An impregnation apparatus and method for impregnating a solid particulate catalyst

Abstract

The present application belongs to the field of impregnation device, and particularly relates to a kind of solid particle catalyst impregnation device and impregnation method.The impregnation device includes: shell, impregnation liquid pipe, elastic device, shell cover, pressing plate, vacuum extraction pipe, settling cylinder, upper and lower through rising cylinder, inner container.The impregnation device bed body of the present application is provided with settling cylinder and rising cylinder, settling cylinder drops due to elastic force and gravity, and rising cylinder rises due to elastic force, so that carrier moves slightly all the time due to friction in the impregnation process, gas in the carrier can be fully sucked out by vacuum device, impregnation liquid can fully contact with carrier, impregnation quality is improved, and impregnation adsorption efficiency is improved, so as to improve the performance of catalyst.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of impregnation devices, and in particular, relates to an impregnation device and an impregnation method for solid particle catalysts. BACKGROUND

[0002] In chemical production processes, catalysts are often used to improve the yield of reaction products, especially solid particle catalysts of different sizes or shapes. The preparation of solid particle catalysts mostly uses impregnation, hot impregnation, room temperature static impregnation and spraying methods to realize the loading of active components onto the surface or internal pores of solid particle carriers. The traditional impregnation method is to pour the solution into the impregnation kettle in advance after being heated and then placed in the impregnation kettle with the carrier particles, and then static impregnation is carried out. This method has a long impregnation time. For carriers with small specific surface area or a large proportion of micropores, the adsorption of active components is not uniform, and the adsorption efficiency is low. For large particle carriers with some shapes, part of the carriers are easily aggregated into clusters, making it difficult to achieve the impregnation standard for the vacuum degree of this small part of the carriers. In addition, during impregnation, the impregnation liquid cannot completely enter this part of the carrier, resulting in a low concentration of active components on the surface of the carrier, which leads to unqualified catalysts. To solve the above problems, the existing technology mostly uses impregnation devices containing stirring devices to meet the requirements of uniform adsorption and high adsorption efficiency. However, the presence of stirring devices can cause the breakage of some catalyst carriers with small hardness, reducing the impregnation effect. SUMMARY

[0003] The present application aims to solve the above problems and provide an impregnation device and an impregnation method for solid particle catalysts, which can not only make the active components on the carrier of the solid particle catalyst adsorb uniformly and quickly during the impregnation process, but also efficiently complete the impregnation process of the solid particle catalyst, and avoid the problems of carrier breakage and aggregation during stirring. Compared with traditional impregnation devices and methods, the present application improves the yield of solid particle catalysts and reduces production costs.

[0004] To solve the above technical problems, the first aspect of the present application provides an impregnation device for solid particle catalysts, which comprises a shell, an impregnation liquid pipe, an elastic device, a shell cover, a pressing plate, a vacuum pipe, a settling cylinder, an upward cylinder, and an inner container.

[0005] One end of the impregnation liquid pipe and one end of the vacuum pipe are respectively in communication with the impregnation device; the other end of the impregnation liquid pipe is used to connect an impregnation liquid providing device, and the other end of the vacuum pipe is used to connect a vacuum device.

[0006] The impregnation device is a radial bed structure, the inner container, the ascending cylinder, the settling cylinder and the pressing plate are arranged in the shell; the ascending cylinder is partially or wholly located in the inner container, the settling cylinder is partially located in the ascending cylinder; the pressing plate is arranged on the settling cylinder and connected with the ascending cylinder through the elastic device;

[0007] A plurality of impregnation liquid holes are arranged on the walls of the settling cylinder, the ascending cylinder and the inner container respectively, the size of the impregnation liquid holes is such that the impregnation liquid can enter and exit but the carrier of the solid particle catalyst cannot enter and exit.

[0008] The second aspect of the present application provides an impregnation method of a solid particle catalyst, which uses the above-mentioned impregnation device of a solid particle catalyst, and the impregnation method comprises the following steps:

[0009] a. The inner container is arranged in the shell, the ascending cylinder is arranged in the inner container, the carrier of the solid particle catalyst is added to a first preset height, then the settling cylinder is arranged in the ascending cylinder, the carrier of the solid particle catalyst is continuously added to a second preset height, the pressing plate is arranged above the settling cylinder, and the pressing plate is connected with the ascending cylinder through the elastic device in the stretching state;

[0010] b. The shell and the shell cover are tightly connected;

[0011] c. The inside of the shell is vacuumized through the vacuumizing pipe, the impregnation liquid is input through the impregnation liquid pipe, and the impregnation liquid enters the inside of the inner container, the ascending cylinder and the settling cylinder through the impregnation liquid holes; in the process of vacuumizing and impregnation, the settling cylinder slowly descends due to the elastic force provided by the elastic device and the gravity provided by the pressing plate, and the ascending cylinder slowly ascends due to the elastic force provided by the elastic device, and after the impregnation is completed, the impregnation liquid and the carrier of the solid particle catalyst are discharged.

[0012] The present application has the following advantages:

[0013] The impregnation device of the present application adopts a radial bed structure, which is simple in structure, the inner container is internally arranged with the settling cylinder, the ascending cylinder and the pressing plate, the carrier filled in the inner container, the settling cylinder and the ascending cylinder is separated from the impregnation liquid by the cylinder wall uniformly covered with holes of a certain diameter, and the exposure area of the carrier is increased.

[0014] The settling cylinder and the ascending cylinder are arranged in the bed body of the impregnation device, the settling cylinder descends due to the elastic force and the gravity, and the ascending cylinder ascends due to the elastic force, so that the carrier always slightly moves due to the friction force in the impregnation process, the gas in the carrier can be fully sucked out by the vacuum device, the impregnation liquid can fully contact with the carrier, the impregnation quality is improved, the impregnation adsorption efficiency is improved, and the performance of the catalyst is improved.

[0015] Other features and advantages of the present application will be described in detail in the following specific embodiments. BRIEF DESCRIPTION OF DRAWINGS

[0016] The exemplary embodiments of the present application will be described in more detail by way of specific examples with reference to the accompanying drawings.

[0017] Figure 1 The structure of the impregnation device of the solid particle catalyst of the present application is shown.

[0018] Explanation of reference numerals: 1 - shell, 2 - impregnation liquid pipe, 3 - jacket, 4 - elastic device, 5 - shell cover, 6 - pressing plate, 7 - vacuum pipe, 8 - settling cylinder, 9 - rising cylinder, 10 - discharge plate, 11 - inner container. DETAILED DESCRIPTION

[0019] The specific embodiments of the present application will be described in detail below. It should be understood that the specific embodiments described herein are merely intended to illustrate and explain the present application, and are not intended to limit the present application.

[0020] The first aspect of the present application provides an impregnation device of a solid particle catalyst, which comprises: a shell, an impregnation liquid pipe, an elastic device, a shell cover, a pressing plate, a vacuum pipe, a settling cylinder, a rising cylinder penetrating up and down, and an inner container.

[0021] One end of the impregnation liquid pipe and the vacuum pipe is respectively communicated with the impregnation device; the other end of the impregnation liquid pipe is used for connecting an impregnation liquid providing device, and the other end of the vacuum pipe is used for connecting a vacuum device.

[0022] The impregnation device is of a radial bed structure, and the inner container, the rising cylinder, the settling cylinder and the pressing plate are all arranged in the shell; the rising cylinder is partially or entirely located in the inner container, and the settling cylinder is partially located in the rising cylinder; the pressing plate cover is arranged on the settling cylinder and connected with the rising cylinder through the elastic device.

[0023] A plurality of impregnation liquid holes are respectively arranged on the walls of the settling cylinder, the rising cylinder and the inner container, and the size of the impregnation liquid holes is such that the impregnation liquid can enter and exit, while the carrier of the solid particle catalyst cannot enter and exit.

[0024] As a preferred solution, a jacket is arranged outside the shell of the impregnation device for controlling the temperature of the impregnation liquid in the shell.

[0025] As a preferred solution, the impregnation device further comprises a discharge plate arranged at the bottom of the inner container.

[0026] As a preferred solution, the impregnation liquid holes are uniformly arranged on the walls of the settling cylinder, the rising cylinder and the inner container.

[0027] As a preferred solution, the impregnation liquid pipe is arranged diagonally to the vacuum pipe; more preferably, the impregnation liquid pipe is arranged below one side of the shell, and the vacuum pipe is arranged above the other side of the shell.

[0028] As a preferred solution, the elastic device is arranged to generate upward force on the rising cylinder and downward force on the pressing plate and the settling cylinder.

[0029] As a preferred solution, the elastic device is fixedly connected to one of the pressing plate and the rising cylinder, and detachably connected to the other one.

[0030] The elastic device is detachably connected to both the pressing plate and the rising cylinder.

[0031] As a preferred solution, the shell cover is detachably connected to the shell, and a sealing gasket is arranged between the shell cover and the shell.

[0032] The second aspect of the present application provides a method for impregnating solid particle catalysts, which employs the impregnation device for solid particle catalysts described above, and the method comprises:

[0033] a. placing the inner container in the shell, putting the rising cylinder into the inner container, adding the carrier of solid particle catalysts to a first preset height, then putting the settling cylinder into the rising cylinder, continuously adding the carrier of solid particle catalysts to a second preset height, covering the pressing plate above the settling cylinder, and connecting the pressing plate to the rising cylinder through the elastic device in a stretched state;

[0034] b. sealingly connecting the shell to the shell cover;

[0035] c. drawing the inside of the shell to a certain vacuum degree through the vacuum pipe, inputting the impregnation liquid through the impregnation liquid pipe, and making the impregnation liquid enter the inside of the inner container, the rising cylinder and the settling cylinder through the impregnation liquid holes; during the process of vacuum drawing and impregnation, the settling cylinder slowly descends due to the elastic force provided by the elastic device and the gravity provided by the pressing plate, and the rising cylinder slowly ascends due to the elastic force provided by the elastic device; after the impregnation is completed, the impregnation liquid and the carrier of solid particle catalysts are discharged.

[0036] As a preferred solution in step a, the carrier of solid particle catalysts covers the height h of the bottom of the inner container, and 5 cm≤h≤0.5*the height of the inner container.

[0037] According to the present application, the stretching state in step b needs to satisfy the condition that "the elastic force provided by the elastic force device and the gravity provided by the pressing plate slowly decrease, and then the ascending cylinder slowly ascends due to the elastic force provided by the elastic force device" in step c. The skilled in the art can realize the control of the elastic force device by adjusting the elastic force of the elastic force device and the weight of the descending cylinder and the pressing plate itself. As a preferred solution, in step c, the descending speed of the descending cylinder and the ascending speed of the ascending cylinder are each 0.5-1.5 cm per 10 minutes. As a preferred solution, in step c, the certain vacuum degree is 0.01-0.1 mpa. As a preferred solution, in step c, the time for impregnation is 0.5-2 hours.

[0038] In the process of vacuumizing and impregnation in step c of the present application, the process that "the elastic force provided by the elastic force device and the gravity provided by the pressing plate slowly decrease, and then the ascending cylinder slowly ascends due to the elastic force provided by the elastic force device" makes the carrier move due to the friction force, so that the gas in the carrier can be sufficiently sucked out by the vacuumizing device, and the impregnation liquid can be sufficiently contacted with the carrier, thereby improving the impregnation quality.

[0039] According to the present application, the impregnation method of the solid particulate catalyst is especially used for the carrier with a hardness of 40-200 N / cm.

[0040] According to the present application, in a specific embodiment, the shell and the shell cover are fixed by bolts, and preferably a sealing gasket is used between the shell cover and the shell to maintain the sealing of the shell.

[0041] In the present application, after the shell and the shell cover are tightly connected, the sealing of the shell is further checked.

[0042] In the present application, after the impregnation and the discharge of the impregnation liquid are completed, the air pressure in the shell can be restored to the normal pressure, the shell cover is opened, the elastic force device and the pressing plate are taken out, the inner container is taken out, and the discharge plate is opened, so that the impregnated material can be used in the next process.

[0043] The present application is further described below in conjunction with examples, but the scope of the present application is not limited thereto.

[0044] In the embodiment of the present application, the preparation method of the carrier is as follows:

[0045] A solid mixture of 372 g of 200-500 mesh trihydrated α-Al2O3, 112 g of 200-400 mesh pseudo-hydrated Al2O3, 3 g of MgF2 and 0.5 g of Ba(NO3)2 was mixed in a mixer and then transferred to a kneader, 90 mL of dilute nitric acid was added and kneaded to form an extrudable paste, which was extruded into a five-hole columnar body having an outer diameter of 8.0 mm, a length of 6.0 mm and an inner diameter of 1.0 mm. The five-hole columnar body was dried at 80-120°C for 10 hours to reduce the free water content to less than 10% by weight, thereby producing a shaped α-alumina carrier precursor. The precursor was then placed in an electric furnace and heated from room temperature to 1400°C over 30 hours and then held at 1400°C for 2 hours, thereby producing a white α-Al2O3 carrier. The white α-Al2O3 carrier thus produced was designated as Z, and the side pressure hardness of the carrier of the solid particulate catalyst was 100 N / cm.

[0046] In the present embodiment, the preparation method of the impregnation solution is as follows:

[0047] A stainless steel tank with stirring was charged with 30 kg of butylamine, 11 kg of 1,3-propanediamine and 37.5 kg of deionized water to obtain a mixed solution. While stirring, 65 kg of silver oxalate was slowly added to the mixed solution to completely dissolve the silver oxalate, and then 0.32 kg of potassium nitrate and 0.21 kg of calcium nitrate were added. Deionized water was added to bring the total mass of the solution to 200 kg, and the resulting solution was mixed uniformly to obtain a silver catalyst impregnation solution. The silver content of the obtained silver compound impregnation solution was 22% by weight.

[0048] Example 1:

[0049] The present embodiment 1 provides an impregnation device and an impregnation method for a solid particulate catalyst. Referring to Figure 1 A structural schematic diagram of an impregnation device for a solid particulate catalyst is shown.

[0050] The impregnation device of the solid particle catalyst comprises a shell 1, an impregnation liquid pipe 2, a jacket 3, an elastic device 4, a shell cover 5, a pressing plate 6, a vacuum pipe 7, a settling cylinder 8, an up-and-down rising cylinder 9, a discharge plate 10, and an inner container 11; the shell 1 is externally provided with the jacket 3; one end of the impregnation liquid pipe 2 and the vacuum pipe 7 are respectively communicated with the impregnation device; the other end of the impregnation liquid pipe 2 is used for connecting an impregnation liquid providing device, and the other end of the vacuum pipe 7 is used for connecting a vacuum device; the impregnation device is of a radial bed structure, the inner container 11, the rising cylinder 9, the settling cylinder 8, and the pressing plate 6 are all arranged in the shell 1; the rising cylinder 9 is located in the inner container 11, and the settling cylinder 8 is partially located in the rising cylinder 9; the pressing plate 6 is arranged on the settling cylinder 8 and connected with the rising cylinder 9 through the elastic device 4; a plurality of impregnation liquid holes are uniformly arranged on the walls of the settling cylinder 8, the rising cylinder 9, and the inner container 11 respectively, the size of the impregnation liquid holes is such that the impregnation liquid can enter and exit but the carrier of the solid particle catalyst cannot enter and exit, and the pore diameter is specifically 2 mm; the inner container 11 is provided with the discharge plate 10 at the bottom.

[0051] The impregnation method of the solid particle catalyst comprises:

[0052] a. The inner container 11 is placed in the shell 1, the rising cylinder 9 is put into the inner container 11, the carrier of the solid particle catalyst is added to a height of 15 cm, then the settling cylinder 8 is put into the rising cylinder 9, the remaining carrier of the solid particle catalyst is continuously added, and when the carrier height is flush with the upper edge of the rising cylinder 9, the pressing plate 6 is covered above the settling cylinder 8 and connected with the rising cylinder 9 through the elastic device 4 in a stretched state;

[0053] b. The shell 1 and the shell cover 5 are tightly connected through bolts with the aid of sealing pads, and the shell sealing property is checked;

[0054] c. The vacuum device draws the inside of the shell 1 to a vacuum degree of 0.05 mPa through the vacuum pipe 7, the impregnation liquid is input through the impregnation liquid pipe 2, and the impregnation liquid enters the inside of the inner container 11, the rising cylinder 9, and the settling cylinder 8 through the impregnation liquid holes; in the process of vacuumizing and impregnation, the settling cylinder 8 slowly descends at an average speed of about 2 cm per 10 minutes due to the elastic force provided by the elastic device 4 and the gravity provided by the pressing plate 6, and then the rising cylinder 9 slowly rises at an average speed of about 2 cm per 10 minutes due to the elastic force provided by the elastic device 4, in this process, the carrier moves due to the friction force, the gas in the carrier can be fully sucked out by the vacuum device, and the impregnation liquid can fully contact with the carrier; after the impregnation is completed, the air pressure in the shell 1 is restored to normal pressure, the impregnation liquid is discharged, the shell cover 5 is opened, the elastic device 4 and the pressing plate 6 are taken out, the inner container 11 is taken out, the discharge plate 10 is opened, and the impregnated carrier of the solid particle catalyst is used in the next process.

[0055] The silver catalyst CZ-1 was prepared by using the carrier sample Z15 kg, immersing for 3 hours, removing the excess silver catalyst impregnation solution by draining, and heating the impregnated carrier in an air stream at 350°C for 5 minutes, and then cooling. The silver and promoter contents in the prepared silver catalyst were analyzed, and the silver content was about 16.1% by weight. The activity and selectivity of the silver catalyst were determined by using a micro-reactor evaluation device, and the temperature and selectivity data on the 8th day of the reaction are shown in Table 1.

[0056] Example 2

[0057] The specific implementation steps were the same as those in Example 1, except that the holes in the wall of the inner container 11, the settling cylinder 8, and the rising cylinder 9 of the impregnation device were rectangular, with a length of 5 mm and a width of 2 mm.

[0058] The prepared silver catalyst was named CZ-2, and the silver and promoter contents in the prepared silver catalyst were analyzed, and the silver and promoter contents in CZ-2 were basically the same as those in CZ-1. The activity and selectivity of the silver catalyst were determined by using a micro-reactor evaluation device, and the temperature and selectivity data on the 8th day of the reaction are shown in Table 1.

[0059] Comparative Example 1

[0060] The specific implementation steps were mostly the same as those in Example 1, except that only the inner container 11 was provided, and the settling cylinder 8, the pressing plate 6, the rising cylinder 9, and the elastic device 4 were not provided.

[0061] The prepared silver catalyst was named CZ-4, and the silver and promoter contents in the prepared silver catalyst were analyzed, and the silver and promoter contents in CZ-4 were basically the same as those in CZ-1. The activity and selectivity of the silver catalyst were determined by using a micro-reactor evaluation device, and the temperature and selectivity data on the 8th day of the reaction are shown in Table 1.

[0062] Comparative Example 2

[0063] The specific implementation steps were mostly the same as those in Example 1, except that only the settling cylinder 8 and the pressing plate 6 were provided in the inner container 11, and the rising cylinder 9 and the elastic device 4 were not provided.

[0064] The prepared silver catalyst was named CZ-3, and the silver and promoter contents in the prepared silver catalyst were analyzed, and the silver and promoter contents in CZ-3 were basically the same as those in CZ-1. The activity and selectivity of the silver catalyst were determined by using a micro-reactor evaluation device, and the temperature and selectivity data on the 8th day of the reaction are shown in Table 1.

[0065] Table 1 Physical parameters of catalysts

[0066] Catalyst source Catalyst Initial reaction temperature (°C) EO (mol%) Selectivity (%) Example 1 CZ-1 222.8 2.50 85.77 Example 2 CZ-2 223.0 2.51 85.19 Comparative Example 1 CZ-4 228.9 2.49 80.89 Comparative Example 2 CZ-3 225.9 2.51 82.10

[0067] From the data in Table 1, it can be seen that the silver catalyst prepared by the impregnation device provided by the present application, when applied to the reaction process of ethylene oxidation to produce ethylene oxide, is beneficial to the dispersion of the active center and improves the catalytic performance of the active center. Compared with the catalysts CZ-4 and CZ-3 prepared by Comparative Example 1 and Comparative Example 2, the selectivity and activity of the catalysts CZ-1 and CZ-2 prepared by Experimental Example 1 and Experimental Example 2 are obviously improved. The selectivity and activity of the catalysts CZ-1 and CZ-2 are improved to a certain extent.

[0068] The above has described various embodiments of the present application, and the above description is exemplary and is not exhaustive, and is not limited to the disclosed embodiments. Many modifications and changes are obvious to those skilled in the art without departing from the scope and spirit of the described embodiments.

[0069] The endpoints of the ranges and any values disclosed herein are not limited to the precise values stated. The ranges or values should be construed to be roughly around the ranges or values. For ranges of values, the endpoints of the ranges are combinable with one another to form one or more new ranges or values not expressly disclosed. The same applies to any intervening value or values.

Claims

1. An impregnation apparatus for a solid particulate catalyst, characterized in that, The impregnation device includes: a shell (1), an impregnation liquid pipe (2), an elastic device (4), a shell cover (5), a pressure plate (6), a vacuum pipe (7), a settling cylinder (8), an ascending cylinder that runs vertically through the top and bottom (9), and an inner liner (11). One end of the impregnation liquid tube (2) and the vacuum tube (7) are respectively connected to the impregnation device; the other end of the impregnation liquid tube (2) is used to connect to the impregnation liquid supply device, and the other end of the vacuum tube (7) is used to connect to the vacuum device. The impregnation device is a radial bed structure. The inner liner (11), the rising cylinder (9), the settling cylinder (8), and the pressure plate (6) are all disposed inside the shell (1). The rising cylinder (9) is partially or entirely located in the inner liner (11), and the settling cylinder (8) is partially located in the rising cylinder (9). The pressure plate (6) covers the settling cylinder (8) and is connected to the rising cylinder (9) through the elastic device (4). The walls of the settling cylinder (8), the rising cylinder (9), and the inner liner (11) are each provided with multiple impregnation liquid holes. The size of the impregnation liquid holes allows the impregnation liquid to enter and exit while the carrier of the solid particle catalyst cannot enter or exit.

2. The impregnation apparatus for the solid particulate catalyst according to claim 1, wherein, The impregnation device is provided with a jacket (3) outside the housing (1); The impregnation device also includes a discharge plate (10) disposed at the bottom of the inner liner (11). The impregnation liquid holes are evenly distributed on the walls of the settling cylinder (8), the rising cylinder (9), and the inner liner (11).

3. The impregnation apparatus for the solid particulate catalyst according to claim 1, wherein, The impregnation liquid tube (2) and the vacuum tube (7) are arranged diagonally.

4. The impregnation apparatus for the solid particulate catalyst according to claim 3, wherein, The impregnation liquid tube (2) is located below one side of the housing (1), and the vacuum tube (7) is located above the other side of the housing (1).

5. The impregnation apparatus for the solid particulate catalyst according to claim 1, wherein, The elastic device (4) is configured to exert an upward force on the rising cylinder (9) and a downward force on the pressure plate (6) and the settling cylinder (8).

6. The impregnation apparatus for the solid particulate catalyst according to claim 1, wherein, The elastic device (4) is fixedly connected to one of the pressure plate (6) and the rising cylinder (9), and detachably connected to the other; or, The elastic device (4) is detachably connected to the pressure plate (6) and the rising cylinder (9).

7. The impregnation apparatus for the solid particulate catalyst according to claim 1, wherein, The housing cover (5) is detachably connected to the housing (1), and a sealing gasket is provided between the housing cover (5) and the housing (1).

8. A method for impregnating a solid particulate catalyst, characterized in that, The impregnation method employs the impregnation apparatus for the solid particulate catalyst according to any one of claims 1-7, and the impregnation method includes: a. Place the inner liner (11) in the shell (1), put the rising cylinder (9) into the inner liner (11), add the carrier of the solid particle catalyst to the first preset height, then put the settling cylinder (8) into the rising cylinder (9), continue to add the carrier of the solid particle catalyst to the second preset height, cover the settling cylinder (8) with the pressure plate (6), and connect the pressure plate (6) to the rising cylinder (9) through the elastic device (4) in the tension state; b. Seal the connection between the housing (1) and the housing cover (5); c. The vacuum inside the shell (1) is evacuated to a certain degree through the vacuum tube (7), and the impregnation liquid is input through the impregnation liquid tube (2). The impregnation liquid enters the inner liner (11), the rising cylinder (9), and the settling cylinder (8) through the impregnation liquid hole. During the vacuuming and impregnation process, the settling cylinder (8) slowly descends due to the elastic force provided by the elastic device (4) and the gravity provided by the pressure plate (6), and the rising cylinder (9) slowly rises due to the elastic force provided by the elastic device (4). After the impregnation is completed, the impregnation liquid and the carrier of the solid particle catalyst are discharged.

9. The impregnation method for the solid particulate catalyst according to claim 8, wherein, In step a, the height h of the solid particle catalyst carrier covering the bottom of the inner liner (11) is 5cm≤h≤0.5*height of the inner liner (11).

10. The impregnation method for a solid particulate catalyst according to claim 8, wherein, In step c, the descent speed of the settling cylinder (8) and the ascent speed of the rising cylinder (9) are each 0.5~1.5cm every 10 minutes.

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