Equipment and process for preparing a propane oxidation catalyst
By designing the pitch adjustment component and purification mechanism, the problem of low water removal efficiency in the hydrothermal treatment during catalyst preparation was solved, realizing efficient catalyst production and controllable drainage of the solution reaction, thereby improving the preparation efficiency of propane oxidation catalyst.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- ANHUI UNIV OF SCI & TECH
- Filing Date
- 2023-10-07
- Publication Date
- 2026-05-26
AI Technical Summary
In the preparation of propane oxidation catalyst, the water removal efficiency of the catalyst is low during hydrothermal treatment, which leads to the catalyst precipitate being discharged with the water, resulting in waste and low reaction efficiency.
A preparation device comprising a support column, a transmission belt, a motor, a differential mechanism, a stirring mechanism, a stirring drum, a reaction drum, and a purification mechanism was designed. Through the cooperation of the distance adjustment component and the purification mechanism, the distance between the stirring drum and the reaction drum and the depth of the puncture rod can be adjusted, thereby precisely controlling the drainage rate and solution distribution.
It improves the production efficiency of the catalyst, ensures the integrity of the catalyst, reduces waste, and achieves controllability of solution reaction and efficient drainage.
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Figure CN117258589B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of propane oxidation catalyst preparation technology, specifically to a propane oxidation catalyst preparation apparatus and preparation process. Background Technology
[0002] Propylene oxide is the third largest derivative of propylene in the propylene industry, after polypropylene and acrylonitrile. As an important basic organic chemical synthesis raw material, propylene oxide is mainly used to produce various surfactants, flame retardants, and emulsifiers. At present, the main industrial production methods of propylene oxide are the chlorohydrin method, the co-oxidation method, and the direct oxidation method. In the preparation process, the active components of the catalyst and the support material are fully mixed by mixing equipment to ensure uniform dispersion.
[0003] In the propane oxidation process, since the reaction is exothermic, heat is released when propane reacts with oxygen. This exothermic effect can increase the reaction rate because the released heat lowers the activation energy and accelerates the reaction. However, exothermic reactions require precise temperature control to avoid overheating and side reactions. Furthermore, hydrothermal treatment during preparation can adjust the crystal structure and porosity of the catalyst, thereby optimizing its catalytic activity. The water removal step, on the other hand, needs to ensure that the catalyst is free of excess water to avoid unnecessary competitive reactions. During the drainage process, due to the presence of precipitated solid particles, some catalyst is discharged with the water, resulting in significant waste.
[0004] To address these issues and improve the production efficiency of propane oxidation catalysts, this invention provides a propane oxidation catalyst preparation apparatus and process to solve the aforementioned problems. Summary of the Invention
[0005] The technical problem to be solved by the present invention is that in order to optimize its catalytic activity during the hydrothermal treatment of the preparation process, it is necessary to ensure that there is no excess water in the catalyst during the water removal step. However, during the drainage process, due to the presence of precipitated solid particles, the reaction precipitate of the catalyst will be discharged along with the water, resulting in low drainage efficiency and significant waste.
[0006] To solve the aforementioned technical problem, the present invention adopts the following technical solution: A propane oxidation catalyst preparation device is provided, comprising a support column, a transmission belt, a motor, a differential speed mechanism, a stirring mechanism, a stirring cylinder, a reaction cylinder, and a purification mechanism; a motor is installed at one end of the support column, and the motor drives the differential speed assembly via the transmission belt; the stirring mechanism is installed at the lower end of the differential speed assembly, and the stirring cylinder and the reaction cylinder are placed vertically in mirror image; the purification mechanism is installed between the stirring cylinder and the reaction cylinder, and during the process of adjusting the distance between the stirring cylinder and the reaction cylinder, the purification mechanism inserts a piercing rod into the non-precipitated layer, and changes the drainage rate according to the different piercing depths.
[0007] A motor is mounted on one end of the support column, and the motor is connected to the differential mechanism via a transmission belt to achieve energy transfer. The stirring mechanism is installed at the bottom of the differential mechanism, allowing the stirring tank and the reaction tank to be placed in a vertical mirror arrangement. The purification mechanism is placed between the stirring tank and the reaction tank, and drains water according to the reaction steps while adjusting the distance between the stirring tank and the reaction tank. During this adjustment process, the function of the purification mechanism is to insert the puncture rod into the non-precipitated layer, and adjust the drainage speed according to the change in puncture depth to achieve the best drainage effect.
[0008] The purification mechanism includes a distance adjustment component, a support frame, and a puncture component. The distance adjustment component is slidably connected to the side wall of the support column, and one end of the distance adjustment component is fixedly connected to the support frame. The support frame is configured as two vertically placed components, which are respectively fixedly connected to the lower bottom surface of the stirring tank and the upper bottom surface of the reaction tank. The puncture component is fixedly connected inside the support frame. During the process of the distance adjustment component adjusting the support frame, the vertical position of the puncture component is changed, thereby placing the outlet of the puncture rod in the non-precipitation layer and adjusting the reaction rate.
[0009] Two support frames are provided, the main purpose of which is to fix the support frames to the bottom surface of the stirring tank respectively to provide support. The other support frame is fixedly connected to the reaction tank, thereby driving the reaction tank. By adjusting the position of the meshing gear, the position of the reaction tank and the stirring tank can be changed, so that the purification mechanism can work synchronously. At the same time, the purpose of vertical placement is to place the stirring tank and the reaction tank coaxially, so that the puncture hole can be accurately aligned with the puncture rod, and the puncture rod can accurately pass through the puncture hole during the movement.
[0010] The pitch adjustment assembly includes a sliding ring, a rack, a meshing gear, a rotating shaft, and a rotating handle. The sliding ring is slidably connected to the side wall of the support column, the rack is fixedly connected to the side wall of the support column, one end of the rotating shaft is fixedly connected to the meshing gear, the sliding ring is provided with a sliding groove, the rack passes through the sliding groove vertically, and the pitch adjustment assembly adjusts the solution content in the stirring drum by twisting the rotating handle, so that the meshing gear slides and meshes on the surface of the rack.
[0011] The rotating handle drives the rotating shaft to rotate. Since one end of the rotating shaft is fixedly connected to a meshing gear, the meshing gear continuously engages with the rack during the movement, thereby adjusting the distance between the stirring tank and the reaction tank. This allows the adjustment component to change the position of the stirring tank simply by rotating the rotating handle. Furthermore, due to its own friction and the number of teeth of the meshing gear, after the rotation adjustment, the friction can naturally stabilize on the rack, and the stirring tank will naturally descend due to gravity.
[0012] The puncture assembly includes a puncture rod and a water-blocking baffle; the puncture rod is fixedly connected to the surface of the lower plate, the lower plate and the support plate are coaxial, the lower plate has a centrally recessed structure, the puncture rod has a hollow structure and multiple layers of water-blocking baffles are provided on the surface, so that the drainage between different layers of water-blocking baffles will not affect each other during the reaction process.
[0013] The puncture rod enters the upper plate through puncture. Since the lower plate is designed with a central concave structure, when the air vent of the lower plate is opened, the solution in the stirring tank enters the interior of the puncture rod through the drain port. Due to the multiple drain ports, when some solution enters the flexible plate from the drain port, that is, when it enters between the upper and lower plates, the liquid will collect at the axis due to the central concave structure. Since a water inlet is provided, the solution can enter the reaction tank through the water inlet after collecting in the central concave structure, thereby preventing solution accumulation.
[0014] Furthermore, the multiple layers of water-blocking baffles serve a crucial purpose. Since multiple drainage ports are located at different layers, when the puncture rod pierces the "+" shaped incision, the solution, due to its varying diameter, would essentially flow through the incision during puncture without these multiple water-blocking baffles. This would lead to solution accumulation between the mixing tank and the reaction vessel, rendering the drainage from the drainage ports largely ineffective and negating the purpose of draining the non-precipitation layer. The multiple layers of water-blocking baffles, combined with the incision and the flexible rubber properties of the baffles, allow the structure to conform to the puncture hole. When the pores are not open, the drainage ports are closed, ensuring the solution's airtightness. Simultaneously, since the puncture hole is normally closed, a seal is maintained when the puncture rod is not piercing.
[0015] Drainage ports are provided between the water-blocking baffles. Multiple drainage ports are arranged in a ring array around the side wall of the puncture rod, so that drainage can be carried out at different rates under the layered restriction of the water-blocking baffles, making the solution reaction process of propane oxidation catalyst controllable.
[0016] Multiple drain ports are arranged in a ring array on the piercing rod. Combined with the water-blocking baffle, this ensures normal drainage. Due to pressure control, when the air port is closed, the pressure inside the reaction cylinder is stable, preventing the solution from entering. When the air port is open, gravity prevents the piercing rod from draining when passing through the sediment layer. However, when the drain port passes through the sediment layer, drainage is achieved, discharging the solution and leaving the sediment at the bottom of the stirring cylinder.
[0017] The surface of the upper plate is provided with multiple puncture holes, each containing a cross-shaped incision. This allows the cone-shaped structure to puncture the upper plate through the incision, achieving water-resistant puncture and ensuring drainage stability in conjunction with the water-blocking baffle. The upper end of the puncture rod is also cone-shaped, with its lower surface fitting against the water-blocking baffle. The cone-shaped puncture head ensures water-blocking during puncture of the upper plate. The cone-shaped structure allows the puncture rod to advance layer by layer during puncture, and the cross-shaped incision further ensures the sealing of the solution.
[0018] A vent is provided on one side of the reaction cylinder. By controlling the opening and closing of the vent, the solution inside the stirring cylinder can be discharged through the drain port. This allows for adjustable drainage and purification of the solution inside the stirring cylinder. When the vent is closed, the reaction cylinder is a closed space. Therefore, when the drain port is opened, the solution will not drop due to the pressure. When drainage is required, i.e., when the drain port of the puncture rod is located in a non-precipitation layer, the vent can be released to provide a channel for gas discharge, thereby achieving drainage.
[0019] A flexible plate is fixedly connected between the lower plate and the upper plate. The maximum extension length of the flexible plate is the same as the length of the rack, so that the water overflowing from the drain port can be sealed during the adjustment of the pitch component to meet the purification requirements. The surface of the lower plate is provided with multiple water inlets, so that the water overflowing from the drain port can enter the reaction cylinder through the water inlets. And the lengths are the same, so that when the pitch component is at its maximum length, the sealing between the two can be maintained, and compression and extension can be achieved.
[0020] A process for preparing a propane oxidation catalyst includes the following steps:
[0021] S1: Material preparation: Prepare a certain amount of AgNO3 and NaH2PO4, as well as deionized water, and seal the gas port of the preparation equipment;
[0022] S2: Then, the prepared AgNO3 and NaH2PO4 are dissolved in a stirring tank filled with deionized water at a molar ratio of 1:1. The stirring mechanism is powered by a motor to stir the solution. At this time, the distance of the adjusting component in the purification mechanism is set to the maximum, the extension length of the flexible plate is also the longest, and the puncture rod does not penetrate the lower plate; thus, the precursor solution of AgPO4 is obtained.
[0023] S3: At room temperature, deionized water containing sodium ethylenediaminetetraacetate was added to the AgPO4 precursor solution and stirred evenly with a stirring mechanism to obtain a white precipitate, thus obtaining the AgPO4 precursor solid.
[0024] S4: Next, by inserting a piercing rod into different depths of the stirring tube, the solution inside the stirring tube is increased or decreased. The precipitate is subjected to hydrothermal treatment under different temperature and time conditions to obtain AgPO4 crystals with different morphologies. The crystal growth and crystal face exposure of AgPO4 are controlled by the hydrothermal method.
[0025] S5: Finally, the precipitate is washed with ethanol at 80°C. Since the crystal growth of AgPO4 has ended, the precipitate and solution are separated at this time. The precipitate is located at the bottom of the stirred tank and the water is discharged through the purification mechanism. Then the puncture rod is removed from the stirred tank, the puncture hole is closed, and the precipitate is retained in the stirred tank. It is dried at 60°C for 12 hours to obtain the AgPO4 catalyst.
[0026] The beneficial effects of this invention are as follows:
[0027] 1. This invention, by designing a pitch-adjustable component that can be subjectively adjusted according to the production process, synchronizes the drainage process with the reaction catalysis process, thereby improving the reaction efficiency. At the same time, different solutions can be added according to the reaction time, which greatly improves the production efficiency.
[0028] 2. This invention designs an insertion-type purification mechanism, which uses multiple layers of puncture components combined with a distance adjustment component to adjust the distance between the stirring tank and the reaction tank, while simultaneously changing the insertion depth of the puncture components into the stirring tank, thereby enabling the drain port to drain non-precipitated water within the stirring tank.
[0029] 3. This invention achieves layered water isolation by designing a water-blocking baffle and puncture holes, and isolates water through the puncture head and the "+" opening, and seals the reaction cylinder through the air vent, thereby ensuring that the cavity can be maintained by pressure when purification is not required. Attached Figure Description
[0030] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the accompanying drawings used in the description of the specific embodiments or the prior art will be briefly introduced below.
[0031] Figure 1 This is an overall schematic diagram of the present invention;
[0032] Figure 2 This is a schematic diagram of the differential mechanism of the present invention.
[0033] Figure 3 This is a schematic diagram of the distance adjustment component of the present invention;
[0034] Figure 4 This is a schematic diagram of the puncture assembly of the present invention;
[0035] Figure 5 This is a partially enlarged view A of the puncture assembly of the present invention;
[0036] Figure 6 This is a schematic diagram of the puncture rod of the present invention;
[0037] Figure 7 This is a schematic diagram of the arrangement of the puncture rod of the present invention;
[0038] Figure 8 This is a schematic diagram of the support frame of the present invention;
[0039] Figure 9 This is a schematic diagram of the upper plate cutout of the present invention;
[0040] Figure 10 This is a schematic diagram of the solution flow of the present invention;
[0041] Figure 11 This is a schematic diagram illustrating the structural working principle of the present invention;
[0042] Figure 12 This is a process flow diagram of the present invention.
[0043] In the diagram: 1. Support column; 2. Transmission belt; 3. Motor; 4. Differential mechanism; 5. Stirring mechanism; 6. Stirring drum; 61. Upper plate; 62. Flexible plate; 7. Reaction drum; 71. Lower plate; 72. Air inlet; 73. Water inlet; 8. Purification mechanism; 81. Adjustment assembly; 811. Sliding ring; 812. Rack; 813. Meshing gear; 814. Rotating shaft; 815. Rotating handle; 816. Sliding groove; 82. Support frame; 83. Puncture assembly; 831. Puncture rod; 832. Water-blocking baffle; 833. Drain; 834. Puncture head; 835. Puncture hole. Detailed Implementation
[0044] The specific embodiments of the present invention will be further described below with reference to the accompanying drawings. It should be noted that these descriptions are for the purpose of aiding understanding the present invention and do not constitute a limitation thereof. Furthermore, the technical features involved in the various embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.
[0045] like Figure 1 and Figure 2 As shown, a propane oxidation catalyst preparation device includes a support column 1, a transmission belt 2, a motor 3, a differential speed mechanism 4, a stirring mechanism 5, a stirring cylinder 6, a reaction cylinder 7, and a purification mechanism 8. A motor 3 is installed at one end of the support column 1, and the motor 3 drives the differential speed assembly via the transmission belt 2. The stirring mechanism 5 is installed at the lower end of the differential speed assembly, and the stirring cylinder 6 and the reaction cylinder 7 are placed vertically in a mirror image. The purification mechanism 8 is installed between the stirring cylinder 6 and the reaction cylinder 7. During the process of adjusting the distance between the stirring cylinder 6 and the reaction cylinder 7, the purification mechanism 8 inserts a piercing rod 831 into the non-precipitated layer, and changes the drainage purification speed according to the different piercing depths.
[0046] A motor 3 is mounted on one end of the support column 1, and the motor 3 is connected to the differential mechanism 4 via a transmission belt 2, thereby realizing energy transfer. The stirring mechanism 5 is installed at the bottom of the differential mechanism 4, so that the stirring tank 6 and the reaction tank 7 can be placed in a vertical mirror arrangement; the purification mechanism 8 is placed between the stirring tank 6 and the reaction tank 7, and drains water according to the reaction steps while adjusting the distance between the stirring tank 6 and the reaction tank 7; in this adjustment process, the function of the purification mechanism 8 is to insert the puncture rod 831 into the non-precipitated layer, and adjust the drainage speed according to the change of puncture depth to achieve the best drainage effect.
[0047] like Figure 4 As shown, the purification mechanism 8 includes an adjustment component 81, a support frame 82, and a puncture component 83. The adjustment component 81 is slidably connected to the side wall of the support column 1, and one end of the adjustment component 81 is fixedly connected to the support frame 82. The support frame 82 is configured as two vertically placed components that are fixedly connected to the lower bottom surface of the stirring tank 6 and the upper bottom surface of the reaction tank 7, respectively. The puncture component 83 is fixedly connected inside the support frame 82. During the process of the adjustment component 81 adjusting the support frame 82, the vertical position of the puncture component 83 is changed, thereby placing the outlet 833 of the puncture rod 831 in the non-precipitate layer and adjusting the reaction rate.
[0048] Two support frames 82 are provided. The main purpose is to fix the support frames 82 to the bottom surface of the stirring tank 6 respectively to provide support. The other support frame 82 is fixedly connected to the reaction tank 7, thereby driving the reaction tank 7. The position of the reaction tank 7 and the stirring tank 6 can be changed by adjusting the position of the meshing gear 813, so that the purification mechanism 8 can work synchronously. At the same time, the purpose of vertical placement is to place the stirring tank 6 and the reaction tank 7 coaxially, so that the puncture hole 835 can be accurately aligned with the puncture rod 831, so that the puncture rod 831 can accurately pass through the puncture hole 835 during the movement.
[0049] like Figure 3 As shown, the adjusting component 81 is slidably connected to the side wall of the support column 1, and one end is fixedly connected to the support frame 82. There are two support frames 82, one connected to the lower bottom surface of the stirring tank 6 and the other connected to the upper bottom surface of the reaction tank 7; the purpose is to achieve synchronous movement of the two through the fixed connection of the support frame 82. The puncture component 83 is fixed inside the support frame 82, and the vertical position of the puncture component 83 will change accordingly when the adjusting component 81 adjusts the position of the support frame 82. This allows the drain port 833 of the puncture rod 831 to be accurately positioned on the non-precipitated layer, thereby adjusting the reaction rate; one is connected to the lower bottom surface of the stirring tank 6, providing support for the stirring tank 6; the other is connected to the reaction tank 7, driving the movement of the reaction tank 7. By adjusting the position of the meshing gear 813, the position change between the reaction tank 7 and the stirring tank 6 can be realized, thereby enabling the purification mechanism 8 to operate synchronously. The vertical placement of the support frame 82 is intended to place the stirring tank 6 and the reaction tank 7 coaxially, ensuring precise alignment between the puncture hole 835 and the puncture rod 831. This allows the puncture rod 831 to accurately pass through the puncture hole 835 during movement, achieving the required function.
[0050] The pitch adjustment assembly 81 includes a sliding ring 811, a rack 812, a meshing gear 813, a rotating shaft 814, and a rotating handle 815. The sliding ring 811 is slidably connected to the side wall of the support column 1, the rack 812 is fixedly connected to the side wall of the support column 1, one end of the rotating shaft 814 is fixedly connected to the meshing gear 813, the sliding ring 811 is provided with a sliding groove 816, the rack 812 passes vertically through the sliding groove 816, and the pitch adjustment assembly 81, by twisting the rotating handle 815, causes the meshing gear 813 to slide and mesh on the surface of the rack 812, thereby adjusting the solution content in the stirring drum 6 during the stirring process.
[0051] The rotating handle 815 drives the rotating shaft 814 to rotate. Since one end of the rotating shaft 814 is fixedly connected to the meshing gear 813, the meshing gear 813 continuously engages with the rack 812 during the movement, thereby realizing the distance adjustment between the stirring tank 6 and the reaction tank 7. This allows the distance adjustment component 81 to change the position of the stirring tank 6 simply by rotating the rotating handle 815. Furthermore, due to its own friction and the number of teeth of the meshing gear 813, after the rotation adjustment, the friction can naturally stabilize it on the rack 812.
[0052] like Figure 8As shown, the sliding ring 811 is slidably connected to the side wall of the support column 1, and the rack 812, parallel to it, is also fixedly connected to the side wall of the support column 1. One end of the rotating shaft 814 is fixedly connected to the meshing gear 813, and the sliding ring 811 has a sliding groove 816, allowing the rack 812 to pass vertically through it. By twisting the rotating handle 815, the pitch adjustment assembly 81 realizes the process of the meshing gear 813 slidingly engaging with the surface of the rack 812. The rotation of the rotating handle 815 drives the movement of the rotating shaft 814. Because one end of the rotating shaft 814 is connected to the meshing gear 813, the meshing gear 813 will always remain engaged with the rack 812 during the movement. This allows the distance between the stirring tank 6 and the reaction tank 7 to be continuously adjusted, so that the pitch adjustment assembly 81 can change the position of the stirring tank 6 simply by rotating the rotating handle 815. Furthermore, due to the friction of the adjusting component 81 itself and the number of teeth of the meshing gear 813, once the rotation adjustment is completed, the friction will naturally stabilize on the rack 812.
[0053] like Figure 6 As shown, the puncture assembly 83 includes a puncture rod 831 and a water-blocking baffle 832; the puncture rod 831 is fixedly connected to the surface of the lower plate 71, the lower plate 71 and the support plate are coaxial, the lower plate 71 has a centrally recessed structure, the puncture rod 831 has a hollow structure and the surface is provided with multiple layers of water-blocking baffles 832, so that the drainage between different layers of water-blocking baffles 832 will not affect each other during the reaction process.
[0054] like Figure 5 As shown, the puncture rod 831 penetrates the upper plate 61 through puncture. Since the lower plate 71 is designed with a central concave structure, when the air port 72 is opened, the solution in the stirring tank 6 enters the interior of the puncture rod 831 through the drain port 833. Due to the multiple drain ports 833, when some solution enters the flexible plate 62 from the drain port 833, that is, when it enters between the upper plate 61 and the lower plate 71, the liquid will collect at the axis due to the central concave structure. Since a water inlet 73 is provided, the solution can enter the reaction tank 7 through the water inlet 73 after collecting in the central concave structure, thereby preventing solution accumulation.
[0055] like Figure 9As shown, the main purpose of the multi-layered water-blocking baffles 832 is that, since there are multiple drain ports 833 at different layers, when the piercing rod 831 pierces the "+" shaped cut, due to the different diameters, without the multi-layered water-blocking baffles 832, the solution would basically fall through the cut during piercing, causing solution accumulation between the stirring tank and the reaction tank 7. The drainage of the drain ports 833 would be of little significance and would lose the purpose of drainage of the non-sedimentation layer. However, the multi-layered water-blocking baffles 832, combined with the cut, and their own soft rubber properties, allow the structure to fit the piercing hole 835. When the pores are not open, the drain ports 833 can be closed, thereby ensuring the sealing of the solution. At the same time, since the piercing hole 835 is normally closed, it can ensure a seal when the piercing rod 831 is not piercing.
[0056] like Figure 7 As shown, the piercing rod 831 is connected to the surface of the lower plate 71, which is coaxial with the support plate. Its central recessed structure is a key feature. The piercing rod 831 has a hollow structure, and its surface is equipped with multiple layers of water-blocking baffles 832. This structure ensures that drainage between different layers of water-blocking baffles 832 does not interfere with each other during the reaction. The piercing rod 831 penetrates the upper plate 61, and the central recessed structure of the lower plate 71 allows the solution in the stirring tank 6 to flow into the interior of the piercing rod 831 through the drain port 833 when the gas port 72 is opened. The presence of multiple drain ports 833 allows some solution to enter the flexible plate 62, i.e., into the space between the upper plate 61 and the lower plate 71. Due to the central recessed structure, the liquid accumulates at the axis and then enters the reaction tank 7 through the water inlet 73, thus achieving effective solution accumulation without affecting normal drainage.
[0057] Furthermore, the multi-layer water-blocking baffle 832 plays a crucial role. When the puncture rod 831 forms a cross-shaped incision, due to the different incision diameters, without the multi-layer water-blocking baffle 832, the solution would primarily fall through the incision during puncture. This would cause the solution to accumulate between the stirring tank 6 and the reaction tank 7, rendering the drain port 833 ineffective for drainage and preventing drainage of the non-precipitated layer. The presence of the multi-layer water-blocking baffle 832, combined with the incision and the properties of soft rubber, allows the structure to conform to the puncture hole 835, effectively closing the drain port 833, especially when the vent is not open, ensuring the solution's airtightness. Moreover, the puncture hole 835 is normally in a closed state, thus maintaining airtightness in the non-puncture state.
[0058] The surface of the upper plate 61 is provided with multiple puncture holes 835, each containing a cross-shaped cut, allowing the cone-shaped structure to be punctured through the cut for water-resistant penetration. This, combined with the water-blocking baffle 832, ensures stable drainage. The upper end of the puncture rod 831 is a cone-shaped structure, and its lower surface is in contact with the water-blocking baffle 832. The cone-shaped puncture head 834 ensures water-blocking during the puncture of the upper plate 61. The cone-shaped structure allows the puncture rod 831 to advance layer by layer during puncture, and the cross-shaped cut ensures the sealing of the solution.
[0059] Drainage ports 833 are provided between the water-blocking baffles 832. Multiple drainage ports 833 are arranged in a ring array around the side wall of the piercing rod 831. Under the layered restriction of the water-blocking baffles 832, drainage is carried out at different rates, making the solution reaction process of propane oxidation catalyst controllable. The multiple drainage ports 833 arranged in a ring array on the piercing rod 831, combined with the water-blocking baffles 832, can ensure normal drainage. Due to pressure control, when the gas port 72 is closed, the pressure inside the reaction cylinder 7 is stable, and the solution cannot enter. When the gas port 72 is open, due to natural gravity, the piercing rod 831 does not drain when passing through the sedimentation layer. When the drainage port 833 passes through the sedimentation layer, drainage is achieved, and the solution is discharged, leaving the sediment at the bottom of the stirring cylinder 6.
[0060] A vent 72 is provided on one side of the reaction cylinder 7. By controlling the opening and closing of the vent 72, the solution inside the stirring cylinder 6 can be discharged through the drain port 833. When the vent 72 is closed, the reaction cylinder 7 is a closed space. Therefore, when the solution enters through the drain port 833, the pressure will prevent the solution from dropping. When drainage is required, i.e., when the drain port 833 of the piercing rod 831 is located in a non-precipitation layer, the vent 72 can be released to provide a channel for gas discharge, thereby achieving drainage.
[0061] A flexible plate 62 is fixedly connected between the lower plate 71 and the upper plate 61. The maximum extension length of the flexible plate 62 is the same as the length of the rack 812. The surface of the lower plate 71 is provided with multiple water inlets 73, so that the water overflowing from the drain port 833 enters the reaction cylinder 7 through the water inlets 73. The inlets 73 are also provided with the same length, so that when the adjustable component 81 is at its maximum length, the sealing between the two can be maintained, and compression and extension can be achieved.
[0062] The process is as follows Figure 10 , Figure 11 and Figure 12As shown, during operation, the vent 72 is in a closed state. Under different reaction steps, the distance between the stirring tank 6 and the reaction tank 7 is changed by rotating the pitch adjustment component 81, and the solution enters the stirring tank 6 through the piercing component 83. Since the vent 72 is sealed, the solution in the non-precipitated layer of the stirring tank 6 will not enter the reaction tank 7 through the drain port 833. When drainage is required, the vent 72 is released. At this time, the gas overflows under the gravity of the solution, and the solution enters the reaction tank 7 through the drain port 833. During this process, the drainage speed and stop can be adjusted by opening and closing the vent 72.
[0063] Even though the present invention has been described with reference to specific exemplary embodiments, many different alternatives and modifications will become apparent to those skilled in the art. It should also be noted that the circuit layout and identification / detection methods within the device of the present invention can be omitted, and can be interchanged or arranged in various ways, while the structure of the device still enables it to perform the functionality of the present invention.
Claims
1. A propane oxidation catalyst preparation apparatus, comprising a support column (1), a transmission belt (2), a motor (3), a differential speed mechanism (4), a stirring mechanism (5), a stirring tank (6), and a reaction tank (7); a motor (3) is installed at one end of the support column (1), and the motor (3) is driven by the differential speed assembly via the transmission belt (2); the stirring mechanism (5) is installed at the lower end of the differential speed assembly, and the stirring tank (6) and the reaction tank (7) are placed vertically in a mirror image; characterized in that: It also includes a purification mechanism (8); the purification mechanism (8) is installed between the stirring tank (6) and the reaction tank (7). The purification mechanism (8) inserts the piercing rod (831) into the non-precipitated layer by adjusting the distance between the stirring tank (6) and the reaction tank (7), and changes the solution concentration in the stirring tank (6) according to the different piercing depth, thereby achieving purification. The purification mechanism (8) includes a distance adjustment component (81), a support frame (82), and a puncture component (83). The distance adjustment component (81) is slidably connected to the side wall of the support column (1), and one end of the distance adjustment component (81) is fixedly connected to the support frame (82). The support frame (82) is configured as two vertically placed components that are fixedly connected to the lower bottom surface of the stirring tank (6) and the upper bottom surface of the reaction tank (7), respectively. The puncture component (83) is fixedly connected inside the support frame (82). During the process of the distance adjustment component (81) adjusting the support frame (82), the vertical position of the puncture component (83) is changed, thereby placing the outlet (833) of the puncture rod (831) in the non-precipitate layer and adjusting the reaction rate. The pitch adjustment assembly (81) includes a sliding ring (811), a rack (812), a meshing gear (813), a rotating shaft (814), and a rotating handle (815). The sliding ring (811) is slidably connected to the side wall of the support column (1), the rack (812) is fixedly connected to the side wall of the support column (1), one end of the rotating shaft (814) is fixedly connected to the meshing gear (813), the sliding ring (811) is provided with a sliding groove (816), the rack (812) passes through the sliding groove (816) vertically, and the pitch adjustment assembly (81) twists the rotating handle (815) so that the meshing gear (813) slides and meshes on the surface of the rack (812), thereby adjusting the solution content in the stirring drum (6) during the stirring process. The puncture assembly (83) includes a puncture rod (831) and a water-blocking baffle (832); the puncture rod (831) is fixedly connected to the surface of the lower plate (71), the lower plate (71) and the support plate are coaxial, the lower plate (71) has a central recessed structure, the puncture rod (831) has a hollow structure and multiple layers of water-blocking baffles (832) are provided on the surface, so that the purification of different layers of water-blocking baffles (832) will not affect each other during the reaction process.
2. The apparatus for preparing a propane oxidation catalyst according to claim 1, characterized in that: Drainage ports (833) are provided between the water-blocking baffles (832). Multiple drainage ports (833) are arranged in a ring array around the side wall of the piercing rod (831). Under the layered restriction of the water-blocking baffles (832), drainage and purification are carried out at different rates, so that the solution reaction process of the propane oxidation catalyst is controllable.
3. The apparatus for preparing a propane oxidation catalyst according to claim 1, characterized in that: The upper end of the puncture rod (831) is set as a "cone" structure and the bottom surface is in contact with the water-blocking baffle (832). Through the "cone" puncture head (834), the puncture rod (831) can ensure the water-blocking effect during the puncture of the upper plate (61).
4. The apparatus for preparing a propane oxidation catalyst according to claim 3, characterized in that: The surface of the upper plate (61) is provided with a plurality of puncture holes (835), wherein the puncture holes (835) are provided with a cross-shaped cut, so that the cone-shaped structure can be punctured through the cut and achieve water-resistant puncture, and combined with the water-blocking baffle (832) to achieve drainage stability.
5. The apparatus for preparing a propane oxidation catalyst according to claim 2, characterized in that: A gas inlet (72) is provided on one side of the reaction cylinder (7). By controlling the opening and closing of the gas inlet (72), the solution in the stirring cylinder (6) can be discharged through the drain port (833), thereby allowing the solution in the stirring cylinder (6) to be purified by controlled drainage.
6. The apparatus for preparing a propane oxidation catalyst according to claim 2, characterized in that: A flexible plate (62) is fixedly connected between the lower plate (71) and the upper plate (61). The maximum extension length of the flexible plate (62) is the same as the length of the rack (812), so that the water overflowing from the drain (833) can be sealed during the adjustment process of the adjustment component (81) to meet the purification requirements. The surface of the lower plate (71) is provided with multiple water inlets (73), so that the water overflowing from the drain (833) enters the reaction cylinder (7) through the water inlets (73).
7. A process for preparing a propane oxidation catalyst, wherein the process uses the equipment for preparing a propane oxidation catalyst according to any one of claims 1 to 6, characterized in that: The preparation process of the propane oxidation catalyst includes the following steps: S1: Material preparation: Prepare a certain amount of AgNO3 and NaH2PO4, as well as deionized water, and seal the gas port (72) of the preparation equipment; S2: Then, the prepared AgNO3 and NaH2PO4 are dissolved in a stirring tank (6) filled with deionized water at a molar ratio of 1:
1. The stirring mechanism (5) is powered by the motor (3) to stir the solution. At this time, the distance of the adjusting component (81) in the purification mechanism (8) is set to the maximum, the extension length of the flexible plate (62) is also the longest, and the piercing rod (831) does not penetrate the lower plate (71); the precursor solution of AgPO4 is obtained. S3: At room temperature, deionized water containing sodium ethylenediaminetetraacetate (EDTA) was added to the AgPO4 precursor solution and stirred evenly by stirring mechanism (5) to obtain a white precipitate and AgPO4 precursor solid. S4: Next, by inserting the piercing rod (831) into the stirring tube (6) at different depths, the solution in the stirring tube (6) is increased or decreased, and the precipitate is subjected to hydrothermal treatment under different temperature and time conditions to obtain AgPO4 crystals with different morphologies. The crystal growth and crystal face exposure of AgPO4 are controlled by hydrothermal method. S5: Finally, the precipitate is washed with ethanol at 80°C. Since the crystal growth of AgPO4 has ended, the precipitate and solution are separated into layers. The precipitate is located at the bottom of the stirred tank (6) and the water is discharged through the purification mechanism (8). Then the puncture rod (831) is removed from the stirred tank (6), the puncture hole (835) is closed, and the precipitate is retained in the stirred tank (6). It is dried at 60°C for 12 hours to obtain the AgPO4 catalyst.