Preparation method and preparation device of novel tris (hydroxymethyl) aminomethane

Abstract

The invention belongs to the technical field of compound preparation, and relates to a preparation method and a preparation device of novel tris (hydroxymethyl) aminomethane. The method comprises the following steps: 1, spraying a methanol aqueous solution into a reaction tank in an atomization manner, directly contacting trimethylolmethane with the atomized methanol aqueous solution in the process of spraying the trimethylolmethane into the reaction tank, heating the interior of the reaction tank to 65-55 DEG C, and stirring for dissolving to form a solution; 2, adding charcoal activated carbon into the solution, keeping the temperature at 45-60 DEG C for 40 minutes, filtering while the solution is hot, and collecting filtrate; 3, carrying out reduced pressure concentration on the filtrate at the concentration temperature of 70-85 DEG C until crystals appear, and cooling and standing; and 4, separating the crystal by using a suction filtration method, leaching for 1-3 times by using absolute ethyl alcohol, and drying at 40-60 DEG C for 6 hours to obtain a finished product. According to the invention, trimethylolmethane and a methanol aqueous solution are rapidly combined by replacing the feeding states of the trimethylolmethane and the methanol aqueous solution, so that the preparation efficiency is improved.

Description

Technical Field

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

[0002] Tris(hydroxymethyl)aminomethane (TMA) is an important organic compound widely used in medicine and biochemical experiments. It has buffering capacity and can adjust pH to maintain a stable chemical environment. In addition, TMA plays a key role in the synthesis of various drugs. Because it can absorb hydrogen ions and correct acidosis, it is often used to treat acute metabolic and respiratory acidemia and is considered an ideal drug.

[0003] The following is a method for preparing trishydroxymethylaminomethane: 1. Add trishydroxymethylmethane to a methanol-water solution, heat and stir until completely dissolved; 2. Add charcoal activated carbon to the solution, keep it warm for a period of time, filter it while hot, and collect the filtrate; 3. Concentrate the filtrate under reduced pressure until crystals appear, then let it cool. The recovered methanol can be recycled; 4. Separate the crystals by suction filtration, rinse with anhydrous ethanol, and finally dry to obtain the finished product.

[0004] The tris(hydroxymethylaminomethane) produced by the above method not only meets experimental requirements but can also be used as a pharmaceutical intermediate in drug synthesis processes. However, existing tris(hydroxymethylaminomethane) production equipment has the following problems during production: when tris(hydroxymethylaminomethane) is directly mixed with a methanol-water solution, powder agglomeration is easily caused due to density differences and insufficient stirring. This causes the agglomerated material to suspend and settle, resulting in significantly inconsistent distribution of ingredients in the mixture, with some areas having too much, too little, or even no powder at all. This prolongs the dissolution time and reduces the material preparation efficiency. Summary of the Invention

[0005] In order to solve the problems mentioned in the background technology, the present invention provides a novel preparation method and preparation device of trishydroxymethylaminomethane.

[0006] The technical implementation scheme of the present invention is: a novel method for preparing trishydroxymethylaminomethane, comprising the following steps:

[0007] Step 1: spraying the methanol aqueous solution into the reaction tank in an atomized manner, wherein the trimethylolmethane directly contacts the atomized methanol aqueous solution during the spraying process into the reaction tank, and then heating the reaction tank to 55°C-65°C and stirring to dissolve, thereby forming a solution;

[0008] Step 2: Add activated charcoal to the solution, keep it at 45-60°C for 40 minutes, filter it while hot, and collect the filtrate;

[0009] Step 3: Concentrate the filtrate under reduced pressure at a temperature of 70°C-85°C until crystals appear, then let it cool.

[0010] Step 4: After separating the crystals by filtration, rinse with anhydrous ethanol 1-3 times, and dry at 40℃-60℃ for 6 hours to obtain the finished product.

[0011] Furthermore, during the addition of trimethylolmethane and methanol aqueous solution, the mass volume ratio of the two is 8:4-8, the methanol aqueous solution is prepared by mixing pure water and methanol in a volume ratio of 2:3, and the weight ratio of charcoal activated carbon to trimethylolmethane is 0.4-3:100.

[0012] A novel tris(hydroxymethyl)aminomethane preparation device is applied to the above-mentioned novel tris(hydroxymethyl)aminomethane preparation method, comprising:

[0013] A support frame, wherein a base is fixedly connected to the upper side of the support frame, a first guide shell is fixedly connected to the upper side of the base, a first fixed shell is fixedly connected to the outer side of the first guide shell, a fixed cylinder is fixedly connected to the outer side of the first fixed shell, a second fixed shell is fixedly connected to the inner side of the fixed cylinder, a cover plate is fixedly connected to the upper side of the second fixed shell, the second fixed shell and the fixed cylinder are jointly fixedly connected to a material guide tube and a mirror-distributed first liquid guide tube, the material guide tube is located between the mirror-distributed first liquid guide tubes, and the opposite sides of the mirror-distributed first liquid guide tubes are fixedly connected to and connected to an atomizing nozzle;

[0014] A dispersion component is provided on the base and located in the first guide shell, and is used for processing agglomerated materials in the first guide shell.

[0015] Furthermore, the second guide shell is fixedly connected between the second fixing shell and the first guide shell and is in contact with the first fixing shell. The inner side surface of the second guide shell is a wavy surface.

[0016] Furthermore, the dispersed components include:

[0017] a first driving member, disposed on the support frame, wherein a driving shaft of the first driving member passes through the base and is in sealed rotational connection therewith;

[0018] a rotating frame, fixedly connected to the driving shaft of the first driving member and located above the base;

[0019] A plurality of limiting rods are fixedly connected to the rotating frame;

[0020] A sliding frame is fixedly connected to the limiting rods distributed in a mirror image;

[0021] an elastic bellows, slidably connected to the mirror-imaged limiting rods, the elastic bellows being in sealing and sliding connection with the sliding frame, the sliding frame being provided with a plurality of first guide holes, and a first one-way valve being provided in each of the first guide holes of the sliding frame;

[0022] The porous plate is fixedly connected to the upper side of the elastic bellows. The aperture of the porous plate is larger than the aperture of the first guide hole of the sliding frame, and both holes are inclined.

[0023] Furthermore, the dispersed component further comprises:

[0024] a rotating member rotatably connected to the porous plate, the rotating member being provided with a plurality of second guide holes, the holes of the second guide holes of the rotating member corresponding one-to-one to the holes on the porous plate and having the same aperture, a second one-way valve being provided in the second guide holes of the rotating member, a guide rod being fixedly connected to the porous plate, the guide rod being slidably connected to a liquid housing, the liquid housing being sealingly and slidably connected to the rotating member, and a spring being provided between the liquid housing and the rotating member;

[0025] The pushing component is arranged in the second fixed shell and is used for driving the porous plate to move in a vertical direction.

[0026] Furthermore, the pushing component includes:

[0027] The second driving member is arranged in the second fixed shell through the connecting shell. The telescopic end of the second driving member is rotatably connected to the liquid holding shell. The liquid holding shell is slidably connected to a guide rod fixed to the upper part of the rotating member. The upper part of the liquid holding shell is provided with a plurality of spiral grooves. The guide rod moves along all the spiral grooves in the upper part of the liquid holding shell. The lower part of the liquid holding shell is fixed and connected to a second liquid guide pipe.

[0028] Furthermore, a stirring member is fixedly connected to the lower side of the rotating member, and the stirring member is composed of a circular ring and a plurality of corrugated plates located thereon. A liquid bag connected to the second liquid guide tube is provided on the outer side of the lower part of the rotating member.

[0029] Furthermore, a first annular inclined surface and an annular arc surface are provided on the upper part of the first guide shell, and the first annular inclined surface is located on the upper side of the annular arc surface. The upper side of the porous plate is fixedly connected to a third guide shell located below the arc surface of the first guide shell, and the upper side of the third guide shell is provided with a second annular inclined surface.

[0030] Furthermore, the lower part of the elastic bellows is provided with evenly distributed inclined holes, the sliding frame is used to seal all the inclined holes on the lower side of the elastic bellows, and the lower side of the elastic bellows is provided with a fourth guide shell corresponding one-to-one to the inclined holes on it, and the fourth guide shell is used to guide the material into the adjacent inclined holes on the elastic bellows.

[0031] The present invention has the following advantages: in order to solve the problem that, in the preparation of tris(hydroxymethyl)aminomethane in existing equipment, tris(hydroxymethyl)methane and methanol aqueous solution are easily agglomerated when directly mixed, and the dissolution time is prolonged when the agglomerated material is suspended and deposited, the present invention adopts a method of changing the feeding state of tris(hydroxymethyl)methane and methanol aqueous solution, so that the methanol aqueous solution is sprayed from two atomizing nozzles, and tris(hydroxymethyl)methane is sprayed from between the two atomizing nozzles, so that tris(hydroxymethyl)methane and methanol aqueous solution are already in contact when the material is discharged, thereby increasing the contact area between tris(hydroxymethyl)methane and methanol aqueous solution, allowing tris(hydroxymethyl)methane to be quickly dispersed in methanol aqueous solution, reducing the probability of powder agglomeration or even suspension and deposition, thereby shortening the preparation time of tris(hydroxymethyl)aminomethane and improving the preparation efficiency;

[0032] When preparing trishydroxymethylaminomethane, if agglomeration occurs, the present invention places the agglomerated material into an elastic bellows and presses and rubs the agglomerated material within the elastic bellows to destroy the internal structure of the agglomerated material, thereby redispersing the agglomerated material into smaller particles to facilitate subsequent process operations. The deagglomeration process also avoids material loss due to inability to participate in the reaction due to agglomeration, thereby improving material utilization. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 It is a schematic diagram of the three-dimensional structure of the present invention;

[0034] Figure 2 A bottom view of the three-dimensional structure of the present invention;

[0035] Figure 3 It is a three-dimensional structural diagram of the positional relationship between the first fixed shell and the fixed cylinder of the present invention;

[0036] Figure 4 A schematic diagram of the three-dimensional structure of the positional relationship between the fixing cylinder and the second guide shell of the present invention;

[0037] Figure 5 A schematic diagram of the three-dimensional structure of the positional relationship between the fixing cylinder and the second fixing shell of the present invention;

[0038] Figure 6 is a sectional view of the three-dimensional structure of the first guide housing of the present invention;

[0039] Figure 7 is a sectional view of the three-dimensional structure of the third guide housing of the present invention;

[0040] Figure 8 A sectional view of the three-dimensional structure of the elastic bellows of the present invention;

[0041] Figure 9A bottom view showing the three-dimensional structure of the rotating member and the stirring member of the present invention;

[0042] Figure 10 It is a sectional view of the three-dimensional structure of the liquid-containing shell of the present invention;

[0043] Figure 11 The figure is an exploded view showing the three-dimensional structure of the rotating member, the liquid storage shell and the guide rod of the present invention;

[0044] Figure 12 It is a schematic diagram of the three-dimensional structure of the liquid storage shell and the guide rod of the present invention.

[0045] The accompanying drawings are marked as follows: 1. support frame, 2. base, 3. first guide shell, 4. first fixed shell, 5. fixed cylinder, 6. second fixed shell, 7. cover plate, 8. material guide tube, 9. first liquid guide tube, 10. second guide shell, 11. first driving member, 12. rotating frame, 13. limiting rod, 14. sliding frame, 15. elastic bellows, 16. porous plate, 17. rotating member, 18. liquid holding shell, 19. guide rod, 20. second driving member, 21. guide rod, 22. second liquid guide tube, 23. stirring member, 24. liquid capsule, 25. third guide shell, 26. fourth guide shell. DETAILED DESCRIPTION

[0046] The following is a clear and complete description of 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 making creative efforts are within the scope of protection of the present invention.

[0047] When preparing tris(hydroxymethyl)aminomethane, if tris(hydroxymethyl)methane is directly mixed with methanol-water solution, the difference in density between the two and insufficient stirring can easily lead to powder agglomeration, resulting in suspension and sedimentation of agglomerated materials, inconsistent distribution of mixture components, affecting subsequent process steps, and ultimately reducing product quality and performance. To solve the above problems, the present invention adopts a method of replacing the feeding state of tris(hydroxymethyl)methane and methanol-water solution, so that the methanol-water solution is sprayed from two atomizing nozzles, and tris(hydroxymethyl)methane is placed between the two atomizing nozzles, so that tris(hydroxymethyl)methane begins to contact with methanol-water solution during discharge, thereby increasing the contact area between tris(hydroxymethyl)methane and methanol-water solution, and quickly dispersing tris(hydroxymethyl)methane in methanol-water solution, reducing the probability of powder agglomeration and even suspension and sedimentation.

[0048] Subsequently, tris(hydroxymethylaminomethane) and methanol aqueous solution are referred to as powder and liquid, and the mixture of the two is referred to as material.

[0049] A novel method for preparing trishydroxymethylaminomethane comprises the following steps:

[0050] Step 1: spraying the methanol aqueous solution into the reaction tank in an atomized manner, wherein the trimethylolmethane directly contacts the atomized methanol aqueous solution during the spraying process into the reaction tank, and then heating the reaction tank to 55°C-65°C and stirring to dissolve, thereby forming a solution;

[0051] Step 2: Add activated charcoal to the solution, keep it at 45-60°C for 40 minutes, filter it while hot, and collect the filtrate;

[0052] Step 3: Concentrate the filtrate under reduced pressure at a temperature of 70°C-85°C until crystals appear, then let it cool.

[0053] Step 4: After separating the crystals by filtration, rinse with anhydrous ethanol 1-3 times, and dry at 40℃-60℃ for 6 hours to obtain the finished product.

[0054] During the addition of trimethylolmethane and methanol aqueous solution, the mass volume ratio of the two is 8:4-8, the methanol aqueous solution is prepared by mixing pure water and methanol in a volume ratio of 2:3, and the weight ratio of charcoal activated carbon to trimethylolmethane is 0.4-3:100.

[0055] like Figures 1-6 As shown, a novel tris(hydroxymethyl)aminomethane preparation device of the present invention is applied to the novel tris(hydroxymethyl)aminomethane preparation method described above, comprising: a support frame 1, a base 2 is fixedly connected to the upper side of the support frame 1, a first guide shell 3 is fixedly connected to the upper side of the base 2, a first fixed shell 4 is fixedly connected to the outer side of the first guide shell 3, a fixed cylinder 5 is fixedly connected to the outer side of the first fixed shell 4, a second fixed shell 6 located above the first guide shell 3 is fixedly connected to the inner side of the fixed cylinder 5, and the second fixed shell 6 is located on the upper side of the first fixed shell 4, a cover plate 7 is fixedly connected to the upper side of the second fixed shell 6, and the second fixed shell 6 and the fixed cylinder 5 are jointly fixed with a guide pipe 8 and a mirror image dividing The first liquid guide pipe 9 of the cloth, the material guide pipe 8 is located between the first liquid guide pipes 9 of the mirror distribution, and the opposite sides of the mirror distribution first liquid guide pipes 9 are fixedly connected and connected with an atomizing nozzle. The powder transported by the material guide pipe 8 is located between the liquid sprayed by the atomizing nozzle on the mirror distribution first liquid guide pipe 9, so as to enable the powder and liquid to be mixed in advance; a dispersion component is arranged on the base 2 and located in the first guide shell 3, and is used to process the agglomerated material in the first guide shell 3. A second guide shell 10 that is in contact with the first fixed shell 4 is fixed between the second fixed shell 6 and the first guide shell 3, and the inner side surface of the second guide shell 10 is a wavy surface for increasing the heating area.

[0056] The above scheme provides a method in which when powder and liquid are mixed, powder is sprayed between two layers of mist liquid, so that powder and liquid begin to contact when discharging, thereby increasing the contact area between powder and liquid and reducing the uneven distribution caused by powder agglomeration. When using this device, an external feeding device (i.e., a device for conveying trishydroxymethylaminomethane) is connected to the rear side of the material guide pipe 8, and an external liquid feeding device (i.e., a device for conveying methanol aqueous solution) is connected to the rear sides of the two first liquid guide pipes 9. The first guide shell 3, the first fixed shell 4, the fixed cylinder 5, the second fixed shell 6 and the second guide shell 10 are all made of heat-conducting materials, and the second guide shell 10 is sealed to the first guide shell 3 and the second fixed shell 6.

[0057] like Figures 4-10 As shown, the dispersion component includes: a first driving member 11, which is arranged on the support frame 1, and the driving shaft of the first driving member 11 passes through the base 2 and is sealed and rotatably connected thereto; a rotating frame 12, which is fixed to the driving shaft of the first driving member 11 and is located above the base 2; a plurality of limit rods 13, all of which are fixed to the rotating frame 12; a sliding frame 14, which is fixed to the limit rods 13 distributed in a mirror image; an elastic bellows 15, which is slidably connected to the limit rods 13 distributed in a mirror image, and the elastic bellows 15 is sealed and slidably connected to the sliding frame 14, and the sliding frame 14 is provided with a plurality of first guide holes, and a first one-way valve is provided in the first guide hole of the sliding frame 14; a porous plate 16, which is fixed to the upper side of the elastic bellows 15, and the porous plate The aperture of hole 16 is larger than the aperture of the first guide hole of the sliding frame 14 and both holes are inclined. The dispersion component also includes: a rotating member 17, which is rotatably connected to the porous plate 16. The rotating member 17 is provided with a plurality of second guide holes. The holes of the second guide holes of the rotating member 17 correspond one-to-one to the holes on the porous plate 16 and the apertures of the two are consistent. A second one-way valve is provided in the second guide hole of the rotating member 17. The porous plate 16 is fixed with a guide rod 19, and the guide rod 19 is slidably connected to the liquid housing 18. The liquid housing 18 is sealed and slidably connected to the rotating member 17, and a spring is provided between the liquid housing 18 and the rotating member 17; a pushing component is provided in the second fixed shell 6, for driving the porous plate 16 to move in the vertical direction.

[0058] The above scheme provides that when the material lumps, the elastic bellows 15 actively contracts to squeeze the material entering the elastic bellows 15, destroying the internal structure of the agglomerated material, thereby facilitating subsequent processing. The first driving member 11 is a self-locking motor, and the first guide hole of the sliding frame 14 faces the outer edge of the base 2, which is used to drive the material to the four sides. When the elastic bellows 15 contracts, the first one-way valve in the first guide hole of the sliding frame 14 is in an open state. At this time, the material in the elastic bellows 15 can be sprayed out from the first guide hole on the sliding frame 14. The material sprayed here causes the material to be driven and impact the deposited material at the bottom of the base 2, causing the material to float upward again. The elastic bellows 15 can be made of fluororubber. When the elastic bellows 15 expands from the contracted state, the second one-way valve in the second guide hole of the rotating member 17 is in an open state. Hydraulic oil is stored between the rotating member 17 and the lower side of the liquid storage shell 18. The elastic coefficient of the elastic bellows 15 is less than the elastic coefficient of the spring in the liquid storage shell 18.

[0059] like Figure 5-Figure 12 As shown, the pushing assembly includes: a second driving member 20, which is arranged in the second fixed shell 6 through a connecting shell, and the telescopic end of the second driving member 20 is rotatably connected to the liquid holding shell 18. The liquid holding shell 18 is slidably connected to a guide rod 21 fixed to the upper part of the rotating member 17. The upper part of the liquid holding shell 18 is provided with a plurality of spiral grooves. The guide rod 21 moves along all the spiral grooves in the upper part of the liquid holding shell 18. The guide rod 21 is T-shaped, and the spiral grooves in the liquid holding shell 18 are two centrally symmetrically distributed. The lower part of the liquid holding shell 18 is fixed and connected to a second liquid guide tube 22.

[0060] In the above scheme, when the guide rod 21 moves upward along the two spiral grooves in the upper part of the liquid holding shell 18, the guide rod 21 drives the rotating part 17 to rotate, so that the rotating part 17 rubs the material in the elastic bellows 15 during the rotation process to achieve further processing of the agglomerated material.

[0061] like Figures 6-11 As shown, the lower side of the rotating member 17 is fixed with a stirring member 23, which is composed of a ring and a plurality of corrugated plates located thereon. The outer side of the lower part of the rotating member 17 is provided with a liquid bag 24 connected to the second liquid guide tube 22. The holes on the porous plate 16 close to the second liquid guide tube 22 are rotated in the counterclockwise direction (in Figure 1The top view is used as an example for description) and an arc groove is provided on the top for the movement of the second liquid guide tube 22. When the liquid capsule 24 expands, the surrounding materials are squeezed to reduce the particle size of the materials. The upper part of the first guide shell 3 is provided with a first annular inclined surface and an annular arc surface, and the first annular inclined surface is located on the upper side of the annular arc surface. The upper side of the porous plate 16 is fixed with a third guide shell 25 located below the arc surface of the first guide shell 3. The upper side of the third guide shell 25 is provided with a second annular inclined surface. The holes on the porous plate 16 are inclined, and the holes on the porous plate 16 face the third guide shell 25. The inner side surface is used to shorten the time for the material on the upper side of the third guide shell 25 to enter the elastic bellows 15. The first annular inclined surface and the annular arc surface on the first guide shell 3 are both used to guide the material to the upper side of the third guide shell 25. The lower part of the elastic bellows 15 is provided with evenly distributed inclined holes. The sliding frame 14 is used to block all the inclined holes on the lower side of the elastic bellows 15. The lower side of the elastic bellows 15 is provided with a fourth guide shell 26 corresponding to the inclined holes thereon. The fourth guide shell 26 is used to guide the material to the adjacent inclined holes on the elastic bellows 15.

[0062] Working principle: Before preparing tris(hydroxymethyl)aminomethane, the staff first connects the external feeding equipment and the external liquid feeding equipment to the rear sides of the two first liquid guiding tubes 9 on the rear side of the material guiding tube 8, and then connects the external heating equipment to this device to complete the preparation work before preparing tris(hydroxymethyl)aminomethane.

[0063] After completing the preparatory work for preparing trishydroxymethylaminomethane, the staff respectively feeds trimethylolmethane and methanol aqueous solution into the feed pipe 8 and the two first liquid guide pipes 9 through the external feeding equipment and the external liquid feeding equipment. The two first liquid guide pipes 9 spray the liquid from the atomizing nozzles on the opposite sides of the two guide pipes 9, so that the atomized liquid covers the front side of the feed pipe 8. The feed pipe 8 transports the powder to between the atomizing nozzles on the front side of the two guide pipes 8, so that the powder directly contacts the atomized liquid after being sprayed, thereby achieving the effect of pre-mixing the two.

[0064] During the preparation of trishydroxymethylaminomethane, the powder contacts the atomized liquid to form a material and falls downward (during this process, the staff heats the first guide shell 3 and the second guide shell 10 and their internal environment through external heating equipment). Part of the material falls downward to the upper side of the third guide shell 25 and the base 2, and the other part of the material slides along the inner wall of the second fixed shell 6 to the inner wall of the second guide shell 10. In the process of the material sliding along the inner wall of the second guide shell 10, the area of the material in contact with heat is increased through the second guide shell 10, thereby enhancing the heating efficiency of the material.

[0065] As the feeding work continues, the liquid level in the first guide shell 3 gradually rises to be full, and then enters the second guide shell 10, causing the liquid level in the second guide shell 10 to gradually rise. When the liquid level of the material is flush with the upper side of the second guide shell 10, no more powder and liquid are fed in (but there are still suspended and deposited agglomerated materials at this time). At this time, the telescopic end of the second driving member 20 is controlled to move downward by the control terminal, and the driving shaft of the first driving member 11 will not rotate at will. During the downward movement of the telescopic end of the second driving member 20, the liquid holding shell 18 is driven to move synchronously. Under the action of the spring between the rotating member 17 and the liquid holding shell 18, the liquid holding shell 18 will not be displaced relative to the guide rod 21 during the downward movement. At that time, the liquid holding shell 18, the guide rod 21, the rotating member 17, the porous plate 16, and the third guide shell 25 move downward, and the process of the porous plate 16 moving downward The elastic bellows 15 is squeezed in the middle. After the elastic bellows 15 is squeezed, the gas inside the bellows 15 first pushes open the first one-way valve in the first guide hole of the sliding frame 14, and then discharges from the first guide hole of the sliding frame 14 (when the elastic bellows 15 is squeezed until the pressure inside it does not decrease again, the first one-way valve in the first guide hole of the sliding frame 14 remains closed). The gas is discharged from the holes on the sliding frame 14 in an inclined manner to all sides, thereby blowing the agglomerated materials deposited on the upper side of the base 2, so that the materials are pushed by the gas to move toward the inner wall of the first guide shell 3, and part of the materials move upward along the inner wall of the first guide shell 3, lifting the deposited agglomerated materials. Part of the agglomerated materials gradually come into contact with the third guide shell 25 in the process of falling along the annular arc surface on the lower side of the upper part of the first guide shell 3, and move to the upper side and the holes of the porous plate 16 under the guidance of the upper side of the third guide shell 25.

[0066] When the lower side of the stirring member 23 is in contact with the upper side of the sliding frame 14, the telescopic end of the second driving member 20 continues to move downward. At this time, the spring in the liquid holding shell 18 is compressed, and the liquid holding shell 18 and the rotating member 17 produce relative displacement (the liquid holding shell 18 and the guide rod 19 also produce relative displacement). At that time, the hydraulic oil between the liquid holding shell 18 and the upper part of the rotating member 17 is compressed, and then enters the liquid bag 24 through the guidance of the second liquid guide tube 22, causing the liquid bag 24 to expand.

[0067] When the liquid holding shell 18 and the rotating part 17 produce relative displacement, the guide rod 21 slides along the two spiral grooves in the liquid holding shell 18, so that the guide rod 21 and the rotating part 17 can rotate during the relative displacement with the liquid holding shell 18, and the rotating part 17 drives the stirring part 23 to rotate synchronously during the rotation process.

[0068] When the upper side of the guide rod 21 slides on the upper side of the spiral groove in the liquid receiving shell 18, the telescopic portion of the second driving member 20 stops extending and then retracts.

[0069] When the telescopic part of the second driving member 20 moves upward, the second driving member 20 drives the liquid holding shell 18 to move upward. Under the action of the extension and reset of the spring in the liquid holding shell 18, the liquid holding shell 18, the guide rod 21 and the rotating member 17 are displaced in the opposite direction. During the displacement of the guide rod 21, it moves downward and reset relative to the liquid holding shell 18 along the two spiral grooves in the liquid holding shell 18 (the guide rod 21 drives the rotating member 17 to rotate in the opposite direction during the process). During the downward movement and reset of the rotating member 17 relative to the liquid holding shell 18, the hydraulic oil in the liquid bag 24 is extracted through the second liquid guide tube 22, so that the liquid bag 24 contracts and recovers.

[0070] When the guide rod 21 is located at the lower side of the spiral groove in the liquid holding shell 18, the telescopic part of the second driving member 20 moves upward to reset, and can drive the porous plate 16 to move upward to reset through the liquid holding shell 18 and the rotating member 17. During the upward movement of the porous plate 16, the upper part of the elastic bellows 15 is stretched, and the elastic bellows 15 maintains contact with the sliding frame 14 when resetting due to its own elastic force.

[0071] As the porous plate 16 pulls the upper side of the elastic bellows 15, the pressure inside the elastic bellows 15 gradually decreases, causing the second one-way valve in the second guide hole of the rotating member 17 to be in an open state, so that the agglomerated material falling on the upper side of the porous plate 16 can enter the elastic bellows 15 along the holes of the porous plate 16 and the second guide hole of the rotating member 17, thereby realizing the collection of the material before processing and facilitating the subsequent processing of the material.

[0072] When the telescopic portion of the second driving member 20 is retracted to the initial state (i.e. Figure 4 and Figure 5 The elastic bellows 15 returns to its initial state (at this time, the pressure in the elastic bellows 15 will not change arbitrarily, the second one-way valve in the second guide hole of the rotating member 17 remains closed, and the elastic bellows 15 remains sealed). Subsequently, the telescopic portion of the second driving member 20 is controlled by the control terminal to move downward, and the downward movement process of the telescopic portion of the second driving member 20, the liquid holding shell 18, and the parts thereon repeats the above-mentioned action until the stirring member 23 moves downward and is blocked by the material. The stirring member 23 and the rotating member 17 stop moving, and the subsequent rotation of the rotating member 17 is consistent with the above-mentioned rotation of the rotating member 17.

[0073] The lower side of the rotating member 17 squeezes the material in the elastic bellows 15 during its downward movement, disintegrating the agglomerated material. When the liquid housing 18 and the rotating member 17 produce relative displacement, the liquid capsule 24 expands through the conduction of hydraulic oil. During the expansion of the liquid capsule 24, the surrounding material is squeezed, and under the action of the rotation of the rotating member 17 and the stirring member 23, the agglomerated material is rubbed to reduce the particle size of the agglomerated material, thereby accelerating the subsequent dissolution rate. The subsequent processing steps for the agglomerated material can repeat the above actions. The elastic bellows 15 will squeeze out the agglomerated material processed last time from the lower side through the material entering from above during the next compression.

[0074] After the processing of the agglomerated material is completed, the control terminal controls the telescopic part of the second driving member 20 to move upward (at this time, the telescopic end of the second driving member 20 will move upward again based on the premise of the above process), so that the telescopic part of the second driving member 20 pulls the porous plate 16 and the elastic bellows 15 upward through the liquid holding shell 18, the guide rod 21, and the rotating member 17. During the upward movement of the elastic bellows 15, its lower side slides along the two limit rods 13. When the upper side surface of the lower part of the elastic bellows 15 contacts the limit rod 13 (the telescopic part of the second driving member 20 stops moving), the upper side surface of the sliding frame 14 no longer contacts the lower side surface of the elastic bellows 15, and the sliding frame 14 no longer blocks the inclined hole on the lower side of the elastic bellows 15.

[0075] After the oblique hole on the lower side of the elastic bellows 15 is exposed, the material enters the elastic bellows 15 through the oblique hole on the lower side of the elastic bellows 15. At this time, the first driving member 11 is started through the control terminal. The driving shaft of the first driving member 11 drives the rotating frame 12, the two limit rods 13, the elastic bellows 15, the guide rod 19, and the liquid holding shell 18 to rotate clockwise along the telescopic end of the second driving member 20 (clockwise when viewed from top to bottom), stirring the material (the material entering the elastic bellows 15 can push open the one-way valve in the hole on the sliding frame 14 and flow out from the hole on the sliding frame 14), thereby accelerating the mixing speed of the material (when cleaning the device later, it can be cleaned according to the current state).

[0076] During the mixing process of the materials, the staff put charcoal activated carbon into the materials, and then maintained the current temperature through external heating equipment until the mixing of the materials was completed.

[0077] After the stirring of the material is completed, the movement of the first driving member 11 is stopped first, and then the material is taken out from the first guide shell 3 and the second guide shell 10, and placed in the subsequent equipment to continue processing the material, and then the device is cleaned to complete the use of the device.

[0078] Before tris(hydroxymethylaminomethane) needs to be prepared again, the staff controls the second driving member 20 through the control terminal to push the liquid container 18, the elastic bellows 15 and its accessories downward, and the elastic bellows 15 moves to a state where its lower side is in contact with the upper side of the sliding frame 14 and all the inclined holes on the lower side of the elastic bellows 15 are blocked by the sliding frame 14.

[0079] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A novel method for preparing trishydroxymethylaminomethane, characterized in that: The following steps are included: Step 1: spraying the methanol aqueous solution into the reaction tank in an atomized manner, wherein the trimethylolmethane directly contacts the atomized methanol aqueous solution during the spraying process into the reaction tank, and then heating the reaction tank to 55°C-65°C and stirring to dissolve, thereby forming a solution; Step 2: Add activated charcoal to the solution, keep it at 45-60°C for 40 minutes, filter it while hot, and collect the filtrate; Step 3: Concentrate the filtrate under reduced pressure at a temperature of 70°C-85°C until crystals appear, then let it cool. Step 4: After separating the crystals by filtration, rinse with anhydrous ethanol 1-3 times, and dry at 40℃-60℃ for 6 hours to obtain the finished product.

2. The method for preparing a novel trishydroxymethylaminomethane according to claim 1, wherein: During the addition of trimethylolmethane and methanol aqueous solution, the mass volume ratio of the two is 8:4-8. The methanol aqueous solution is prepared by mixing pure water and methanol in a volume ratio of 2:3, and the weight ratio of charcoal activated carbon to trimethylolmethane is 0.4-3:

100.

3. A novel tris(hydroxymethyl)aminomethane preparation device, applied to the novel tris(hydroxymethyl)aminomethane preparation method according to claim 1, characterized in that: include: A support frame (1) is provided, wherein the upper side of the support frame (1) is fixedly connected to a base (2), the upper side of the base (2) is fixedly connected to a first guide shell (3), the outer side of the first guide shell (3) is fixedly connected to a first fixed shell (4), the outer side of the first fixed shell (4) is fixedly connected to a fixed cylinder (5), the inner side of the fixed cylinder (5) is fixedly connected to a second fixed shell (6), the upper side of the second fixed shell (6) is fixedly connected to a cover plate (7), the second fixed shell (6) and the fixed cylinder (5) are jointly fixedly connected to a material guide pipe (8) and a mirror-distributed first liquid guide pipe (9), the material guide pipe (8) is located between the mirror-distributed first liquid guide pipes (9), and the opposite sides of the mirror-distributed first liquid guide pipes (9) are fixedly connected to and communicated with an atomizing nozzle; a dispersion component is provided on the base (2) and located in the first guide shell (3), and is used to process agglomerated materials in the first guide shell (3).

4. A novel tris(hydroxymethyl)aminomethane preparation device according to claim 3, characterized in that: The second guide shell (10) is fixedly connected between the second fixed shell (6) and the first guide shell (3) and is in contact with the first fixed shell (4). The inner side surface of the second guide shell (10) is a wavy surface.

5. A novel tris(hydroxymethyl)aminomethane preparation device according to claim 4, characterized in that: The dispersed components include: A first driving member (11) is arranged on the support frame (1), and a driving shaft of the first driving member (11) passes through the base (2) and is connected to the base in a sealed and rotatable manner; A rotating frame (12) is fixedly connected to the driving shaft of the first driving member (11) and is located above the base (2); A plurality of limiting rods (13) are fixedly connected to the rotating frame (12); A sliding frame (14) is fixedly connected to the limiting rods (13) distributed in a mirror image; An elastic bellows (15) is slidably connected to the mirror-distributed limit rods (13), the elastic bellows (15) is sealed and slidably connected to the sliding frame (14), the sliding frame (14) is provided with a plurality of first guide holes, and a first one-way valve is provided in the first guide hole of the sliding frame (14); a porous plate (16) is fixed to the upper side of the elastic bellows (15), the aperture of the porous plate (16) is larger than the aperture of the first guide hole of the sliding frame (14), and both holes are inclined.

6. A novel tris(hydroxymethyl)aminomethane preparation device according to claim 5, characterized in that: The dispersion assembly further comprises: A rotating member (17) is rotatably connected to the porous plate (16). The rotating member (17) is provided with a plurality of second guide holes. The holes of the second guide holes of the rotating member (17) correspond to the holes on the porous plate (16) one by one and the hole diameters of the two are consistent. A second one-way valve is provided in the second guide hole of the rotating member (17). The porous plate (16) is fixed with a guide rod (19). The guide rod (19) is slidably connected to a liquid housing (18). The liquid housing (18) is sealed and slidably connected to the rotating member (17). A spring is provided between the liquid housing (18) and the rotating member (17). The pushing component is arranged in the second fixed shell (6) and is used to drive the porous plate (16) to move in the vertical direction.

7. A novel tris(hydroxymethyl)aminomethane preparation device according to claim 6, characterized in that: The pushing component includes: The second driving member (20) is arranged in the second fixed housing (6) through the connecting housing. The telescopic end of the second driving member (20) is rotatably connected to the liquid holding housing (18). The liquid holding housing (18) is slidably connected to a guide rod (21) fixed to the upper part of the rotating member (17). The upper part of the liquid holding housing (18) is provided with a plurality of spiral grooves. The guide rod (21) moves along all the spiral grooves in the upper part of the liquid holding housing (18). The lower part of the liquid holding housing (18) is fixed to and communicated with a second liquid guide pipe (22).

8. The novel tris(hydroxymethyl)aminomethane preparation device according to claim 7, characterized in that: A stirring member (23) is fixedly connected to the lower side of the rotating member (17), and the stirring member (23) is composed of a circular ring and a plurality of corrugated plates located thereon. A liquid bag (24) connected to the second liquid guide tube (22) is provided on the outer side of the lower part of the rotating member (17).

9. A novel tris(hydroxymethyl)aminomethane preparation device according to claim 8, characterized in that: The upper portion of the first guide shell (3) is provided with a first annular inclined surface and an annular arc surface, and the first annular inclined surface is located on the upper side of the annular arc surface. The upper side of the porous plate (16) is fixedly connected to a third guide shell (25) located below the arc surface of the first guide shell (3), and the upper side of the third guide shell (25) is provided with a second annular inclined surface.

10. The novel tris(hydroxymethyl)aminomethane preparation device according to claim 9, characterized in that: The lower part of the elastic bellows (15) is provided with evenly distributed inclined holes, the sliding frame (14) is used to block all the inclined holes on the lower side of the elastic bellows (15), and the lower side of the elastic bellows (15) is provided with a fourth guide shell (26) corresponding to the inclined holes on it, and the fourth guide shell (26) is used to guide the material into the adjacent inclined holes on the elastic bellows (15).

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