CN112266335A - Preparation process of aminoacetonitrile hydrochloride - Google Patents
Preparation process of aminoacetonitrile hydrochloride Download PDFInfo
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- CN112266335A CN112266335A CN202011291902.7A CN202011291902A CN112266335A CN 112266335 A CN112266335 A CN 112266335A CN 202011291902 A CN202011291902 A CN 202011291902A CN 112266335 A CN112266335 A CN 112266335A
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- motor
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- mixed solution
- fixedly connected
- centrifugal barrel
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- XFKYKTBPRBZDFG-UHFFFAOYSA-N 2-aminoacetonitrile;hydrochloride Chemical compound Cl.NCC#N XFKYKTBPRBZDFG-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 84
- 239000011259 mixed solution Substances 0.000 claims abstract description 49
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000010438 heat treatment Methods 0.000 claims abstract description 35
- 239000000243 solution Substances 0.000 claims abstract description 30
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 28
- 238000002347 injection Methods 0.000 claims abstract description 21
- 239000007924 injection Substances 0.000 claims abstract description 21
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims description 37
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 30
- 230000006835 compression Effects 0.000 claims description 16
- 238000007906 compression Methods 0.000 claims description 16
- 230000001681 protective effect Effects 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000004140 cleaning Methods 0.000 claims description 14
- 238000005096 rolling process Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- KXZJHVJKXJLBKO-UHFFFAOYSA-N chembl1408157 Chemical compound N=1C2=CC=CC=C2C(C(=O)O)=CC=1C1=CC=C(O)C=C1 KXZJHVJKXJLBKO-UHFFFAOYSA-N 0.000 claims description 11
- 238000005192 partition Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 5
- 230000005484 gravity Effects 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 230000007246 mechanism Effects 0.000 abstract description 15
- 239000013067 intermediate product Substances 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 2
- 238000005119 centrifugation Methods 0.000 description 5
- GFZMFCVDDFHSJK-UHFFFAOYSA-N 2-(methylideneamino)acetonitrile Chemical compound C=NCC#N GFZMFCVDDFHSJK-UHFFFAOYSA-N 0.000 description 4
- 230000002146 bilateral effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- TWBNMYSKRDRHAT-RCWTXCDDSA-N (S)-timolol hemihydrate Chemical compound O.CC(C)(C)NC[C@H](O)COC1=NSN=C1N1CCOCC1.CC(C)(C)NC[C@H](O)COC1=NSN=C1N1CCOCC1 TWBNMYSKRDRHAT-RCWTXCDDSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- ANMATWQYLIFGOK-UHFFFAOYSA-N Iguratimod Chemical compound CS(=O)(=O)NC1=CC=2OC=C(NC=O)C(=O)C=2C=C1OC1=CC=CC=C1 ANMATWQYLIFGOK-UHFFFAOYSA-N 0.000 description 1
- HFCYZXMHUIHAQI-UHFFFAOYSA-N Thidiazuron Chemical compound C=1C=CC=CC=1NC(=O)NC1=CN=NS1 HFCYZXMHUIHAQI-UHFFFAOYSA-N 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000002220 antihypertensive agent Substances 0.000 description 1
- 239000003435 antirheumatic agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003925 brain function Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229950003909 iguratimod Drugs 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 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
- 239000000575 pesticide Substances 0.000 description 1
- 239000005648 plant growth regulator Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229960004605 timolol Drugs 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/08—Preparation of carboxylic acid nitriles by addition of hydrogen cyanide or salts thereof to unsaturated compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation process of aminoacetonitrile hydrochloride, which comprises the steps of injecting ammonia chloride, formaldehyde and water from a material injection pipe on a reaction preparation device, starting a first motor, rotating the end part of an output shaft of the first motor to drive a speed reducer to rotate so as to drive a rotating rod to rotate, rotating a stirring frame fixedly connected with the rotating rod along with the rotating rod, and stirring a first mixed solution formed by the ammonia chloride, the formaldehyde and the water; through set up rabbling mechanism and centrifugal mechanism simultaneously in reation kettle, reduce the equipment volume size in the whole preparation process to set up the heating rod on rabbling mechanism, realize reaction temperature's control, float on the rabbling mechanism and set up and clean the inner wall that the mechanism can be automatic cleans reation kettle, can the pollution abatement, the intermediate product that produces in the reduction solution reaction is attached to on the reation kettle inner wall.
Description
Technical Field
The invention relates to a preparation process of hydrochloride, in particular to a preparation process of aminoacetonitrile hydrochloride.
Background
The aminoacetonitrile hydrochloride is an important intermediate of medicines and pesticides, and can be used for synthesizing various organic compounds, such as a plant growth regulator thidiazuron, a brain function improver oxiracetam, an antirheumatic drug Iguratimod, an ocular hypotensive drug timolol and the like.
At present, the commonly adopted process is that sodium cyanide, formaldehyde, ammonium chloride and the like are used as raw materials to synthesize a one-step intermediate methylene amino acetonitrile, and then the methylene amino acetonitrile reacts in a hydrogen chloride alcohol solution to obtain amino acetonitrile hydrochloride. The disadvantages of this method are mainly three points: firstly, the process is long, three times of solid-liquid separation and two times of solid drying are needed, the production period is long, the energy consumption is large, and the equipment occupation is large. Secondly, the wastewater amount is large, and the wastewater is difficult to treat due to high cyanide, high COD, high ammonia nitrogen and high salt, so that the wastewater treatment cost is increased. Thirdly, the yield is low, the product quality is unstable, therefore, the preparation process of the aminoacetonitrile hydrochloride is provided.
Disclosure of Invention
The invention aims to provide a preparation process of aminoacetonitrile hydrochloride.
The technical problem solved by the invention is as follows: through set up rabbling mechanism and centrifugal mechanism simultaneously in reation kettle, reduce the equipment volume size in the whole preparation process to set up the heating rod on rabbling mechanism, realize reaction temperature's control, float on the rabbling mechanism and set up and clean the inner wall that the mechanism can be automatic cleans reation kettle, can the pollution abatement, the intermediate product that produces in the reduction solution reaction is attached to on the reation kettle inner wall.
The purpose of the invention can be realized by the following technical scheme: the preparation process of the aminoacetonitrile hydrochloride specifically comprises the following steps:
the method comprises the following steps: injecting ammonia chloride, formaldehyde and water from an injection pipe on a reaction preparation device, starting a first motor, rotating the end part of an output shaft of the first motor to drive a speed reducer to rotate so as to drive a rotating rod to rotate, rotating a stirring frame fixedly connected with the rotating rod along with the rotating rod to stir a first mixed solution formed by the ammonia chloride, the formaldehyde and the water, after the first mixed solution is uniformly stirred, injecting a sodium cyanide solution into the first mixed solution through the injection pipe to obtain a second mixed solution, adding acetic acid into the second mixed solution when the volume of the injected sodium cyanide solution is half of that of the first mixed solution, after the addition of the acetic acid is finished, starting the first motor again to stir the final mixed solution, electrifying a stirring heating rod in the stirring process, heating the final mixed solution, raising the temperature of the final mixed solution to 35-40 ℃, and adding a catalyst into the final mixed solution;
step two: when the temperature of the final mixed liquid reaches 35-40 ℃, the first motor is closed, the stirring of the final mixed liquid is stopped, the heating of the final mixed liquid is stopped, the final mixed liquid is kept standing for reaction for 2 hours, then the electromagnetic valve is opened, the solution after the reaction enters the centrifugal barrel through the connecting pipe, the methanol solution of hydrogen chloride is pre-filled in the centrifugal barrel, after the standing reaction is carried out for 1 hour, the second motor is started, the end part of the output shaft of the second motor drives the centrifugal barrel to rotate, a roller rotationally connected with the centrifugal barrel through a short pin rolls in the rolling groove, the solution in the centrifugal barrel and the resultant are centrifugally separated, aminoacetonitrile hydrochloride powder is obtained, and the separated liquid slides along the inner wall of the reaction kettle under the action of gravity and is discharged through a liquid discharge pipe.
The invention has further technical improvements that: the reaction preparation device comprises a reaction kettle, support rods, a top cover, a material injection pipe, a speed reducer, a first motor, a liquid discharge pipe, a stirring frame, a stirring heating rod, a rotary rod, a cleaning head, a sleeve seat, a connecting column, a compression spring, a partition plate, a connecting pipe, an electromagnetic valve, a centrifugal barrel, a short pin, a roller, a connecting rod, a protective box and a second motor, wherein the three support rods are arranged on the outer side of the reaction kettle at equal angles, the support rods are fixedly connected with the reaction kettle, the top cover is arranged at the top of the reaction kettle, and the top cover is fixedly connected with the reaction kettle through bolts;
a speed reducer is fixedly connected right above the top cover, a first motor is arranged at the top of the speed reducer, the end part of an output shaft of the first motor is fixedly connected with the input end of the speed reducer, the output end of the speed reducer is fixedly connected with a rotating rod, a material injection pipe is arranged on one side of the speed reducer, the material injection pipe is communicated with the top cover, and a liquid discharge pipe is communicated with the bottom of the reaction kettle;
the reaction kettle is internally provided with a stirring frame, a partition plate is arranged under the stirring frame and is fixedly connected with the inner wall of the reaction kettle, one end of a speed reducer far away from a rotary rod is rotatably connected with the partition plate through a bearing, the top of the stirring frame is provided with a circular mounting hole, the rotary rod is arranged in the circular mounting hole and is fixedly connected with the stirring frame, the stirring frame is provided with a stirring heating component at an equal angle, the stirring heating component consists of two stirring heating rods which are arranged in parallel, the stirring heating rods are fixedly connected with the stirring frame, the stirring frame is provided with four cleaning mounting grooves at an equal angle, a plurality of sleeve seats are arranged in the cleaning mounting grooves at equal intervals, the sleeve seats are fixedly connected with the stirring frame, compression springs are arranged in the sleeve seats, and one ends of the compression springs are fixedly connected with the bottoms of the cleaning mounting grooves, the other end fixedly connected with spliced pole of compression spring, the one end setting of spliced pole is in the cover seat and spliced pole and cover seat sliding connection, it is provided with the cleaning head to clean the mounting groove, the one end and the cleaning head fixed connection that compression spring was kept away from to the spliced pole.
The invention has further technical improvements that: the below symmetry of division board is provided with the connecting pipe, connecting pipe and division board through connection, the one end fixedly connected with solenoid valve of division board is kept away from to the connecting pipe, the one end through connection that the connecting pipe was kept away from to the solenoid valve has the drain pipe.
The invention has further technical improvements that: be provided with the centrifugation bucket under the division board, the bilateral symmetry of centrifugation bucket is provided with the short round pin, the one end and the centrifugation bucket fixed connection of short round pin, the other end of short round pin rotate and are connected with the short round pin, the rolling groove has been seted up to reation kettle's inner wall, the short round pin sets up in the rolling groove, and short round pin and reation kettle roll connection, be provided with the protective housing under the centrifugation bucket, the bilateral symmetry of protective housing is provided with the connecting rod, the protective housing passes through connecting rod and reation kettle fixed connection, fixed mounting has the second motor in the protective housing, the output shaft tip of second motor and the bottom fixed connection of centrifugation bucket.
Compared with the prior art, the invention has the beneficial effects that:
injecting ammonia chloride, formaldehyde and water from an injection pipe on a reaction preparation device, starting a first motor, rotating the end part of an output shaft of the first motor to drive a speed reducer to rotate so as to drive a rotating rod to rotate, rotating a stirring frame fixedly connected with the rotating rod along with the rotating rod to stir a first mixed solution formed by the ammonia chloride, the formaldehyde and the water, after the first mixed solution is uniformly stirred, injecting a sodium cyanide solution into the first mixed solution through the injection pipe to obtain a second mixed solution, adding acetic acid into the second mixed solution when the volume of the injected sodium cyanide solution is half of that of the first mixed solution, after the addition of the acetic acid is finished, starting the first motor again to stir the final mixed solution, electrifying a stirring heating rod in the stirring process, heating the final mixed solution, raising the temperature of the final mixed solution to 35-40 ℃, and adding a catalyst into the final mixed solution; when the temperature of the final mixed liquid reaches 35-40 ℃, the first motor is closed, the stirring of the final mixed liquid is stopped, the heating of the final mixed liquid is stopped, the final mixed liquid is kept standing for reaction for 2 hours, then the electromagnetic valve is opened, the solution after the reaction enters the centrifugal barrel through the connecting pipe, the methanol solution of hydrogen chloride is pre-filled in the centrifugal barrel, after the standing reaction is carried out for 1 hour, the second motor is started, the end part of the output shaft of the second motor drives the centrifugal barrel to rotate, a roller rotationally connected with the centrifugal barrel through a short pin rolls in the rolling groove, the solution and the resultant in the centrifugal barrel are centrifugally separated, aminoacetonitrile hydrochloride powder is obtained, the separated liquid slides along the inner wall of the reaction kettle under the action of gravity and is discharged through a liquid discharge pipe, the volume of the equipment in the whole preparation process is reduced by simultaneously arranging the stirring mechanism and the centrifugal mechanism in the reaction kettle, the heating rod is arranged on the stirring mechanism, so that the control of the reaction temperature is realized, the cleaning mechanism is arranged on the stirring mechanism in a floating mode, the inner wall of the reaction kettle can be automatically cleaned, the pollution can be reduced, and the adhesion of intermediate products generated in the solution reaction to the inner wall of the reaction kettle is reduced.
Drawings
In order to facilitate understanding for those skilled in the art, the present invention will be further described with reference to the accompanying drawings.
FIG. 1 is a schematic front view of the overall structure of the present invention;
FIG. 2 is a schematic view of the internal structure of the reaction vessel of the present invention;
FIG. 3 is an enlarged view of the detail of area A in FIG. 2 according to the present invention;
FIG. 4 is a schematic view of the connection structure of the stirring frame and the stirring heating rod of the present invention.
In the figure: 1. a reaction kettle; 2. a support bar; 3. a top cover; 4. a material injection pipe; 5. a speed reducer; 6. a first motor; 7. a liquid discharge pipe; 8. a stirring frame; 9. stirring a heating rod; 10. rotating the rod; 11. cleaning the head; 12. a sleeve seat; 13. connecting columns; 14. a compression spring; 15. a partition plate; 16. a connecting pipe; 17. an electromagnetic valve; 18. a centrifuge bucket; 19. a short pin; 20. a roller; 21. a connecting rod; 22. a protective box; 23. a second motor; 101. cleaning the installation groove; 102. and (4) rolling the groove.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-4, a process for preparing aminoacetonitrile hydrochloride, the process specifically comprises the following steps:
the method comprises the following steps: injecting ammonia chloride, formaldehyde and water from an injection pipe 4 on the reaction preparation device, starting a first motor 6, rotating the end part of an output shaft of the first motor 6 to drive a speed reducer 5 to rotate, thereby driving the rotating rod 10 to rotate, the stirring frame 8 fixedly connected with the rotating rod 10 rotates along with the rotating rod, stirring a first mixed solution formed by ammonia chloride, formaldehyde and water, injecting a sodium cyanide solution into the first mixed solution through an injection pipe 4 to obtain a second mixed solution after uniformly stirring, when the volume of the injected sodium cyanide solution is half of that of the first mixed solution, adding acetic acid into the second mixed solution, after the addition of the acetic acid is finished, the first motor 6 is started again to stir the final mixed liquid, the stirring heating rod 9 is electrified in the stirring process, heating the final mixed solution, raising the temperature of the final mixed solution to 35-40 ℃, and adding a catalyst into the final mixed solution;
step two: when the temperature of the final mixed liquid reaches 35-40 ℃, the first motor 6 is closed, the stirring of the final mixed liquid is stopped, the heating of the final mixed liquid is stopped, the final mixed liquid is kept standing for 2 hours, then the electromagnetic valve 17 is opened, the reacted solution enters the centrifugal barrel 18 through the connecting pipe 16, the methanol solution of hydrogen chloride is pre-filled in the centrifugal barrel 18, after the mixture is kept standing for 1 hour, the second motor 23 is started, the end part of the output shaft of the second motor 23 drives the centrifugal barrel 18 to rotate, the roller 20 which is rotatably connected with the centrifugal barrel 18 through the short pin 19 rolls in the rolling groove 102, the solution and the resultant in the centrifugal barrel 18 are centrifugally separated, aminoacetonitrile hydrochloride powder is obtained, and the separated liquid slides along the inner wall of the reaction kettle 1 under the action of gravity and is discharged through the liquid discharge pipe 7.
The reaction preparation device comprises a reaction kettle 1, support rods 2, a top cover 3, a material injection pipe 4, a speed reducer 5, a first motor 6, a liquid discharge pipe 7, a stirring frame 8, a stirring heating rod 9, a rotary rod 10, a cleaning head 11, a sleeve seat 12, a connecting column 13, a compression spring 14, a partition plate 15, a connecting pipe 16, a solenoid valve 17, a centrifugal barrel 18, a short pin 19, a roller 20, a connecting rod 21, a protective box 22 and a second motor 23, wherein the three support rods 2 are arranged on the outer side of the reaction kettle 1 at equal angles, the support rods 2 are fixedly connected with the reaction kettle 1, the top cover 3 is arranged at the top of the reaction kettle 1, and the top cover 3 is fixedly connected with the reaction kettle 1 through bolts;
a speed reducer 5 is fixedly connected right above the top cover 3, a first motor 6 is arranged at the top of the speed reducer 5, the end part of an output shaft of the first motor 6 is fixedly connected with the input end of the speed reducer 5, the output end of the speed reducer 5 is fixedly connected with a rotating rod 10, a material injection pipe 4 is arranged on one side of the speed reducer 5, the material injection pipe 4 is communicated with the top cover 3, and a liquid discharge pipe 7 is communicated with the bottom of the reaction kettle 1;
the inside of reation kettle 1 is provided with stirring frame 8, set up division board 15 under stirring frame 8, division board 15 and reation kettle 1's inner wall fixed connection, the one end of speed reducer 5 that rotary rod 10 kept away from passes through the bearing and is connected with division board 15 rotation, circular mounting hole has been seted up at the top of stirring frame 8, rotary rod 10 sets up in circular mounting hole, and rotary rod 10 and stirring frame 8 fixed connection, the equidistance is provided with stirring heating element on stirring frame 8, stirring heating element comprises two parallel arrangement's stirring heating rod 9, stirring heating rod 9 and stirring frame 8 all fixed connection, the equidistance is seted up four on stirring frame 8 and is cleaned mounting groove 101, it is provided with a plurality of cover seat 12 to clean the equidistance in mounting groove 101, cover seat 12 and stirring frame 8 fixed connection, set up compression spring 14 in cover seat 12, compression spring 14's one end with clean mounting groove 101 bottom fixed connection, compression spring 14's other end fixedly connected with spliced pole 13, the one end setting of spliced pole 13 is in cover seat 12 and spliced pole 13 and cover seat 12 sliding connection, it is provided with cleaning head 11 in the mounting groove 101 to clean, the one end and the cleaning head 11 fixed connection of compression spring 14 are kept away from to spliced pole 13.
The below symmetry of division board 15 is provided with connecting pipe 16, connecting pipe 16 and division board 15 through connection, the one end fixedly connected with solenoid valve 17 of division board 15 is kept away from to connecting pipe 16, the one end through connection that connecting pipe 16 was kept away from to solenoid valve 17 has the drain pipe.
Be provided with centrifuge drum 18 under division board 15, centrifuge drum 18's bilateral symmetry is provided with short round pin 19, short round pin 19's one end and centrifuge drum 18 fixed connection, short round pin 19's the other end rotate and be connected with short round pin 19, rolling groove 102 has been seted up to reation kettle 1's inner wall, short round pin 19 sets up in rolling groove 102, and short round pin 19 and reation kettle 1 roll connection, be provided with protective housing 22 under centrifuge drum 18, protective housing 22's bilateral symmetry is provided with connecting rod 21, protective housing 22 passes through connecting rod 21 and reation kettle 1 fixed connection, fixed mounting has second motor 23 in protective housing 22, the output shaft tip of second motor 23 and centrifuge drum 18's bottom fixed connection.
The working principle is as follows: when the device is used, ammonia chloride, formaldehyde and water are injected from the material injection pipe on the reaction preparation device, the first motor is started, the end part of the output shaft of the first motor rotates to drive the speed reducer to rotate, so that the rotating rod is driven to rotate, the stirring frame fixedly connected with the rotating rod rotates along with the rotating rod, stirring a first mixed solution formed by ammonia chloride, formaldehyde and water, injecting a sodium cyanide solution into the first mixed solution through an injection pipe after uniformly stirring to obtain a second mixed solution, when the volume of the injected sodium cyanide solution is half of that of the first mixed solution, adding acetic acid into the second mixed solution, after the addition of the acetic acid is finished, the first motor is started again to stir the final mixed liquid, the stirring heating rod is electrified in the stirring process, heating the final mixed solution, raising the temperature of the final mixed solution to 35-40 ℃, and adding a catalyst into the final mixed solution; when the temperature of the final mixed liquid reaches 35-40 ℃, the first motor is closed, the stirring of the final mixed liquid is stopped, the heating of the final mixed liquid is stopped, the final mixed liquid is kept standing for reaction for 2 hours, then the electromagnetic valve is opened, the solution after the reaction enters the centrifugal barrel through the connecting pipe, the methanol solution of hydrogen chloride is pre-filled in the centrifugal barrel, after the standing reaction is carried out for 1 hour, the second motor is started, the end part of the output shaft of the second motor drives the centrifugal barrel to rotate, a roller rotationally connected with the centrifugal barrel through a short pin rolls in the rolling groove, the solution in the centrifugal barrel and the resultant are centrifugally separated, aminoacetonitrile hydrochloride powder is obtained, and the separated liquid slides along the inner wall of the reaction kettle under the action of gravity and is discharged through a liquid discharge pipe.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "left", "right", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation and a specific orientation configuration and operation, and thus, should not be construed as limiting the present invention. Furthermore, "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and the like are to be construed broadly and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be directly connected or indirectly connected through an intermediate member, or they may be connected through two or more elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
While one embodiment of the present invention has been described in detail, the description is only a preferred embodiment of the present invention and should not be taken as limiting the scope of the invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (4)
1. A preparation process of aminoacetonitrile hydrochloride is characterized in that: the preparation process of the aminoacetonitrile hydrochloride specifically comprises the following steps:
the method comprises the following steps: injecting ammonia chloride, formaldehyde and water from an injection pipe (4) on a reaction preparation device, starting a first motor (6), rotating the end part of an output shaft of the first motor (6) to drive a speed reducer (5) to rotate so as to drive a rotary rod (10) to rotate, rotating a stirring frame (8) fixedly connected with the rotary rod (10) along with the first motor to stir a first mixed solution formed by the ammonia chloride, the formaldehyde and the water, after the uniform stirring, injecting a sodium cyanide solution into the first mixed solution through the injection pipe (4) to obtain a second mixed solution, adding acetic acid into the second mixed solution when the volume of the injected sodium cyanide solution is half of that of the first mixed solution, after the acetic acid is added, starting the first motor (6) again to stir the final mixed solution, electrifying a stirring heating rod (9) in the stirring process, heating the final mixed solution, raising the temperature of the final mixed solution to 35-40 ℃, and adding a catalyst thereto;
step two: when the temperature of the final mixed solution reaches 35-40 ℃, the first motor (6) is closed, the stirring of the final mixed solution is stopped, and the heating of the final mixed solution is stopped, the final mixed solution is kept standing for reaction for a support rod (2) hours, then opening an electromagnetic valve (17) to enable the solution after reaction to enter a centrifugal barrel (18) through a connecting pipe (16), pre-filling a methanol solution of hydrogen chloride in the centrifugal barrel (18), standing for reaction for 1h, the second motor (23) is started, the end part of an output shaft of the second motor (23) drives the centrifugal barrel (18) to rotate, a roller (20) which is rotationally connected with the centrifugal barrel (18) through a short pin (19) rolls in the rolling groove (102), and (3) centrifugally separating the solution and the product in the centrifugal barrel (18) to obtain aminoacetonitrile hydrochloride powder, wherein the separated liquid slides down along the inner wall of the reaction kettle (1) under the action of gravity and is discharged through a liquid discharge pipe (7).
2. The aminoacetonitrile hydrochloride preparation process of claim 1, wherein the reaction preparation device comprises a reaction kettle (1), support rods (2), a top cover (3), a material injection pipe (4), a speed reducer (5), a first motor (6), a liquid discharge pipe (7), a stirring rack (8), a stirring heating rod (9), a rotary rod (10), a cleaning head (11), a sleeve seat (12), a connecting column (13), a compression spring (14), a partition plate (15), a connecting pipe (16), an electromagnetic valve (17), a centrifugal barrel (18), a short pin (19), a roller (20), a connecting rod (21), a protective box (22) and a second motor (23), wherein three support rods (2) are arranged at equal angles outside the reaction kettle (1), the support rods (2) are fixedly connected with the reaction kettle (1), the top cover (3) is arranged at the top of the reaction kettle (1), the top cover (3) is fixedly connected with the reaction kettle (1) through bolts;
a speed reducer (5) is fixedly connected right above the top cover (3), a first motor (6) is arranged at the top of the speed reducer (5), the end part of an output shaft of the first motor (6) is fixedly connected with the input end of the speed reducer (5), the output end of the speed reducer (5) is fixedly connected with a rotating rod (10), a material injection pipe (4) is arranged on one side of the speed reducer (5), the material injection pipe (4) is communicated with the top cover (3), and a liquid discharge pipe (7) is communicated with the bottom of the reaction kettle (1);
the inside of reation kettle (1) is provided with stirring frame (8), set up division board (15) under stirring frame (8), division board (15) and the inner wall fixed connection of reation kettle (1), the one end of speed reducer (5) that rotary rod (10) kept away from is passed through the bearing and is connected with division board (15) rotation, circular mounting hole has been seted up at the top of stirring frame (8), rotary rod (10) set up in circular mounting hole, and rotary rod (10) and stirring frame (8) fixed connection, the first-class angle of stirring frame (8) is provided with stirring heating element, stirring heating element comprises two parallel arrangement's stirring heating rod (9), stirring heating rod (9) and stirring frame (8) equal fixed connection, the first-class angle of stirring frame (8) has been seted up four and has been cleaned mounting groove (101), it sets up seat (12) to clean in mounting groove (101), cover seat (12) and stirring frame (8) fixed connection, set up compression spring (14) in cover seat (12), the one end of compression spring (14) with clean mounting groove (101) bottom fixed connection, the other end fixedly connected with spliced pole (13) of compression spring (14), the one end setting of spliced pole (13) is in cover seat (12) and spliced pole (13) and cover seat (12) sliding connection, it cleans first (11) to be provided with in mounting groove (101), the one end and the cleaning head (11) fixed connection of compression spring (14) are kept away from in spliced pole (13).
3. The preparation process of aminoacetonitrile hydrochloride according to claim 2 characterized in that connecting pipes (16) are symmetrically arranged below the partition plate (15), the connecting pipes (16) are connected with the partition plate (15) in a through manner, one end of the connecting pipe (16) far away from the partition plate (15) is fixedly connected with an electromagnetic valve (17), and one end of the electromagnetic valve (17) far away from the connecting pipe (16) is connected with a liquid outlet pipe in a through manner.
4. The aminoacetonitrile hydrochloride preparation process of claim 2 characterized in that a centrifugal barrel (18) is arranged right below the partition plate (15), short pins (19) are symmetrically arranged on both sides of the centrifugal barrel (18), one end of the short pin (19) is fixedly connected with the centrifugal barrel (18), the other end of the short pin (19) is rotatably connected with the short pin (19), a rolling groove (102) is arranged on the inner wall of the reaction kettle (1), the short pin (19) is arranged in the rolling groove (102), the short pin (19) is in rolling connection with the reaction kettle (1), a protective box (22) is arranged right below the centrifugal barrel (18), connecting rods (21) are symmetrically arranged on both sides of the protective box (22), the protective box (22) is fixedly connected with the reaction kettle (1) through the connecting rods (21), a second motor (23) is fixedly arranged in the protective box (22), the end part of an output shaft of the second motor (23) is fixedly connected with the bottom of the centrifugal barrel (18).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011291902.7A CN112266335A (en) | 2020-11-18 | 2020-11-18 | Preparation process of aminoacetonitrile hydrochloride |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011291902.7A CN112266335A (en) | 2020-11-18 | 2020-11-18 | Preparation process of aminoacetonitrile hydrochloride |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432501A (en) * | 2012-01-13 | 2012-05-02 | 太仓市茜泾化工有限公司 | Preparation method of aminoacetonitrile hydrochloride |
| CN102531960A (en) * | 2012-01-13 | 2012-07-04 | 太仓市茜泾化工有限公司 | Method for preparing aminoacetonitrile sulfate |
| CN206064402U (en) * | 2016-08-24 | 2017-04-05 | 庞荣花 | A kind of chemical reaction stir mixing device |
| CN109806826A (en) * | 2017-11-19 | 2019-05-28 | 湖北智权专利技术应用开发有限公司 | A kind of abstersive environmentally friendly reaction kettle of tool |
-
2020
- 2020-11-18 CN CN202011291902.7A patent/CN112266335A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432501A (en) * | 2012-01-13 | 2012-05-02 | 太仓市茜泾化工有限公司 | Preparation method of aminoacetonitrile hydrochloride |
| CN102531960A (en) * | 2012-01-13 | 2012-07-04 | 太仓市茜泾化工有限公司 | Method for preparing aminoacetonitrile sulfate |
| CN206064402U (en) * | 2016-08-24 | 2017-04-05 | 庞荣花 | A kind of chemical reaction stir mixing device |
| CN109806826A (en) * | 2017-11-19 | 2019-05-28 | 湖北智权专利技术应用开发有限公司 | A kind of abstersive environmentally friendly reaction kettle of tool |
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