CN117486745A - Preparation method of glycinamide hydrochloride - Google Patents
Preparation method of glycinamide hydrochloride Download PDFInfo
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- CN117486745A CN117486745A CN202311427048.6A CN202311427048A CN117486745A CN 117486745 A CN117486745 A CN 117486745A CN 202311427048 A CN202311427048 A CN 202311427048A CN 117486745 A CN117486745 A CN 117486745A
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- assembly shaft
- reaction
- water
- reaction kettle
- clutch
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- WKNMKGVLOWGGOU-UHFFFAOYSA-N 2-aminoacetamide;hydron;chloride Chemical compound Cl.NCC(N)=O WKNMKGVLOWGGOU-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 139
- 239000013078 crystal Substances 0.000 claims abstract description 118
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 107
- 238000003756 stirring Methods 0.000 claims abstract description 92
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 87
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000007790 scraping Methods 0.000 claims abstract description 17
- FOCAUTSVDIKZOP-UHFFFAOYSA-M chloroacetate Chemical compound [O-]C(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-M 0.000 claims abstract description 12
- 229940089960 chloroacetate Drugs 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 230000007246 mechanism Effects 0.000 claims description 102
- 230000005540 biological transmission Effects 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 14
- 238000004891 communication Methods 0.000 claims description 13
- 239000012043 crude product Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 9
- 238000009826 distribution Methods 0.000 claims description 9
- 230000002093 peripheral effect Effects 0.000 claims description 8
- 238000005086 pumping Methods 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 4
- 239000007789 gas Substances 0.000 abstract description 11
- 150000001298 alcohols Chemical class 0.000 abstract description 7
- 238000002425 crystallisation Methods 0.000 abstract description 7
- 230000008025 crystallization Effects 0.000 abstract description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 abstract description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 abstract description 6
- 230000009471 action Effects 0.000 abstract description 5
- 239000002904 solvent Substances 0.000 abstract description 5
- 239000002351 wastewater Substances 0.000 abstract description 4
- 230000035484 reaction time Effects 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 10
- QABLOFMHHSOFRJ-UHFFFAOYSA-N methyl 2-chloroacetate Chemical compound COC(=O)CCl QABLOFMHHSOFRJ-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000543 intermediate Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000013459 approach Methods 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XFKYKTBPRBZDFG-UHFFFAOYSA-N 2-aminoacetonitrile;hydrochloride Chemical compound Cl.NCC#N XFKYKTBPRBZDFG-UHFFFAOYSA-N 0.000 description 1
- DYAQXLDQUHCRBU-UHFFFAOYSA-N 2-chloroacetamide;hydrochloride Chemical compound Cl.NC(=O)CCl DYAQXLDQUHCRBU-UHFFFAOYSA-N 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- VGCXGMAHQTYDJK-UHFFFAOYSA-N Chloroacetyl chloride Chemical compound ClCC(Cl)=O VGCXGMAHQTYDJK-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 238000005915 ammonolysis reaction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- VEUUMBGHMNQHGO-UHFFFAOYSA-N ethyl chloroacetate Chemical compound CCOC(=O)CCl VEUUMBGHMNQHGO-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- IHLAQQPQKRMGSS-UHFFFAOYSA-N oxiracetam Chemical compound NC(=O)CN1CC(O)CC1=O IHLAQQPQKRMGSS-UHFFFAOYSA-N 0.000 description 1
- 229960001227 oxiracetam Drugs 0.000 description 1
- 239000012450 pharmaceutical intermediate Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
- B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/02—Crystallisation from solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/20—Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/005—Feed or outlet devices as such, e.g. feeding tubes provided with baffles
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of glycinamide hydrochloride, which comprises the steps of adding water and a catalyst into a reaction kettle, introducing ammonia gas at 0-5 ℃, then dropwise adding chloroacetate, stirring for reaction, heating to 30-35 ℃ after the addition, introducing ammonia gas for continuous reaction for 2-3 hours, deaminizing and dehydrating after the reaction is finished, adding a methanol solvent for crystallization to obtain a glycinamide hydrochloride product, and scraping and collecting crystals. According to the invention, chloroacetate is adopted to generate glycinamide hydrochloride under the action of ammonia water and a catalyst, and the glycinamide hydrochloride is crystallized by alcohols to obtain a product, so that hydrogen chloride gas or a large amount of alcohols are prevented from being used as solvents, the safety risk caused by centralized use of a large amount of alcohols is reduced, the reaction time is shortened, the product quality and the yield are improved, the subsequent treatment is simple, the operation is convenient, the removed ammonia is absorbed by the removed water, and then ammonia gas is recycled, so that no waste water is generated, and the method is environment-friendly. The invention is suitable for preparing glycinamide hydrochloride.
Description
Technical Field
The invention belongs to the field of preparation of pharmaceutical intermediates, and particularly relates to a preparation method of glycinamide hydrochloride.
Background
Glycinamide hydrochloride is an important intermediate, is a key intermediate for preparing oxiracetam, is also used for producing sulfa drug SMPZ, can be used as an intermediate of other materials, and has a very wide market. In the prior art, the preparation method of glycinamide hydrochloride mainly comprises the following steps: firstly, aminoacetonitrile hydrochloride is taken as a raw material, dry hydrogen chloride is introduced to obtain glycinamide hydrochloride, and hydrogen chloride gas used in the method has corrosiveness and serious corrosion to equipment. Secondly, chloracetyl chloride is taken as a raw material, ammonia gas is introduced, the reaction is carried out in an alcohol solvent, and after the reaction is finished, a product glycinamide hydrochloride crude product is obtained. Thirdly, ammonia is introduced by using chloroacetate under a certain positive pressure under the action of an organic solvent, chloroacetamide hydrochloride is generated by ammonolysis, and then ammonia is introduced, so that glycinamide hydrochloride is obtained.
Disclosure of Invention
The invention provides a preparation method of glycinamide hydrochloride, which is used for achieving the purpose of simple purification treatment steps, avoiding the use of hydrogen chloride gas, reducing the safety risk, and being simple in subsequent treatment, free from waste water and environment-friendly.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a process for the preparation of glycinamide hydrochloride comprising the steps of:
s1, firstly, adding 2.5-10.0 parts by weight of catalyst into a feeder, and pumping the reaction water in a reaction water tank into a reaction kettle of a reactor through a pressure pump until the weight of the reaction water is 180-240;
s2, introducing cold water into a water bath box of the reactor to enable the temperature in the reaction kettle to be 0-5 ℃;
s3, introducing 60 parts by weight of ammonia into the reaction kettle, and adding 50 parts by weight of chloroacetate through a feeder;
s4, controlling a pressure pump to pump out the solution in the reaction kettle and then pumping the solution into the reaction kettle, so that the solution is circulated, chloroacetate in a feeder is completely dissolved into the solution, and then stopping the pressure pump;
s5, operating the clutch mechanism to change the stirring type crystal attachment mechanism into a stirring type, and driving the stirring type crystal attachment mechanism in the reaction kettle to rotate in the reaction kettle to perform stirring reaction;
s6, after the stirring reaction is completed, cold water in the water bath box is pumped out, warm water is introduced into the water bath box until the temperature in the reaction kettle is increased to 30-35 ℃, ammonia gas is continuously introduced, and the temperature is kept at 30-35 ℃;
s7, reacting for 2-3 hours, heating the reaction kettle to distill ammonia and reaction water in the reaction kettle to obtain the ammonia and the reaction water, adding 50 parts by weight of methanol, extracting hot water in the water bath tank, introducing cold water into the water bath tank, cooling and crystallizing to obtain a crude product, and extracting methanol carrying impurities in the reaction kettle;
s8, replacing cold water in the water bath tank with warm water until the temperature in the reaction kettle is increased to 30-35 ℃, introducing 50 parts by weight of methanol into the reaction kettle, dissolving the crude product in the methanol, and then performing cooling operation to recrystallize the crude product to obtain glycinamide hydrochloride crystals;
s9, extracting methanol from the reaction kettle, operating the clutch mechanism to enable the stirring type crystal attachment mechanism to be in a crystal scraping state, driving the stirring type crystal attachment mechanism to act, enabling the glycinamide hydrochloride crystals attached to the inner wall of the reaction kettle and the stirring type crystal attachment mechanism to fall off, operating the clutch mechanism again to enable the stirring type crystal attachment mechanism to be in a stirring state, driving the stirring type crystal attachment mechanism to rotate, and enabling the glycinamide hydrochloride crystals in the reaction kettle to be gradually conveyed to a discharge joint and collected by the collecting box.
Further, the water bath box comprises a box body, the lower end of the box body is supported on the ground through a plurality of supporting legs, the upper end of the box body is in an open state, a water inlet joint and a water outlet joint are respectively constructed on two opposite side walls of the box body, and a water inlet main valve and a water outlet main valve are respectively installed on the water inlet joint and the water outlet joint.
Further, the reaction kettle is arranged in the water bath box, the stirring type crystal attachment mechanism is arranged in the reaction cavity of the reaction kettle, the number of the clutch mechanisms is two, the two clutch mechanisms are respectively arranged at the two axial ends of the horizontal kettle body, and the clutch mechanisms are constructed at the same side end parts of the horizontal kettle body and the stirring type crystal attachment mechanism.
Further, the reaction kettle comprises a cylindrical horizontal kettle body, end covers are detachably connected to the axial ends of the horizontal kettle body, a steam outlet connector and a discharging connector are respectively constructed at the upper end and the lower end of the horizontal kettle body, one end of a communicating elbow is communicated with the lower end of the horizontal kettle body, and the other end of the communicating elbow is communicated with the outside through a stirring type crystal attachment mechanism.
Further, the stirring type crystal attachment mechanism comprises an assembly shaft, a first spiral blade and a second spiral blade which are coaxially assembled in the horizontal kettle body, the first spiral blade and the second spiral blade have the same structure, both extend spirally along the axial direction of the assembly shaft, and the end parts of the ends of the second spiral blade are connected with the corresponding end covers through conical springs; two ends of the assembly shaft extend out of the horizontal kettle body through corresponding end covers respectively, the assembly shaft is rotationally connected with the two end covers, the first spiral blade is fixedly connected with the assembly shaft, and the second spiral blade is movably sleeved outside the assembly shaft; one end of the assembly shaft is provided with a driving wheel which is driven to drive the assembly shaft to rotate.
Further, the assembly shaft is provided with a supply and discharge channel which coincides with the axis of the assembly shaft, the supply and discharge channel extends from one end of the assembly shaft to the other end, the communication elbow is rotationally assembled at one end of the assembly shaft far away from the driving wheel, the communication elbow is communicated with the supply and discharge channel, and a supply and discharge valve is arranged on the communication elbow.
Further, a plurality of air supply channels are formed in the assembly shaft, each air supply channel extends along the axial direction of the assembly shaft, the part of each air supply channel in the horizontal kettle body is communicated with the reaction cavity through a plurality of air outlet holes, the air outlet holes are arranged on the assembly shaft at intervals along the axial direction of the assembly shaft, and the part of each air supply channel in the outside of the horizontal kettle body is communicated with the outside through a through hole formed in the assembly shaft; the assembly shaft is provided with a distribution sleeve in a rotating mode at the position of the guide hole, the distribution sleeve is provided with an air supply connector, and the air supply connector is communicated with the reaction cavity through the distribution sleeve, the guide hole, the air supply channel and the air outlet hole.
Further, annular fixing seats are fixedly connected to the two ends of the second helical blade respectively, the large-diameter ends of the conical springs are mounted on the corresponding annular fixing seats, the small-diameter ends of the conical springs are connected with adapter seats, and the adapter seats are rotatably connected to corresponding end covers.
Further, the clutch mechanism comprises an inner gear ring, a movable clutch piece and a transmission gear, wherein the inner gear ring, the movable clutch piece and the transmission gear are sequentially arranged outwards along the axis of the assembly shaft, the inner gear ring is arranged on the outer side of the end cover, the transmission gear is arranged at the end part of the assembly shaft, and the movable clutch piece is sleeved outside the assembly shaft.
Further, the movable clutch piece comprises a clutch gear ring which is overlapped with the axes of the inner gear ring and the transmission gear, inner gear teeth are uniformly formed on the inner peripheral wall of the clutch gear ring along the circumferential direction of the clutch gear ring, outer gear teeth are uniformly formed on the outer peripheral wall of the clutch gear ring along the circumferential direction of the clutch gear ring, the clutch gear ring is connected with the rotating ring through two connecting arms, the rotating ring is rotationally connected in an annular groove of the connecting ring, the axes of the rotating ring, the connecting ring and the clutch gear ring are overlapped, guide posts are formed on the connecting seat at intervals, each guide post penetrates through the clutch gear ring along the axial direction of the assembly shaft, the guide posts are in sliding connection with the clutch gear ring, and the lower end of the operating rod is hinged to the upper end of the connecting ring; when the inner gear of the clutch gear ring is meshed with the transmission gear, the stirring type crystal attachment mechanism is changed into a stirring type, and the first spiral blade and the second spiral blade synchronously rotate when the assembly shaft is driven to rotate; when the outer gear of the clutch gear ring is meshed with the inner gear ring, the stirring type crystal attachment mechanism is changed into a scraping type state, the first spiral blade rotates along with the assembly shaft, and the second spiral blade is indirectly and fixedly connected with the end cover through the conical spring.
Compared with the prior art, the invention adopts the structure, and the technical progress is that: according to the invention, chloroacetate is adopted to generate glycinamide hydrochloride under the action of ammonia water and a catalyst, the glycinamide hydrochloride is crystallized by methanol to obtain a product, and the obtained product is recrystallized to improve purity, so that hydrogen chloride gas or a large amount of alcohols are avoided to be used as solvents, the safety risk caused by centralized use of a large amount of alcohols is reduced, the reaction time is shortened, the removed ammonia is absorbed by the removed water, and then ammonia gas is introduced for recycling, so that no waste water is generated, and the method is environment-friendly. The stirring type crystal attachment mechanism has two modes, namely a stirring mode and a crystal scraping mode; in the reaction process, the stirring type crystal attachment mechanism is switched into a stirring mode through the clutch mechanism, so that when the stirring type crystal attachment mechanism is driven to act, the solution in the reaction kettle is stirred, and further, the mixing and the reaction are more complete and rapid; because the glycinamide hydrochloride crystals have the adhesion property, and the purity of crystals attached to the surface of an object is higher than that of crystals not attached to the object, the invention increases the attachment area of the crystals by adopting the stirring type crystal attachment mechanism and the reaction kettle, namely, the crystals are gradually attached to the inner wall of the reaction kettle and the surface of the stirring type crystal attachment mechanism in the crystallization process, and the purity of the crystals is improved. After the recrystallization is finished and the methanol is completely pumped out of the reaction kettle, the stirring type crystal attachment mechanism is switched into a crystal scraping state through the clutch mechanism, the stirring type crystal attachment mechanism is driven to rotate, the stirring type crystal attachment mechanism scrapes off crystals attached to the inner wall of the reaction kettle and the inner wall of the reaction kettle, the crystals are separated from the attached substances and are gradually conveyed to a discharging joint through the stirring type crystal attachment mechanism, and then the crystals are collected by the collecting box; and further, under the condition of improving the product quality and the yield, the subsequent treatment is simple and the operation is convenient.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention.
In the drawings:
FIG. 1 is a process flow diagram of an embodiment of the present invention;
FIG. 2 is a schematic diagram showing the structure of a reactor and a water bath tank assembled with each other in the reactor according to the embodiment of the present invention;
FIG. 3 is a schematic view of the structure of a water bath in a reactor according to an embodiment of the present invention;
FIG. 4 is a schematic structural view of a reaction vessel in a reactor according to an embodiment of the present invention;
FIG. 5 is an axial structural cross-sectional view of a reaction vessel in a reactor according to an embodiment of the present invention;
FIG. 6 is an enlarged view of the structure of the portion A in FIG. 5;
FIG. 7 is an enlarged view of the structure of the portion B in FIG. 5;
FIG. 8 is a schematic diagram of a structure in which two clutch mechanisms are connected to a stirring crystal attachment mechanism according to an embodiment of the present invention;
FIG. 9 is a schematic view showing a partial structure of a stirring type crystal attachment mechanism according to an embodiment of the present invention;
FIG. 10 is a front view showing the structure in which the assembly shaft is connected to the first screw blade in the stirring type crystal attachment mechanism according to the embodiment of the present invention;
FIG. 11 is a front view showing a structure in which a second helical blade is connected to an adapter by a conical spring in the stirring type crystal attachment mechanism according to the embodiment of the present invention;
FIG. 12 is a schematic view showing a structure in which a first helical blade gradually approaches a second helical blade as the first helical blade rotates along with an assembly shaft when a stirring type crystal attachment mechanism is converted into a crystal scraping form by a clutch mechanism;
FIG. 13 is a schematic view of a clutch mechanism according to an embodiment of the present invention connected to one end of an assembly shaft;
fig. 14 is a schematic structural view of the clutch mechanism according to the embodiment of the invention after being detached.
Marking parts: 100-water bath box, 101-box body, 102-water inlet joint, 103-water outlet joint, 104-water inlet main valve, 105-water outlet main valve, 106-supporting leg, 107-connecting seat, 108-first limiting rod, 109-second limiting rod, 200-reaction kettle, 201-horizontal kettle body, 202-end cover, 203-discharge joint, 204-discharge valve, 205-steam outlet joint, 206-communication elbow pipe, 207-supply and discharge valve, 208-reaction cavity, 300-stirring type crystal attachment mechanism, 301-assembly shaft, 302-driving wheel, 303-supply and discharge channel, 304-air supply channel, 305-guide hole, 306-air outlet hole, 307-first helical blades, 308-second helical blades, 309-annular fixed seat, 310-conical spring, 311-adapter, 400-clutch mechanism, 401-fixed disk, 402-annular gear, 403-clutch gear, 404-inner gear, 405-outer gear, 406-connecting arm, 407-rotating ring, 408-guide post, 409-guide sleeve, 410-connecting ring, 411-annular groove, 412-driving gear, 413-limiting disk, 414-operating lever, 500-connecting pipe, 501-first joint, 502-second joint, 503-first valve body, 504-second valve body, 600-feeder, 700-split set, 701-air supply joint.
Detailed Description
Preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are presented for purposes of illustration and explanation only and are not intended to limit the present invention.
The invention discloses a preparation method of glycinamide hydrochloride, which is shown in figures 1-14 and comprises the following steps:
s1, firstly, adding 2.5-10.0 parts by weight of catalyst into a feeder 600, and pumping the reaction water in a reaction water tank into a reaction kettle 200 of the reactor through a pressure pump until the weight of the reaction water is 180-240;
s2, introducing cold water into the water bath box 100 of the reactor, so that the temperature in the reaction kettle 200 is 0-5 ℃;
s3, introducing 60 parts by weight of ammonia into the reaction kettle 200, and adding 50 parts by weight of chloroacetate through a feeder 600;
s4, controlling a pressure pump to pump out the solution in the reaction kettle 200 and then pump the solution into the reaction kettle 200, so that the solution is circulated, chloroacetate in the feeder 600 is completely dissolved into the solution, and then stopping the pressure pump;
s5, operating the clutch mechanism 400 to change the stirring type crystal attachment mechanism 300 into a stirring type, and driving the stirring type crystal attachment mechanism 300 in the reaction kettle 200 to rotate in the reaction kettle 200 to perform stirring reaction;
s6, after the stirring reaction is completed, cold water in the water bath box 100 is pumped out, warm water is introduced into the water bath box 100 until the temperature in the reaction kettle 200 is increased to 30-35 ℃, ammonia gas is continuously introduced, and the temperature is kept at 30-35 ℃;
s7, reacting for 2-3 hours, heating the reaction kettle 200 to distill ammonia and reaction water in the reaction kettle to obtain ammonia and reaction water, adding 50 parts by weight of methanol, extracting hot water in the water bath 100, introducing cold water into the water bath 100, cooling and crystallizing to obtain a crude product, and extracting methanol carrying impurities in the reaction kettle 200;
s8, replacing cold water in the water bath 100 with warm water until the temperature in the reaction kettle 200 is increased to 30-35 ℃, introducing 50 parts by weight of methanol into the reaction kettle 200, dissolving the crude product in the methanol, and then performing cooling operation to recrystallize the crude product to obtain glycinamide hydrochloride crystals;
s9, methanol is pumped out of the reaction kettle 200, the clutch mechanism 400 is operated, the stirring type crystal attachment mechanism 300 is changed into a crystal scraping state, the stirring type crystal attachment mechanism 300 is driven to act, the glycinamide hydrochloride crystals attached to the inner wall of the reaction kettle 200 and the stirring type crystal attachment mechanism 300 are separated, the clutch mechanism 400 is operated again, the stirring type crystal attachment mechanism 300 is changed into a stirring state, the stirring type crystal attachment mechanism 300 is driven to rotate, and the glycinamide hydrochloride crystals in the reaction kettle 200 are gradually conveyed to the discharge joint 203 and collected by the collecting box.
The working principle and the advantages of the invention are as follows: according to the invention, chloroacetate is adopted to generate glycinamide hydrochloride under the action of ammonia water and a catalyst, the glycinamide hydrochloride is crystallized by methanol to obtain a product, and the obtained product is recrystallized to improve purity, so that hydrogen chloride gas or a large amount of alcohols are avoided to be used as solvents, the safety risk caused by centralized use of a large amount of alcohols is reduced, the reaction time is shortened, the removed ammonia is absorbed by the removed water, and then ammonia gas is introduced for recycling, so that no waste water is generated, and the method is environment-friendly. The stirring type crystal attachment mechanism 300 of the present invention has two modes, namely a stirring mode and a crystal scraping mode; in the reaction process, the stirring crystal attachment mechanism 300 is switched into a stirring mode by the clutch mechanism 400, so that when the stirring crystal attachment mechanism 300 is driven to act, the solution in the reaction kettle 200 is stirred, and further, the mixing and the reaction are more complete and rapid; since glycinamide hydrochloride crystals have adhesion and the purity of crystals adhered to the surface of an object is higher than that of crystals not adhered to the surface of the object, the invention increases the adhering area of crystals by adopting the stirring type crystal adhering mechanism 300 and the reaction kettle 200, namely, crystals are gradually adhered to the inner wall of the reaction kettle 200 and the surface of the stirring type crystal adhering mechanism 300 in the crystallization process, thereby improving the purity of crystals. After the recrystallization is finished and the methanol is completely pumped out of the reaction kettle 200, the stirring type crystal attachment mechanism 300 is switched into a crystal scraping state through the clutch mechanism 400, the stirring type crystal attachment mechanism 300 is driven to rotate, the stirring type crystal attachment mechanism 300 scrapes off crystals attached to the inner wall of the reaction kettle 200 and the inner wall of the reaction kettle, the crystals are separated from the attached substances and are gradually conveyed to a discharge joint 203 by the stirring type crystal attachment mechanism 300, and then the crystals are collected by a collecting box; and further, under the condition of improving the product quality and the yield, the subsequent treatment is simple and the operation is convenient.
As a preferred embodiment of the present invention, as shown in fig. 2 and 3, the water bath tank 100 includes a tank body 101, and a plurality of support legs 106 are fixed to the lower end of the tank body 101, and the support legs 106 support the tank body 101 on the ground, with the upper end of the tank body 101 being in an open state. In this embodiment, two opposite side walls of the tank 101 are respectively provided with a water inlet joint 102 and a water outlet joint 103, and a water inlet main valve 104 and a water outlet main valve 105 are respectively installed on the water inlet joint 102 and the water outlet joint 103. The reaction kettle 200 of the embodiment is arranged in the water bath box 100, cold water or warm water is supplied to the water bath box 100 through the water inlet joint 102, and the purpose of water bath of the solution in the reaction kettle 200 is further achieved; cold or warm water in the water bath 100 can be discharged through the water outlet joint 103 so as to replace water bath water with a corresponding temperature.
As a preferred embodiment of the present invention, as shown in fig. 4 and 5, the reaction vessel 200 has a reaction chamber 208, and a stirring crystal attachment mechanism 300 is provided in the reaction chamber 208. The number of the clutch mechanisms 400 of the present embodiment is two, the two clutch mechanisms 400 are respectively provided at both axial ends of the horizontal kettle body 201, and each clutch mechanism 400 is configured at the same side end of the horizontal kettle body 201 and the stirring crystal attachment mechanism 300. The reaction kettle 200 has a specific structure that the reaction kettle 200 comprises a horizontal kettle body 201, a communicating elbow 206 and two end covers 202, wherein the horizontal kettle body 201 is of a cylindrical structure, the two end covers 202 are respectively arranged at two axial ends of the horizontal kettle body 201, and each end cover 202 is detachably connected to the corresponding end part of the horizontal kettle body 201. The steam outlet joint 205 and the discharge joint 203 are respectively arranged at the upper end and the lower end of the horizontal kettle body 201, and a discharge valve 204 is arranged on the discharge joint 203. The gas outlet joint 205 can be communicated with two pipelines, one pipeline is used for collecting ammonia gas and reaction water which are distilled out; the other pipeline is communicated with an ammonia tank through a dryer, and the ammonia tank is communicated with the reaction cavity 208 of the reaction kettle 200 through a gas booster pump, so that ammonia can circulate between the reaction cavity 208 and the ammonia tank. In this embodiment, one end of the communicating elbow 206 is communicated with the lower end of the horizontal kettle 201, and the other end of the communicating elbow 206 is communicated with the outside through the stirring type crystal attachment mechanism 300. The components of the embodiment except ammonia are supplied to the communication elbow 206 through the stirring type crystal attachment mechanism 300, and then enter the reaction chamber 208 from the communication elbow 206; and after the coarse crystallization and the recrystallization are finished, the methanol in the reaction cavity 208 is pumped away, specifically, the methanol enters the stirring crystal attachment mechanism 300 through the communication elbow 206 and is pumped out through the pressure pump and enters the recovery tank so as to remove impurities through subsequent distillation, and the methanol is obtained again.
As a preferred embodiment of the present invention, as shown in fig. 8 to 11, the stirring crystallization attaching mechanism 300 includes a fitting shaft 301, a first screw blade 307 and a second screw blade 308, wherein the fitting shaft 301, the first screw blade 307 and the second screw blade 308 are all fitted in the horizontal kettle 201, and all of them coincide with the axis of the horizontal kettle 201. The first helical blade 307 and the second helical blade 308 of this embodiment have the same structure, both extend helically in the axial direction of the assembly shaft 301, and are connected with conical springs 310 at both end portions of the second helical blade 308, respectively, each conical spring 310 being connected with the corresponding end cap 202. In this embodiment, two ends of the assembly shaft 301 respectively pass through the corresponding end caps 202 and extend out of the horizontal kettle body 201, and the assembly shaft 301 is rotationally connected with the two end caps 202, the first spiral blade 307 is fixedly connected with the assembly shaft 301, and the second spiral blade 308 is movably sleeved outside the assembly shaft 301. The present embodiment is provided with a driving wheel 302 at one end of the fitting shaft 301, and the driving wheel 302 is driven to rotate the fitting shaft 301. Specifically, the driving wheel 302 is located outside the water bath tank 100, a forward and reverse rotation motor is further arranged outside the water bath tank 100, a driving wheel is mounted on an output shaft of the forward and reverse rotation motor, and the driving wheel is connected with the driving wheel 302 through a driving belt. In this embodiment, the first screw blade 307 and the second screw blade 308 are controlled to be connected to or disconnected from each other by the clutch mechanism 400, and when the first screw blade 307 and the second screw blade 308 are connected to each other, the stirring type crystal attachment mechanism 300 is in a stirring state, and when the first screw blade 307 and the second screw blade 308 are disconnected from each other, the stirring type crystal attachment mechanism 300 is in a scraping state. And when the stirring type crystal attachment mechanism 300 is in a stirring mode and is in a crystallization process at the moment, the assembly shaft 301 is slowly driven to rotate, so that the assembly shaft 301 drives the first spiral blade 307 and the second spiral blade 308 to synchronously and slowly rotate, and crystals are gradually attached to the inner wall of the reaction kettle 200, the surface of the first spiral blade 307, the surface of the second spiral blade 308 and the peripheral surface of the assembly shaft 301, thereby improving the efficiency and purity of crystallization. When the first screw blade 307 and the second screw blade 308 are disengaged, the assembly shaft 301 is driven to rotate, so that the assembly shaft 301 drives the first screw blade 307 to rotate, and the second screw blade 308 does not rotate; the relative position of the first spiral blade 307 and the second spiral blade 308 is gradually changed from the position shown in fig. 5 to the position shown in fig. 12 in the rotating process, so that the second spiral blade 308 rotates relative to the assembly shaft 301, the second spiral blade 308 scrapes crystals on the rotating assembly shaft 301, when the first spiral blade 307 approaches to and contacts with the second spiral blade 308, the first spiral blade 307 and the second spiral blade 308 relatively rotate, crystals on the corresponding surfaces of the first spiral blade 307 and the second spiral blade 308 are scraped off under the action of friction force, and after the first spiral blade 307 and the second spiral blade 308 contact, the first spiral blade 307 further continuously compresses the second spiral blade 308 axially, and at the moment, the second spiral blade 308 axially displaces correspondingly, and the two conical springs 310 elastically deform correspondingly to adapt to the axial displacement of the second spiral blade. When the crystals on one side of the first and second spiral blades 307 and 308 are scraped off, the assembly shaft 301 is driven to rotate in a reverse direction, so that the crystals on the other side of the first and second spiral blades 307 and 308 are scraped off. In this embodiment, when the first screw blade 307 rotates forward and backward, the first screw blade 307 scrapes off crystals on the inner peripheral wall of the reaction kettle 200, and after the scraping of crystals is completed, the clutch mechanism 400 is controlled to switch the stirring crystal attachment mechanism 300 to a stirring mode, and the assembly shaft 301 is controlled to rotate, so that the first screw blade 307 and the second screw blade 308 gradually convey the scraped crystals to the discharge joint 203, so as to collect the crystals by the collection box. In this embodiment, when the crystal scraping operation is performed, the driving motor can be controlled to perform forward and backward intermittent operations, so as to synchronously complete the crystal scraping operation on the two sides of the first spiral blade 307 and the two sides of the second spiral blade 308, so as to improve the crystal scraping efficiency, and the second spiral blade 308 that reciprocates can effectively drive the conical spring 310 to reciprocate, thereby promoting the crystals on the conical spring 310 to rapidly fall off.
As a preferred embodiment of the present invention, as shown in fig. 5, the fitting shaft 301 has a supply and discharge passage 303, the supply and discharge passage 303 coincides with the axis of the fitting shaft 301, and the supply and discharge passage 303 extends from one end to the other end of the fitting shaft 301. The communication elbow 206 of the present embodiment is rotatably mounted at one end of the mounting shaft 301 away from the driving wheel 302, the communication elbow 206 is communicated with the supply and discharge channel 303, and the supply and discharge valve 207 is mounted on the communication elbow 206. As shown in fig. 2, in this embodiment, a connection pipe 500 is rotatably connected to one end of the assembly shaft 301 near the transmission wheel 302, a first joint 501 and a second joint 502 are configured on the connection pipe 500, and a first valve body 503 and a second valve body 504 are respectively mounted on the first joint 501 and the second joint 502, wherein the first joint 501 is connected to an outlet of the pressure pump, and the second joint 502 is connected to an inlet of the pressure pump. The feeder 600 of the present embodiment is installed on the connection pipe 500, and a feeding valve is installed at a portion where the feeder 600 is connected to the connection pipe 500, and when feeding is required, the feeding valve is first closed, then a predetermined amount of components is added to the feeder 600, and finally the feeding valve is opened.
As a preferred embodiment of the present invention, as shown in fig. 5-7, a plurality of air supply channels 304 are formed on the assembly shaft 301, each air supply channel 304 extends along the axial direction of the assembly shaft 301, and the portion of each air supply channel 304 located in the horizontal kettle body 201 is communicated with the reaction chamber 208 through a plurality of air outlet holes 306, and the air outlet holes 306 are formed on the assembly shaft 301 at intervals along the axial direction of the assembly shaft 301. Each gas supply channel 304 is located at a position outside the horizontal kettle body 201 and is communicated with a through hole 305, the through hole 305 is formed on the assembly shaft 301, and the through hole 305 is used for communicating the gas supply channels 304 with the outside. In this embodiment, a distribution sleeve 700 is rotatably sleeved on the assembly shaft 301 and located at the position of the through hole 305, an air supply connector 701 is configured on the distribution sleeve 700, the air supply connector 701 is communicated with the reaction cavity 208 through the distribution sleeve 700, the through hole 305, the air supply channel 304 and the air outlet hole 306, and the air supply connector 701 is communicated with the ammonia tank through a dryer. The working principle of the embodiment is as follows: the ammonia gas is introduced into the multiple gas supply channels 304 synchronously, and then enters the reaction chamber 208 through the gas outlet holes 306, and in the process, the assembly shaft 301 is driven to be driven, so that the ammonia gas can uniformly enter into the regions of the reaction chamber 208 and fully react with the reaction water and other components.
As a preferred embodiment of the present invention, as shown in fig. 8-14, two ends of the second spiral blade 308 are fixedly connected with annular fixing seats 309, a large diameter end of each conical spring 310 is mounted on the corresponding annular fixing seat 309, and a small diameter end of the conical spring 310 is connected with an adapter 311, wherein the adapter 311 is rotatably connected to the corresponding end cover 202. The clutch mechanism 400 of this embodiment has a specific structure that the clutch mechanism 400 includes an inner gear ring 402, a movable clutch member and a transmission gear 412, wherein the inner gear ring 402, the movable clutch member and the transmission gear 412 are sequentially arranged outwards along the axis of the assembly shaft 301, the inner gear ring 402 is mounted on the outer side of the end cover 202, the transmission gear 412 is mounted on the end portion of the assembly shaft 301, and the movable clutch member is sleeved outside the assembly shaft 301. In this embodiment, the ring gear 402 is coaxially welded to the fixed disc 401, and the fixed disc 401 is located on the side of the ring gear 402 near the end cover 202, the fixed disc 401 is connected to the outer side of the end cover 202 through a plurality of bolts, and the limiting disc 413 is coaxially configured on the side of the transmission gear 412 far from the end cover 202. The fixed disc 401 and the limiting disc 413 of this embodiment are both used for limiting the displacement of the movable clutch member, so as to avoid the situation that the movable clutch member is separated from the ring gear 402 after being matched with the ring gear 402, or the situation that the movable clutch member is separated from the transmission gear 412 after being matched with the transmission gear 412. The movable clutch of the present embodiment is specifically structured such that the movable clutch includes a clutch ring gear 403 and a lever 414, wherein the axes of the clutch ring gear 403, the ring gear 402, and the transmission gear 412 coincide, inner teeth 404 are uniformly formed on the inner peripheral wall of the clutch ring gear 403 along the circumferential direction thereof, and outer teeth 405 are uniformly formed on the outer peripheral wall of the clutch ring gear 403 along the circumferential direction thereof. The clutch ring gear 403 of the present embodiment is connected to the rotary ring 407 by two connecting arms 406, the rotary ring 407 is rotatably connected in the annular groove 411 of the connecting ring 410, and the axes of the rotary ring 407, the connecting ring 410, and the clutch ring gear 403 coincide. In this embodiment, guide posts 408 are configured on the adaptor base 311 at intervals, guide sleeves 409 are configured 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 posts 408 are slidably connected with the guide sleeves 409. The lower end of the operating rod 414 of the embodiment is hinged at the upper end of the connecting ring 410, two sides of the upper end of the water bath 100 are respectively provided with a connecting seat 107, and a first limiting rod 108 and a second limiting rod 109 are arranged on the connecting seat 107 and are arranged at intervals along the axial direction of the assembly shaft 301. When the operator pulls the operating lever 414 to contact with the first limiting lever 108, the operator continues to pull the operating lever 414, so that the lower end of the operating lever 414 drives the clutch gear ring 403 to move towards the annular gear 402 through the connecting ring 410 until the clutch gear ring 403 is meshed with the annular gear ring 402, at this time, the stirring crystal attachment mechanism 300 is in a crystal scraping state, that is, the assembly shaft 301 is in a free state, and the end adapter 311 of the conical spring 310 is connected with the end cover 202 through the meshed annular gear ring 402 and the clutch gear ring 403. When the operator pulls the operating lever 414 to contact with the second limiting lever 109, the operator continues to pull the operating lever 414, so that the lower end of the operating lever 414 drives the clutch gear ring 403 to move towards the transmission gear 412 through the connecting ring 410 until the clutch gear ring 403 is meshed with the transmission gear 412, at this time, the stirring crystal attachment mechanism 300 is in a stirring mode, that is, the assembly shaft 301 is meshed with the adapter seat 311 through the clutch gear ring 403 of the transmission gear 412, so that the adapter seat 311 drives the second helical blade 308 to rotate through the conical spring 310 in the process of rotating along with the assembly shaft 301, and meanwhile, the first helical blade 307 synchronously rotates along with the assembly shaft 301.
In the embodiment, reaction water with the weight portion of 200 and catalyst with the weight portion of 5 are added into a reaction kettle 200, ammonia with the weight portion of 60 is started at the temperature of 0-5 ℃, and after the completion, 50 weight portions of methyl chloroacetate are weighted, and the temperature is kept for 1 hour. Slowly heating to 30 ℃, continuously introducing ammonia gas, controlling the temperature between 30 ℃ and 35 ℃ for reaction for 2 hours, sampling and detecting that the raw material residue is less than 0.5%, distilling ammonia water after the reaction is finished for recovery, adding 50 parts by weight of methanol, cooling and crystallizing and filtering to obtain 42 parts by weight of crude glycinamide hydrochloride, and recrystallizing the crude product by 50 parts by weight of methanol to obtain 40 parts by weight of product with the melting point of 201-204 ℃, the content of more than 99.5% and the yield of 78.59%.
In the embodiment, 200 parts by weight of reaction water and 2.5 parts by weight of catalyst are added into a reaction kettle 200, 60 parts by weight of ammonia gas is started at the temperature of 0-5 ℃,50 parts by weight of methyl chloroacetate is weighted after the completion of the reaction, and the reaction is kept for 1 hour. Slowly heating to 30 ℃, continuously introducing ammonia gas, controlling the temperature between 30 and 35 ℃, reacting for 4.5 hours, sampling and detecting, distilling out ammonia water after the reaction is finished for recycling, adding 50 parts by weight of methanol, cooling and crystallizing and filtering to obtain 36 parts by weight of crude glycinamide hydrochloride, recrystallizing the crude product by 50 parts by weight of methanol to obtain 32.4 parts by weight of product, wherein the melting point is 198-203 ℃, the content is more than 98%, and the yield is 63.65%.
In the embodiment, reaction water with the weight portion of 200 and catalyst with the weight portion of 10 are added into a reaction kettle 200, ammonia with the weight portion of 60 is started at the temperature of 0-5 ℃, and after the completion, 50 weight portions of methyl chloroacetate are weighted, and the temperature is kept for 1 hour. Slowly heating to 30 ℃, continuously introducing ammonia gas, controlling the temperature between 30 and 35 ℃, reacting for 2 hours, sampling and detecting, distilling out ammonia water after the reaction is finished to recover the raw material residue less than 0.5%, adding 50 parts by weight of methanol, cooling and crystallizing and filtering to obtain 41.6 parts by weight of crude glycinamide hydrochloride, and recrystallizing the crude product by 50 parts by weight of methanol to obtain 39.4 parts by weight of product, wherein the melting point is 201-203 ℃, the content is more than 99.5%, and the yield is 77.4%.
The catalyst of the invention is ammonium carbonate, and the chloroacetate is methyl chloroacetate or ethyl chloroacetate.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.
Claims (10)
1. A process for the preparation of glycinamide hydrochloride comprising the steps of:
s1, firstly, adding 2.5-10.0 parts by weight of catalyst into a feeder, and pumping the reaction water in a reaction water tank into a reaction kettle of a reactor through a pressure pump until the weight of the reaction water is 180-240;
s2, introducing cold water into a water bath box of the reactor to enable the temperature in the reaction kettle to be 0-5 ℃;
s3, introducing 60 parts by weight of ammonia into the reaction kettle, and adding 50 parts by weight of chloroacetate through a feeder;
s4, controlling a pressure pump to pump out the solution in the reaction kettle and then pumping the solution into the reaction kettle, so that the solution is circulated, chloroacetate in a feeder is completely dissolved into the solution, and then stopping the pressure pump;
s5, operating the clutch mechanism to change the stirring type crystal attachment mechanism into a stirring type, and driving the stirring type crystal attachment mechanism in the reaction kettle to rotate in the reaction kettle to perform stirring reaction;
s6, after the stirring reaction is completed, cold water in the water bath box is pumped out, warm water is introduced into the water bath box until the temperature in the reaction kettle is increased to 30-35 ℃, ammonia gas is continuously introduced, and the temperature is kept at 30-35 ℃;
s7, reacting for 2-3 hours, heating the reaction kettle to distill ammonia and reaction water in the reaction kettle to obtain the ammonia and the reaction water, adding 50 parts by weight of methanol, extracting hot water in the water bath tank, introducing cold water into the water bath tank, cooling and crystallizing to obtain a crude product, and extracting methanol carrying impurities in the reaction kettle;
s8, replacing cold water in the water bath tank with warm water until the temperature in the reaction kettle is increased to 30-35 ℃, introducing 50 parts by weight of methanol into the reaction kettle, dissolving the crude product in the methanol, and then performing cooling operation to recrystallize the crude product to obtain glycinamide hydrochloride crystals;
s9, extracting methanol from the reaction kettle, operating the clutch mechanism to enable the stirring type crystal attachment mechanism to be in a crystal scraping state, driving the stirring type crystal attachment mechanism to act, enabling the glycinamide hydrochloride crystals attached to the inner wall of the reaction kettle and the stirring type crystal attachment mechanism to fall off, operating the clutch mechanism again to enable the stirring type crystal attachment mechanism to be in a stirring state, driving the stirring type crystal attachment mechanism to rotate, and enabling the glycinamide hydrochloride crystals in the reaction kettle to be gradually conveyed to a discharge joint and collected by the collecting box.
2. A process for the preparation of glycinamide hydrochloride according to claim 1 wherein: the water bath box comprises a box body, the lower end of the box body is supported on the ground through a plurality of supporting legs, the upper end of the box body is in an open state, a water inlet joint and a water outlet joint are respectively constructed on two opposite side walls of the box body, and a water inlet main valve and a water outlet main valve are respectively installed on the water inlet joint and the water outlet joint.
3. A process for the preparation of glycinamide hydrochloride according to claim 1 wherein: the reaction kettle is arranged in the water bath box, the stirring type crystal attachment mechanism is arranged in the reaction cavity of the reaction kettle, the number of the clutch mechanisms is two, the two clutch mechanisms are respectively arranged at the two axial ends of the horizontal kettle body, and the clutch mechanisms are constructed at the same side end parts of the horizontal kettle body and the stirring type crystal attachment mechanism.
4. A process for the preparation of glycinamide hydrochloride according to claim 3 wherein: the reaction kettle comprises a cylindrical horizontal kettle body, end covers are detachably connected to the axial ends of the horizontal kettle body, a steam outlet connector and a discharging connector are respectively constructed at the upper end and the lower end of the horizontal kettle body, one end of a communicating elbow is communicated with the lower end of the horizontal kettle body, and the other end of the communicating elbow is communicated with the outside through a stirring type crystal attachment mechanism.
5. The process for preparing glycinamide hydrochloride according to claim 4 wherein: the stirring type crystal attachment mechanism comprises an assembly shaft, a first spiral blade and a second spiral blade which are coaxially assembled in the horizontal kettle body, the first spiral blade and the second spiral blade have the same structure, both extend spirally along the axial direction of the assembly shaft, and the end parts of the ends of the second spiral blade are connected with corresponding end covers through conical springs; two ends of the assembly shaft extend out of the horizontal kettle body through corresponding end covers respectively, the assembly shaft is rotationally connected with the two end covers, the first spiral blade is fixedly connected with the assembly shaft, and the second spiral blade is movably sleeved outside the assembly shaft; one end of the assembly shaft is provided with a driving wheel which is driven to drive the assembly shaft to rotate.
6. The process for preparing glycinamide hydrochloride according to claim 5 wherein: the assembly shaft is provided with a supply and discharge channel which coincides with the axis of the assembly shaft, the supply and discharge channel extends from one end of the assembly shaft to the other end of the assembly shaft, the communication elbow is rotationally assembled at one end of the assembly shaft far away from the driving wheel, the communication elbow is communicated with the supply and discharge channel, and a supply and discharge valve is arranged on the communication elbow.
7. The process for preparing glycinamide hydrochloride according to claim 5 wherein: the assembly shaft is provided with a plurality of air supply channels, each air supply channel extends along the axial direction of the assembly shaft, the part of each air supply channel in the horizontal kettle body is communicated with the reaction cavity through a plurality of air outlet holes, the air outlet holes are arranged on the assembly shaft at intervals along the axial direction of the assembly shaft, and the part of each air supply channel in the outside of the horizontal kettle body is communicated with the outside through a conducting hole arranged on the assembly shaft; the assembly shaft is provided with a distribution sleeve in a rotating mode at the position of the guide hole, the distribution sleeve is provided with an air supply connector, and the air supply connector is communicated with the reaction cavity through the distribution sleeve, the guide hole, the air supply channel and the air outlet hole.
8. The process for preparing glycinamide hydrochloride according to claim 5 wherein: annular fixing seats are fixedly connected to the two ends of the second spiral blade respectively, the large-diameter ends of the conical springs are arranged on the corresponding annular fixing seats, the small-diameter ends of the conical springs are connected with adapter seats, and the adapter seats are rotatably connected to corresponding end covers.
9. A process for the preparation of glycinamide hydrochloride according to claim 8 wherein: the clutch mechanism comprises an inner gear ring, a movable clutch piece and a transmission gear, wherein the inner gear ring, the movable clutch piece and the transmission gear are sequentially arranged outwards along the axis of the assembly shaft, the inner gear ring is arranged on the outer side of the end cover, the transmission gear is arranged at the end part of the assembly shaft, and the movable clutch piece is sleeved outside the assembly shaft.
10. A process for the preparation of glycinamide hydrochloride according to claim 9 wherein: the movable clutch piece comprises a clutch gear ring which is overlapped with the axes of the inner gear ring and the transmission gear, inner gear teeth are uniformly constructed on the inner peripheral wall of the clutch gear ring along the circumferential direction of the clutch gear ring, outer gear teeth are uniformly constructed on the outer peripheral wall of the clutch gear ring along the circumferential direction of the clutch gear ring, the clutch gear ring is connected with a rotating ring through two connecting arms, the rotating ring is rotationally connected in an annular groove of the connecting ring, the axes of the rotating ring, the connecting ring and the clutch gear ring are overlapped, guide posts are constructed on the adapter at intervals, each guide post penetrates through the clutch gear ring along the axial direction of an assembly shaft, the guide posts are in sliding connection with the clutch gear ring, and the lower end of an operating rod is hinged to the upper end of the connecting ring; when the inner gear of the clutch gear ring is meshed with the transmission gear, the stirring type crystal attachment mechanism is changed into a stirring type, and the first spiral blade and the second spiral blade synchronously rotate when the assembly shaft is driven to rotate; when the outer gear of the clutch gear ring is meshed with the inner gear ring, the stirring type crystal attachment mechanism is changed into a scraping type state, the first spiral blade rotates along with the assembly shaft, and the second spiral blade is indirectly and fixedly connected with the end cover through the conical spring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311427048.6A CN117486745A (en) | 2023-10-31 | 2023-10-31 | Preparation method of glycinamide hydrochloride |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311427048.6A CN117486745A (en) | 2023-10-31 | 2023-10-31 | Preparation method of glycinamide hydrochloride |
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| CN202311427048.6A Pending CN117486745A (en) | 2023-10-31 | 2023-10-31 | Preparation method of glycinamide hydrochloride |
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