CN104829472A - Refining process for glycine - Google Patents
Refining process for glycine Download PDFInfo
- Publication number
- CN104829472A CN104829472A CN201510247803.1A CN201510247803A CN104829472A CN 104829472 A CN104829472 A CN 104829472A CN 201510247803 A CN201510247803 A CN 201510247803A CN 104829472 A CN104829472 A CN 104829472A
- Authority
- CN
- China
- Prior art keywords
- glycine
- refining
- crystallizer
- crystal
- whizzer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses a refining process for glycine. The refining process comprises the following steps: discoloring, filtering, centrifuging, multi-time recycling, drying, weighing and packaging. According to the refining process, the obtained product has purity of 99% or more, light transmittance of about 96, iron salt content lower than 10 ppm, and heavy metal content lower than 10 ppm, and the mother liquor can be recycled by many times. The integral process is simple to control and relatively convenient, and the national glycine standards are met.
Description
Technical field
The present invention relates to chemical field, what be specifically related to is a kind of process for refining of glycine.
Background technology
Glycine is the important source material of the industry such as chemical industry, medicine, agricultural chemicals, tool has been widely used, at present, multiple method is had to produce glycine, such as, alpha-halogen acid system-a kind of domestic main industrialized preparing process, it is with Mono Chloro Acetic Acid, ammonia for raw material, reacts under catalyzer urotropine exists in solvent phase.Adopt and produce glycine in this way, what can produce in process of production is difficult to the inorganic salt such as the ammonium chloride be separated, and aftertreatment workload is large.
Current amino acetic acid in China manufacturer all adopts alcohol-water system to wash the method being separated pure glycine, its technical scheme is, by glycine crude product first with after water dissolution, stream adds 95-99% methyl alcohol to methanol solution is again about 70-80%, centrifugal glycine product, mother liquor adopts rectifying to reclaim methyl alcohol and ammonification ammonium.There is following defect in this method: alcohol analyse after mother liquor partial glycine product can be taken away, and can not reclaim, cause product loss, mother liquor needs to carry out rectifying, not only the loss of solvent is large and energy consumption is high, general production glycine product per ton need consume steam 10-12 ton, when reclaiming alcohol, high and large to equipment corrosion to equipment requirements, need to process a large amount of solvents, general production glycine product per ton need consume methyl alcohol 500-800 ton, and the rate of recovery is low, generally about 90%.
Summary of the invention
The object of the invention is to the above problem overcoming prior art existence, a kind of process for refining of glycine is provided, improve productive rate.
For realizing above-mentioned technical purpose, reach above-mentioned technique effect, the present invention is achieved through the following technical solutions:
A process for refining for glycine, comprises the following steps:
Step 1) drops into glycine crude product add the pure water of 1400L in dissolving vessel after, adds activated carbon when being heated to 70-75 DEG C, and the mass ratio of activated carbon and crude product is 1:3, after reheating 90-95 DEG C, and insulation 15-20 minute;
Step 2) by filter funnel, solution is evacuated in crystallizer, open the vacuum valve of crystallizer, keep crystallizer to be in vacuum state;
Step 3) is by the liquid in stirrer agitated crystallizer, and the churning time of agitator is 2 hours, and stirring velocity is 40r/min, add the temperature of cool brine to crystallizer between 10-15 DEG C, complete cloth bag, the product after filtration is put into whizzer by conduit and gets rid of worry, the rotating speed of whizzer is 1200r/min, rotation time is 60min, when material does not drip, obtain crystal, then use salt-free water washing crystal, dried by crystal, disposing mother liquor applies mechanically 6 times again;
After step 4) mother liquid recycle 6 times, use vacuum method to carry out concentrating under reduced pressure, reclaim the glycine in mother liquor;
The crystal whizzer that step 3 and step 4 obtain by step 5) gets rid of worry, the rotating speed of whizzer is 1200r/min, time is 50 minutes, then load moisture eliminator, the rotating speed of moisture eliminator is 10-15r/min, and time of drying is 2-2.5h, temperature is 60-85 DEG C, carry out steam heating under vacuum conditions, Heating temperature is 80-90 DEG C, and time of drying is 1.5-2 hour;
The dried crystal of step 6) sieves packaging, inspection.
The invention has the beneficial effects as follows:
The present invention adopts activated carbon as sorbing material, except having decoloration performance, also have the ability of adsorbing metal ions, have good decolouring and Impurity removal effect, the crude product of 97% purity is through refining, reach the purity of more than 99%, transmittance 96%, molysite <10ppm, heavy metal <10ppm, substantially without the three wastes, and mother liquor can also recycled for multiple times, technology controlling and process is simple, more convenient, meets the standard of country for glycine.
Embodiment
Below in conjunction with embodiment, describe the present invention in detail.
Embodiment 1
A process for refining for glycine, comprises the following steps:
Step 1) drops into glycine crude product add the pure water of 1400L in dissolving vessel after, adds activated carbon when being heated to 70 DEG C, and the mass ratio of activated carbon and crude product is 1:3, after reheating 90 DEG C, is incubated 15 minutes;
Step 2) by filter funnel, solution is evacuated in crystallizer, open the vacuum valve of crystallizer, keep crystallizer to be in vacuum state;
Step 3) is by the liquid in stirrer agitated crystallizer, and the churning time of agitator is 2 hours, and stirring velocity is 40r/min, add the temperature of cool brine to crystallizer between 10 DEG C, complete cloth bag, the product after filtration is put into whizzer by conduit and gets rid of worry, the rotating speed of whizzer is 1200r/min, rotation time is 60min, when material does not drip, obtain crystal, then use salt-free water washing crystal, dried by crystal, disposing mother liquor applies mechanically 6 times again;
After step 4) mother liquid recycle 6 times, use vacuum method to carry out concentrating under reduced pressure, reclaim the glycine in mother liquor;
The crystal whizzer that step 3 and step 4 obtain by step 5) gets rid of worry, the rotating speed of whizzer is 1200r/min, time is 50 minutes, then load moisture eliminator, the rotating speed of moisture eliminator is 10r/min, and time of drying is 2h, temperature is 60 DEG C, carry out steam heating under vacuum conditions, Heating temperature is 80 DEG C, and time of drying is 1.5 hours;
The dried crystal of step 6) sieves packaging, inspection.
Through inspection, the purity of product is 99.2%, transmittance 96%, molysite content 8ppm, heavy metal content 9ppm, conformance with standard.
Embodiment 2
A process for refining for glycine, comprises the following steps:
Step 1) drops into glycine crude product add the pure water of 1400L in dissolving vessel after, adds activated carbon when being heated to 73 DEG C, and the mass ratio of activated carbon and crude product is 1:3, after reheating 92 DEG C, is incubated 18 minutes;
Step 2) by filter funnel, solution is evacuated in crystallizer, open the vacuum valve of crystallizer, keep crystallizer to be in vacuum state;
Step 3) is by the liquid in stirrer agitated crystallizer, and the churning time of agitator is 2 hours, and stirring velocity is 40r/min, add the temperature of cool brine to crystallizer between 12 DEG C, complete cloth bag, the product after filtration is put into whizzer by conduit and gets rid of worry, the rotating speed of whizzer is 1200r/min, rotation time is 60min, when material does not drip, obtain crystal, then use salt-free water washing crystal, dried by crystal, disposing mother liquor applies mechanically 6 times again;
After step 4) mother liquid recycle 6 times, use vacuum method to carry out concentrating under reduced pressure, reclaim the glycine in mother liquor;
The crystal whizzer that step 3 and step 4 obtain by step 5) gets rid of worry, the rotating speed of whizzer is 1200r/min, time is 50 minutes, then load moisture eliminator, the rotating speed of moisture eliminator is 10-15r/min, and time of drying is 2.2h, temperature is 75 DEG C, carry out steam heating under vacuum conditions, Heating temperature is 85 DEG C, and time of drying is 1.8 hours;
The dried crystal of step 6) sieves packaging, inspection.
Through inspection, the purity of product is 99.35%, transmittance 96.3%, molysite content 9ppm, heavy metal content 8ppm, conformance with standard.
Embodiment 3
A process for refining for glycine, comprises the following steps:
Step 1) drops into glycine crude product add the pure water of 1400L in dissolving vessel after, adds activated carbon when being heated to 75 DEG C, and the mass ratio of activated carbon and crude product is 1:3, after reheating 95 DEG C, is incubated 20 minutes;
Step 2) by filter funnel, solution is evacuated in crystallizer, open the vacuum valve of crystallizer, keep crystallizer to be in vacuum state;
Step 3) is by the liquid in stirrer agitated crystallizer, and the churning time of agitator is 2 hours, and stirring velocity is 40r/min, add the temperature of cool brine to crystallizer between 15 DEG C, complete cloth bag, the product after filtration is put into whizzer by conduit and gets rid of worry, the rotating speed of whizzer is 1200r/min, rotation time is 60min, when material does not drip, obtain crystal, then use salt-free water washing crystal, dried by crystal, disposing mother liquor applies mechanically 6 times again;
After step 4) mother liquid recycle 6 times, use vacuum method to carry out concentrating under reduced pressure, reclaim the glycine in mother liquor;
The crystal whizzer that step 3 and step 4 obtain by step 5) gets rid of worry, the rotating speed of whizzer is 1200r/min, time is 50 minutes, then load moisture eliminator, the rotating speed of moisture eliminator is 15r/min, and time of drying is 2.5h, temperature is 60-85 DEG C, carry out steam heating under vacuum conditions, Heating temperature is 90 DEG C, and time of drying is 2 hours;
The dried crystal of step 6) sieves packaging, inspection.
Through inspection, the purity of product is 99.4%, transmittance 96.5%, molysite content 8.7ppm, heavy metal content 8.9ppm, conformance with standard.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. a process for refining for glycine, is characterized in that, comprises the following steps:
Step 1) drops into glycine crude product add the pure water of 1400L in dissolving vessel after, adds activated carbon when being heated to 70-75 DEG C, after reheating 90-95 DEG C, and insulation 15-20 minute;
Step 2) by filter funnel, solution is evacuated in crystallizer, open the vacuum valve of crystallizer, keep crystallizer to be in vacuum state;
Step 3) is by the liquid in stirrer agitated crystallizer, add the temperature of cool brine to crystallizer between 10-15 DEG C, complete cloth bag, product after filtration is put into whizzer by conduit and gets rid of worry, when material does not drip, obtain crystal, then use salt-free water washing crystal, dried by crystal, disposing mother liquor applies mechanically 6 times again;
After step 4) mother liquid recycle 6 times, use vacuum method to carry out concentrating under reduced pressure, reclaim the glycine in mother liquor;
The crystal whizzer that step 3 and step 4 obtain by step 5) gets rid of worry, then loads moisture eliminator, carries out steam heating under vacuum conditions;
The dried crystal of step 6) sieves packaging, inspection.
2. the process for refining of glycine according to claim 1, is characterized in that: in described step 1, the mass ratio of activated carbon and crude product is 1:3.
3. the process for refining of glycine according to claim 1, is characterized in that: in described step 3, the churning time of agitator is 2 hours, and stirring velocity is 40r/min.
4. the process for refining of glycine according to claim 1, is characterized in that: in described step 3, the rotating speed of whizzer is 1200r/min, and rotation time is 60min.
5. the process for refining of glycine according to claim 1, is characterized in that: the Heating temperature in described step 5 is 80-90 DEG C, and time of drying is 1.5-2 hour.
6. the process for refining of glycine according to claim 1, is characterized in that: in described step 5, the rotating speed of whizzer is 1200r/min, and the time is 50 minutes.
7. the process for refining of glycine according to claim 1, is characterized in that: in described step 5, the rotating speed of moisture eliminator is 10-15r/min, and time of drying is 2-2.5h, and temperature is 60-85 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510247803.1A CN104829472A (en) | 2015-05-15 | 2015-05-15 | Refining process for glycine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510247803.1A CN104829472A (en) | 2015-05-15 | 2015-05-15 | Refining process for glycine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104829472A true CN104829472A (en) | 2015-08-12 |
Family
ID=53807720
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510247803.1A Pending CN104829472A (en) | 2015-05-15 | 2015-05-15 | Refining process for glycine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104829472A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106397236A (en) * | 2016-08-31 | 2017-02-15 | 冀州市华阳化工有限责任公司 | Glycine purification method |
| CN115043746A (en) * | 2022-06-21 | 2022-09-13 | 山西晶硕科技有限公司 | Preparation method of food-grade glycine capable of preventing agglomeration |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03190851A (en) * | 1989-12-21 | 1991-08-20 | Mitsui Toatsu Chem Inc | Decoloring of glycine |
| EP0459803A1 (en) * | 1990-05-31 | 1991-12-04 | MITSUI TOATSU CHEMICALS, Inc. | Method for purifying glycine |
| CN1101341A (en) * | 1994-06-10 | 1995-04-12 | 河北大学 | Purifying process for glycine |
| CN1288884A (en) * | 1999-09-22 | 2001-03-28 | 苏州市永达精细化工有限公司 | Glycine purifying and closed production process |
-
2015
- 2015-05-15 CN CN201510247803.1A patent/CN104829472A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03190851A (en) * | 1989-12-21 | 1991-08-20 | Mitsui Toatsu Chem Inc | Decoloring of glycine |
| EP0459803A1 (en) * | 1990-05-31 | 1991-12-04 | MITSUI TOATSU CHEMICALS, Inc. | Method for purifying glycine |
| CN1101341A (en) * | 1994-06-10 | 1995-04-12 | 河北大学 | Purifying process for glycine |
| CN1288884A (en) * | 1999-09-22 | 2001-03-28 | 苏州市永达精细化工有限公司 | Glycine purifying and closed production process |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106397236A (en) * | 2016-08-31 | 2017-02-15 | 冀州市华阳化工有限责任公司 | Glycine purification method |
| CN115043746A (en) * | 2022-06-21 | 2022-09-13 | 山西晶硕科技有限公司 | Preparation method of food-grade glycine capable of preventing agglomeration |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102167668A (en) | Method for producing glycin with environmentally-friendly alcohol phase chloroethanoic acid method | |
| CN102897747B (en) | Carbon nanotube purification system | |
| CN104649300B (en) | The method of recovery and refining sodium bromide from dipropyl cyanoacetate mixture | |
| CN104877135A (en) | Washing and purifying method for polyphenylene sulfide resin production | |
| CN102807497A (en) | Method for recovering chloroacetic acid method glycine catalyst methenamine | |
| CN103570523B (en) | A kind of production method of 95% sodium formiate | |
| CN101982456A (en) | Production method of environmental-friendly chloroacetic acid-process glycine | |
| CN104829472A (en) | Refining process for glycine | |
| CN102442917A (en) | Energy-saving and environment-friendly method for producing glycin based on chloroacetic acid method | |
| CN104892971B (en) | Method for recycling solvent NMP in polyphenylene sulfide resin production process | |
| CN111137911A (en) | Method for preparing high-purity superfine aluminum hydroxide flame retardant by decomposition method | |
| CN111254231B (en) | Method for extracting crystalline xylose from xylose mother liquor | |
| CN103723736A (en) | Resource recovery method in white carbon black production process | |
| CN102826959B (en) | Method for extracting erythritol from erythritol mother liquor | |
| CN111732120A (en) | Environment-friendly efficient production method of high-purity silver nitrate | |
| CN106564913A (en) | Method for producing high-purity ammonium chloride from meta-position aramid by-products | |
| CN106517244A (en) | Method for producing ammonium bifluoride through fluorine-containing waste etching liquid | |
| CN102746134A (en) | Method for decreasing content of sodium chloride impurities in recovered sodium formate | |
| CN109097603A (en) | The process of Ti recovery from germanium wafer intensive processing spent acid | |
| CN113860331B (en) | Method for synthesizing high-activity potassium fluoride and co-producing sodium fluoride by using waste liquid as raw material | |
| CN106082332A (en) | A kind of ammonium metavanadate removal of impurities purifying technique | |
| CN103936639A (en) | Production process for extracting cystine by hair | |
| CN106744996A (en) | A kind of Ludox and preparation method thereof | |
| CN102417192B (en) | Process for processing potassium chloride raw material for making ion membrane potassium hydroxide | |
| CN1312122C (en) | Method for preparing and purifying cyanate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150812 |