A preparation method and preparation device of pharmaceutical grade trishydroxymethylaminomethane

Abstract

The present invention belongs to the technical field of compound preparation, and in particular, is a method and device for preparing pharmaceutical-grade tris(hydroxymethyl)aminomethane. S1: Add raw materials into a reactor, heat, stir and mix; S2: Add nitromethane dropwise for condensation reaction; S3: Add the solution into a reaction tank and atomize it; S4: Pass hydrogen, and the hydrogen mixes with the atomized solution, contacts with a catalyst and undergoes a reduction reaction; S4: After the reaction is completed, stop atomizing the solution; S5: Add activated carbon to the solution, filter the solution, and cool and crystallize it to obtain crude particles; S6: Dissolve the crude particles in deionized water and add activated carbon to remove impurities; S7: Filter the solution, cool and crystallize it; S8: Dry the precipitated crystals. The present invention improves the utilization rate of discharged hydrogen and production efficiency by atomizing tris(hydroxymethyl)nitromethane and uniformly mixing it with hydrogen, and then fully contacting the mixed fluid with a catalyst for reaction.

Description

Technical Field

[0001] The present invention relates to the technical field of compound preparation, and in particular to a preparation method and a preparation device of pharmaceutical-grade trishydroxymethylaminomethane. Background Art

[0002] Tris(hydroxymethyl)aminomethane (TMA) is an important organic compound. In the pharmaceutical field, it is often used for acute metabolic and respiratory acidosis because it can absorb hydrogen ions and correct acidosis. It is an ideal drug and an important pharmaceutical intermediate. The existing preparation of TMA mostly involves a condensation reaction between nitromethane and excess paraformaldehyde to produce the intermediate TMN. This intermediate is then reduced with hydrogen to produce TMA. After the reduction reaction is complete, the product is neutralized and filtered to remove the catalyst, and then purified by crystallization and recrystallization, and finally dried to obtain solid TMA.

[0003] In the above-mentioned reduction reaction, since the reaction between hydrogen and tris(hydroxymethylnitromethane) requires contact with a catalyst, in the preparation process of the existing device, the catalyst is mostly directly added to the tris(hydroxymethylnitromethane) solution, and then hydrogen is gradually introduced into the tris(hydroxymethylnitromethane) solution, and the tris(hydroxymethylnitromethane) and hydrogen are simultaneously contacted with the catalyst by stirring. However, in this process, due to the low solubility of hydrogen in the solution, the gaseous hydrogen must first be dissolved in the solution before it can contact and react with the tris(hydroxymethylnitromethane) and catalyst. At the same time, the existing method uses a powdered catalyst directly dispersed in the solution, and hydrogen is introduced in the form of bubbles. The gas-liquid-solid three-phase contact efficiency is low, and unreacted hydrogen easily escapes from the solution, resulting in low hydrogen utilization per unit time, affecting production efficiency. Summary of the Invention

[0004] The present invention provides a preparation method and a preparation device for pharmaceutical-grade tris(hydroxymethylaminomethane), which are used to solve the defect in existing reaction devices that hydrogen cannot be uniformly mixed with tris(hydroxymethylaminomethane) before contacting with a catalyst.

[0005] The technical implementation scheme of the present invention is: a preparation method of pharmaceutical-grade tris(hydroxymethyl)aminomethane, comprising the following steps: S1: adding nitromethane and paraformaldehyde in a certain molar ratio of 1:3.3 and a catalyst into a reactor, heating and stirring until the paraformaldehyde is completely dissolved; S2: slowly adding nitromethane dropwise into the solution to carry out a condensation reaction, and maintaining the temperature of the solution between 40 and 55°C; S3: adding the solution after the reaction into a reaction tank, and atomizing the solution, and the temperature in the reaction tank is between 40 and 50°C; S4: introducing hydrogen into the reaction tank, and the hydrogen is mixed with the atomized solution and then mixed with the catalyst. The reduction reaction is carried out by contacting the reaction tank to obtain tris(hydroxymethyl)aminomethane; S4: after the reduction reaction is completed, the atomizing solution is stopped and the temperature of the solution in the reaction tank is maintained at 60°C; S5: activated carbon is added to the solution and slowly stirred to allow the activated carbon to adsorb impurities in the solution, and then the solution is filtered and cooled to crystallize to obtain crude particles; S6: the crude particles are dissolved in deionized water and activated carbon is added again to remove impurities, and the solution temperature is maintained at 80°C; S7: the above-mentioned secondary impurity-removed solution is filtered again, and then cooled and crystallized again; S8: the precipitated crystals are dried to obtain finished tris(hydroxymethyl)aminomethane particles.

[0006] A device for preparing pharmaceutical-grade tris(hydroxymethyl)aminomethane, applicable to the aforementioned method for preparing pharmaceutical-grade tris(hydroxymethyl)aminomethane, comprising: a reaction tank, wherein the upper and lower sides of the reaction tank are respectively provided with a feed port and a discharge port, and the lower portion of the reaction tank is provided with a circulation port; a motor fixedly connected to the reaction tank; an air intake pipe fixedly connected to the output shaft of the motor, the air intake pipe being externally connected to a hydrogen tank, the air intake pipe being provided with a sliding shell, the air intake pipe being connected to the sliding shell via an air delivery pipe; a plurality of exhaust pipes, each provided on the sliding shell, the exhaust pipes being connected to the sliding shell; A stirring frame is fixedly connected to the air inlet pipe; a liquid inlet pipe is fixedly connected to the air inlet pipe, the liquid inlet pipe is rotatably connected to the reaction tank, and the liquid inlet pipe and the circulation port are jointly connected to a circulation pump through a hose; an atomizing shell is fixedly connected to and communicated with the liquid inlet pipe; a fixed ring is fixedly connected to the reaction tank, the fixed ring is fixedly connected to a fixed frame through a connecting rod, the fixed ring and the fixed frame are rotatably connected to an annular filter screen, and the annular filter screen is filled with a catalyst; a power assembly is arranged in the reaction tank, and is used to adjust the position of the annular filter screen to disperse the catalyst after the catalyst agglomerates in the annular filter screen.

[0007] Furthermore, the fixing ring is located below the fixing frame.

[0008] Furthermore, the power assembly includes: a first electric push rod, fixedly connected to the reaction tank, a telescopic end of the first electric push rod fixedly connected to a sliding frame, the sliding frame is slidably connected to the liquid inlet pipe, the sliding frame is slidably connected to the fixed frame, and an air pressure sensor is provided on the fixed ring, and the air pressure sensor is used to detect the pressure of the gas in the reaction tank; a transmission plate has multiple, which are evenly hinged to the sliding frame in the circumference, and a torsion spring is fixed between the transmission plate and the sliding frame; annular soft strips, the number of which is the same as the number of the transmission plates, are evenly fixed to the annular filter screen in the circumference, the fixed frame and the fixed ring are both slidably connected to the annular soft strips, and the annular soft strips are fixed with evenly distributed limit plates, and the limit plates are located on the moving path of adjacent transmission plates; a smoothing assembly is provided on the sliding frame, and is used to slap the catalyst in the annular filter screen in the process of driving the annular filter screen to rotate.

[0009] Furthermore, the limiting plate is an L-shaped plate.

[0010] Furthermore, the smoothing component includes: a rotating ring, which is slidably connected to the liquid inlet pipe, and the rotating ring is rotatably connected to the sliding frame; an annular plate, which is rotatably and slidably connected to the rotating ring, and the annular plate is fixed with a circumferentially distributed smoothing plate, and the smoothing plate is used to squeeze the annular filter; a vibration component, which is arranged on the annular plate, and is used to drive the annular plate to move up and down, so that the smoothing plate hits the annular filter.

[0011] Furthermore, the vibration assembly includes: a first spring, fixed between the rotating ring and the annular plate, and circumferentially distributed extrusion blocks are fixed to the facing sides of the annular plate and the fixed frame, and the extrusion blocks at different heights squeeze each other to drive the annular plate to move.

[0012] Furthermore, it also includes: a sliding component, which is arranged on the air intake pipe and is used to adjust the distance between the exhaust pipe and the atomization shell, and the sliding component includes: a second electric push rod, which is fixed to the fixed ring, and the air intake pipe and the sliding shell are slidably connected, and the telescopic end of the second electric push rod is fixed to a limiting ring, and the limiting ring is slidably connected to the reaction tank; elastic rods, the number of which is the same as the number of the exhaust pipes, are respectively fixed to adjacent exhaust pipes, and the elastic rods are slidably and rotatably connected to the limiting rings.

[0013] Furthermore, a second spring is fixedly connected between the air intake pipe and the sliding shell, and the exhaust pipe is hinged to the sliding shell.

[0014] Furthermore, the included angle between the exhaust pipe and the horizontal plane is less than 30°, and one end of the exhaust pipe away from the air inlet pipe is higher than the other end.

[0015] Compared with the prior art, the present invention has the following advantages: 1. In the process of producing trishydroxymethylaminomethane, the present invention improves the utilization rate of the discharged hydrogen by atomizing trishydroxymethylnitromethane and uniformly mixing it with hydrogen, and then fully contacts and reacts the mixed fluid with a catalyst, thereby improving the production efficiency of trishydroxymethylaminomethane.

[0016] 2. When the catalyst in the annular filter screen agglomerates, the annular filter screen is driven to move by the annular soft strip, so that the annular filter screen drives the catalyst to move, and the catalyst in the annular filter screen remains loose, thereby ensuring the contact area between trishydroxymethylnitromethane and the catalyst, thereby ensuring the production efficiency of trishydroxymethylaminomethane.

[0017] 3. When adjusting the position of the annular filter, the present invention reduces the impact force of the gas on the atomized solution and the amount of contact between the atomized solution and the annular filter by adjusting the angle and position of the exhaust pipe. At the same time, the gas discharged from the exhaust pipe blows the catalyst particles in the annular filter, accelerating the flow rate of the solution between the catalyst particles, thereby quickly dealing with the catalyst agglomeration and ensuring the normal progress of the reaction. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is a schematic diagram of the three-dimensional structure of the present invention;

[0019] Figure 2 Schematic diagram of the three-dimensional structure of the motor, air inlet pipe and liquid inlet pipe of the present invention;

[0020] Figure 3 Schematic diagram of the three-dimensional structure of the liquid inlet pipe, sliding frame and fixed frame of the present invention;

[0021] Figure 4 Schematic diagram of the three-dimensional structure of the transmission plate, annular soft strip and smoothing plate of the present invention;

[0022] Figure 5 It is a schematic diagram of the three-dimensional structure of the rotating ring, the annular plate and the second spring of the present invention;

[0023] Figure 6 It is a three-dimensional structural cross-sectional view of the sliding frame, the fixed frame and the rotating ring of the present invention;

[0024] Figure 7 Schematic diagram of the three-dimensional structure of the transmission plate, annular soft strip and limit plate of the present invention;

[0025] Figure 8 A schematic diagram of the three-dimensional structure of the intake pipe, the exhaust pipe and the second spring of the present invention;

[0026] Figure 9 It is a three-dimensional structural cross-sectional view of the air intake pipe, sliding shell and exhaust pipe of the present invention.

[0027] In the accompanying drawings: 1-reaction tank, 101-circulation port, 2-motor, 3-inlet pipe, 4-sliding shell, 5-exhaust pipe, 6-stirring frame, 7-liquid inlet pipe, 8-atomizing shell, 9-fixed ring, 10-sliding frame, 11-fixed frame, 12-annular filter, 13-first electric push rod, 14-transmission plate, 15-torsion spring, 16-annular soft strip, 17-limiting plate, 1101-rotating ring, 18-annular plate, 19-smoothing plate, 20-first spring, 21-extrusion block, 24-second spring, 25-second electric push rod, 26-limiting ring, 27-elastic rod. DETAILED DESCRIPTION

[0028] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. 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 making creative efforts are within the scope of protection of the present invention.

[0029] A method for preparing pharmaceutical grade trishydroxymethylaminomethane, such as Figures 1-9 As shown, the method comprises the following steps: S1: adding nitromethane and paraformaldehyde in a certain molar ratio of 1:3.3 and a catalyst into a reactor, heating and stirring until the paraformaldehyde is completely dissolved; S2: slowly adding nitromethane dropwise into the solution to carry out a condensation reaction, and maintaining the temperature of the solution between 40 and 55°C; S3: adding the solution after the reaction into a reaction tank, and atomizing the solution, and the temperature in the reaction tank is between 40 and 50°C; S4: introducing hydrogen into the reaction tank, mixing the hydrogen with the atomized solution and then contacting with the catalyst to carry out a reduction reaction to obtain trihydroxy Methylaminomethane; S4: after the reduction reaction is completed, stop atomizing the solution and keep the temperature of the solution in the reaction tank at 60°C; S5: add activated carbon to the solution and stir slowly to allow the activated carbon to adsorb impurities in the solution, then filter the solution and cool it to crystallize to obtain crude particles; S6: use deionized water to dissolve the crude particles and add activated carbon again to remove impurities, keeping the solution temperature at 80°C; S7: filter the above-mentioned secondary impurity-removed solution again, and then cool it to crystallize again; S8: dry the precipitated crystals to obtain finished trishydroxymethylaminomethane particles.

[0030] like Figure 1-Figure 5As shown, the preparation device of a pharmaceutical-grade tris(hydroxymethyl)aminomethane described in the present invention is applied to the preparation method of the pharmaceutical-grade tris(hydroxymethyl)aminomethane described above, comprising: a reaction tank 1, wherein the upper and lower sides of the reaction tank 1 are respectively provided with a feed port and a discharge port, and the lower part of the reaction tank 1 is provided with a circulation port 101; a motor 2, fixedly connected to the reaction tank 1; an air intake pipe 3, fixedly connected to the output shaft of the motor 2, the air intake pipe 3 is externally connected to a hydrogen tank, the air intake pipe 3 is provided with a sliding shell 4, and the air intake pipe 3 is connected to the sliding shell 4 through an air delivery pipe; a plurality of exhaust pipes 5, all of which are provided on the sliding shell 4, and the exhaust pipe 5 is connected to the sliding shell 4 The stirring frame 6 is fixed to the air inlet pipe 3; the liquid inlet pipe 7 is fixed to the air inlet pipe 3, the liquid inlet pipe 7 is rotatably connected to the reaction tank 1, and the liquid inlet pipe 7 and the circulation port 101 are connected to a circulation pump through a hose; the atomizing shell 8 is fixed to and communicated with the liquid inlet pipe 7; the fixing ring 9 is fixed to the reaction tank 1, the fixing ring 9 is fixed to the fixing frame 11 through a connecting rod, the fixing ring 9 and the fixing frame 11 are rotatably connected to an annular filter screen 12, and the annular filter screen 12 is filled with a catalyst; a power assembly is arranged in the reaction tank 1, and is used to adjust the position of the annular filter screen 12 to disperse the catalyst after the catalyst is agglomerated in the annular filter screen 12.

[0031] Further, such as Figure 4 and Figure 5 As shown, the fixing ring 9 is located below the fixing frame 11 .

[0032] The above scheme provides a method for atomizing the solution and mixing it with hydrogen to directly react with the catalyst during the reduction reaction, thereby improving the utilization rate of hydrogen and accelerating the reaction speed of the material; the circulation port 101 is used to extract the solution in the reaction tank 1 during the reaction of the solution in the reaction tank 1. In the following, the electrical components in the reaction tank 1 are all installed with a protective shell to prevent the electrical components from contacting the reactants. The upper part of the reaction tank 1 is provided with an air outlet, which is connected to an external vacuum pump. The vacuum pump is used to extract the solution in the reaction tank 1 through the annular The unreacted hydrogen after the filter 12 allows the hydrogen in the reaction tank 1 to circulate normally; the upper end of the intake pipe 3 is provided with a rotating shell, and the intake pipe 3 is connected to the hydrogen tank through the rotating shell. In this embodiment, the intake pipe 3 and the sliding shell 4 are fixed; the number of exhaust pipes 5 is five, evenly distributed on the side of the sliding shell 4. In this embodiment, the relative position between the exhaust pipe 5 and the sliding shell 4 is fixed, and the upper side of the exhaust pipe 5 is provided with axially distributed exhaust holes, which are used to discharge hydrogen into the reaction tank 1, so that part of the hydrogen contacts the solution, and at the same time The atomized solution is blown upward and contacts the catalyst; the stirring rack 6 is used to stir the solution gathered at the bottom of the reaction tank 1; the liquid inlet pipe 7 is located on the outside of the air inlet pipe 3, and a rotating shell is also provided on the upper part of the liquid inlet pipe 7. The rotating shell of the liquid inlet pipe 7 and the circulation port 101 are connected to the circulation pump through a hose. The circulation pump is an existing device and is not shown in the figure. The circulation pump is used to extract the solution in the reaction tank 1 and transport it to the liquid inlet pipe 7; the atomizing shell 8 is located on the upper side of the sliding shell 4, and the atomizing shell 8 is provided with evenly distributed atomizing nozzles; the annular filter 1 Reference numeral 2 denotes an elastic filter screen or elastic filter cloth, which is used to adapt the annular filter screen 12 to changes in the shape of the fixing ring 9 and the fixing frame 11 during movement. The annular filter screen 12 is filled with a catalyst. In actual use, a fixing ring may be added to the annular filter screen 12 at the position where the fixing ring 9 and the fixing frame 11 contact with the annular filter screen 12 to stabilize the shape of the annular filter screen 12. The catalyst in the annular filter screen 12 is a granular nickel catalyst, which is used to increase the contact area between the nickel catalyst and the solution and hydrogen. The particle size of the nickel catalyst may be adjusted according to the situation.

[0033] Further, such as Figure 2-Figure 7As shown, the power assembly includes: a first electric push rod 13, which is fixed in the reaction tank 1, and a sliding frame 10 is fixed to the telescopic end of the first electric push rod 13, which is slidably connected to the liquid inlet pipe 7, and the sliding frame 10 is slidably connected to the fixed frame 11. An air pressure sensor is provided on the fixed ring 9, and the air pressure sensor is used to detect the pressure of the gas in the reaction tank 1; a transmission plate 14, which has multiple transmission plates 14, which are evenly hinged to the sliding frame 10 in the circumferential direction, and a torsion spring 15 is fixed between the transmission plate 14 and the sliding frame 10; an annular soft strip 16, the number of which is the same as the number of the transmission plates 14, which is evenly fixed to the annular filter 12 in the circumferential direction, and the fixed frame 11 and the fixed ring 9 are both slidably connected to the annular soft strip 16, and the annular soft strip 16 is fixed with evenly distributed limit plates 17, which are located on the moving path of adjacent transmission plates 14; a smoothing assembly, which is provided on the sliding frame 10, and is used to slap the catalyst in the annular filter 12 in the process of driving the annular filter 12 to rotate.

[0034] Further, such as Figure 6 and Figure 7 As shown, the limiting plate 17 is an L-shaped plate.

[0035] The above scheme provides a method for driving the annular filter 12 to rotate and adjusting the position of the catalyst in the annular filter 12 to loosen it after the solution in the catalyst on the annular filter 12 becomes too much and agglomerates. Initially, the telescopic end of the first electric push rod 13 is in an extended state, and the telescopic end of the first electric push rod 13 is fixedly connected to the sliding frame 10. The air pressure sensor on the fixing ring 9 is used to detect the pressure of the gas under the annular filter 12 in the reaction tank 1. In this embodiment, the number of the transmission plates 14 is six, and the transmission plate 14 has a barb on the side away from the liquid inlet pipe 7. The barb It is used to hook the limit plate 17 and drive the sliding frame 10 to move when the sliding frame 10 moves upward. Initially, the barb of the transmission plate 14 has hooked the adjacent limit plate 17, and the torsion spring 15 is used to drive the transmission plate 14 to rotate and reset, and the torsion spring 15 is always in a stored force state; the fixing ring 9 and the fixing frame 11 are both provided with an arc groove, and the arc groove is used to enable the annular soft strip 16 to drive the limit plate 17 to move so that the limit plate 17 can pass through the fixing ring 9 and the fixing frame 11. The transmission plate 14 and the limit plate 17 are both provided with rounded corners to prevent the transmission plate 14 from being stuck by the limit plate 17 when it is reset.

[0036] Further, such as Figure 3-Figure 6 As shown, the smoothing component includes: a rotating ring 1101, which is slidably connected to the liquid inlet pipe 7, and the rotating ring 1101 is rotatably connected to the sliding frame 10; an annular plate 18, which is rotatably and slidably connected to the rotating ring 1101, and the annular plate 18 is fixed with circumferentially distributed smoothing plates 19, which are used to squeeze the annular filter 12; a vibration component, which is arranged on the annular plate 18, and is used to drive the annular plate 18 to move up and down, so that the smoothing plate 19 slaps the annular filter 12.

[0037] Further, such as Figure 3-Figure 6 As shown, the vibration assembly includes: a first spring 20, which is fixed between the rotating ring 1101 and the annular plate 18, and the facing sides of the annular plate 18 and the fixed frame 11 are fixed with circumferentially distributed extrusion blocks 21, and the extrusion blocks 21 at different heights squeeze each other to drive the annular plate 18 to move.

[0038] The above solution provides a method for initially loosening the catalyst within the annular filter 12 during adjustment of the annular filter 12, thereby reducing the resistance encountered by the annular filter 12 during rotation. The rotating ring 1101 is located at the lower portion of the sliding frame 10. Initially, the extrusion blocks 21 on the annular plate 18 do not contact the extrusion blocks 21 on the sliding frame 10. In this embodiment, the annular plate 18 has six smoothing plates 19. When the annular plate 18 is not moving upward, the smoothing plates 19 rotate with the annular plate 18 and mix the atomized solution and hydrogen. After the annular plate 18 moves upward, the smoothing plates 19 squeeze the underside of the annular filter 12, dispersing any agglomerated catalyst within the annular filter 12. The smoothing plates 19 may be provided with bumps to enhance their effectiveness in loosening the catalyst within the annular filter 12. A first spring 20 is used to push the annular plate 18 to move and reset. The extrusion blocks 21 have rounded corners, so that when the extrusion blocks 21 at different heights press against each other, the annular plate 18 moves downward under the force of the extrusion blocks 21 thereon, thereby driving the smoothing plates 19 to move up and down.

[0039] Workflow: When the generated trishydroxymethylnitromethane solution needs to be reduced, the staff adds the solution to be reacted into the reaction tank 1 through the feed port. After the liquid level of the solution approaches the lower end of the air inlet pipe 3, the staff seals the feed port after the solution is added, and then starts the motor 2, the circulation pump and activates the air pressure sensor on the fixed ring 9. The circulation pump extracts the solution in the reaction tank 1 from the circulation port 101 and transports it to the liquid inlet pipe 7 through a hose. The solution then enters the atomizing shell 8 and is discharged through the atomizing nozzle to realize circulation. The output shaft of the motor 2 drives the air inlet pipe 3 to rotate, and the air inlet pipe 3 drives the sliding shell 4, the stirring frame 6 and the liquid inlet pipe 7 to rotate. The sliding shell 4 drives the exhaust pipe 5 to rotate, and the stirring frame 6 rotates to stir the solution in the reaction tank 1. The liquid inlet pipe 7 drives the atomizing shell 8 and the rotating ring 1101 to rotate synchronously. The atomizing shell 8 rotates so that the atomized solution sprayed by it covers the exhaust pipe 5. The rotating ring 1101 drives the smoothing plate 19 to rotate through the annular plate 18.

[0040] After the above solution starts to circulate, the staff opens the hydrogen tank to transport hydrogen into the air inlet pipe 3. The hydrogen enters the sliding shell 4 through the air inlet pipe 3 and the air delivery pipe, and then enters the exhaust pipe 5 and is discharged through the exhaust hole on it. The discharged hydrogen pushes the atomized solution sprayed from the atomizing shell 8 to move upward, so that the atomized solution gradually approaches the annular filter 12 (hereinafter referred to as the mixture of hydrogen and atomized solution). In the process of the fluid moving upward, when the fluid moves near the caressing plate 19, the rotating caressing plate 19 further mixes the hydrogen in the fluid with the atomized solution, making the hydrogen in the fluid and the atomized solution more evenly distributed, thereby promoting the reaction between the two and improving the utilization of hydrogen. rate. After the fluid contacts the catalyst in the annular filter 12, the substances in the fluid react under the action of the catalyst in the annular filter 12 to generate trishydroxymethylaminomethane, and the generated trishydroxymethylaminomethane is located in the atomized solution. At the same time, the atomized solution in the fluid adheres to the surface of the catalyst and forms liquid droplets that are separated from the hydrogen. As the reaction proceeds, the number of liquid droplets gradually increases, and under the action of gravity, they gather into droplets that are separated from the annular filter 12 and then fall into the solution in the reaction tank 1. At the same time, the incompletely reacted hydrogen passes through the annular filter 12 and gathers above the reaction tank 1. At this time, the staff starts the vacuum pump to collect the hydrogen gathered on the upper part of the reaction tank 1 and reuse it.

[0041] During the above reaction, when the liquid content between the catalyst particles in the annular filter 12 is too much and agglomerates appear, the rate at which the fluid passes through the annular filter 12 decreases, causing the air pressure between the annular filter 12 and the liquid level in the reaction tank 1 to increase, and the value of the air pressure sensor increases and sends a signal to the first electric push rod 13. The telescopic end of the first electric push rod 13 is retracted and drives the sliding frame 10 to move upward. During this process, the air inlet pipe 3 continues to drive the parts thereon to rotate, and the sliding frame 10 drives the transmission plate 14 and the rotating ring 1101 to move upward. Since the transmission plate 14 hooks the limit plate 17, the transmission plate 14 drives the annular soft strip 16 to move through the limit plate 17. During this process, under the action of the limit plate 17, the transmission plate 14 gradually deflects the lower end of the transmission plate 14 toward the axis of the liquid inlet pipe 7 and reduces the degree of force stored in the torsion spring 15. The annular soft strip 16 drives the annular filter screen 12 to move synchronously, thereby completing the flipping of the inner and outer edges of the annular filter screen 12, so that the annular filter screen 12 rubs the catalyst particles therein during the movement, so that the catalyst particles are active and separated, thereby completing the adjustment of the position of the annular filter screen 12 and the loosening of the catalyst particles, facilitating the passage and reaction of the fluid, until the telescopic end of the first electric push rod 13 is completely retracted, the transmission plate 14 stops moving, and the position of the annular filter screen 12 is flipped.

[0042] In the process of the rotating ring 1101 moving upward, the rotating ring 1101 drives the annular plate 18 to move upward through the first spring 20, and the annular plate 18 drives the smoothing plate 19 and the extrusion block 21 thereon to move upward. When the smoothing plate 19 contacts the annular filter 12, the smoothing plate 19 loosens the catalyst in the annular filter 12 to facilitate the flow of liquid between the catalyst particles. Until the extrusion block 21 on the annular plate 18 contacts the fixed frame 11, the annular plate 18 and the parts thereon stop moving, and the sliding frame 10 continues to drive the rotating ring 1101 to move upward. The rotating ring 1101 moves upward relative to the annular plate 18 and compresses the first spring 20 until the sliding frame 10 After stopping movement, the rotating ring 1101 stops moving. During this process, as the annular plate 18 drives the parts on it to rotate, when the extrusion block 21 on the annular plate 18 contacts the extrusion block 21 on the fixed frame 11, the annular plate 18 moves downward under the extrusion of the two corresponding extrusion blocks 21 above and below and compresses the first spring 20 again, so that the smoothing plate 19 is separated from the annular filter screen 12. When the two corresponding extrusion blocks 21 above and below are separated, the first spring 20 pushes the annular plate 18 to move upward and slap the annular filter screen 12 again, thereby completing the loosening of the catalyst at different positions in the annular filter screen 12, improving the looseness of the catalyst in the annular filter screen 12, and facilitating the movement of the annular filter screen 12.

[0043] After the telescopic end of the first electric push rod 13 is retracted and waits for a period of time, the telescopic end of the first electric push rod 13 is extended and drives the parts on it to move in the opposite direction and reset. The sliding frame 10 drives the rotating ring 1101 and the transmission plate 14 to move downward and reset. The transmission plate 14 is squeezed by the annular soft strip 16 to rotate in the opposite direction and causes the torsion spring 15 to store force and twist again. When the transmission plate 14 passes the limit plate 17, the transmission plate 14 passes over the limit plate 17 by squeezing. The first spring 20 stretches and pushes the annular plate 18 to reset. Until the telescopic end of the first electric push rod 13 is fully extended, the sliding frame 10 stops moving downward. At this time, the position of the telescopic end of the sliding frame 10 is lower than its initial position. After that, the telescopic end of the first electric push rod 13 drives the sliding frame 10 to move downward and reset. The frame 10 moves upward again until the telescopic end of the first electric push rod 13 is reset, the sliding frame 10 is reset, and the transmission plate 14 again locks the limit plate 17, and the device is reset. When the catalyst agglomerates again, the above process is repeated to adjust the position of the annular filter 12 to loosen the catalyst in the annular filter 12. When the flow rate of hydrogen entering the air inlet pipe 3 is the same as the flow rate of the upper gas extracted by the vacuum pump in the reaction tank 1, the trihydroxymethylnitromethane solution is completely reacted, the staff will turn off the open electrical components, and then discharge the reacted solution through the discharge port of the reaction tank 1 and collect it. After the reaction solution is collected, the above process is repeated to prepare trihydroxymethylaminomethane again.

[0044] Further, such as Figure 2 and Figure 3 As shown, it also includes: a sliding component, which is arranged on the air intake pipe 3 and is used to adjust the distance between the exhaust pipe 5 and the atomizing shell 8. The sliding component includes: a second electric push rod 25, which is fixed to the fixing ring 9, and the air intake pipe 3 and the sliding shell 4 are slidingly connected. The telescopic end of the second electric push rod 25 is fixed to the limiting ring 26, and the limiting ring 26 is slidingly connected to the reaction tank 1; elastic rods 27, the number of which is the same as the number of exhaust pipes 5, are respectively fixed to adjacent exhaust pipes 5, and the elastic rods 27 are slidingly and rotatably connected to the limiting ring 26.

[0045] Further, such as Figure 2 and Figure 3 As shown, a second spring 24 is fixed between the intake pipe 3 and the sliding housing 4 , and the exhaust pipe 5 is hinged to the sliding housing 4 .

[0046] Further, such as Figure 2 、 Figure 3 、 Figure 5 、 Figure 8 and Figure 9 As shown, the included angle between the exhaust pipe 5 and the horizontal plane is less than 30°, and one end of the exhaust pipe 5 away from the air inlet pipe 3 is higher than the other end.

[0047] The above scheme provides a method of increasing the distance between the exhaust pipe 5 and the atomizing shell 8, reducing the impact force of hydrogen on the atomized solution sprayed from the atomizing shell 8, and reducing the manner in which the subsequent atomized solution adheres to the surface of the catalyst in the annular filter 12 during the process of adjusting the position of the annular filter 12. In this embodiment, the exhaust pipe 5 can only swing around the sliding shell 4 on the vertical plane to adjust the direction of the airflow discharged from the exhaust pipe 5. The second electric push rod 25 is used to drive the limit ring 26 to move, so that the limit ring 26 drives the exhaust pipe 5 to move through the elastic rod 27; the elastic rod 27 can be compressed. During the downward movement of the limit ring 26, the angle between the exhaust pipe 5 and the horizontal plane is adjusted by compressing the elastic rod 27. The elastic coefficient of the elastic rod 27 is greater than the elastic coefficient of the second spring 24, and is used to synchronously move the sliding shell 4 downward during the downward movement of the limit ring 26. The initial angle of the exhaust pipe 5 is used to make the gas blown out of the exhaust pipe 5 have an impact force on the atomized solution discharged from the atomizing shell 8, so that the atomized solution discharged from the atomizing shell 8 can normally contact the catalyst in the annular filter 12.

[0048] Working process: After the air pressure sensor detects the increase in air pressure between the annular filter 12 and the solution, the air pressure sensor transmits a signal to the first electric push rod 13 and the second electric push rod 25. The telescopic end of the first electric push rod 13 is retracted to drive the sliding frame 10 to move upward, and the telescopic end of the second electric push rod 25 is extended to drive the limiting ring 26 to move downward. The limiting ring 26 drives the exhaust pipe 5 to move downward through the elastic rod 27, reducing the impact of the exhaust gas from the exhaust pipe 5 on the atomizing shell 8 to blow out the atomized solution (the circulating pump can also be turned off at this time). The exhaust pipe 5 drives the sliding shell 4 to move downward and compresses the second spring 24. After the second spring 24 can no longer be compressed, the sliding shell 4 stops moving downward, and the limiting ring 26 continues to move upward. The elastic rod 27 moves downward and compresses the elastic rod 27, which drives the exhaust pipe 5 to rotate, so that the exhaust pipe 5 moves downward away from one end of the air inlet pipe 3, thereby adjusting the direction of the exhaust port of the exhaust pipe 5, further reducing the impact force of the gas on the atomized solution, and increasing the impact force on the annular filter 12, by blowing air flow toward the catalyst particles in the annular filter 12, thereby accelerating the flow of the solution between the catalyst particles in the annular filter 12, further accelerating the processing speed of the agglomerated catalyst, and ensuring the normal progress of the reaction. After the telescopic end of the second electric push rod 25 is fully extended, the limit ring 26 stops moving. Taking the limit ring 26 on the left side of Figure 3 as an example, at this time, the limit ring 26 is close to horizontal, and the left end of the limit ring 26 is higher than its right end.

[0049] As the position of the annular filter 12 is adjusted, when the telescopic end of the first electric push rod 13 drives the sliding frame 10 to move in the opposite direction and reset, the telescopic end of the second electric push rod 25 is retracted and drives the limit ring 26 to move in the opposite direction and reset. The extrusion force of the limit ring 26 on the elastic rod 27 is reduced, and the elastic rod 27 extends and resets, driving the exhaust pipe 5 to swing in the opposite direction and reset. After the elastic rod 27 is reset, as the limit ring 26 continues to move upward, the second spring 24 pushes the sliding shell 4 to move upward and reset.

[0050] The above description is only a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with this technical field can easily think of changes or replacements within the technical scope disclosed by the present invention, which should be covered by the scope of protection of the present invention.

Claims

1. A device for preparing pharmaceutical-grade tris(hydroxymethyl)aminomethane, characterized in that: Includes: A reaction tank (1), wherein the upper and lower sides of the reaction tank (1) are respectively provided with a feed port and a discharge port, and the lower part of the reaction tank (1) is provided with a circulation port (101); A motor (2) is fixedly connected to the reaction tank (1); An air intake pipe (3) is fixedly connected to the output shaft of the motor (2), the air intake pipe (3) is externally connected to a hydrogen tank, the air intake pipe (3) is provided with a sliding shell (4), and the air intake pipe (3) is connected to the sliding shell (4) through an air delivery pipe; There are multiple exhaust pipes (5), all of which are arranged on the sliding shell (4), and the exhaust pipes (5) are in communication with the sliding shell (4); A stirring frame (6) fixedly connected to the air inlet pipe (3); A liquid inlet pipe (7) is fixedly connected to the air inlet pipe (3), the liquid inlet pipe (7) is rotatably connected to the reaction tank (1), and the liquid inlet pipe (7) and the circulation port (101) are connected to a circulation pump via a hose; An atomizing shell (8) is fixedly connected to and communicated with the liquid inlet pipe (7); A fixed ring (9) is fixed to the reaction tank (1), the fixed ring (9) is fixed to a fixing frame (11) via a connecting rod, the fixed ring (9) and the fixing frame (11) rotate together to connect an annular filter (12), and the annular filter (12) is filled with a catalyst; A power assembly is provided in the reaction tank (1) and is used to adjust the position of the annular filter (12) to disperse the catalyst after the catalyst agglomerates in the annular filter (12); The power assembly includes: A first electric push rod (13) is fixedly connected to the reaction tank (1); a sliding frame (10) is fixedly connected to the telescopic end of the first electric push rod (13); the sliding frame (10) is slidably connected to the liquid inlet pipe (7); the sliding frame (10) is slidably connected to the fixed frame (11); an air pressure sensor is provided on the fixed ring (9); the air pressure sensor is used to detect the pressure of the gas in the reaction tank (1); A plurality of transmission plates (14) are hinged to the sliding frame (10) in a circumferentially uniform manner, and a torsion spring (15) is fixedly connected between the transmission plates (14) and the sliding frame (10); annular soft strips (16), the number of which is the same as the number of the transmission plates (14), and are uniformly fixed to the annular filter screen (12) in the circumferential direction; the fixing frame (11) and the fixing ring (9) are both slidably connected to the annular soft strips (16); the annular soft strips (16) are fixed with uniformly distributed limiting plates (17), and the limiting plates (17) are located on the moving path of the adjacent transmission plates (14); A smoothing component is arranged on the sliding frame (10) and is used to beat the catalyst in the annular filter (12) while driving the annular filter (12) to rotate.

2. The preparation device of pharmaceutical grade tris(hydroxymethylaminomethane) according to claim 1, characterized in that: The fixing ring (9) is located below the fixing frame (11).

3. The preparation device of pharmaceutical grade tris(hydroxymethyl)aminomethane according to claim 1, characterized in that: The limiting plate (17) is an L-shaped plate.

4. The preparation device of pharmaceutical grade tris(hydroxymethylaminomethane) according to claim 1, characterized in that: The smoothing component includes: A rotating ring (1101) is slidably connected to the liquid inlet pipe (7), and the rotating ring (1101) is rotatably connected to the sliding frame (10); an annular plate (18) rotatably and slidably connected to the rotating ring (1101); the annular plate (18) is fixedly connected to circumferentially distributed smoothing plates (19); the smoothing plates (19) are used to squeeze the annular filter screen (12); A vibration component is provided on the annular plate (18) and is used to drive the annular plate (18) to move up and down, so that the smoothing plate (19) strikes the annular filter (12).

5. The device for preparing pharmaceutical-grade tris(hydroxymethyl)aminomethane according to claim 4, characterized in that: The vibration component includes: The first spring (20) is fixed between the rotating ring (1101) and the annular plate (18). The annular plate (18) and the fixed frame (11) are fixed with circumferentially distributed extrusion blocks (21) on the opposite sides thereof. The extrusion blocks (21) at different heights squeeze each other to drive the annular plate (18) to move.

6. The device for preparing pharmaceutical-grade tris(hydroxymethyl)aminomethane according to claim 5, characterized in that: Also included are: A sliding assembly is provided on the air inlet pipe (3) and is used to adjust the distance between the exhaust pipe (5) and the atomizing shell (8). The sliding assembly comprises: A second electric push rod (25) is fixed to the fixed ring (9), the air inlet pipe (3) and the sliding shell (4) are slidably connected, the telescopic end of the second electric push rod (25) is fixed to a limiting ring (26), and the limiting ring (26) is slidably connected to the reaction tank (1); The elastic rods (27) are the same in number as the exhaust pipes (5) and are respectively fixed to adjacent exhaust pipes (5). The elastic rods (27) are connected to the limiting rings (26) in a sliding and rotational manner.

7. The device for preparing pharmaceutical-grade tris(hydroxymethyl)aminomethane according to claim 6, characterized in that: A second spring (24) is fixedly connected between the intake pipe (3) and the sliding shell (4), and the exhaust pipe (5) is hinged to the sliding shell (4).

8. The device for preparing pharmaceutical-grade tris(hydroxymethyl)aminomethane according to claim 7, characterized in that: The included angle between the exhaust pipe (5) and the horizontal plane is less than 30°, and one end of the exhaust pipe (5) away from the air inlet pipe (3) is higher than the other end.

Images