Method for equivalent-volume impregnation in loading process of metal-loaded catalyst and stirring device thereof

Abstract

The invention discloses an equivalent-volume impregnation method in a loading process of a metal-loaded catalyst and a stirring device thereof. The method comprises the following steps: S1, sampling and detecting the water absorption rate of a substrate material and the volatilization speed per hour of impregnation mixture slurry; s2, feeding the substrate material into a mixing tank; s3, preparing a metal salt solution of equal-proportion water according to the water absorption rate, and storing the metal salt solution into a storage tank; s4, putting an execution end of a stirrer into the mixing tank, and synchronously starting the stirrer and a pump: stirring the substrate material by the stirrer, extracting the metal salt solution by the pump, injecting the substrate material through a liquid injection pipeline and the execution end until the solution is completely injected, and closing the pump to complete initial-stage stirring; s5, calculating the middle-section stirring duration according to the weight of the substrate material, and stirring at an initial-section rotating speed to form mixture slurry; s6, reducing the stirring rotating speed, and accounting the final-stage stirring duration according to the weight of the substrate material; meanwhile, a pump is started, equal-proportion ionized water is extracted according to the volatilization speed of the mixture slurry and injected through an execution end, and equal-volume impregnation is completed.

Description

Technical Field

[0001] This invention relates to the field of equal-volume impregnation of catalysts, specifically a method for equal-volume impregnation during the loading process of a metal-supported catalyst and its stirring device. Background Technology

[0002] When producing metal-supported catalysts, existing support technologies are generally divided into equal volume impregnation and ion exchange methods, with equal volume impregnation being the mainstream method. Currently, the equal volume impregnation method includes the following steps in sequence: testing the water absorption of the substrate material - preparing a metal salt solution - mixing an appropriate amount of substrate material and metal salt solution according to the water absorption rate and stirring to form a toothpaste-like slurry - allowing the slurry mixture to stand.

[0003] The current equal-volume impregnation method has the following main disadvantages: 1. When mixing the substrate material and the metal salt solution, uneven mixing can easily occur, resulting in uneven density of the metal loaded on the substrate material, which negatively affects the catalytic effect of the finished catalyst. 2. When the mixture slurry is left to stand, it will continue to volatilize, and the solvent water in the mixture will gradually decrease, causing the mixture slurry to dry and clump, greatly reducing the loading effect. Summary of the Invention

[0004] The purpose of this invention is to provide a method for equal-volume impregnation of a metal-supported catalyst during loading and a stirring device thereof, so as to solve the problems mentioned in the background art.

[0005] To address the aforementioned technical problems, this invention provides the following technical solution: a method for equal-volume impregnation during the loading process of a metal-supported catalyst, comprising the following steps: S1: Take small samples of the base material and the mixture slurry impregnated with the base material respectively, and test the water absorption rate of the base material and the volatilization rate of the mixture slurry per hour; S2: Store the base material into the mixing tank; S3: Prepare a metal salt solution containing an equal proportion of water based on the water absorption rate of the substrate material in the mixing tank, and store it in a storage tank; S4: The substrate material in the mixing tank is placed into the agitator actuator. Then, the agitator and pump are started simultaneously. The agitator actuator stirs the substrate material, while the pump draws out the metal salt solution and delivers it to the agitator actuator through the injection pipe. The metal salt solution is pumped into the substrate material through the agitator actuator and mixed with the substrate material until all the metal salt solution in the storage tank is injected into the substrate material. Then, the pump is turned off to complete the initial stirring. S5: Calculate the intermediate stirring time based on the weight of the substrate material, and perform intermediate stirring to form a slurry mixture of substrate material and metal salt solution. Maintain the initial stirring speed during intermediate stirring. S6: Reduce the stirring speed and calculate the final stirring time based on the weight of the substrate material. At the same time, start the pump. The pump extracts and delivers an equal proportion of deionized water to the mixer execution end based on the hourly evaporation rate of the mixture slurry, and pumps it into the substrate material. The deionized water is stirred and mixed with the substrate material until the impregnation is completed with equal volume.

[0006] Furthermore, the mixer speed for the initial and intermediate mixing stages in steps S4-5 is 5-10 r / min, and the mixer speed for the final mixing stage in step S6 is 1-3 r / min.

[0007] Furthermore, the mixing times for the initial mixing, intermediate mixing, and final mixing in steps S4-6 are 1 kg / 10 min, 1 kg / 1 h, and 1 kg / 24 h, respectively.

[0008] Furthermore, the flow rate of the metal salt solution pumped in step S4 is obtained by subtracting the initial stirring time from the metal salt solution content in the storage tank, and the flow rate of the deionized water pumped in step S6 is equal to the hourly evaporation rate of the mixed slurry in step S1.

[0009] Furthermore, the hourly evaporation rate of the mixture slurry in step S1 is derived from Dalton's law of evaporation, and the environment of the mixture slurry during the final stirring in step S6 is the same as the environment of the mixture slurry during detection in step S1.

[0010] A stirring apparatus for an equal-volume impregnation method applied in the loading process of a metal-supported catalyst includes: a storage tank for storing a metal salt solution, a pump, a stirrer, and a mixing tank for storing a substrate material; The input end of the pump is connected to the output end of the electrically controlled three-way valve through a liquid extraction pipeline. The two input ends of the electrically controlled three-way valve are respectively connected to the storage tank and the external ionized water supply end through two branch pipelines. The actuator of the mixer includes an injection shaft that is driven by the mixer drive shaft, a mixing and distributing plate that is fixedly connected to the bottom of the injection shaft, and a plurality of mixing pipes that are fixed and evenly connected to the bottom of the mixing and distributing plate. The injection shaft and the mixing pipes are both connected to the mixing and distributing plate. The pump is connected to the injection shaft through an injection pipe and a transfer mechanism.

[0011] Furthermore, the middle part of the stirring tube is bent at 90°, and the output end of the stirring tube faces the outside of the mixing and distributing disc.

[0012] The beneficial effects achieved by this invention patent are as follows: By placing the agitator's actuator into the substrate material within the mixing tank, the metal salt solution is directly pumped into the substrate material. Combined with the stirring tubes evenly positioned at the bottom of the mixing and dispersing plate, the metal salt solution is uniformly dispersed within the substrate material, preventing the agglomeration of the active metal components and improving the yield of the catalyst product.

[0013] By modifying the original static mixture slurry to a slowly stirred mixture slurry, and by extracting and supplying an equal proportion of deionized water to the mixture slurry based on the hourly evaporation rate of the mixture slurry, the drying and caking phenomenon that occurs during static standing is effectively avoided, the loading rate of the metal active components is increased, and the catalytic performance of the catalyst is enhanced.

[0014] The supporting equipment realizes the automatic switching supply of metal salt solution and deionized water through an electrically controlled three-way valve. Combined with the unified signal control of pump, agitator and electrically controlled three-way valve by the external control system, the output flow rate of pump, speed and duration of agitator can be set in advance to realize the automation and standardization of the entire impregnation process, reduce human operation error, and improve the stability and repeatability of the production process. At the same time, the segmented stirring process and precise parameter design optimize the production process and improve production efficiency. Attached Figure Description

[0015] Figure 1 This is a flowchart of an equal-volume impregnation method during the loading process of a metal-supported catalyst in Example 1; Figure 2 This is a schematic diagram of the stirring device in Example 2; Figure 3 This is a comparison diagram showing the effect of catalyst A produced by the method of this invention and catalyst B produced by the conventional method. Detailed Implementation

[0016] The present invention will be further described below with reference to the accompanying drawings. Example

[0017] like Figure 1 As shown, Example 1 discloses a method for equal-volume impregnation during the loading process of a metal-supported catalyst, comprising the following steps: S1: Take small samples of the base material and the mixture slurry impregnated with the base material respectively, and test the water absorption rate of the base material and the volatilization rate of the mixture slurry per hour; S2: Store the base material into the mixing tank 6; S3: Prepare a metal salt solution containing an equal proportion of water based on the water absorption rate of the substrate material in the mixing tank 6, and store it in the storage tank 1; S4: The substrate material in the mixing tank 6 is placed into the agitator 4. Then, the agitator 4 and pump 3 are started simultaneously. The agitator 4 agitates the substrate material, while the pump 3 draws out the metal salt solution and delivers it to the agitator 4 through the injection pipe 5. The metal salt solution is pumped into the substrate material through the agitator 4 and mixed with the substrate material until all the metal salt solution in the storage tank 1 is injected into the substrate material. Then, the pump is turned off to complete the initial mixing and achieve the effect of uniformly dispersing the metal salt solution into the substrate material. S5: Maintain the initial stirring speed during the intermediate stirring stage, and calculate the intermediate stirring time based on the weight of the substrate material. Perform intermediate stirring to ensure that the substrate material and metal salt solution are mixed evenly, ensuring that the loading density of the metal salt solution on the substrate material is consistent, forming a mixed slurry, thereby ensuring the catalytic effect of the finished catalyst. S6: Reduce the stirring speed and calculate the final stirring time based on the weight of the substrate material. At the same time, start pump 3. Pump 3 extracts and delivers an equal proportion of deionized water to the actuator of mixer 4 based on the hourly evaporation rate of the mixture slurry, and pumps it into the substrate material. The deionized water is stirred and mixed with the substrate material until the impregnation is completed in equal volume. During this process, the pumping of deionized water accurately maintains the solvent content and humidity of the mixture slurry, which completely solves the problem of drying and caking caused by the reduction of solvent during the standing process, effectively improves the metal loading effect, and thus increases the catalytic effect of the finished catalyst.

[0018] Furthermore, the speed of mixer 4 in the initial and intermediate stages of mixing in steps S4-5 is 5-10 r / min, and the speed of mixer 4 in the final stage of mixing in step S6 is 1-3 r / min.

[0019] Furthermore, the mixing times for the initial mixing, intermediate mixing, and final mixing in steps S4-6 are 1 kg / 10 min, 1 kg / 1 h, and 1 kg / 24 h, respectively.

[0020] Furthermore, the flow rate of the metal salt solution pumped in step S4 is obtained by subtracting the initial stirring time from the metal salt solution content in storage tank 1, and the flow rate of the deionized water pumped in step S6 is equal to the hourly evaporation rate of the mixed slurry in step S1.

[0021] Furthermore, the hourly evaporation rate of the mixture slurry in step S1 is derived from Dalton's law of evaporation, and the environment of the mixture slurry during the final stirring in step S6 is the same as the environment of the mixture slurry during detection in step S1. Example

[0022] Please see Figure 2Example 2 discloses a stirring device for an equal-volume impregnation method applied to the loading process of a metal-supported catalyst, comprising: a storage tank 1 for storing a metal salt solution, a pump 3, a stirrer 4, and a mixing tank 6 for storing a substrate material; The input end of pump 3 is connected to the output end of electric three-way valve 21 through the liquid extraction pipe 2. The two input ends of electric three-way valve 21 are connected to storage tank 1 and external ion water supply end through two branch lines respectively. The actuator of the mixer 4 includes an injection shaft 41 that is connected to the mixer drive shaft, a mixing and distributing plate 42 that is fixedly connected to the bottom of the injection shaft 41, and a plurality of mixing pipes 43 that are fixed and evenly connected to the bottom of the mixing and distributing plate 42. The injection shaft 41 and the mixing pipes 43 are both connected to the mixing and distributing plate 42. The pump 3 is connected to the injection shaft 41 through the injection pipe 5 and the transfer mechanism. The metal salt solution / ionized water output by pump 3 is sequentially pumped into the base material / mixture slurry through injection pipe 5, transfer mechanism, injection shaft 41, mixing and dispersing plate 42 and stirring pipe 43.

[0023] Furthermore, such as Figure 2 As shown, the middle part of the stirring tube 43 is bent at 90°, and the output end of the stirring tube 43 faces the outside of the mixing and distributing plate 42.

[0024] Furthermore, pump 3, mixer 4, and electrically controlled three-way valve 21 are all connected to an external control system. During the initial stirring stage, the external control system controls the electrically controlled three-way valve 21 to connect the input end of the liquid extraction pipe 2 with the output end of the branch line connecting to the storage tank 1. During the final stirring stage, the external control system controls the electrically controlled three-way valve 21 to connect the input end of the liquid extraction pipe 2 with the output end of the branch line connecting to the external ion water supply end.

[0025] Furthermore, the liquid output flow rate of pump 3 and the running time and speed of mixer 4 are all set in advance by on-site personnel based on production needs.

[0026] The transfer mechanism of the stirring device in this invention patent consists of cavity 204, inlet 205 and oil seal 207 of the closed fermentation organic fertilizer gas-supply and liquid-transfer stirring device (hereinafter referred to as the prior art) with publication number CN204417365U and patent name CN204417365U. It is already prior art and will not be described in detail here. The liquid injection shaft 41 of the stirring device in this invention patent has the same structure as the rotating shaft 202 in the prior art, which is already prior art and will not be described in detail here; The process of transporting the metal salt solution / ionized water sequentially through the injection pipe 5 and the transfer mechanism to the injection shaft 41 in this invention patent is the same as the process of transporting tap water sequentially through the inlet pipe a to the rotating shaft 20 in the prior art. It is already prior art and will not be described again here.

[0027] This invention patents amplify the process by placing the agitator's actuator into the substrate material within the mixing tank, allowing the metal salt solution to be directly pumped into the substrate material. Combined with agitator tubes evenly positioned at the bottom of the mixing and distributing plate, this ensures the metal salt solution is uniformly dispersed within the substrate material, preventing the agglomeration of active metal components and improving the yield of the catalyst product. Furthermore, by modifying the original static mixing slurry to a slowly agitated mixing slurry, and by extracting and supplying an equal proportion of deionized water to the slurry based on its hourly evaporation rate, this invention effectively avoids the drying and caking phenomenon that occurs during static mixing, increasing the loading rate of the active metal components and enhancing the catalytic performance of the catalyst.

[0028] The above are merely preferred embodiments of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A method for equal-volume impregnation during the loading process of a metal-supported catalyst, characterized in that, Includes the following steps: S1: Take small samples of the base material and the mixture slurry impregnated with the base material respectively, and test the water absorption rate of the base material and the volatilization rate of the mixture slurry per hour; S2: Store the base material in the mixing tank; S3: Prepare a metal salt solution containing an equal proportion of water based on the water absorption rate of the substrate material in the mixing tank, and store it in a storage tank; S4: The substrate material in the mixing tank is placed into the agitator actuator. Then, the agitator and pump are started simultaneously. The agitator actuator stirs the substrate material, while the pump draws out the metal salt solution and delivers it to the agitator actuator through the injection pipe. The metal salt solution is pumped into the substrate material through the agitator actuator and mixed with the substrate material until all the metal salt solution in the storage tank is injected into the substrate material. Then, the pump is turned off to complete the initial stirring. S5: Calculate the intermediate stirring time based on the weight of the substrate material, and perform intermediate stirring to form a slurry mixture of substrate material and metal salt solution. Maintain the initial stirring speed during intermediate stirring. S6: Reduce the stirring speed and calculate the final stirring time based on the weight of the substrate material. Perform the final stirring and start the pump. The pump extracts and delivers an equal proportion of deionized water to the mixer execution end based on the hourly evaporation rate of the mixture slurry. The deionized water is then pumped into the substrate material. The deionized water is stirred and mixed with the substrate material until the impregnation is completed with an equal volume.

2. The method for equal-volume impregnation according to claim 1, characterized in that: The mixer speed for the initial and intermediate mixing stages in steps S4-5 is 5-10 r / min, and the mixer speed for the final mixing stage in step S6 is 1-3 r / min.

3. The method for equal-volume impregnation according to claim 1, characterized in that: The mixing times for the initial mixing, intermediate mixing, and final mixing in steps S4-6 are 1 kg / 10 min, 1 kg / 1 h, and 1 kg / 24 h, respectively.

4. The method for equal-volume impregnation according to claim 3, characterized in that: The flow rate of the metal salt solution pumped in step S4 is obtained by subtracting the initial stirring time from the metal salt solution content in the storage tank. The flow rate of the deionized water pumped in step S6 is equal to the hourly evaporation rate of the mixed slurry in step S1.

5. The method for equal-volume impregnation according to any one of claims 1-4, characterized in that: The hourly evaporation rate of the mixture slurry in step S1 is determined according to Dalton's law of evaporation. The environment of the mixture slurry during the final stirring in step S6 is the same as that of the mixture slurry during detection in step S1.

6. A stirring apparatus for use in the equal-volume impregnation method of claim 5, characterized in that: include: Storage tanks, pumps, agitators, and mixing tanks for storing metal salt solutions; The input end of the pump is connected to the output end of the electrically controlled three-way valve through a liquid extraction pipeline. The two input ends of the electrically controlled three-way valve are respectively connected to the storage tank and the external ionized water supply end through two branch pipelines. The actuator of the mixer includes an injection shaft that is driven by the mixer drive shaft, a mixing and distributing plate that is fixedly connected to the bottom of the injection shaft, and a plurality of mixing pipes that are fixed and evenly connected to the bottom of the mixing and distributing plate. The injection shaft and the mixing pipes are both connected to the mixing and distributing plate. The pump is connected to the injection shaft through an injection pipe and a transfer mechanism.

7. The control method for the equal-volume impregnation method according to claim 6, characterized in that: The stirring tube is bent at 90° in the middle, and the output end of the stirring tube faces the outside of the mixing and distributing plate.

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