CN106699589A - Glycine production technology - Google Patents
Glycine production technology Download PDFInfo
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- CN106699589A CN106699589A CN201510785112.7A CN201510785112A CN106699589A CN 106699589 A CN106699589 A CN 106699589A CN 201510785112 A CN201510785112 A CN 201510785112A CN 106699589 A CN106699589 A CN 106699589A
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- Prior art keywords
- glycine
- ammonium chloride
- solution
- production technology
- ceramic membrane
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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
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a glycine production technology. The glycine production technology comprises steps as follows: a mixed solution is prepared from a crude glycine product which is produced with a chloroacetic acid aminolysis method and contains glycine and inorganic salt through dissolving with deionized water, the mixed solution is subjected to ceramic membrane separation, continuous chromatographic separation, concentration, crystallization, centrifugation and crystal drying, and glycine crystals and ammonium chloride crystals are obtained. With the adoption of the technical scheme of the glycine production technology, glycine production is performed by adopting ceramic membrane separation and continuous chromatographic separation systems, and the glycine production technology has the beneficial effects that the target products, namely, glycine and ammonium chloride, are high in product quality, high in yield and low in energy consumption.
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, are that structure is the simplest in amino acid series, a kind of nonessential ammonia of human body
Base acid, has acid and basic functionality simultaneously in the molecule, is in aqueous strong electrolyte, in intensive polar solvent
Solubility is larger, is substantially insoluble in non-polar solven, and with boiling point and fusing point higher, by aqueous solution acid-base property
Regulation can make glycine that different molecular conformations are presented.The glycine of wherein technical grade is mainly used as pesticides, is weeding
The primary raw material of agent glyphosate.At present, the technology path of industrialized production glycine mainly has Chloroacetic Aminolysis, Shi Te
Rake method (cstercker methods), hydrogen cyanogen method synthesis glycine and biological synthesis process etc., wherein domestic main with traditional handicraft
Based on Chloroacetic Aminolysis.The traditional handicraft is that with methenamine, monoxone, ammoniacal liquor, (ammonia or liquefied ammonia are equal in alcohol phase
Can) it is Material synthesis.The advantage of Chloroacetic Aminolysis is that raw material is easy to get, and synthesis technique is simple, not high to equipment requirement,
It is easy to operate, it is substantially nuisanceless;Have the disadvantage that the reaction time is more long, by-product ammonium chloride inorganic salts material is difficult to remove, produce
Quality is poor, refines high cost, meanwhile, the technique produces a large amount of waste water rich in inorganic salts (ammonium chloride) and formaldehyde,
Required environmental protection treatment is costly, and methenamine as catalyst is difficult to recycling use, causes raw material
Significant wastage, increase 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
The mixed solution of glycine and ammonium chloride be raw material, using electrodialytic method separation of glycine and ammonium chloride.It is with biography
Based on system Chloroacetic Aminolysis, the cleaning preparation technology carried out using electrodialytic technique compared with traditional handicraft, is had
The advantages of matter is measured, but its shortcoming is exactly, and 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 a kind of purity is high, high income and the low glycine production technology of energy consumption.
To reach above-mentioned purpose, technical scheme proposed by the invention is:A kind of glycine production technology, it is characterised in that
Comprise the following steps:
Step 1:By using the glycine crude product deionized water containing glycine and inorganic salts of Chloroacetic Aminolysis production
Dissolving is configured to the mixed solution that mass concentration is 20-30%;
Step 2:It is 50-200 nanometers of ceramic membrane filter that above-mentioned mixed solution is used into pore size filter, obtains ceramic membrane saturating
Analysis liquid;
Step 3:Ceramic membrane dialyzate is carried out using the continuous chromatography piece-rate system filled with monium resin or calcium type resin
Separate, 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 crystallization, centrifugation, 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, and the mass fraction of ammonium chloride is
40%-45%.
Further, the concentration described in step 4 is that four-effect evaporator is concentrated or mechanical vapor recompression technology (MVR) concentration.
Further, described Glycine crystals purity is more than 99.5%, reaches the Glycine Levels of feed grade.Further,
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 continuous color
Spectrum piece-rate system, carries out the production of glycine, has the advantage that to be target product glycine, ammonium chloride product purity
It is high, yield is big and energy consumption is low.
Specific embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
Step 1:Will using Chloroacetic Aminolysis production the glycine crude product 20kg containing glycine and inorganic salts spend from
Sub- water dissolves are configured to mixed solution 100kg, and its mass concentration is 20%;And the quality of glycine is divided in glycine crude product
Number is 54%, and the mass fraction of ammonium chloride is 45%, and remaining is impurity;Being adjusted by ammoniacal liquor controls the mixed solution pH to be
The pH value of glycine solution is 5.5-7;
Step 2:It is 50 nanometers of ceramic membrane filter that above-mentioned mixed solution is used into pore size filter, obtains ceramic membrane dialyzate;
The pH value for controlling mixed solution pH to be glycine solution is adjusted for 5.5-7 by ammoniacal liquor during ceramic membrane filter;
Step 3:Ceramic membrane dialyzate is separated using the continuous chromatography piece-rate system filled with monium resin, obtains sweet ammonia
Acid solution and ammonium chloride solution;Wherein the separation purity of glycine is more than 99%, concentration more than 5%, the separation of ammonium chloride
Purity is more than 95%, and concentration is more than 4%, and control mixed solution pH is adjusted by ammoniacal liquor in continuous chromatography separation process
For the pH value of glycine solution is 5.5-7;
Step 4:Glycine solution and ammonium chloride solution are respectively adopted into four-effect evaporator carries out being concentrated to give glycine concentrate
With ammonium chloride concentrate;It is again that glycine concentrate and ammonium chloride concentrate is dry by crystallization, centrifugation, crystal respectively
Purity is more than the 99.5% Glycine crystals 10.5kg for reaching feed grade;It is more than 99% with purity, can be as fertilizer
The ammonia chloride crystal 8.9kg for using;
In above-mentioned steps, by the pH value of the glycine solution in the solution and step 4 in aqueous ammonia conditions rate-determining steps 1-3
It is 5.5-7.
Embodiment 2
Step 1:Will using Chloroacetic Aminolysis production the glycine crude product 50kg containing glycine and inorganic salts spend from
Sub- water dissolves are configured to mixed solution 100kg, and its mass concentration is 50%;And the quality of glycine is divided in glycine crude product
Number is 59%, and the mass fraction of ammonium chloride is 40%, and remaining is impurity;Being adjusted by ammoniacal liquor controls the mixed solution pH to be
The pH value of glycine solution is 5.5-7;
Step 2:It is 100 nanometers of ceramic membrane filter that above-mentioned mixed solution is used into pore size filter, obtains ceramic membrane dialysis
Liquid;The pH value for controlling mixed solution pH to be glycine solution is adjusted for 5.5-7 by ammoniacal liquor during ceramic membrane filter;
Step 3:Ceramic membrane dialyzate is separated using the continuous chromatography piece-rate system filled with calcium type resin, obtains sweet ammonia
Acid solution and ammonium chloride solution;Wherein the separation purity of glycine be more than 99%, concentration more than 15%, ammonium chloride point
It is more than 95% from purity, concentration is more than 14%, control mixed solution is adjusted by ammoniacal liquor in continuous chromatography separation process
PH is 5.5-7 for the pH value of glycine solution;
Step 4:Glycine solution and ammonium chloride solution are respectively adopted into four-effect evaporator carries out being concentrated to give glycine concentrate
With ammonium chloride concentrate;It is again that glycine concentrate and ammonium chloride concentrate is dry by crystallization, centrifugation, crystal respectively
Purity is more than the 99.5% Glycine crystals 28.5kg for reaching feed grade;It is more than 99% with purity, can be as fertilizer
The ammonia chloride crystal 19.8kg for using;
Embodiment 3
Step 1:Will using Chloroacetic Aminolysis production the glycine crude product 30kg containing glycine and inorganic salts spend from
Sub- water dissolves are configured to mixed solution 100kg, and its mass concentration is 30%;And the quality of glycine is divided in glycine crude product
Number is 50%, and the mass fraction of ammonium chloride is 48%, and remaining is impurity;Being adjusted by ammoniacal liquor controls the mixed solution pH to be
The pH value of glycine solution is 5.5-7;
Step 2:It is 200 nanometers of ceramic membrane filter that above-mentioned mixed solution is used into pore size filter, obtains ceramic membrane dialysis
Liquid;The pH value for controlling mixed solution pH to be glycine solution is adjusted for 5.5-7 by ammoniacal liquor during ceramic membrane filter;
Step 3:Ceramic membrane dialyzate is separated using the continuous chromatography piece-rate system filled with monium resin, obtains sweet ammonia
Acid solution and ammonium chloride solution;Wherein the separation purity of glycine is more than 99%, concentration more than 9%, the separation of ammonium chloride
Purity is more than 95%, and concentration is more than 7%, and control mixed solution pH is adjusted by ammoniacal liquor in continuous chromatography separation process
For the pH value of glycine solution is 5.5-7;
Step 4:Glycine solution and ammonium chloride solution are respectively adopted into four-effect evaporator carries out being concentrated to give glycine concentrate
With ammonium chloride concentrate;It is again that glycine concentrate and ammonium chloride concentrate is dry by crystallization, centrifugation, crystal respectively
Purity is more than the 99.5% Glycine crystals 14.8kg for reaching feed grade;It is more than 99% with purity, can be as fertilizer
The ammonia chloride crystal 13.7kg for using.
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 specially
Various modifications can be carried out to the present invention without departing from the spirit and scope of the present invention after profit application.
Claims (3)
1. a kind of glycine production technology, it is characterised in that comprise the following steps:
Step 1:By using the glycine crude product deionized water dissolving containing glycine and inorganic salts of Chloroacetic Aminolysis production
It is configured to the mixed solution that mass concentration is 20-50%;
Step 2:It is 50-200 nanometers of ceramic membrane filter that above-mentioned mixed solution is used into pore size filter, obtains ceramic membrane dialyzate;
Step 3:Ceramic membrane dialyzate is separated using the continuous chromatography piece-rate system filled with monium resin or calcium type resin,
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 crystallization, centrifugation, 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.
2. a kind of 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 is concentrated.
Priority Applications (1)
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CN201510785112.7A CN106699589A (en) | 2015-11-16 | 2015-11-16 | Glycine production technology |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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CN201510785112.7A CN106699589A (en) | 2015-11-16 | 2015-11-16 | Glycine production technology |
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Publication Number | Publication Date |
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CN106699589A true CN106699589A (en) | 2017-05-24 |
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CN201510785112.7A Pending CN106699589A (en) | 2015-11-16 | 2015-11-16 | Glycine production technology |
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2015
- 2015-11-16 CN CN201510785112.7A patent/CN106699589A/en active Pending
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Application publication date: 20170524 |