Synthesis equipment and synthesis process of memantine hydrochloride

Abstract

The invention discloses synthesis equipment and a synthesis process of memantine hydrochloride, and relates to the technical field of memantine hydrochloride processing.The synthesis equipment comprises a reaction kettle body, a conveying pipe is arranged at the top end of the reaction kettle body, a discharging pipe is arranged at the bottom of the reaction kettle body, and a stirring assembly is arranged in the reaction kettle body; the device further comprises a sampling mechanism used for sampling and a sampling hole matched with the sampling mechanism, the sampling hole is formed in one side of the reaction kettle body, the sampling mechanism comprises an outer cylinder fixedly connected with the reaction kettle body, and a baffle is fixedly connected to the end, away from the reaction kettle body, of the interior of the outer cylinder. A first pushing assembly is fixedly connected to the baffle, an external connector matched with the sampling device is formed in the baffle, and a drainage assembly is arranged in the outer cylinder in a matched mode. The sampling efficiency can be improved, meanwhile, sample liquid can be prevented from being in direct contact with the outside, and the reliability of reference data is guaranteed.

Description

Technical Field

[0001] The invention relates to the technical field of memantine hydrochloride processing, and in particular to a synthesis device and a synthesis process of memantine hydrochloride. Background Art

[0002] Memantine hydrochloride is an anti-dementia drug for the treatment of moderate to severe Alzheimer's dementia. It is a dementia treatment drug developed by the German company Merz. It is a new, low-to-moderate affinity, voltage-dependent, non-competitive N-methyl-D-aspartate (NMDA) Chemibook receptor antagonist that can non-competitively block NMDA receptors, reduce excessive excitement of NMDA receptors caused by glutamate, prevent cell apoptosis, and improve memory. It is a new generation of drugs to improve cognitive function.

[0003] During the processing of memantine hydrochloride, the drug solution needs to be tested frequently. During the testing process, the stirring device and the negative pressure state of the reactor need to be closed to make the pressure of the reactor the same as the external air pressure. The sampling hole on the reactor is opened and some samples are extracted from the inside of the reactor through special tools. After the sampling is completed, the sampling hole is closed to complete the sampling process.

[0004] The shortcomings of the existing technical solutions are: during the sampling process of the reactor, the sampling hole needs to be opened. Since the locking device on the sampling hole is generally fixed by bolts, the opening and closing operations of the sampling hole are relatively cumbersome. When sampling, special tools need to be sent into the reactor to extract the sample liquid, and each step needs to be carefully performed to ensure the accuracy and safety of the sampling, which increases the difficulty of operation and time cost to a certain extent. Summary of the invention

[0005] The object of the present invention is to provide a synthesis device and a synthesis process of memantine hydrochloride, which solves the problem that in the sampling process of a reactor, since the locking device on the sampling hole is generally fixed by bolts, the opening and closing operations of the sampling hole are relatively cumbersome.

[0006] The purpose of the present invention can be achieved through the following technical solutions:

[0007] A synthesis device for memantine hydrochloride comprises a reactor body, a feeding pipe is arranged at the top of the reactor body, a discharging pipe is arranged at the bottom of the reactor body, a stirring assembly is arranged inside the reactor body, the device also comprises a sampling mechanism for sampling and a sampling hole matched with the sampling mechanism, the sampling hole is arranged on one side of the reactor body, the sampling mechanism comprises an outer cylinder fixedly connected to the reactor body, a baffle is fixedly connected to one end of the outer cylinder away from the reactor body, a first pushing assembly is fixedly connected to the baffle, an external interface matched with the sampling device is arranged on the baffle, a drainage assembly is matched inside the outer cylinder, a pressure-type one-way valve for liquid material flow is arranged on the drainage assembly, a sealing plug rod slidably matched with the sampling hole is fixedly connected to the output end of the first pushing assembly, the sealing plug rod slidably matches with the drainage assembly, and an observation assembly for observing the color of the liquid material is arranged on the outer cylinder.

[0008] As a further solution of the present invention: the drainage assembly includes a sealing push plate that slides with the inside of the outer cylinder, a second push assembly is fixedly connected to the baffle, an output end of the second push assembly is fixedly connected to the sealing push plate, the sealing push plate is slidably sleeved on the sealing plug rod, and the pressure-type one-way valve is arranged on the sealing push plate.

[0009] As a further solution of the present invention: the pressure-type one-way valve includes a through hole arranged on the sealing push plate, a spring with one end fixedly connected to the inner wall of the through hole, and a sealing valve plate fixedly connected to the other end of the spring.

[0010] As a further solution of the present invention: the observation assembly includes a lighting device arranged on one side of the outer tube, and an observation window arranged on the other side of the outer tube, and the lighting device and the observation window are both provided with a curved glass plate that matches the inner wall of the outer tube on the side close to the axis of the outer tube.

[0011] As a further solution of the present invention: the stirring assembly includes a motor fixedly connected to the reactor body, a transmission rod is rotatably connected inside the reactor body, a plurality of stirring plates are fixedly connected to the transmission rod at equal intervals, and the transmission rod is coaxially fixedly connected to the output end of the motor.

[0012] As a further solution of the present invention: each group of the stirring plates is fixedly connected to an oblique arc scraper at one end away from the transmission rod, and each group of the oblique arc scrapers is in contact with the inner wall of the reactor body at one side away from the stirring plates, and there is a certain angle between the oblique arc scrapers and the horizontal plane, and the angle ranges from 30° to 60°.

[0013] As a further solution of the present invention: a temperature control component is arranged on the outside of the reactor body, a high-position tank is arranged on the top of the reactor body, and a regulating valve is connected between the high-position tank and the reactor body.

[0014] As a further solution of the present invention: a tail gas output pipe is arranged on the top of the reactor body, a negative pressure device is arranged at one end of the tail gas output pipe away from the reactor body, and a condensing device is connected to the output end of the negative pressure device.

[0015] As a further solution of the present invention: a manhole cover is provided on the top of the reactor body.

[0016] A synthesis process of memantine hydrochloride comprises the following steps:

[0017] S1: Add 150-250 kg of drinking water and 30-50 kg of sodium sulfite to the reactor body in sequence and stir evenly;

[0018] S2: Then, 4.86*A±0.5kg of bromine is introduced. In this process, A is a proportional coefficient, and the value range of A is between 18 and 20. Then, the feed pipe is closed and the negative pressure device is started. The negative pressure device changes the inside of the reactor body into a negative pressure state through the tail gas output pipe;

[0019] S3: Control the temperature of the liquid inside the reactor body to between 10 and 20° C. through the temperature control component, and start stirring;

[0020] S4: Introduce 1*A kg 1,3-dimethyladamantane into the high-position tank, and control the drop rate of 1,3-dimethyladamantane by controlling the opening size of the regulating valve to ensure that the drop time range is between 3 and 5 hours, control the temperature control component, so that the temperature of the reaction liquid in the reactor body is between 15 and 25° C., and the reaction time is 24 hours;

[0021] S5: Take samples through the sampling mechanism to check whether the 1,3-dimethyladamantane content is less than 5%. If the test result meets the requirements, proceed to the next step. If the test result does not meet the requirements, continue stirring and take samples again for testing after at least two hours until the requirements are met;

[0022] S6: decompressing the interior of the reactor body by a negative pressure device, setting the initial circulation temperature between 30 and 35° C., achieving a decompression concentration operation on the reaction liquid, concentrating for 8 to 10 hours, and sampling to monitor bromine residue;

[0023] S7: Introduce 0.5*A kg of n-heptane with bromine into the high-level tank, control the temperature control component to set the temperature between 45 and 40° C., and reduce the pressure and concentrate until no condensate drips at the output end of the condensation device;

[0024] S8: Continue to repeat S6 operation until the condensate becomes colorless and transparent and no condensate drops;

[0025] S9: Continue to add 10.0±0.5*A kg of n-heptane, control the temperature control component to set the temperature between 55 and 50°C, continue to reduce pressure and concentrate until the condensate is colorless and transparent and there is no liquid dripping from the condensate, stop concentrating, turn off stirring, and empty the reactor body;

[0026] S10: Open the manhole cover and perform maintenance and cleaning on the inside of the reactor body.

[0027] Beneficial effects of the present invention:

[0028] 1. In the present invention, the relative position of the sealing rod and the sampling hole can be controlled by the first pushing assembly, thereby the through state of the sampling hole, and the sealing push plate can be driven to move by the second pushing assembly, so that the sealing push plate is convenient for extracting the medicine liquid from the inside of the reactor body, and the sealing rod is pushed into the sampling hole by the first pushing assembly, so as to prevent the medicine liquid inside the outer cylinder from flowing back into the reactor body, and then the second pushing assembly is extended to push the sealing push plate to squeeze the medicine liquid, so that the medicine liquid can flow to the other side of the sealing push plate through the pressure-type one-way valve on the sealing push plate, until the sealing push plate squeezes all the medicine liquid to the other side of the sealing push plate, and then the second pushing assembly is contracted to drive the sealing push plate to move toward the external interface, and directly squeeze all the medicine liquid close to the side of the external interface from the external interface to the inside of the sampling device, thereby realizing the sampling of the sampling device, and the sampling efficiency is improved, and at the same time, it can also prevent the sample liquid from contacting with the outside world, and ensure the reliability of the reference data.

[0029] 2. In the present invention, after sampling, the staff can remove the sampling device at the external interface and connect the pure water output pipe. The second push assembly extends to drive the sealing push plate to move. Since the sealing rod does not block the sampling hole at this time, and the pressure of the drug liquid is not enough to push open the pressure-type one-way valve, the sealing push plate can directly push all the drug liquid on one side from the inside of the sampling hole back to the reactor body. At the same time, the pure water output pipe outputs pure water. The movement of the sealing push plate will drive the pure water into the outer cylinder, thereby cleaning the inside of the outer cylinder.

[0030] 3. In the present invention, when it is necessary to maintain and clean the inside of the reactor body, the manhole cover can be opened to facilitate the cleaning of the inside of the reactor body, and then the motor is started. The motor drives the oblique arc scraper to rotate along the axis of the transmission rod. When the oblique arc scraper moves, it can scrape off the liquid inside the reactor body, achieving an automatic cleaning effect, thereby reducing the difficulty of maintenance for the staff. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] The present invention will be further described below in conjunction with the accompanying drawings.

[0032] Figure 1It is a schematic diagram of the overall structure of the present invention;

[0033] Figure 2 It is a schematic diagram of the overall longitudinal section structure of the present invention;

[0034] Figure 3 It is a schematic diagram of the internal structure of the reactor body of the present invention;

[0035] Figure 4 yes Figure 3 A schematic diagram of the enlarged structure of the middle A position;

[0036] Figure 5 It is a schematic diagram of the initial state structure of the sampling mechanism of the present invention;

[0037] Figure 6 It is a schematic diagram of the state structure of the sampling mechanism of the present invention when sampling liquid;

[0038] Figure 7 It is a schematic diagram of the state structure of the sampling mechanism of the present invention when transferring sample liquid;

[0039] Figure 8 It is a schematic diagram of the state structure of the sampling mechanism of the present invention when outputting sample liquid.

[0040] In the figure: 1. Reactor body; 2. Feed pipe; 3. High-level tank; 4. Regulating valve; 5. Temperature control component; 6. Sampling mechanism; 601. Outer cylinder; 602. Baffle; 603. First push component; 604. Second push component; 605. External interface; 606. Sealing rod; 607. Sealing push plate; 608. Illuminating device; 609. Observation window; 610. Pressure-type one-way valve; 7. Transmission rod; 8. Stirring plate; 9. Oblique arc scraper; 10. Sampling hole; 11. Discharge pipe; 12. Exhaust gas output pipe; 13. Manhole cover; 14. Motor. DETAILED DESCRIPTION

[0041] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0042] See also Figure 1-8As shown, the present invention is a synthesis device of memantine hydrochloride, comprising a reactor body 1, a feeding pipe 2 is arranged at the top of the reactor body 1, a discharge pipe 11 is arranged at the bottom of the reactor body 1, a solenoid valve is arranged on the discharge pipe 11 for controlling the discharge, a stirring component is arranged inside the reactor body 1, and the stirring component is used to achieve mixing of the liquid medicine, the device also includes a temperature control component 5 arranged outside the reactor body 1, the temperature control component 5 includes a heat transfer oil pipe arranged around the outside of the reactor body 1, and the temperature inside the reactor body 1 is controlled by controlling the oil temperature inside the heat transfer oil pipe.

[0043] A high-position tank 3 is provided on the top of the reactor body 1. The high-position tank 3 is used to store 1,3-dimethyladamantane. A regulating valve 4 is connected between the high-position tank 3 and the reactor body 1. The high-position tank 3 is used to store materials to be mixed, such as 1,3-dimethyladamantane. The materials to be mixed in the high-position tank 3 can enter the reactor body 1 through the regulating valve 4. The regulating valve 4 can control the dripping speed of 1,3-dimethyladamantane into the reactor body 1. A tail gas output pipe 12 is arranged on the top of the reactor body 1. A negative pressure device is arranged at one end of the tail gas output pipe 12 away from the reactor body 1. The negative pressure device may be a negative pressure pump. A condensing device is connected to the output end of the negative pressure device. The condensing device may be a water-cooled condenser. The negative pressure device can adjust the pressure inside the reactor body 1. This change will affect the boiling point of the solution. By precisely controlling the temperature inside the reactor body 1, certain components in the solution can be caused to boil at a lower temperature, thereby achieving separation of these components. The negative pressure device extracts the separated substances from the reactor body 1 through the tail gas output pipe 12 and discharges them to the condensing device. The separated gas is gradually cooled and liquefied through the condensing device, thereby achieving separation of the substances.

[0044] In order to achieve stirring of the medicinal liquid, the stirring assembly includes a motor 14 fixedly connected to the reactor body 1, a transmission rod 7 is rotatably connected inside the reactor body 1, and a plurality of stirring plates 8 are equidistantly arranged and fixedly connected to the transmission rod 7. The transmission rod 7 is coaxially fixedly connected to the output end of the motor 14. After the motor 14 is started, the transmission rod 7 can be driven to rotate, and the rotation of the transmission rod 7 drives the stirring plate 8 to move, thereby achieving stirring of the medicinal liquid through the stirring plate 8.

[0045] In order to improve the heating efficiency, each group of stirring plates 8 is fixedly connected to an oblique arc scraper 9 at one end away from the transmission rod 7. The side of each group of oblique arc scrapers 9 away from the stirring plates 8 is in contact with the inner wall of the reactor body 1, and there is a certain angle between the oblique arc scraper 9 and the horizontal plane, and the angle range is 30° to 60°. When the transmission rod 7 drives the stirring plates 8 to move, it will drive the oblique arc scraper 9 to rotate along the axis of the transmission rod 7. When the oblique arc scraper 9 moves, it will push the medicine liquid to move toward the bottom of the reactor body 1, thereby accelerating the mixing effect, thereby improving the reaction efficiency, and at the same time ensuring that the medicine liquid is heated evenly and the processing effect is guaranteed.

[0046] A sampling hole 10 is provided at one side of the bottom of the reactor body 1, and a sampling mechanism 6 matching the sampling hole 10 is provided on the reactor body 1. The sampling mechanism 6 includes an outer cylinder 601 fixedly connected to the reactor body 1, and a baffle 602 is fixedly connected to one end of the outer cylinder 601 away from the reactor body 1, and a first push assembly 603 and a second push assembly 604 are fixedly connected to the baffle 602. The first push assembly 603 and the second push assembly 604 are both electric telescopic rods, and an external interface 605 matching the sampling device is provided on the baffle 602; a sealing push plate 607 is slidably matched inside the outer cylinder 601, and the output end of the second push assembly 604 is fixedly connected to the sealing push plate 607, and the second push assembly 604 can drive the sealing push plate 607 to move. The sealing push plate 607 moves, and the output end of the first pushing component 603 is fixedly connected to a sealing plug rod 606 that slides with the sampling hole 10. The sealing push plate 607 is slidably sleeved on the sealing plug rod 606, and the first pushing component 603 can drive the sealing plug rod 606 to move relative to the sealing push plate 607; a pressure-type one-way valve 610 for liquid material flow is provided on the sealing push plate 607, and the output end faces the external interface 605. The pressure-type one-way valve 610 includes a through hole provided on the sealing push plate 607, and a spring with one end fixedly connected to the inner wall of the through hole, and a sealing valve plate fixedly connected to the other end of the spring. The spring pulls the sealing valve plate to block the through hole to ensure that the liquid medicine itself needs to have a certain pressure to push open the sealing valve plate.

[0047] In order to facilitate the staff to observe the color of the medicine liquid, an observation component for observing the color of the liquid material is provided on the outer cylinder 601. The observation component includes a lighting device 608 arranged on one side of the outer cylinder 601 and an observation window 609 arranged on the other side of the outer cylinder 601. The lighting device 608 can release white light after being powered on, which is convenient for the staff to observe the color of the medicine liquid. The lighting device 608 and the observation window 609 are both provided with an arc-shaped glass plate that matches the inner wall of the outer cylinder 601 on the side close to the axis of the outer cylinder 601 to ensure that the sealing push plate 607 can slide on the inner wall of the outer cylinder 601 and the arc-shaped glass plate. When sampling, the lighting device 608 is started. When the sealing push plate 607 drives the medicine liquid into the interior of the outer cylinder 601, with the light-transmitting effect of the lighting device 608, the staff can clearly observe the color of the medicine liquid through the observation window 609, so that the staff can judge whether the time for sampling is ripe by comparing the color of the medicine liquid.

[0048] In order to facilitate cleaning, a manhole cover 13 is provided on the top of the reactor body 1. When the reactor body 1 is emptied and the inside of the reactor body 1 needs to be maintained and cleaned, the manhole cover 13 can be opened to facilitate cleaning of the inside of the reactor body 1. Then, the motor 14 is started. The motor 14 drives the oblique arc scraper 9 to rotate along the axis of the transmission rod 7. When the oblique arc scraper 9 moves, it can scrape off the liquid medicine inside the reactor body 1, thereby achieving an automatic cleaning effect, thereby reducing the difficulty of maintenance for the staff.

[0049] A synthesis process of memantine hydrochloride comprises the following steps:

[0050] S1: 150-250 kg of drinking water and 30-50 kg of sodium sulfite are added to the reactor body 1 in sequence, stirred evenly, and then 4.86*A±0.5 kg of bromine is introduced. In this process, A is a proportional coefficient, and the value range of A is between 18 and 20. Then the feed pipe is closed and the negative pressure device is started. The negative pressure device changes the inside of the reactor body 1 into a negative pressure state through the tail gas output pipe 12;

[0051] S2: Control the temperature of the liquid inside the reactor body 1 to be between 10 and 20° C. through the temperature control component 5, and start stirring;

[0052] S3: Introduce 1*A kg 1,3-dimethyladamantane into the high-position tank 3, and control the drop rate of 1,3-dimethyladamantane by controlling the opening size of the regulating valve 4 to ensure that the drop time range is between 3 and 5 hours, and control the temperature control component 5 so that the temperature of the reaction liquid in the reactor body 1 is between 15 and 25° C., and the reaction time is 24 hours;

[0053] S4: Sampling is performed through the sampling mechanism 6 to check whether the content of 1,3-dimethyladamantane is less than 5%. If the test result meets the requirements, the next step is carried out. If the test result does not meet the requirements, stirring is continued, and sampling can be performed again after at least two hours until the requirements are met;

[0054] S5: decompressing the interior of the reactor body 1 by a negative pressure device, setting the initial circulation temperature between 30 and 35° C., realizing the decompression concentration operation of the reaction liquid, concentrating for 8 to 10 hours, and sampling to monitor the bromine residue;

[0055] S6: Introduce 0.5*A kg of n-heptane with bromine into the high-level tank 3, control the temperature control component 5 to set the temperature between 45 and 40° C., and reduce the pressure and concentrate until no condensate drips at the output end of the condensation device;

[0056] S7: Continue to repeat S6 operation until the condensate becomes colorless and transparent and no condensate drops;

[0057] S8: Continue to add 10.0±0.5*A kg of n-heptane, control the temperature control component 5 to set the temperature between 55 and 50° C., continue to reduce pressure and concentrate until the condensate is colorless and transparent and there is no liquid dripping from the condensate, stop concentrating, turn off stirring, and empty the reactor body 1.

[0058] S9: Open the manhole cover 13 and perform maintenance and cleaning on the inside of the reactor body 1.

[0059] The working principle of the present invention is as follows: drinking water, sodium sulfite and bromine are sequentially added into the reactor body 1 through the feed pipe 2, the temperature control component 5 is started, so that the reactor body 1 reaches the most suitable reaction temperature, and the motor 14 is started. The motor 14 can drive the transmission rod 7 to rotate, and the rotation of the transmission rod 7 drives the stirring plate 8 to move, and the stirring plate 8 is used to stir the liquid medicine. When the transmission rod 7 drives the stirring plate 8 to move, it will drive the oblique arc scraper 9 to rotate along the axis of the transmission rod 7. When the oblique arc scraper 9 moves, it will push the liquid medicine toward the bottom of the reactor body 1, thereby accelerating the mixing effect, thereby improving the reaction efficiency, and at the same time ensuring that the liquid medicine is heated evenly and the processing effect is guaranteed.

[0060] When in use, ingredients to be mixed can be put into the high-level tank 3. The ingredients to be mixed can be n-heptane with bromine or n-heptane. The ingredients to be mixed can enter the reactor body 1 through the regulating valve 4. The dripping speed of the ingredients to be mixed into the reactor body 1 can be changed by adjusting the regulating valve 4, so as to achieve the input of materials. The negative pressure device can adjust the pressure inside the reactor body 1. This change will further affect the boiling point of the solution. The temperature in the reactor body 1 can be accurately controlled by the temperature control component 5, which can cause certain components in the solution to start boiling at a lower temperature, so as to achieve the separation of these components. The negative pressure device extracts the separated substances from the reactor body 1 through the tail gas output pipe 12 and discharges them to the condensing device. The separated gas is gradually cooled and liquefied by the condensing device, so as to achieve the separation of substances.

[0061] Initially, the external interface 605 is connected to the pure water output pipe. When the solution inside the reactor body 1 needs to be sampled, the pure water output pipe needs to be unplugged, and the first push component 603 is started. The first push component 603 draws the sealing rod 606 out of the sampling hole 10, and the liquid medicine enters the sampling hole 10 along with the sealing rod 606. Then, the second push component 604 contracts and drives the sealing push plate 607 to move backward. The sealing push plate 607 draws the liquid medicine out of the sampling hole 10, so that part of the liquid medicine is located inside the outer cylinder 601.

[0062] After that, the sampling device is docked with the external interface 605, and the first push assembly 603 pushes the sealing rod 606 into the sampling hole 10, so as to prevent the liquid medicine in the outer cylinder 601 from flowing back into the reactor body 1, and then the second push assembly 604 extends to push the sealing push plate 607 to squeeze the liquid medicine, so that the liquid medicine can flow to the other side of the sealing push plate 607 through the pressure-type one-way valve 610 on the sealing push plate 607, until the sealing push plate 607 squeezes all the liquid medicine to the other side of the sealing push plate 607. On the other side, the first push component 603 drives the sealing rod 606 to be drawn out from the sampling hole 10, so that the liquid medicine inside the reactor body 1 enters the sampling hole 10, and the second push component 604 contracts, driving the sealing push plate 607 to move toward the external interface 605, and the sealing push plate 607 draws out the liquid medicine inside the sampling hole 10, and at the same time, can directly squeeze all the liquid medicine near the external interface 605 side from the external interface 605 into the sampling device, thereby realizing the sampling of the sampling device;

[0063] After that, the sampling device at the external interface 605 is removed, and the pure water output pipe is connected. The second push assembly 604 extends to drive the sealing push plate 607 to move. Since the sealing plug rod 606 does not block the sampling hole 10 at this time, and the pressure of the liquid medicine is not enough to push open the pressure-type one-way valve 610, the sealing push plate 607 can directly push all the liquid medicine on one side from the inside of the sampling hole 10 back to the reactor body 1. At the same time, the pure water output pipe outputs pure water. The movement of the sealing push plate 607 will drive the pure water to enter the outer cylinder 601, thereby cleaning the inside of the outer cylinder 601. After that, the first push assembly 603 drives the sealing plug rod 606 to enter the inside of the sampling hole 10, thereby pushing the liquid medicine in the sampling hole 10 into the reactor body 1. During the whole process, the staff cooperates with the sealing push plate 607 to dock the sampling device and the pure water output pipe with the external interface 605 in turn, which has a high sampling efficiency and can also avoid the contact of the sample liquid with the outside world, thereby ensuring the reliability of the reference data.

[0064] When it is necessary to maintain and clean the inside of the reactor body 1, the manhole cover 13 can be opened to facilitate the cleaning of the inside of the reactor body 1, and then the motor 14 is started. The motor 14 drives the oblique arc scraper 9 to rotate along the axis of the transmission rod 7. When the oblique arc scraper 9 moves, it can scrape off the liquid inside the reactor body 1, achieving an automatic cleaning effect, thereby reducing the difficulty of maintenance for the staff.

[0065] The above is a detailed description of an embodiment of the present invention, but the content is only a preferred embodiment of the present invention and cannot be considered to limit the scope of implementation of the present invention. All equivalent changes and improvements made within the scope of the present invention should still fall within the scope of the patent coverage of the present invention.

Claims

1. A synthesis device for memantine hydrochloride, comprising a reactor body (1), wherein a feed pipe (2) is arranged at the top of the reactor body (1), a discharge pipe (11) is arranged at the bottom of the reactor body (1), and a stirring assembly is arranged inside the reactor body (1), characterized in that: Also includes: A sampling mechanism (6) for sampling and a sampling hole (10) matched with the sampling mechanism (6), wherein the sampling hole (10) is provided on one side of the reactor body (1), and the sampling mechanism (6) comprises an outer cylinder (601) fixedly connected to the reactor body (1), a baffle (602) is fixedly connected to one end of the outer cylinder (601) away from the reactor body (1), a first pushing assembly (603) is fixedly connected to the baffle (602), and a first pushing assembly (603) is provided on the baffle (602). There is an external interface (605) that cooperates with the sampling device, and a drainage component is arranged inside the outer tube (601). The drainage component is provided with a pressure-type one-way valve (610) for the flow of liquid materials. The output end of the first push component (603) is fixedly connected to a sealing rod (606) that slides with the sampling hole (10). The sealing rod (606) slides with the drainage component. The outer tube (601) is provided with an observation component for observing the color of the liquid material.

2. A synthesis device for memantine hydrochloride according to claim 1, characterized in that: The drainage assembly includes a sealing push plate (607) that is slidably matched with the inside of the outer tube (601), and a second push assembly (604) is fixedly connected to the baffle (602). The output end of the second push assembly (604) is fixedly connected to the sealing push plate (607). The sealing push plate (607) is slidably sleeved on the sealing plug rod (606), and the pressure-type one-way valve (610) is arranged on the sealing push plate (607).

3. A synthesis device for memantine hydrochloride according to claim 2, characterized in that: The pressure-type one-way valve (610) comprises a through hole arranged on the sealing push plate (607), a spring having one end fixedly connected to the inner wall of the through hole, and a sealing valve plate fixedly connected to the other end of the spring.

4. A synthesis device for memantine hydrochloride according to claim 1, characterized in that: The observation assembly comprises a lighting device (608) arranged on one side of the outer tube (601), and an observation window (609) arranged on the other side of the outer tube (601); the lighting device (608) and the observation window (609) are both provided with a curved glass plate that matches the inner wall of the outer tube (601) on one side close to the axis of the outer tube (601).

5. A synthesis device for memantine hydrochloride according to claim 1, characterized in that: The stirring assembly comprises a motor (14) fixedly connected to a reactor body (1); a transmission rod (7) is rotatably connected inside the reactor body (1); a plurality of groups of stirring plates (8) are fixedly connected to the transmission rod (7) at equal intervals; and the transmission rod (7) is coaxially fixedly connected to an output end of the motor (14).

6. A synthesis device for memantine hydrochloride according to claim 5, characterized in that: Each group of the stirring plates (8) is fixedly connected to an oblique arc scraper (9) at one end away from the transmission rod (7); the side of each group of the oblique arc scrapers (9) away from the stirring plates (8) is in contact with the inner wall of the reactor body (1); and there is a certain angle between the oblique arc scrapers (9) and the horizontal plane, and the range of the angle is 30° to 60°.

7. A synthesis device for memantine hydrochloride according to claim 1, characterized in that: A temperature control component (5) is arranged on the outside of the reactor body (1), a high-position tank (3) is arranged on the top of the reactor body (1), and a regulating valve (4) is connected between the high-position tank (3) and the reactor body (1).

8. A synthesis device for memantine hydrochloride according to claim 1, characterized in that: An exhaust gas output pipe (12) is arranged on the top of the reactor body (1), a negative pressure device is arranged at one end of the exhaust gas output pipe (12) away from the reactor body (1), and an output end of the negative pressure device is connected to a condensing device.

9. A synthesis device for memantine hydrochloride according to claim 1, characterized in that: A manhole cover (13) is provided on the top of the reactor body (1).

10. A synthesis process of a synthesis device for producing memantine hydrochloride according to any one of claims 1 to 9, characterized in that: The following steps are involved: S1: Add 150-250 kg of drinking water and 30-50 kg of sodium sulfite to the reactor body (1) in sequence and stir evenly; S2: Then, 4.86*A±0.5kg of bromine is introduced. In this process, A is a proportional coefficient, and the value range of A is between 18 and 20. The feed pipe is closed and the negative pressure device is started. The negative pressure device changes the inside of the reactor body (1) into a negative pressure state through the tail gas output pipe (12); S3: controlling the temperature of the liquid inside the reactor body (1) to be between 10° C. and 20° C. through the temperature control component (5), and starting stirring; S4: introducing 1*Akg 1,3-dimethyladamantane into the high-position tank (3), and controlling the opening size of the regulating valve (4) to control the dripping speed of the 1,3-dimethyladamantane, ensuring that the dripping time ranges between 3 and 5 hours, and controlling the temperature control component (5) so that the temperature of the reaction liquid in the reactor body (1) is between 15 and 25° C., and the reaction time is 24 hours; S5: sampling is performed through the sampling mechanism (6) to check whether the content of 1,3-dimethyladamantane is less than 5%. If the test result meets the requirements, the next step is carried out. If the test result does not meet the requirements, stirring is continued. Sampling can be performed again after at least two hours until the requirements are met; S6: decompressing the interior of the reactor body (1) by means of a negative pressure device, with the initial circulation temperature set between 30 and 35° C., to achieve a decompressed concentration operation on the reaction liquid, concentrating for 8 to 10 hours, and taking samples to monitor bromine residues; S7: 0.5*Akg of n-heptane with bromine is introduced into the high-position tank (3), the temperature control component (5) is controlled to be set between 45 and 40° C., and the condensation is performed under reduced pressure until no condensate drips from the output end of the condensation device; S8: Continue to repeat S6 operation until the condensate becomes colorless and transparent and no condensate drops; S9: Continue to add 10.0±0.5*Akg of n-heptane, control the temperature control component (5) to set the temperature between 55 and 50°C, continue to reduce pressure and concentrate until the condensate is colorless and transparent and no liquid drips from the condensate, stop concentrating, turn off stirring, and empty the reactor body (1); S10: Open the manhole cover (13) and perform maintenance and cleaning on the interior of the reactor body (1).

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