CN102234239A - Optimization process of glycine ethyl ester hydrochloride - Google Patents
Optimization process of glycine ethyl ester hydrochloride Download PDFInfo
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- CN102234239A CN102234239A CN201010160723XA CN201010160723A CN102234239A CN 102234239 A CN102234239 A CN 102234239A CN 201010160723X A CN201010160723X A CN 201010160723XA CN 201010160723 A CN201010160723 A CN 201010160723A CN 102234239 A CN102234239 A CN 102234239A
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- mother liquor
- ethyl ester
- ester hydrochloride
- glycine ethyl
- ethanol
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Abstract
The invention relates to an optimization process of glycine ethyl ester hydrochloride; the glycine ethyl ester hydrochloride is synthesized by glycine, ethanol and glycolic acid; the invention is characterized in that the process comprises the following steps: performing synthesis with 95% ethanol instead of anhydrous alcohol; after the synthetic reaction, cooling with cooling water, performing crystallization, performing centrifugation when the temperature is decreased to 15-30 DEG C, after centrifugation, drying the materials in a drying chamber; adding the mother liquor into a mother liquor pot, injecting the mother liquor into a concentrator for concentration, after concentration, cooling with circulating water to 15-30 DEG C for crystallization, discharging the materials and performing centrifugation, performing centrifugal drying of the crystal substance which is used as a raw material, mixing the centrifuged mother liquor and a next mother liquor, performing cyclic concentration, crystallization and centrifugation, neutralizing the steamed fraction from the concentrator in a neutralization kettle by liquid alkali, and recovering ethanol for recycle by rectification. The process has simple operations, reduced cost, and low restriction degree of raw materials; in the new process, product yield is increased, and cost is greatly saved; in the new process, the recovery of 95% ethanol reduces the using amount of steam, and decreases labor cost.
Description
Technical field
The present invention relates to the technology that a kind of glycine ethyl ester hydrochloride is optimized, belong to the agricultural chemical insecticide field.
Background technology
Glycine ethyl ester hydrochloride, another name aminoguanidine hydrochloride ethyl acetate or Glycocoll hydrochloride ethyl ester.
Chemical name: 1-ethyl aminoacetate hydrochloride
Molecular formula: C
4H
10NClO
2
Molecular weight: 139.56;
Outward appearance: pure product are white or faint yellow acicular crystals;
Solvability: soluble in water, be slightly soluble in ethanol, be insoluble to ether.
The chemical property less stable of glycine ethyl ester hydrochloride slowly decomposes in the time of 200 ℃, and long-term storage is because of its content of acid gas volatilization the reduction.Glycine ethyl ester hydrochloride mainly as the intermediate of pyrethrin and the intermediate of aerial fog pesticide, also is used for Biochemical Research.Former glycine ethyl ester hydrochloride production technique adopts the stationary crystallization method, and ethanol consumes high, and production environment is poor, can't produce in plant area of company, and glycine ethyl ester hydrochloride quality shakiness, yield is low when being used for chrysanthemumic acid production.
Summary of the invention
The technical problem that the present invention mainly solves is: optimize original technology, reduce the consumption of glycine in the production process, improve the yield of glycine ethyl ester hydrochloride to glycine.Technological operation after the improvement is simple, and raw material restriction degree is low, and chrysanthemum esters product industrial chain is further extended.
A kind of optimization technology of glycine ethyl ester hydrochloride is pressed the synthetic glycine ethyl ester hydrochloride of known technology with glycine, ethanol and oxyacetic acid, and its feature may further comprise the steps:
A. replacing dehydrated alcohol with 95% ethanol synthesizes;
B. after building-up reactions finishes,, carry out crystallization by cooling water temperature, when reduce to 15～30 ℃ centrifugal, centrifugal back material is gone into the drying shed oven dry;
C. mother liquor enters mother liquor tank, squeeze into again in the concentration kettle and concentrate, after concentrating, open cycle is water-cooled to 15～30 ℃ of crystallizations, blowing is centrifugal, makes raw material after this crystallisate dries and uses, and throwing away circulates after mother liquor and next mother liquor merge concentrates, crystallization, centrifugal, concentration kettle steam cut in and still with in the liquid caustic soda and after, reclaim ethanol through rectifying and recycle.
Described cooling water temperature process is carried out under whipped state.
Described crystallisation process is at first with cooling water temperature to 50～70 ℃, then with per hour 3～7 ℃ speed cooling.
Described simmer down to reaches 90～100 ℃ when concentration kettle top temperature, and material steams fraction and accounts for institute's 70 of mother liquor total amount～90% of throwing and o'clock stop to heat.
The beneficial effect that the present invention had is: this technological operation is simple, can reduce cost greatly and the reduction of raw material restriction degree; Product yield improves in the novel process, has saved great amount of cost; 95% alcoholic acid reclaims in the novel process, has significantly reduced the usage quantity of steam, has also reduced cost of labor.
Specific embodiment
Embodiment 1
The preparation of alkyd: in the alkyd jar, add ethanol 1000L, under the state that stirs, feed hydrogen chloride gas, stop after qualified by regulating the flow of spinner-type flowmeter control hydrogen chloride gas, adds to take a sample after 5 hours; Qualified alkyd hydrogen chloride content 〉=30%.It is stand-by that qualified alkyd is squeezed into the alkyd basin.
Building-up reactions: add alkyd 1300L again after in reactor, adding the 500Kg glycine earlier.Heating elevated temperature to 72 ℃ begins insulation, and soaking time is more than 1 hour.Insulation is cooled to 60 ℃ after finishing, and controlled temperature makes system per hour lower the temperature 3 ℃.When reduced to begin after crystallization is separated out centrifugal.
Centrifugal crystallisate is sweet salt, the qualified back of oven dry sampling packing.Mother liquor after centrifugal is squeezed in the concentration kettle with pump and is concentrated.When concentration kettle top temperature reaches 100 ℃, material steams fraction and accounts for 90% o'clock of the mother liquor total amount of throwing and stop heating, squeezes in the rectifying jar concentrating the cut that steams, and reclaims the ethanol recycled through rectifying; The open cycle of still bed material is water-cooled to crystallization separate out after, blowing is centrifugal; This crystallisate dries and applies mechanically as raw material, throws away mother liquor and next mother liquor and merges concentrated, the crystallization, centrifugal of back circulation.
Rectifying: will concentrate the material that steams and squeeze into rectifying still, open steam brake, the control vapor pressure is about 0.02MPa, after having backflow, opens material total reflux earlier, reflux and collect fraction by regulating under meter 400L/h dominant discharge after 1 hour, when still temperature during at 100 ℃, close discharging flow and take into account the discharging lock and stop steam, stop stirring.Production data sees Table one.
Embodiment 2
The preparation of alkyd: in the alkyd jar, add ethanol 1000L, under the state that stirs, feed hydrogen chloride gas, stop after qualified by regulating the flow of spinner-type flowmeter control hydrogen chloride gas, adds to take a sample after 5 hours; Qualified alkyd hydrogen chloride content 〉=30%.It is stand-by that qualified alkyd is squeezed into the alkyd basin.
Building-up reactions: add alkyd 1300L again after in reactor, adding the 500Kg glycine earlier.Heating elevated temperature to 72 ℃ begins insulation, and soaking time is more than 1 hour.Insulation is cooled to 50 ℃ after finishing, and controlled temperature makes system per hour lower the temperature 5 ℃.When reduced to begin after crystallization is separated out centrifugal.
Centrifugal crystallisate is sweet salt, the qualified back of oven dry sampling packing.Mother liquor after centrifugal is squeezed in the concentration kettle with pump and is concentrated.When concentration kettle top temperature reaches 90 ℃, material steams fraction and accounts for 70% o'clock of the mother liquor total amount of throwing and stop heating, squeezes in the rectifying jar concentrating the cut that steams, and reclaims the ethanol recycled through rectifying; The open cycle of still bed material is water-cooled to crystallization separate out after, blowing is centrifugal; This crystallisate dries and applies mechanically as raw material, throws away mother liquor and next mother liquor and merges concentrated, the crystallization, centrifugal of back circulation.
Rectifying: will concentrate the material that steams and squeeze into rectifying still, open steam brake, the control vapor pressure is about 0.02MPa, after having backflow, opens material total reflux earlier, reflux and collect fraction by regulating under meter 400L/h dominant discharge after 1 hour, when still temperature during at 100 ℃, close discharging flow and take into account the discharging lock and stop steam, stop stirring.Table one between production data.
Embodiment 3
The preparation of alkyd: in the alkyd jar, add ethanol 1000L, under the state that stirs, feed hydrogen chloride gas, stop after qualified by regulating the flow of spinner-type flowmeter control hydrogen chloride gas, adds to take a sample after 5 hours; Qualified alkyd hydrogen chloride content 〉=30%.It is stand-by that qualified alkyd is squeezed into the alkyd basin.
Building-up reactions: add alkyd 1300L again after in reactor, adding the 500Kg glycine earlier.Heating elevated temperature to 72 ℃ begins insulation, and soaking time is more than 1 hour.Insulation is cooled to 70 ℃ after finishing, and controlled temperature makes system per hour lower the temperature 7 ℃.When reduced to begin after crystallization is separated out centrifugal.
Centrifugal crystallisate is sweet salt, the qualified back of oven dry sampling packing.Mother liquor after centrifugal is squeezed in the concentration kettle with pump and is concentrated.When concentration kettle top temperature reaches 95 ℃, material steams fraction and accounts for 80% o'clock of the mother liquor total amount of throwing and stop heating, squeezes in the rectifying jar concentrating the cut that steams, and reclaims the ethanol recycled through rectifying; The open cycle of still bed material is water-cooled to crystallization separate out after, blowing is centrifugal; This crystallisate dries and applies mechanically as raw material, throws away mother liquor and next mother liquor and merges concentrated, the crystallization, centrifugal of back circulation.
Rectifying: will concentrate the material that steams and squeeze into rectifying still, open steam brake, the control vapor pressure is about 0.02MPa, after having backflow, opens material total reflux earlier, reflux and collect fraction by regulating under meter 400L/h dominant discharge after 1 hour, when still temperature during at 100 ℃, close discharging flow and take into account the discharging lock and stop steam, stop stirring.Table one between production data.
Table one: sweet salt production data
Claims (4)
1. the optimization technology of a glycine ethyl ester hydrochloride is synthesized glycine ethyl ester hydrochloride with glycine, ethanol and oxyacetic acid, and its feature may further comprise the steps:
A. replacing dehydrated alcohol with 95% ethanol synthesizes;
B. after building-up reactions finishes,, carry out crystallization by cooling water temperature, when reduce to 15～30 ℃ centrifugal, centrifugal back material is gone into the drying shed oven dry;
C. mother liquor enters mother liquor tank, squeeze into again in the concentration kettle and concentrate, after concentrating, open cycle is water-cooled to 15～30 ℃ of crystallizations, blowing is centrifugal, makes raw material after this crystallisate dries and uses, and throwing away circulates after mother liquor and next mother liquor merge concentrates, crystallization, centrifugal, concentration kettle steam cut in and still with in the liquid caustic soda and after, reclaim ethanol through rectifying and recycle.
2. the optimization technology of glycine ethyl ester hydrochloride according to claim 1 is characterized in that described cooling water temperature process carries out under whipped state.
3. the optimization technology of glycine ethyl ester hydrochloride according to claim 1 is characterized in that described crystallisation process is at first with cooling water temperature to 50～70 ℃, then with per hour 3～7 ℃ speed cooling.
4. the optimization technology of glycine ethyl ester hydrochloride according to claim 1 is characterized in that reaching 90～100 ℃ when concentration kettle top temperature, and material steams fraction and accounts for institute's 70 of mother liquor total amount～90% of throwing and o'clock stop to heat.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010160723XA CN102234239A (en) | 2010-04-30 | 2010-04-30 | Optimization process of glycine ethyl ester hydrochloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010160723XA CN102234239A (en) | 2010-04-30 | 2010-04-30 | Optimization process of glycine ethyl ester hydrochloride |
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| CN102234239A true CN102234239A (en) | 2011-11-09 |
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| CN201010160723XA Pending CN102234239A (en) | 2010-04-30 | 2010-04-30 | Optimization process of glycine ethyl ester hydrochloride |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010770A (en) * | 2020-09-07 | 2020-12-01 | 河北东华舰化工有限公司 | Novel production method of glycine ethyl ester hydrochloride |
| CN112375007A (en) * | 2020-12-02 | 2021-02-19 | 江苏优普生物化学科技股份有限公司 | Treatment process for leftovers generated in preparation process of glycine ethyl ester hydrochloride |
| CN115466188A (en) * | 2022-06-24 | 2022-12-13 | 大连凯飞化学股份有限公司 | Novel synthesis process of glycine ethyl ester hydrochloride |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0376230A2 (en) * | 1988-12-27 | 1990-07-04 | MITSUI TOATSU CHEMICALS, Inc. | Preparation and isolation of mineral acid salt of an amino methyl ester |
-
2010
- 2010-04-30 CN CN201010160723XA patent/CN102234239A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0376230A2 (en) * | 1988-12-27 | 1990-07-04 | MITSUI TOATSU CHEMICALS, Inc. | Preparation and isolation of mineral acid salt of an amino methyl ester |
Non-Patent Citations (2)
| Title |
|---|
| 金维高: "《医药中间体生产实用技术手册》", 30 June 2002, 化学工业出版社 * |
| 顾伯琴: "甘氨酸乙酯盐酸盐的工艺改进", 《江苏化工》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010770A (en) * | 2020-09-07 | 2020-12-01 | 河北东华舰化工有限公司 | Novel production method of glycine ethyl ester hydrochloride |
| CN112375007A (en) * | 2020-12-02 | 2021-02-19 | 江苏优普生物化学科技股份有限公司 | Treatment process for leftovers generated in preparation process of glycine ethyl ester hydrochloride |
| CN112375007B (en) * | 2020-12-02 | 2022-09-16 | 江苏优普生物化学科技股份有限公司 | Treatment process of leftovers generated in preparation process of glycine ethyl ester hydrochloride |
| CN115466188A (en) * | 2022-06-24 | 2022-12-13 | 大连凯飞化学股份有限公司 | Novel synthesis process of glycine ethyl ester hydrochloride |
| CN115466188B (en) * | 2022-06-24 | 2023-08-18 | 大连凯飞化学股份有限公司 | Novel process for synthesizing glycine ethyl ester hydrochloride |
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