CN117129397A - Evaluation system for adsorption moisture resistance of solid porous material - Google Patents

Evaluation system for adsorption moisture resistance of solid porous material Download PDF

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Publication number
CN117129397A
CN117129397A CN202311002294.7A CN202311002294A CN117129397A CN 117129397 A CN117129397 A CN 117129397A CN 202311002294 A CN202311002294 A CN 202311002294A CN 117129397 A CN117129397 A CN 117129397A
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fixed bed
gas
bed reactor
sensor
mass flow
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郄志鹏
孙晔
孔庆天
赵富斌
胡明慧
张新翰
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Beijing University of Technology
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Beijing University of Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N15/0806Details, e.g. sample holders, mounting samples for testing
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00Investigating resistance of materials to the weather, to corrosion, or to light
    • G01N17/002Test chambers
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/56Investigating or analyzing materials by the use of thermal means by investigating moisture content
    • G01N25/58Investigating or analyzing materials by the use of thermal means by investigating moisture content by measuring changes of properties of the material due to heat, cold or expansion
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N2015/0866Sorption

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  • Life Sciences & Earth Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Environmental & Geological Engineering (AREA)
  • Environmental Sciences (AREA)
  • Treating Waste Gases (AREA)

Abstract

The application discloses an evaluation system for adsorption moisture resistance of a solid porous material, and relates to the technical field of material physicochemical property evaluation and environmental protection. The gas flow sensor comprises a fixed bed reactor, wherein the gas is divided into two paths after flowing through the first sensor, the first path is sequentially connected with a second gas mass flow controller and the first fixed bed reactor, and the second path is sequentially connected with the first gas mass flow controller and the second fixed bed reactor; the second fixed bed reactor is also connected with a third gas pipeline which is connected with the water vapor generating device and the fourth sensor; the gas flows out from the two fixed bed reactors, then respectively passes through a third sensor and a second sensor, and finally is treated by an exhaust gas treatment device; all the sensors are electrically connected with a signal processing and calculating device; temperature control devices are arranged on two sides of each fixed bed reactor; the solid adsorbent is placed in a fixed bed reactor. The application is easy to build, has no pollution, is simple and practical, and can carry out scientific evaluation on the environmental humidity tolerance of the solid adsorbent.

Description

Evaluation system for adsorption moisture resistance of solid porous material
Technical Field
The application belongs to the technical field of material physical and chemical property evaluation and environmental protection, and particularly relates to an evaluation system for the adsorption moisture resistance of a solid porous material.
Background
Adsorption is carried out by flue gas pollutants (e.g. sulfur dioxide SO 2 Nitrogen oxides NO x And volatile organic contaminants VOCs, etc.) and carbon dioxide. Compared with the traditional liquid phase absorption method, the adsorption method has the advantages of long cycle life, low regeneration energy consumption and the like, and is widely applied to the engineering fields of dry desulfurization of power plants, carbon capture of flue gas and the like. The performance of solid porous adsorbent materials (such as activated carbon, molecular sieves, metal organic framework compounds, silica gel and the like) is the core for realizing efficient adsorption, and in the laboratory range, the indexes of the adsorbent, such as the adsorption efficiency, the adsorption capacity and the like, on pollutants and carbon dioxide are widely studied.
However, unlike laboratory ideal adsorption conditions, in practical industrial applications, the flue gas environment often has high humidity, residual temperature, etc., which results in a significant compromise in the performance of the adsorbent compared to laboratory measurements. Among the influencing factors, the effect of humidity is most pronounced, the essence of which is the competition of water molecules and contaminant molecules within the adsorbent pores for the space of occurrence. In addition to gaseous contaminants, the presence of water vapor also has an adverse effect on the adsorption of carbon dioxide within the solid porous material. In order to solve the above problems, many scholars and enterprise developers have been devoted to develop hydrophobic adsorbents, i.e., to alleviate competition of water for the space of occurrence of target adsorbate molecules by weakening the host-guest interactions of the adsorbent-water. Analysis, test and evaluation are carried out based on the contact angle, the water adsorption amount and other methods, so that the effectiveness of the hydrophobization treatment of the solid adsorbent is proved.
However, judging the enhancement effect of the adsorbent on the adsorption performance of contaminants in a humid environment by evaluating the "degree of hydrophobization" is not scientific, because the conventional hydrophobization treatment (such as dealumination of molecular sieves, organofunctionalization of porous carbon, etc.) often has a negative effect on the adsorption of target contaminants at the expense of pore structure and polar adsorption sites. Therefore, it is necessary to develop a suitable method and define a suitable index, scientifically evaluate the environmental humidity tolerance (i.e., the adsorption capacity of a target substance when humidity increases) of a solid adsorbent, accurately and quantitatively analyze the humidity tolerance of the adsorbent by a small device, and link a laboratory scale index with an engineering application index.
Disclosure of Invention
The technical problem to be solved by the application is to provide an evaluation system for the adsorption moisture resistance of the solid porous material, which is easy to build, pollution-free, simple and practical, and can scientifically evaluate the environmental humidity tolerance of the solid adsorbent.
In order to solve the technical problems, the application adopts the following technical scheme: an evaluation system for the adsorption moisture resistance of a solid porous material comprises two fixed bed reactors, a plurality of sensors, a plurality of gas mass flow controllers, a water vapor generating device, a temperature control device, a tail gas treatment device and a signal processing and calculating device; the gas pipeline is connected with a gas source first and then connected with a first sensor, then the gas pipeline is divided into two paths, the first path of gas pipeline is connected with a second gas mass flow controller and then connected with a first fixed bed reactor, and the second path of gas pipeline is connected with the first gas mass flow controller and then connected with a second fixed bed reactor; the second fixed bed reactor is also connected with a third gas pipeline, and the third gas pipeline is firstly connected with a third gas mass flow controller, then connected with a water vapor generating device, then connected with a fourth sensor, and then converged with the second gas pipeline according to the gas flowing direction, and the convergence point is behind the first gas mass flow controller; the gas flows out of the first fixed bed reactor and then passes through the third sensor, the gas flows out of the second fixed bed reactor and then passes through the second sensor, then two paths of gas pipelines are converged, and finally the converged gas is treated by the tail gas treatment device; all the sensors are electrically connected with a signal processing and calculating device; temperature control devices are arranged on two sides of each fixed bed reactor, so that the temperatures of the two fixed bed reactors can be controlled respectively; the solid adsorbent is placed in a fixed bed reactor and is a solid porous material to be tested.
Preferably, the first fixed bed reactor and the second fixed bed reactor are vertical column-shaped or cube fixed bed reactors, and a heating layer connected with the temperature control device is enclosed outside the fixed bed reactors to form the required test environment temperature. The temperature is controlled in the range of room temperature to 500 ℃.
Preferably, porous plates or sand cores are arranged in the first fixed bed reactor and the second fixed bed reactor so as to carry the solid adsorbent to be evaluated, and the sizes and positions of the adsorbent areas of the two fixed bed reactors are the same.
Preferably, the fixed bed reactor is made of quartz, glass or stainless steel.
Preferably, the temperature control device comprises a heating device and a program temperature controller, the heating device is arranged outside the fixed bed reactor, the heating device is electrically heated or water bath heated, and specifically comprises a resistance wire, a water area heating sleeve and the like, and simulates the environmental temperature (60-180 ℃) of industrial flue gas; the inside of the fixed bed reactor is provided with a sensor for measuring temperature, the temperature sensor can be a thermocouple sensor, an infrared sensor and the like, and PID program control is arranged in the temperature sensor.
The beneficial effects of adopting above-mentioned technical scheme to produce lie in:
(1) The test result has strong referential property: in the whole operation period, the adsorption performance of the adsorbent under the influence of humidity can be obtained by only one operation, the experimental conditions in the two fixed bed reactors are the same except the content of water vapor, and the reaction is in the same time, and the influence on the experimental result is small after being influenced by other factors, so that the application can scientifically evaluate the environmental humidity tolerance (namely the adsorption capacity of the target substance when the humidity is increased) of the solid adsorbent; the application adopts an integration method to measure the whole adsorption process, takes the water-resistant adsorption parameter obtained by program operation as the water-resistant index of the adsorption material, carries out omnibearing summarization on the adsorption process, can rapidly display the water resistance of the material, improves the evaluation efficiency, and has evaluation significance.
(2) The application can quickly and directly obtain the water-resistant adsorption capacity of the adsorbent, automatically generate the water-resistant adsorption parameters according to the data given by the computer, and is simple and convenient. The system and the testing method thereof have higher safety, and the signal processing and computing device can monitor the air tightness and the air flow and ensure the safety when recording and computing data.
(3) No or little exhaust emissions: in the experimental process, the gas used for carrying the water vapor is nitrogen, is nontoxic and harmless, and the channels of the flue gas are subjected to double adsorption of the adsorbent and the tail gas treatment device, so that the gas which needs to be filtered is discharged to the outside, and no or only a small amount of waste gas is discharged to the outside during the whole operation period.
(4) High heat utilization: in the experiment, the temperature control device is surrounded on the fixed bed reactor, and the fixed bed reactor made of quartz or metal has good heat conductivity and good heat utilization.
(5) The application has simple equipment and low cost: the double-tower fixed bed is utilized to be matched with a signal processing and operation device, and the used equipment has simple structure and lower cost.
Drawings
FIG. 1 is a schematic view of the overall structure of the present application;
FIG. 2 is a schematic structural view of a fixed bed reactor;
in the figure: 1. a first sensor; 2. a first gas mass flow controller; 3. a second gas mass flow controller; 4. a first fixed bed reactor; 5. a water vapor generating device; 6. a temperature control device; 7. a tail gas treatment device; 8. a third gas mass flow controller; 9. a second sensor; 10. a third sensor; 11. a signal processing and computing device; 12. a switch; 13. a fourth sensor; 14. a second fixed bed reactor; 15. and (5) heating the layer.
Detailed Description
The following description of the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
As shown in fig. 1, the evaluation system comprises two fixed bed reactors, a plurality of sensors, a plurality of gas mass flow controllers, a water vapor generating device 5, a temperature control device 6, an exhaust gas treatment device 7 and a signal processing and calculating device 11. The gas pipeline is connected with a gas source first and then connected with a first sensor 1, then the gas pipeline is divided into two paths, the first path of gas pipeline is connected with a second gas mass flow controller 3 and then connected with an upper vent hole of a first fixed bed reactor 4, and the second path of gas pipeline is connected with a first gas mass flow controller 2 and then connected with an upper vent hole of a second fixed bed reactor 14; the second fixed bed reactor 14 is also connected to a third gas line which is connected to the third gas mass flow controller 8, then to the water vapor generating device 5, then to the fourth sensor 13, and then to the second gas line, according to the gas flow direction, the junction being after the first gas mass flow controller 2. The gas flows out from the lower vent hole of the first fixed bed reactor 4 and then passes through the third sensor 10, the gas flows out from the lower vent hole of the second fixed bed reactor 14 and then passes through the second sensor 9, then two gas pipelines are converged, and finally the converged gas is treated by the tail gas treatment device 7; all sensors are electrically connected with the signal processing and computing device 11. Wherein the second sensor 9 and the third sensor 10 measure the smoke content, the first sensor 1 measures the smoke content, and the fourth sensor measures the water vapor content. Temperature control devices 6 are arranged on two sides of each fixed bed reactor, so that the temperatures of the two fixed bed reactors can be controlled respectively, and the industrial environment temperature can be simulated. As shown in fig. 2, the solid adsorbent, which is a solid porous material to be tested, is placed in a fixed bed reactor.
Example 1
Assuming that the adsorbent is a molecular sieve, the dosage is 2g, the total flow is 500ml/min, the relative humidity of a wet gas path is 50%, and the pollutant component in simulated flue gas is 500ppm toluene.
Connecting four sensors with a signal processing and calculating device 11, and drawing toluene concentration-time coordinates; introducing flue gas containing toluene from a gas source, acquiring the total toluene concentration through a first sensor 1, dividing the flue gas into two paths, measuring a first path of gas flow and a second path of gas flow respectively through a first gas mass flow controller 2 and a second gas mass flow controller 3, and connecting the first path of gas flow and the second path of gas flow with a first fixed bed reactor 4 and a second fixed bed reactor 14; before entering the second fixed bed reactor 14, nitrogen is introduced into the steam generator 5, then the flow rate of the steam is controlled by the third gas mass flow controller 8, the two fixed bed reactors are heated by the temperature control device 6 and wait for complete reaction, after the reaction is finished, the toluene concentrations of the two paths of gases are respectively measured by the second sensor 9 and the third sensor 10, and then are connected to a gas outlet by a pipeline together and discharged to the tail gas treatment device 7 (a gas washing bottle), and when the process is carried out, a corresponding curve is drawn on the toluene concentration-time coordinate by signal processing and operation, so that the observation and comparison are convenient.
In the above-described gas line, the first sensor 1 is used to detect the target gas concentration at the inlet, and the second sensor 9 and the third sensor 10 are used to detect the gas concentrations output from the left and right side solid bed reactors, respectively. In addition, these three sensors are connected by a sensor line and input signals to the signal processing and computing device 11; the signal processing and calculating device 11 obtains the difference between the signals of the first sensor 1 and the third sensor 10 and the signals of the first sensor 1 and the second sensor 1 and the signals of the second sensor 9 by obtaining the signals of the first sensor 1, the second sensor 9 and the signals of the third sensor 10 and converting the signals into the concentration of the target gas component, namely the concentration of the left fixed bed generator device and the right fixed bed generator device which is reduced due to the absorption and the trapping of toluene at each signal acquisition time, and obtains the absorption capacity by integrating/differentiating operation of time. The first gas mass flow controller 2 and the second gas mass flow controller 3 respectively control the gas flow of the gas entering the left and right fixed bed generators; in the fixed bed reactor, the solid adsorbent is arranged at the position of a sand core in the reactor from an opening, and the temperature control device 6 comprises a heating device, a program temperature controller and a temperature control circuit connected with the heating device and the program temperature controller, so that the temperatures of the fixed bed reactor on the left side and the right side can be respectively controlled; the third gas mass flow controller 8 is used for controlling the gas flow entering the water vapor generating device 5 and reaching the right side solid bed reactor through corresponding pipelines so as to achieve the detection of the moisture resistance of the adsorbent.
The operation steps of the application are as follows;
(1) And (3) connecting a pipeline: the experimental setup was connected as in fig. 1.
(2) Checking air tightness: after the connection is completed, the ventilation test operation is performed, and if the gas flow rate of the first sensor 1 plus the gas flow rate of the fourth sensor 13=the gas flow rate of the second sensor 9 plus the gas flow rate of the third sensor 10, the device has good air tightness, and charging can be performed. In this example 2g of molecular sieve was charged into a fixed bed reactor.
(3) Heating: the switch 12 of the temperature control device 5 is opened to ensure that it reaches the simulated plant temperature environment.
(4) Ventilation: the first sensor 1 was fed with a flue gas containing 500ppm toluene at a flow rate of 500ml/min.
(5) Humidifying: the vent holes on the steam generator 5 are filled with nitrogen gas to carry saturated wet steam generated in the steam generator so as to open the switch of the steam generator 5, improve the steam content and enable the relative humidity of the wet gas path (the second fixed bed reactor 14) to reach 50 percent. The nitrogen is introduced to carry water vapor, and saturated wet vapor at high temperature is carried into the flue gas through nitrogen flow.
(6) And (3) gas washing: and the exhaust gas is adsorbed and recovered to prevent environmental pollution.
(7) Drawing comparison: and automatically generating water-resistant adsorption parameters according to the data given by the computer.
Example 2:
the principle, operational steps and advantageous effects of the present embodiment are similar to those of embodiment 1. The embodiment is characterized in that: the adsorbent is activated carbon, the granularity is 3mm, the dosage is 2g, the total flow is 500ml/min, the relative humidity of a wet gas path is 100%, and the pollutant component in simulated flue gas is 500ppm toluene. The parts not mentioned in this embodiment are similar to those in embodiment 1, and will not be described again here.
Example 3:
the principle, operational steps and advantageous effects of the present embodiment are similar to those of embodiment 1. The embodiment is characterized in that: the adsorbent is molecular sieve, the dosage is 2g, the total flow is 500ml/min, the relative humidity of the wet gas path is 50%, and the pollutant component in the simulated flue gas is 15% of CO by volume 2 . The parts not mentioned in this embodiment are similar to those in embodiment 1, and will not be described again here.
The present application is not limited to the above-mentioned embodiments, and any person skilled in the art, based on the technical solution of the present application and the inventive concept thereof, can be replaced or changed within the scope of the present application.

Claims (5)

1. The evaluation system for the adsorption moisture resistance of the solid porous material is characterized by comprising two fixed bed reactors, a plurality of sensors, a plurality of gas mass flow controllers, a water vapor generating device, a temperature control device, a tail gas treatment device and a signal processing and calculating device; the gas pipeline is connected with a gas source first and then connected with a first sensor, then the gas pipeline is divided into two paths, the first path of gas pipeline is connected with a second gas mass flow controller and then connected with a first fixed bed reactor, and the second path of gas pipeline is connected with the first gas mass flow controller and then connected with a second fixed bed reactor; the second fixed bed reactor is also connected with a third gas pipeline, and the third gas pipeline is firstly connected with a third gas mass flow controller, then connected with a water vapor generating device, then connected with a fourth sensor, and then converged with the second gas pipeline according to the gas flowing direction, and the convergence point is behind the first gas mass flow controller; the gas flows out of the first fixed bed reactor and then passes through the third sensor, the gas flows out of the second fixed bed reactor and then passes through the second sensor, then two paths of gas pipelines are converged, and finally the converged gas is treated by the tail gas treatment device; all the sensors are electrically connected with a signal processing and calculating device; temperature control devices are arranged on two sides of each fixed bed reactor, so that the temperatures of the two fixed bed reactors can be controlled respectively; the solid adsorbent is placed in a fixed bed reactor and is a solid porous material to be tested.
2. The evaluation system for the adsorption moisture resistance of the solid porous material according to claim 1, wherein the first fixed bed reactor and the second fixed bed reactor are vertical column-shaped or cube fixed bed reactors, and a heating layer connected with the temperature control device is enclosed outside the fixed bed reactors to form a required test environment temperature.
3. The system for evaluating the adsorption moisture resistance of a solid porous material according to claim 2, wherein porous plates or sand cores are arranged in the first fixed bed reactor and the second fixed bed reactor so as to carry the solid adsorbent to be evaluated, and the sizes and positions of the adsorbent areas of the two fixed bed reactors are the same.
4. A system for evaluating the adsorption moisture resistance of a solid porous material according to any one of claims 1 to 3, wherein the fixed bed reactor is made of quartz, glass or stainless steel.
5. The evaluation system for the adsorption moisture resistance of the solid porous material according to claim 1, wherein the temperature control device comprises a heating device and a program temperature controller, and the heating device is arranged outside the fixed bed reactor; the heating device is electrically heated or heated in water bath, and simulates the temperature of the industrial environment; a sensor for measuring the temperature is arranged in the fixed bed reactor, and PID program control is arranged in the sensor.
CN202311002294.7A 2023-08-10 2023-08-10 Evaluation system for adsorption moisture resistance of solid porous material Pending CN117129397A (en)

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