CN115711950A - Construction method and use method of high-efficiency evaluation device for blast furnace gas desulfurization catalyst - Google Patents
Construction method and use method of high-efficiency evaluation device for blast furnace gas desulfurization catalyst Download PDFInfo
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- CN115711950A CN115711950A CN202211325136.0A CN202211325136A CN115711950A CN 115711950 A CN115711950 A CN 115711950A CN 202211325136 A CN202211325136 A CN 202211325136A CN 115711950 A CN115711950 A CN 115711950A
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- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 87
- 230000023556 desulfurization Effects 0.000 title claims abstract description 87
- 239000003054 catalyst Substances 0.000 title claims abstract description 82
- 238000011156 evaluation Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 29
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 62
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- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 31
- 239000011593 sulfur Substances 0.000 claims abstract description 31
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- 230000007062 hydrolysis Effects 0.000 claims description 29
- 238000006460 hydrolysis reaction Methods 0.000 claims description 29
- 239000007788 liquid Substances 0.000 claims description 20
- 239000006200 vaporizer Substances 0.000 claims description 17
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- 239000007789 gas Substances 0.000 description 70
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
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- 230000003301 hydrolyzing effect Effects 0.000 description 2
- YECIFGHRMFEPJK-UHFFFAOYSA-N lidocaine hydrochloride monohydrate Chemical compound O.[Cl-].CC[NH+](CC)CC(=O)NC1=C(C)C=CC=C1C YECIFGHRMFEPJK-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention belongs to the field of evaluation of blast furnace gas desulfurization agents, and relates to a construction method and a use method of a high-efficiency evaluation device for a blast furnace gas desulfurization catalyst. The using method comprises the following steps: judging the current connection mode of the device, and filling proper amounts of catalysts in the three reactors respectively; starting a water vaporization device and a tail gas condensation device; determining the feeding amount of raw material and water according to the required airspeed and catalyst loading; switching the on-off states of the A-type stop valve, the C-type stop valve and the B-type stop valve to control the current connection mode; controlling sulfur-containing gas and water feeds; setting three reactors to respective specified temperatures; starting an electromagnetic six-way valve at the outlet of the desulfurization reactor for automatic switching, and carrying out sampling analysis; and stopping sampling analysis when the total sulfur concentration of the tail gas is detected to be higher than 30ppm along with the extension of the reaction time. According to the scheme, the multiple reaction channels are highly integrated, and the desulfurization performance of different desulfurization catalysts can be efficiently evaluated and different working conditions can be efficiently screened.
Description
Technical Field
The invention belongs to the field of blast furnace desulfurization catalyst evaluation, and relates to a construction method and a use method of a high-efficiency evaluation device for a blast furnace gas desulfurization catalyst.
Background
The blast furnace gas is a byproduct containing CO and H in the blast furnace iron-making process 2 、CH 4 The combustible gas with equal components takes CO as the main component and accounts for about 28 to 33 percent of the total composition of the gas. In addition, it also contains CO 2 、O 2 、N 2 Especially containing H 2 S、COS、CS 2 And after the sulfur-containing gas and the blast furnace gas which is not subjected to desulfurization treatment are combusted, the blast furnace gas is directly discharged to seriously pollute the environment. The blast furnace gas can be directly discharged after being desulfurized to reach the standard and then used by users, and the operation maintenance cost of the environment-friendly device of the iron and steel enterprises can be effectively reduced. The sulfur-containing substances of blast furnace gas mainly contain organic sulfur such as COS and the like, and can be converted into H through hydrolysis 2 And removing the S. The desulfurization catalyst (desulfurizer for short) plays a decisive role in whether the desulfurization treatment reaches the standard or not, the desulfurization performance of the desulfurization catalyst can be evaluated through the working sulfur capacity, and the working sulfur capacity is defined as follows: the total weight of the sulfur simple substance which can be removed by the desulfurization catalyst per unit mass within the range of ensuring the emission to reach the standard.
The evaluation period of the working sulfur capacity of the desulfurization catalyst is long, so that the working efficiency is low. CN 111579708A discloses an activity evaluation device and method for a desulfurization catalyst, wherein the evaluation device can realize the evaluation of deoxidizing agent, organic sulfur hydrolytic agent and hydrogen sulfide adsorbent on the deoxidation, organic sulfur hydrolysis and hydrogen sulfide adsorption effects of blast furnace gas with different compositions by flexibly adjusting the ratio of each component of inlet air, but cannot solve the high-efficiency evaluation of the working sulfur capacity of different desulfurization catalysts and the desulfurization performance evaluation of different desulfurization catalysts under different working conditions. Therefore, on the premise of ensuring the integrated evaluation of three processes of the simulated blast furnace gas pretreatment, the organic sulfur hydrolysis and the desulfurization, how to efficiently evaluate the desulfurization performance of different desulfurization catalysts and efficiently screen different working conditions is still an important technical problem.
Disclosure of Invention
In view of the above, the invention aims to provide a building method and a using method of a high-efficiency evaluation device for a blast furnace gas desulfurization catalyst, so as to overcome the defects that the existing desulfurization catalyst evaluation device cannot efficiently screen desulfurization catalysts with different formulas and cannot efficiently screen the optimal use working conditions of the desulfurization catalysts, so as to shorten the evaluation period of the desulfurization catalysts and improve the working efficiency.
In order to achieve the purpose, the invention provides the following technical scheme:
the construction method of the high-efficiency evaluation device for the blast furnace gas desulfurization catalyst comprises the following steps: the method comprises the following steps that three feeding pipelines are arranged, the inlet end of each feeding pipeline is respectively connected with an air inlet branch and a water inlet steam branch, a gas flow controller is arranged on the air inlet branch, and a plunger pump and a vaporizer are arranged on the water inlet branch; connecting each feeding pipeline with a reaction pipe through an A-type stop valve respectively, and sleeving a heater on each reaction pipe; connecting each reaction tube with a gas-liquid separator through a C-type stop valve, respectively winding a coil pipe on a pipeline between each reaction tube and the corresponding connected gas-liquid separator, and respectively connecting a water cooler at two ends of each coil pipe; each gas-liquid separator is respectively connected with a gas phase pipeline and a water drainage pipeline, and a needle valve, an electromagnetic six-way valve and a gas chromatography are sequentially connected at a gas phase outlet; a communicating pipeline is arranged between every two reaction tubes, and the outlet of one reaction tube is connected with the inlet of the other reaction tube through a B-type stop valve by each communicating pipeline.
The invention also provides a using method of the high-efficiency evaluation device for the blast furnace gas desulfurization catalyst, and the device built based on the building method of the high-efficiency evaluation device for the blast furnace gas desulfurization catalyst comprises the following steps:
s1: judging the current connection mode of the device, and filling proper amounts of catalysts in the three reactors respectively; starting a water vaporization device and a tail gas condensation device; determining the feed amount of raw material and water according to the required airspeed and catalyst loading;
s2: switching the on-off states of the A-type stop valve, the B-type stop valve and the C-type stop valve to control the current connection mode;
s3: controlling sulfur-containing gas and water feeds;
s4: setting three reactors to respective specified temperatures;
s5: starting an electromagnetic six-way valve at the outlet of the desulfurization reactor for automatic switching, and carrying out sampling analysis; when the total sulfur concentration of the tail gas is detected to be higher than 30ppm along with the extension of the reaction time, the sampling analysis is stopped.
Further, in the S1, the connection mode includes a series mode and a parallel mode; the series mode is used for simulating series reaction mode evaluation of dechlorination, hydrolysis and desulfurization, and the parallel mode is used for evaluating desulfurization performance of different desulfurization catalysts.
Further, in the S1, when the connection mode is the series mode, the three reactors are sequentially filled with a dechlorination catalyst, an organic sulfur hydrolysis catalyst and a desulfurization catalyst in a gas flow direction; the reaction tube filled with dechlorination catalyst is a pretreatment reactor, the reaction tube filled with hydrolysis catalyst is an organic sulfur hydrolysis reactor, and the reaction tube filled with desulfurization catalyst is a desulfurization reactor; when the connection mode is the parallel mode, appropriate amount of desulfurization catalysts with different formulas are respectively filled in the three reactors.
Further, in S2, the method for controlling the current connection mode to be the series mode includes: switching and opening a B-type stop valve between the pretreatment reactor and the organic sulfur hydrolysis reactor, opening a B-type stop valve between the organic sulfur hydrolysis reactor and the desulfurization reactor, closing an A-type stop valve for feeding blast furnace gas of the organic sulfur hydrolysis reactor and the desulfurization reactor respectively, closing a C-type stop valve between an outlet of the dechlorination reactor and the cooler, closing a C-type stop valve between the outlet of the organic sulfur hydrolysis reactor and the cooler, and opening a C-type stop valve between the desulfurization reactor and the cooler.
Further, in S2, the method for controlling the current connection mode to be the parallel mode includes: and closing a class B stop valve between the reactors, opening class A stop valves for feeding the reactors respectively, and opening a class C stop valve between the outlet of the reactor and the gas-liquid separator.
The invention has the beneficial effects that:
the scheme can realize flexible switching of dechlorination, organic sulfur hydrolysis and desulfurization series reaction and parallel three-channel desulfurization reaction evaluation, particularly can quickly screen out a better desulfurization catalyst or quickly screen out a better reaction condition aiming at the same desulfurization catalyst according to experimental requirements, and has the advantages of flexible operation and high efficiency.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the means of the instrumentalities and combinations particularly pointed out hereinafter.
Drawings
For the purposes of promoting a better understanding of the objects, aspects and advantages of the invention, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:
fig. 1 is a schematic diagram of a high-efficiency evaluation device for a blast furnace gas desulfurization catalyst capable of switching between series-parallel modes.
Reference numerals are as follows: the system comprises a feeding system 1, a reaction system 2, a collecting system 3, a first organic sulfur raw material gas mass flow controller 4, a second organic sulfur raw material gas mass flow controller 7, a third organic sulfur raw material gas mass flow controller 10, a first feeding water vaporizer 5, a second feeding water vaporizer 8, a third feeding water vaporizer 11, a first plunger pump 6, a second plunger pump 9, a third plunger pump 12, a first class A stop valve 13, a second class A stop valve 14, a third class A stop valve 15, a first class B stop valve 18, a second class B stop valve 21, a first class D stop valve 25, a second class D stop valve 27, a third class D stop valve 29, a first class C stop valve 30, a second class C stop valve 31, a third class C stop valve 32, a first reaction tube 16, a first electric heating furnace 17, a second reaction tube 19, a second electric heating furnace 20, a third reaction tube 22, a third electric heating furnace 23, a first cooler 24, a second cooler 26, a third cooler 28, a first water cooler 33, a second water cooler 34, a third water-cooling machine 35, a first gas-liquid separator 37, a third gas-liquid separator 38, a first back pressure valve 39, a second back pressure valve 40 and a third back pressure valve 41.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It should be noted that the drawings provided in the following embodiments are only for illustrating the basic idea of the present invention in a schematic way, and the features in the following embodiments and examples may be combined with each other without conflict.
Wherein the showings are for the purpose of illustrating the invention only and not for the purpose of limiting the same, and in which there is shown by way of illustration only and not in the drawings in which there is no intention to limit the invention thereto; to better illustrate the embodiments of the present invention, some parts of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.
The same or similar reference numerals in the drawings of the embodiments of the present invention correspond to the same or similar components; in the description of the present invention, it should be understood that if there is an orientation or positional relationship indicated by terms such as "upper", "lower", "left", "right", "front", "rear", etc., based on the orientation or positional relationship shown in the drawings, it is only for convenience of description and simplification of description, but it is not an indication or suggestion that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and therefore, the terms describing the positional relationship in the drawings are only used for illustrative purposes, and are not to be construed as limiting the present invention, and the specific meaning of the terms may be understood by those skilled in the art according to specific situations.
Referring to fig. 1, the device is constructed for the method for constructing the high-efficiency evaluation device for the blast furnace gas desulfurization catalyst.
The specific building steps comprise:
building a pipeline: connecting an upstream pipeline at the inlet end of the stop valve, and connecting a downstream pipeline at the outlet end of the stop valve to form a communication pipeline, and preparing eleven communication pipelines; connecting a gas phase inlet pipeline at the inlet end of the back pressure valve, and connecting a gas phase outlet pipeline at the outlet end of the back pressure valve to form a gas phase pipeline, and preparing three gas phase pipelines;
building a feeding mechanism: the two ends of the gas flow controller are respectively connected with a gas inlet pipeline and a gas outlet pipeline, the two ends of the plunger pump are respectively connected with a water inlet pipeline and a water outlet pipeline, the water outlet pipeline is connected with the vaporizer, the other end of the vaporizer is connected with the gas outlet pipeline to form a main pipeline, and the three same main pipelines form a feeding mechanism;
building a reaction mechanism: preparing three reaction tubes, respectively connecting a feeding pipeline and a discharging pipeline at two ends of each reaction tube, and respectively connecting three main pipelines with one reaction tube through a communication pipeline, wherein each main pipeline is respectively connected with an upstream pipeline, and a feeding pipeline is respectively connected with a downstream pipeline which is positioned in the same communication pipeline with the upstream pipeline; a communicating pipeline is arranged between every two reaction tubes, wherein the upstream pipeline is connected with the discharging pipeline of one reaction tube, and the downstream pipeline which is positioned in the same communicating pipeline with the upstream pipeline is connected with the feeding pipeline of the other reaction tube;
building a collection mechanism: the discharge pipeline of each reaction pipe is connected with a gas-liquid separator through a communication pipeline, wherein the upstream pipeline is connected with the discharge pipeline, and the downstream pipeline is connected with the inlet end of the gas-liquid separator; a coil pipe is wound on the downstream pipeline, and two ends of the coil pipe are connected with a water cooling machine; a gas phase pipeline is arranged at a gas outlet of each gas-liquid separator, the gas outlet is connected with a gas phase inlet pipeline, a water outlet of each gas-liquid separator is connected with a water drainage pipeline through a communication pipeline, and the same water drainage pipeline is connected in the embodiment;
building a monitoring mechanism: an electronic balance is arranged below the plunger pump, a thermocouple is arranged in the reaction tube, and an air pressure sensor is arranged on the gas phase inlet pipeline;
constructing an analysis mechanism: the gas outlet pipeline is connected with a needle valve, an electromagnetic six-way valve and a gas chromatograph in sequence.
In one embodiment, the gas flow controller can be selected as an organosulfur feedstock gas mass flow controller.
The scheme also provides a using method of the high-efficiency evaluation device for the blast furnace gas desulfurization catalyst, and the using method comprises the following steps:
s1: judging the current connection mode of the device, and filling proper amounts of catalysts in the three reactors respectively; when the connection mode is a series connection mode, a dechlorination catalyst, an organic sulfur hydrolysis catalyst and a desulfurization catalyst are filled in the three reactors in sequence according to the gas flow direction; the reaction tube filled with dechlorination catalyst is a pretreatment reactor, the reaction tube filled with hydrolysis catalyst is an organic sulfur hydrolysis reactor, and the reaction tube filled with desulfurization catalyst is a desulfurization reactor; when the connection mode is the parallel mode, appropriate amount of desulfurization catalysts with different formulas are respectively filled in the three reactors; after the catalyst is filled, starting a water vaporization device and a tail gas condensation device; the feed of feed gas and water is determined according to the desired space velocity and catalyst loading.
S2: switching the on-off states of the A-type stop valve, the C-type stop valve and the B-type stop valve to control the current connection mode; the control method of the series mode comprises the following steps: switching and opening a B-type stop valve between the pretreatment reactor and the organic sulfur hydrolysis reactor, opening a B-type stop valve between the organic sulfur hydrolysis reactor and the desulfurization reactor, closing an A-type stop valve for feeding blast furnace gas of the organic sulfur hydrolysis reactor and the desulfurization reactor respectively, closing a C-type stop valve between an outlet of the dechlorination reactor and the cooler, closing a C-type stop valve between the outlet of the organic sulfur hydrolysis reactor and the cooler, and opening a C-type stop valve between the desulfurization reactor and the cooler; the parallel mode control method comprises the following steps: and closing the B-class stop valve between the reactors, opening the A-class stop valves for feeding the reactors respectively, and opening the C-class stop valve between the outlet of the reactor and the gas-liquid separator.
S3: after switching to the corresponding connection mode, the sulfur-containing gas and water feeds are controlled.
S4: three reactors were set to respective specified temperatures.
S5: starting an electromagnetic six-way valve at the outlet of the desulfurization reactor for automatic switching, and carrying out sampling analysis; when the total sulfur concentration of the tail gas is detected to be higher than 30ppm along with the extension of the reaction time, the sampling analysis is stopped.
Specifically, the method comprises the following steps:
in the series mode, the method comprises the following steps:
1) Loading a catalyst: and a certain amount of dechlorinating agent, organic sulfur hydrolytic agent and desulfurization catalyst are respectively filled in the first reaction pipe 16, the second reaction pipe 19 and the third reaction pipe 22.
2) Starting a heating and condensing device: and starting the third vaporizer 11 and setting the temperature of the third vaporizer to be 120 ℃, starting the third cooler 28 and the third water cooler 35, and setting the water cooling temperature to be 5 ℃. And closing the first vaporizer 5, the second vaporizer 8, the first cooler 24, the second cooler 26, the first water cooler 33 and the second water cooler 34. And after all heaters and condensers are heated to the required temperature, the step 3) is carried out.
3) Starting feeding: opening a class A stop valve III 15, a class B stop valve I18, a class B stop valve II 21 and a class C stop valve 32, and closing a class mass flow controller I4, a class mass flow controller II 7, a plunger pump I6, a plunger pump II 9, a class A stop valve I13, a class A stop valve II 14, a class D stop valve 29, a class C stop valve 30 and a class C stop valve 31. Setting the mass flow controller three 10 and the plunger pump three 12 to specified values, and turning on the mass flow controller three 10 and the plunger pump three 12. Back pressure valve three 41 is set to the desired reaction pressure.
4) Starting a heating furnace: respectively setting the temperature of a first electric heating furnace 17 at 130 ℃, the temperature of a second electric heating furnace 20 at 80 ℃ and the temperature of a third electric heating furnace 23 at 80 ℃.
5) Sampling and analyzing: and after all the heating furnaces rise to the specified temperature and are stabilized for 30-60 min, starting automatic sampling of the tail gas of the degassing chromatography arranged at the gas outlet of the gas-liquid separator III 38 for sampling analysis.
6) And (4) finishing the experiment: and stopping sampling analysis after the total sulfur concentration in the tail gas of the gas chromatography exceeds 30 ppm. And (3) closing the first electric heating furnace 17, the second electric heating furnace 20 and the third electric heating furnace 23, fully opening the third backpressure valve 41 to release pressure, closing the third mass flow controller 10 and the third plunger pump 12, closing the third vaporizer 11, closing the third cooler 28 and the third water cooler 35, opening the D-type stop valve 29 to drain water, and finishing the reaction evaluation.
In parallel mode, the method comprises the following steps:
1) Loading a catalyst: three desulfurization catalysts with different formulas are respectively filled in the first reaction tube 16, the second reaction tube 19 and the third reaction tube 22.
2) Starting a heating and condensing device: and starting all the vaporizers and setting the temperature of the vaporizers to be 120 ℃, starting all the coolers and the water coolers, and setting the water cooling temperature to be 5 ℃. And 3) after all the electric heaters and the water cooling machines reach the required temperature, performing step 3).
3) Starting feeding: all A-class stop valves (a-class stop valve I13, A-class stop valve II 14 and A-class stop valve III 15) and all C-class stop valves (C-class stop valve 30, C-class stop valve 31 and C-class stop valve 32) are opened, all mass flow controllers (organic sulfur raw material gas mass flow controller I4, organic sulfur raw material gas mass flow controller II 7 and organic sulfur raw material gas mass flow controller III 10) and all plunger pumps (plunger pump I6, plunger pump II 9 and plunger pump III 12) are set to be specified values, and the mass flow controllers and the plunger pumps are opened. All back pressure valves (a back pressure valve I39, a back pressure valve II 40, a back pressure valve III 41) are set to the required reaction pressure respectively.
4) Starting a heating furnace: the temperature of all the electric heating furnaces (the first electric heating furnace 17, the second electric heating furnace 20 and the third electric heating furnace 23) is set to be 80 ℃.
5) Sampling and analyzing: and after all the electric heating furnaces are heated to the specified temperature and stabilized for 30-60 min, starting automatic program sampling of the gas chromatographic tail gas at all the gas outlet ports for sampling analysis.
6) And (4) finishing the experiment: and stopping sampling analysis after the total sulfur concentration in the three paths of tail gases exceeds 30 ppm. And closing all heating furnaces, fully opening all back pressure valves for pressure relief, closing all mass flow controllers and all plunger pumps, closing all vaporizers, closing all coolers and all water coolers, opening all D-type stop valves (a D-type stop valve 25, a D-type stop valve 27 and a D-type stop valve 29) for drainage, and finishing the reaction evaluation.
Three-channel parallel reactors of the parallel desulfurization catalyst are not interfered with each other, and the operation of the three groups of parallel reaction tubes when the experiment is finished can be flexibly adjusted. For example, if the total sulfur concentration detected in one degassing chromatography tail gas is higher than 30ppm, and the total sulfur concentration detected in the other two degassing chromatography tail gases is still lower than 30ppm, the first electric heating furnace 17 is closed, the first backpressure valve 39 is fully opened to release pressure, the third mass flow controller 10 and the third plunger pump 12 are closed, the third vaporizing tube 11 is closed, the first cooler 24 and the first water cooler 33 are closed, the drain water of the class D stop valve 25 is opened, and the rest of the components are kept unchanged, and the evaluation of the second reaction tube 19 and the third reaction tube 22 is continued. The rest similar experimental conditions can be flexibly adjusted according to specific situations.
The classification of a, B, C, and D of the stop valve in this embodiment does not represent the specific model of the stop valve, but is divided according to the actual functions of the stop valve at different positions, and should not be considered as limiting the model of the stop valve.
Two specific experimental examples are listed below:
example 1:
preparation H 2 S、COS、HCl、O 2 、CO、CO 2 、N 2 Sulfur-containing gases at concentrations of 35ppm, 45ppm, 10ppm, 0.1%, 25%, 49.9% were charged with dechlorination catalyst, organosulfur hydrolysis catalyst and desulfurization catalyst, respectively, to reactors 16, 19, 22. The temperature of the water vaporizer 11 is set to 105 ℃, the temperature of the low-temperature circulating water of the water cooler 35 is set to 5 ℃, and the circulating water is started. The shut-off valves 30, 31 are closed, the shut-off valves 18, 21, 32 are opened and the three reactors are switched to the series operating mode. The feed flow rate of the mass flow controller 10 was started to 300mL/min, and the water concentration after gasification was controlled to 5% by starting the plunger pump 12. The reaction temperatures of the heating furnaces 17, 20, 23 were set at 130 ℃, 80 ℃ respectively, and after the reaction temperature was raised to the specified reaction temperature, the reaction temperature was raised from the outlet of the back pressure valve 41And analyzing the outlet total sulfur concentration, and stopping the test when the outlet total sulfur concentration is higher than 30ppm, wherein the working sulfur capacity of the desulfurization catalyst is 40%. The pressure of the reaction device is relieved through a backpressure valve 41, condensed water in a gas-liquid separator 38 is discharged through a stop valve 29, all heating furnaces are closed, a plunger pump 12 and a vaporizer 11 are closed, a water cooler 35 is closed, and after all heating and condensing devices return to the room temperature, a mass flow controller 10 is closed, so that the experiment is finished.
Example 2:
preparation H 2 S、COS、O 2 、CO、CO 2 、N 2 The sulfur-containing gases with concentrations of 35ppm, 45ppm, 0.1%, 25%, 49.9% respectively fill three desulfurization catalysts with different formulas into the reactors 16, 19, 22 respectively. The temperatures of the water vaporization devices 5, 8 and 11 are respectively set to be 105 ℃, the temperatures of the low-temperature circulating water of the water cooling machines 33, 34 and 35 are all set to be 5 ℃, and the circulating water is started. The shut-off valves 18, 21 are closed, the shut-off valves 30, 31, 32 are opened and the three reactors are switched to a parallel mode of operation. The feed flow of the mass flow controllers 4, 7 and 10 is started to be 300mL/min, the plunger pumps 6, 9 and 12 are started, and the concentration of gasified inlet water is controlled to be 5%. The reaction temperatures of the heating furnaces 17, 20, 23 were all set to 80 ℃, and after the reaction temperature had risen to the specified reaction temperature, the outlet total sulfur concentrations were analyzed from the outlets of the back pressure valves 39, 40, 41, respectively. After 15 hours, the gas chromatography detects that the total sulfur concentration of the tail gas outlet at the outlet of the back pressure valve 39 is higher than 30ppm, the working sulfur capacity of the desulfurization catalyst in the reactor 16 is 21%, the pressure is relieved through the back pressure valve 39, the heating furnace 17 is closed, the condensed water in the gas-liquid separator 36 is discharged through the stop valve 25, the vaporizer 11 and the water cooler 33 are closed, the plunger pump 12 is closed, and the mass flow controller 10 is closed after all heating and condensing devices recover to the room temperature; after 23 hours, detecting that the total sulfur concentration of tail gas at the outlet of the back pressure valve 40 is higher than 30ppm by gas chromatography, wherein the working sulfur capacity of the desulfurization catalyst in the reactor 19 is 33 percent, releasing pressure by the back pressure valve 40, closing the heating furnace 20, discharging condensed water in the gas-liquid separator 37 by the stop valve 27, closing the vaporizer 8 and the water cooler 34, closing the plunger pump 9, and closing the mass flow controller 7 after all heating and condensing devices recover to room temperature; after 41 hours, the gas chromatography detects the tail gas at the outlet of the back pressure valve 41The total sulfur concentration is higher than 30ppm, at this time, the working sulfur capacity of the desulfurization catalyst in the reactor 22 is 41%, the pressure is relieved through the backpressure valve 41, the heating furnace 23 is closed, the condensed water in the gas-liquid separator 38 is discharged through the stop valve 29, the vaporizer 5 and the water cooler 35 are closed, the plunger pump 6 is closed, after all the heating and condensing devices are returned to the room temperature, the mass flow controller 4 is closed, and the whole experiment is ended.
The above examples show that the evaluation device and the evaluation method provided by the invention can not only carry out serial evaluation on dechlorination, organic sulfur hydrolysis and desulfurization catalysts, but also simultaneously evaluate three desulfurization catalysts with different formulas in parallel or efficiently screen optimal reaction conditions for the desulfurization catalyst with the same formula, and have the advantages of high efficiency, short period and accelerated project progress.
Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.
Claims (6)
1. The construction method of the high-efficiency evaluation device for the blast furnace gas desulfurization catalyst is characterized by comprising the following steps of: the method comprises the following steps that three feeding pipelines are arranged, the inlet end of each feeding pipeline is respectively connected with an air inlet branch and a water inlet steam branch, a gas flow controller is arranged on the air inlet branch, and a plunger pump and a vaporizer are arranged on the water inlet branch; connecting each feeding pipeline with a reaction pipe through an A-type stop valve respectively, and sleeving a heater on each reaction pipe; connecting each reaction tube with a gas-liquid separator through a C-type stop valve, respectively winding a coil pipe on a pipeline between each reaction tube and the corresponding connected gas-liquid separator, and respectively connecting a water cooler at two ends of each coil pipe; each gas-liquid separator is respectively connected with a gas phase pipeline and a water drainage pipeline, and a needle valve, an electromagnetic six-way valve and a gas chromatography are sequentially connected at a gas phase outlet; a communicating pipeline is arranged between every two reaction tubes, and the outlet of one reaction tube is connected with the inlet of the other reaction tube through a B-type stop valve by each communicating pipeline.
2. The use method of the high-efficiency evaluation device of the blast furnace gas desulfurization catalyst is characterized by comprising the following steps of: the device constructed based on the construction method of the high efficiency evaluation device for the desulfurization catalyst for blast furnace gas according to claim 1, comprises the following steps:
s1: judging the current connection mode of the device, and filling proper amounts of catalysts in the three reactors respectively; starting a water vaporization device and a tail gas condensation device; determining the feeding amount of raw material and water according to the required airspeed and catalyst loading;
s2: switching the on-off states of the A-type stop valve, the B-type stop valve and the C-type stop valve to control the current connection mode;
s3: controlling sulfur-containing gas and water feeds;
s4: setting three reactors to respective specified temperatures;
s5: starting an electromagnetic six-way valve at the outlet of the desulfurization reactor for automatic switching, and carrying out sampling analysis; when the total sulfur concentration of the tail gas is detected to be higher than 30ppm along with the extension of the reaction time, the sampling analysis is stopped.
3. The method of using the high-efficiency evaluation apparatus for a blast furnace gas desulfurization catalyst according to claim 2, characterized in that: in the S1, the connection mode includes a series mode and a parallel mode; the series mode is used for simulating series reaction mode evaluation of dechlorination, hydrolysis and desulfurization, and the parallel mode is used for evaluating desulfurization performance of different desulfurization catalysts.
4. The method of using the high efficiency evaluation apparatus for a blast furnace gas desulfurization catalyst according to claim 3, characterized in that: in the S1, when the connection mode is a series connection mode, a dechlorination catalyst, an organic sulfur hydrolysis catalyst and a desulfurization catalyst are filled in the three reactors in sequence according to the gas flow direction; the reaction tube filled with dechlorination catalyst is a pretreatment reactor, the reaction tube filled with hydrolysis catalyst is an organic sulfur hydrolysis reactor, and the reaction tube filled with desulfurization catalyst is a desulfurization reactor; when the connection mode is a parallel connection mode, appropriate desulfurization catalysts with different formulas are respectively filled in the three reactors.
5. The method of using the high efficiency evaluation apparatus for a blast furnace gas desulfurization catalyst according to claim 4, wherein the step of controlling the current connection mode to the series mode in S2 comprises: switching and opening a B-type stop valve between the pretreatment reactor and the organic sulfur hydrolysis reactor, opening a B-type stop valve between the organic sulfur hydrolysis reactor and the desulfurization reactor, closing an A-type stop valve for respective blast furnace gas feeding of the organic sulfur hydrolysis reactor and the desulfurization reactor, closing a C-type stop valve between an outlet of the dechlorination reactor and the cooler, closing a C-type stop valve between the outlet of the organic sulfur hydrolysis reactor and the cooler, and opening a C-type stop valve between the desulfurization reactor and the cooler.
6. The method for using a high-efficiency evaluation apparatus for a blast furnace gas desulfurization catalyst according to claim 4, wherein the step S2 of controlling the current connection mode to be the parallel mode includes: and closing the B-class stop valve between the reactors, opening the A-class stop valves for feeding the reactors respectively, and opening the C-class stop valve between the outlet of the reactor and the gas-liquid separator.
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| CN117030920A (en) * | 2023-08-03 | 2023-11-10 | 北京铝能清新环境技术有限公司 | Performance test device and method for integral skid-mounted blast furnace gas fine desulfurization agent |
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| CN204214820U (en) * | 2014-08-28 | 2015-03-18 | 天津市鹏翔科技有限公司 | A kind of integrating device for hydrogenation process evaluating catalyst |
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| CN114994233A (en) * | 2022-06-29 | 2022-09-02 | 重庆赛迪热工环保工程技术有限公司 | Blast furnace gas desulfurization catalyst evaluation device and method |
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| CN204214820U (en) * | 2014-08-28 | 2015-03-18 | 天津市鹏翔科技有限公司 | A kind of integrating device for hydrogenation process evaluating catalyst |
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| CN114994233A (en) * | 2022-06-29 | 2022-09-02 | 重庆赛迪热工环保工程技术有限公司 | Blast furnace gas desulfurization catalyst evaluation device and method |
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| CN117030920A (en) * | 2023-08-03 | 2023-11-10 | 北京铝能清新环境技术有限公司 | Performance test device and method for integral skid-mounted blast furnace gas fine desulfurization agent |
| CN117030920B (en) * | 2023-08-03 | 2024-04-12 | 北京铝能清新环境技术有限公司 | Performance test device and method for integral skid-mounted blast furnace gas fine desulfurization agent |
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