Method for preparing catalyst through coprecipitation method based on vermiculite as carrier

Abstract

The invention provides a method for preparing a catalyst by a coprecipitation method based on vermiculite as a carrier, which comprises the following steps: firstly, taking vermiculite and putting into a beaker, adding about 400g of pure water, stirring, standing for 5 minutes, removing surface floating objects, and repeating the operation for 3 times to basically remove impurities; carrying out suction filtration on the washed vermiculite by using suction filtration equipment, pumping out water, and putting the vermiculite into a beaker for later use; pure water is weighed and added into a beaker, ammonium molybdate is weighed and added into the beaker to be stirred and dissolved at normal temperature, and cobalt nitrate, aluminum nitrate and magnesium nitrate are sequentially added to be stirred and dissolved at normal temperature after ammonium molybdate is completely dissolved. According to the method for preparing the catalyst through the coprecipitation method based on the vermiculite as the carrier, the natural vermiculite is used as the carrier, the preparation cost of the catalyst is reduced due to the porous structure and the cheap characteristic of the natural vermiculite, the source is wide, the catalyst is environmentally friendly, the catalyst is prepared through the coprecipitation method, and technological parameters of all the steps are accurately controlled.

Description

Technical Field

[0001] This invention relates to the field of catalyst preparation, and more particularly to a method for preparing catalysts using vermiculite as a support via co-precipitation. Background Technology

[0002] By fully utilizing the porous and inexpensive properties of vermiculite, it was made the primary support for this catalyst. A metal salt solution was then prepared, and the metal salt solution was thoroughly mixed with the vermiculite support through a co-precipitation method. This resulted in a synergistic effect between the metal ions and the vermiculite support, thus preparing a novel carbon nanotube catalyst.

[0003] Vermiculite-based catalysts have been used in the preparation of carbon nanotubes. According to the patent application with publication number CN114632521A, the vermiculite support is first pretreated by acid washing with nitric acid, followed by centrifugation to obtain semi-dry vermiculite. Then, ferric nitrate, aluminum nitrate, magnesium nitrate, ammonium heptamolybdate, citric acid, and deionized water are mixed to prepare an impregnation solution. The pretreated vermiculite is impregnated with the impregnation solution in the presence of aluminum sheets. Finally, the impregnated vermiculite is calcined to obtain the vermiculite-based catalyst.

[0004] Defects and shortcomings of the background technology: While the impregnation method is simple and convenient, it also has certain drawbacks: The active components have limited dispersion and are prone to uneven distribution. The interaction between the active component and the support is relatively weak; For multi-component systems, it is difficult to control uniform distribution. The fundamental reason is that when the catalyst contains two or more active metals, different metal precursors may have different adsorption capacities and distribution behaviors on the support.

[0005] Therefore, it is necessary to provide a method for preparing catalysts using vermiculite as a support via co-precipitation to solve the above-mentioned technical problems. Summary of the Invention

[0006] This invention provides a method for preparing catalysts using vermiculite as a support via co-precipitation, which solves the problem that when preparing catalysts by impregnation, the active components have limited dispersion and are prone to unevenness, have weak interaction with the support, and the adsorption capacity and distribution behavior of different metal precursors on the support in multi-component systems are different, making it difficult to control the uniform distribution of multi-component active metals.

[0007] To solve the above-mentioned technical problems, the present invention provides a method for preparing a catalyst based on vermiculite as a support via co-precipitation, comprising the following steps: S1. First, put vermiculite into a beaker, add about 400g of pure water, stir, let stand for 5 minutes to remove floating matter on the surface. Repeat this operation 3 times to basically remove the impurities. S2. Filter the washed vermiculite using a vacuum filter to remove the water, and then put it into a beaker for later use. S13. Weigh pure water and add it to a beaker. Weigh ammonium molybdate and add it to the beaker. Stir and dissolve it at room temperature. After the ammonium molybdate is dissolved, add cobalt nitrate, aluminum nitrate and magnesium nitrate in sequence and stir and dissolve them at room temperature. S4. Add the dissolved nitrate solution to the beaker containing vermiculite and stir for 4 hours to disperse it evenly. S5. After the stirring time is over, add 25 ml of ammonia reagent dropwise into the vermiculite solution using a peristaltic pump. The dropwise addition time is 60 min, and then stir for 30 min after the addition is complete. S6. Let the vermiculite solution after adding ammonia stand overnight; S7. After standing, stir evenly and put into a crucible. Dry at 150℃ for 2-3 hours, then put into a muffle furnace and calcine at 450℃ for 120 minutes to obtain vermiculite catalyst.

[0008] Preferably, the muffle furnace in S7 includes a furnace body, a placement assembly, two movable components, and a movable door; The placement assembly is disposed inside the furnace body. The placement assembly includes two fixed rods, two movable sleeves, and a placement plate. The two fixed rods are symmetrically installed inside the furnace body. The two movable sleeves are respectively sleeved on the surfaces of the two fixed rods. The placement plate is connected between the two movable sleeves. The two movable components are respectively disposed on both sides of the furnace body; The movable door is positioned between the two movable components.

[0009] Preferably, one end of each of the two fixing rods is connected to a fixing seat.

[0010] Preferably, a handle is connected to the center of one side of the bottom of the placement plate.

[0011] Preferably, the movable component includes a fixed rod, a movable sleeve, an L-shaped fixing block, a fixing bolt, and two connecting seats. The fixed rod is connected to one side of the furnace body surface through the two connecting seats. The movable sleeve is fitted onto the surface of the fixed rod, and the L-shaped fixing block is connected to one side of the movable sleeve.

[0012] Preferably, the fixing bolt is disposed between the movable sleeve and the fixing rod.

[0013] Preferably, the two fixed rods and the two movable sleeves are used for pulling the placement plate.

[0014] Preferably, the surface of the furnace body is provided with a protective component, which includes a protective cover, two mounting blocks, two rectangular plates and four magnetic blocks. The protective cover is fitted onto the surface of the furnace body, and the two mounting blocks are respectively connected to the two ends of the protective cover.

[0015] Preferably, the two rectangular plates are respectively connected to both sides of the surface of the furnace body.

[0016] Preferably, the four magnetic blocks are respectively connected to the two mounting blocks and the two rectangular plates on opposite sides.

[0017] Compared with related technologies, the method for preparing a catalyst based on vermiculite as a carrier via co-precipitation provided by the present invention has the following beneficial effects: This invention provides a method for preparing catalysts using vermiculite as a support via co-precipitation. Natural vermiculite is used as a support, and its porous structure and low cost reduce the preparation cost of the catalyst. It is also widely available and environmentally friendly. By using the co-precipitation method and precisely controlling the process parameters of each step, the uniform dispersion of multi-metal active components on the vermiculite support is achieved, solving the problem of uneven dispersion of active components in the traditional impregnation method. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the structure of a second embodiment of a method for preparing a catalyst based on vermiculite as a carrier via co-precipitation, provided by the present invention. Figure 2 for Figure 1 The enlarged schematic diagram of part A shown below; Figure 3 for Figure 1 A three-dimensional structural diagram of the main body of the furnace shown; Figure 4 for Figure 3 The enlarged schematic diagram of section B is shown below; Figure 5 A schematic diagram of the structure of a third embodiment of a method for preparing a catalyst based on vermiculite as a carrier via co-precipitation provided by the present invention; Figure 6 for Figure 5 The enlarged schematic diagram of section C is shown.

[0019] Numbered in the diagram: 1. Main body of the furnace. 2. Placement components, 21. Fixing rod, 22. Moving sleeve, 23. Placement plate. 3. Fixed base, 4. Handle 5. Movable components; 51. Fixing rod; 52. Movable sleeve; 53. L-shaped fixing block; 54. Fixing bolt; 55. Connecting seat. 6. Movable door, 7. Protective components; 71. Protective cover; 72. Mounting block; 73. Rectangular plate; 74. Magnetic block. Detailed Implementation

[0020] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0021] First Embodiment A method for preparing a catalyst using vermiculite as a support via co-precipitation, characterized by comprising the following steps: S1. First, put vermiculite into a beaker, add about 400g of pure water, stir, let stand for 5 minutes to remove floating matter on the surface. Repeat this operation 3 times to basically remove the impurities. S2. Filter the washed vermiculite using a vacuum filter to remove the water, and then put it into a beaker for later use. S13. Weigh pure water and add it to a beaker. Weigh ammonium molybdate and add it to the beaker. Stir and dissolve it at room temperature. After the ammonium molybdate is dissolved, add cobalt nitrate, aluminum nitrate and magnesium nitrate in sequence and stir and dissolve them at room temperature. S4. Add the dissolved nitrate solution to the beaker containing vermiculite and stir for 4 hours to disperse it evenly. S5. After the stirring time is over, add 25 ml of ammonia reagent dropwise into the vermiculite solution using a peristaltic pump. The dropwise addition time is 60 min, and then stir for 30 min after the addition is complete. S6. Let the vermiculite solution after adding ammonia stand overnight; S7. After standing, stir evenly and put into a crucible. Dry at 150℃ for 2-3 hours, then put into a muffle furnace and calcine at 450℃ for 120 minutes to obtain vermiculite catalyst.

[0022] The working principle of the method for preparing a catalyst based on vermiculite as a support via co-precipitation provided by this invention is as follows: First, vermiculite undergoes multiple washing and filtration pretreatments to remove surface impurities and excess moisture, creating favorable conditions for subsequent bonding with metal salts. Then, a nitrate solution containing various active metal components is prepared through precise weighing and stirring, ensuring accurate proportions and uniform dispersion of each component. The nitrate solution is mixed with vermiculite and stirred for an extended period, allowing metal ions to fully penetrate the porous structure of the vermiculite. Ammonia is then added evenly using a peristaltic pump to adjust the pH of the system, causing a co-precipitation reaction of metal ions on and within the vermiculite, forming stable metal compounds. After drying and high-temperature calcination, moisture and volatile impurities are removed from the system, while simultaneously forming strong chemical bonds between the metal compounds and the vermiculite carrier. This ultimately results in a catalyst with a stable structure and uniformly distributed active components. The subsequent pulverization and sieving steps can be adjusted to modify the particle size of the catalyst according to the specific application scenario, improving its ease of use.

[0023] Compared with related technologies, the method for preparing a catalyst based on vermiculite as a carrier via co-precipitation provided by the present invention has the following beneficial effects: This invention provides a method for preparing catalysts using vermiculite as a support via co-precipitation. Natural vermiculite, with its porous structure and low cost, reduces the preparation cost of the catalyst. It is also widely available and environmentally friendly. The co-precipitation method, through precise control of process parameters at each step, achieves uniform dispersion of multi-metal active components on the vermiculite support. This overcomes the technical shortcomings of traditional impregnation methods, such as uneven dispersion of active components and weak interaction with the support. The strong chemical bonds formed between metal ions and the support during co-precipitation effectively prevent the migration and sintering of active components under high-temperature reaction conditions, significantly improving the thermal stability and lifespan of the catalyst. The uniformly distributed active sites allow the catalyst to fully function during the reaction, enhancing catalytic efficiency and intrinsic activity. The entire preparation process is clear, highly controllable, and requires no complex equipment or harsh reaction conditions, facilitating large-scale industrial production. It is applicable to various catalytic reaction scenarios, including carbon nanotube synthesis.

[0024] Second Embodiment Please refer to the following: Figure 1 , Figure 2 , Figure 3 and Figure 4 Based on the first embodiment of this application, which provides a method for preparing a catalyst using vermiculite as a support via co-precipitation, the second embodiment of this application proposes another method for preparing a catalyst using vermiculite as a support via co-precipitation. The second embodiment is merely a preferred embodiment of the first embodiment, and its implementation will not affect the independent implementation of the first embodiment.

[0025] Specifically, the second embodiment of this application provides a method for preparing a catalyst based on vermiculite as a carrier via co-precipitation, which differs in that the muffle furnace in S7 includes a furnace body 1, a placement component 2, two movable components 5, and a movable door 6; The placement component 2 is disposed inside the furnace body 1. The placement component 2 includes two fixed rods 21, two movable sleeves 22 and a placement plate 23. The two fixed rods 21 are symmetrically installed inside the furnace body 1. The two movable sleeves 22 are respectively sleeved on the surfaces of the two fixed rods 21. The placement plate 23 is connected between the two movable sleeves 22. The two movable components 5 are respectively disposed on both sides of the furnace body 1; The movable door 6 is positioned between the two movable components 5.

[0026] Each of the two fixing rods 21 is connected to a fixing seat 3 at one end.

[0027] A handle 4 is connected to the center of one side of the bottom of the placement plate 23.

[0028] The fixed base 3 is fixedly connected to the inner wall of the furnace body 1 to limit and fix the fixed rod 21, preventing the fixed rod 21 from shifting during use. The surface of the handle 4 is provided with anti-slip texture, which makes it easy for the operator to pull the placement plate 23 and convenient to pick up and put down the crucible.

[0029] To ensure the stability of the installation of the fixed rod 51; the movable sleeve 52 is fitted onto the surface of the fixed rod 51, and the movable sleeve 52 can slide freely along the axial direction of the fixed rod 51 and can rotate around the axis of the fixed rod 51; the L-shaped fixing block 53 is connected to one side of the movable sleeve 52, and the horizontal section of the L-shaped fixing block 53 is used to press the movable door 6.

[0030] The fixing bolt 54 is threadedly connected to the movable sleeve 52. Tightening the fixing bolt 54 will make one end of the fixing bolt 54 fit tightly against the fixing rod 51, thereby fixing the movable sleeve 52 in the designated position of the fixing rod 51.

[0031] The movable sleeve 22 slides in conjunction with the fixed rod 21, allowing the placement plate 23 to smoothly enter and exit the interior of the furnace body 1.

[0032] The movable component 5 includes a fixed rod 51, a movable sleeve 52, an L-shaped fixing block 53, a fixing bolt 54, and two connecting seats 55. The fixed rod 51 is connected to one side of the surface of the furnace body 1 through the two connecting seats 55. The movable sleeve 52 is fitted onto the surface of the fixed rod 51, and the L-shaped fixing block 53 is connected to one side of the movable sleeve 52.

[0033] The fixing bolt 54 is disposed between the movable sleeve 52 and the fixing rod 51.

[0034] The two fixed rods 21 and the two movable sleeves 23 are used for pulling the placement plate 23.

[0035] The working principle of the method for preparing a catalyst based on vermiculite as a support via co-precipitation provided by this invention is as follows: When using this muffle furnace for catalyst calcination, first loosen the fixing bolt 54 in the movable component 5, push the movable sleeve 52 to slide along the fixing rod 51, and rotate the movable sleeve 52 to move the L-shaped fixing block 53 away from the movable door 6, then open the movable door 6; grasp the handle 4 at the bottom of the placement plate 23, pull the placement plate 23, so that the movable sleeve 22 slides along the fixing rod 21, pull the placement plate 23 out of the furnace body 1, and place the ceramic crucible containing the dried material steadily on the placement plate 23; push the handle 4, and move the placement plate 23 together with the crucible... Push the furnace body 1 into the furnace and close the movable door 6; adjust the position of the movable sleeve 52 so that the horizontal section of the L-shaped fixing block 53 presses against the surface of the movable door 6, tighten the fixing bolt 54 to fix the movable sleeve 52, thereby locking the movable door 6; start the muffle furnace, set the roasting temperature to 450℃ and the roasting time to 120min, and roast the catalyst; after roasting is completed, close the muffle furnace, wait for the furnace temperature to cool to room temperature, loosen the fixing bolt 54, open the movable door 6, pull the handle 4 to pull out the placement plate 23, and take out the crucible.

[0036] Compared with related technologies, the method for preparing a catalyst based on vermiculite as a carrier via co-precipitation provided by the present invention has the following beneficial effects: This invention provides a method for preparing catalysts using vermiculite as a carrier via co-precipitation. A placement assembly 2, consisting of a fixed rod 21, a movable sleeve 22, and a placement plate 23, is installed inside a muffle furnace. With a handle 4, operators can quickly place or remove crucibles from the muffle furnace without needing to reach inside, improving operational convenience and safety. The fixed base 3 enhances the installation stability of the fixed rod 21 and ensures the smoothness of the placement plate 23 during sliding. The movable assembly 5, through the cooperation of the fixed rod 51, the movable sleeve 52, and the L-shaped fixing block 53, enables the rapid locking and opening of the movable door 6. The fixing bolt 54 firmly secures the movable sleeve 52, preventing the movable door 6 from loosening during roasting and ensuring the stability of the furnace temperature, thereby ensuring the consistency of the catalyst roasting effect. The overall muffle furnace structure is rationally designed and easy to operate, providing a stable and reliable roasting environment for catalyst preparation and further improving the quality of catalyst preparation.

[0037] Third Embodiment Please refer to the following: Figure 5 and Figure 6Based on the first embodiment of this application, which provides a method for preparing a catalyst using vermiculite as a support via coprecipitation, the third embodiment of this application proposes another method for preparing a catalyst using vermiculite as a support via coprecipitation. The third embodiment is merely a preferred embodiment of the first embodiment, and its implementation will not affect the independent implementation of the first embodiment.

[0038] Specifically, the third embodiment of this application provides a method for preparing a catalyst based on vermiculite as a carrier via co-precipitation, which differs in that it further includes a protective component 7. The protective component 7 is disposed on the surface of the furnace body 1. The protective component 7 includes a protective cover 71, two mounting blocks 72, two rectangular plates 73, and four magnetic blocks 74. The protective cover 71 is fitted onto the surface of the furnace body 1, and the two mounting blocks 72 are respectively connected to the two ends of the protective cover 71.

[0039] The two rectangular plates 73 are respectively connected to both sides of the surface of the furnace body 1.

[0040] The four magnetic blocks 74 are respectively connected to the two mounting blocks 72 and the two rectangular plates 73 on opposite sides.

[0041] The magnetic block 74 on the mounting block 72 and the magnetic block 74 on the rectangular plate 73 are attracted to each other by opposite polarities, and the protective cover 71 is quickly connected and fixed to the furnace body 1 through the magnetic attraction force.

[0042] The protective cover 71 is made of high-temperature resistant heat insulation material, which can effectively block the heat from the surface of the furnace body 1 from dissipating outward, preventing operators from accidentally touching and getting burned. At the same time, it can also reduce heat loss inside the furnace and save energy. The mounting block 72 and the protective cover 71 are integrally formed, and the structure is stable.

[0043] The rectangular plate 73 is fixedly connected to the furnace body 1 by bolts, which makes the connection firm and easy to disassemble.

[0044] The working principle of the method for preparing a catalyst based on vermiculite as a support via co-precipitation provided by this invention is as follows: Before using the muffle furnace for catalyst roasting, the protective cover 71 is fitted onto the surface of the furnace body 1, aligning the magnetic blocks 74 on the mounting blocks 72 at both ends of the protective cover 71 with the magnetic blocks 74 on the rectangular plates 73 on both sides of the furnace body 1. The magnetic force between the magnetic blocks 74 securely fixes the protective cover 71 to the furnace body 1. At this time, the protective cover 71 can block the high temperature generated on the surface of the furnace body 1 during heating, preventing accidental burns to operators. When maintenance or repair of the muffle furnace is required, simply pull the protective cover 71 to separate the magnetic blocks 74 on the mounting blocks 72 from the magnetic blocks 74 on the rectangular plates 73, and the protective cover 71 can be removed from the furnace body 1. The operation is convenient.

[0045] Compared with related technologies, the method for preparing a catalyst based on vermiculite as a carrier via co-precipitation provided by the present invention has the following beneficial effects: This invention provides a method for preparing a catalyst using vermiculite as a carrier via co-precipitation. By incorporating a protective component 7, the protective cover 71, made of high-temperature resistant insulating material, effectively blocks the high temperatures on the surface of the muffle furnace during operation, providing excellent protection and ensuring the safety of operators. Simultaneously, the protective cover 71 reduces heat loss within the furnace, improving energy efficiency and ensuring temperature stability during roasting. The coordinated design of the mounting block 72, rectangular plate 73, and magnetic block 74 enables rapid assembly and disassembly of the protective cover 71 from the furnace body 1 without the need for additional tools. This simple and convenient operation does not affect the normal use of the muffle furnace and facilitates subsequent maintenance and repair.

[0046] The above description is merely an embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural or procedural transformations made based on the content of the present invention specification and drawings, or direct or indirect applications in other related technical fields, are similarly included within the patent protection scope of the present invention.

Claims

1. A method for preparing a catalyst using vermiculite as a carrier via co-precipitation, characterized in that, Includes the following steps: S1. First, put vermiculite into a beaker, add about 400g of pure water, stir, let stand for 5 minutes to remove floating matter on the surface. Repeat this operation 3 times to basically remove the impurities. S2. Filter the washed vermiculite using a vacuum filter to remove the water, and then put it into a beaker for later use. S13. Weigh pure water and add it to a beaker. Weigh ammonium molybdate and add it to the beaker. Stir and dissolve the ammonium molybdate at room temperature. After the ammonium molybdate is dissolved, add cobalt nitrate, aluminum nitrate and magnesium nitrate in sequence and stir and dissolve them at room temperature. S4. Add the dissolved nitrate solution to the beaker containing vermiculite and stir for 4 hours to disperse it evenly. S5. After the stirring time is over, add 25 ml of ammonia reagent dropwise to the vermiculite solution using a peristaltic pump. The dropwise addition time is 60 min, and then stir for 30 min after the addition is complete. S6. Let the vermiculite solution after adding ammonia stand overnight; S7. After standing, stir evenly and put into a crucible. Dry at 150℃ for 2-3 hours, then put into a muffle furnace and calcine at 450℃ for 120 minutes to obtain vermiculite catalyst.

2. The method for preparing a catalyst based on vermiculite as a carrier via co-precipitation according to claim 1, characterized in that, The muffle furnace in S7 includes a furnace body, a placement assembly, two movable components, and a movable door; The placement assembly is disposed inside the furnace body. The placement assembly includes two fixed rods, two movable sleeves, and a placement plate. The two fixed rods are symmetrically installed inside the furnace body. The two movable sleeves are respectively sleeved on the surfaces of the two fixed rods. The placement plate is connected between the two movable sleeves. The two movable components are respectively disposed on both sides of the furnace body; The movable door is positioned between the two movable components.

3. The method for preparing a catalyst based on vermiculite as a carrier via co-precipitation according to claim 2, characterized in that, Each of the two fixing rods has a fixing seat connected to one end.

4. The method for preparing a catalyst based on vermiculite as a carrier via co-precipitation according to claim 2, characterized in that, A handle is attached to the center of one side of the bottom of the placement plate.

5. The method for preparing a catalyst based on vermiculite as a carrier via co-precipitation according to claim 2, characterized in that, The movable component includes a fixed rod, a movable sleeve, an L-shaped fixing block, a fixing bolt, and two connecting seats. The fixed rod is connected to one side of the furnace body surface through the two connecting seats. The movable sleeve is fitted onto the surface of the fixed rod, and the L-shaped fixing block is connected to one side of the movable sleeve.

6. The method for preparing a catalyst based on vermiculite as a carrier via co-precipitation according to claim 5, characterized in that, The fixing bolt is positioned between the movable sleeve and the fixing rod.

7. The method for preparing a catalyst based on vermiculite as a carrier via co-precipitation according to claim 2, characterized in that, The two fixed rods and the two movable sleeves are used for pulling the placement plate.

8. The method for preparing a catalyst based on vermiculite as a carrier via co-precipitation according to claim 1, characterized in that, The surface of the furnace body is provided with a protective component, which includes a protective cover, two mounting blocks, two rectangular plates and four magnetic blocks. The protective cover is fitted onto the surface of the furnace body, and the two mounting blocks are respectively connected to the two ends of the protective cover.

9. The method for preparing a catalyst based on vermiculite as a carrier via co-precipitation according to claim 8, characterized in that, The two rectangular plates are respectively connected to both sides of the surface of the furnace body.

10. The method for preparing a catalyst based on vermiculite as a carrier via co-precipitation according to claim 8, characterized in that, The four magnetic blocks are respectively connected to the two mounting blocks and the two rectangular plates on opposite sides.

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