Preparation device and method of high-dispersion platinum group noble metal-based catalyst

Abstract

The invention belongs to the technical field of catalyst preparation, and particularly relates to a preparation method of a high-dispersion platinum group noble metal-based catalyst, which comprises the following steps: preparing a porous rod-like cobaltosic oxide carrier material, cleaning with deionized water, drying, and roasting for 4-8 hours; dissolving chloroplatinic acid or platinum chloride in deionized water to form a noble metal solution; soaking the treated cobaltosic oxide carrier in a noble metal solution, taking out the carrier from the solution after soaking is completed, filtering, cleaning, drying, and roasting for 4-6 hours in an inert gas atmosphere; and keeping the temperature and reducing for 2-4 hours in a hydrogen atmosphere. When the porous rodlike cobaltosic oxide carrier material is prepared, firstly, a cobalt chloride solution is poured into the lower part of the double-layer cavity for stirring, a urea solution drips into the cavity through a spray head in the stirring process, a stirring barrel is turned over after stirring is completed, the stirred solution flows out and is filtered, the cobalt chloride solution and the urea solution are continuously added into the double-layer cavity for stirring and mixing, and the porous rodlike cobaltosic oxide carrier material is prepared. Therefore, the porous rod-like cobalt oxide solvent material is efficiently prepared.

Description

Technical Field

[0001] The present invention relates to the technical field of catalyst preparation, and particularly relates to a preparation device and method for a highly dispersed platinum group noble metal-based catalyst. Background Art

[0002] With the expansion of the application fields of natural gas, its atmospheric emissions have become an increasingly serious environmental problem. Designing and developing a low-temperature and highly efficient methane catalytic combustion catalyst is of great significance. Platinum group metal (Pd, Pt, Rh, etc.) catalysts have very important applications in many key fields of energy conversion and environmental protection, and are also the catalyst systems with the most extensive research and the best low-temperature activity in methane catalytic combustion reactions.

[0003] The processing steps of the highly dispersed platinum group noble metal-based catalyst are divided into raw material preparation and pretreatment, noble metal loading, surface modification and shaping, activation and detection. And in the raw material preparation and pretreatment, carrier material treatment is included. Usually, the following carrier preparation steps are adopted: Dissolve 4.7586 g of cobalt chloride in 60 mL of deionized water to form a 0.3 mol / L cobalt chloride solution, and take 6.006 g of urea and dissolve it in 20 mL of deionized water to form a 5 mol / L urea solution. Under stirring conditions, gradually drop the urea solution into the cobalt chloride solution, and continue stirring for 30 min after the dropping is completed. Transfer the mixed solution to a hydrothermal reaction kettle, carry out hydrothermal reaction at 140 °C for 12 h, then cool to room temperature, filter, wash with hot water at 80 °C, dry in an oven at 80 °C for 12 h, and calcine at 300 °C for 4 h to obtain a porous rod-shaped cobalt tetroxide carrier. The processing process of traditional preparation equipment is relatively cumbersome, it is not convenient to control the dropping of the urea solution, and at the same time, it is necessary to stop the machine during the discharging process, and it is laborious to take out the materials on the inner wall, which affects the processing efficiency. Summary of the Invention

[0004] The purpose of the present invention is to solve the disadvantages in the prior art that it is not convenient to control the dropping of the urea solution when preparing porous rod-shaped cobalt oxide, and at the same time, it is necessary to stop the machine during the discharging process, and it is laborious to take out the materials on the inner wall, which affects the processing efficiency. A preparation device and method for a highly dispersed platinum group noble metal-based catalyst are proposed, so as to effectively mix the solvent, improve the uniformity and dispersibility of the solvent, and further facilitate the efficient preparation of porous rod-shaped cobalt oxide and enhance its stability.

[0005] In order to achieve the above purpose, the present invention adopts the following technical scheme:

[0006] A preparation method for a highly dispersed platinum group noble metal-based catalyst includes the following steps:

[0007] S1. Prepare a porous rod-shaped cobalt tetroxide carrier material, wash it with deionized water, dry it in an oven at 60 - 120 °C, and calcine it at 300 - 500 °C for 4 - 8 h after drying;

[0008] S2. Dissolve the noble metal precursor in deionized water to form a noble metal solution, where the noble metal precursor includes chloroplatinic acid or platinum chloride;

[0009] S4. Immerse the treated cobalt tetroxide support in the noble metal solution. After the impregnation is completed, take out the support from the solution, filter, wash it, and then dry it at 60 - 120 °C to remove the solvent. After drying, calcine it in an inert gas atmosphere for 4 - 6 h, where the calcination temperature is 300 - 500 °C;

[0010] S5. Keep the temperature at 300 - 500 °C and reduce it in a hydrogen atmosphere for 2 - 4 h to obtain the product;

[0011] Among them, the preparation of the porous rod-shaped cobalt tetroxide support material specifically includes the following sub-steps:

[0012] S11: Add the urea solution into the water tank, and pour the cobalt chloride solution into the lower part of the double-layer cavity through the feed pipe and stir;

[0013] S12: During the stirring process, pump the urea solution in the water tank into the spray head and drip it into the cavity through the spray holes, while continuing to stir;

[0014] S13: After the stirring is completed, turn over the stirring barrel, exchange the positions of the upper and lower parts of the double-layer cavity, so that the material in the upper part of the cavity flows into the filter box for filtration;

[0015] S14: Continue to add the cobalt chloride solution and the urea solution under the cavity and stir and mix them;

[0016] S15: During the mixing process, reciprocate the scraper to turn over the precipitate.

[0017] In a possible design, after step S2, the following steps are further included:

[0018] S3: Add titanium dioxide and alumina into deionized water, stir and disperse them evenly to prepare a surface modification component liquid. Immerse the calcined catalyst material in the surface modification component liquid for 1 - 2 h and then take it out, filter, wash it, and then dry it at 60 - 120 °C for 30 - 60 min. After drying, perform a shaping treatment by pressing, granulating or spray drying.

[0019] A preparation device for a highly dispersed platinum group noble metal-based catalyst, comprising a base, wherein two support seats are fixedly arranged on the top of the base, and the same stirring barrel is rotatably arranged through between the two support seats. End caps for sealing the stirring barrel are fixedly arranged at both ends of the stirring barrel. A partition is fixedly arranged inside the stirring barrel, and the partition divides the inside of the stirring barrel into two cavities for alternating use. A feed pipe corresponding to the cavity is fixedly arranged through one side of the end cap for cobalt chloride solution to enter the cavity.

[0020] A water tank, the water tank is fixedly arranged on the top of the base. A rotating ring is rotatably sleeved on the outer wall of the stirring barrel, and a spraying mechanism is arranged on the top of the rotating ring for spraying the urea solution in the water tank into the lower cavity.

[0021] A stirring mechanism is arranged on the stirring barrel for stirring the solvents in the cavity and providing power for the spraying mechanism.

[0022] Two filter boxes, both of the two filter boxes are fixedly arranged on the top of the base and are located below the corresponding feed pipes for receiving the solvents. A filter plate for filtering the solvents is fixedly arranged inside the filter box.

[0023] A first rotating shaft is rotatably arranged through between the two support seats. A first gear is fixedly sleeved on the outer wall of the first rotating shaft. An external tooth ring meshing with the first gear is fixedly sleeved on the outer wall of the stirring barrel. A rotating block is rotatably sleeved on the outer wall of the first rotating shaft, and the rotating block is fixedly connected with the rotating ring for limiting the rotating ring. A first motor is fixedly arranged on one side of one of the support seats, and the output end of the first motor is fixedly connected with the first rotating shaft.

[0024] In a possible design, the spraying mechanism includes an annular pipe embedded in the rotating ring. Two spray heads are arranged on the annular pipe. A first connecting pipe is fixedly arranged on the top of the rotating ring, the bottom end of the first connecting pipe is communicated with the annular pipe, the top end of the first connecting pipe is communicated with an air bag, and the top end of the air bag is communicated with the water tank through a second connecting pipe. Two groups of spray holes for cooperating with the two spray heads are arranged on the outer wall of the stirring barrel.

[0025] In a possible design, a first one-way valve is arranged on the first connecting pipe, and a second one-way valve is arranged on the second connecting pipe for controlling the flow direction of the urea solvent.

[0026] In a possible design, the stirring mechanism includes a second rotating shaft rotatably arranged through the partition plate. Both ends of the second rotating shaft are rotatably connected to two end covers respectively. An installation frame is fixedly arranged at the outer end of one of the end covers. A second motor is fixedly arranged on the installation frame. The output end of the second motor is fixedly connected to the second rotating shaft. Two groups of stirring spoons are fixedly arranged on the outer wall of the second rotating shaft. The two groups of stirring spoons are respectively located in two cavities and become shorter in turn along the inclination direction of the cavities.

[0027] In a possible design, a first sliding rod is slidably arranged through one side of the support seat. One end of the first sliding rod contacts the outer wall of the airbag. A first spring is sleeved on the outer wall of the first sliding rod. Both ends of the first spring are fixedly connected to one side of the support seat and the outer wall of the first sliding rod respectively. A first fixing seat is fixedly arranged on one side of the end cover. A push rod used in cooperation with the first sliding rod is slidably arranged through the top of the first fixing seat. Extension blocks are fixedly arranged on both sides of the push rod. A first guiding rod is fixedly arranged on the top of the extension block. Both of the first guiding rods are slidably arranged through the top of the first fixing seat. A second spring is sleeved on the outer wall of the first guiding rod. Both ends of the second spring are fixedly connected to the mutually close sides of the extension block and the first fixing seat respectively. Cam wheels used in cooperation with the push rod are fixedly sleeved on the outer walls of both ends of the second rotating shaft for pushing the push rod to move upward.

[0028] In a possible design, two stirring shafts are rotatably arranged through between the two end covers. The two stirring shafts are respectively located in corresponding cavities. Second gears are fixedly sleeved on the outer walls of the stirring shafts. A second fixing seat is fixedly arranged on one side of the end cover. A rack meshing with the second gear is slidably arranged through the top of the second fixing seat. The bottom end of the rack is connected to the cam wheel through a connecting part for driving the stirring shaft to rotate reciprocally to stir the solvent in the cavity.

[0029] In a possible design, the connecting part includes a second guiding rod slidably arranged through the top of the second fixing seat. The bottom ends of the rack and the second guiding rod are fixedly provided with the same connecting frame. An extension column is fixedly arranged on one side of the connecting frame. An annular groove is formed at the outer end of the cam wheel. The extension column is located in the annular groove for driving the rack to move up and down reciprocally.

[0030] In a possible design, two third guiding rods are slidably arranged through the filter box. A plurality of scraping plates are fixedly sleeved on the outer walls of the two third guiding rods. The bottoms of the plurality of scraping plates all contact the filter plate. One of the scraping plates is used in cooperation with the corresponding push rod through a transmission part for turning over the sediment on the filter plate.

[0031] In a possible design, the transmission member includes a second sliding rod that penetrates and slides on one side of the support base. One end of the second sliding rod abuts against the support base, and the other end of the second sliding rod is fixedly connected to one of the scraping plates. A tension spring is sleeved on the outer wall of the second sliding rod, and both ends of the tension spring are fixedly connected to one side of the support base and the outer wall of the second sliding rod respectively. The second sliding rod is used in cooperation with the corresponding push rod.

[0032] Beneficial effects: In the present invention, for the preparation device of the highly dispersed platinum group noble metal-based catalyst, by providing a rotatable stirring barrel and arranging a partition in the stirring barrel to divide it into two cavities for alternating use, the function of continuously preparing the highly dispersed platinum group noble metal-based catalyst in the same device is realized, significantly improving the preparation efficiency and reducing the equipment occupation space.

[0033] In the present invention, for the preparation device of the highly dispersed platinum group noble metal-based catalyst, the stirring barrel is driven to rotate by a first motor, and at the same time, by using the stirring mechanism and the spraying mechanism, the automatic spraying of the urea solution and the uniform stirring of the solvent are realized, without manual intervention, improving the automation degree of the preparation process, reducing the operation difficulty. By setting a first one-way valve and a second one-way valve in the spraying mechanism, the accurate flow direction of the urea solution is ensured, avoiding the problem of improper solvent mixing, and improving the stability and accuracy of the preparation process.

[0034] In the present invention, for the preparation device of the highly dispersed platinum group noble metal-based catalyst, in the stirring mechanism, the stirring spoons with gradually shortened lengths and the reciprocally rotating stirring shaft are adopted, which can more effectively mix the solvent, improving the uniformity and dispersion of the solvent, and being beneficial to preparing a high-quality highly dispersed platinum group noble metal-based catalyst.

[0035] In the present invention, for the preparation device of the highly dispersed platinum group noble metal-based catalyst, by providing a filter box and a scraping plate mechanism, the solvent can be automatically collected and filtered during the preparation process, and at the same time, by using the linkage effect of the push rod and the scraping plate, the sediment on the filter plate can be automatically cleaned, enabling it to quickly filter the required sediment.

[0036] In the present invention, through the newly designed stirring barrel and partition structure, the alternating use of the two cavities is realized, improving the preparation efficiency, and being able to automatically discharge the material after flipping; the combination of the spraying mechanism and the stirring mechanism ensures the uniform mixing and efficient preparation of the solvent. At the same time, the setting of the filter box and the scraping plate mechanism realizes the automatic filtration of the solvent and the automatic cleaning of the sediment. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Figure 1 It is a three-dimensional structure diagram of a preparation device for a highly dispersed platinum group noble metal-based catalyst proposed by the present invention.

[0038] Figure 2 Schematic structural diagram of the stirring barrel of a preparation device for a highly dispersed platinum group noble metal-based catalyst proposed by the present invention;

[0039] Figure 3 Schematic cross-sectional structural diagram of the stirring barrel of a preparation device for a highly dispersed platinum group noble metal-based catalyst proposed by the present invention;

[0040] Figure 4 Schematic cross-sectional structural diagram of the rotating ring of a preparation device for a highly dispersed platinum group noble metal-based catalyst proposed by the present invention;

[0041] Figure 5 Schematic structural diagram of the end cover of a preparation device for a highly dispersed platinum group noble metal-based catalyst proposed by the present invention;

[0042] Figure 6 Schematic structural diagram of the cam of a preparation device for a highly dispersed platinum group noble metal-based catalyst proposed by the present invention;

[0043] Figure 7 Schematic structural diagram of the filter box of a preparation device for a highly dispersed platinum group noble metal-based catalyst proposed by the present invention.

[0044] In the figure: 1, base; 2, support seat; 3, stirring barrel; 4, first rotating shaft; 5, first motor; 6, external toothed ring; 7, first gear; 8, end cover; 9, second rotating shaft; 10, feed pipe; 11, water tank; 12, filter box; 13, mounting frame; 14, second motor; 15, first sliding rod; 16, push rod; 17, rotating ring; 18, rotating block; 19, first connecting pipe; 20, first one-way valve; 21, airbag; 22, second connecting pipe; 23, second one-way valve; 24, first spring; 25, stirring shaft; 26, stirring spoon; 27, partition board; 28, cavity; 29, annular pipe; 30, nozzle; 31, spray hole; 32, second gear; 33, rack; 34, cam; 35, first fixing seat; 36, first guide rod; 37, extension block; 38, second spring; 39, second fixing seat; 40, second guide rod; 41, connecting frame; 42, extension column; 43, annular groove; 44, filter plate; 45, third guide rod; 46, scraper; 47, second sliding rod; 48, tension spring. Specific embodiments

[0045] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments.

[0046] Embodiment 1

[0047] Preparation of porous rod-shaped cobalt ferrite carrier material:

[0048] Add a urea solution (concentration: 0.2 mol / L) into the water tank, and add a cobalt chloride solution (concentration: 0.1 mol / L) to the water tank. Start the stirring device to fully mix the urea solution and the cobalt chloride solution in the water tank. At the same time, the urea solution drips from the nozzle to the lower part of the double-layer cavity and mixes with the cobalt chloride solution to form cobalt precipitate. Continue stirring for a period of time to ensure uniform mixing. After completion of stirring, turn over the double-layer cavity to swap the upper and lower positions. The mixture flows into the filtration box, and the cobalt precipitate is separated by filtration. Continue to add cobalt chloride solution and urea solution below the double-layer cavity and continue stirring and mixing to ensure completion of the reaction. During this process, use a scraper to reciprocate and turn over the precipitate to make the precipitate evenly distributed.

[0049] The filtered precipitate is sent to an oven and dried at 120 °C for 5 hours. After removing the moisture, it is calcined at 500 °C for 8 hours to convert the cobalt precipitate into cobalt tetroxide. During the calcination process, the cobalt tetroxide forms a porous structure and provides excellent surface properties for the subsequent catalyst support.

[0050] Preparation of highly dispersed platinum group noble metal-based catalyst:

[0051] Dissolve chloroplatinic acid (concentration: 0.01 mol / L) in deionized water to form a uniform noble metal solution.

[0052] Immerse the calcined porous rod-shaped cobalt tetroxide support in the noble metal solution to ensure uniform impregnation. After completion of impregnation, take out the support, filter and wash it with deionized water to remove the excess noble metal solution. After washing, dry it at 120 °C to remove the solvent.

[0053] Calcine the dried support in an inert gas atmosphere at a calcination temperature of 500 °C for 6 hours. During the calcination process, the dispersion of the noble metal is further stabilized, and good combination of the noble metal and the support is promoted.

[0054] After completion of calcination, maintain the temperature at 500 °C, place the support in a hydrogen atmosphere, and carry out reduction treatment for 4 hours to reduce the noble metal to a highly active state and further improve the activity of the catalyst.

[0055] Example 2

[0056] Refer to Figure 1 - Figure 7, the present invention also provides a preparation device for a highly dispersed platinum group noble metal-based catalyst, which is used in the field of catalyst preparation and includes: a base 1, and two support seats 2 are fixedly arranged on the top of the base 1. A stirring barrel 3 is rotatably arranged through between the two support seats 2, and end covers 8 are fixedly arranged at both ends of the stirring barrel 3, and the end covers 8 are used to seal the stirring barrel 3. A partition plate 27 is fixedly arranged inside the stirring barrel 3, and the partition plate 27 divides the inside of the stirring barrel 3 into two alternately used cavities 28. A feed pipe 10 corresponding to the cavity 28 is fixedly arranged through one side of the end cover 8, and is used to input the cobalt chloride solution into the cavity 28.

[0057] A water tank 11 is fixedly arranged on the top of the base 1, and a rotating ring 17 is rotatably sleeved on the outer wall of the stirring barrel 3. A spraying mechanism is arranged on the top of the rotating ring 17, and is used to spray the urea solution in the water tank 11 into the lower cavity 28. The specific structure of the spraying mechanism is: an annular pipe 29 is embedded in the rotating ring 17, and two nozzles 30 are arranged on the annular pipe 29. A first connecting pipe 19 is fixedly arranged on the top of the rotating ring 17, and the bottom end of the first connecting pipe 19 is communicated with the annular pipe 29. The top end of the first connecting pipe 19 is communicated with an air bag 21, and the top end of the air bag 21 is communicated with the water tank 11 through a second connecting pipe 22. Spray holes 31 matched with the two nozzles 30 are arranged on the outer wall of the stirring barrel 3. A first one-way valve 20 is arranged on the first connecting pipe 19, and a second one-way valve 23 is arranged on the second connecting pipe 22, which are used to control the flow direction of the urea solvent. By squeezing the air bag 21, the urea solvent in the water tank 11 can be sprayed into the lower cavity 28.

[0058] In order to stir the solvent in the cavity 28 and provide power for the spraying mechanism, a stirring mechanism is arranged. The stirring mechanism includes a second rotating shaft 9 rotatably arranged through the partition plate 27, and both ends of the second rotating shaft 9 are rotatably connected with the two end covers 8 respectively. A mounting frame 13 is fixedly arranged at the outer end of one of the end covers 8, and a second motor 14 is fixedly arranged on the mounting frame 13. The output end of the second motor 14 is fixedly connected with the second rotating shaft 9. Two groups of stirring spoons 26 are fixedly arranged on the outer wall of the second rotating shaft 9, and the two groups of stirring spoons 26 are respectively located in the two cavities 28 and become shorter in turn along with the inclination direction of the cavity 28. By starting the second motor 14, the second rotating shaft 9 can be driven to rotate, so as to drive the stirring spoons 26 to stir.

[0059] A first rotating shaft 4 is rotatably arranged through between two supporting seats 2. A first gear 7 is fixedly sleeved on the outer wall of the first rotating shaft 4, and an external tooth ring 6 meshing with the first gear 7 is fixedly sleeved on the outer wall of the stirring barrel 3. A rotating block 18 is rotatably sleeved on the outer wall of the first rotating shaft 4, and the rotating block 18 is fixedly connected with a rotating ring 17 for limiting the rotating ring 17. A first motor 5 is fixedly arranged on one side of one of the supporting seats 2, and the output end of the first motor 5 is fixedly connected with the first rotating shaft 4. By starting the first motor 5, the stirring barrel 3 can be driven to turn over, the positions of the two cavities 28 are swapped, and the rotating ring 17 will not rotate during the rotation of the stirring barrel 3.

[0060] A first sliding rod 15 is slidably arranged through on one side of the supporting seat 2, and one end of the first sliding rod 15 contacts with the outer wall of the air bag 21. A first spring 24 is sleeved on the outer wall of the first sliding rod 15, and the two ends of the first spring 24 are respectively fixedly connected with one side of the supporting seat 2 and the outer wall of the first sliding rod 15. A first fixing seat 35 is fixedly arranged on one side of the end cover 8, and a push rod 16 cooperating with the first sliding rod 15 is slidably arranged through the top of the first fixing seat 35. Extension blocks 37 are fixedly arranged on both sides of the push rod 16, and first guide rods 36 are fixedly arranged on the tops of the extension blocks 37. Both of the two first guide rods 36 are slidably arranged through the top of the first fixing seat 35. A second spring 38 is sleeved on the outer wall of the first guide rod 36, and the two ends of the second spring 38 are respectively fixedly connected with the mutually close sides of the extension block 37 and the first fixing seat 35 for driving the push rod 16 to reset and move. Cam wheels 34 cooperating with the push rod 16 are fixedly sleeved on the outer walls of both ends of the second rotating shaft 9 for pushing the push rod 16 to move upward.

[0061] Embodiment 3

[0062] Reference Figure 1 - Figure 7 On the basis of Embodiment 1, an improvement is made: in order to further enhance the stirring effect, two stirring shafts 25 are rotatably arranged through between the two end covers 8, and the two stirring shafts 25 are respectively located in the corresponding cavities 28. A second gear 32 is fixedly sleeved on the outer wall of the stirring shaft 25, and a second fixing seat 39 is fixedly arranged on one side of the end cover 8. A rack 33 meshing with the second gear 32 is slidably arranged through the top of the second fixing seat 39. The bottom end of the rack 33 is connected with the cam wheel 34 through a connecting member for driving the stirring shaft 25 to rotate reciprocally to stir the solvent in the cavity 28. The specific structure of the connecting member is: a second guide rod 40 slidably arranged through the top of the second fixing seat 39, the bottom ends of the rack 33 and the second guide rod 40 are fixedly provided with the same connecting frame 41, one side of the connecting frame 41 is fixedly provided with an extension column 42, and an annular groove 43 is formed in the outer end of the cam wheel 34, and the extension column 42 is located in the annular groove 43.

[0063] At the top of the base 1, two filter boxes 12 are fixedly arranged. Both of the two filter boxes 12 are located below the corresponding feed pipes 10 and are used to receive the solvent. A filter plate 44 for filtering the solvent is fixedly arranged in the filter box 12. Two third guide rods 45 are slidably arranged through the filter box 12. A plurality of scraping plates 46 are fixedly sleeved on the outer walls of the two third guide rods 45. The bottoms of the plurality of scraping plates 46 are all in contact with the filter plate 44. One of the scraping plates 46 is used in cooperation with the corresponding push rod 16 through a transmission member to turn the sediment on the filter plate 44. The specific structure of the transmission member is: a second sliding rod 47 slidably arranged through one side of the support base 2. One end of the second sliding rod 47 abuts against the support base 2, and the other end of the second sliding rod 47 is fixedly connected to one of the scraping plates 46. A tension spring 48 is sleeved on the outer wall of the second sliding rod 47. The two ends of the tension spring 48 are respectively fixedly connected to one side of the support base 2 and the outer wall of the second sliding rod 47. The second sliding rod 47 is used in cooperation with the corresponding push rod 16.

[0064] In this embodiment, first, the urea solution is added into the water tank 11, and the cobalt chloride solution is poured into the lower cavity 28 through the feed pipe 10, and the second motor 14 is started. The rotation of the second motor 14 can drive the rotation of the second rotating shaft 9. The rotation of the second rotating shaft 9 can drive the stirring spoon 26 to stir the liquid, and at the same time can drive the rotation of the cam 34. During the rotation of the cam 34, it can drive the connecting frame 41 to reciprocate up and down through the extension column 42 and the annular groove 43. The movement of the connecting frame 41 can drive the movement of the rack 33. The movement of the rack 33 can drive the rotation of the second gear 32. The rotation of the second gear 32 can drive the rotation of the stirring shaft 25 to stir the liquid.

[0065] During the stirring process, the convex part of the cam 34 can also push the push rod 16 on one side to move upward. The upward movement of the push rod 16 can drive the movement of the first sliding rod 15 and compress the first spring 24. During the movement of the first sliding rod 15, it can squeeze the airbag 21 through the other end. When the convex part of the cam 34 moves away from the push rod 16, the push rod 16 can reset under the action of the second spring 38, and the first sliding rod 15 can reset under the action of the first spring 24, so that one end of the first sliding rod 15 moves away from the airbag 21. During the reset process of the airbag 21, it can extract the urea solution in the water tank 11 through the second connecting pipe 22, so that the urea solution enters the airbag 21. When the first sliding rod 15 continues to squeeze the airbag 21, it can squeeze the urea solution in the airbag 21 into the nozzle 30 and drip it into the cavity 28 through the spray holes 31, and continue to stir at the same time.

[0066] After the stirring is completed, start the first motor 5 to drive the first rotating shaft 4 to rotate. The rotation of the first rotating shaft 4 can drive the first gear 7 to rotate. During the rotation of the first gear 7, the stirring barrel 3 can be driven to turn over through the external tooth ring 6, swapping the positions of the two cavities 28. At this time, the material in the upper cavity 28 will flow into the filter box 12 through the feed pipe 10 for filtration. The precipitates filtered out will accumulate on the filter plate 44;

[0067] At the same time, continue to add cobalt chloride solution and urea solution to the lower cavity 28 and continue to stir and mix;

[0068] During the mixing process, the corresponding push rod 16 can be driven to move downward by the cam 34 on the other side. The downward movement of the push rod 16 can drive the second sliding rod 47 to move. The movement of the second sliding rod 47 can drive a plurality of scraping plates 46 to move. When the push rod 16 moves upward, the second sliding rod 47 can be reset under the action of the tension spring 48 and drive a plurality of scraping plates 46 to be reset to turn over the precipitates. Finally, the precipitates are taken out for subsequent processing.

[0069] However, as is well known to those skilled in the art, the working principles and wiring methods of the first motor 5 and the second motor 14 are common knowledge. They both belong to conventional means or well-known common sense, so they will not be elaborated here. Those skilled in the art can make any selection according to their needs or convenience.

[0070] The above is only a preferred specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present invention, according to the technical solution and inventive concept of the present invention, makes equivalent substitutions or changes, and should be covered by the protection scope of the present invention.

Claims

1. A preparation method of a highly dispersed platinum group noble metal-based catalyst, characterized in that, It includes the following steps: S1. Prepare a porous rod-shaped cobalt tetroxide support material, wash it with deionized water, dry it in an oven at 60 - 120 °C, and then calcine it at 300 - 500 °C for 4 - 8 h; S2. Dissolve the noble metal precursor in deionized water to form a noble metal solution, and the noble metal precursor includes chloroplatinic acid or platinum chloride; S4. Immerse the treated cobalt tetroxide support in the noble metal solution. After impregnation is completed, take out the support from the solution, filter, wash it, and then dry it at 60 - 120 °C to remove the solvent. After drying, calcine it in an inert gas atmosphere for 4 - 6 h, where the calcination temperature is 300 - 500 °C; S5. Keep the temperature at 300 - 500 °C, reduce it in a hydrogen atmosphere for 2 - 4 h, and then it is obtained; Among them, the preparation of the porous rod-shaped cobalt tetroxide support material specifically includes the following sub-steps: S11: Add the urea solution into the water tank, and pour the cobalt chloride solution into the lower part of the double-layer cavity through the feed pipe for stirring; S12: During the stirring process, pump the urea solution in the water tank into the nozzle and drip it into the cavity through the spray holes, while continuing to stir; S13: After the stirring is completed, turn over the stirring barrel to exchange the positions of the upper and lower parts of the double-layer cavity, so that the material in the upper part of the cavity flows into the filter box for filtration; S14: Continue to add the cobalt chloride solution and the urea solution under the cavity and stir and mix them; S15: During the mixing process, move the scraper back and forth to turn over the precipitate.

2. The preparation method of the highly dispersed platinum group noble metal-based catalyst according to claim 1, wherein, After step S2, the following steps are also included: S3: Add titanium dioxide and alumina into deionized water, stir and disperse them evenly to prepare a surface modification component liquid. Immerse the calcined catalyst material in the surface modification component liquid for 1 - 2 h and then take it out, filter, wash it, dry it at 60 - 120 °C for 30 - 60 min, and after drying, carry out a shaping treatment by pressing, granulating or spray drying.

3. Preparation device for highly dispersed platinum group noble metal-based catalyst, characterized in that, For implementing the preparation method of the highly dispersed platinum group noble metal-based catalyst as described in claim 1 or 2, the preparation device of the highly dispersed platinum group noble metal-based catalyst includes a base (1), on the top of the base (1), two support seats (2) are fixedly arranged, between the two support seats (2), the same stirring barrel (3) is rotatably arranged through, both ends of the stirring barrel (3) are fixedly provided with end caps (8) for sealing the stirring barrel (3), a partition plate (27) is fixedly arranged in the stirring barrel (3), the partition plate (27) divides the inside of the stirring barrel (3) into two alternately used cavities (28), and on one side of the end cap (8), a feed pipe (10) corresponding to the cavity (28) is fixedly arranged through, for the cobalt chloride solution to enter the cavity (28); A water tank (11), the water tank (11) is fixedly arranged on the top of the base (1), a rotating ring (17) is rotatably sleeved on the outer wall of the stirring barrel (3), and a spraying mechanism is arranged on the top of the rotating ring (17) for spraying the urea solution in the water tank (11) into the lower cavity (28); A stirring mechanism, arranged on the stirring barrel (3), for stirring the solvent in the cavity (28) and providing power for the spraying mechanism; Two filter boxes (12), both of the two filter boxes (12) are fixedly arranged on the top of the base (1) and are located below the corresponding feed pipes (10) for receiving solvents, and a filter plate (44) for filtering the solvents is fixedly arranged in the filter box (12); A first rotating shaft (4) is rotatably arranged through between the two support seats (2). An outer gear ring (6) meshing with the first gear (7) is fixedly sleeved on the outer wall of the first rotating shaft (4). An outer gear ring (6) is fixedly sleeved on the outer wall of the stirring barrel (3). A rotating block (18) is rotatably sleeved on the outer wall of the first rotating shaft (4). The rotating block (18) is fixedly connected to the rotating ring (17) for limiting the rotating ring (17). A first motor (5) is fixedly arranged on one side of one of the support seats (2). The output end of the first motor (5) is fixedly connected to the first rotating shaft (4).

4. The preparation device of a highly dispersed platinum group noble metal-based catalyst according to claim 3, characterized in that, The spraying mechanism includes an annular pipe (29) embedded in the rotating ring (17). Two nozzles (30) are arranged on the annular pipe (29). A first connecting pipe (19) is fixedly arranged on the top of the rotating ring (17). The bottom end of the first connecting pipe (19) is communicated with the annular pipe (29). The top end of the first connecting pipe (19) is communicated with an air bag (21). The top end of the air bag (21) is communicated with a water tank (11) through a second connecting pipe (22). Two groups of spray holes (31) matched with the two nozzles (30) are arranged on the outer wall of the stirring barrel (3).

5. The preparation device of a highly dispersed platinum group noble metal-based catalyst according to claim 4, characterized in that, A first one-way valve (20) is arranged on the first connecting pipe (19), and a second one-way valve (23) is arranged on the second connecting pipe (22) for controlling the flow direction of the urea solvent.

6. The preparation device of a highly dispersed platinum group noble metal-based catalyst according to claim 4, characterized in that, The stirring mechanism includes a second rotating shaft (9) rotatably arranged through the partition plate (27). The two ends of the second rotating shaft (9) are respectively rotatably connected to the two end covers (8). An installation frame (13) is fixedly arranged on the outer end of one of the end covers (8). A second motor (14) is fixedly arranged on the installation frame (13). The output end of the second motor (14) is fixedly connected to the second rotating shaft (9). Two groups of stirring spoons (26) are fixedly arranged on the outer wall of the second rotating shaft (9). The two groups of stirring spoons (26) are respectively located in the two cavities (28) and become shorter in turn along the inclination direction of the cavities (28).

7. The preparation device of a highly dispersed platinum group noble metal-based catalyst according to claim 6, characterized in that, One side of the support base (2) is provided with a first sliding rod (15) penetrating and sliding therein. One end of the first sliding rod (15) contacts the outer wall of the airbag (21). A first spring (24) is sleeved on the outer wall of the first sliding rod (15). Two ends of the first spring (24) are respectively fixedly connected to one side of the support base (2) and the outer wall of the first sliding rod (15). One side of the end cover (8) is fixedly provided with a first fixing base (35). A push rod (16) which is used in cooperation with the first sliding rod (15) is provided penetrating and sliding through the top of the first fixing base (35). Extension blocks (37) are fixedly provided on both sides of the push rod (16). First guide rods (36) are fixedly provided on the tops of the extension blocks (37). Both of the first guide rods (36) are provided penetrating and sliding through the top of the first fixing base (35). A second spring (38) is sleeved on the outer wall of the first guide rod (36). Two ends of the second spring (38) are respectively fixedly connected to the relatively close sides of the extension block (37) and the first fixing base (35). Cam wheels (34) which are used in cooperation with the push rod (16) are fixedly sleeved on the outer walls of both ends of the second rotating shaft (9) and are used for pushing the push rod (16) to move upward.

8. The preparation device of a highly dispersed platinum group noble metal-based catalyst according to claim 7, characterized in that, Two stirring shafts (25) are provided penetrating and rotating between the two end covers (8). The two stirring shafts (25) are respectively located in corresponding cavities (28). Second gear wheels (32) are fixedly sleeved on the outer walls of the stirring shafts (25). One side of the end cover (8) is fixedly provided with a second fixing base (39). A rack (33) which meshes with the second gear wheel (32) is provided penetrating and sliding through the top of the second fixing base (39). The bottom end of the rack (33) is connected to the cam wheel (34) through a connecting member and is used for driving the stirring shaft (25) to rotate reciprocally to stir the solvent in the cavity (28).

9. The preparation device of a highly dispersed platinum group noble metal-based catalyst according to claim 8, characterized in that, The connecting member includes a second guide rod (40) provided penetrating and sliding through the top of the second fixing base (39). The bottom ends of the rack (33) and the second guide rod (40) are fixedly provided with the same connecting frame (41). An extension column (42) is fixedly provided on one side of the connecting frame (41). An annular groove (43) is formed in the outer end of the cam wheel (34). The extension column (42) is located in the annular groove (43) and is used for driving the rack (33) to move up and down reciprocally.

10. The preparation device of a highly dispersed platinum group noble metal-based catalyst according to claim 7, wherein: Two third guide rods (45) are provided penetrating and sliding through the filter box (12). A plurality of scraping plates (46) are fixedly sleeved on the outer walls of the two third guide rods (45). The bottoms of the plurality of scraping plates (46) all contact the filter plate (44). One of the scraping plates (46) is used in cooperation with the corresponding push rod (16) through a transmission member and is used for turning over the sediment on the filter plate (44); The transmission member includes a second sliding rod (47) that penetrates and slides on one side of the support base (2). One end of the second sliding rod (47) abuts against the support base (2), and the other end of the second sliding rod (47) is fixedly connected to one of the scraping plates (46). A tension spring (48) is sleeved on the outer wall of the second sliding rod (47), and both ends of the tension spring (48) are fixedly connected to one side of the support base (2) and the outer wall of the second sliding rod (47). The second sliding rod (47) is used in cooperation with the corresponding push rod (16).

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