income and energy consumption are low.
To reach above-mentioned purpose, technical scheme proposed by the invention is：A kind of glycine production technology, its feature exist
In comprising the following steps：
Step 1：By using the glycine crude product deionization containing glycine and inorganic salts of Chloroacetic Aminolysis production
Water dissolving is configured to the mixed solution that mass concentration is 20-30%；
Step 2：Use pore size filter that it is saturating to obtain ceramic membrane for the ceramic membrane filter of 50-200 nanometers above-mentioned mixed solution
Analyse liquid；
Step 3：Ceramic membrane dialyzate uses the continuous chromatography piece-rate system filled with monium resin or calcium type resin to enter
Row separation, obtains glycine solution and ammonium chloride solution；
Step 4：Glycine solution and ammonium chloride solution are carried out respectively to be concentrated to give glycine concentrate and ammonium chloride concentration
Liquid；
Step 5：By glycine concentrate and ammonium chloride concentrate respectively by crystallizing, centrifuging, crystal it is dry glycine
Crystal and ammonia chloride crystal；
In above-mentioned steps, the pH value by the solution in aqueous ammonia conditions rate-determining steps 1-3 is 5.5-7.
Further, the mass fraction of glycine is 54%-59% in described glycine crude product, the mass fraction of ammonium chloride
For 40%-45%.
Further, the concentration described in step 4 is that four-effect evaporator concentrates or mechanical vapor recompression technology (MVR) concentrates.
Further, described Glycine crystals purity is more than 99.5%, reaches the Glycine Levels of feed grade.Enter one
Step, the purity of described ammonia chloride crystal is more than 99%, can be as the raw material of fertilizer.
Using above-mentioned technical proposal, glycine production technology of the present invention, by using ceramic membrane separation and continuously
Chromatographic fractionation system, the production of glycine is carried out, had the advantage that as target product glycine, ammonium chloride product purity
Height, yield is big and energy consumption is low.
Embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
Step 1：The glycine crude product 20kg containing glycine and inorganic salts using Chloroacetic Aminolysis production is spent
Ionized water dissolving is configured to mixed solution 100kg, and its mass concentration is 20%；And in glycine crude product glycine mass fraction
For 54%, the mass fraction of ammonium chloride is 45%, and remaining is impurity；It is that glycine is molten by ammoniacal liquor adjustment control mixed solution pH
The pH value of liquid is 5.5-7；
Step 2：Pore size filter is used to obtain ceramic membrane dialysis for 50 nanometers of ceramic membrane filter above-mentioned mixed solution
Liquid；By the pH value that ammoniacal liquor adjustment control mixed solution pH is glycine solution it is 5.5-7 during ceramic membrane filter；
Step 3：Ceramic membrane dialyzate uses the continuous chromatography piece-rate system filled with monium resin to be separated, and obtains sweet ammonia
Acid solution and ammonium chloride solution；Wherein the separation purity of glycine is more than 99%, concentration more than 5%, and the separation of ammonium chloride is pure
Spend for more than 95%, concentration is more than 4%, by ammoniacal liquor adjustment control mixed solution pH is sweet ammonia in continuous chromatography separation process
The pH value of acid solution is 5.5-7；
Step 4：Glycine solution and ammonium chloride solution are respectively adopted into four-effect evaporator to carry out being concentrated to give glycine concentration
Liquid and ammonium chloride concentrate；Again by glycine concentrate and ammonium chloride concentrate respectively by crystallizing, centrifuging, crystal it is purely dry
Spend for more than the 99.5% Glycine crystals 10.5kg for reaching feed grade；It is more than 99% with purity, Fertilizer application can be used as
Ammonia chloride crystal 8.9kg；
In above-mentioned steps, pass through the pH value of the glycine solution in the solution and step 4 in aqueous ammonia conditions rate-determining steps 1-3
For 5.5-7.
Embodiment 2
Step 1：The glycine crude product 50kg containing glycine and inorganic salts using Chloroacetic Aminolysis production is spent
Ionized water dissolving is configured to mixed solution 100kg, and its mass concentration is 50%；And in glycine crude product glycine mass fraction
For 59%, the mass fraction of ammonium chloride is 40%, and remaining is impurity；It is that glycine is molten by ammoniacal liquor adjustment control mixed solution pH
The pH value of liquid is 5.5-7；
Step 2：Pore size filter is used to obtain ceramic membrane dialysis for 100 nanometers of ceramic membrane filter above-mentioned mixed solution
Liquid；By the pH value that ammoniacal liquor adjustment control mixed solution pH is glycine solution it is 5.5-7 during ceramic membrane filter；
Step 3：Ceramic membrane dialyzate uses the continuous chromatography piece-rate system filled with calcium type resin to be separated, and obtains sweet ammonia
Acid solution and ammonium chloride solution；Wherein the separation purity of glycine is more than 99%, concentration more than 15%, and the separation of ammonium chloride is pure
Spend for more than 95%, concentration is more than 14%, by ammoniacal liquor adjustment control mixed solution pH is sweet in continuous chromatography separation process
The pH value of propylhomoserin solution is 5.5-7；
Step 4：Glycine solution and ammonium chloride solution are respectively adopted into four-effect evaporator to carry out being concentrated to give glycine concentration
Liquid and ammonium chloride concentrate；Again by glycine concentrate and ammonium chloride concentrate respectively by crystallizing, centrifuging, crystal it is purely dry
Spend for more than the 99.5% Glycine crystals 28.5kg for reaching feed grade；It is more than 99% with purity, Fertilizer application can be used as
Ammonia chloride crystal 19.8kg；
Embodiment 3
Step 1：The glycine crude product 30kg containing glycine and inorganic salts using Chloroacetic Aminolysis production is spent
Ionized water dissolving is configured to mixed solution 100kg, and its mass concentration is 30%；And in glycine crude product glycine mass fraction
For 50%, the mass fraction of ammonium chloride is 48%, and remaining is impurity；It is that glycine is molten by ammoniacal liquor adjustment control mixed solution pH
The pH value of liquid is 5.5-7；
Step 2：Pore size filter is used to obtain ceramic membrane dialysis for 200 nanometers of ceramic membrane filter above-mentioned mixed solution
Liquid；By the pH value that ammoniacal liquor adjustment control mixed solution pH is glycine solution it is 5.5-7 during ceramic membrane filter；
Step 3：Ceramic membrane dialyzate uses the continuous chromatography piece-rate system filled with monium resin to be separated, and obtains sweet ammonia
Acid solution and ammonium chloride solution；Wherein the separation purity of glycine is more than 99%, concentration more than 9%, and the separation of ammonium chloride is pure
Spend for more than 95%, concentration is more than 7%, by ammoniacal liquor adjustment control mixed solution pH is sweet ammonia in continuous chromatography separation process
The pH value of acid solution is 5.5-7；
Step 4：Glycine solution and ammonium chloride solution are respectively adopted into four-effect evaporator to carry out being concentrated to give glycine concentration
Liquid and ammonium chloride concentrate；Again by glycine concentrate and ammonium chloride concentrate respectively by crystallizing, centrifuging, crystal it is purely dry
Spend for more than the 99.5% Glycine crystals 14.8kg for reaching feed grade；It is more than 99% with purity, Fertilizer application can be used as
Ammonia chloride crystal 13.7kg.
In the above-described embodiments, exemplary description has only been carried out to the present invention, but those skilled in the art are reading this
Various modifications can be carried out to the present invention without departing from the spirit and scope of the present invention after patent application.
Claims (3)
1. a kind of glycine production technology, it is characterised in that comprise the following steps：
Step 1：Will be molten using the glycine crude product deionized water containing glycine and inorganic salts of Chloroacetic Aminolysis production
Solution is configured to the mixed solution that mass concentration is 20-50%；
Step 2：Above-mentioned mixed solution is used into pore size filter as the ceramic membrane filter of 50-200 nanometers, obtains ceramic membrane dialysis
Liquid；
Step 3：Ceramic membrane dialyzate uses the continuous chromatography piece-rate system filled with monium resin or calcium type resin to be separated,
Obtain glycine solution and ammonium chloride solution；
Step 4：Glycine solution and ammonium chloride solution are carried out respectively to be concentrated to give glycine concentrate and ammonium chloride concentrate；
Step 5：By glycine concentrate and ammonium chloride concentrate respectively by crystallizing, centrifuging, crystal it is dry Glycine crystals
And ammonia chloride crystal；
In above-mentioned steps, the pH value by the solution in aqueous ammonia conditions rate-determining steps 1-3 is 5.5-7.
A kind of 2. glycine production technology according to claim 1, it is characterised in that sweet ammonia in described glycine crude product
The mass fraction of acid is 54%-59%, and the mass fraction of ammonium chloride is 40%-45%.
3. a kind of glycine production technology according to claim 1, it is characterised in that the concentration described in step 4 is quadruple effect
Evaporator concentrates.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610852146.8A CN107868011A (en) | 2016-09-26 | 2016-09-26 | A kind of glycine production technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610852146.8A CN107868011A (en) | 2016-09-26 | 2016-09-26 | A kind of glycine production technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107868011A true CN107868011A (en) | 2018-04-03 |
Family
ID=61752002
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610852146.8A Pending CN107868011A (en) | 2016-09-26 | 2016-09-26 | A kind of glycine production technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107868011A (en) |
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2016
- 2016-09-26 CN CN201610852146.8A patent/CN107868011A/en active Pending
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180403 |
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| WD01 | Invention patent application deemed withdrawn after publication |