A multifunctional coal gas desulfurization catalyst / adsorbent performance evaluation device and method

Abstract

The present invention discloses a multifunctional coal gas fine desulfurization catalyst / adsorbent performance evaluation device and method, belonging to the technical field of coal gas fine desulfurization. The device of the present invention includes a coal gas purification system, a regeneration and analysis gas system, a purge and release system, a reaction parameter monitoring system and an automatic control system. The system flow path is reorganized by controlling the valve switch through the automatic control system, and the design of the hydrolysis and adsorption integrated tower is used to realize the switching of two mainstream coal gas fine desulfurization processes. It has the function of evaluating the effects of various types of fine desulfurization catalysts and adsorbents under the conditions of two fine desulfurization processes, and the function of evaluating the effect of coal gas organic sulfur hydrolysis catalyst and the desulfurization efficiency of the whole process of fine desulfurization process. It also has the function of analyzing and exploring the optimal process range of fine desulfurization catalysts and adsorbents under different fine desulfurization processes and different coal gas conditions.

Description

Technical Field

[0001] The invention belongs to the technical field of coal gas desulfurization, and more specifically, relates to a multifunctional coal gas desulfurization catalyst / adsorbent performance evaluation device and method. Background Art

[0002] In the steel industry, it has become a new way to control pollutant emissions by controlling the source of SO2. For the treatment of flue gas from terminal gas-fired furnaces such as heating furnaces and hot blast furnaces, the current common method is to carry out fine desulfurization of the source gas. By controlling the sulfide content in the source gas, the SO2 in the flue gas emitted after combustion can be made to meet the standards. Since the sulfides in the gas are mainly composed of inorganic sulfur (H2S) and organic sulfur (COS, CS2, etc.), the two sulfides must be removed separately in the process of fine desulfurization of the gas. Common technical routes are organic sulfur hydrolysis + inorganic sulfur dry process and organic-inorganic integrated adsorption removal and regeneration process.

[0003] The removal process of inorganic sulfur (H2S) is relatively mature, but the treatment technology of organic sulfur is still under development. At present, there are devices for detecting the conversion efficiency of hydrolyzing agents, but their functions are relatively simple and can only detect the conversion efficiency of hydrolyzing agents under working conditions. They cannot meet the evaluation of the comprehensive desulfurization effect of the hydrolysis + dry process, nor can they meet the conversion efficiency of the catalyst / adsorbent of the organic-inorganic integrated adsorption process and the detection and evaluation of the desulfurization efficiency of the coal gas fine desulfurization system.

[0004] After searching, there are related patents about the device and method for evaluating catalyst performance. For example, the patent document with Chinese patent authorization number CN216082636U discloses a catalyst performance evaluation device. For another example, the patent documents with Chinese patent authorization numbers CN212391449U, CN212391448U, CN215179965U, CN111579708B disclose coal gas desulfurization catalyst performance evaluation devices. Although there are many devices and methods for evaluating catalyst performance, their basic functions are relatively simple. However, there are relatively few devices and methods for evaluating the effect of coal gas fine desulfurization catalysts. Only a few are for carbonyl sulfide hydrolysis catalyst effect evaluation devices, or only for the catalyst performance evaluation of a certain process. It is difficult to use them to evaluate the effects of catalysts and adsorbents under a variety of fine desulfurization process conditions, to evaluate the effect of organic sulfur hydrolysis catalysts, and to evaluate the desulfurization efficiency of the entire fine desulfurization process. Therefore, it is urgently necessary to develop an evaluation device with a simple structure, comprehensive functions, and easy operation to improve the current situation of single function and imperfect evaluation methods of existing coal gas fine desulfurization catalyst evaluation devices. Summary of the invention

[0005] 1. Problem to be solved

[0006] The main purpose of the present invention is to solve the problems of single function and imperfect evaluation method of the current evaluation devices for the adsorbent / catalyst effect of coal gas fine desulfurization and the comprehensive desulfurization efficiency of the mainstream coal gas fine desulfurization process, and to design a set of multifunctional coal gas fine desulfurization catalyst / adsorbent effect evaluation device and method by organically combining the hydrolysis + dry fine desulfurization process and the organic-inorganic integrated adsorption fine desulfurization process.

[0007] 2. Technical solution

[0008] In order to solve the above problems, the technical solution adopted by the present invention is as follows:

[0009] The present invention provides a multifunctional coal gas desulfurization catalyst / adsorbent performance evaluation device, comprising:

[0010] The coal gas purification system is used to remove sulfides from the coal gas;

[0011] Regeneration and analysis gas system, used to analyze and regenerate the failed adsorbent in the adsorption tower;

[0012] The purge and release system is used to purge and replace the gas inside the equipment and pipelines of the entire device;

[0013] Reaction parameter monitoring system, used to detect the changes of various reaction parameters during the reaction process;

[0014] The automatic control system is used for the overall automatic control of the device, including multiple control functions such as function switching, electric control flow valve opening control, reaction parameter control and realization of various functions.

[0015] As a further preferred embodiment of the present invention, the coal gas purification system of the present invention comprises a water decomposition adsorption regeneration integrated tower, an adsorption regeneration integrated tower and a coal gas blower, and the outer dimensions and internal filling volume of the water decomposition adsorption regeneration integrated tower and the adsorption regeneration integrated tower are designed to be consistent. Among them:

[0016] The design of the adsorption regeneration integrated tower is:

[0017] The integrated tower is an upright container, adopts a fixed bed vertical channel design, and the adsorbent bed is filled with adsorbent materials; the adsorption tower is designed so that the gas flows from top to bottom and the analytical gas flows from bottom to top, and the gas is discharged into the gas network through the gas blower; it is designed according to the requirement of 100% gas volume under the gas design working condition, and the design pressure is 0.1MPa; the external design of the adsorption and regeneration integrated tower is equipped with an insulation layer, a desulfurization pipeline inlet and outlet, a regeneration pipeline inlet and outlet, a material change door for adsorbent filling in the tower, etc., and the adsorbent is replaced through the material change door; an adsorbent support structure is provided inside, and a gas uniform distribution baffle is set at the desulfurization inlet to make the gas entering the adsorption layer evenly distributed, and a reaction parameter detection probe interface is designed in the tower.

[0018] The design of the hydrolysis adsorption regeneration integrated tower is:

[0019] The hydrolysis adsorption regeneration integrated tower is equipped with an electric heating system, which can control the temperature of the filling material inside the tower and the change of temperature parameters during the hydrolysis reaction (the temperature control range is 20°C to 300°C). Other parameters remain consistent with the adsorption regeneration integrated tower.

[0020] The gas blower is designed as:

[0021] The full pressure of the gas fan must meet the system pressure drop requirement and leave a certain margin; the fan adopts a centrifugal fan with an operating temperature of 60-300℃ and an explosion-proof motor; the fan outlet is equipped with a check valve and soft connection, and the noise in the fan noise area meets the national standard requirements. The fan should operate at the highest efficiency point, and the fan should have an almost flat efficiency characteristic curve to ensure that the unit has the best efficiency under various loads during operation. The fan is equipped with an electric motor, a common chassis (including shock-absorbing pads), a corrugated expansion joint, a counter flange, a coupling guard, a transmission box, etc.

[0022] Connection method:

[0023] like Figure 1 As shown, the gas inlets of the water decomposition adsorption regeneration integrated tower and the adsorption regeneration integrated tower are both connected to the outlet end of the raw gas pipeline, and an electric control flow valve S04 is provided on the pipeline at the gas inlet end of the water decomposition adsorption regeneration integrated tower, and an electric control flow valve S06 is provided on the pipeline at the gas inlet end of the adsorption regeneration integrated tower.

[0024] The gas outlets of the two towers are connected to the gas blower through pipelines, and the gas outlet of the water decomposition adsorption regeneration integrated tower is also connected to the gas inlet of the adsorption regeneration integrated tower through a separate pipeline. An electric control flow valve S08 is provided on the pipeline at the gas outlet end of the water decomposition adsorption regeneration integrated tower, an electric control flow valve S10 is provided on the pipeline connecting the water decomposition adsorption regeneration integrated tower and the adsorption regeneration integrated tower, and an electric control flow valve S12 is provided on the pipeline connected to the gas blower of the water decomposition adsorption regeneration integrated tower. An electric control flow valve S13 is provided on the pipeline at the gas outlet end of the adsorption regeneration integrated tower.

[0025] The gas blower is arranged at the main outlet of the device. The blower pressurizes the purified gas in the system and sends it to the gas network. The pressurization pressure can be adjusted according to the network pressure.

[0026] As a further preferred embodiment of the present invention, the regeneration and analysis system is connected to the gas purification system through a pipeline, and is used to analyze and regenerate the failed adsorbent in the water decomposition adsorption regeneration integrated tower and the adsorption regeneration integrated tower. Specifically, the regeneration and analysis system is provided with an electric heater, the air inlet of the electric heater is connected to the raw gas pipeline through a pipeline, and the pipeline is provided with an electric control flow valve S03, the air outlet of the electric heater is connected to the regeneration and analysis gas inlet of the water decomposition adsorption regeneration integrated tower through a pipeline, and the pipeline is provided with an electric control flow valve S09, and the air outlet of the electric heater is also connected to the regeneration and analysis gas inlet of the adsorption regeneration integrated tower through a pipeline, and the pipeline is provided with an electric control flow valve S14.

[0027] The regeneration gas outlet of the hydrolysis adsorption regeneration integrated tower and the regeneration gas outlet of the adsorption regeneration integrated tower are both connected to the gas blower through pipelines, and an electric control flow valve S05 is provided on the pipeline at the regeneration gas outlet end of the hydrolysis adsorption regeneration integrated tower, and an electric control flow valve S07 is provided on the pipeline at the regeneration gas outlet end of the adsorption regeneration integrated tower.

[0028] The electric heater can heat the coal gas or nitrogen to the adsorbent regeneration temperature (determined by the type of adsorbent). The heated hot gas is transported through a pipeline to the tower that needs to be regenerated to analyze and regenerate the adsorbent. This system and the coal gas purification system share a gas blower to transport the analyzed gas to the pipeline network.

[0029] More optimally, the electric heater in the present invention is an explosion-proof pipe heater with an operating temperature of 60-300°C and a working pressure of 12 kPa. The outer shell and the inner bore are both designed with stainless steel. The pipe heater is composed of multiple tubular electric heating elements, a cylinder, a guide plate and the like. The tubular electric heating element is a metal tube in which a high-temperature resistance wire is placed, and the gap is tightly filled with crystalline magnesium oxide powder with good insulation and thermal conductivity. A guide baffle is installed in the cylinder to allow the gas to be heated evenly during circulation.

[0030] As a further preferred embodiment of the present invention, the purge and release system is provided with a back-blowing gas pipeline, which is connected to the air inlet end of the raw gas pipeline, and an electrically controlled flow valve S01 is provided on the back-blowing gas pipeline. When the device is stopped, the flow valve S01 is opened to introduce nitrogen to purge the internal pipelines, adsorption towers, blowers, electric heaters and other equipment of the system, and the purge gas is then discharged into the atmosphere through the rear end of the gas blower or directly sent back to the pipe network. The opening and closing of the flow valves provided at various locations during the purge process are controlled by an automatic control system.

[0031] As a further preferred embodiment of the present invention, the reaction parameter monitoring system is composed of an online sulfide detector, a reaction parameter monitoring table, a sampling port and related pipelines. The automatic control system includes a main control computer, a reaction parameter detection controller and an electric control flow valve. The online sulfide detector is connected to the sampling port at the air inlet of the raw gas pipeline through a sampling gas pipeline (the sampling gas pipeline is provided with an electric control flow valve S02); on the other hand, it is connected to the sampling port at the air outlet of the gas purification system and the sampling port at the air outlet of the regeneration analysis system through a sampling gas pipeline, wherein the sampling gas pipeline connected to the air outlet of the gas purification system is provided with electric control flow valves S11 and S15, and the sampling gas pipeline connected to the air outlet of the regeneration analysis system is provided with an electric control flow valve S16. In addition, the sulfide online detector is also electrically connected to the main control computer. Through the setting of the sulfide online detector, the sulfide in the coal gas at different reaction stages can be detected online. The detection components include H2S, COS, CS2, CO, etc., and the detection results can also be sent to the main control computer in real time for storage.

[0032] The signal input end of the reaction parameter detection controller is electrically connected to the water decomposition adsorption regeneration integrated tower and the adsorption regeneration integrated tower of the gas purification system, and the signal output end of the reaction parameter detection controller is electrically connected to the main control computer through the reaction parameter monitoring table. Figure 1 As shown, the signal input end of the reaction parameter monitoring table is connected to the reaction parameter detection controller on the one hand, and is electrically connected to the electric heater on the other hand. The signal output end of the reaction parameter monitoring table is connected to the main control computer. By setting the reaction parameter monitoring table, the temperature, pressure, flow rate and other parameters in the reaction process of the electric heater, the hydrolysis adsorption regeneration integrated tower and the adsorption regeneration integrated can be monitored, and the data can be sent to the main control computer for storage, and all the electric control flow valves set in the present invention are connected to the main control computer, and the main control computer needs to be controlled by the actual monitoring. An automatic control system is set in the present invention to realize the overall automatic control of the device of the present invention, including function switching, flow valve opening control, reaction parameter control and other multi-functional realization and control functions. The real-time parameters transmitted to the computer by the reaction parameter monitoring table form feedback control on the system, and the reaction parameters in the hydrolysis, adsorption and regeneration processes are controllable by adjusting the flow rate, electric heating power, fan power and other parameters. By controlling the switch of the electric control valve, the switching of different gas desulfurization process modes, the switching of the adsorption analysis regeneration pipeline, and the realization of the internal pipeline purge and release function of the system are realized.

[0033] The multifunctional coal gas desulfurization catalyst / adsorbent performance evaluation method of the present invention adopts the above device to carry out the test, and includes the following two mode functions:

[0034] Mode 1: Hydrolysis conversion + dry adsorption fine desulfurization process route;

[0035] Mode 2: Adsorption regeneration fine desulfurization process route;

[0036] The specific operations are as follows:

[0037] Select the corresponding catalyst or adsorbent according to the experimental needs, first purge the device, and then fill the catalyst or adsorbent to be evaluated in the corresponding tower, and then conduct an air tightness test. After passing the test, connect the device to the raw gas, turn on the system and adjust the system to the corresponding mode. At this time, the gas blower is turned on and the system runs normally. According to the experimental needs, the parameters of the reaction process are controlled by the main control computer, and the reaction parameter monitoring system function is turned on. By adjusting different reaction parameters, the actual performance and effect of the catalyst or adsorbent in the system and the total desulfurization efficiency of the system under this process can be obtained.

[0038] The multifunctional coal gas fine desulfurization catalyst / adsorbent effect evaluation device provided by the present invention is designed in combination with the characteristics of the above two processes, and a set of devices can meet the needs of catalyst / adsorbent performance and desulfurization effect evaluation under the two processes. Compared with the catalyst / adsorbent effect evaluation device under a single process, the evaluation device provided by the present invention has the advantages of lower cost under the premise of achieving the same function, and can evaluate the effects of catalysts / adsorbents required for different types of fine desulfurization processes and the desulfurization effect of the system, and at the same time, it can also explore the influence of parameters such as temperature, pressure, flow rate on the performance of catalysts / adsorbents under different processes, as well as the optimal process range of catalysts / adsorbents.

[0039] As a further preferred embodiment of the present invention, when the device of the present invention is used to conduct tests and evaluate the effects of the catalyst or adsorbent, the system closes all the electric control flow valves by default, and the switching function of different coal gas fine desulfurization process modes is realized by the following logic:

[0040] Mode 1: When mode 1 is turned on in the main control computer, the automatic control system opens the electric control flow valves S04, S08, S10, and S13, and the other electric control flow valves are all closed; the system turns on the electric heating function authority of the hydrolysis adsorption regeneration integrated tower, and sets the hydrolysis temperature as needed. At this time, the hydrolysis adsorption regeneration integrated tower only uses its hydrolysis function, and the adsorption regeneration integrated tower only uses its adsorption function. The two towers are used in series, and the gas inside the system first enters the hydrolysis tower for hydrolysis reaction, and then enters the adsorption tower to complete the desulfurization reaction. After the reaction, the gas fan transports the purified gas to the gas network.

[0041] Mode 2: When mode 2 is turned on in the main control computer, the automatic control system opens the electric control flow valves S04, S08, S06, S12, and S13, and the other electric control flow valves are all closed. The system opens the regeneration and analysis system authority, and the regeneration temperature can be set as needed. At this time, the hydrolysis adsorption and regeneration integrated tower uses its adsorption and regeneration functions, and the hydrolysis function is unavailable. The adsorption and regeneration integrated tower is used normally, and the two towers are used in parallel. According to needs, any of the two towers can be switched between adsorption and regeneration. The purified gas and the regenerated analysis gas are both sent to the gas network by the gas fan.

[0042] As a further preferred embodiment of the present invention, the adsorption and desorption process can be realized only under the premise that mode 2 is turned on. At this time, the regeneration function in the main control computer is turned on, and the main control computer opens the corresponding valve of the regeneration tower according to the needs, including two methods:

[0043] Method 1: When regenerating the hydrolysis adsorption regeneration integrated tower, the system will close the electric control flow valves S04, S08, and S012 under the valve state controlled by mode 2, and open the electric control flow valves S03, S05, and S09. At this time, tower 1 enters the regeneration state, and only the adsorption regeneration integrated tower performs adsorption desulfurization work. The regeneration temperature can be set as needed in the main control computer.

[0044] Method 2: When regenerating the adsorption regeneration integrated tower, the system will close the electric control flow valves S06 and S13 under the valve state controlled by mode 2, and open the electric control flow valves S03, S07, and S14. At this time, the adsorption regeneration integrated tower enters the regeneration state, and only the desorption regeneration integrated tower performs adsorption desulfurization work. The regeneration temperature can be set as needed in the main control computer.

[0045] As a further optimization of the present invention, the internal purge and release function is realized. When the system needs to switch modes or replace the packing, the system purge function needs to be turned on in the main control computer. At this time, the system is controlled in multiple steps. First, the electric control flow valves S01, S03, S05, S07, S09, and S14 are opened. At this time, the electric heater and the regeneration analysis gas pipeline are purged. After 5 minutes, the computer automatically controls the electric control flow valve S16 to open, and the sulfide detection system starts to work. When the CO detection is 0 mg / m 3 The system automatically enters the second stage of purging. At this time, all the electric control flow valves are closed, and the electric control flow valves S01, S04, S06, S08, S10, S12, and S13 are opened. At this time, the two reaction towers and the crude gas pipeline are purged. After 5 minutes, the computer automatically controls the electric control flow valve S15 to open, and the sulfide detection system starts working. When the CO detection is 0mg / m 3 When the purge is completed, close all valves.

[0046] As a further preferred embodiment of the present invention, the reaction parameter monitoring function is realized by turning on the reaction parameter monitoring system when the device is running. The system can be turned on in each mode.

[0047] When the device is in mode 1 and the module is turned on, the system will open the electric control flow valves S02, S11, and S15 based on the valve switch status in the current mode. At this time, the sulfide monitoring system can monitor and record the sulfide changes before and after hydrolysis, hydrolysis efficiency, sulfide concentration changes before and after desulfurization, desulfurization efficiency, and the total desulfurization efficiency of the system. The calculation formula is as follows:

[0048]

[0049] Where: ηhydrolysis is the hydrolysis conversion rate, in %; N COS1 The CO at the sampling port of the electric control flow valve S02 S Concentration, in mg / m 3 ; N COS2 COS concentration at the sampling port of the electric control flow valve S11, in mg / m 3 .

[0050]

[0051] Where: η desulfurization is the dry desulfurization efficiency, in %; N S2 It is the total sulfur concentration at the sampling port of the electric control flow valve S11, in mg / m 3 ; N S3 It is the total sulfur concentration at the sampling port of the electric control flow valve S15, in mg / m 3 ;

[0052]

[0053] Where: ηtotal is the total desulfurization efficiency of the system, in %; N S1 It is the total sulfur concentration at the sampling port of the electric control flow valve S02, in mg / m 3 ; N S3 It is the total sulfur concentration at the sampling port of the electric control flow valve S15, in mg / m 3 .

[0054]

[0055] Where: N S is the total sulfur concentration at the sampling point, in mg / m 3 ; N COS COS concentration at the sampling point, in mg / m 3 ; N CS2 is the CS2 concentration at the sampling point, in mg / m3 ; N H2S is the H2S concentration at the sampling point, in mg / m 3 .

[0056] When the device is in mode 2 and the module is turned on, the system will open the valve electric control flow valves S02, S15, and S16 based on the valve switch status in the current mode. At this time, the sulfide monitoring system can monitor and record the sulfide changes before and after adsorption fine desulfurization, the total desulfurization efficiency of the system, the concentration of sulfide in the analyzed gas during regeneration, and other parameters. The calculation formula is similar to that when the device is turned on in mode 1.

[0057] 3. Beneficial effects

[0058] Compared with the prior art, the present invention has the following beneficial effects:

[0059] (1) The present invention organically combines the two mainstream coal gas fine desulfurization processes of "hydrolysis + dry process" and "organic sulfur and inorganic sulfur integrated adsorption removal process", designs and develops a set of devices and methods that can be used to evaluate the effects of fine desulfurization catalysts and adsorbents under the two process conditions and evaluate the efficiency of the fine desulfurization system. The system gas flow path is reorganized by controlling the opening and closing of valves using an automatic control system, and the switching of the two mainstream coal gas fine desulfurization processes is achieved by using the design of a hydrolysis and adsorption integrated tower. It not only has the function of evaluating the effects of various types of fine desulfurization catalysts and adsorbents under the two fine desulfurization process conditions, but also has the function of evaluating the effect of coal gas organic sulfur hydrolysis catalysts and evaluating the desulfurization efficiency of the entire fine desulfurization process, and has the function of analyzing and exploring the optimal process range of a certain type of catalyst and adsorbent under different fine desulfurization processes and different coal gas conditions, thereby improving the current situation of single function and imperfect evaluation methods of existing evaluation devices.

[0060] (2) The device provided by the present invention is also designed as a movable device, which can be effectively used not only in laboratory tests but also in production site tests. When used in site tests, it is only necessary to connect part of the gas from the site gas pipeline to the device.

[0061] (3) The device of the present invention can explore the optimal reaction parameters of a certain type of catalyst and the catalytic effects of different catalysts under the same process conditions, and can provide technical support for the selection of the catalyst with the best catalytic performance under the process, and can provide technical support for the efficiency and stability of the coal gas desulfurization project during operation. Therefore, the device and method of the present invention are highly practical and instructive.

[0062] (4) The evaluation of the dry desulfurization process in the present invention can meet the evaluation of the effect of desulfurizers in various dry desulfurization processes such as metal oxide desulfurization, such as FeO, ZnO, etc.; activated carbon adsorption, blue charcoal adsorption desulfurization; nano adsorption desulfurization, etc. BRIEF DESCRIPTION OF THE DRAWINGS

[0063] Figure 1 It is a schematic structural diagram of the multifunctional coal gas desulfurization catalyst / adsorbent performance evaluation device of the present invention.

[0064] In the figure:

[0065] 1. Sampling port; 2. Electric control flow valve (S01~S16); 3. Sulfide online detector; 4. Main control computer; 5. Electric heater; 6. Hydrolysis adsorption regeneration integrated tower; 7. Adsorption regeneration integrated tower; 8. Reaction parameter detection controller; 9. Material change door; 10. Reaction parameter detection table; 11. Gas blower. DETAILED DESCRIPTION

[0066] The following will be combined with the accompanying drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, many specific details are set forth in the following description to facilitate a full understanding of the present invention, but the present invention can also be implemented in other ways different from those described herein, and therefore, the present invention is not limited to the specific embodiments of the following disclosure.

[0067] Example 1

[0068] like Figure 1 As shown, the device and method of the present invention are used to evaluate the hydrolysis effect of a certain type of hydrolysis catalyst and the desulfurization effect of a certain type of adsorbent, and the specific steps are as follows:

[0069] a) Turn on the device, and then open the purge and release function 4 in the main control computer. First, complete the purge and replacement of the residual gas in the pipelines inside the device and the two reaction towers (i.e., the hydrolysis adsorption regeneration integrated tower 6 and the adsorption regeneration integrated tower 7). After the purge operation is completed, the hydrolysis agent and desulfurization agent to be tested need to be loaded into the reactor respectively.

[0070] b) Open the material change door on the hydrolysis adsorption regeneration integrated tower 6 to remove the residual sample in the tower. After removal, fill the hydrolysis agent to be evaluated into the hydrolysis adsorption regeneration integrated tower 6. After filling, close the material change door, open the material change door 9 on the adsorption regeneration integrated tower 7, and replace the desulfurizer to be evaluated into the adsorption regeneration integrated tower 7 according to the same operating steps. After completion, close the material change door 9.

[0071] c) After completing the filling operation, the air tightness of the device needs to be tested. If no leakage is found, proceed to the next step. If leakage is found, the leakage point needs to be checked. Only after passing the air tightness test can the next step be performed.

[0072] d) After the airtightness is completed, open the system, close all the valves of the electric control flow valve 2 through the automatic control system, connect the raw coal gas to the device, select mode 1 on the main control computer 4, and control the parameters in the reaction process through the main control computer 4 according to the experimental design parameters. Turn on the reaction parameter monitoring function, and the main control computer 4 automatically records the effects of the catalysts at each stage under the reaction parameters, the hydrolysis efficiency, and the system desulfurization efficiency. Adjust the reaction parameters and record the data changes.

[0073] e) After completing all experiments, disconnect the raw gas access, turn on the purge and release function in the main control computer 4, complete the system purge, and after the purge is completed, close all valves in the system and shut down.

[0074] Example 2

[0075] like Figure 1 As shown, if the effect and regeneration effect of a certain type of fine desulfurization adsorbent need to be evaluated during the experiment, the specific implementation steps of the device of the present invention are as follows:

[0076] a) Turn on the device, and then turn on the purge and release function in the main control computer 4. First, complete the purge and replacement of residual gas in the pipelines inside the device and the two reaction towers (hydrolysis adsorption regeneration integrated tower 6 and adsorption regeneration integrated tower 7). After the purge operation is completed, the fine desulfurization adsorbent to be tested needs to be loaded into the reactor.

[0077] b) Open the material change doors on the hydrolysis adsorption regeneration integrated tower 6 and the adsorption regeneration integrated tower 7 to remove the residual samples in the towers. After removal, fill the refined desulfurization adsorbent to be evaluated into the hydrolysis adsorption regeneration integrated tower 6 and the adsorption regeneration integrated tower 7. After filling, close the material change door 9.

[0078] c) After completing the filling operation, the air tightness of the device needs to be tested. If no leakage is found, proceed to the next step. If leakage is found, the leakage point needs to be checked. Only after passing the air tightness test can the next step be performed.

[0079] d) After the airtightness is completed, open the system, close all the valves of the electric control flow valve 2 through the automatic control system, connect the raw coal gas to the device, select mode 2 on the main control computer 4, and control the parameters in the reaction process through the main control computer 4 according to the experimental design parameters. Turn on the reaction parameter monitoring function, and the main control computer 4 automatically records the effect of the adsorbent at each stage and the system desulfurization efficiency and other parameters under the reaction parameters. Adjust the reaction parameters and record the data changes.

[0080] e) When the reaction proceeds to a certain extent, the required reaction tower is selected for analytical regeneration. The tower to be regenerated is selected in the main control computer 4, and the analytical regeneration system is turned on. At this time, the electric heater 5 starts to work. The regeneration temperature can be set through the main control computer 4. The optimal time for analytical regeneration of the adsorbent can be determined based on the detection data of the sulfide online detector 3.

[0081] f) Switch the regeneration tower, select the tower that needs to be regenerated in the system, and the system will automatically switch to another tower to enter the adsorption desulfurization operation. After a certain number of cycles, the adsorption effect inflection point of the adsorbent can be determined based on the detection data recorded by the main control computer 4.

[0082] g) After completing all experiments, disconnect the gas connection, turn on the purge and release function in the main control computer 4, complete the system purge, and after the purge is completed, close all valves in the system and shut down.

[0083] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A multifunctional coal gas desulfurization catalyst / adsorbent performance evaluation device, characterized in that: It includes gas purification system, regeneration and analysis system, purge and release system, automatic control system and reaction parameter monitoring system, among which: The coal gas purification system comprises a water decomposition adsorption regeneration integrated tower (6) and an adsorption regeneration integrated tower (7), wherein the coal gas inlets of the water decomposition adsorption regeneration integrated tower (6) and the adsorption regeneration integrated tower (7) are both connected to the gas outlet end of the raw coal gas pipeline, and are used to remove sulfides in the coal gas; The regeneration and analysis system is connected to the coal gas purification system through a pipeline and is used to analyze and regenerate the failed adsorbent in the water decomposition adsorption and regeneration integrated tower (6) and the adsorption and regeneration integrated tower (7); The purge and release system is arranged at the gas inlet end of the crude gas pipeline and is used to purge and replace the gas inside the equipment and pipeline of the entire device; The reaction parameter monitoring system comprises an online sulfide detector (3) and a reaction parameter detection meter (10), wherein the online sulfide detector (3) is connected to the gas inlet end of the raw gas pipeline, the gas outlet end of the gas purification system, and the gas outlet end of the regeneration analysis system through a sampling gas pipeline, and the reaction parameter detection meter (10) is electrically connected to the gas purification system and the regeneration analysis system, and is used to detect changes in all reaction parameters before, during, and after the entire reaction process; The automatic control system comprises a main control computer (4), a reaction parameter detection controller (8) and an electric control flow valve (2); the signal input end of the reaction parameter detection controller (8) is electrically connected to the gas purification system, and the signal output end of the reaction parameter detection controller (8) is electrically connected to the main control computer (4) through a reaction parameter detection meter (10); the electric control flow valve (2) is arranged on the pipeline and is used to control the gas flow; the sulfide online detector (3) and the electric control flow valve (2) are both electrically connected to the main control computer (4).

2. A multifunctional coal gas desulfurization catalyst / adsorbent performance evaluation device according to claim 1, characterized in that: The coal gas purification system further comprises a coal gas blower (11), the coal gas outlets of the water decomposition adsorption regeneration integrated tower (6) and the adsorption regeneration integrated tower (7) are respectively connected to the coal gas blower (11) via pipelines, and the coal gas outlet of the water decomposition adsorption regeneration integrated tower (6) is also separately connected to the coal gas inlet of the adsorption regeneration integrated tower (7) via a pipeline, and an electric control flow valve (2) is provided on the pipeline.

3. A multifunctional coal gas desulfurization catalyst / adsorbent performance evaluation device according to claim 2, characterized in that: The hydrolysis adsorption regeneration integrated tower (6) is provided with an electric heating system, and the temperature control range is 20°C to 300°C; the gas blower (11) is a centrifugal blower, the working temperature is 60 to 300°C, and the motor is an explosion-proof motor.

4. A multifunctional coal gas desulfurization catalyst / adsorbent performance evaluation device according to claim 2, characterized in that: The regeneration and analysis system comprises an electric heater (5), wherein an air inlet of the electric heater (5) is connected to a raw gas pipeline via a pipeline, and an air outlet of the electric heater (5) is connected to a regeneration and analysis gas inlet of a water decomposition and adsorption regeneration integrated tower (6) and a regeneration and analysis gas inlet of an adsorption and regeneration integrated tower (7) via pipelines, respectively, and the regeneration and analysis gas outlet of the water decomposition and adsorption regeneration integrated tower (6) and the regeneration and analysis gas outlet of the adsorption and regeneration integrated tower (7) are both connected to a gas blower (11) via pipelines.

5. A multifunctional coal gas desulfurization catalyst / adsorbent performance evaluation device according to claim 4, characterized in that: The air inlet end of the electric heater (5), the regeneration gas inlet and outlet ends of the hydrolysis adsorption regeneration integrated tower (6), and the regeneration gas inlet and outlet ends of the adsorption regeneration integrated tower (7) are all provided with electric control flow valves (2).

6. A multifunctional coal gas desulfurization catalyst / adsorbent performance evaluation device according to any one of claims 1 to 5, characterized in that: The purge and release system is provided with a back-blowing air pipeline, which is connected to the air inlet end of the raw coal gas pipeline, and an electric control flow valve (2) is provided on the back-blowing air pipeline.

7. A multifunctional coal gas desulfurization catalyst / adsorbent performance evaluation device according to any one of claims 1 to 5, characterized in that: The reaction parameter monitoring system further comprises a plurality of sampling ports (1), the sampling ports (1) being respectively arranged on a raw gas pipeline and a regeneration analysis gas pipeline; each sampling port (1) is individually connected to an online sulfide detector (3) via a pipeline, and an electric control flow valve (2) is correspondingly arranged on the pipeline; the signal input end of the reaction parameter detection controller (8) is respectively electrically connected to a hydrolysis adsorption regeneration integrated tower (6) and an adsorption regeneration integrated tower (7).

8. A multifunctional coal gas desulfurization catalyst / adsorbent performance evaluation method, characterized in that: The test is carried out using the evaluation device as claimed in any one of claims 2 to 7, including the following two mode functions: Mode 1: Hydrolysis conversion + dry adsorption fine desulfurization process route; Mode 2: Adsorption regeneration fine desulfurization process route; The specific operations are as follows: According to the experimental needs, the corresponding catalyst or adsorbent is selected, and the device is first purged. After the purging is completed, the catalyst or adsorbent to be evaluated is loaded into the corresponding tower, and then an air tightness test is performed. After the test is qualified, the device is connected to the raw coal gas, and the system is turned on and adjusted to the corresponding mode. At this time, the coal gas blower (11) is turned on and the system runs normally. According to the experimental needs, the parameters of the reaction process are controlled by the main control computer (4), and the reaction parameter monitoring system function is turned on. By adjusting different reaction parameters, the actual performance and effect of the catalyst or adsorbent in the system and the total desulfurization efficiency of the system under this process can be obtained.

9. A multifunctional coal gas desulfurization catalyst / adsorbent performance evaluation method according to claim 8, characterized in that: When the process route of mode 1 is selected, the specific evaluation method is as follows: Step 1: Start the machine and open the purge and release system to complete the purge and replacement of the gas in the device and pipeline; Step 2: In this mode, the two towers are used in series. After the residual samples in the two towers are cleaned, the catalyst is loaded into the hydrolysis adsorption regeneration integrated tower (6), and the adsorption regeneration integrated tower (7) is loaded with the adsorbent; Step 3: Check the overall air tightness of the device. If there is any leakage, check the leakage point until it passes the air tightness test before proceeding to the next step; Step 4: Close all the electric control flow valves (2) in the device, connect the raw coal gas, select mode 1 in the main control computer (4), control the parameters in the reaction process and control the opening of the relevant electric control flow valves (2) through the main control computer (4) according to the experimental design parameters, and then start the reaction parameter monitoring system for real-time monitoring; Step 5, the main control computer (4) automatically records and outputs the experimental results under the specific reaction parameters in this mode, and the experimental results include the effect of the catalyst at each stage, the hydrolysis efficiency and the system desulfurization efficiency parameters; Step 6: After the experiment is completed, disconnect the raw gas supply, open the purge and release system, complete the device purge, and after the purge is completed, close all the electric control flow valves (2) and shut down the machine.

10. A multifunctional coal gas desulfurization catalyst / adsorbent performance evaluation method according to claim 8, characterized in that: When the process route of mode 2 is selected, the specific evaluation method is as follows: Step 1: Start the purge and release system to complete the purge and replacement of the gas in the device and pipeline; Step 2: In this mode, the hydrolysis function of the hydrolysis adsorption regeneration integrated tower (6) is not used, and the hydrolysis adsorption regeneration integrated tower (6) and the adsorption regeneration integrated tower (7) are used in parallel. According to experimental requirements, it is determined that any one of the two towers is switched between adsorption and regeneration, and adsorbent is loaded into the two towers; Step 3: Check the overall air tightness of the device. If there is any leakage, check the leakage point until it passes the air tightness test before proceeding to the next step; Step 4: Close all the electric control flow valves (2) in the device, connect the raw coal gas, select mode 2 in the main control computer (4), control the parameters in the reaction process and control the opening of the relevant electric control flow valves (2) through the main control computer (4) according to the experimental design parameters, and then start the reaction parameter monitoring system for real-time monitoring; Step 5, the main control computer (4) automatically records the experimental results under the specific reaction parameters in this mode, and the experimental results include the effect of the adsorbent at each stage and the system desulfurization efficiency parameters; Step 6: When the tower needs to be regenerated, the main control computer (4) controls the regeneration and regeneration system to start, sets the regeneration temperature, and determines the optimal time for regeneration of the adsorbent through the monitoring data of sulfide by the reaction parameter monitoring system; Step 7: Switch to another tower to perform adsorption desulfurization operation. After multiple cycles, the detection data automatically recorded by the main control computer (4) is used to evaluate the inflection point of the adsorption effect of the adsorbent; Step 8: After the experiment is completed, disconnect the raw coal gas, open the purge and release system, complete the device purge, and after the purge is completed, close all the electric control flow valves (2) and shut down the machine.

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