Automatic washing device for catalysts

Abstract

The utility model relates to the field of catalytic cracking catalyst washing discloses a kind of automatic washing device of catalyst, and the automatic washing device includes catalytic cracking catalyst supply unit, electronic control unit, water feed pipe, washing solution feed pipe, tank and suction filter machine;The catalytic cracking catalyst supply unit is used to provide catalytic cracking catalyst to tank;The water feed pipe and the washing solution feed pipe are set to the top of tank;The suction filter machine is communicated with the bottom outlet of tank;The electronic control unit is used to control the whole process of automatic washing.The device can realize the full-process automatic washing of catalytic cracking catalyst, not only improve the washing effect of catalytic cracking catalyst, but also reduce the labor cost.

Description

Technical Field

[0001] This utility model relates to the field of catalyst washing in catalytic cracking, and specifically to an automated catalyst washing device. Background Technology

[0002] Catalytic cracking (FCC) is one of the most important secondary petroleum processing steps and a crucial technology for the lightening of heavy oil. The catalytic cracking catalyst is the core component for achieving efficient conversion and clean utilization of heavy oil in the FCC process. The preparation of catalytic cracking catalysts typically includes: mixing and gelling the components, spray drying and molding, calcination, and catalyst washing. The resulting catalyst microspheres often contain impurities that affect catalyst performance, such as Na₂O, Fe₂O₃, and Cl₂. - Among these, Na2O has a significant impact on the activity and stability of the catalyst. Na2O mainly originates from the Y-type molecular sieve, the active component of FCC catalysts. Generally, the Na2O mass fraction in spray-formed catalysts can reach over 1.5%, while actual FCC catalyst products require a Na2O mass fraction ≤0.3%, and ideally ≤0.25%. Therefore, FCC catalysts need to undergo washing treatment to reduce the content of Na2O and other impurities.

[0003] Currently, catalytic cracking catalysts prepared in the laboratory are generally washed manually. During the washing process, workers need to be on-site throughout, and there is no fixed washing method. The washing process for each catalyst takes approximately 50-60 minutes. This washing method suffers from problems such as being time-consuming and having high labor costs.

[0004] Following market research and patent searches, CN211513570U discloses a vacuum filtration device for washing laboratory-prepared polyolefin catalysts, related to automated catalyst washing. This device uses a vacuum pump to create a vacuum in the waste liquid recovery bottle, then uses this vacuum for filtration, without damaging the reactor's seal, and can completely remove excess titanium tetrachloride, alcohols, and other substances, achieving a thorough washing effect. However, it is not suitable for catalytic cracking catalysts. CN213316526U discloses a catalyst washing device. This device is mainly used for washing large-sphere catalysts Pb / Al2O3. A special design reduces the amount of washing water used. CN204247233U discloses a polyolefin catalyst washing device. This device, through a special structure, reduces the catalyst's contact with air, ensuring catalyst performance, effectively controlling the volatilization of toxic and harmful gases, and avoiding or reducing pollution to humans and the environment. However, existing technologies lack automated washing devices and methods specifically for catalytic cracking catalysts. Utility Model Content

[0005] The purpose of this invention is to overcome the problems existing in the prior art and provide an automated catalyst washing device. Using the device described in this invention, the entire process of catalytic cracking catalyst washing can be automated, which not only improves the washing effect of the catalytic cracking catalyst but also reduces labor costs.

[0006] To achieve the above objectives, this utility model provides an automated catalyst washing device, which includes a catalytic cracking catalyst supply unit, an electronic control unit, a water feed pipe, a washing solution feed pipe, a tank, and a filter press.

[0007] The catalytic cracking catalyst supply unit is used to supply catalytic cracking catalyst to the tank;

[0008] The water inlet pipe and the washing solution inlet pipe are located at the top of the tank.

[0009] The filter is connected to the bottom outlet of the tank.

[0010] The electronic control unit is used to control the entire automated washing process.

[0011] The beneficial effects of this utility model through the above technical solution include:

[0012] Using the device described in this invention, the washing of catalytic cracking catalysts can be automated, which can improve the efficiency and quality of catalyst washing and reduce labor costs. Attached Figure Description

[0013] Figure 1 This is a schematic diagram of the structure of the automated catalyst washing device described in this utility model.

[0014] Explanation of reference numerals in the attached figures

[0015] 1. Electronic control panel; 2. Water inlet pipe; 3. Washing solution inlet pipe;

[0016] 4. Tank body; 5. Screen; 6. Sealing valve;

[0017] 7. Electric valve; 8. Filter press; 9. Drain port;

[0018] 10. Mixing equipment; 11. Cover plate. Detailed Implementation

[0019] The endpoints and any values ​​of the ranges disclosed herein are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.

[0020] This utility model provides an automated catalyst washing device, which includes a catalytic cracking catalyst supply unit, an electronic control unit, a water feed pipe 2, a washing solution feed pipe 3, a tank 4, and a vacuum filter 8;

[0021] The catalytic cracking catalyst supply unit is used to supply catalytic cracking catalyst to tank 4;

[0022] The water inlet pipe 2 and the washing solution inlet pipe 3 are located at the top of the tank body 4;

[0023] The filter press 8 is connected to the bottom outlet of the tank 4;

[0024] The electronic control unit is used to control the entire automated washing process.

[0025] In this invention, the electronic control unit includes a control circuit and an electronic control panel 1, which enables parameter control throughout the washing process.

[0026] According to a preferred embodiment of this utility model, the automated washing device further includes a microwave transmission unit, and the tank 4 is connected to the microwave transmission unit. With this preferred embodiment, microwave assistance during the washing process results in a more thorough washing.

[0027] This invention does not impose any particular limitation on the specific configuration of the microwave conduction unit, and can be a conventional choice in the field.

[0028] According to a preferred embodiment of this invention, the microwave transmission device includes a power supply, a magnetron, and a waveguide device. In this invention, a high-frequency voltage is supplied to the magnetron by the power supply, and then the microwaves are transmitted to the washing solution inside the tank 4 via the waveguide device. With microwave assistance, heating is achieved while simultaneously allowing the sulfate ions in the washing solution to fully react with the sodium ions in the catalyst, resulting in a stronger bond and more thorough washing.

[0029] According to a preferred embodiment of this utility model, the interior of the tank 4 is coated with an acid- and alkali-resistant non-magnetic material. This preferred embodiment ensures that the tank is not easily corroded by acid or alkali solutions during the washing process, and also prevents the generation of electric current with microwaves, thus avoiding any potential danger.

[0030] In this invention, the acid and alkali resistant non-magnetic material can be any of the common acid and alkali resistant non-magnetic materials in the art, such as polytetrafluoroethylene, enamel, etc.

[0031] According to a preferred embodiment of this utility model, the tank 4 is a funnel-shaped tank, which includes a main body and a variable diameter section. The main body is cylindrical. In this utility model, the variable diameter section is a cone with a long spout.

[0032] According to a preferred embodiment of the present invention, the tank body 4 is made of stainless steel.

[0033] In this invention, the automated washing device may include one tank 4 or multiple tanks 4, which can be selected according to the amount of catalytic cracking catalyst.

[0034] According to a preferred embodiment of the present invention, the automated washing device further includes a screen 5, which is horizontally arranged on the main body of the funnel-shaped tank.

[0035] More preferably, the screen 5 is horizontally positioned at the bottom of the funnel-shaped tank body. This preferred embodiment facilitates full utilization of the tank while simultaneously ensuring adequate drainage of the liquid within.

[0036] According to this utility model, preferably, the diameter of the screen 5 is 40-80% of the diameter of the main body of the tank 4, and more preferably 50-70%.

[0037] This invention does not impose any particular limitation on the aperture of the screen 5, as long as it can achieve the purpose of retaining the catalytic cracking catalyst.

[0038] According to a preferred embodiment of the present invention, the automated washing device further includes a stirring device 10, the stirring paddle of which is disposed in the lower middle part of the main body of the tank 4. This preferred embodiment enables the stirring of the washing solution and the catalytic cracking catalyst during the washing process.

[0039] According to a preferred embodiment of the present invention, the filter 8 is connected to the bottom outlet of the tank 4 via a pipe, and an electric valve 7 is provided on the pipe for switching between washing mode and filter mode.

[0040] According to a preferred embodiment of this utility model, the bottom outlet of the tank 4 is connected to the pipeline via a sealing valve 6. This preferred embodiment allows for the connection and disconnection of the tank 4 and the pipeline.

[0041] When connected, the catalytic cracking catalyst is washed throughout the entire process; when separated, the catalytic cracking catalyst is poured out.

[0042] To achieve the above functions, the sealing valve 6 of this utility model is a detachable sealing valve, for example, it can be a snap-fit ​​connection.

[0043] According to a preferred embodiment of the present invention, the automated washing device further includes a cover plate 11, which covers the tank body 4 to achieve the closure of the automated washing device.

[0044] According to a preferred embodiment of the present invention, the filter press 8 is further provided with a drain port 9 for discharging the washing solution.

[0045] According to a specific embodiment of this utility model, please refer to Figure 1 Close the electric valve 7, tighten the sealing valve 6, and cover with the cover plate 11. Feed the catalytic cracking catalyst into the tank 4. The screen 5 serves to trap the catalytic cracking catalyst. Turn on the switch on the electronic control panel 1, set the washing parameters, and the washing solution automatically enters the tank 4 from the washing solution inlet pipe 3, and water (pure water / acidic water) automatically enters the tank 4 from the water inlet pipe 2. The stirring device 10 is turned on for stirring, and the microwave is turned on to begin washing. After each washing cycle, open the electric valve 7, extract the washing solution through the filter press 8, and discharge it from the drain port 9. At this time, the sodium oxide content is no more than 0.25 wt%.

[0046] Water (pure water / acidic water) automatically enters the tank 4 from the water inlet pipe 2. The stirring device 10 is turned on to stir, the microwave is turned on, and the water washing begins. After the water washing is completed, the electric valve 7 is opened, the water is extracted through the filter 8 and discharged from the drain port 9.

[0047] After the entire washing process is completed, the cover plate 11, water inlet pipe 2, washing liquid inlet pipe 3, and stirring device 10 are raised together. The tank body 4 is separated from other parts through the sealing valve 6, and the washed catalytic cracking catalyst is poured out.

[0048] In this invention, under the action of microwaves, the internal temperature of the tank rises to a certain level, which is beneficial to improving the washing effect. According to this invention, preferably, the washing conditions include: a temperature of 50-90℃ and a time of 3-13 minutes, preferably 5-10 minutes.

[0049] According to this invention, preferably, the washing is carried out under stirring conditions. This preferred embodiment facilitates sufficient contact between the washing solution and the catalytic cracking catalyst.

[0050] According to this utility model, preferably, the stirring conditions include: a stirring rate of 30-200 r / min, more preferably 50-150 r / min.

[0051] According to this invention, preferably, the mass ratio of detergent to catalytic cracking catalyst in the washing solution is 0.02-0.05:1.

[0052] This invention allows for a wide range of choices regarding the specific types of washing solutions, which can be conventional choices in the field. Preferably, the washing solution is selected from at least one of aqueous solutions of ammonium sulfate, ammonium chloride, ammonium nitrate, and ammonium carbonate.

[0053] According to this invention, preferably, the concentration of detergent in the washing solution is 0.1-0.7 wt%.

[0054] In this invention, the water introduced through the water inlet pipe 2 can be pure water or acidic water, preferably acidic water. This preferred embodiment, working synergistically with the washing solution, achieves better washing results while reducing the amount of washing solution used.

[0055] Preferably, the pH of the acidic water is 1.5-4, and more preferably 2-3.

[0056] In this invention, the acid in the acidic water can be a conventional choice in the art, such as sulfuric acid.

[0057] Catalytic cracking catalysts prepared by conventional methods often contain impurities that affect their performance, such as Na₂O, Fe₂O₃, and Cl₂. - Among these factors, Na₂O has a significant impact on the activity and stability of catalytic cracking catalysts. Washing the catalytic cracking catalyst using the apparatus described in this invention can significantly reduce the Na₂O content, thereby effectively reducing its impact on the activity and stability of the catalytic cracking catalyst. According to this invention, preferably, the sodium oxide content in the washed catalytic cracking catalyst is no more than 0.25 wt%.

[0058] In this invention, the washing solution can be used to wash once or multiple times, with the sodium oxide content not exceeding 0.25 wt%.

[0059] In this invention, the sodium oxide content in the catalytic cracking catalyst is determined by fluorescence spectroscopy.

[0060] In this invention, preferably, the sodium oxide content is reduced to no more than 0.25 wt% by washing with a washing solution, followed by a water wash. This preferred embodiment is beneficial for removing residual detergent.

[0061] In this invention, the water used for washing can be pure water or the aforementioned acidic water, with the aforementioned acidic water being preferred.

[0062] This invention does not specifically limit the type of catalytic cracking catalyst, and can be any common catalytic cracking catalyst.

[0063] This invention does not particularly limit the source of the catalytic cracking catalyst, and it can be a catalytic cracking catalyst obtained by various means in the art, such as a catalytic cracking catalyst prepared by spray molding.

[0064] The present invention will be described in detail below through embodiments.

[0065] Example 1

[0066] Boehmite (from China Aluminum Shanxi Aluminum Co., Ltd.) was acidified with hydrochloric acid (the weight ratio of hydrochloric acid to boehmite, calculated as alumina, was 0.2). This mixture was then slurried with alumina sol (a product of Sinopec Catalyst Qilu Branch), kaolin (a product of Suzhou China Kaolin Co., Ltd.), and SOY-8 molecular sieve (a product of Sinopec Catalyst Qilu Branch) to prepare a slurry with a solid content of 30 wt%. The slurry was then spray-dried to form the catalytic cracking catalyst C1. The weight ratio of boehmite (based on Al2O3), alumina sol (based on Al2O3), kaolin (based on a dry basis), and SOY-8 molecular sieve (based on a dry basis) was 20:9:36:35. Add the catalytic cracking catalyst C1 above the screen 5 (screen diameter is 50% of the bottom diameter of the cylinder of tank 4) in tank 4. Close the electric valve 7, turn on the switch on the electronic control panel 1, and set the following settings: catalyst to acidic water (pH 3, 98wt% concentrated sulfuric acid added to deionized water) mass ratio 1:10, add acidic water, and add ammonium sulfate aqueous solution (0.02wt%) according to the catalyst to ammonium sulfate mass ratio 1:0.02; stirring speed 80r / min, stirring time 5min; filtration time 5min. Simultaneously turn on the microwave to heat the liquid temperature inside the tank to 70℃. Start washing. After stirring for 5 minutes, the stirring device 10 automatically stops stirring, the electric valve 7 opens, and the vacuum filter 8 starts filtration, the washing solution is drawn away and discharged through the drain port 9. After filtration is completed, the electric valve 7 closes. Repeat the above operation twice, that is, perform the above washing three times. Finally, only acidic water is added for washing, with a catalyst-to-acidic-water mass ratio of 1:10. Other operations are the same as the washing process described above. After the entire process is complete, the cover plate 11, water inlet pipe 2, washing solution inlet pipe 3, and stirring device 10 are raised together. The tank 4 is separated from other parts through the detachable sealing valve 6, and the washed catalytic cracking catalyst is poured out to obtain the washed catalyst S1. The entire process takes 45 minutes. After cleaning the tank, it is reinstalled for the next catalyst washing. Only the addition and removal of the catalyst requires manual intervention; the rest of the time, the device operates automatically.

[0067] Example 2

[0068] Boehmite (from China Aluminum Shandong New Materials Co., Ltd.) was acidified with hydrochloric acid (the weight ratio of hydrochloric acid to boehmite, calculated as alumina, was 0.2), and then slurried with alumina sol (a product of Sinopec Catalyst Qilu Branch), kaolin (a product of Suzhou China Kaolin Co., Ltd.), and PSRY molecular sieve (a product of Sinopec Catalyst Qilu Branch) to prepare a slurry with a solid content of 30 wt%. This slurry was then spray-dried to form the catalytic cracking catalyst C2. The weight ratio of boehmite (based on Al2O3), alumina sol (based on Al2O3), kaolin (based on a dry basis), and PSRY molecular sieve (based on a dry basis) was 24:9:32:35. Add catalytic cracking catalyst C2 above the screen 5 (screen diameter is 50% of the bottom diameter of the cylinder of tank 4) in tank 4. Close the electric valve 7, turn on the switch on the electronic control panel 1, and set the following settings: catalyst to acidic water (pH 2, 98wt% concentrated sulfuric acid added to deionized water) mass ratio 1:8, add acidic water; catalyst to ammonium sulfate mass ratio 1:0.02, add ammonium sulfate aqueous solution (0.02wt%); set the stirring speed to 100 r / min, stirring time to 8 min; and filtration time to 5 min. Simultaneously turn on the microwave to heat the liquid temperature inside the tank to 65℃. Begin washing. After stirring for 8 min, the stirring device 10 automatically stops stirring, the electric valve 7 opens, and the filtration machine 8 begins filtration, removing the catalyst washing solution through the drain port 9. After filtration is complete, close the electric valve 7. Repeat the above operation twice, for a total of three washing operations. Finally, only the aforementioned acidic water is added for washing, with a catalyst-to-acidic-water mass ratio of 1:8. Other operations are the same as the washing process described above. After the entire process is completed, the cover plate 11, water inlet pipe 2, washing solution inlet pipe 3, and stirring device 10 are raised together. The tank 4 is separated from other parts through the detachable sealing valve 6, and the washed catalytic cracking catalyst is poured out to obtain the washed catalyst S2. The entire process takes 56 minutes. After cleaning the tank, it is reinstalled for the next catalyst washing.

[0069] Example 3

[0070] The procedure was carried out according to Example 1, except that the microwave was not turned on, and the washed catalyst S3 was obtained.

[0071] Comparative Example 1

[0072] The existing process involves manual sample washing.

[0073] The catalytic cracking catalyst from Example 1 was added to a beaker. Deionized water was added at a mass ratio of 1:10 (catalyst to deionized water), and the deionized water temperature was 80°C. Simultaneously, an ammonium sulfate aqueous solution (0.02 wt%) was added at a mass ratio of 1:0.02 (catalyst to ammonium sulfate), and the washing solution temperature was 30°C. The beaker was then stirred at 80 rpm for 10 minutes. Stirring was then stopped, and filtration was prepared. Filter paper was placed in a vacuum funnel, and the liquid in the beaker was poured into the funnel. Filtration was completed in 5 minutes. The catalytic cracking catalyst in the funnel was then transferred back to the beaker, and the washing process was repeated twice, for a total of three washes. Finally, deionized water was added at a mass ratio of 1:10 (catalyst to water). After washing, the above filtration process was repeated. After the entire process was completed, catalyst sample D1 was obtained. The entire process took 65 minutes.

[0074] The operators need to be at the sample washing site for an extended period of time throughout the process.

[0075] Table 1

[0076]

[0077] As can be seen from the results in Table 1, the device described in this invention has a significantly better sodium removal effect when used to wash the catalytic cracking catalyst.

[0078] The preferred embodiments of this utility model have been described in detail above; however, this utility model is not limited thereto. Within the scope of the technical concept of this utility model, various simple modifications can be made to the technical solution of this utility model, including combining the various technical features in any other suitable manner. These simple modifications and combinations should also be considered as the content disclosed by this utility model and are all within the protection scope of this utility model.

Claims

1. An automated catalyst washing device, characterized in that, The automated washing device includes a catalytic cracking catalyst supply unit, an electronic control unit, a water feed pipe (2), a washing solution feed pipe (3), a tank (4), and a vacuum filter (8); The catalytic cracking catalyst supply unit is used to supply catalytic cracking catalyst to the tank (4); The water inlet pipe (2) and the washing solution inlet pipe (3) are located at the top of the tank body (4); The filter press (8) is connected to the bottom outlet of the tank (4); The electronic control unit is used to control the entire automated washing process.

2. The apparatus according to claim 1, characterized in that, The automated washing device also includes a microwave transmission unit, and the tank (4) is connected to the microwave transmission unit.

3. The apparatus according to claim 1, characterized in that, The interior of the tank (4) is coated with an acid and alkali resistant non-magnetic material.

4. The apparatus according to claim 1, characterized in that, The tank (4) is a funnel-shaped tank, which includes a main body and a variable diameter part. The main body is a cylinder.

5. The apparatus according to claim 4, characterized in that, The automated washing device also includes a screen (5), which is horizontally arranged on the main body of the funnel-shaped tank.

6. The apparatus according to claim 5, characterized in that, The diameter of the screen (5) is 40-80% of the diameter of the main body of the tank (4).

7. The apparatus according to claim 6, characterized in that, The diameter of the screen (5) is 50-70% of the diameter of the main body of the tank (4).

8. The apparatus according to claim 5, characterized in that, The automated washing device also includes a stirring device (10), the stirring paddle of which is located in the lower middle part of the main body of the tank (4).

9. The apparatus according to any one of claims 1-8, characterized in that, The filter press (8) is connected to the bottom outlet of the tank (4) through a pipe. An electric valve (7) is installed on the pipe for switching between washing mode and filter mode.

10. The apparatus according to claim 9, characterized in that, The bottom outlet of the tank (4) is connected to the pipeline via a sealing valve (6).

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