Multi-stage horizontal fluidized bed reactor for activating Fischer-Tropsch synthesis catalyst and continuous activation process

Abstract

The invention discloses a multistage horizontal fluidized bed reactor for activating a Fischer-Tropsch synthesis catalyst and a continuous activation process. A main body of the multi-stage horizontal fluidized bed reactor is a narrow-edge horizontal container with an arc, and 2-4 gas distribution plates are arranged along the axial direction of the reactor to divide the reactor into 2-4 stages of dense-phase reaction zones; a flap valve is arranged between the adjacent reaction areas to serve as a catalyst channel; an activated gas inlet pipe is arranged at the lower part of the gas distribution plate, and activated gas is continuously blown into the reaction area through the gas distribution plate; a powder Fischer-Tropsch synthesis catalyst is continuously fed through a catalyst feeding tank and flows through a multi-stage reaction area step by step from top to bottom, and the catalyst and activation gas are subjected to a reduction reaction to be activated. Compared with a common fluidized bed reactor, the continuous flow of the powder Fischer-Tropsch synthesis catalyst in the multistage horizontal fluidized bed reactor can effectively reduce backmixing, the retention time distribution is narrower, the activation quality of catalysts with different particle sizes is more uniform, and the Fischer-Tropsch reaction product yield is improved.

Description

Technical Field

[0001] The invention relates to the technical field of Fischer-Tropsch synthesis, and in particular to a multi-stage horizontal fluidized bed reactor and a continuous activation process for activating a Fischer-Tropsch synthesis catalyst. Background Art

[0002] As the main method of indirect coal liquefaction, Fischer-Tropsch synthesis uses iron, cobalt or other metal catalysts to catalyze the reaction of hydrogen and carbon monoxide (synthesis gas) under appropriate reaction conditions to produce synthetic oil and various chemicals. As an important way to cleanly utilize coal, Fischer-Tropsch synthesis can reduce the consumption of crude oil in the production of liquid fuels or chemicals, alleviating my country's oil shortage problem.

[0003] Among the catalysts used in Fischer-Tropsch synthesis, iron-based catalysts are the mainstream. Iron-based catalysts have a wide range of raw materials, are inexpensive, and have high water-gas shift reaction activity when used to catalyze coal-based synthesis gas with a low hydrogen-to-carbon ratio.

[0004] Since fresh iron-based Fischer-Tropsch synthesis catalysts do not have Fischer-Tropsch synthesis activity, the iron-based catalyst needs to be activated before the Fischer-Tropsch synthesis reaction to change it from an oxidized state to a phase with stable activity. The activity of the iron-based catalyst has an important influence on the product selectivity and yield of the Fischer-Tropsch synthesis, so the activation quality of the iron-based catalyst has become a prerequisite for the Fischer-Tropsch synthesis reaction to achieve ideal operating results.

[0005] CN116920961A discloses a Fischer-Tropsch synthesis catalyst activation method and a Fischer-Tropsch synthesis method: during the reduction activation process, the superficial gas velocity of the reducing gas is increased in a step-by-step manner, so that particles of different particle sizes in the catalyst can achieve differentiation in activation time, and the activated catalyst is separated from the activation environment in time. The activation method can effectively solve the problem of over-activation of small particles, improve the overall activation effect of the catalyst, and reduce wear. The catalyst activated according to this method can bring higher carbon monoxide conversion and lower by-product selectivity in the Fischer-Tropsch synthesis reaction.

[0006] CN116174056A discloses a device and method for continuously activating a Fischer-Tropsch synthesis catalyst: a fresh catalyst is gradually moved from the top to the bottom of the device in a moving bed reactor, and an activation gas is introduced from the bottom to contact the catalyst in countercurrent. The temperature of the fresh catalyst is 120-180°C, the pressure of the first activation reaction is 2-3MPa, and the temperature is programmed along the moving direction of the catalyst, from 150°C-220°C to 240°C-450°C at a heating rate of 15-25°C / h, and the temperature is kept for 2-8h after reaching the temperature. The method utilizes the continuous feeding and continuous discharging characteristics of the moving bed reactor itself to improve the intermittent activation process into a continuous activation process, which not only ensures the catalyst activation performance and production capacity, but also greatly reduces the wear of the catalyst due to the small back mixing and low linear velocity of the moving bed.

[0007] CN107149948A discloses a reduction method for a Fischer-Tropsch synthesis iron-based catalyst: in the presence of a reducing gas, the Fischer-Tropsch synthesis iron-based catalyst particles are subjected to a programmed temperature reduction in a fixed fluidized bed reactor. The method allows the Fischer-Tropsch synthesis iron-based catalyst to undergo a stable reduction reaction, reduces the influence of water and the influence on the catalyst strength, and the reduced catalyst is not broken during Fischer-Tropsch synthesis, has high catalyst activity, low carbon dioxide selectivity, and low low-carbon hydrocarbon selectivity.

[0008] However, in the above technical solutions, CN116920961A and CN107149948A adopt intermittent activation operation mode, and the activation process needs to go through the steps of adding materials, replacing gas, program pressurization and heating, program cooling and pressure reduction, and discharging. The problem of insufficient processing capacity caused by intermittent operation is more prominent in industrial devices. CN116174056A adopts a moving bed device to realize the continuous feeding and discharging of catalysts, but it is difficult for the moving bed device to control the uniform downward movement of solid particles. If the radial distribution of the bed layer is uneven during falling, it will affect the activation quality of the catalyst particles, and further affect the reaction efficiency and product quality of Fischer-Tropsch synthesis. Summary of the invention

[0009] The purpose of the present invention is to overcome the defects of the existing Fischer-Tropsch synthesis iron-based catalyst activation technology, such as low intermittent operation efficiency, long activation cycle and uneven activation quality during moving bed continuous operation, and provide a multi-stage horizontal fluidized bed reactor and a continuous activation process for activating Fischer-Tropsch synthesis catalysts. The activation device and the continuous activation process can ensure the effect of high-quality Fischer-Tropsch synthesis catalysts while effectively improving the processing efficiency of the activation link and shortening the activation cycle.

[0010] In order to achieve the above-mentioned object, the first aspect of the present invention provides a multi-stage horizontal fluidized bed reactor for activating a Fischer-Tropsch synthesis catalyst, comprising: a horizontal reactor shell (a narrow-sided horizontal container with a circular arc), one or more gas distribution plates, activation gas inlet pipes having the same number as the gas distribution plates, three or more vertical baffles, one or more flap valves, a catalyst feed trough, a catalyst discharge trough, a gas sideline outlet pipe and a gas top outlet pipe;

[0011] The horizontal reactor shell serves as a container for the catalyst particle activation reaction, ensuring that the catalyst particles have a certain residence time in the device;

[0012] The gas distribution plates are arranged at different heights of the horizontal reactor shell to evenly distribute the activated gas to form a continuous fluidized zone and divide the internal space of the horizontal reactor shell into multiple layers of dense phase reaction zones;

[0013] The activated gas inlet pipe is arranged below the gas distribution plate, and is used to transport the activated gas into the horizontal fluidized bed reactor body and provide fluidization power; the activated gas inlet pipe is connected to the gas distribution plate through a transition pipe, and the transition pipe has a structure that is wide at the top and narrow at the bottom, so as to evenly introduce the activated gas into the gas distribution plate.

[0014] The vertical baffle is arranged above each gas distribution plate to further divide each layer of dense phase area so as to reduce the back mixing of particles;

[0015] The flap valve is arranged at the end of each gas distribution plate to control the rate at which particles fall to the next dense phase reaction zone;

[0016] The catalyst inlet and outlet trough is used to add the catalyst to be activated into the fluidized bed reactor and to discharge the activated catalyst particles out of the fluidized bed reactor;

[0017] The gas sideline outlet pipe is arranged at the top of other dense phase reaction zones except the top dense phase reaction zone, and further, is arranged on the side of the horizontal fluidized bed reactor body, with a height between the gas distribution plate and the activated gas pipeline, and is used to discharge part of the gas of each layer to prevent the apparent gas inside the horizontal fluidized bed reactor from being too large;

[0018] The gas top outlet pipe is used for discharging the fluidizing gas in the device;

[0019] Preferably, the catalyst feed trough is arranged on one side of the horizontal fluidized bed reactor body and is located at a height position of 3 / 4 to 4 / 5 of the horizontal fluidized bed reactor body, and the catalyst particle discharge trough is arranged on the other side of the horizontal fluidized bed reactor body and is located at a height position of 1 / 5 to 1 / 4 of the horizontal fluidized bed reactor body.

[0020] Preferably, the number of the gas distribution plates is 2 to 4;

[0021] Preferably, the number of vertical baffles per layer is 3, and the height of the vertical baffle in the middle is 1 / 3 to 1 / 4 of the height of the vertical baffles on both sides;

[0022] The second aspect of the present invention provides a continuous activation process for a Fischer-Tropsch synthesis catalyst, which is implemented based on a multi-stage fluidized bed reactor and includes the following steps: continuously adding the catalyst to be activated from a catalyst feed trough to the multi-stage fluidized bed reactor, and continuously inputting the activation gas into the multi-stage fluidized bed reactor through an activation gas inlet pipe for activation, the activated catalyst is continuously output from a catalyst discharge trough, and the activated gas is discharged from the gas top outlet pipe and the side line outlet pipe.

[0023] According to the process of the present invention, optionally, the activation gas consists of hydrogen, carbon monoxide or synthesis gas.

[0024] According to the process of the present invention, preferably, the catalyst to be activated is an iron-based catalyst commonly used in the Fischer-Tropsch synthesis process, and further preferably, the particle size of the catalyst ranges from 0 to 130 μm.

[0025] According to the process of the present invention, preferably, the activation pressure ranges from 0.5 to 2 MPa.

[0026] According to the method of the present invention, preferably, the activation temperature ranges from 260 to 280°C.

[0027] According to the method of the present invention, preferably, the superficial velocity of the activated gas ranges from 0.3 to 0.9 m / s.

[0028] According to the method of the present invention, preferably, the average residence time of the catalyst is 4 to 12 hours.

[0029] According to the method of the present invention, preferably, the catalyst circulation amount / catalyst storage amount ratio ranges from 1 / 12 to 1 / 4 h -1 .

[0030] Compared with the prior art, the present invention has the following advantages:

[0031] 1) Compared with the intermittent process, the continuous feeding and discharging process does not require frequent adjustment of parameters such as the gas inlet rate, reactor temperature and reaction pressure, and reduces the complex processes such as frequent opening and closing of valves for feeding and unloading, programmed heating and cooling, thereby simplifying the process and shortening the entire activation cycle, reducing the fluctuation of device operation, and improving the activation efficiency and processing volume per unit time.

[0032] 2) The use of a multi-stage horizontal fluidized bed structure can greatly increase the processing capacity of the device and reduce the length of the device compared to the traditional horizontal fluidized bed. The catalyst reduction degree after activation in the multi-stage horizontal fluidized bed reactor is uniform, the degree of backmixing is small, and catalyst particles of different particle sizes have similar residence time distribution and reduction degree, reducing the problem of different reduction degrees of outlet particles in the moving bed continuous process.

[0033] In the subsequent specific embodiments of the present invention, the above features will be further explained in detail. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] The drawings constituting a part of the present application are used to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the drawings:

[0035] Figure 1 A cross-sectional view of the internal structure of a multi-stage horizontal fluidized bed reactor used for Fischer-Tropsch synthesis catalyst activation is shown.

[0036] Figure 2 A schematic structural diagram of a multi-stage horizontal fluidized bed reactor for Fischer-Tropsch synthesis catalyst activation is shown.

[0037] Figure 3 A schematic diagram of the structure after the top is removed of a multi-stage horizontal fluidized bed reactor used for Fischer-Tropsch synthesis catalyst activation is shown.

[0038] Figure 4 A schematic diagram of the structure of the gas distribution plate and the activated gas inlet pipe inside the multi-stage horizontal fluidized bed reactor is shown.

[0039] The above drawings include the following reference numerals:

[0040] 1-catalyst feed trough; 2-vertical baffle; 3-flap valve; 4-activated gas inlet pipe; 5-gas side line outlet pipe; 6-gas distribution plate; 7-catalyst discharge trough; 8-gas top outlet pipe; DETAILED DESCRIPTION

[0041] The present invention is further described below in conjunction with the embodiments and drawings, but the present invention is not limited to the listed embodiments, but also includes equivalent improvements and modifications of the technical solutions defined in the claims attached to the present application.

[0042] Example 1

[0043] like Figures 1 to 4The multi-stage horizontal fluidized bed reactor for Fischer-Tropsch synthesis catalyst activation shown in the figure has a length and height of 3.2 m, a width of 0.8 m, an operating temperature of 280°C, an operating pressure of 1.5 MPa, an activation gas superficial velocity of 0.6 m / s, a catalyst particle size range of 0 to 130 μm, a catalyst storage of 8 t, and a catalyst circulation volume / catalyst storage ratio of 0.125 h -1 . Inside the multi-stage horizontal fluidized bed reactor, three gas distribution plates 6 are arranged along the bed height of 0.8m, 1.6m and 2.4m, respectively. The upper and lower distribution plates are arranged in a staggered manner, and a flap valve is arranged behind each distribution plate. The catalyst to be activated is continuously added to the horizontal fluidized bed reactor device from the catalyst feed trough 1, and is first accumulated on the gas distribution plate 6 located at the bed height of 2.4m under the action of gravity, and then the particle bed will slowly move to the end of the distribution plate over time. When a certain amount of particles are accumulated above the flap valve, the valve will open to discharge the particles to the next layer of gas distribution plate 6 for re-accumulation, and finally the particles move to the end of the bottom distribution plate of the horizontal fluidized bed and are discharged through the catalyst discharge trough 7. Three sets of activation gas inlet pipes 4 are also arranged, all located below each gas distribution plate 6. The activation gas is continuously input into the horizontal fluidized bed device through the activation gas inlet pipe 4, and is evenly distributed through the gas distribution plate 6 to form a continuous and uniform fluidized area. In the fluidized area, the catalyst particles contact the gas and are fully reacted and activated. In order to reduce the back mixing of particles, three vertical baffles 2 are arranged along the gas distribution plate 6, and the vertical baffle 2 in the middle position is in contact with the gas distribution plate 6, while the vertical baffles 2 near the two sides of the gas distribution plate 6 are located above the gas distribution plate 6, and the three vertical distribution plates are arranged in a staggered manner. In order to prevent the gas from overflowing from the flap valve between the upper and lower layers, causing the gas velocity at the flap valve to be too high and making it difficult for the particles to fall, a gas sideline outlet pipe 5 is arranged on the side of each layer of the horizontal fluidized bed reactor body at a height between the gas distribution plate 6 and the activated gas inlet pipe 4 to divert and discharge part of the gas. The remaining undiverted gas will rise to the upper layer through the flap valve 3 when the flap valve 3 is opened, and finally be discharged through the gas top outlet pipe 8. The definition of the degree of activation is shown in the following formula.

[0044] Formula 1. Definition of activation degree

[0045]

[0046] From the results in Table 1, it can be seen that the average residence times of catalyst particles of different particle sizes are relatively close, all close to the average residence time of the full particle size of 8.2h, and the activation degree fluctuates around 0.97.

[0047] Table 1. Activation results of Example 1

[0048]

[0049] Comparative Example 1

[0050] The process conditions and reactor size are the same as those of Example 1, except that there is no vertical baffle 2 above each layer of gas distribution plate 6, that is, the particle bed is not divided along the gas distribution plate 6, and the particles will move radially along the gas distribution plate 6 through the flap valve 3 and fall to the next layer of gas distribution plate 6 and finally be discharged through the catalyst discharge trough 7. From the results in Table 2, it can be seen that the average residence time of all particles in Comparative Example 1 without vertical baffle 4 is 8.3h, the average residence time of small particles is 8.7h, the average residence time of medium particles is 8.4h, the average residence time of large particles is 7.9h, and the average residence time of coarse particles is 7.4h. Since the radial movement of particles is intensified after the vertical baffle is not added, the degree of back mixing increases, especially the back mixing of small particles is more serious, which will extend the residence time of small particles. Moreover, the smaller the particle size, the easier it is to be distributed in the upper layer of the bed. Therefore, it is more difficult for particles with small particle size to pass through the flap valve 3 and fall to the next layer of gas distribution plate 6, thereby further increasing the residence time. Particles with large particle size are more likely to pass through the flap valve 3 and fall to the next layer of gas distribution plate 6, thereby significantly shortening the residence time. This leads to slightly different activation degrees of catalyst particles of different particle sizes, and the activation quality is uneven compared with Example 1.

[0051] Table 2. Activation results of comparative example 1

[0052]

[0053] Comparative Example 2

[0054] The process conditions and reactor size are the same as those in Example 1, except that the number of vertical baffles 2 above each layer of gas distribution plate 6 is 5, and the arrangement is short plate-long plate-short plate-long plate-short plate, wherein the short plate fits the gas distribution plate 6, and the long and short plates are staggered. From the results in Table 3, it can be seen that the average residence time of all particle sizes is 8.4h, the average residence time of small particles is 7.9h, the average residence time of medium particles is 8.1h, the average residence time of large particles is 8.6h, and the average residence time of coarse particles is 8.9h. By comparing the average residence time and activation degree of Example 1 and Comparative Example 2, it can be seen that the average residence time of all particle sizes in the multi-stage horizontal fluidized bed reactor with 5 vertical baffles 2 in each dense phase reaction zone is longer, and the average residence time of particles with larger particle sizes is extended to a greater extent, which shows that increasing the number of vertical baffles 2 will reduce the back mixing of particles but will increase the dead zone range of particles, resulting in more particles staying too long in the reactor.

[0055] Table 3. Activation results of comparative example 2

[0056]

[0057] Comparative Example 3

[0058] The process conditions are the same as those in Example 1, except that there is only one gas distribution plate inside the reactor, the number of vertical baffles on the gas distribution plate is 7, and the catalyst circulation amount / catalyst storage amount ratio is 0.125h -1 , the horizontal fluidized bed reactor is 7.2m long, 2.0m high and 0.8m wide. From the results in Table 4, it can be seen that the average residence time of all particle sizes is 8.3h, the average residence time of small particles is 7.8h, the average residence time of medium particles is 7.9h, the average residence time of large particles is 8.5h, and the average residence time of coarse particles is 8.8h. Comparing the average residence time and activation degree of Example 1 and Comparative Example 3, it can be seen that the average residence time of all particle sizes in the conventional single-stage horizontal fluidized bed reactor is longer, and the average residence time of particles with larger particle sizes is extended to a greater extent. This is because the single-stage horizontal fluidized bed requires a longer length than the multi-stage horizontal fluidized bed at the same processing capacity, and more baffles are required to divide the dense phase section to reduce the particle backmixing phenomenon, but it brings the problem of dead zone, resulting in more particles staying in the reactor for too long.

[0059] Table 4. Activation results of comparative example 3

[0060]

[0061] Example 2

[0062] The process conditions are the same as those in Example 1, except that the catalyst storage is 1 t and the catalyst circulation volume / catalyst storage ratio is 0.142 h -1 The length and height of the multi-stage horizontal fluidized bed reactor are both 2.0m, and the width is 0.5m. From the results in Table 5, it can be seen that after reducing the catalyst processing capacity and the reactor size, the average residence time of all particles is 7.1h, the average residence time of small particles is 6.8h, the average residence time of medium particles is 6.9h, the average residence time of large particles is 7.2h, and the average residence time of coarse particles is 7.4h. The reduction degree of each particle size is relatively close.

[0063] Table 5. Activation results of Example 2

[0064]

[0065] Example 3

[0066] The process conditions are the same as those in Example 1, except that the operating pressure is 0.5 MPa and the catalyst circulation volume / catalyst storage volume ratio is 0.071 h -1The length and height of the multi-stage horizontal fluidized bed reactor are both 4.6m and 1.2m wide. From the results in Table 6, it can be seen that after reducing the catalyst processing capacity and the reactor size, the average residence time of the full particle size is 14.4h, the average residence time of small particles is 13.4h, the average residence time of medium particles is 13.8h, the average residence time of large particles is 14.6h, and the average residence time of coarse particles is 15.2h. The reduction degree of each particle size is relatively close. By comparing the average residence time and activation degree of Example 1 and Example 3, it can be seen that reducing the operating pressure requires a larger device size, while reducing the mass transfer between the gas and solid phases, thereby extending the average residence time required for full activation.

[0067] Table 6. Activation results of Example 3

[0068]

[0069] Obviously, the above embodiments of the present invention are merely examples for clearly explaining the present invention, and are not intended to limit the implementation methods of the present invention. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. It is impossible to list all implementation methods here. All obvious changes or modifications derived from the technical solution of the present invention are within the spirit scope of the present invention.

Claims

1. A multi-stage horizontal fluidized bed reactor for activating a Fischer-Tropsch synthesis catalyst, characterized in that: The horizontal fluidized bed reactor comprises: Horizontal reactor shell; A catalyst feed trough (1), arranged at the upper part of the side wall of the horizontal reactor shell, for adding the catalyst to be activated into the horizontal reactor shell; A plurality of gas distribution plates (6) are arranged at different heights inside the shell of the horizontal reactor, and are used to evenly distribute the activated gas to form a continuous fluidized zone, while dividing the internal space of the shell of the horizontal reactor into multiple layers of dense phase reaction zones; An activation gas inlet pipe (4) is arranged below each gas distribution plate and is used to transport activation gas into the shell of the horizontal reactor and provide fluidization power; A vertical baffle (2) is arranged above each gas distribution plate and is used to further divide each layer of dense phase reaction zone; A flap valve (3) is arranged at the gap between each gas distribution plate and the side wall of the horizontal reactor shell, and is used to control the rate at which particles fall to the next dense phase reaction zone; A catalyst discharge chute (7), arranged on the bottom of the side wall of the horizontal reactor shell, for discharging activated catalyst particles out of the horizontal reactor shell; A gas sideline outlet pipe is configured at the top of other dense phase reaction zones except the top dense phase reaction zone, and is used to discharge part of the gas; The gas top outlet pipe (8) is arranged at the top of the horizontal reactor shell and is used for discharging the fluidizing gas in the device.

2. The multi-stage horizontal fluidized bed reactor according to claim 1, characterized in that: The catalyst feed trough is configured at a height of 3 / 4 to 4 / 5 of the height of the multi-stage horizontal fluidized bed reactor.

3. The multi-stage horizontal fluidized bed reactor according to claim 1, characterized in that: The number of the gas distribution plates is 2 to 4; The two adjacent upper and lower gas distribution plates are staggered.

4. The multi-stage horizontal fluidized bed reactor according to claim 1, characterized in that: The activated gas inlet pipe (4) and the gas distribution plate (6) are connected via a transition pipe.

5. The multi-stage horizontal fluidized bed reactor according to any one of claims 1 to 4, characterized in that: The gas distribution plate located at the uppermost layer is located below the catalyst feed slot; Preferably, the distance between the topmost gas distribution plate and the catalyst feed slot is 1 / 10 to 1 / 8 of the height of the multi-stage fluidized bed reactor, and the distance between two adjacent gas distribution plates is 1 / 8 to 1 / 5 of the height of the multi-stage horizontal fluidized bed reactor.

6. The multi-stage horizontal fluidized bed reactor according to any one of claims 1 to 4, characterized in that: The number of the vertical baffles is preferably 3, and the interval between two adjacent vertical baffles is 1 / 4 to 1 / 5 of the length of the gas distribution plate, and the distribution is short plate-long plate-short plate alternating staggered distribution; Furthermore, the length of the short plate is 1 / 3 to 1 / 4 of the long plate, and the short plate is in close contact with the gas distribution plate.

7. The multi-stage fluidized bed reactor according to any one of claims 1 to 4, characterized in that: The number of the gas side line outlet pipes is the number of the gas distribution plates minus one, each gas side line outlet pipe is arranged at a height between the gas distribution plate and the middle position of the activated gas pipeline, and no gas side line outlet pipe is arranged below the lowest gas distribution plate.

8. A continuous activation process for activating a Fischer-Tropsch synthesis catalyst using a multi-stage fluidized bed reactor according to any one of claims 1 to 7, characterized in that: The following steps are involved: The catalyst to be activated is continuously added to the multi-stage fluidized bed reactor from the catalyst feed tank (1), and the activation gas is continuously input into the multi-stage fluidized bed reactor through the activation gas inlet pipe (4) for activation. The activated catalyst is continuously output from the catalyst discharge tank (7), and the activated gas is discharged from the gas top outlet pipe (8) and the side line outlet pipe (5).

9. The continuous activation process according to claim 8, characterized in that: The activation pressure is 0.5-2MPa, the activation temperature is 260-280℃, the superficial velocity of the activation gas is 0.3-0.9m / s, the average residence time of the catalyst is 4-12h, and the catalyst circulation volume / catalyst storage volume ratio ranges from 1 / 12 to 1 / 4h. -1 .

10. The continuous activation process according to claim 9, characterized in that: The activation gas rate introduced into each gas distribution plate is equal.

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