CN116298065A - Multifunctional gas fine desulfurization catalyst/adsorbent performance evaluation device and method - Google Patents
Multifunctional gas fine desulfurization catalyst/adsorbent performance evaluation device and method Download PDFInfo
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- CN116298065A CN116298065A CN202310190393.6A CN202310190393A CN116298065A CN 116298065 A CN116298065 A CN 116298065A CN 202310190393 A CN202310190393 A CN 202310190393A CN 116298065 A CN116298065 A CN 116298065A
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- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 90
- 230000023556 desulfurization Effects 0.000 title claims abstract description 90
- 238000000034 method Methods 0.000 title claims abstract description 71
- 239000003463 adsorbent Substances 0.000 title claims abstract description 64
- 239000003054 catalyst Substances 0.000 title claims abstract description 57
- 238000011156 evaluation Methods 0.000 title claims abstract description 37
- 238000011069 regeneration method Methods 0.000 claims abstract description 131
- 230000008929 regeneration Effects 0.000 claims abstract description 127
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- 230000008569 process Effects 0.000 claims abstract description 50
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- 239000007789 gas Substances 0.000 description 113
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- 229910052717 sulfur Inorganic materials 0.000 description 9
- 239000011593 sulfur Substances 0.000 description 9
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 7
- 230000003009 desulfurizing effect Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
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- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
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- 238000004364 calculation method Methods 0.000 description 2
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
- C10K1/002—Removal of contaminants
- C10K1/003—Removal of contaminants of acid contaminants, e.g. acid gas removal
- C10K1/004—Sulfur containing contaminants, e.g. hydrogen sulfide
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- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
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Abstract
The invention discloses a multifunctional gas fine desulfurization catalyst/adsorbent performance evaluation device and method, and belongs to the technical field of gas fine desulfurization. The device comprises a gas purifying system, a regeneration analysis gas system, a blowing and diffusing system, a reaction parameter monitoring system and an automatic control system, wherein a valve switch is controlled by the automatic control system to reorganize a system flow path, and meanwhile, the two main flow gas fine desulfurization processes are switched by utilizing the design of a hydrolysis and adsorption integrated tower, so that the device has the functions of evaluating the effects of each type of fine desulfurization catalyst and adsorbent under the two fine desulfurization process conditions, evaluating the effects of the gas organic sulfur hydrolysis catalyst and evaluating the full-flow desulfurization efficiency of the fine desulfurization process, and analyzing and exploring the optimal process intervals of the fine desulfurization catalyst and adsorbent under different fine desulfurization processes and different gas conditions.
Description
Technical Field
The invention belongs to the technical field of gas fine desulfurization, and particularly relates to a multifunctional gas fine desulfurization catalyst/adsorbent performance evaluation device and method.
Background
The method for controlling pollutant emission by adopting a source treatment mode in the steel industry has become a new way for SO (sulfur dioxide) in the flue gas of tail gas furnaces such as heating furnaces, hot blast stoves and the like 2 At present, a method for carrying out fine desulfurization on source gas is generally adopted for treatment, and SO in the flue gas discharged after combustion is caused by controlling the content of sulfide in the source gas 2 The sulfide in the gas is mainly formed by inorganic sulfur (H 2 S) and organic sulfur (COS, CS) 2 Etc.), so that two sulfides are respectively removed in the process of finely desulfurizing the coal gas, and common technical routes are an organic sulfur hydrolysis and inorganic sulfur dry process, an organic and inorganic integrated adsorption removal regeneration process, and the like.
Inorganic Sulfur (H) 2 S) the removal process is relatively mature, but the organic sulfur treatment technology is continuously developed, and at present, a device for detecting the conversion efficiency of the hydrolytic agent is already provided, but the function is relatively single, the conversion efficiency of the hydrolytic agent under the working condition can only be detected, the comprehensive desulfurization effect evaluation of the hydrolysis and dry process can not be met, and the conversion efficiency of the catalyst/adsorbent of the organic-inorganic integrated adsorption process and the detection and evaluation of the desulfurization efficiency of a gas fine desulfurization system can not be met.
As a result of the search, a device and a method for evaluating the performance of a catalyst have been disclosed in related patents, such as patent document CN 216082636U. For another example, patent literature, such as chinese patent No. CN212391449U, CN212391448U, CN215179965U, CN111579708B, discloses a gas fine desulfurization catalyst performance evaluation device. The prior device and method for evaluating the performance of the catalyst have single basic function although a few devices and methods are disclosed. The effect evaluation device and method for the gas fine desulfurization catalyst are relatively few, only part of the effect evaluation device is aimed at the carbonyl sulfide hydrolysis catalyst effect evaluation device, or the effect evaluation device is aimed at the catalyst performance of a certain process, and the effect evaluation device and method are difficult to be used for evaluating the effects of the catalyst and the adsorbent under various fine desulfurization process conditions, and the effect evaluation of the organic sulfur hydrolysis catalyst and the full-flow desulfurization efficiency evaluation of the fine desulfurization process are limited.
Disclosure of Invention
1. Problems to be solved
The invention mainly aims to solve the problems that the existing evaluation device for the comprehensive desulfurization efficiency of the gas fine desulfurization adsorbent/catalyst effect and the main stream gas fine desulfurization process is single in function and the evaluation method is imperfect, and designs a set of multifunctional gas fine desulfurization catalyst/adsorbent effect evaluation device and method by organically combining the hydrolysis and dry fine desulfurization process flow and the organic-inorganic integrated adsorption fine desulfurization process flow.
2. Technical proposal
In order to solve the problems, the technical scheme adopted by the invention is as follows:
the invention provides a multifunctional gas fine desulfurization catalyst/adsorbent performance evaluation device, which comprises:
the gas purifying system is used for removing sulfide in the gas;
the regeneration analysis gas system is used for analyzing and regenerating the invalid adsorbent in the adsorption tower;
the purging and diffusing system is used for purging and replacing the gas in the equipment and the pipeline of the whole device;
the reaction parameter monitoring system is used for detecting the change condition of each reaction parameter in the reaction process;
the automatic control system is used for the integral automatic control of the device and comprises a plurality of control functions such as function switching, electric control flow valve opening control, reaction parameter control, realization of each function and the like.
As a further preferred aspect of the present invention, the gas purification system of the present invention comprises a hydrolysis-adsorption-regeneration integrated tower, an adsorption-regeneration integrated tower, and a gas blower, wherein the external dimensions and the internal packing amounts of the hydrolysis-adsorption-regeneration integrated tower and the adsorption-regeneration integrated tower are designed to be identical. Wherein:
the design of the adsorption and regeneration integrated tower is as follows:
the integrated tower is a vertical container, adopts a fixed bed vertical channel type design, and an adsorbent bed layer is filled with an adsorbent material; the gas is designed to flow from top to bottom in the adsorption tower, the analysis gas flows from bottom to top, and the gas is discharged into a gas pipe network through a gas fan; according to the requirement of 100% gas quantity of gas design working condition, the design pressure is 0.1MPa; the outside of the adsorption and regeneration integrated tower is provided with an insulating layer, a desulfurization pipeline inlet and outlet, a regeneration pipeline inlet and outlet, an adsorbent filling material changing door in the tower and the like, and the adsorbent is changed through the changing door; the inside is equipped with adsorbent bearing structure, in order to make the gas distribution that gets into the adsorbed layer even, sets up gas equipartition baffle at desulfurization import, designs the reaction parameter test probe interface in the tower.
The design of the hydrolysis adsorption regeneration integrated tower is as follows:
an electric tracing system is arranged in the hydrolysis adsorption regeneration integrated tower, so that the temperature of the filling material in the tower can be controlled, the temperature parameter change (the temperature control range is 20-300 ℃) in the hydrolysis reaction process can be controlled, and other parameters are consistent with the adsorption regeneration integrated tower.
The gas fan is designed as follows:
the full pressure of the gas fan needs to meet the pressure drop requirement of the system, and a certain margin is reserved; the fan adopts a centrifugal fan, the working temperature is 60-300 ℃, and an explosion-proof motor is adopted; the outlet of the fan is provided with a check valve and flexible connection, noise in a noise area of the fan meets the national standard requirement, the fan is required to run on the highest efficiency point, and the fan is required to have an almost flat efficiency characteristic curve so as to ensure that the unit has optimal efficiency under various loads during running, and the fan is provided with a motor, a public chassis (comprising a shock pad), a corrugated expansion joint, a counter flange, a coupler protection cover, a transmission box and the like.
The connection mode is as follows:
as shown in fig. 1, the gas inlets of the hydrolysis adsorption regeneration integrated tower and the adsorption regeneration integrated tower are connected with the gas outlet end of the raw gas pipeline, an electric control flow valve S04 is arranged on the pipeline at the gas inlet end of the hydrolysis adsorption regeneration integrated tower, and an electric control flow valve S06 is arranged on the pipeline at the gas inlet end of the adsorption regeneration integrated tower.
The gas outlets of the two towers are respectively connected with the gas blower through pipelines, and the gas outlet of the hydrolysis adsorption regeneration integrated tower is also connected with the gas inlet of the adsorption regeneration integrated tower through a pipeline. An electric control flow valve S08 is arranged on a pipeline at the gas outlet end of the hydrolysis adsorption regeneration integrated tower, an electric control flow valve S10 is arranged on a pipeline connected with the adsorption regeneration integrated tower, and an electric control flow valve S12 is arranged on a pipeline connected with a gas fan of the hydrolysis adsorption regeneration integrated tower. An electric control flow valve S13 is arranged on a pipeline at the gas outlet end of the adsorption and regeneration integrated tower.
The gas blower is arranged at the position of the main outlet of the device, the blower pressurizes the purified gas in the system and then sends the gas to the gas pipe network, and the pressurizing pressure is adjustable according to the pressure of the pipe network.
As a further preferred aspect of the present invention, the regeneration analysis system is connected to the gas purification system through a pipe, and is configured to analyze and regenerate the hydrolytic adsorption regeneration integrated tower and the spent adsorbent in the adsorption regeneration integrated tower. Specifically, the regeneration analysis system is provided with an electric heater, an air inlet of the electric heater is connected with a raw gas pipeline through a pipeline, an electric control flow valve S03 is arranged on the pipeline, an air outlet of the electric heater is connected with a regeneration analysis air inlet of the hydrolysis adsorption regeneration integrated tower through a pipeline, an electric control flow valve S09 is arranged on the pipeline, an air outlet of the electric heater is also connected with a regeneration analysis air inlet of the adsorption regeneration integrated tower through a pipeline, and an electric control flow valve S14 is arranged on the pipeline.
The regeneration analysis gas outlet of the hydrolysis adsorption regeneration integrated tower and the regeneration analysis gas outlet of the adsorption regeneration integrated tower are connected with the gas fan through pipelines, an electric control flow valve S05 is arranged on the pipeline at the regeneration analysis gas outlet end of the hydrolysis adsorption regeneration integrated tower, and an electric control flow valve S07 is arranged on the pipeline at the regeneration analysis gas outlet end of the adsorption regeneration integrated tower.
The electric heater can heat the gas or nitrogen to the regeneration temperature of the adsorbent (determined according to the type of the adsorbent), the heated hot gas is conveyed into a tower to be regenerated through a pipeline to analyze and regenerate the adsorbent, and the system and the gas purifying system share a gas fan to convey analysis gas into a pipe network.
More optimally, the electric heater is an explosion-proof pipeline heater, the working temperature is 60-300 ℃, the working pressure is 12kPa, the outer shell and the inner bore are all designed by stainless steel, the pipeline heater consists of a plurality of tubular electric heating elements, a cylinder body, a guide plate and the like, the tubular electric heating elements are high-temperature resistance wires arranged in metal pipes, the gap part is tightly filled with crystalline magnesia powder with good insulativity and heat conductivity, and the guide baffle plate is arranged in the cylinder body, so that the gas is heated uniformly during circulation.
As a further preferable mode of the invention, the purging and diffusing system is provided with a back-blowing pipeline, the back-blowing pipeline is connected with the air inlet end of the raw gas pipeline, and an electric control flow valve S01 is arranged on the back-blowing pipeline. When the device is stopped, the flow valve S01 is opened to introduce nitrogen, equipment such as an internal pipeline, an adsorption tower, a fan, an electric heater and the like of the system are purged, purge gas is discharged into the atmosphere through the rear end of the gas fan or is directly returned to a pipe network, and the opening and closing of the flow valve valves arranged at all positions in the purging process are controlled by an automatic control system.
As a further preferable aspect of the present invention, the reaction parameter monitoring system comprises a sulfide on-line detector, a reactionParameter monitoring table, sampling port and related pipeline. The automatic control system comprises a main control computer, a reaction parameter detection controller and an electric control flow valve. The sulfide on-line detector is connected with a sampling port at the gas inlet of the raw gas pipeline through a sampling gas pipeline (an electric control flow valve S02 is arranged on the sampling gas pipeline); on the other hand, the gas purifying system is connected with a sampling port at the gas outlet of the gas purifying system and a sampling port at the gas outlet of the regeneration analysis system through a sampling gas pipeline, wherein the sampling gas pipeline connected with the gas outlet of the gas purifying system is provided with electric control flow valves S11 and S15, and the sampling gas pipeline connected with the gas outlet of the regeneration analysis system is provided with an electric control flow valve S16. In addition, the sulfide on-line detector is electrically connected with the main control computer, and can detect sulfide in gas in different reaction stages on line through the arrangement of the sulfide on-line detector, and the detection components comprise H 2 S、COS、CS 2 And CO, and the like, and can also send the detection result to a main control computer for storage in real time.
The signal input end of the reaction parameter detection controller is electrically connected with the hydrolysis adsorption regeneration integrated tower and the adsorption regeneration integrated tower of the gas purification system respectively, and the signal output end of the reaction parameter detection controller is electrically connected with the main control computer through the reaction parameter monitoring table. Specifically, as shown in fig. 1, the signal input end of the reaction parameter monitoring table is connected with the reaction parameter detection controller on one hand, and is electrically connected with the electric heater on the other hand, the signal output end of the reaction parameter monitoring table is connected with the main control computer, parameters such as temperature, pressure, flow rate and the like in the reaction process of the electric heater, the hydrolysis adsorption regeneration integrated tower and the adsorption regeneration integrated tower can be monitored by setting the reaction parameter monitoring table, data can be sent to the main control computer for storage, and all the electric control flow valves arranged in the invention are connected with the main control computer and are controlled by the main control computer by actual monitoring. The invention is provided with an automatic control system, can realize the integral automatic control of the device, and comprises the multifunctional realization and control functions of function switching, flow valve opening control, reaction parameter control and the like. The real-time parameters transmitted to the computer through 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 parameters such as flow, electric heating power, fan power and the like. The switching of different gas fine desulfurization process modes, the pipeline switching of adsorption analysis regeneration and the realization of the purging and diffusing function of the pipeline inside the system are realized by controlling the switch of the electric control valve.
The invention relates to a performance evaluation method of a multifunctional gas fine desulfurization catalyst/adsorbent, which adopts the device to test and comprises the following two mode functions:
mode one, hydrolysis conversion and dry adsorption fine desulfurization process route;
mode two, adsorption regeneration fine desulfurization process route;
the specific operation is as follows:
the method comprises the steps of selecting a corresponding catalyst or adsorbent according to experimental requirements, firstly purging the device, filling the catalyst or adsorbent to be evaluated in a corresponding tower after purging, then detecting air tightness, switching in raw gas to the device after detecting the qualified catalyst or adsorbent, switching on a system and adjusting the system to a corresponding mode, switching on a gas fan at the moment, enabling the system to normally operate, controlling parameters of a reaction process through a main control computer according to experimental requirements, switching on a reaction parameter monitoring system function, and obtaining actual performance and effect of the catalyst or adsorbent in the system and total desulfurization efficiency of the system under the process by adjusting different reaction parameters.
The multifunctional gas fine desulfurization catalyst/adsorbent effect evaluation device provided by the invention is designed by combining the characteristics of the two processes, and can meet the requirements of evaluating the performance and desulfurization effect of the catalyst/adsorbent under the two processes through one set of device. Compared with a catalyst/adsorbent effect evaluation device under a single process, the catalyst/adsorbent effect evaluation device provided by the invention has the advantages that the cost is lower on the premise of realizing the same function, the effect of catalysts/adsorbents required by different types of fine desulfurization processes and the desulfurization effect of a system can be evaluated, and meanwhile, the influence of parameters such as temperature, pressure, flow rate and the like on the performance of the catalysts/adsorbents under different processes and the optimal process interval of the catalysts/adsorbents can be explored.
As a further preferred aspect of the invention, when the device of the invention is used for testing and evaluating the effect of the catalyst or the adsorbent, the system defaults to close all the electric control flow valves, and the switching function of different gas fine desulfurization process modes is realized through the following logic:
when the mode one is opened in the main control computer, the automatic control system opens the electric control flow valves S04, S08, S10 and S13, and all the other electric control flow valves are in a closed state; the system opens the electric tracing function authority of the hydrolysis, adsorption and regeneration integrated tower, the hydrolysis temperature is set according to the requirement, at the moment, the hydrolysis, adsorption and regeneration integrated tower only uses the hydrolysis function, the adsorption and regeneration integrated tower only uses the adsorption function, the two towers are connected in series, gas in the system firstly enters the hydrolysis tower for hydrolysis reaction, the gas enters the adsorption tower for desulfurization reaction after reaction, and the purified gas is conveyed to a gas pipe network by a gas fan after reaction.
When the mode II is opened in the main control computer, the automatic control system opens the electric control flow valves S04, S08, S06, S12 and S13, all the other electric control flow valves are in a closed state, the system opens the authority of the regeneration analysis system, the regeneration temperature can be set according to the requirement, the hydrolysis, adsorption and regeneration integrated tower uses the adsorption and regeneration functions, the hydrolysis function is unavailable, the adsorption and regeneration integrated tower is normally used, the two towers are used in parallel, the adsorption and regeneration of any one of the two towers can be switched according to the requirement, and the purified gas and the regenerated analysis gas are both supplied to the gas pipe network by the gas fan.
As a further preferred mode of the invention, the implementation of the adsorption analysis process can be used only on the premise of opening the second mode, at this time, the main control computer opens the regeneration function in the main control computer, and the main control computer opens the corresponding valve of the regeneration tower according to the need, comprising two modes:
mode one: when regenerating the hydrolysis adsorption regeneration integrated tower, the system closes the electric control flow valves S04, S08 and S012 under the valve state of the mode two control, and opens the electric control flow valves S03, S05 and S09, at this time, the tower 1 enters a regeneration state, only the adsorption regeneration integrated tower performs adsorption desulfurization operation, and the regeneration temperature can be set in the main control computer as required.
Mode two: when the adsorption and regeneration integrated tower is regenerated, the system closes the electric control flow valves S06 and S13 in the valve state of the mode two control, opens the electric control flow valves S03, S07 and S14, and at the moment, the adsorption and regeneration integrated tower enters a regeneration state, only the desorption and regeneration integrated tower performs adsorption and desulfurization work, and the regeneration temperature can be set in the main control computer as required.
As a further preferable mode of the invention, when the system needs to switch modes or change filler, the system purging function needs to be started in the main control computer, the system is controlled in multiple steps, the electric control flow valves S01, S03, S05, S07, S09 and S14 are firstly opened, the electric heater and the regeneration analysis gas pipeline are purged at the moment, the computer automatically controls the electric control flow valve S16 to be opened after 5 minutes, the sulfide detection system starts to work, and when the CO is detected to be 0mg/m 3 When the system automatically enters the second purging stage, all the electric control flow valves are closed at the moment, the electric control flow valves S01, S04, S06, S08, S10, S12 and S13 are opened, at the moment, purging is carried out on the two reaction towers and the raw gas pipeline, the computer automatically controls the electric control flow valve S15 to be opened after 5 minutes, the sulfide detection system starts to work, and when the CO is detected to be 0mg/m 3 And when the purging is finished, closing all valves.
As a further preferred aspect of the invention, the reaction parameter monitoring function is implemented such that the reaction parameter monitoring system is turned on after operation of the device, the system being turned on in each mode,
when the device is in a mode one and the module is opened, the system can open the electric control flow valves S02, S11 and S15 on the basis of the valve opening and closing state in the current mode, and at the moment, the vulcanization monitoring system can monitor and record parameters such as the vulcanization change condition before and after hydrolysis, the hydrolysis efficiency, the sulfide concentration change condition before and after desulfurization, the desulfurization efficiency, the total desulfurization efficiency of the system and the like, and the calculation formula is shown as follows:
wherein: eta is hydrolyzed into hydrolysis conversion rate with unit being; n (N) COS1 For electrically controlling CO at the sampling port of the flow valve S02 S Concentration in mg/m 3 ；N COS2 For electrically controlling COS concentration at the sampling port of the flow valve S11, the unit is mg/m 3 。
Wherein: η desulfurization is dry desulfurization efficiency in units of; n (N) S2 The total sulfur concentration at the sampling port of the electric control flow valve S11 is expressed as mg/m 3 ；N S3 The total sulfur concentration at the sampling port of the electric control flow valve S15 is expressed as mg/m 3 ；
Wherein: eta is the total desulfurization efficiency of the system, and the unit is; n (N) S1 The total sulfur concentration at the sampling port of the electric control flow valve S02 is expressed as mg/m 3 ；N S3 The total sulfur concentration at the sampling port of the electric control flow valve S15 is expressed as mg/m 3 。
Wherein: n (N) S The total sulfur concentration at the sampling site is in mg/m 3 ；N COS For COS concentration at the sample in mg/m 3 ；N CS2 For sampling CS 2 Concentration in mg/m 3 ；N H2S For the sampling site H 2 S concentration in mg/m 3 。
When the device is in a second mode and the module is opened, the system can open the valve electric control flow valves S02, S15 and S16 on the basis of the valve opening and closing state in the current mode, and at the moment, the vulcanization monitoring system can monitor and record parameters such as the vulcanization change condition before and after the fine desulfurization by the adsorption method, the total desulfurization efficiency of the system, the concentration of the analyzed gas sulfide during regeneration and the like. The calculation formula is similar to when the device is turned on in the state of mode one.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention organically combines the two main stream gas fine desulfurization processes of the hydrolysis and dry process and the organic sulfur and inorganic sulfur integrated adsorption removal process, designs and develops a set of device and method for evaluating the effect of a fine desulfurization catalyst and an adsorbent under two process conditions and evaluating the efficiency of a fine desulfurization system, realizes the recombination of a system gas flow path by adopting an automatic control system to control the opening and closing of a valve, realizes the switching of the two main stream gas fine desulfurization processes by utilizing the design of a hydrolysis adsorption integrated tower, has the effect evaluation function of each type of fine desulfurization catalyst and the adsorbent under the two fine desulfurization process conditions, has the function of evaluating the effect of a gas organic sulfur hydrolysis catalyst and the whole flow desulfurization efficiency of the fine desulfurization process, has the function of analyzing and exploring the optimal process interval of a certain type of catalyst and an adsorbent under different fine desulfurization processes and different gas conditions, and improves the current situation that the existing evaluation device has single function and imperfect evaluation method.
(2) The device provided by the invention is also designed into a movable device, not only can be effectively used for laboratory tests, but also can be used for production field tests, and only needs to introduce a part of gas into the device through a field gas pipeline when the device is used for the field tests.
(3) The device can explore the optimal reaction parameters of a catalyst of a certain model and the catalytic effects of different catalysts under the same process condition, can provide technical support for the selection of the catalyst with the optimal catalytic performance under the process, and can provide technical support for the high efficiency and the stability of the gas fine desulfurization engineering project in the operation process. Therefore, the device and the method have strong practicability and guidance.
(4) The evaluation of the dry desulfurization process in the invention can meet the requirement of metal oxide desulfurization, such as FeO, znO and the like; activated carbon adsorption and semi-coke adsorption desulfurization; and evaluating the effect of various desulfurizing agents in dry desulfurizing processes such as nano adsorption desulfurization.
Drawings
FIG. 1 is a schematic diagram of a multifunctional gas fine desulfurization catalyst/adsorbent performance evaluation device according to the present invention.
In the figure:
1. a sampling port; 2. electrically controlling flow valves (S01-S16); 3. a sulfide on-line detector; 4. a main control computer; 5. an electric heater; 6. hydrolysis, adsorption and regeneration integrated tower; 7. an adsorption and regeneration integrated tower; 8. a reaction parameter detection controller; 9. a material changing door; 10. a reaction parameter detection table; 11. a gas fan.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It will be apparent that numerous specific details are set forth in the following description in order to provide a thorough understanding of the present invention, however, the present invention may be practiced in other ways than as described herein, and therefore the present invention is not limited to the specific embodiments of the present disclosure.
Example 1
As shown in fig. 1, the device and the method of the invention are adopted 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:
a) The device is started, after the device is started, the purging and diffusing function of the main control computer 4 is opened, purging and replacement of residual gas in a pipeline inside the device and in two reaction towers (namely the hydrolysis and adsorption integrated tower 6 and the adsorption and regeneration integrated tower 7) are preferably completed, and the hydrolysis agent and the desulfurizing agent to be tested are required to be respectively filled into the reactor after purging operation is completed.
b) And opening a material changing door on the hydrolysis adsorption regeneration integrated tower 6, removing residual samples in the tower, filling the hydrolytic agent to be evaluated into the hydrolysis adsorption regeneration integrated tower 6 after removing, sealing the material changing door after filling, opening a material changing door 9 on the adsorption regeneration integrated tower 7, changing the desulfurizing agent to be evaluated into the adsorption regeneration integrated tower 7 according to the same operation steps, and sealing the material changing door 9 after finishing.
c) After the packing operation is completed, the air tightness of the device needs to be detected, when the air leakage is detected, the next step is carried out, if the air leakage exists, the air leakage point needs to be checked, and the next step operation can not be carried out until the air tightness is detected.
d) After the air tightness is finished, the system is opened, after all valves of the electric control flow valve 2 are closed through the automatic control system, the raw gas is connected into the device, a mode I is selected on the main control computer 4, and parameters in the reaction process are controlled through the main control computer 4 according to experimental design parameters. The reaction parameter monitoring function is turned on, and the master control computer 4 automatically records the parameters such as the effect of the catalyst, the hydrolysis efficiency, the system desulfurization efficiency and the like at each stage under the reaction parameters. And (5) adjusting reaction parameters and recording the change condition of the data.
e) After all experiments are completed, the access of the crude gas is disconnected, the purging and diffusing function in the main control computer 4 is opened, the purging of the system is completed, all valves of the system are closed after the purging is completed, and the system is shut down.
Example 2
As shown in fig. 1, if the effect and the regeneration effect of a certain type of fine desulfurization adsorbent are evaluated in the experimental process, the specific implementation steps of the device are as follows:
a) The device is started, the purging and diffusing function in the main control computer 4 is opened after the device is started, purging and replacement of residual gas in a pipeline inside the device and two reaction towers (the hydrolysis and adsorption integrated tower 6 and the adsorption and regeneration integrated tower 7) are preferably completed, and the precise desulfurization adsorbent to be tested is required to be loaded into the reactor after purging operation is completed.
b) And opening the material changing doors on the hydrolysis adsorption regeneration integrated tower 6 and the adsorption regeneration integrated tower 7, removing residual samples in the towers, filling the precise desulfurization adsorbent to be evaluated into the hydrolysis adsorption regeneration integrated tower 6 and the adsorption regeneration integrated tower 7 after removing the residual samples, and sealing the material changing door 9 after filling.
c) After the packing operation is completed, the air tightness of the device needs to be detected, when the air leakage is detected, the next step is carried out, if the air leakage exists, the air leakage point needs to be checked, and the next step operation can not be carried out until the air tightness is detected.
d) After the air tightness is finished, the system is opened, after all valves of the electric control flow valve 2 are closed through the automatic control system, the crude gas is connected into the device, a mode II is selected on the main control computer 4, and parameters in the reaction process are controlled through the main control computer 4 according to experimental design parameters. The reaction parameter monitoring function is started, and the main control computer 4 automatically records parameters such as the effect of the adsorbent at each stage under the reaction parameters, the desulfurization efficiency of the system and the like. And (5) adjusting reaction parameters and recording the change condition of the data.
e) When the reaction is performed to a certain extent, a required reaction tower is selected for analysis and regeneration, a tower to be regenerated is selected in the main control computer 4, an analysis and regeneration system is started, at the moment, the electric heater 5 starts to work, the main control computer 4 can set the regeneration temperature, and the analysis and regeneration optimal time of the adsorbent can be judged according to the detection data of the sulfide online detector 3.
f) And switching the regeneration tower, and selecting a tower needing regeneration in the system, wherein the system automatically switches the other tower to enter the adsorption desulfurization operation. After a certain number of cycles, the inflection point of the adsorption effect of the adsorbent can be judged according to the detection data recorded by the main control computer 4.
g) And after all experiments are completed, cutting off gas access, opening a purging and diffusing function in the main control computer 4, completing purging of the system, closing all valves of the system after purging is completed, and shutting down.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The multifunctional gas fine desulfurization catalyst/adsorbent performance evaluation device is characterized by comprising a gas purification system, a regeneration analysis system, a blowing and diffusing system, an automatic control system and a reaction parameter monitoring system, wherein:
the gas purification system comprises a hydrolysis adsorption regeneration integrated tower (6) and an adsorption regeneration integrated tower (7), wherein gas inlets of the hydrolysis adsorption regeneration integrated tower (6) and the adsorption regeneration integrated tower (7) are connected with a gas outlet end of a raw gas pipeline and are used for removing sulfides in gas;
the regeneration analysis system is connected with the gas purification system through a pipeline and is used for analyzing and regenerating the invalid adsorbents in the hydrolysis adsorption regeneration integrated tower (6) and the adsorption regeneration integrated tower (7);
the purging and diffusing system is arranged at the air inlet end of the raw gas pipeline and is used for purging and replacing equipment of the whole device and gas in the pipeline;
the reaction parameter monitoring system comprises a sulfide online detector (3) and a reaction parameter detection table (10), wherein the sulfide online detector (3) is respectively connected with the gas inlet end of the crude gas pipeline, the gas outlet end of the gas purification system and the gas outlet end of the regeneration analysis system through sampling gas pipelines, and the reaction parameter detection table (10) is electrically connected with the gas purification system and the regeneration analysis system and is used for detecting the change condition of all reaction parameters in the whole reaction process of the front, middle and rear processes;
the automatic control system comprises a main control computer (4), a reaction parameter detection controller (8) and an electric control flow valve (2), wherein the signal input end of the reaction parameter detection controller (8) is electrically connected with the gas purification system, and the signal output end of the reaction parameter detection controller (8) is electrically connected with the main control computer (4) through a reaction parameter detection table (10); the electric control flow valve (2) is arranged on the pipeline and used for controlling the gas flow, and the sulfide online detector (3) and the electric control flow valve (2) are electrically connected with the main control computer (4).
2. The multifunctional gas fine desulfurization catalyst/adsorbent performance evaluation device according to claim 1, characterized in that: the gas purification system further comprises a gas fan (11), gas outlets of the hydrolysis adsorption regeneration integrated tower (6) and the adsorption regeneration integrated tower (7) are respectively connected with the gas fan (11) through pipelines, the gas outlet of the hydrolysis adsorption regeneration integrated tower (6) is also connected with a gas inlet of the adsorption regeneration integrated tower (7) through a pipeline, and an electric control flow valve (2) is arranged on the pipeline.
3. The multifunctional gas fine 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 tracing system, and the temperature control range is 20-300 ℃; the gas fan (11) adopts a centrifugal fan, the working temperature is 60-300 ℃, and the motor adopts an explosion-proof motor.
4. The multifunctional gas fine desulfurization catalyst/adsorbent performance evaluation device according to claim 2, characterized in that: the regeneration analysis system comprises an electric heater (5), an air inlet of the electric heater (5) is connected with a raw gas pipeline through a pipeline, an air outlet of the electric heater (5) is connected with a regeneration analysis air inlet of the hydrolysis adsorption regeneration integrated tower (6) and a regeneration analysis air inlet of the adsorption regeneration integrated tower (7) through pipelines respectively, and a regeneration analysis air outlet of the hydrolysis adsorption regeneration integrated tower (6) and a regeneration analysis air outlet of the adsorption regeneration integrated tower (7) are connected with a gas fan (11) through pipelines.
5. The multifunctional gas fine desulfurization catalyst/adsorbent performance evaluation device according to claim 4, characterized in that: the air inlet end of the electric heater (5), the regeneration analysis air inlet and the air outlet end of the hydrolysis adsorption regeneration integrated tower (6) and the regeneration analysis air inlet and the air outlet end of the adsorption regeneration integrated tower (7) are respectively provided with an electric control flow valve (2).
6. The multifunctional gas fine desulfurization catalyst/adsorbent performance evaluation device according to any one of claims 1 to 5, characterized in that: the purging and diffusing system is provided with a back-blowing pipeline which is connected with the air inlet end of the raw gas pipeline, and an electric control flow valve (2) is arranged on the back-blowing pipeline.
7. The multifunctional gas fine 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), wherein the sampling ports (1) are respectively arranged on the raw gas pipeline and the regeneration analysis gas pipeline; each sampling port (1) is connected with a sulfide online detector (3) through 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 electrically connected with the hydrolysis adsorption regeneration integrated tower (6) and the adsorption regeneration integrated tower (7) respectively.
8. A method for evaluating the performance of a multifunctional gas fine desulfurization catalyst/adsorbent, which is characterized in that the evaluation device as claimed in any one of claims 2 to 7 is adopted for test, and comprises the following two mode functions:
mode one, hydrolysis conversion and dry adsorption fine desulfurization process route;
mode two, adsorption regeneration fine desulfurization process route;
the specific operation is as follows:
the method comprises the steps of selecting a corresponding catalyst or adsorbent according to experimental requirements, firstly purging a device, filling the catalyst or adsorbent to be evaluated in a corresponding tower after purging, then performing air tightness detection, accessing the device into raw gas after detecting qualification, opening a system and adjusting the system to a corresponding mode, opening a gas fan (11), normally operating the system, controlling parameters of a reaction process through a main control computer (4) according to experimental requirements, opening a reaction parameter monitoring system function, and obtaining actual performance and effect of the catalyst or adsorbent in the system and total desulfurization efficiency of the system under the process by adjusting different reaction parameters.
9. The method for evaluating the performance of the multifunctional gas fine desulfurization catalyst/adsorbent according to claim 8, wherein when the process route of the mode one is selected, the specific evaluation method is as follows:
starting up, starting a purging and diffusing system, and completing purging and replacement of gas in equipment and pipelines;
step two, two towers are used in series in the mode, after residual samples in the two towers are cleaned, a catalyst is filled in a hydrolysis adsorption regeneration integrated tower (6), and an adsorbent is filled in an adsorption regeneration integrated tower (7);
detecting the overall air tightness of the device, and if an air leakage condition exists, checking the air leakage point until the air tightness is detected, and then entering the next operation;
step four, all the electric control flow valves (2) in the device are closed, raw gas is accessed, a mode one is selected in a main control computer (4), parameters in the reaction process and the opening of the relevant electric control flow valves (2) are controlled through the main control computer (4) according to experimental design parameters, and a reaction parameter monitoring system is started to monitor in real time;
step five, automatically recording and outputting experimental results under specific reaction parameters in the mode by a main control computer (4), wherein the experimental results comprise the effect of the catalyst at each stage, hydrolysis efficiency and system desulfurization efficiency parameters;
and step six, after the experiment is completed, the raw gas is disconnected, a purging and diffusing system is started, purging of the device is completed, and after purging is completed, all the electric control flow valves (2) are closed, and the device is shut down.
10. The method for evaluating the performance of the multifunctional gas fine desulfurization catalyst/adsorbent according to claim 8, wherein when the process route of the mode two is selected, the specific evaluation method is as follows:
step one, starting a purging and diffusing system to complete purging and replacement of gas in device equipment and pipelines;
step two, the hydrolysis function of the hydrolysis adsorption regeneration integrated tower (6) is not used in the mode, the hydrolysis adsorption regeneration integrated tower (6) and the adsorption regeneration integrated tower (7) are used in parallel, and according to experimental requirements, the switching of adsorption and regeneration of any one of the two towers is determined, and the two towers are filled with the adsorbent;
detecting the overall air tightness of the device, and if an air leakage condition exists, checking the air leakage point until the air tightness is detected, and then entering the next operation;
step four, all the electric control flow valves (2) in the device are closed, crude gas is accessed, a mode two is selected in the main control computer (4), parameters in the reaction process and the opening of the relevant electric control flow valves (2) are controlled through the main control computer (4) according to experimental design parameters, and meanwhile, a reaction parameter monitoring system is started for real-time monitoring;
step five, a main control computer (4) automatically records experimental results under specific reaction parameters in the mode, wherein the experimental results comprise the effect of the adsorbent at each stage and the system desulfurization efficiency parameters;
step six, when the tower to be reacted is required to be analyzed and regenerated, a main control computer (4) is used for controlling a regeneration analysis system to be started, the regeneration temperature is set, and the optimal analysis and regeneration time of the adsorbent is judged according to the monitoring data of the sulfide by a reaction parameter monitoring system;
step seven, switching another tower to perform adsorption desulfurization operation, wherein after multiple cycles, the detection data automatically recorded by the main control computer (4) are used for evaluating the inflection point of the adsorption effect of the adsorbent;
and step eight, after the experiment is completed, the raw gas is disconnected, a purging and bleeding system is started, purging of the device is completed, and after purging is completed, all the electric control flow valves (2) are closed, and the device is shut down.
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