CN111426623B - Device for simulating high-temperature corrosion environment of biomass and detecting experimental reaction gas in real time - Google Patents
Device for simulating high-temperature corrosion environment of biomass and detecting experimental reaction gas in real time Download PDFInfo
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- CN111426623B CN111426623B CN202010212562.8A CN202010212562A CN111426623B CN 111426623 B CN111426623 B CN 111426623B CN 202010212562 A CN202010212562 A CN 202010212562A CN 111426623 B CN111426623 B CN 111426623B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
Abstract
The invention discloses a device for simulating a high-temperature corrosion environment of biomass and detecting experimental reaction gas in real time, wherein an oxygen cylinder and a nitrogen cylinder are respectively connected with two flowmeters, the two flowmeters are respectively connected with two ports of a T-shaped tee joint, the third port of the T-shaped tee joint is connected with a first gas washing cylinder, the first gas washing cylinder is arranged in a water bath kettle, the first gas washing cylinder is also provided with a first gas outlet guide pipe, the first gas outlet guide pipe is connected with the first end of a quartz pipe, the second end of the quartz pipe is connected with a second gas washing cylinder through a tee joint guide pipe, the third end of the tee joint guide pipe is connected with a gas detection system, the second gas washing cylinder is also provided with a second gas outlet guide pipe, and experimental gas generated in the quartz pipe is discharged through the second gas outlet guide pipe. The device is simple to operate, the settable experiment temperature range is wide, the flow of the introduced mixed gas can be accurately controlled, and the humidity of the water vapor can be accurately controlled; the gas detection system can judge the specific process of the high-temperature corrosion of the biomass by measuring the concentration of the target gas in the gas generated after the high-temperature corrosion reaction of the biomass.
Description
Technical Field
The invention relates to the field of material high temperature resistance and corrosion resistance experimental equipment, in particular to an experimental device for simulating a biomass high-temperature corrosion environment and detecting experimental reaction gas in real time.
Background
High-temperature biomass corrosion is a common phenomenon existing in the existing biomass power plant and is also a main reason for influencing the service life of a boiler of the biomass power plant. In order to prolong the service life of a boiler of a biomass power plant and improve the benefit of the power plant, a corrosion test of a biomass high-temperature corrosion environment is widely researched. The mechanism of biomass high-temperature corrosion is various, so that multiple experiments are required to be carried out as much as possible to find a corrosion source; at the same time, multiple experiments are also required to find ways to reduce and prevent corrosion. However, it is not very feasible to conduct experiments directly at power plants using biomass fuels.
Therefore, it is necessary to design a laboratory facility having the same corrosive environment as the biomass power plant in the laboratory.
Disclosure of Invention
In view of the above, the present invention aims to provide a simple and effective experimental device for simulating a high-temperature biomass corrosion environment and detecting experimental reaction gas in real time.
The technical scheme of the invention is as follows:
the utility model provides a device of simulation living beings high temperature corrosion environment and real-time detection experiment reaction gas, oxygen cylinder and nitrogen cylinder are connected with two flowmeters respectively, and two flowmeters are connected with two ports of T shape tee bend respectively, and the three port of T shape tee bend is connected with first gas washing bottle, and during water bath was arranged in to first gas washing bottle, first gas washing bottle still set up first pipe of giving vent to anger, first pipe of giving vent to anger is connected with the first end of quartz capsule, and the quartz capsule second end is passed through the tee bend pipe and is connected with second gas washing bottle, and the third end and the gas detection system of tee bend pipe are connected, and second gas washing bottle still sets up the second pipe of giving vent to anger, and the experimental gas that produces in the quartz capsule is discharged through the second pipe of giving vent to anger.
Preferably, the gas detection system comprises two gas tanks, three flow controllers, a test cavity, a data collector, a humidity simulator and a controller, the third end of the three-way pipe is connected with a second gas tank of the gas detection system, the second gas tank is connected with the gas inlet end of the third flow controller, the gas inlet end of the first flow controller is connected with the gas inlet end of the second flow controller, the gas inlet end of the first flow controller and the gas inlet end of the second flow controller are connected with the first gas tank, the gas inlet end of the humidity simulator is connected with the gas outlet end of the second flow controller, the gas outlet end of the humidity simulator and the gas outlet end of the first flow controller are connected with the test cavity after being connected with the gas outlet end of the third flow controller, the test cavity is connected with the data collector, and the data collector is connected with the controller.
Specifically, the first air tank contains air.
Preferably, the quartz tube is placed in the groove of the tube furnace, and the experimental environment is provided for the quartz tube through the tube furnace.
Preferably, liquid is filled in the first gas washing bottle, and the third port of the T-shaped tee joint is connected with the liquid in the first gas washing bottle.
Preferably, the second gas washing bottle is filled with liquid, and the guide pipe is connected with the liquid in the second gas washing bottle.
Specifically, the liquid in the first gas washing bottle and the liquid in the second gas washing bottle are both deionized water.
Compared with the prior art, the invention has the advantages that: the device is simple to operate, the settable experiment temperature range is wide, the flow of the introduced mixed gas can be accurately controlled, and the humidity of water vapor can be accurately controlled; the gas detection system in the device can judge the specific process of the high-temperature corrosion of the biomass by measuring the concentration of the target gas in the gas generated after the high-temperature corrosion reaction of the biomass.
Drawings
FIG. 1 is a diagram of the overall structure of the apparatus for simulating a high-temperature biomass corrosion environment and detecting experimental reaction gas in real time according to the present invention.
Fig. 2 is a schematic structural diagram of a gas detection system according to the present invention.
FIG. 3 is a diagram showing the experimental results of the device for simulating the high-temperature corrosion environment of biomass and detecting the experimental reaction gas in real time.
In fig. 1 and 2, the component reference numerals are as follows: the device comprises a nitrogen gas cylinder 1, an oxygen gas cylinder 2, a first flowmeter 3-1, a second flowmeter 3-2, a water bath kettle 4, a first gas washing cylinder 5-1, a second gas washing cylinder 5-2, a tube furnace 6, a quartz tube 7, a first gas outlet conduit 8-1, a second gas outlet conduit 8-2, a gas detection system 9, a first gas tank 10, a second gas tank 11, a first flow controller 12, a second flow controller 13, a third flow controller 14, a humidity simulator 15, a test cavity 16, a data collector 17, a controller 18, a power supply 19, a front interdigital Au electrode 20 and a back interdigital Pt electrode 21.
Detailed Description
The invention provides automatic experimental equipment for simulating a high-temperature biomass corrosion environment and detecting experimental reaction gas in real time, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, in the automated experimental equipment for simulating a biomass high-temperature corrosion environment and detecting experimental reaction gas in real time, outlets of an oxygen cylinder 1 and a nitrogen cylinder 2 are respectively connected with a first flowmeter 3-1 and a second flowmeter 3-2, the first flowmeter 3-1 and the second flowmeter 3-2 are connected with two ports of a T-shaped tee joint, a third port of the T-shaped tee joint penetrates through the top of a first gas washing cylinder 5-1 and is contacted with liquid arranged in the first gas washing cylinder 5-1, the first gas washing cylinder 5-1 is placed in a water bath pot 4, a first gas outlet conduit 8-1 is further arranged at the top of the first gas washing cylinder 5-1, the first gas outlet conduit 8-1 is connected with a first end of a quartz tube 7, a second end of the quartz tube 7 is contacted with liquid arranged in the second gas washing cylinder 5-2 through a tee joint conduit, the third end of the three-way guide pipe is connected with a gas detection system 9, a second gas outlet guide pipe 8-2 is further arranged at the top of the second gas washing bottle 5-2, experimental gas is discharged through the second gas outlet guide pipe 8-2, the quartz tube 7 is placed in a groove of the tube furnace 6, and an experimental environment is provided for the quartz tube 7 through the tube furnace 6.
Specifically, the gas detection system 9 is used for detecting the experimental reaction gas flowing into the three-way pipe through the quartz pipe 7.
Specifically, after the gases in the oxygen cylinder 1 and the nitrogen cylinder 2 are quantitatively mixed through a first flowmeter 3-1 and a second flowmeter 3-2, the gases are introduced into a first gas washing cylinder 5-1 arranged in a water bath kettle 4, carry quantitative water vapor required by an experiment, and finally are introduced into a quartz tube 7 of a tube furnace 6.
Specifically, the water bath 4 can adjust the mixed gas to carry water vapor with specific humidity from the first gas washing bottle 5-1 by setting the temperature.
Specifically, the experimental waste gas generated by the corrosion reaction of the sample through the quartz tube 7 and the redundant mixed gas introduced from the oxygen cylinder 1 and the nitrogen cylinder 2 are connected into the second gas washing cylinder 5-2 through the second end of the quartz tube 7 for reasonable treatment.
Specifically, the quartz tube 7 is used for placing a sample and giving the sample the required experimental environment, and the quartz tube is made of high-temperature-resistant and corrosion-resistant quartz.
Specifically, the tubular furnace 6 can set an experiment temperature and an experiment time according to experiment requirements, provides the same corrosion environment contacted with the biomass fuel boiler for an experiment, the settable experiment temperature range of the tubular furnace 6 is 0-1200 ℃, the combustion temperature of the existing biomass fuel boiler is completely met, and the model of the tubular furnace is OTF-1200X.
Specifically, the nitrogen cylinder 1 and the oxygen cylinder 2 are made of high-pressure-resistant alloy steel.
Specifically, the liquids in the first gas washing bottle 5-1 and the second gas washing bottle 5-2 are deionized water. The deionized water in the first gas washing bottle 5-1 is used for leading the mixed gas entering from the top of the first gas washing bottle to carry water vapor with specific humidity required by experiments; the deionized water in the second gas washing bottle 5-2 was used to collect the experimental off-gas in the quartz tube 7 in the tube furnace 6.
Specifically, the temperature rise and decrease speed of the tube furnace cannot exceed 10 ℃/min.
Referring to fig. 2, the gas detection system 9 includes a first gas tank 10, a second gas tank 11, a first flow controller 12, a second flow controller 13, a third flow controller 14, a humidity simulator 15, a test chamber 16, a data collector 17, a controller 18, and a power supply 19, the second gas tank 11 is connected to an air inlet of the third flow controller 14, an air inlet of the first flow controller 12 is connected to an air inlet of the second flow controller 13, an air inlet of the first flow controller 12 and an air inlet of the second flow controller 13 are connected to the first gas tank 10, an air inlet of the humidity simulator 15 is connected to an air outlet of the second flow controller 13, an air outlet of the humidity simulator 15 and an air outlet of the first flow controller 12 are connected to the test chamber 16 after being connected to an air outlet of the third flow controller 14, the test chamber 16 is connected to both the data collector 17 and the power supply 19, the data collector 17 is connected to the controller 18.
Specifically, the third end of the three-way conduit is connected with the second gas tank 11 of the gas detection system 9.
Specifically, the first gas tank 10 is filled with air to adjust the concentration of the reaction gas.
Specifically, the humidity simulator 15 is used to simulate the humidity of water vapor in an actual corrosive environment.
Specifically, the power supply 19 employs a dc power supply to regulate the operating temperature of the gas sensor in the test chamber 16.
Specifically, the test cavity 16 is made of polytetrafluoroethylene, a gas sensor is arranged in the test cavity, and a substrate of the gas sensor is made of aluminum oxide; the front interdigital Au electrode 20 (shown in fig. 2) of the gas sensor is covered with a semiconductor gas sensitive layer, the signal collector 17 can obtain an electric signal, and the back interdigital Pt electrode 21 (shown in fig. 2) of the gas sensor controls the temperature of the gas sensor through the power supply 19.
Specifically, the test chamber 16 is configured to detect the concentration of the mixed gas introduced therein and convert the concentration of the mixed gas into an electrical signal through a gas sensor therein.
Referring to fig. 1-2, the apparatus of the present invention mainly comprises a tube furnace 6, a water bath 4, a nitrogen gas cylinder 1 and an oxygen gas cylinder 2, during the experiment, an alloy sample to be corroded is placed in a quartz tube 7, the quartz tube 7 is placed in a groove of the tube furnace 6, the tube furnace 6 is covered and the tube furnace 6 is fixed by a buckle, the tube furnace 6 is a main space for corrosion of the alloy sample, and the whole cycle corrosion of the alloy sample is in the space. During the experiment, firstly, an alloy sample for the experiment is put into a quartz tube 7 and sealed by a flange sealing disc, then an oxygen cylinder 2 and a nitrogen cylinder 1 are opened, the gas flow required by the experiment can be adjusted by a first flowmeter 3-1 and a second flowmeter 3-2, then a water bath pot 4 is opened, the temperature is adjusted to the target temperature according to the experiment requirement, the oxygen provided by the oxygen cylinder 2 and the nitrogen provided by the nitrogen cylinder 1 form mixed gas through two ports of a T-shaped tee joint, the mixed gas is introduced into a first gas washing bottle 5-1 arranged in the water bath pot 4 through a third port of the T-shaped tee joint and is mixed with deionized water in the first gas washing bottle 5-1, water vapor with specific humidity is carried at the target temperature and enters the first end of the quartz tube 7 through a first gas outlet conduit 8-1, and impurity gas in the quartz tube 7 is removed completely, opening a switch of the tube furnace 6 after impurity gas is completely removed, setting initial temperature, heating time, experiment constant temperature, constant temperature time, cooling temperature and cooling time according to the preset experiment requirements, then carrying mixed gas of water vapor with specific humidity to perform high-temperature corrosion reaction with an alloy sample in the quartz tube 7 at the experiment temperature, enabling the reacted experiment waste gas to enter a second gas washing bottle 5-2 through a second end of the quartz tube 7 through a three-way guide pipe, collecting water-soluble experiment waste gas generated in the experiment process through deionized water in the second gas washing bottle 5-2, and discharging the remaining water-insoluble experiment waste gas through a second gas outlet guide pipe 8-2, wherein a third end of the three-way guide pipe is connected with a second gas tank 11 of a gas detection system 9. The second gas tank 11 is connected with the gas inlet end of the third flow controller 14, the gas inlet end of the first flow controller 12 is connected with the gas inlet end of the second flow controller 13, the gas inlet end of the first flow controller 12 and the gas inlet end of the second flow controller 13 are connected with the first gas tank 10, the gas inlet end of the humidity simulator 15 is connected with the gas outlet end of the second flow controller 13, the gas outlet end of the humidity simulator 15 and the gas outlet end of the first flow controller 12 are connected with the gas outlet end of the third flow controller 14 and then connected with the test cavity 16, the test cavity 16 is connected with the data collector 17 and the power supply 19, and the data collector 17 is connected with the controller 18. Experimental reaction gas generated after reaction in the quartz tube 7 enters an air inlet end of a third flow controller 14 through a second air tank 11, air in a first air tank 10 enters air inlet ends of a first flow controller 12 and a second flow controller 13, air flowing into the second flow controller 13 enters an air inlet end of a humidity simulator 15 from an air outlet end of the second flow controller 13 and then flows out from an air outlet end of the humidity simulator 15, the air and the experimental reaction gas flowing out from the air outlet end of the first flow controller 12 and the air outlet end of the third flow controller 14 flow into a test cavity 16 together, a preliminary test result can be obtained through mixed gas of the test cavity 16, and after the preliminary test result is collected by a data collector 17, the experimental result is automatically displayed on a controller 18 (a computer).
Examples
Firstly, putting an alloy sample for experiment into a quartz tube 7 and sealing the alloy sample by a flange sealing disc, then opening an oxygen cylinder 2 and a nitrogen cylinder 1, adjusting a first flow meter 3-1 to 55 percent, adjusting a second flow meter 3-2 to 30 percent, then opening a water bath pot 4, adjusting the target temperature to 55 ℃ according to the experiment requirement, forming mixed gas by the oxygen provided by the oxygen cylinder 2 and the nitrogen provided by the nitrogen cylinder 1 through two ports of a T-shaped tee joint, leading the mixed gas into a first washing gas cylinder 5-1 placed in the water bath pot 4 through a third port of the T-shaped tee joint, mixing the mixed gas with deionized water in the first washing gas cylinder 5-1, leading the mixed gas to carry water vapor with specific humidity at the target temperature of 55 ℃ and enter a first end of the quartz tube 7 through a first gas outlet conduit 8-1, and coating the surface of the alloy sample in the quartz tube 7 with corrosive salt required for experiment, the mixed gas introduced into the quartz tube 7 from the first gas outlet guide tube 8-1 is very close to the environment atmosphere of the biomass during high-temperature corrosion; in addition, the experiment temperature and the experiment time set by the tube furnace 6 are consistent with the temperature and the time of high-temperature corrosion of various biomasses. FIG. 3 is the corrosion weight gain results after KCl coating of samples coated with nickel aluminum under the experimental conditions set forth in this experimental setup. Wherein the initial temperature of the tubular furnace 6 is 10 ℃, the temperature rise time is 60min, the experimental constant temperature is 600 ℃, the constant temperature time is 4320min, the temperature reduction temperature is 10 ℃, and the temperature reduction time is 60 min.
In addition, the gas generated during the experiment process, i.e. the experiment reaction gas, enters the gas monitoring system 9 in real time. As shown in fig. 2, the experimental reaction gas is the target gas in the second gas tank 11 in fig. 2, the first gas tank 10 is the synthetic air, which passes through the first flow controller 12, the second flow controller 13 and the humidity simulator 15 to reach 20% humidity when the experiment is performed, the experimental reaction gas directly enters the air inlet end of the third flow controller 14, and the synthetic air passing through the first flow controller 12, the second flow controller 13 and the humidity simulator 15 enters the test chamber 16 at a ratio of 1: 4. After the temperature of the gas sensor in the test chamber 16 is regulated and controlled by a power supply 19 (direct current), a gas concentration signal of mixed gas consisting of experimental reaction gas and regulated synthetic air is converted into an electric signal by the gas sensor in the test chamber 16, and then the electric signal is transmitted into the data acquisition unit 17, the data acquisition unit 17 transmits the acquired electric signal into a controller 18 connected with the data acquisition unit, and a real-time result is displayed after the data acquisition unit 17 analyzes the electric signal by the controller.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still make modifications or equivalent substitutions on the technical solutions described in the foregoing embodiments or on some technical features of the embodiments, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A device for simulating a high-temperature corrosion environment of biomass and detecting experimental reaction gas in real time is characterized in that an oxygen cylinder and a nitrogen cylinder are respectively connected with two flowmeters, the two flowmeters are respectively connected with two ports of a T-shaped tee joint, a third port of the T-shaped tee joint is connected with a first gas washing cylinder, the first gas washing cylinder is arranged in a water bath kettle, the first gas washing cylinder is also provided with a first gas outlet guide pipe, the first gas outlet guide pipe is connected with a first end of a quartz pipe, a second end of the quartz pipe is connected with a second gas washing cylinder through a tee joint guide pipe, a third end of the tee joint guide pipe is connected with a gas detection system, the second gas washing cylinder is also provided with a second gas outlet guide pipe, and experimental gas generated in the quartz pipe is discharged through the second gas outlet guide pipe;
wherein the content of the first and second substances,
the gas detection system is used for detecting experimental reaction gas flowing into the three-way guide pipe through the quartz pipe;
the gas detection system comprises two gas tanks, three flow controllers, a test cavity, a data collector, a humidity simulator and a controller, wherein the third end of the three-way conduit is connected with a second gas tank of the gas detection system, the second gas tank is connected with the gas inlet end of the third flow controller, the gas inlet end of the first flow controller is connected with the gas inlet end of the second flow controller, the gas inlet end of the first flow controller and the gas inlet end of the second flow controller are connected with the first gas tank, the gas inlet end of the humidity simulator is connected with the gas outlet end of the second flow controller, the gas outlet end of the humidity simulator and the gas outlet end of the first flow controller are connected with the test cavity after being connected with the gas outlet end of the third flow controller, the test cavity is connected with the data collector, and the data collector is connected with the controller;
the test cavity is used for detecting the concentration of the mixed gas introduced into the test cavity and converting the concentration signal of the mixed gas into an electric signal;
the test cavity is made of polytetrafluoroethylene, a gas sensor is arranged in the test cavity, and a substrate of the gas sensor is made of aluminum oxide; the front interdigital Au electrode of the gas sensor is covered with a semiconductor gas-sensitive layer, an electric signal can be obtained through a signal collector, and the back interdigital Pt electrode of the gas sensor controls the temperature of the gas sensor through a power supply.
2. The apparatus of claim 1, wherein the test chamber comprises a gas sensor.
3. The apparatus of claim 1, wherein the first gas tank contains air for regulating the concentration of the test reactant gas.
4. The apparatus of claim 1, wherein a quartz tube is placed in a recess of a tube furnace, and the experimental environment is provided to the quartz tube through the tube furnace.
5. The apparatus of claim 1, wherein the first gas scrubber bottle contains liquid and the third port of the tee is fluidly connected to the liquid in the first gas scrubber bottle.
6. The apparatus of claim 1, wherein the second scrubber bottle contains a liquid and the conduit is in fluid communication with the liquid in the second scrubber bottle.
7. The apparatus of claim 1, wherein the liquids in the first and second scrubbers are deionized water.
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| CN111982739A (en) * | 2020-08-08 | 2020-11-24 | 天目湖先进储能技术研究院有限公司 | Detection device and method for detecting sulfide electrolyte material |
| CN114778613A (en) * | 2022-04-15 | 2022-07-22 | 四川大学 | Evaluation system for MEMS gas sensor |
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| CN102539272A (en) * | 2011-12-21 | 2012-07-04 | 西安交通大学 | Experimental device and representation method of multiphase medium high-temperature corrosion rate |
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| US20160116364A1 (en) * | 2014-10-24 | 2016-04-28 | Air Products And Chemicals, Inc. | Leak Test Apparatus and Method |
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| CN101251467A (en) * | 2008-03-19 | 2008-08-27 | 华东理工大学 | Apparatus and method for testing resistance dew-point corrosion of evaluating material |
| CN102539272A (en) * | 2011-12-21 | 2012-07-04 | 西安交通大学 | Experimental device and representation method of multiphase medium high-temperature corrosion rate |
| CN105572028A (en) * | 2016-03-03 | 2016-05-11 | 中国计量学院 | Simulated boiler high-temperature smoke gas corrosion test device |
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