CN111548281B - Production method and production equipment of glycine ethyl ester hydrochloride - Google Patents
Production method and production equipment of glycine ethyl ester hydrochloride Download PDFInfo
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- CN111548281B CN111548281B CN202010446356.3A CN202010446356A CN111548281B CN 111548281 B CN111548281 B CN 111548281B CN 202010446356 A CN202010446356 A CN 202010446356A CN 111548281 B CN111548281 B CN 111548281B
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Abstract
The invention discloses a production method of glycine ethyl ester hydrochloride, which comprises the steps of preparing absolute ethyl alcohol and hydrogen chloride into a hydrogen chloride ethanol solution, gradually adding glycine into the solution to esterify and form salt, adding dichloroethane, and forming a ternary system by ethanol-dichloroethane-water, boiling, absorbing water in a water absorbing layer, changing the color of the water absorbing layer, continuously esterifying the water absorbing layer into glycine ethyl ester hydrochloride, cooling, crystallizing and filtering reaction liquid, drying to obtain glycine ethyl ester hydrochloride, extracting and distilling filtrate for separation, wherein the recovered ethanol, dichloroethane and water can be recycled; the production equipment mainly comprises a reaction kettle, a crystallizing tank and a separating tank, wherein a water absorption layer and an electric heating device are arranged in the reaction kettle, a water spraying device and a filtering layer are arranged in the crystallizing tank, and the electric heating device and a reflux device are arranged in the separating tank. The production method of the invention improves the conversion rate, yield and quality of glycine ethyl ester hydrochloride, and integrates a plurality of working procedures into one process device, thereby reducing the loss of materials and products and reducing the working procedure devices.
Description
Technical Field
The invention relates to a production method and production equipment of glycine ethyl ester hydrochloride, and belongs to the technical field of glycine ethyl ester hydrochloride production.
Background
The glycine ethyl ester hydrochloride is chemically named as glycine ethyl ester hydrochloride, is used as a raw material of pesticide pyrethroid insecticides and pharmaceutical industry, for example, is used as an intermediate for preparing chrysanthemic acid and dichlorochrysanthemic acid, bactericide iprodione, medical anti-inflammatory drugs, tetrazolyl acetic acid and the like, and is also used for preparations such as biochemical research and the like. Glycine is usually used as a raw material for industrially producing glycine ethyl ester hydrochloride, dry hydrogen chloride gas is introduced into absolute ethyl alcohol to prepare a hydrogen chloride ethanol solution, then glycine is added, the mixture is heated and stirred to carry out esterification reaction to produce glycine ethyl ester hydrochloride, and simultaneously water is generated, the glycine ethyl ester hydrochloride is very easy to dissolve in water, so that the content of residual products in mother liquor is increased, even partial glycine ethyl ester hydrochloride is hydrolyzed to generate glycine hydrochloride in the esterification reaction process, and the conversion rate, yield and product quality of the generated glycine ethyl ester hydrochloride are reduced; at present, more process equipment is needed in the production process of glycine ethyl ester hydrochloride, the glycine ethyl ester hydrochloride is moved from one process equipment to the next process equipment, material and product loss is caused in the process of multiple transfer, the material cost is increased, the yield of the glycine ethyl ester hydrochloride is reduced, and meanwhile, the production cost of the equipment is high.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a production method and production equipment for improving the conversion rate, yield and quality of glycine ethyl ester hydrochloride.
The invention provides a production method of glycine ethyl ester hydrochloride, which takes glycine as a raw material and comprises the following steps:
(1) Firstly, absolute ethyl alcohol which is 0.92 to 1.23 times of the weight of the glycine is added into a reaction kettle, then dry hydrogen chloride which is 48.62 to 49.05 percent of the weight of the glycine is introduced, and the hydrogen chloride and part of the absolute ethyl alcohol are prepared into hydrogen chloride ethanol solution;
(2) Then gradually adding glycine into the hydrogen chloride ethanol solution, heating and stirring, raising the temperature to 75-80 ℃, and carrying out esterification reaction on the glycine and the hydrogen chloride ethanol solution to generate glycine ethyl ester hydrochloride;
(3) Reacting until 80-90% of glycine is dissolved, adding dichloroethane which is 1.58-2.1 times of the weight of the glycine and absolute ethyl alcohol which is 0.61-1.23 times of the weight of the glycine, gradually heating until boiling, wherein the water generated by the reaction, the dichloroethane and the ethyl alcohol form a ternary system, gradually heating until boiling, allowing the gas phase in the azeotropic system to pass through a water absorption layer, taking away the water in the water absorption layer, changing the color of the water absorption layer, simultaneously condensing the dichloroethane and the ethyl alcohol downwards, refluxing into a reaction kettle, and continuously esterifying the glycinate hydrochloride and the ethyl alcohol to generate glycinate hydrochloride until the color of the water absorption layer is not changed or the water absorption layer is saturated;
(4) Reducing the temperature in the reaction kettle to 60-65 ℃, transferring the reaction liquid into a crystallization tank, flushing the reaction kettle with absolute ethyl alcohol accounting for 15.34-21.47% of the weight of the glycine, then feeding the reaction liquid into the crystallization tank, cooling and crystallizing the reaction liquid in the crystallization tank, filtering after complete crystallization, feeding the filtrate into a separation tank, flushing the filtrate with absolute ethyl alcohol accounting for 5.34-21.47% of the weight of the glycine, then feeding the filtrate into the separation tank, taking out a filter layer, and drying to obtain glycine ethyl ester hydrochloride;
(5) Adding water 2-3 times of the weight of the glycine into the separation tank, stirring and mixing the water and the filtrate, standing, dissolving the ethanol in the filtrate, layering the water and the dichloroethane, transferring the dichloroethane into a dichloroethane recovery tank, heating and distilling the ethanol aqueous solution in the separation tank at the temperature of 80-85 ℃, and distilling the ethanol out to enter the ethanol recovery tank.
Preferably, the water absorption layer is filled with water absorption silica gel beads added with cobalt chloride, the color of the water absorption silica gel beads is blue when the water absorption layer is dried, and after water absorption, the blue color gradually becomes light and becomes bluish violet and purplish red gradually, so that whether the esterification reaction is finished or not can be determined conveniently.
Preferably, after the reaction kettle is washed clean, the water absorption layer is heated and dried, the absorbed water is completely evaporated, the color of the water absorption layer is recovered to the anhydrous color blue, and the water absorption layer can be recycled.
The invention also provides production equipment of glycine ethyl ester hydrochloride, which comprises a reaction kettle with a stirring function, a crystallizing tank communicated with a reaction liquid outlet on the reaction kettle, a separating tank communicated with a filtrate outlet on the crystallizing tank, and an ethanol outlet, a dichloroethane outlet and a water outlet which are correspondingly communicated, wherein the reaction kettle is sequentially arranged from the upper left to the lower right, the separating tank with the stirring function is communicated, and the ethanol outlet, the dichloroethane outlet and the water outlet of the separating tank are correspondingly communicated; the separation tank is a transparent separation tank.
Preferably, a reaction stirring shaft of the reaction kettle penetrates through the center of the water absorption layer, the water absorption layer is in sliding connection with the water absorption layer, the water absorption layer comprises two clamping plates which are connected up and down and provided with through holes, and water absorption silica gel beads filled between the two clamping plates, cobalt chloride is added into the water absorption silica gel beads, and the diameter of each water absorption silica gel bead is larger than the aperture of each through hole; the hydrogen chloride inlet, the glycine inlet, the ethanol inlet and the dichloroethane inlet on the reaction kettle are circumferentially arranged on the upper part of the reaction kettle in the anticlockwise direction and are positioned below the water absorption layer, the hydrogen chloride inlet, the glycine inlet, the ethanol inlet and the dichloroethane inlet are arranged, the steam outlet and the reaction liquid outlet on the reaction kettle are respectively positioned at the top and the bottom center of the reaction kettle, the reaction liquid outlet on the reaction kettle is communicated with the reaction liquid inlet on the crystallization tank, the height of the reaction liquid outlet is higher than that of the reaction liquid inlet, battery valves are respectively arranged on the reaction liquid outlet, the glycine inlet, the ethanol inlet, the dichloroethane inlet and the steam outlet, and sealing covers are respectively arranged on the hydrogen chloride inlet and the crystal outlet.
Preferably, the reflux device comprises a condensation plate and an elliptical ring baffle plate, the center of the condensation plate protrudes upwards to form an umbrella-shaped structure, a separation stirring rod of the separation tank penetrates through the center of the condensation plate and is in sliding connection with the condensation plate, the separation stirring rod of the separation tank penetrates through the elliptical ring baffle plate and forms a through cavity hole with the elliptical ring baffle plate, the condensation plate is fixedly connected with the top of the separation tank, the elliptical ring baffle plate is obliquely arranged in the separation tank, the outer edge of the elliptical ring baffle plate is fixedly connected with the inner wall of the separation tank, an annular groove which is inclined with the inner wall of the separation tank is obliquely and upwards arranged at the inner edge of the elliptical ring baffle plate, and the edge of the condensation plate is positioned above the elliptical ring baffle plate; the filtering liquid inlet on the separating tank is positioned below the highest point of the elliptical ring baffle, the ethanol outlet on the separating tank is positioned at the lowest point of the elliptical ring baffle, the water inlet on the separating tank is positioned below the ethanol outlet, the water inlet is communicated with the water recovery tank, a water pump is arranged on a pipeline of the water inlet, the dichloroethane outlet and the water outlet on the separating tank are respectively positioned at the center and the lower part of the bottom of the separating tank, the filtering liquid inlet on the separating tank is communicated with the filtering liquid outlet on the crystallizing tank, the height of the filtering liquid outlet is higher than that of the filtering liquid inlet, and battery valves are respectively arranged on the dichloroethane outlet, the filtering liquid outlet, the water inlet and the water outlet.
Preferably, the drying column is filled with water-absorbing silica gel beads, the outer side of the drying column is provided with an electric heating device, the drying column is provided with a vent hole, and the vent hole is provided with a sealing cover.
The invention has the beneficial effects that:
1. according to the production method, firstly, absolute ethyl alcohol and hydrogen chloride are prepared into a hydrogen chloride ethanol solution, then glycine is gradually added to esterify and form salt, dichloroethane is added after most glycine ester is dissolved, an ethanol-dichloroethane-water ternary system is formed with water generated in the reaction, mixed steam is formed by heating and azeotropy and enters a water absorption layer to absorb water, the generated water is timely taken out of the reaction liquid, the generation of glycine hydrochloride and the dissolution of glycine ethyl ester hydrochloride are reduced, the reaction time can be shortened, and the energy consumption is reduced; the water content in the reaction liquid is reduced, glycine hydrochloride generated by hydrolysis is continuously esterified into glycine ethyl ester hydrochloride, the conversion rate and the quality of the glycine ethyl ester hydrochloride are improved, meanwhile, the water content in the reaction liquid is reduced, more glycine ethyl ester hydrochloride is separated out, and the yield of the glycine ethyl ester hydrochloride is improved.
2. Meanwhile, dichloroethane and ethanol in the azeotropic gas phase composition are liquefied, refluxed and dropped into the reaction liquid in the water absorption layer, so that dichloroethane or ethanol does not need to be supplemented in the continuous esterification process, the operation procedures are reduced, the using amount is reduced, and the cost is saved.
3. In the process of removing water by the water absorption layer, the dried water absorption layer is blue, the blue water absorption layer gradually becomes blue purple and purple red, so that whether the esterification reaction is finished or not is easily judged according to the color change condition of the water absorption layer; after the esterification in the reaction kettle is finished and the reaction kettle is washed clean, the water absorption layer can be heated and dried, the absorbed water is completely evaporated, the color of the water absorption layer is recovered to the original color, the operation is simple and convenient, the absorption layer is recycled, and the energy consumption and the cost are saved.
4. The invention can integrate a plurality of working procedures into one process device, reduce the material transfer times, reduce the loss of materials and products, reduce the used working procedure devices, reduce the production cost of the device, save the material cost and further improve the yield of the glycine ethyl ester hydrochloride.
5. The esterification reaction, the crystallization process and the separation process are correspondingly carried out in a reaction kettle, a crystallization tank and a separation tank of production equipment; meanwhile, a water absorption layer is arranged in the reaction kettle, water can be directly removed in the reaction process, separation is not required after evaporation, ethanol and dichloroethane do not need to be supplemented and added again during backflow, and a water spraying device and a filter layer are arranged in the crystallization tank, so that filtering and washing are integrated; the separating tank has a stirring function, can perform extraction stirring to separate dichloroethane, and is additionally provided with the electric heating device and the reflux device to perform distillation to separate ethanol, so that water, ethanol and dichloroethane are completely separated and can be recycled.
6. The reflux device comprises the umbrella-shaped condensing plate and the elliptical ring baffle plate which forms an inclined ring groove with the separating tank, and is beneficial to the distilled ethanol to flow out and enter the ethanol recovery tank.
7. The drying column can dry the distilled ethanol to obtain the absolute ethanol, so that the absolute ethanol can be recycled.
Drawings
FIG. 1 is a schematic view of a production apparatus of the present invention;
FIG. 2 is a schematic view of the structure of a reaction vessel of the production apparatus of the present invention;
FIG. 3 is a plan view of a reaction vessel of the production apparatus of the present invention;
FIG. 4 isbase:Sub>A cross-sectional view taken along line A-A of FIG. 3;
FIG. 5 is a schematic sectional view of a separation tank of the production apparatus of the present invention;
fig. 6 is a cross-sectional view taken at B-B in fig. 5.
In the figure: 1. the device comprises a reaction kettle, 1-1 parts of a hydrogen chloride inlet, 1-2 parts of a glycine inlet, 1-3 parts of an ethanol inlet, 1-4 parts of a dichloroethane inlet, 1-5 parts of a steam outlet, 1-6 parts of a reaction liquid outlet, 2 parts of a crystallizing tank, 2-1 parts of a reaction liquid inlet, 2-2 parts of a filtrate outlet, 2-3 parts of a crystal outlet, 3 parts of a separating tank, 3-1 parts of a filtrate inlet, 3-2 parts of an ethanol outlet, 3-3 parts of a dichloroethane outlet, 3-4 parts of a water outlet, 3-5 parts of a water inlet, 5 parts of an ethanol recovery tank, 6 parts of a dichloroethane recovery tank, 7 parts of a water recovery tank, 8 parts of a water absorbing layer, 9 parts of an observation window, 10 parts of a filter layer, 11 parts of a liquid spraying device, 12 parts of a condensation plate, 13 parts of an elliptical ring baffle, 14 parts of a ring groove, 15 parts of a drying column, 16 parts of an electric heating device, 17 parts of a heat preservation and insulation layer, 18 parts of a battery valve, 19 parts of an ethanol pump, 20 parts of a water pump.
Detailed Description
The technical solutions in the implementation of the present invention will be made clear and fully described below with reference to the accompanying drawings, and the described embodiments are only a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A production method of glycine ethyl ester hydrochloride comprises the following steps:
(1) Firstly, putting 82.93kg of absolute ethyl alcohol into a reaction kettle, then introducing dry hydrogen chloride at the flow rate of 10.47kg/min for 3.5min, and firstly preparing hydrogen chloride and part of absolute ethyl alcohol into a hydrogen chloride ethanol solution;
(2) Then gradually adding 75.07kg of glycine into the hydrogen chloride ethanol solution, heating and stirring, raising the temperature to 75-80 ℃, and carrying out esterification reaction on the glycine and the hydrogen chloride ethanol solution to generate glycine ethyl ester hydrochloride;
(3) Reacting until 80-90% of glycine by weight is dissolved, adding 128.66kg of dichloroethane and 59.89kg of absolute ethyl alcohol, reacting to generate water, dichloroethane and ethyl alcohol to form a ternary system, gradually heating until the solution is boiled, allowing the gas phase in the azeotropic system to pass through a water absorption layer, wherein the color of water absorption silica gel beads of the water absorption layer is blue at the beginning, absorbing water by the water absorption silica gel beads of the water absorption layer, gradually lightening the blue color, simultaneously condensing the dichloroethane and the ethyl alcohol downwards, refluxing the condensed water to a reaction kettle, and continuously esterifying the glycine hydrochloride with the ethyl alcohol to generate glycine ethyl ester hydrochloride, which is gradually bluish-purple until the color of the water absorption layer is not changed any more;
(4) Reducing the temperature in the reaction kettle to 60-65 ℃, transferring the reaction liquid into a crystallization tank, flushing the reaction kettle with 12.44kg of absolute ethyl alcohol, then feeding the reaction liquid into the crystallization tank, cooling and crystallizing the reaction liquid in the crystallization tank, filtering the reaction liquid after complete crystallization, feeding the filtrate into a separation tank, flushing the reaction liquid with 12.56kg of absolute ethyl alcohol, then feeding the filtrate into the separation tank, taking out a filter layer, drying the filter layer to obtain glycine ethyl ester hydrochloride, simultaneously flushing the reaction kettle, heating and drying a water absorption layer, completely evaporating the absorbed water, and recovering the color of the water absorption layer to blue;
(5) Adding 172kg of water into a separation tank, stirring and mixing the water and the filtrate, standing, dissolving ethanol into the mixture, layering the water and dichloroethane, heating and distilling the ethanol aqueous solution in the separation tank until the temperature is raised to 80-85 ℃, and distilling the ethanol out to enter an ethanol recovery tank;
(6) The weight of the resulting dried glycine ethyl ester hydrochloride was determined to be 137.04kg with a yield of 97.46% (calculated as glycine, the same applies below); and detecting the purity of the dried glycine ethyl ester hydrochloride, wherein the content of the glycine ethyl ester hydrochloride is 98.51 percent, and the content of the glycine hydrochloride is 0.82 percent; and simultaneously detecting the recovered ethanol, dichloroethane and water, wherein the recovered ethanol contains water and trace hydrogen chloride, the content of water is less than 0.45%, the recovered dichloroethane contains water and ethanol, the content of water is 0.12%, the content of ethanol is 0.31%, the recovered water contains ethanol, and the content of ethanol is 0.41%.
Example 2
A production method of glycine ethyl ester hydrochloride comprises the following steps:
(1) Firstly putting 108.1kg of absolute ethyl alcohol into a reaction kettle, then introducing dry hydrogen chloride at the flow rate of 13.74kg/min for 4min, and firstly preparing hydrogen chloride and part of absolute ethyl alcohol into hydrogen chloride ethanol solution;
(2) Then gradually adding 112.60kg of glycine into the hydrogen chloride ethanol solution, heating and stirring, raising the temperature to 75-80 ℃, and carrying out esterification reaction on the glycine and the hydrogen chloride ethanol solution to generate glycine ethyl ester hydrochloride;
(3) Reacting until 80-90 wt% of glycine is dissolved, adding 197.06kg of dichloroethane and 96.84kg of absolute ethanol, reacting to generate water, dichloroethane and ethanol to form a ternary system, gradually heating until the solution is boiled, allowing the gas phase in the azeotropic system to pass through a water absorption layer, wherein the water absorption silica gel bead of the water absorption layer is blue at the beginning, absorbing water by the water absorption silica gel bead of the water absorption layer, and gradually lightening the blue color, and simultaneously condensing the dichloroethane and the ethanol downwards and refluxing the condensed water into a reaction kettle to allow glycine hydrochloride to continuously esterify with the ethanol to generate glycine ethyl ester hydrochloride which gradually turns into blue-violet until the color of the water absorption layer is not changed;
(4) Reducing the temperature in the reaction kettle to 60-65 ℃, transferring the reaction liquid into a crystallizing tank by heating, flushing the reaction kettle with 18.35kg of absolute ethyl alcohol, then feeding the reaction liquid into the crystallizing tank, cooling and crystallizing the reaction liquid in the crystallizing tank, filtering the reaction liquid after crystallization is complete, feeding the filtrate into a separating tank, flushing the reaction liquid with 19.21kg of absolute ethyl alcohol, then feeding the filtrate into the separating tank, taking out a filter layer, drying the filter layer to obtain glycine ethyl ester hydrochloride, simultaneously flushing the reaction kettle, heating and drying a water absorbing layer, completely evaporating out the absorbed water, and recovering the color of the water absorbing layer to blue;
(5) Adding 245kg of water into a separation tank, stirring and mixing the water and the filtrate, standing, dissolving ethanol in the mixture, layering the water and dichloroethane, heating and distilling the ethanol water solution in the separation tank until the temperature is increased to 80-85 ℃, and distilling the ethanol to enter an ethanol recovery tank;
(6) The weight of the obtained dry glycine ethyl ester hydrochloride is determined to be 204.45kg, and the yield is 97.65%; and detecting the purity of the dried glycine ethyl ester hydrochloride, wherein the content of the glycine ethyl ester hydrochloride is 98.38 percent, and the content of the glycine hydrochloride is 0.86 percent; and simultaneously detecting the recovered ethanol, dichloroethane and water, wherein the recovered ethanol contains water and trace hydrogen chloride, the content of water is less than 0.41%, the recovered dichloroethane contains water and ethanol, the content of water is 0.11%, the content of ethanol is 0.32%, the recovered water contains ethanol, and the content of ethanol is 0.40%.
Example 3
A production method of glycine ethyl ester hydrochloride comprises the following steps:
(1) Firstly putting 166.65kg of absolute ethyl alcohol into a reaction kettle, then introducing dry hydrogen chloride at the flow rate of 24.40kg/min for 3min, and firstly preparing hydrogen chloride and part of absolute ethyl alcohol into hydrogen chloride ethanol solution;
(2) Then gradually adding 150.14kg of glycine into the hydrogen chloride ethanol solution, heating and stirring, raising the temperature to 75-80 ℃, and carrying out esterification reaction on the glycine and the hydrogen chloride ethanol solution to generate glycine ethyl ester hydrochloride;
(3) Reacting until 80-90% of glycine by weight is dissolved, adding 267.24kg of dichloroethane and 132.32kg of absolute ethyl alcohol, reacting to generate water, forming a ternary system with the dichloroethane and the ethyl alcohol, gradually heating until the solution is boiled, allowing the gas phase in the azeotropic system to pass through a water absorption layer, wherein the color of water absorption silica gel beads of the water absorption layer is blue at the beginning, absorbing water by the water absorption silica gel beads of the water absorption layer, gradually lightening the blue color, simultaneously condensing the dichloroethane and the ethyl alcohol downwards, refluxing the condensed water to enter a reaction kettle, and continuously esterifying the glycine hydrochloride with the ethyl alcohol to generate glycine ethyl ester hydrochloride, which gradually turns into blue-violet until the color of the water absorption layer is not changed;
(4) Reducing the temperature in the reaction kettle to 60-65 ℃, transferring the reaction liquid into a crystallization tank, flushing the reaction kettle with 26.15kg of absolute ethyl alcohol, then feeding the reaction liquid into the crystallization tank, cooling and crystallizing the reaction liquid in the crystallization tank, filtering the reaction liquid after complete crystallization, feeding the filtrate into a separation tank, flushing the reaction liquid with 26.58kg of absolute ethyl alcohol, then feeding the filtrate into the separation tank, taking out a filter layer, drying the filter layer to obtain glycine ethyl ester hydrochloride, simultaneously flushing the reaction kettle, heating and drying a water absorption layer, completely evaporating the absorbed water, and recovering the color of the water absorption layer to blue;
(5) Adding 360kg of water into a separation tank, stirring and mixing the water and the filtrate, standing, dissolving ethanol in the mixture, layering the water and dichloroethane, heating and distilling the ethanol aqueous solution in the separation tank until the temperature is increased to 80-85 ℃, and distilling the ethanol to enter an ethanol recovery tank;
(6) The weight of the obtained dry glycine ethyl ester hydrochloride is determined to be 270.74kg, and the yield is 96.98%; and detecting the purity of the dried glycine ethyl ester hydrochloride, wherein the content of the glycine ethyl ester hydrochloride is 98.67 percent, and the content of the glycine hydrochloride is 0.88 percent; and simultaneously detecting the recovered ethanol, dichloroethane and water, wherein the recovered ethanol contains water and trace hydrogen chloride, the content of water is less than 0.45%, the recovered dichloroethane contains water and ethanol, the content of water is 0.12%, the content of ethanol is 0.34%, the recovered water contains ethanol, and the content of ethanol is 0.39%.
Example 4
A production method of glycine ethyl ester hydrochloride comprises the following steps:
(1) Firstly putting 166.65kg of absolute ethyl alcohol into a reaction kettle, then introducing dry hydrogen chloride at the flow rate of 22.90kg/min for 4min, and firstly preparing hydrogen chloride and part of absolute ethyl alcohol into hydrogen chloride ethanol solution;
(2) Then, gradually adding 186.67kg of glycine into the hydrogen chloride ethanol solution, heating and stirring, raising the temperature to 75-80 ℃, and carrying out esterification reaction on the glycine and the hydrogen chloride ethanol solution to generate glycine ethyl ester hydrochloride;
(3) Reacting until 80-90% of glycine by weight is dissolved, adding 362.25kg of dichloroethane and 178.30kg of absolute ethyl alcohol, reacting to generate water, dichloroethane and ethyl alcohol to form a ternary system, gradually heating until the mixture is boiled, allowing the gas phase in the azeotropic system to pass through a water absorption layer, wherein the color of a water absorption silica gel bead of the water absorption layer is blue at the beginning, absorbing water by the water absorption silica gel bead of the water absorption layer, and then gradually lightening the blue color, and simultaneously condensing the dichloroethane and the ethyl alcohol downwards and refluxing the condensed water to enter a reaction kettle, so that glycine hydrochloride continuously performs esterification reaction with the ethyl alcohol to generate glycine ethyl ester hydrochloride which gradually turns to mauve until the color of the water absorption layer is not changed any more;
(4) Reducing the temperature in the reaction kettle to 60-65 ℃, transferring the reaction liquid into a crystallizing tank by heating, flushing the reaction kettle with 36.5kg of absolute ethyl alcohol, then feeding the reaction liquid into the crystallizing tank, cooling and crystallizing the reaction liquid in the crystallizing tank, filtering the reaction liquid after crystallization is complete, feeding the filtrate into a separating tank, flushing the reaction liquid with 37.2kg of absolute ethyl alcohol, then feeding the obtained product into the separating tank, taking out a filter layer, drying the filter layer to obtain glycine ethyl ester hydrochloride, simultaneously flushing the reaction kettle, heating and drying a water absorbing layer, completely evaporating out the absorbed water, and recovering the color of the water absorbing layer to blue;
(5) Adding 480kg of water into a separation tank, stirring and mixing the water and the filtrate, standing, dissolving ethanol into the mixture, layering the water and dichloroethane, heating and distilling the ethanol aqueous solution in the separation tank until the temperature is increased to 80-85 ℃, and distilling the ethanol to enter an ethanol recovery tank;
(6) The weight of the obtained dried glycine ethyl ester hydrochloride is measured to be 338.01kg, and the yield is 96.86 percent; and detecting the purity of the dried glycine ethyl ester hydrochloride, wherein the content of the glycine ethyl ester hydrochloride is 98.29 percent, and the content of the glycine hydrochloride is 0.92 percent; and simultaneously detecting the recovered ethanol, dichloroethane and water, wherein the recovered ethanol contains water and trace hydrogen chloride, the content of water is less than 0.47%, the recovered dichloroethane contains water and ethanol, the content of water is 0.14%, the content of ethanol is 0.36%, the recovered water contains ethanol, and the content of ethanol is 0.43%.
Example 5
A production method of glycine ethyl ester hydrochloride comprises the following steps:
(1) Firstly, 270.25kg of absolute ethyl alcohol is put into a reaction kettle, then dry hydrogen chloride is introduced at the flow rate of 55.08kg/min, the inflow time is 2min, and hydrogen chloride and part of absolute ethyl alcohol are prepared into hydrogen chloride ethanol solution;
(2) Then, gradually adding 225.21kg of glycine into the hydrogen chloride ethanol solution, heating and stirring, raising the temperature to 75-80 ℃, and carrying out esterification reaction on the glycine and the hydrogen chloride ethanol solution to generate glycine ethyl ester hydrochloride;
(3) Reacting until 80-90 wt% of glycine is dissolved, then adding 416.65kg of dichloroethane and 247.75kg of absolute ethanol, reacting to generate water, forming a ternary system with dichloroethane and ethanol, gradually heating until boiling, allowing the gas phase in the azeotropic system to pass through a water absorption layer, wherein the color of water absorption silica gel beads of the water absorption layer is blue at the beginning, absorbing water by the water absorption silica gel beads of the water absorption layer, gradually lightening the blue color, simultaneously condensing dichloroethane and refluxing the ethanol downwards, and then feeding the condensed water into a reaction kettle to continuously esterify glycine hydrochloride with the ethanol to generate glycine ethyl ester hydrochloride, and gradually turning to mauve until the color of the water absorption layer is not changed any more;
(4) Reducing the temperature in the reaction kettle to 60-65 ℃, transferring the reaction liquid into a crystallization tank, flushing the reaction kettle with 44.75kg of absolute ethyl alcohol, then feeding the reaction liquid into the crystallization tank, cooling and crystallizing the reaction liquid in the crystallization tank, filtering the reaction liquid after complete crystallization, feeding the filtrate into a separation tank, flushing the reaction liquid with 44.5kg of absolute ethyl alcohol, then feeding the filtrate into the separation tank, taking out a filter layer, drying the filter layer to obtain glycine ethyl ester hydrochloride, simultaneously flushing the reaction kettle, heating and drying a water absorption layer, completely evaporating the absorbed water, and recovering the color of the water absorption layer to blue;
(5) Adding 500kg of water into a separation tank, stirring and mixing the water and the filtrate, standing, dissolving ethanol in the mixture, layering the water and dichloroethane, heating and distilling the ethanol aqueous solution in the separation tank until the temperature is increased to 80-85 ℃, and distilling the ethanol to enter an ethanol recovery tank;
(6) The weight of the obtained dried glycine ethyl ester hydrochloride was determined to be 406.73kg, and the yield was 97.11%; and detecting the purity of the dried glycine ethyl ester hydrochloride, wherein the content of the glycine ethyl ester hydrochloride is 98.22 percent, and the content of the glycine hydrochloride is 0.94 percent; and simultaneously detecting the recovered ethanol, dichloroethane and water, wherein the recovered ethanol contains water and trace hydrogen chloride, the content of water is less than 0.48%, the recovered dichloroethane contains water and ethanol, the content of water is 0.18%, the content of ethanol is 0.43%, and the recovered water contains ethanol, the content of ethanol is 0.47%.
The present invention also provides an embodiment of the production apparatus used in embodiments 1 to 5, in this embodiment, as shown in fig. 1 to 6, the production apparatus includes a reaction vessel 1 with a stirring function, a crystallization vessel 2 communicated with reaction liquid outlets 1 to 6 on the reaction vessel 1, a separation vessel 3 with a stirring function communicated with a filtrate outlet 2-2 on the crystallization vessel 2, and an ethanol recovery vessel 5, a dichloroethane recovery vessel 6, and a water recovery vessel 7 correspondingly communicated with an ethanol outlet 3-2, a dichloroethane outlet 3-3, and a water outlet 3-4 of the separation vessel 3, the reaction vessel 1 is provided with a water absorbing layer 8 located on the upper portion thereof, the side surface of the water absorbing layer 8 is connected with the inner side wall of the reaction vessel 1, the reaction vessel 1 is provided with an observation window 9 for observing the color change of the water absorbing layer 8 on the wall of the water absorbing layer 8, a liquid spraying device 11 positioned on the upper part of the crystallizing tank 2 and a filter layer 10 of a filter hole connected with the bottom of the crystallizing tank in a clinging manner are arranged in the crystallizing tank 2, the upper surface of the filter layer 10 and the lowest point of a crystal outlet 2-3 on the crystallizing tank 2 are positioned in the same horizontal plane, the liquid spraying device 11 is fixedly connected with the top of the crystallizing tank 2, the liquid spraying device 11 is communicated with an ethanol recovery tank 5, an ethanol pump 19 is arranged on a pipeline of the liquid spraying device 11 to provide anhydrous ethanol for the liquid spraying device 11 to wash and crystallize, a reflux device for refluxing the ethanol is arranged in the separating tank 3, a transparent drying column 15 is arranged at a position where the ethanol outlet 3-2 of the separating tank 3 of the ethanol recovery tank 5 is communicated, the distilled ethanol can be recycled after being dried by the drying column 15, and the middle-lower part of the outer side of the reaction kettle 1, the position of the water absorbing layer 8 and the middle-lower part of the outer side of the separating tank 3 are both provided with a filter layer for recycling the distilled ethanol An electric heating device 16 for heating and warming, wherein a heat insulation layer 17 is arranged outside the electric heating device 16, the electric heating device 16 at the middle lower part outside the reaction kettle 1, the electric heating device 16 at the position of the water absorption layer 8 outside the reaction kettle 1 and the electric heating device 16 at the middle lower part outside the separation tank 3 are respectively and independently arranged, and can independently heat and influence each part; the separation tank 3 is a transparent separation tank 3, and the phenomena of extraction separation and distillation separation can be observed; in this embodiment, a temperature control device for detecting and controlling the reaction temperature in the reaction kettle is further disposed outside the reaction kettle 1, and the temperature control device is electrically connected to the electric heating device 16 at the middle lower portion outside the reaction kettle 1.
In this embodiment, as shown in fig. 1 to 4, a reaction stirring shaft of a reaction kettle 1 penetrates through the center of a water absorbing layer 8, the water absorbing layer 8 is connected in a sliding manner, the water absorbing layer 8 comprises two clamping plates with through holes connected up and down and water absorbing silica gel beads filled between the two clamping plates, cobalt chloride is added into the water absorbing silica gel beads, the diameter of the water absorbing silica gel beads is larger than the aperture of the through holes, water mixed with steam in the reaction kettle 1 can be removed, the cobalt chloride added into the water absorbing silica gel beads is blue, and the water absorbing silica gel beads have color change, so that the reaction proceeding condition can be judged according to the color change of the water absorbing layer 8, and silica gel having no adsorption effect on ethanol and dichloroethane is selected; a hydrogen chloride inlet 1-1, a glycine inlet 1-2, an ethanol inlet 1-3 and a dichloroethane inlet 1-4 on a reaction kettle 1 are circumferentially arranged on the upper portion of the reaction kettle 1 in an anticlockwise direction and are located below a water absorption layer 8, the hydrogen chloride inlet 1-1, the glycine inlet 1-2, the ethanol inlet 1-3 and the dichloroethane inlet 1-4 are arranged, a water vapor outlet 1-5 and a reaction liquid outlet 1-6 on the reaction kettle 1 are respectively located at the top and the bottom center of the reaction kettle 1, a reaction liquid outlet 1-6 on the reaction kettle 1 is communicated with a reaction liquid inlet 2-1 on a crystallization tank 2, the height of the reaction liquid outlet 1-6 is higher than that of the reaction liquid inlet 2-1, the glycine inlet 1-2, the ethanol inlet 1-3, the dichloroethane inlet 1-4 and the water vapor outlet 1-5 are all provided with a battery valve 18, and the hydrogen chloride inlet 1-1 and the crystal outlet 2-3 are all provided with sealing covers.
In this embodiment, as shown in fig. 1, 5 and 6, the reflux device includes a condensation plate 12 and an elliptical ring baffle 13, the center of the condensation plate 12 protrudes upward to form an umbrella-shaped structure, a separation stirring rod of the separation tank 3 passes through the center of the condensation plate 12 and is connected with the condensation plate 12 in a sliding manner, the separation stirring rod of the separation tank 3 passes through the elliptical ring baffle 13 and forms a through cavity hole with the elliptical ring baffle, the condensation plate 12 is fixedly connected with the top of the separation tank 3, the elliptical ring baffle 13 is obliquely arranged in the separation tank 3 and is fixedly connected with the inner wall of the separation tank 3 at the outer edge thereof, an annular groove 14 forming an inclination with the inner wall of the separation tank 3 is obliquely arranged upward at the inner edge of the elliptical ring baffle 13, and the edge of the condensation plate 12 is located above the elliptical ring baffle 13; a filtrate inlet 3-1 on the separating tank 3 is positioned below the highest point of the elliptical ring baffle 13, an ethanol outlet 3-2 on the separating tank 3 is positioned at the lowest point of the elliptical ring baffle 13, a water inlet 3-5 on the separating tank 3 is positioned below the ethanol outlet 3-2, the water inlet 3-5 is communicated with a water recovery tank 7, a water pump 20 is arranged on a pipeline of the water inlet to provide water for separating ethanol and dichloroethane, the water is used as an extractant to extract ethanol and is separated from the dichloroethane, the dichloroethane outlet 3-3 and the water outlet 3-4 on the separating tank 3 are respectively positioned at the center and the lower part of the bottom of the separating tank 3, the filtrate inlet 3-1 on the separating tank 3 is communicated with a filtrate outlet 2-2 on the crystallizing tank 2, the height of the filtrate outlet 2-2 is higher than that of the filtrate inlet 3-1, when the ethanol aqueous solution is subjected to distillation separation, the evaporated ethanol gas rises to be liquefied by the condensing plate 12 and flows to the edge of the condensing plate 12 along the condensing plate 12 to drop into the annular groove 14, the ethanol flows along the annular groove 14 towards the ethanol outlet 3-2 to flow out of the separating tank 3, the battery valves 18 are respectively arranged on the dichloroethane outlet 3-3, the filtrate outlet 2-2, the water inlet 3-5 and the water outlet 3-4, when the water pump 20 sends water to the separating tank 3, the battery valve 18 at the water inlet 3-5 is opened, and when the water pump 20 does not send water to the separating tank 3, the battery valve 18 at the water inlet 3-5 is closed.
In this embodiment, as shown in fig. 1, the drying column 15 is filled with water-absorbing silica gel beads to dry the ethanol fractionated by the separation tank 3, the electric heating device 16 is installed outside the drying column 15, the drying column 15 is provided with an air vent, the air vent is provided with a sealing cover, and the sealing cover is opened when the water-absorbing silica gel beads of the drying column 15 are dry.
The working process comprises the following steps: before feeding, battery valves 18 of a reaction liquid outlet 1-6, a water vapor outlet 1-5, a filtrate outlet 2-2, a dichloroethane outlet 3-3, an ethanol inlet 1-3, a dichloroethane inlet 1-4, a glycine inlet 1-2 and a water outlet 3-4 are all closed, sealing covers of a hydrogen chloride inlet 1-1 and a crystal outlet 2-3 are tightly covered, the battery valve 18 of the ethanol inlet 1-3 is opened and is closed after absolute ethanol is added, the sealing cover of the hydrogen chloride inlet 1-1 is opened and is closed after hydrogen chloride is added, then the battery valve 18 of the glycine inlet 1-2 is opened and is gradually fed, a reaction stirring shaft is stirred, an electric heating device 16 at the middle lower part of the outer side of a reaction kettle 1 is started for heating and heating, the battery valves 18 of the ethanol inlet 1-3 and the dichloroethane inlet 1-4 are opened for reaction for a period of time and then are closed after feeding, a reaction liquid is boiled, boiling mixed steam of dichloroethane, ethanol and water, rising the boiled mixed steam to enter a water absorption layer 8, taking away water of the mixed steam by the water absorption layer 8, liquefying, refluxing and dropping the dichloroethane and the ethanol to a reaction solution, observing the color change of the water absorption layer 8 from an observation window 9, keeping the color of the water absorption layer 8 unchanged, completing the reaction, closing an electric heating device 16 at the middle lower part outside a reaction kettle 1, opening a battery valve 18 at a reaction solution outlet 1-6 to move the reaction solution into a crystallization tank 2 for cooling and crystallization, opening a battery valve 18 at an ethanol inlet 1-3 to feed and wash the reaction kettle 1, then entering the crystallization tank 2, closing the battery valve 18 at the reaction solution outlet 1-6 and opening a battery valve 18 at a water vapor outlet 1-5, opening the electric heating device 16 at the position of the water absorption layer 8 outside the reaction kettle 1 to heat and dry the water absorption layer 8, the water absorption silica gel beads on the water absorption layer recover blue, and the battery valve 18 at the water vapor outlet 1-5 is closed after drying is finished; after the crystallization is completed, opening a battery valve 18 at a filtrate outlet 2-2, filtering to enable the filtrate to enter a separation tank 3, after the filtration is completed, conveying anhydrous ethanol by an ethanol pump 19, spraying and washing the crystals by a liquid spraying device 11, then closing the battery valve 18 at the filtrate outlet 2-2, opening a sealing cover at a crystal outlet 2-3, taking out and drying; opening a battery valve 18 of a water inlet 3-5, conveying water into a separation tank 3 by a water pump 20, then closing the battery valve 18 of the water inlet 3-5, uniformly stirring the water and a filtrate by a separation stirring rod, stopping stirring and standing, after phase separation, opening the battery valve 18 of the dichloroethane outlet 3-3, transferring the dichloroethane in the lower layer into a dichloroethane recovery tank 6, closing the battery valve 18 when the ethanol aqueous solution in the upper layer is about to go out from the battery valve 18 of the dichloroethane outlet 3-3, then heating and warming an electric heating device 16 in the middle lower part outside the separation tank 3 to separate the ethanol from the water, liquefying the ethanol steam by a condensing plate 12 and falling into an annular groove 14 along the edge, flowing and flowing the ethanol in the direction of the annular groove 14 towards an ethanol outlet 3-2, drying the ethanol into the ethanol recovery tank 5 by a drying column 15, after distillation is finished, closing an electric heating device 16 in the middle lower part outside the separation tank 3, opening an electric heating device 18 in the water outlet 3-4, transferring the water into a water recovery tank 7.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the specification describes embodiments, not every embodiment includes only a single embodiment, and such description is for clarity purposes only, and it will be understood by those skilled in the art that the specification as a whole and the embodiments may be combined as appropriate to form other embodiments as would be understood by those skilled in the art.
Claims (6)
1. A production method of glycine ethyl ester hydrochloride takes glycine as a raw material, and is characterized by comprising the following steps:
(1) Firstly, absolute ethyl alcohol which is 0.92-1.23 times of the weight of glycine is added into a reaction kettle, then dry hydrogen chloride which is 48.62-49.05% of the weight of glycine is introduced, and hydrogen chloride and partial absolute ethyl alcohol are prepared into hydrogen chloride ethanol solution;
(2) Then gradually adding glycine into the hydrogen chloride ethanol solution, heating and stirring, raising the temperature to 75-80 ℃, and carrying out esterification reaction on the glycine and the hydrogen chloride ethanol solution to generate glycine ethyl ester hydrochloride;
(3) Reacting until 80-90% of glycine by weight is dissolved, adding dichloroethane which is 1.58-2.1 times of the weight of the glycine and absolute ethyl alcohol which is 0.61-1.23 times of the weight of the glycine, gradually heating until boiling, wherein the water generated by the reaction, the dichloroethane and the ethyl alcohol form a ternary system, gradually heating until boiling, allowing a gas phase in an azeotropic system to pass through a water absorption layer, taking away water in the water absorption layer, changing the color of the water absorption layer, simultaneously condensing the dichloroethane and the ethyl alcohol downwards, refluxing the dichloroethane and the ethyl alcohol into a reaction kettle, and continuously esterifying the glycinate hydrochloride and the ethyl alcohol to generate glycine ethyl ester hydrochloride until the color of the water absorption layer is not changed or the water absorption layer is saturated;
(4) Reducing the temperature in the reaction kettle to 60-65 ℃, transferring the reaction liquid into a crystallization tank, flushing the reaction kettle with absolute ethyl alcohol accounting for 15.34-21.47% of the weight of the glycine, then feeding the reaction liquid into the crystallization tank, cooling and crystallizing the reaction liquid in the crystallization tank, filtering after complete crystallization, feeding the filtrate into a separation tank, flushing the filtrate with absolute ethyl alcohol accounting for 5.34-21.47% of the weight of the glycine, then feeding the filtrate into the separation tank, taking out a filter layer, and drying to obtain glycine ethyl ester hydrochloride;
(5) Adding water which is 2-3 times of the weight of glycine into a separation tank, stirring and mixing the water and filtrate, standing, dissolving ethanol in the filtrate, layering the water and dichloroethane, transferring the dichloroethane into a dichloroethane recovery tank, heating and distilling the ethanol aqueous solution in the separation tank, raising the temperature to 80-85 ℃, and distilling the ethanol to enter the ethanol recovery tank;
the water absorption layer is filled with water absorption silica gel beads added with cobalt chloride, the color of the water absorption silica gel beads is blue when the water absorption layer is dried, and after water absorption, the blue color gradually becomes light and gradually becomes bluish violet and purplish red.
2. The method for producing glycine ethyl ester hydrochloride according to claim 1, wherein the water-absorbing layer is dried by heating after the reaction vessel is washed clean, the absorbed water is completely evaporated, and the color of the water-absorbing layer returns to an anhydrous blue color.
3. A production apparatus for glycine ethyl ester hydrochloride according to claim 1, wherein the production apparatus comprises a reaction vessel with stirring function, a crystallization vessel communicating with a reaction liquid outlet on the reaction vessel, a separation vessel with stirring function communicating with a filtrate outlet on the crystallization vessel, and an ethanol recovery vessel, a dichloroethane recovery vessel, and a water recovery vessel communicating with an ethanol outlet, a dichloroethane outlet, and a water outlet of the separation vessel in this order from top left to bottom right, wherein the reaction vessel is provided with a water-absorbing layer on its upper portion, the side of the water-absorbing layer is connected to the inside wall of the reaction vessel, the reaction vessel is provided with an observation window for observing the color change of the water-absorbing layer on the wall of the water-absorbing layer, the crystallization vessel is provided with a liquid-spraying device on its upper portion and a filter layer closely connected to its bottom, the upper surface of the filter layer is in the same horizontal plane as the lowest point of the crystal outlet on the crystallization vessel, the liquid-spraying device is fixedly connected to the top of the crystallization vessel, the liquid-spraying device is communicated to the ethanol recovery vessel and is provided with an ethanol-heating and an electric heat-insulating layer is provided on the outside of the separation vessel.
4. The production equipment of glycine ethyl ester hydrochloride according to claim 3, wherein the reaction stirring shaft of the reaction kettle penetrates through the center of the water absorption layer, the water absorption layer is connected in a sliding manner, the water absorption layer comprises two clamping plates with through holes and water absorption silica gel beads filled between the two clamping plates, the water absorption silica gel beads are connected up and down, cobalt chloride is added into the water absorption silica gel beads, and the diameter of the water absorption silica gel beads is larger than the aperture of the through holes; chlorine hydride import, glycine import, ethanol import and dichloroethane import circumference anticlockwise on reation kettle arrange on reation kettle's upper portion and be located the below on the layer that absorbs water, and the chlorine hydride import, glycine import, ethanol import and the dichloroethane import that are provided with, last steam outlet of reation kettle, reaction liquid export are located reation kettle's top, bottom center respectively, and the last reaction liquid export of reation kettle communicates with the reaction liquid import on the crystallizer, the height that highly is higher than the reaction liquid import of reaction liquid export, all install the battery valve on reaction liquid export, glycine import, ethanol import, dichloroethane import and the steam export, all install sealed lid on chlorine hydride import, the crystal export.
5. The apparatus for producing glycine ethyl ester hydrochloride according to claim 3 wherein the refluxing device comprises a condensation plate and an elliptical ring baffle, the center of the condensation plate is protruded upwards to form an umbrella-shaped structure, the separation stirring rod of the separation tank passes through the center of the condensation plate and is connected with the condensation plate in a sliding manner, the separation stirring rod of the separation tank passes through the elliptical ring baffle and forms a through cavity hole with the elliptical ring baffle, the condensation plate is fixedly connected with the top of the separation tank, the elliptical ring baffle is obliquely arranged in the separation tank and is fixedly connected with the inner wall of the separation tank at the outer edge, the inner edge of the elliptical ring baffle is obliquely and upwards provided with an annular groove forming an oblique angle with the inner wall of the separation tank, and the edge of the condensation plate is located above the elliptical ring baffle; the filtering liquid inlet on the separating tank is positioned below the highest point of the elliptical ring baffle, the ethanol outlet on the separating tank is positioned at the lowest point of the elliptical ring baffle, the water inlet on the separating tank is positioned below the ethanol outlet, the water inlet is communicated with the water recovery tank, a water pump is arranged on a pipeline of the water inlet, the dichloroethane outlet and the water outlet on the separating tank are respectively positioned at the center and the lower part of the bottom of the separating tank, the filtering liquid inlet on the separating tank is communicated with the filtering liquid outlet on the crystallizing tank, the height of the filtering liquid outlet is higher than that of the filtering liquid inlet, and battery valves are respectively arranged on the dichloroethane outlet, the filtering liquid outlet, the water inlet and the water outlet.
6. The production equipment of glycine ethyl ester hydrochloride according to claim 3, wherein the drying column is filled with water-absorbing silica gel beads, the outer side of the drying column is provided with an electric heating device, the drying column is provided with a vent hole, and the vent hole is provided with a sealing cover.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53127412A (en) * | 1977-04-11 | 1978-11-07 | Showa Denko Kk | Preparation of glycine ethyl ester hydrochloride |
| CN108484421A (en) * | 2018-04-27 | 2018-09-04 | 江苏优普生物化学科技股份有限公司 | The improved method for preparing glycine ethyl ester hydrochloride |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53127412A (en) * | 1977-04-11 | 1978-11-07 | Showa Denko Kk | Preparation of glycine ethyl ester hydrochloride |
| CN108484421A (en) * | 2018-04-27 | 2018-09-04 | 江苏优普生物化学科技股份有限公司 | The improved method for preparing glycine ethyl ester hydrochloride |
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