CN219162025U - Device for quantitatively generating low-dose steam and guiding low-dose steam into thermal analyzer - Google Patents

Device for quantitatively generating low-dose steam and guiding low-dose steam into thermal analyzer Download PDF

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CN219162025U
CN219162025U CN202320035441.XU CN202320035441U CN219162025U CN 219162025 U CN219162025 U CN 219162025U CN 202320035441 U CN202320035441 U CN 202320035441U CN 219162025 U CN219162025 U CN 219162025U
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thermal analyzer
low
mixer
steam
dose
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付娟
苏秋成
郎林
李焱冰
陈凯悦
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Guangzhou Institute of Energy Conversion of CAS
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Guangzhou Institute of Energy Conversion of CAS
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Abstract

The utility model relates to the technical field of thermal analysis in-situ reaction, in particular to a device for quantitatively generating low-dose steam and leading the low-dose steam into a thermal analyzer, which is matched with the thermal analyzer for use, wherein a mixer is respectively communicated with a vaporization chamber, a gas source and the thermal analyzer, and the vaporization chamber is communicated with a feed pump and a liquid storage tank; a first electromagnetic valve is connected between the liquid storage tank and the vaporization chamber, and a second electromagnetic valve is connected between the gas source and the mixer. Aiming at the problems of low-dosage quantitative generation and introduction of low-dosage steam with humidity being accurately controlled in the adsorption experiment with lower temperature and the low-temperature catalytic conversion thermal analysis testing process, the steam inlet amount can be accurately controlled, the device is suitable for the adsorption experiment and the low-temperature catalytic conversion experiment, and simultaneously can meet the requirements of a steam inlet device for biomass and solid waste thermochemical conversion and catalytic conversion thermal analysis research, the low-dosage quantitative generation and introduction of the low-dosage steam with the humidity being accurately controlled into a thermal analyzer is realized, and the accuracy and the importance of the measurement in the reaction process are ensured.

Description

Device for quantitatively generating low-dose steam and guiding low-dose steam into thermal analyzer
Technical Field
The utility model relates to the technical field of thermal analysis in-situ reaction, in particular to a device for quantitatively generating low-dose steam and guiding the low-dose steam into a thermal analyzer.
Background
In the research of biomass and solid waste recycling pyrolysis, gasification and catalytic conversion, the temperature and the humidity play a vital role in the reaction process, the thermal analysis simulates the reaction process of biomass and solid waste recycling pyrolysis, gasification and catalytic conversion, the reaction mechanism is researched, and important reference data is provided for the thermodynamic and kinetic research of the reaction. The conventional thermal analyzer does not have a humidity control module, the commercial steam module needs to be matched with a steam furnace for use, and the temperature range is limited, for example, some steam manufacturers limit the inlet temperature of steam to be more than 150 ℃ because of larger steam quantity. In this case, the adsorption experiment and the low-temperature catalytic conversion experiment at a relatively low temperature cannot be performed. There is therefore a need for a device for the quantitative generation of low doses of water vapor for introduction into a thermal analyzer that allows precise control of humidity.
The patent application with publication number CN105716062A discloses a water vapor generating device for quantitatively controlling the vapor amount at an outlet and a using method, wherein the water vapor generating device comprises a vapor generator, a condenser and an outlet of the vapor generator, wherein the outlet of the vapor generator is connected with a first regulating valve through a water vapor output pipe, and a pipeline passing through the first regulating valve is divided into two branches, namely a vapor outlet branch and a vapor reflux branch; the vapor outlet branch sequentially passes through a second regulating valve and a pressure gauge, and then passes through a fifth regulating valve to output vapor; the steam reflux branch is connected with the water storage tank after passing through the third regulating valve.
The device is suitable for a small-sized water vapor generating device developed in a laboratory or fine chemicals, can realize quantitative vaporization of water vapor, but has large vaporization amount of water vapor and cannot meet the requirements of thermal analysis experiments under different humidity control.
Therefore, there is a need for a device for quantitatively generating low-dose water vapor and introducing the low-dose water vapor into a thermal analyzer, which can accurately control the water amount, and can accurately control the mixing of gas and water vapor by combining a mass flowmeter, so as to realize the control of the gas humidity and the introduction of the low-dose water vapor into the thermal analyzer.
Disclosure of Invention
The utility model aims at: in order to solve the problems in the prior art, the utility model provides a device for quantitatively generating low-dose water vapor and guiding the low-dose water vapor into a thermal analyzer.
In order to solve the problems existing in the prior art, the utility model adopts the following technical scheme:
the device for quantitatively generating low-dose steam and guiding the low-dose steam into the thermal analyzer is matched with the thermal analyzer to use, and comprises a liquid storage tank, a feed pump, a vaporization chamber, a gas source, a mixer, a first electromagnetic valve and a second electromagnetic valve;
the mixer is respectively communicated with the vaporization chamber, the gas source and the thermal analyzer, the vaporization chamber is also communicated with the feed pump, and the feed pump is communicated with the liquid storage tank;
the liquid storage tank is connected with the first electromagnetic valve between the vaporization chamber, and the second electromagnetic valve is connected between the gas source and the mixer.
As an improvement of the technical scheme of the device for quantitatively generating low-dose steam and leading the low-dose steam into the thermal analyzer, the vaporizing chamber is communicated with the mixer through a first transmission pipe, the first transmission pipe is a transmission pipe with heat tracing, and/or the mixer is a mixer with heat tracing.
As an improvement of the technical scheme of the device for quantitatively generating low-dose steam and leading the low-dose steam into the thermal analyzer, the feeding pump and the first flowmeter are connected between the liquid storage tank and the vaporizing chamber, and the feeding pump and the first flowmeter are connected at the upstream position of the first electromagnetic valve.
As an improvement of the device for quantitatively generating low-dose steam for introduction into a thermal analyzer, the feeding pump is connected with the first controller.
As an improvement of the technical scheme of the device for introducing low-dose steam quantitative generation into the thermal analyzer, the device for introducing low-dose steam quantitative generation into the thermal analyzer further comprises a solenoid valve controller, wherein the solenoid valve controller is respectively connected with the first solenoid valve and the second solenoid valve.
As an improvement of the technical scheme of the device for quantitatively generating low-dose steam and leading the low-dose steam into the thermal analyzer, the feeding pump is a low-dose pulse quantitative feeding pump.
As an improvement of the technical scheme of the device for quantitatively generating low-dosage water vapor and leading the low-dosage water vapor into the thermal analyzer, a first mass flowmeter and a first pressure reducing valve are also connected between the gas source and the mixer.
As an improvement of the technical scheme of the device for quantitatively generating low-dose steam and leading the low-dose steam into the thermal analyzer, the mixer is communicated with the thermal analyzer through a second transmission pipe, and the second transmission pipe is a transmission pipe with heat tracing.
As an improvement of the technical scheme of the device for quantitatively generating low-dosage steam and leading the low-dosage steam into the thermal analyzer, the second transmission pipe is connected with a third electromagnetic valve.
The utility model has the beneficial effects that:
aiming at the problems of low-dose quantitative water vapor generation and introduction of humidity control in the adsorption experiment with lower temperature and the low-temperature catalytic conversion thermal analysis testing process, the utility model provides the water vapor introduction device which can control the water vapor air inflow accurately and is suitable for the adsorption experiment and the low-temperature catalytic conversion experiment, can meet the requirements of the thermochemical conversion of biomass and solid waste and the catalytic conversion thermal analysis research, realizes the quantitative low-dose quantitative water vapor generation and introduction of humidity control into the thermal analyzer, and ensures the measurement accuracy and the importance in the reaction process.
Drawings
Fig. 1 is a schematic structural view of the present utility model.
Reference numerals illustrate: 1-a liquid storage tank; 2-a feed pump; 3-a first flowmeter; 4-a first control; 5-a first solenoid valve; 6-a first check valve; 7-a vaporization chamber; 8-a first temperature controller; 9-a first transfer tube; 10-a second temperature controller; 11-a first shut-off valve; 12-a second check valve; 13-a gas source; 14-a first pressure reducing valve; 15-a second solenoid valve; 16-a first mass flow meter; 17-solenoid valve controller; 18-a second shut-off valve; 19-a third check valve; 20-a mixer; 21-a second transfer tube; 22-with a heat tracing manual valve; 23-a third solenoid valve; 24-a second mass flow meter; 25-thermal analyzer.
Detailed Description
In order to make the objects, technical solutions and advantageous effects of the present utility model more apparent, the technical solutions of the embodiments of the present utility model will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present utility model, and it is apparent that the described embodiments are only some embodiments of the present utility model, but not all embodiments of the present utility model.
As shown in fig. 1, a device for low dose quantitative generation of water vapor for introduction into a thermal analyzer is used in conjunction with a thermal analyzer 25. The device comprises a liquid storage tank 1, a feed pump 2, a vaporization chamber 7, a gas source 13, a mixer 20, a first electromagnetic valve 5 and a second electromagnetic valve 15.
The mixer 20 is respectively communicated with the vaporization chamber 7, the gas source 13 and the thermal analyzer 25, the vaporization chamber 7 is also communicated with the feed pump 2, and the feed pump 2 is communicated with the liquid storage tank 1.
A first electromagnetic valve 5 is connected between the liquid storage tank 1 and the vaporization chamber 7, and a second electromagnetic valve 15 is connected between the gas source 13 and the mixer 20.
The gas source 13 is a gas source 13 of a carrier gas or a reaction gas, wherein the carrier gas is typically nitrogen or argon, and the reaction gas is typically carbon dioxide or dry air.
When the utility model is used, the liquid storage tank 1 supplies liquid to the vaporization chamber 7 under the action of the feed pump 2, the liquid is converted into vapor in the vaporization chamber 7, and the vapor enters the mixer 20 through the first transmission pipe 9; meanwhile, the gas in the gas source 13 enters the mixer 20 through a pipe, and the water vapor and the gas in the gas source 13 are mixed in the mixer 20 and introduced into the thermal analyzer 25 after being mixed.
Specifically, in the present utility model, since the first electromagnetic valve 5 is connected between the liquid storage tank 1 and the vaporizing chamber 7, the second electromagnetic valve 15 is connected between the gas source 13 and the mixer 20, the flow rate of the water vapor between the liquid storage tank 1 and the vaporizing chamber 7 is controlled by opening and closing the first electromagnetic valve 5, the flow rate of the gas between the gas source 13 and the mixer 20 is controlled by opening and closing the second electromagnetic valve 15, the amounts of the water vapor and the gas introduced into the mixer 20 are controlled, and when the water vapor and the gas in the gas source 13 are mixed in the mixer 20, the mixture is introduced into the thermal analyzer 25. Since the flow rate of the water vapor introduced into the mixer 20 through the vaporization chamber 7 is quantitatively controlled by the first solenoid valve 5, and at the same time, the flow rate of the gas introduced into the mixer 20 through the gas source 13 is quantitatively controlled by the first mass flowmeter 16, the flow rate of the gas introduced into the thermal analyzer 25 through the mixer 20 is quantitatively controlled after both are mixed in the mixer 20, and thus the quantitative introduction of the mixed gas into the thermal analyzer 25 is achieved.
As a first embodiment of the present utility model, the vaporization chamber 7 is communicated with the mixer 20 through the first transfer pipe 9, the first transfer pipe 9 is a heat-tracing transfer pipe, and/or the mixer 20 is a heat-tracing mixer 20, and the temperature of the water vapor and the temperature of the mixed gas are ensured by the heat-tracing transfer pipe and the mixer 20, and the effect of introducing the water vapor into the thermal analyzer 25 is ensured. Further, a second temperature controller 10 is arranged on the first transmission pipe 9; the first transfer pipe 9 is connected with a first shut-off valve 11 and a second check valve 12.
As a second embodiment of the present utility model, the above-mentioned feed pump 2 and the first flowmeter 3 are connected between the liquid storage tank 1 and the vaporization chamber 7, the feed pump 2 and the first flowmeter 3 are connected at the upstream position of the first electromagnetic valve 5, and when in use, the liquid in the liquid storage tank 1 is pumped into the vaporization chamber 7 under the action of the feed pump 2, the liquid is converted into water vapor in the vaporization chamber 7, ready for being introduced into the thermal analyzer 25, and the flow rate between the liquid storage tank 1 and the vaporization chamber 7 is monitored in real time by the first flowmeter 3, so that the amount entering the mixer 20 as in the prior art is prevented, even the amount entering the thermal analyzer 25 is not controllable. Preferably, the feed pump 2 is a low dose pulse dosing pump 2, whereby the dosing effect can be achieved by means of a pump body.
Wherein, be connected with first check valve 6 between first solenoid valve 5 and the vaporization room 7, be provided with first temperature controller 8 on the vaporization room 7.
Further, the feed pump 2 is connected to the first controller 4, and the start, stop and feed of the feed pump 2 are controlled by the first controller 4. The control of the first controller 4 on the feed pump 2 is controlled by a conventional control manner such as a circuit, and the connection manner is also a conventional connection manner, which is not described herein.
As a third embodiment of the present utility model, the present utility model further includes a solenoid valve controller 17, wherein the solenoid valve controller 17 is connected to the first solenoid valve 5 and the second solenoid valve 15, and the operation of the first solenoid valve 5 and the second solenoid valve 15 is controlled by the solenoid valve controller 17. The control of the solenoid valve controller 17 and the first solenoid valve 5 and the second solenoid valve 15 is controlled by a conventional circuit, and thus will not be described in detail herein.
As a fourth embodiment of the present utility model, one or more of the first mass flow meter 16, the first pressure reducing valve 14, the second shut-off valve 18, and the third check valve 19 are further connected between the gas source 13 and the mixer 20, and monitored in real time by the first mass flow meter 16.
As a fifth embodiment of the present utility model, the mixer 20 and the thermal analyzer 25 are communicated with each other through a second transfer pipe 21, and the second transfer pipe 21 is a heat tracing transfer pipe. Preferably, the second transfer pipe 21 is connected with a third electromagnetic valve 23 and a second mass flowmeter 24. More preferably, the solenoid valve controller 17 is also connected to a third solenoid valve 23. In this control mode, the first electromagnetic valve 5 and the second electromagnetic valve 15 can be closed, the electromagnetic valve 23 can be opened, the flow rate of the second mass flowmeter 24 can be set in certain reaction sections of thermal analysis, and the entry of water vapor can be prevented in the temperature section where the water vapor is not needed.
As a sixth embodiment of the present utility model, a second shut-off valve 18 and a third check valve 19 are connected between the gas source 13 and the mixer 20; the second transmission pipe 21 is also connected with a manual valve 22 with heat tracing.
In the utility model, the flow of water vapor or gas is controlled through a plurality of valve bodies among the liquid storage tank 1, the feed pump 2, the vaporization chamber 7, the gas source 13, the mixer 20 and the thermal analyzer 25, and meanwhile, the flow of water vapor and gas can be monitored in real time through the flow meters, so that the effect of controlling the humidity of the gas entering the thermal analyzer 25 is realized, the adsorption experiment and the low-temperature catalytic conversion experiment are ensured, and the accuracy and the reproducibility of the measurement of the reaction process in the research of thermochemical conversion and catalytic conversion thermal analysis of biomass and solid wastes can be satisfied.
Since the first transfer pipe 9 and the mixer 20 in the present utility model are the transfer pipe with heat tracing and the mixer 20, respectively, the temperature of the gas entering the thermal analyzer 25 can be ensured. When in use, the utility model comprises the following steps:
the thermal analyzer 25 is modified before the experiment, a heat tracing belt is added to the reaction gas path in front of the furnace body, the temperature of a transmission pipe is set to 105 ℃, a clean platform large crucible is replaced, balance protection gas and reaction gas are adjusted, after the sample is cleared, a reaction program, a vapor vaporization program and a gas control program are designed according to the requirements of the reaction process, for example, the water adsorption thermal analysis experiment of the material, the heating program is set to 10 ℃/min to 105 ℃ and the temperature is kept constant for 1 hour, then the vapor carrier gas or the reaction gas with the corresponding vapor volume concentration requirement is introduced according to the requirements, and the vapor volume in unit time is
Figure BDA0004042114180000051
Wherein m is the mass of water per unit time input by the low dose pulse dosing pump 2, the unit is g, R is the molar gas constant, 8.314J/(mol.K), T is the temperature of the vaporization chamber 7, the unit is K,
Figure BDA0004042114180000052
the molar mass of water is 18g/mol, P is pressure, and the unit is Pa.
The volume concentration of the water vapor is
Figure BDA0004042114180000053
V in C The mass of the low-dose pulse quantitative feeding pump 2 and the flow rate of the carrier gas or the reaction gas are set according to the volume concentration of water vapor required by the flow rate of the balance protection gas and the flow rate of the carrier gas or the reaction gas, wherein the volume of the balance protection gas and the flow rate of the carrier gas or the reaction gas in unit time, namely the total flow rate of the non-vaporization gas, is 20 mL/min. The formula can be programmed to input the target volume concentration of the water vapor and the vaporization mass of the input water, i.e. the amount of carrier gas or reaction gas to be mixed is calculated. The electromagnetic valve and the mass flowmeter of the carrier gas are controlled by a program, a gas control program is edited, if the water vapor nitrogen mixed gas with the volume fraction of 10% is required to be set, after 15 minutes, the flow of the quantitative feeding pump 2 is set to be 0.5g/h, the flow of the nitrogen is set to be 128 mL/min, and then the flow of the carrier gas is set to be 108 mL/min; when the constant reaction gas flow rate was 60mL, the flow rate of water was set to 0.235g/h. After 1 hour of adsorption, the steam valve is closed, only the air valve is opened, the temperature of 5 ℃ is reduced to 40 ℃ by the program, and desorption is carried out. At the end of the reaction, the dosing pump 2 is turned off and the solenoid valve is closed. The thermal analyzer 25 records the test data. Other water vapor thermal analysis experimental steps are similar, and the temperature rising program and the gas switching can be set according to actual requirements.
The device for quantitatively generating and introducing the low-dose water vapor into the thermal analyzer 25 can realize quantitative introduction of the water vapor in the thermal analysis process, and is particularly suitable for low-temperature introduction of a small amount of water vapor; the control software compiled by the formula is combined, so that the water vapor content and the amount of water and carrier gas or reaction gas required by the corresponding water vapor content can be conveniently and rapidly calculated, the program control is realized, the testing process of thermal analysis is expanded, and the application range of the thermal analysis is extended; and programmed control improves the reproducibility of the method.
All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.

Claims (9)

1. The device for quantitatively generating low-dose steam and guiding the low-dose steam into the thermal analyzer is matched with the thermal analyzer for use, and is characterized by comprising a liquid storage tank, a feed pump, a vaporization chamber, a gas source, a mixer, a first electromagnetic valve and a second electromagnetic valve;
the mixer is respectively communicated with the vaporization chamber, the gas source and the thermal analyzer, the vaporization chamber is also communicated with the feed pump, and the feed pump is communicated with the liquid storage tank;
the liquid storage tank is connected with the first electromagnetic valve between the vaporization chamber, and the second electromagnetic valve is connected between the gas source and the mixer.
2. The apparatus for low dose vapor quantitative generation introduction into a thermal analyzer of claim 1, wherein the vaporization chamber is in communication with the mixer through a first transfer tube, the first transfer tube being a heat-carrying transfer tube, and/or the mixer being a heat-carrying mixer.
3. The apparatus for quantitative low dose vapor deposition introduction into a thermal analyzer of claim 1 wherein said feed pump and first flow meter are connected between said reservoir and said vaporization chamber, said feed pump and first flow meter being connected at a location upstream of said first solenoid valve.
4. The apparatus for low dose vapor dosing introduction into a thermal analyzer of claim 3, wherein the feed pump is connected to a first controller.
5. The apparatus for low dose steam dosing lead-in thermal analyzer of claim 1, further comprising a solenoid valve controller coupled to the first solenoid valve and the second solenoid valve, respectively.
6. The apparatus for low dose steam dosing introduction into a thermal analyzer of claim 1, wherein the feed pump is a low dose pulse dosing pump.
7. The apparatus for quantitative low dose vapor generation introduction into a thermal analyzer of claim 1, wherein a first mass flow meter and a first pressure relief valve are also connected between the gas source and the mixer.
8. The apparatus for quantitative introduction of low dose water vapor into a thermal analyzer of claim 1 wherein the mixer and the thermal analyzer are in communication via a second transfer tube, the second transfer tube being a heat trace transfer tube.
9. The apparatus for quantitative low dose vapor generation of claim 8 for introduction into a thermal analyzer, wherein a third solenoid valve is connected to the second transfer tube.
CN202320035441.XU 2023-01-06 2023-01-06 Device for quantitatively generating low-dose steam and guiding low-dose steam into thermal analyzer Active CN219162025U (en)

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