A process for the preparation of glycine amide hydrochloride

Abstract

This invention discloses a method for preparing glycine amide hydrochloride, comprising adding water and a catalyst to a reaction vessel, introducing ammonia gas at 0-5°C, then adding chloroacetic acid dropwise, stirring the reaction, raising the temperature to 30-35°C after the addition is complete, introducing ammonia gas again, and continuing the reaction for 2-3 hours until the reaction is complete, removing ammonia and water, adding methanol solvent to crystallize and obtain glycine amide hydrochloride product, and then scraping off and collecting the crystals. This invention uses chloroacetic acid to generate glycine amide hydrochloride under the action of ammonia and a catalyst, and then crystallizing the product with alcohols. This avoids the use of hydrogen chloride gas or large amounts of alcohols as solvents, reducing the safety risks caused by the concentrated use of large amounts of alcohols, shortening the reaction time, improving product quality and yield, and simplifying subsequent processing. The removed ammonia is absorbed by the removed water, and then the ammonia gas is circulated for reuse, without generating wastewater, making it environmentally friendly. This invention is applicable to the preparation of glycine amide hydrochloride.

Description

Technical Field

[0001] This invention belongs to the field of pharmaceutical intermediate preparation, specifically, it relates to a method for preparing glycine hydrochloride. Background Technology

[0002] Glycine amide hydrochloride is an important intermediate, a key intermediate in the preparation of piracetam, and also used in the production of the sulfonamide drug SMPZ. It can also be used as an intermediate in other materials, possessing a very broad market. Existing technologies mainly include the following methods for preparing glycine amide hydrochloride: First, using aminoacetonitrile hydrochloride as a raw material, dry hydrogen chloride is passed through to obtain glycine amide hydrochloride. This method uses corrosive hydrogen chloride gas, which severely corrodes equipment. Second, using chloroacetyl chloride as a raw material, ammonia is passed through in an alcohol solvent for reaction. After the reaction is complete, crude glycine amide hydrochloride is obtained. This method uses expensive raw materials, is highly corrosive, and generates a large amount of ammonium chloride during production. Third, chloroacetate is first passed through ammonia at a certain positive pressure in an organic solvent, resulting in ammonolysis to produce chloroacetamide hydrochloride, which is then passed through again to obtain glycine amide hydrochloride. This method poses significant safety risks, has strict requirements for production equipment and environment, and is costly. Summary of the Invention

[0003] This invention provides a method for preparing glycine hydrochloride, which simplifies the purification process, avoids the use of hydrogen chloride gas, reduces safety risks, and simplifies subsequent treatment, does not generate wastewater, and is environmentally friendly.

[0004] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0005] A method for preparing glycine hydrochloride includes the following steps:

[0006] S1. First, add 2.5-10.0 parts by weight of catalyst into the feeder, and then use a pressure pump to pump the reaction water in the reaction water tank into the reactor until the weight of the reaction water is 180-240.

[0007] S2. Cold water is introduced into the water bath of the reactor to make the temperature inside the reactor 0-5℃;

[0008] S3. Then, 60 parts by weight of ammonia gas are introduced into the reactor, and 50 parts by weight of chloroacetic acid ester are added through the feeder.

[0009] S4. Then, control the pressure pump to extract the solution in the reactor and pump it back into the reactor, so that the solution forms a circulation and completely dissolves the chloroacetic acid ester in the feeder into the solution, and then stop the pressure pump.

[0010] S5. Operate the clutch mechanism to change the stirring crystallization attachment mechanism into stirring mode, drive the stirring crystallization attachment mechanism in the reactor to rotate in the reactor, and carry out stirring reaction.

[0011] S6. After the stirring reaction is complete, the cold water in the water bath is extracted and warm water is introduced into the water bath until the temperature inside the reactor rises to 30-35℃. Then, continue to introduce ammonia gas to maintain the temperature at 30-35℃.

[0012] S7. After reacting for 2-3 hours, heat the reactor to distill out the ammonia and reaction water inside. Then add 50 parts by weight of methanol, remove the hot water from the water bath, and introduce cold water into the water bath to cool down and crystallize, obtaining a crude product. Afterward, remove the methanol carrying impurities from the reactor.

[0013] S8. Replace the cold water in the water bath with warm water until the temperature inside the reactor rises to 30-35℃. Then, introduce 50 parts by weight of methanol into the reactor. The crude product dissolves in the methanol. Then, perform a cooling operation to allow the crude product to recrystallize and obtain glycine hydrochloride crystals.

[0014] S9. Extract methanol from the reactor, operate the clutch mechanism to change the stirring crystallization attachment mechanism to a scraping crystal form, drive the stirring crystallization attachment mechanism to move, causing the glycine hydrochloride crystals attached to the inner wall of the reactor and the stirring crystallization attachment mechanism to fall off. Operate the clutch mechanism again to change the stirring crystallization attachment mechanism to a stirring form, drive the stirring crystallization attachment mechanism to rotate, so that the glycine hydrochloride crystals in the reactor are gradually transported to the discharge joint and collected by the collection box.

[0015] Furthermore, the water bath includes a box body supported on the ground at the lower end by multiple support legs, the upper end of the box body is in an open state, and water inlet connectors and water outlet connectors are respectively constructed on two opposite side walls of the box body, and water inlet main valves and water outlet main valves are respectively installed on the water inlet connectors and water outlet connectors.

[0016] Furthermore, the reactor is located in a water bath, the stirring crystallization attachment mechanism is located in the reaction chamber of the reactor, and there are two clutch mechanisms, which are located at the two axial ends of the horizontal reactor body, and each clutch mechanism is constructed on the same side end of the horizontal reactor body and the stirring crystallization attachment mechanism.

[0017] Furthermore, the reactor includes a cylindrical horizontal vessel body, with end caps detachably connected to each axial end of the horizontal vessel body. A steam outlet and a discharge outlet are respectively constructed at the upper and lower ends of the horizontal vessel body. One end of the connecting bend is connected to the lower end of the horizontal vessel body, and the other end of the connecting bend is connected to the outside through a stirring crystallization attachment mechanism.

[0018] Furthermore, the stirring crystallization attachment mechanism includes an assembly shaft, a first helical blade, and a second helical blade coaxially assembled in the horizontal reactor body. The first and second helical blades have the same structure, both extending helically along the axial direction of the assembly shaft. Each end of the second helical blade is connected to a corresponding end cap via a conical spring. Both ends of the assembly shaft extend out of the horizontal reactor body through corresponding end caps, and the assembly shaft is rotatably connected to both end caps. The first helical blade is fixedly connected to the assembly shaft, and the second helical blade is movably sleeved outside the assembly shaft. A transmission wheel is assembled at one end of the assembly shaft, and the transmission wheel is driven to rotate the assembly shaft.

[0019] Furthermore, the assembly shaft has a supply and discharge channel that coincides with its axis. The supply and discharge channel extends from one end of the assembly shaft to the other end, and the connecting bend is rotatably mounted on the end of the assembly shaft away from the transmission wheel. The connecting bend is connected to the supply and discharge channel, and a supply and discharge valve is installed on the connecting bend.

[0020] Furthermore, multiple gas supply channels are provided on the assembly shaft, each gas supply channel extending axially along the assembly shaft. The portion of each gas supply channel located inside the horizontal vessel body is connected to the reaction chamber through multiple gas outlets, and these gas outlets are spaced apart along the assembly shaft axially. The portion of each gas supply channel located outside the horizontal vessel body is connected to the outside through a through hole on the assembly shaft. A distribution sleeve is rotatably fitted on the assembly shaft at the location of the through hole. The distribution sleeve is equipped with a gas supply connector, which is connected to the reaction chamber through the distribution sleeve, the through hole, the gas supply channel, and the gas outlet.

[0021] Furthermore, annular fixing seats are fixedly connected to both ends of the second helical blade, the large-diameter end of each conical spring is installed on the corresponding annular fixing seat, and the small-diameter end of the conical spring is connected to an adapter seat, which is rotatably connected to the corresponding end cover.

[0022] Furthermore, the clutch mechanism includes an internal gear ring, a movable clutch component, and a transmission gear arranged sequentially outward along the axis of the assembly shaft. The internal gear ring is installed on the outside of the end cover, the transmission gear is installed at the end of the assembly shaft, and the movable clutch component is sleeved on the outside of the assembly shaft.

[0023] Furthermore, the movable clutch includes a clutch gear ring that coincides with the axis of the internal gear ring and the transmission gear. Internal gear teeth are uniformly formed along the circumference of the inner peripheral wall of the clutch gear ring, and external gear teeth are uniformly formed along the circumference of the outer peripheral wall of the clutch gear ring. The clutch gear ring is connected to a rotating ring via two connecting arms. The rotating ring is rotatably connected within an annular groove of the connecting ring, and the axes of the rotating ring, the connecting ring, and the clutch gear ring coincide. Guide posts are spaced apart on the adapter seat, and each guide post is aligned with the axis of the assembly shaft. The lever passes through the clutch gear ring, and the guide post is slidably connected to the clutch gear ring. The lower end of the operating lever is hinged to the upper end of the connecting ring. When the inner gear teeth of the clutch gear ring mesh with the transmission gear, the stirring crystallization attachment mechanism changes to a stirring mode, and when the assembly shaft is driven to rotate, the first and second helical blades rotate synchronously. When the outer gear teeth of the clutch gear ring mesh with the inner gear ring, the stirring crystallization attachment mechanism changes to a scraping mode. The first helical blade rotates with the assembly shaft, while the second helical blade is indirectly fixedly connected to the end cover through a conical spring.

[0024] The technological advancements achieved by this invention compared to existing technologies, due to the aforementioned structure, are as follows: This invention uses chloroacetic acid ester to generate glycine hydrochloride under the action of ammonia and a catalyst. The product is then crystallized from methanol, and the resulting product is recrystallized to improve purity. This avoids the use of hydrogen chloride gas or large amounts of alcohols as solvents, reduces the safety risks caused by the concentrated use of large amounts of alcohols, shortens the reaction time, and the released ammonia is absorbed by the released water and then recycled with ammonia gas, thus producing no wastewater and being environmentally friendly. Furthermore, the stirring crystallization attachment mechanism of the present invention has two forms: stirring mode and crystal scraping mode. During the reaction process, the stirring crystallization attachment mechanism is switched to stirring mode by a clutch mechanism. In this way, when the stirring crystallization attachment mechanism is driven to operate, it stirs the solution in the reaction vessel, thereby making the mixing and reaction more complete and faster. Since glycine hydrochloride crystals have an adhesion property, and the purity of crystals attached to the surface of an object is higher than that of non-attached crystals, the present invention increases the adhesion area of ​​crystals by using a stirring crystallization attachment mechanism and a reaction vessel. That is, during the crystallization process, crystals will gradually adhere to the inner wall of the reaction vessel and the surface of the stirring crystallization attachment mechanism, thereby improving the purity of crystals. After recrystallization is complete and methanol is completely removed from the reactor, the present invention switches the stirring crystallization attachment mechanism to a scraping crystal mode via a clutch mechanism. This drives the stirring crystallization attachment mechanism to rotate, scraping off the crystals attached to the inner wall of the reactor and itself. The crystals detach from their attachments and are gradually transported by the stirring crystallization attachment mechanism to the discharge connector, where they are then collected by a collection box. This improves product quality and yield while simplifying subsequent processing and making operation convenient. Attached Figure Description

[0025] The accompanying drawings are provided to further illustrate the invention and form part of the specification. They are used together with the embodiments of the invention to explain the invention and do not constitute a limitation thereof.

[0026] In the attached diagram:

[0027] Figure 1 This is a process flow diagram of an embodiment of the present invention;

[0028] Figure 2 This is a schematic diagram of the assembly of the reactor and water bath in an embodiment of the present invention;

[0029] Figure 3 This is a schematic diagram of the water bath in the reactor according to an embodiment of the present invention;

[0030] Figure 4 This is a schematic diagram of the structure of the reaction vessel in the reactor of an embodiment of the present invention;

[0031] Figure 5 This is an axial structural cross-sectional view of the reactor in an embodiment of the present invention;

[0032] Figure 6 for Figure 5 Enlarged view of the structure at part A in the middle;

[0033] Figure 7 for Figure 5 Enlarged view of the structure of part B in the middle;

[0034] Figure 8 This is a schematic diagram of the connection between the two clutch mechanisms and the stirring crystallization attachment mechanism in an embodiment of the present invention;

[0035] Figure 9 This is a partial structural schematic diagram of the stirring-type crystallization adhesion mechanism according to an embodiment of the present invention;

[0036] Figure 10 This is a front view of the structure connecting the assembly shaft and the first spiral blade in the stirring crystallization adhesion mechanism of an embodiment of the present invention;

[0037] Figure 11 This is a front view of the structure in the stirring crystallization attachment mechanism of this invention, in which the second helical blade is connected to the adapter seat via a conical spring;

[0038] Figure 12 This is a schematic diagram of the structure of the present invention in which the first helical blade gradually approaches the second helical blade as the assembly shaft rotates when the stirring crystallization attachment mechanism is converted into a crystal scraping form by the clutch mechanism.

[0039] Figure 13 This is a schematic diagram of the structure in an embodiment of the present invention where the clutch mechanism is connected to one end of the assembly shaft;

[0040] Figure 14 This is a schematic diagram of the disassembled clutch mechanism according to an embodiment of the present invention.

[0041] Components labeled: 100-Water bath, 101-Battery body, 102-Inlet connector, 103-Outlet connector, 104-Main inlet valve, 105-Main outlet valve, 106-Support leg, 107-Connecting seat, 108-First limiting rod, 109-Second limiting rod, 200-Reaction vessel, 201-Horizontal vessel body, 202-End cover, 203-Discharge connector, 204-Discharge valve, 205-Steam outlet connector, 206-Connecting elbow, 207-Supply and discharge valve, 208-Reaction chamber, 300-Stirring crystallization adhesion mechanism, 301-Assembly shaft, 302-Drive wheel, 303-Supply and discharge channel, 304-Steam supply channel, 305-Guide hole, 306-Steam outlet, 307-Second limiting rod 308-Second helical blade, 309-Annular fixed seat, 310-Conical spring, 311-Adapter seat, 400-Clutch mechanism, 401-Fixed disc, 402-Internal gear ring, 403-Clutch gear ring, 404-Internal gear tooth, 405-External gear tooth, 406-Connecting arm, 407-Rotating ring, 408-Guide post, 409-Guide sleeve, 410-Connecting ring, 411-Annular groove, 412-Transmission gear, 413-Limiting disc, 414-Operating lever, 500-Connecting pipe, 501-First connector, 502-Second connector, 503-First valve body, 504-Second valve body, 600-Feeder, 700-Distribution sleeve, 701-Air supply connector. Detailed Implementation

[0042] The preferred embodiments of the present invention will now be described with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are for illustrative and explanatory purposes only and are not intended to limit the scope of the invention.

[0043] This invention discloses a method for preparing glycine amide hydrochloride, such as... Figure 1-14 As shown, it includes the following steps:

[0044] S1. First, add 2.5-10.0 parts by weight of catalyst into feeder 600, and then pump the reaction water in the reaction water tank into the reactor 200 of the reactor using a pressure pump until the weight of reaction water is 180-240.

[0045] S2. Cold water is introduced into the water bath 100 of the reactor to make the temperature inside the reactor 200 0-5℃;

[0046] S3. Then, 60 parts by weight of ammonia gas are introduced into the reactor 200, and 50 parts by weight of chloroacetic acid ester are added through the feeder 600.

[0047] S4. Then, control the pressure pump to extract the solution in the reactor 200 and pump it back into the reactor 200, so that the solution forms a circulation and completely dissolves the chloroacetic acid ester in the feeder 600 into the solution, and then stop the pressure pump.

[0048] S5. Operate the clutch mechanism 400 to change the stirring crystallization attachment mechanism 300 into stirring mode, drive the stirring crystallization attachment mechanism 300 in the reactor 200 to rotate in the reactor 200 to carry out stirring reaction;

[0049] S6. After the stirring reaction is completed, the cold water in the water bath 100 is extracted and warm water is introduced into the water bath 100 until the temperature in the reaction vessel 200 rises to 30-35℃. Continue to introduce ammonia gas and maintain the temperature at 30-35℃.

[0050] S7. After reacting for 2-3 hours, heat the reactor 200 to distill out the ammonia and reaction water inside. Then add 50 parts by weight of methanol, remove the hot water from the water bath 100, and introduce cold water into the water bath 100 to cool down and crystallize, obtaining a crude product. Afterward, remove the methanol carrying impurities from the reactor 200.

[0051] S8. Replace the cold water in the water bath 100 with warm water until the temperature in the reaction vessel 200 rises to 30-35℃. Then, introduce 50 parts by weight of methanol into the reaction vessel 200. The crude product dissolves in the methanol. Then, perform a cooling operation to allow the crude product to recrystallize and obtain glycine hydrochloride crystals.

[0052] S9. Extract methanol from reactor 200, operate clutch mechanism 400 to change the stirring crystallization attachment mechanism 300 to crystal scraping mode, drive the stirring crystallization attachment mechanism 300 to move, so that the glycine hydrochloride crystals attached to the inner wall of reactor 200 and the stirring crystallization attachment mechanism 300 fall off. Operate clutch mechanism 400 again to change the stirring crystallization attachment mechanism 300 to stirring mode, drive the stirring crystallization attachment mechanism 300 to rotate, so that the glycine hydrochloride crystals in reactor 200 are gradually transported to discharge joint 203 and collected by collection box.

[0053] The working principle and advantages of this invention are as follows: This invention uses chloroacetic acid ester to generate glycine hydrochloride under the action of ammonia and catalyst. The product is obtained by crystallization with methanol, and the obtained product is recrystallized to improve the purity. This avoids the use of hydrogen chloride gas or a large amount of alcohol as a solvent, reduces the safety risks caused by the concentrated use of a large amount of alcohol, shortens the reaction time, and the ammonia released is absorbed by the released water. Then, ammonia gas is circulated and reused, without generating wastewater, which is environmentally friendly. Furthermore, the stirring crystallization attachment mechanism 300 of the present invention has two forms: stirring form and crystal scraping form. During the reaction process, the stirring crystallization attachment mechanism 300 is switched to stirring form by the clutch mechanism 400. In this way, when the stirring crystallization attachment mechanism 300 is driven to operate, it stirs the solution in the reaction vessel 200, thereby making the mixing and reaction more complete and faster. Since glycine hydrochloride crystals have an adhesion property, and the purity of crystals attached to the surface of an object is higher than that of non-attached crystals, the present invention increases the adhesion area of ​​crystals by using the stirring crystallization attachment mechanism 300 and the reaction vessel 200. That is, during the crystallization process, crystals will gradually adhere to the inner wall of the reaction vessel 200 and the surface of the stirring crystallization attachment mechanism 300, thereby improving the purity of crystals. After recrystallization is complete and methanol is completely removed from the reactor 200, the present invention switches the stirring crystallization attachment mechanism 300 to a crystal scraping mode via the clutch mechanism 400, driving the stirring crystallization attachment mechanism 300 to rotate. The stirring crystallization attachment mechanism 300 scrapes off the crystals attached to the inner wall of the reactor 200 and itself. The crystals detach from the attachment and are gradually transported by the stirring crystallization attachment mechanism 300 to the discharge connector 203, and then collected by the collection box. This improves product quality and yield while simplifying subsequent processing and making operation convenient.

[0054] As a preferred embodiment of the present invention, such as Figure 2 , 3 As shown, the water bath 100 includes a body 101, with multiple support legs 106 fixed to the lower end of the body 101. These support legs 106 support the body 101 on the ground, and the upper end of the body 101 is in an open state. In this embodiment, an inlet connector 102 and an outlet connector 103 are respectively constructed on two opposite side walls of the body 101. An inlet main valve 104 and an outlet main valve 105 are respectively installed on the inlet connector 102 and the outlet connector 103. Furthermore, in this embodiment, the reaction vessel 200 is placed inside the water bath 100. Cold water or warm water is supplied to the water bath 100 through the inlet connector 102, thereby achieving the purpose of water bathing the solution in the reaction vessel 200; the cold water or warm water in the water bath 100 can be discharged through the outlet connector 103 to replace the water bath water at the corresponding temperature.

[0055] As a preferred embodiment of the present invention, such as Figure 4 ,5 As shown, the reactor 200 has a reaction chamber 208, and the stirring crystallization attachment mechanism 300 is disposed within the reaction chamber 208. In this embodiment, there are two clutch mechanisms 400, which are respectively disposed at both axial ends of the horizontal reactor body 201, and each clutch mechanism 400 is constructed on the same side end of the horizontal reactor body 201 and the stirring crystallization attachment mechanism 300. Specifically, the reactor 200 includes a horizontal reactor body 201, a connecting bend 206, and two end caps 202. The horizontal reactor body 201 has a cylindrical structure, and the two end caps 202 are respectively disposed at both axial ends of the horizontal reactor body 201, and each end cap 202 is detachably connected to the corresponding end of the horizontal reactor body 201. A steam outlet 205 and a discharge outlet 203 are respectively constructed at the upper and lower ends of the horizontal reactor body 201, and a discharge valve 204 is installed on the discharge outlet 203. The steam outlet connector 205 can be connected to two pipelines. One pipeline is used to collect the distilled ammonia and reaction water; the other pipeline is connected to the ammonia tank through a dryer, and the ammonia tank is connected to the reaction chamber 208 of the reactor 200 through a gas booster pump, thereby realizing the circulation of ammonia between the reaction chamber 208 and the ammonia tank. In this embodiment, one end of the connecting bend 206 is connected to the lower end of the horizontal reactor body 201, and the other end of the connecting bend 206 is connected to the outside through the stirring crystallization attachment mechanism 300. In this embodiment, all components except ammonia are supplied to the connecting bend 206 through the stirring crystallization attachment mechanism 300, and then enter the reaction chamber 208 through the connecting bend 206. Moreover, after coarse crystallization and recrystallization are completed, the methanol in the reaction chamber 208 is extracted. Specifically, the methanol enters the stirring crystallization attachment mechanism 300 through the connecting bend 206, is then extracted by a pressure pump, and enters the recovery tank for subsequent distillation to remove impurities and obtain methanol again.

[0056] As a preferred embodiment of the present invention, such as Figure 8-11As shown, the stirring-type crystallization attachment mechanism 300 includes an assembly shaft 301, a first helical blade 307, and a second helical blade 308. The assembly shaft 301, the first helical blade 307, and the second helical blade 308 are all assembled inside a horizontal vessel body 201, and all three coincide with the axis of the horizontal vessel body 201. In this embodiment, the first helical blade 307 and the second helical blade 308 have the same structure, both extending helically along the axial direction of the assembly shaft 301. Conical springs 310 are connected to both ends of the second helical blade 308, and each conical spring 310 is connected to a corresponding end cap 202. In this embodiment, both ends of the assembly shaft 301 pass through the corresponding end caps 202 and extend out of the horizontal vessel body 201. The assembly shaft 301 is rotatably connected to the two end caps 202. The first helical blade 307 is fixedly connected to the assembly shaft 301, and the second helical blade 308 is movably fitted outside the assembly shaft 301. In this embodiment, a transmission wheel 302 is mounted at one end of the assembly shaft 301. This transmission wheel 302 is driven to rotate the assembly shaft 301. Specifically, the transmission wheel 302 is located outside the water bath 100. A forward and reverse motor is also provided outside the water bath 100. A drive wheel is mounted on the output shaft of the forward and reverse motor. The drive wheel and the transmission wheel 302 are connected by a transmission belt. In this embodiment, a clutch mechanism 400 is used to control the connection or disengagement of the first spiral blade 307 and the second spiral blade 308. When the first spiral blade 307 and the second spiral blade 308 are connected, the stirring crystallization attachment mechanism 300 is in stirring mode. When the first spiral blade 307 and the second spiral blade 308 are disengaged, the stirring crystallization attachment mechanism 300 is in scraping mode. Furthermore, when the stirring-type crystallization attachment mechanism 300 is in stirring mode and is in the crystallization process, the assembly shaft 301 is slowly driven to rotate. This causes the assembly shaft 301 to drive the first spiral blade 307 and the second spiral blade 308 to rotate slowly and synchronously. This allows the crystals to gradually adhere to the inner wall of the reactor 200, the surface of the first spiral blade 307, the surface of the second spiral blade 308, and the circumferential surface of the assembly shaft 301, thereby improving the efficiency and purity of crystallization. When the first spiral blade 307 and the second spiral blade 308 disengage, the assembly shaft 301 is driven to rotate, causing the assembly shaft 301 to drive the first spiral blade 307 to rotate. At this time, the second spiral blade 308 does not rotate. During the rotation of the first spiral blade 307, its relative position to the second spiral blade 308 changes from... Figure 5 The position shown gradually changes Figure 12As shown, the second helical blade 308 rotates relative to the assembly shaft 301, and the second helical blade 308 scrapes away crystals from the rotating assembly shaft 301. When the first helical blade 307 approaches and contacts the second helical blade 308, they rotate relative to each other, and under the action of friction, the crystals on the corresponding surfaces of the first helical blade 307 and the second helical blade 308 are scraped off. Furthermore, after the first helical blade 307 and the second helical blade 308 come into contact, the first helical blade 307 continues to apply axial pressure to the second helical blade 308. At this time, the second helical blade 308 undergoes a corresponding axial displacement, causing the two conical springs 310 to undergo corresponding elastic deformation to accommodate the axial displacement of the second helical blade 308. After the crystals on one side of the first helical blade 307 and the second helical blade 308 are scraped off, the assembly shaft 301 is driven to rotate in the opposite direction to scrape away the crystals on the other side of the first helical blade 307 and the second helical blade 308. In this embodiment, when the first helical blade 307 rotates in both forward and reverse directions, it scrapes away the crystals on the inner circumferential wall of the reactor 200. After the scraping is completed, the clutch mechanism 400 switches the stirring crystal attachment mechanism 300 to stirring mode, and controls the assembly shaft 301 to rotate, so that the first helical blade 307 and the second helical blade 308 gradually transport the scraped crystals to the discharge joint 203, so as to collect the crystals in the collection box. In this embodiment, during the scraping operation, the drive motor can also be controlled to rotate intermittently in both directions to simultaneously complete the scraping operation on both sides of the first helical blade 307 and the two sides of the second helical blade 308, thereby improving the scraping efficiency. Furthermore, the reciprocating motion of the second helical blade 308 can effectively drive the conical spring 310 to reciprocate, thereby causing the crystals on the conical spring 310 to fall off quickly.

[0057] As a preferred embodiment of the present invention, such as Figure 5 As shown, the assembly shaft 301 has a supply and discharge channel 303, which coincides with the axis of the assembly shaft 301 and extends from one end of the assembly shaft 301 to the other end. In this embodiment, the connecting bend 206 is rotatably mounted on the end of the assembly shaft 301 away from the drive wheel 302. The connecting bend 206 communicates with the supply and discharge channel 303, and a supply and discharge valve 207 is installed on the connecting bend 206. Figure 2As shown, in this embodiment, a connecting pipe 500 is rotatably connected to one end of the assembly shaft 301 near the transmission wheel 302. A first connector 501 and a second connector 502 are constructed on the connecting pipe 500. A first valve body 503 and a second valve body 504 are respectively installed on the first connector 501 and the second connector 502. The first connector 501 is connected to the outlet of the pressure pump, and the second connector 502 is connected to the inlet of the pressure pump. In this embodiment, the feeder 600 is installed on the connecting pipe 500. A feeding valve is installed at the connection point between the feeder 600 and the connecting pipe 500. When feeding is required, the feeding valve is first closed, then a predetermined amount of component is added into the feeder 600, and finally the feeding valve is opened.

[0058] As a preferred embodiment of the present invention, such as Figure 5-7 As shown, multiple gas supply channels 304 are provided on the assembly shaft 301. Each gas supply channel 304 extends axially along the assembly shaft 301, and the portion of each gas supply channel 304 located inside the horizontal vessel body 201 is connected to the reaction chamber 208 through multiple gas outlets 306. These gas outlets 306 are spaced apart along the assembly shaft 301. The portion of each gas supply channel 304 located outside the horizontal vessel body 201 is connected to a through hole 305. The through hole 305 is located on the assembly shaft 301 and is used to connect the gas supply channel 304 to the outside. In this embodiment, a distribution sleeve 700 is rotatably mounted on the assembly shaft 301 at the location of the through hole 305. The distribution sleeve 700 has a gas supply connector 701, which communicates with the reaction chamber 208 through the distribution sleeve 700, the through hole 305, the gas supply channel 304, and the gas outlet 306. Furthermore, the gas supply connector 701 is connected to the ammonia tank via a dryer. The working principle of this embodiment is as follows: Ammonia is added by simultaneously introducing it into multiple gas supply channels 304, and then into the reaction chamber 208 through each gas outlet 306. During this process, the assembly shaft 301 is driven, allowing the ammonia to uniformly enter all areas of the reaction chamber 208 and fully react with the reaction water and other components.

[0059] As a preferred embodiment of the present invention, such as Figure 8-14As shown, annular fixing seats 309 are fixedly connected to both ends of the second helical blade 308. The large-diameter end of each conical spring 310 is mounted on the corresponding annular fixing seat 309, and the small-diameter end of the conical spring 310 is connected to an adapter seat 311, wherein the adapter seat 311 is rotatably connected to the corresponding end cover 202. The specific structure of the clutch mechanism 400 in this embodiment is as follows: the clutch mechanism 400 includes an internal gear ring 402, a movable clutch component, and a transmission gear 412. The internal gear ring 402, the movable clutch component, and the transmission gear 412 are arranged outward along the axis of the assembly shaft 301. The internal gear ring 402 is mounted on the outside of the end cover 202, the transmission gear 412 is mounted on the end of the assembly shaft 301, and the movable clutch component is sleeved on the outside of the assembly shaft 301. In this embodiment, the internal gear ring 402 is coaxially welded to the fixed disk 401, and the fixed disk 401 is located on the side of the internal gear ring 402 near the end cover 202. The fixed disk 401 is connected to the outside of the end cover 202 by multiple bolts. A limiting disk 413 is coaxially constructed on the side of the transmission gear 412 away from the end cover 202. In this embodiment, both the fixed disk 401 and the limiting disk 413 are used to limit the displacement of the movable clutch, preventing the movable clutch from disengaging from the internal gear ring 402 after engagement, or from disengaging from the transmission gear 412 after engagement. The movable clutch in this embodiment is specifically structured as follows: the movable clutch includes a clutch gear ring 403 and an operating lever 414. The axes of the clutch gear ring 403, the internal gear ring 402, and the transmission gear 412 coincide. Internal gear teeth 404 are uniformly arranged circumferentially on the inner peripheral wall of the clutch gear ring 403, and external gear teeth 405 are uniformly arranged circumferentially on the outer peripheral wall of the clutch gear ring 403. In this embodiment, the clutch gear ring 403 is connected to a rotating ring 407 via two connecting arms 406. The rotating ring 407 is rotatably connected within the annular groove 411 of the connecting ring 410, and the axes of the rotating ring 407, the connecting ring 410, and the clutch gear ring 403 coincide. In this embodiment, guide posts 408 are spaced apart on the adapter 311, and guide sleeves 409 are constructed on the clutch gear ring 403 at positions corresponding to the guide posts 408. Each guide post 408 passes through the corresponding guide sleeve 409 along the axial direction of the assembly shaft 301 and extends out of the clutch gear ring 403, and the guide post 408 and guide sleeve 409 are slidably connected. In this embodiment, the lower end of the operating lever 414 is hinged to the upper end of the connecting ring 410, and connecting seats 107 are respectively constructed on both sides of the upper end of the water bath 100. A first limiting rod 108 and a second limiting rod 109 are spaced apart on the connecting seats 107 along the axial direction of the assembly shaft 301.When the operator moves the control lever 414 to contact the first limiting lever 108, the operator continues to move the control lever 414, so that the lower end of the control lever 414 drives the clutch gear ring 403 to move toward the inner gear ring 402 through the connecting ring 410 until the clutch gear ring 403 and the inner gear ring 402 are engaged. At this time, the stirring crystallization attachment mechanism 300 is in the crystal scraping mode, that is, the assembly shaft 301 is in the free state, and the end adapter 311 of the conical spring 310 is connected to the end cover 202 through the engaged inner gear ring 402 and the clutch gear ring 403. When the operator moves the control lever 414 to contact the second limiting lever 109, and continues to move the control lever 414, the lower end of the control lever 414 drives the clutch gear ring 403 to move toward the transmission gear 412 through the connecting ring 410 until the clutch gear ring 403 meshes with the transmission gear 412. At this time, the stirring crystallization adhesion mechanism 300 is in stirring mode, that is, the assembly shaft 301 is connected to the adapter seat 311 through the engagement of the clutch gear ring 403 of the transmission gear 412. In this way, as the adapter seat 311 rotates with the assembly shaft 301, it drives the second spiral blade 308 to rotate through the conical spring 310. At the same time, the first spiral blade 307 rotates synchronously with the assembly shaft 301.

[0060] In this embodiment, 200 parts by weight of reaction water and 5 parts by weight of catalyst were added to reactor 200. Ammonia gas (60 parts by weight) was introduced at 0-5°C, followed by 50 parts by weight of methyl chloroacetate, and the mixture was kept at this temperature for 1 hour. The temperature was slowly increased to 30°C, and ammonia gas was continued to be introduced, maintaining the temperature between 30-35°C. The reaction was carried out for 2 hours, and samples were taken for testing. The residue of the raw materials was less than 0.5%. After the reaction was complete, the ammonia water was distilled off and recovered. 50 parts by weight of methanol were added, and the mixture was cooled, crystallized, and filtered to obtain 42 parts by weight of crude glycine hydrochloride. The crude product was recrystallized from 50 parts by weight of methanol to obtain 40 parts by weight of the final product, with a melting point of 201-204°C, a purity greater than 99.5%, and a yield of 78.59%.

[0061] In this embodiment, 200 parts by weight of reaction water and 2.5 parts by weight of catalyst were added to reactor 200. Ammonia gas (60 parts by weight) was introduced at 0-5°C, followed by 50 parts by weight of methyl chloroacetate, and the mixture was kept at this temperature for 1 hour. The temperature was slowly increased to 30°C, and ammonia gas was continued to be introduced, maintaining the temperature between 30-35°C. The reaction was carried out for 4.5 hours. Samples were taken for testing, and the residual raw material was less than 0.5%. After the reaction was complete, the ammonia water was distilled off and recovered. 50 parts by weight of methanol were added, and the mixture was cooled, crystallized, and filtered to obtain 36 parts by weight of crude glycine hydrochloride. The crude product was recrystallized from 50 parts by weight of methanol to obtain a product with a melting point of 198-203°C, a purity greater than 98%, and a yield of 63.65%.

[0062] In this embodiment, 200 parts by weight of reaction water and 10 parts by weight of catalyst were added to reactor 200. Ammonia gas (60 parts by weight) was introduced at 0-5°C, followed by 50 parts by weight of methyl chloroacetate, and the mixture was kept at this temperature for 1 hour. The temperature was slowly increased to 30°C, and ammonia gas was continued to be introduced, maintaining the temperature between 30-35°C. The reaction was carried out for 2 hours, and samples were taken for testing. The residue of the raw materials was less than 0.5%. After the reaction was complete, the ammonia water was distilled off and recovered. 50 parts by weight of methanol was added, and the mixture was cooled, crystallized, and filtered to obtain a crude glycine hydrochloride product (41.6 parts by weight). The crude product was recrystallized from the crude product with 50 parts by weight of methanol to obtain a product (39.4 parts by weight), with a melting point of 201-203°C, a purity greater than 99.5%, and a yield of 77.4%.

[0063] The catalyst of this invention is ammonium carbonate, and the chloroacetic acid ester is methyl chloroacetate or ethyl chloroacetate.

[0064] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the claims of the present invention.

Claims

1. A method for preparing glycine amide hydrochloride, characterized in that, Includes the following steps: S1. First, add 2.5-10.0 parts by weight of catalyst into the feeder, and then use a pressure pump to pump the reaction water in the reaction water tank into the reactor until the weight of the reaction water is 180-240. S2. Cold water is introduced into the water bath of the reactor to make the temperature inside the reactor 0-5℃; S3. Then, 60 parts by weight of ammonia gas are introduced into the reactor, and 50 parts by weight of chloroacetic acid ester are added through the feeder. S4. Then, control the pressure pump to extract the solution in the reactor and pump it back into the reactor, so that the solution forms a circulation and completely dissolves the chloroacetic acid ester in the feeder into the solution, and then stop the pressure pump. S5. Operate the clutch mechanism to change the stirring crystallization attachment mechanism into stirring mode, drive the stirring crystallization attachment mechanism in the reactor to rotate in the reactor, and carry out stirring reaction. S6. After the stirring reaction is complete, the cold water in the water bath is extracted and warm water is introduced into the water bath until the temperature inside the reactor rises to 30-35℃. Then, continue to introduce ammonia gas to maintain the temperature at 30-35℃. S7. After reacting for 2-3 hours, heat the reactor to distill out the ammonia and reaction water inside. Then add 50 parts by weight of methanol, remove the hot water from the water bath, and introduce cold water into the water bath to cool down and crystallize, obtaining a crude product. Afterward, remove the methanol carrying impurities from the reactor. S8. Replace the cold water in the water bath with warm water until the temperature inside the reactor rises to 30-35℃. Then, introduce 50 parts by weight of methanol into the reactor. The crude product dissolves in the methanol. Then, perform a cooling operation to allow the crude product to recrystallize and obtain glycine hydrochloride crystals. S9. Extract methanol from the reactor, operate the clutch mechanism to change the stirring crystallization attachment mechanism to the crystal scraping mode, drive the stirring crystallization attachment mechanism to move, so that the glycine hydrochloride crystals attached to the inner wall of the reactor and the stirring crystallization attachment mechanism fall off. Operate the clutch mechanism again to change the stirring crystallization attachment mechanism to the stirring mode, drive the stirring crystallization attachment mechanism to rotate, so that the glycine hydrochloride crystals in the reactor are gradually transported to the discharge joint and collected by the collection box. The reactor is set in a water bath, the stirring crystallization attachment mechanism is set in the reaction chamber of the reactor, and there are two clutch mechanisms. The two clutch mechanisms are set at the two ends of the horizontal reactor body, and each clutch mechanism is constructed on the same side end of the horizontal reactor body and the stirring crystallization attachment mechanism. The reactor includes a cylindrical horizontal vessel body, with end caps detachably connected to each axial end of the horizontal vessel body. A steam outlet and a discharge outlet are respectively constructed at the upper and lower ends of the horizontal vessel body. One end of the connecting bend is connected to the lower end of the horizontal vessel body, and the other end of the connecting bend is connected to the outside through a stirring crystallization attachment mechanism. The stirring crystallization attachment mechanism includes an assembly shaft, a first helical blade, and a second helical blade coaxially assembled in a horizontal reactor body. The first and second helical blades have the same structure, both extending helically along the axial direction of the assembly shaft. Each end of the second helical blade is connected to a corresponding end cap via a conical spring. Both ends of the assembly shaft extend out of the horizontal reactor body through corresponding end caps, and the assembly shaft is rotatably connected to both end caps. The first helical blade is fixedly connected to the assembly shaft, and the second helical blade is movably sleeved outside the assembly shaft. A transmission wheel is assembled at one end of the assembly shaft, and the transmission wheel is driven to rotate the assembly shaft.

2. The method for preparing glycine hydrochloride according to claim 1, characterized in that: The water bath includes a box body supported on the ground by multiple support legs at the lower end. The upper end of the box body is in an open state. Water inlet and water outlet are respectively constructed on two opposite side walls of the box body. Water inlet valve and water outlet valve are respectively installed on the water inlet and water outlet.

3. The method for preparing glycine hydrochloride according to claim 1, characterized in that: The assembly shaft has a supply and discharge channel that coincides with its axis. The supply and discharge channel extends from one end of the assembly shaft to the other end. The connecting bend is rotatably mounted on the end of the assembly shaft away from the transmission wheel. The connecting bend is connected to the supply and discharge channel, and a supply and discharge valve is installed on the connecting bend.

4. The method for preparing glycine hydrochloride according to claim 1, characterized in that: Multiple gas supply channels are provided on the assembly shaft, each gas supply channel extending axially along the assembly shaft. The portion of each gas supply channel located inside the horizontal vessel body is connected to the reaction chamber through multiple gas outlets, and these gas outlets are spaced apart along the assembly shaft axially. The portion of each gas supply channel located outside the horizontal vessel body is connected to the outside through a through hole on the assembly shaft. A distribution sleeve is rotatably fitted on the assembly shaft at the location of the through hole. The distribution sleeve is equipped with a gas supply connector, which is connected to the reaction chamber through the distribution sleeve, the through hole, the gas supply channel, and the gas outlet.

5. The method for preparing glycine hydrochloride according to claim 1, characterized in that: Annular fixing seats are fixedly connected to both ends of the second spiral blade. The large-diameter end of each conical spring is installed on the corresponding annular fixing seat, and the small-diameter end of the conical spring is connected to an adapter seat. The adapter seat is rotatably connected to the corresponding end cover.

6. The method for preparing glycine hydrochloride according to claim 5, characterized in that: The clutch mechanism includes an internal gear ring, a movable clutch component, and a transmission gear arranged sequentially outward along the axis of the assembly shaft. The internal gear ring is installed on the outside of the end cover, the transmission gear is installed at the end of the assembly shaft, and the movable clutch component is sleeved on the outside of the assembly shaft.

7. The method for preparing glycine hydrochloride according to claim 6, characterized in that: The movable clutch includes a clutch gear ring whose axis coincides with that of the internal gear ring and the transmission gear. Internal gear teeth are uniformly arranged circumferentially on the inner peripheral wall of the clutch gear ring, and external gear teeth are uniformly arranged circumferentially on the outer peripheral wall of the clutch gear ring. The clutch gear ring is connected to a rotating ring via two connecting arms. The rotating ring is rotatably connected within an annular groove of the connecting ring, and the axes of the rotating ring, the connecting ring, and the clutch gear ring coincide. Guide posts are spaced apart on the adapter seat, and each guide post passes through the axial direction of the assembly shaft. The clutch gear ring is slidably connected to the guide post, and the lower end of the operating lever is hinged to the upper end of the connecting ring. When the inner gear of the clutch gear ring meshes with the transmission gear, the stirring crystallization attachment mechanism changes to a stirring mode, and when the assembly shaft is driven to rotate, the first and second helical blades rotate synchronously. When the outer gear of the clutch gear ring meshes with the inner gear ring, the stirring crystallization attachment mechanism changes to a scraping mode, the first helical blade rotates with the assembly shaft, and the second helical blade is indirectly fixedly connected to the end cover through a conical spring.

Images