CN109030708B - Tubular furnace test device capable of dynamically collecting metal vapor - Google Patents

Tubular furnace test device capable of dynamically collecting metal vapor Download PDF

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Publication number
CN109030708B
CN109030708B CN201810816836.7A CN201810816836A CN109030708B CN 109030708 B CN109030708 B CN 109030708B CN 201810816836 A CN201810816836 A CN 201810816836A CN 109030708 B CN109030708 B CN 109030708B
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furnace
tube
metal vapor
air
furnace tube
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CN109030708A (en
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王昕晔
杜荣
刘玉莹
董昊
林萍芳
张程文
赵志远
程运
卜昌盛
张居兵
朴桂林
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Nanjing Normal University
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Nanjing Normal University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/12Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion

Abstract

The application relates to a tube furnace test device capable of dynamically collecting metal vapor, and belongs to the technical field of chemical test equipment. The tubular furnace test device capable of dynamically collecting metal vapor comprises a horizontal tubular furnace system, a metal vapor collecting system, a gas supply system and a controller; the horizontal tube furnace system comprises a furnace body, a furnace tube, a reactant container, a baffle plate and a telescopic device, wherein the reactant container is arranged in the furnace tube, the furnace tube is positioned in the furnace body, a furnace body slot is arranged on the side wall of the furnace body, a furnace tube slot is arranged at a position on the furnace tube corresponding to the furnace body slot, and the baffle plate is sequentially inserted into the furnace body slot and the furnace tube slot and is connected with the telescopic device; the metal vapor collecting system comprises a plurality of sampling pipes, a three-way electromagnetic valve and an air extracting pump, the air supplying system is connected with one end of the furnace pipe, and when metal vapor is collected, the sampling pipes are alternately inserted into the other end of the furnace pipe. The test device has higher recovery rate of metal reaching more than 90%, and can realize dynamic collection of metal vapor.

Description

Tubular furnace test device capable of dynamically collecting metal vapor
Technical Field
The application relates to the technical field of chemical test equipment, in particular to a tubular furnace test device capable of dynamically collecting metal vapor.
Background
Solid fuels such as coal, refuse, and biomass generally contain semi-volatile metal elements such as Pb, cd, zn, cu, na, K. Under the high temperature condition of combustion, gasification or pyrolysis, part or all of the metal elements volatilize to form metal vapor, then leave the hearth along with flue gas, and then are condensed along with the reduction of the flue gas temperature after passing through a heat exchanger, so that the metal vapor is easily enriched in submicron particles and even ultrafine particles. These fine particles are difficult to be efficiently trapped by dust removal equipment, wherein heavy metal elements are the main source of toxicity of the particles, and alkali metal elements are one of the main matrixes for forming the particles, so that the human health is seriously endangered. For solid fuels with high alkali metal content such as eastern coal (high Na content) and herbaceous biomass (high K content), the high-concentration alkali metal vapor in the high-temperature flue gas can also cause problems of dust accumulation, high-temperature corrosion, furnace slagging and the like of the heat exchanger in the flue, and seriously disturb the operation of the boiler. The method for controlling the volatilization characteristics of the semi-volatile metal in the combustion, gasification and pyrolysis processes of the solid fuel is a first step for reducing the harm of the semi-volatile metal, and is an important research direction of a large number of researchers.
The tubular furnace is a widely used reactor for researching the combustion, gasification and pyrolysis of solid fuel, and has the advantages of simple operation and controllable working condition. In the tube furnace test system designed by the former, the absorption liquid or the quartz fiber filter membrane placed outside the tube furnace is generally adopted to collect the condensed metal fine particles in the tail gas discharged outside the heating section. The disadvantage is that the metal vapor is easily condensed on the cold surface outside the heating section and cannot reach the position of the absorption liquid or the filter membrane; in addition, condensed metal particles in the flue gas are easy to adhere to the wall surfaces of all pipelines or containers flowing through outside the heating section, including the wall surfaces of furnace tubes outside the heating section, the inner walls of connecting pipes of the furnace tubes and the absorption bottle/filter membrane device and the inner walls of inlets of the absorption bottle/filter membrane device. Therefore, when the volatilized metal is collected outside the furnace tube, the surface of the non-heating area at the exhaust end of the furnace tube and the wall surfaces of all containers and pipelines along the way need to be cleaned, so that the theoretical higher recovery rate can be obtained. The sampling operation is very tedious, the generated cleaning liquid amount is large, the storage is not easy, and great inconvenience is brought to experiments. In addition, the pipeline for sampling outside the furnace tube is usually long, and the flow rate of gas in the furnace tube is low and the flow rate is small, so that metal collected at a certain moment may be metal volatilized a few seconds or even tens of seconds before, thus causing poor dynamic response and significant lag in sampling. There have also been separate studies to collect semi-volatile metal vapors using water cooled cold finger tubes that extend into the high temperature zone of the furnace. The principle is that the metal vapor is collected by the cold finger surface through condensation after contacting with the water-cooled cold finger surface, and the defect is that the recovery rate is low because the metal vapor cannot be completely condensed, meanwhile, flowing cooling water is needed, and the test operation condition is complex. In general, the existing tube furnace test device can not well meet the dynamic sampling requirement of semi-volatile metal vapor.
Disclosure of Invention
In order to solve the problem that the recovery rate of metal vapor by the existing tubular furnace experimental device is low, the application provides a tubular furnace experimental device capable of dynamically collecting metal vapor, which comprises a horizontal tubular furnace system, a metal vapor collecting system, an air supply system and a controller;
the horizontal tube furnace system comprises a furnace body, a furnace tube, a reactant container, a baffle and a telescopic device, wherein the reactant container is arranged in the furnace tube, the furnace tube is positioned in the furnace body, two ends of the furnace tube extend out of the furnace body, a furnace body slot is arranged on the side wall of the furnace body, a furnace tube slot is arranged at a position on the furnace tube corresponding to the furnace body slot, the baffle is sequentially inserted into the furnace body slot and the furnace tube slot and is connected with the telescopic device, and the telescopic device can drive the baffle to be inserted into the furnace tube through the furnace tube slot or drive the baffle to retract into the furnace tube slot from the furnace tube;
the metal vapor collecting system comprises a plurality of sampling pipes, a three-way electromagnetic valve and an air pump, wherein each sampling pipe comprises a condensing part and a filtering part, the condensing part comprises an inner cylinder and an outer cylinder, the outer cylinder is sleeved outside the inner cylinder, the end part of the inner cylinder is connected with the end part of the outer cylinder through a ring piece with a hole, the filtering part comprises a hollow plug and a filtering cylinder, the hollow plug is inserted into the inner cylinder at one end of the condensing part, the part of the hollow plug inserted into the inner cylinder is sleeved with the filtering cylinder, the sampling pipe is used for collecting metal vapor, one port of the three-way electromagnetic valve is connected with the air extraction end of the air pump through a pipeline, the other two ports are respectively connected with the two sampling pipes through pipelines;
the air supply system is connected with one end of the furnace tube, when metal vapor is collected, the air supply system supplies air for the furnace tube, the air pump pumps air, the condensing parts of the two sampling tubes connected with the three-way electromagnetic valve are alternately inserted into the other end of the furnace tube, after the other end of the furnace tube is inserted into one of the sampling tubes connected with the three-way electromagnetic valve, the reactant container and the condensing part inserted into the furnace tube are positioned at two sides of the furnace tube slot, the baffle is positioned in the furnace tube slot, the controller controls the opening of the port of the sampling tube inserted into the furnace tube connected with the three-way electromagnetic valve, and simultaneously controls the opening of the air pump connected with the three-way electromagnetic valve, the air pumping quantity of the air pump is larger than the air supply quantity of the air supply system, the condensing parts in the furnace tube and the furnace tube are in a negative pressure state, air enters the furnace tube through the circular ring sheet with holes of the condensing parts, and the air provided by the air and the air supply system cools the metal vapor in the furnace tube, when the metal particles formed by the metal vapor during cooling adhere to the wall surface of the inner cylinder of the condensation part and are filtered by the outer wall surface of the filter cylinder, after one of the sampling pipes connected with the three-way electromagnetic valve is collected, the controller controls the telescopic device to drive the baffle to be inserted into the furnace pipe through the furnace pipe slot, the air supply system stops supplying air, the sampling pipe in the furnace pipe is taken out, the other sampling pipe connected with the three-way electromagnetic valve is inserted into the other end of the furnace pipe, the controller firstly controls the port of the sampling pipe inserted into the furnace pipe and connected with the three-way electromagnetic valve to be opened, then controls the telescopic device to drive the baffle to retract into the furnace pipe slot from the furnace pipe, the air supply system supplies air, the other sampling pipe connected with the three-way electromagnetic valve starts collecting the metal vapor, the sampling pipe connected with the three-way electromagnetic valve and the metal vapor collected is disassembled, and connecting the sampling pipes which are not used for collecting the metal vapor with the three-way electromagnetic valve, wherein the mode of collecting the metal vapor by each sampling pipe connected with the three-way electromagnetic valve is the same.
The air supply system comprises a steel cylinder, a pressure reducing valve, a mass flow controller, a buffer tank and an air inlet electromagnetic valve;
the gas is stored in the steel cylinder, the steel cylinder is connected with one port of the pressure reducing valve, the other port of the pressure reducing valve is connected with the mass flow controller, the mass flow controller is connected with the buffer tank, the buffer tank is connected with one port of the air inlet electromagnetic valve, the other port of the air inlet electromagnetic valve is connected with the furnace tube, and the controller can control the air inlet electromagnetic valve to be opened so that the gas in the steel cylinder is introduced into the furnace tube.
The telescopic device comprises a servo motor, a cam and a connecting rod, wherein one end of the cam is connected with one end of the connecting rod, the other end of the connecting rod is connected with the baffle, the servo motor is connected with the cam, the controller can control the servo motor to drive the cam to rotate, and the baffle is driven to be inserted into the furnace tube through the connecting rod or to retract into the furnace tube slot from the furnace tube.
The cross section of the cavity inside the furnace body is square, the cross section of the part of the furnace tube, which is positioned inside the furnace body, is square, and the cross section of the part of the furnace tube, which extends out of the furnace body, is round.
The metal vapor collection system further comprises a gas washing bottle, the gas inlet end of the gas washing bottle is connected with one port of the three-way electromagnetic valve, and the gas outlet end of the gas washing bottle is connected with the gas extraction end of the gas extraction pump.
The metal vapor collection system further comprises a silica gel drying bottle, the air inlet end of the silica gel drying bottle is connected with the air outlet end of the gas washing bottle, and the air outlet end of the silica gel drying bottle is connected with the air exhaust end of the air exhaust pump.
The hollow plug is a reducing hollow glass plug, the filter cartridge is made of quartz glass fibers, the filter cartridge is sleeved on the reducing part of the hollow plug, an air outlet pipe is arranged on the part, away from the filter cartridge, of the hollow plug, and the air outlet pipe is connected with one port of the three-way electromagnetic valve.
The baffle is made of quartz glass, corundum, zirconia or high-temperature-resistant stainless steel.
The width of the furnace tube slot is 0.5-1 mm larger than the thickness of the baffle.
The air extracting pump is a diaphragm pump.
The test device has higher recovery rate of metal, can reach more than 90 percent, and can realize dynamic collection of metal vapor; the device has simple structure and convenient operation process, realizes ingenious design of integration of negative pressure sampling and cooling, and solves the problems of complex structure and low recovery rate of the existing test device; the metal vapor generated in the furnace tube can be collected in real time, and the problem of sampling lag existing in the conventional test device is solved.
Drawings
The application will be further described with reference to the drawings and examples.
FIG. 1 is a schematic structural view of a tube furnace test apparatus capable of dynamically collecting metal vapors according to the present application;
FIG. 2 is a schematic structural view of a sampling tube of the present application.
In the figure:
the device comprises a furnace body 1, a furnace tube 2, a reactant container 3, a baffle 4, a sampling tube 5, a three-way electromagnetic valve 6, an air pump 7, an inner cylinder 8, an outer cylinder 9, a ring piece 10, a hollow plug 11, a filter cylinder 12, a steel cylinder 13, a pressure reducing valve 14, a mass flow controller 15, a buffer tank 16, an air inlet electromagnetic valve 17, a controller 18, a cam 19, a connecting rod 20, an air outlet pipe 21 and an air washing cylinder 22.
Detailed Description
The application will now be described in further detail with reference to the accompanying drawings. The drawings are simplified schematic representations which merely illustrate the basic structure of the application and therefore show only the structures which are relevant to the application.
In order to solve the problem of low recovery rate of metal vapor in the existing tubular furnace experimental device, as shown in fig. 1 and 2, the application provides a tubular furnace experimental device capable of dynamically collecting metal vapor, which comprises a horizontal tubular furnace system, a metal vapor collecting system, an air supply system and a controller;
the horizontal tube furnace system comprises a furnace body 1, a furnace tube 2, a reactant container 3, a baffle 4 and a telescopic device, wherein the reactant container 3 is arranged in the furnace tube 2, the furnace tube 2 is arranged in the furnace body 1, two ends of the furnace tube 2 extend out of the furnace body 1, the reactant is arranged in the reactant container 3, the furnace body 1 is heated by an electric heating furnace to convert the reactant into metal vapor, a furnace body slot is arranged on the side wall of the furnace body 1, a furnace tube slot is arranged on the furnace tube 2 at a position corresponding to the furnace body slot, the baffle 4 is sequentially inserted into the furnace body slot and the furnace tube slot, the telescopic device can drive the baffle 4 to be inserted into the furnace tube 2 through the furnace tube slot or drive the baffle 4 to retract into the furnace tube slot from the furnace tube 2, and preferably, the telescopic device drives the baffle 4 to retract from the furnace tube 2 to the end face of the baffle 4 to be on the same surface with the inner wall of the furnace tube 2;
the metal vapor collecting system comprises a plurality of sampling pipes 5, a three-way electromagnetic valve 6 and an air pump 7, wherein each sampling pipe 5 comprises a condensing part and a filtering part, the condensing part comprises an inner cylinder 8 and an outer cylinder 9, the outer cylinder 9 is sleeved outside the inner cylinder 8, the end part of the inner cylinder 8 and the end part of the outer cylinder 9 are connected through a circular ring piece 10 with holes, the filtering part comprises a hollow plug 11 and a filter cylinder 12, the hollow plug 11 is inserted into the inner cylinder 8 at one end of the condensing part, the part of the hollow plug 11 inserted into the inner cylinder 8 is sleeved with the filter cylinder 12, no gap exists between the hollow plug 11 and the inner cylinder 8, sealing is formed, the sampling pipes 5 are used for collecting metal vapor, one port of the three-way electromagnetic valve 6 is connected with the air pumping end of the air pump 7 through a pipeline, the other two ports are respectively connected with the two sampling pipes 5, and the other two ports of the three-way electromagnetic valve 6 are respectively connected with the hollow plugs 11 of the two sampling pipes 5 through pipelines;
the gas supply system is connected with one end of the furnace tube 2, when metal vapor is collected, the gas supply system supplies gas to the furnace tube 2, the gas pump 7 pumps gas, the condensing parts of the two sampling tubes 5 connected with the three-way electromagnetic valve 6 are alternately inserted into the other end of the furnace tube 2, after the other end of the furnace tube 2 is inserted into one of the sampling tubes 5 connected with the three-way electromagnetic valve 6, the reactant container 3 and the condensing part inserted into the furnace tube 2 are positioned at two sides of the furnace tube slot, at the moment, the baffle plate 4 is positioned in the furnace tube slot, the controller 18 controls the opening of the port of the sampling tube 5 inserted into the furnace tube 2 connected with the three-way electromagnetic valve 6, and simultaneously controls the opening of the port of the gas pump 7 connected with the three-way electromagnetic valve 6, the gas pumping amount of the gas pump 7 is larger than the gas supply amount of the gas supply system, the condensing parts inserted into the furnace tube 2 and the furnace tube 2 are in a negative pressure state, and air outside the test device enters the furnace tube 2 through the circular ring sheet 10 with holes at the condensing part, the air and the gas provided by the gas supply system cool the metal vapor in the furnace tube 2, the metal particles formed by the metal vapor when encountering cold adhere to the wall surface of the inner cylinder 8 of the condensing part and are filtered by the outer wall surface of the filter cylinder 12, when one of the sampling tubes 5 connected with the three-way electromagnetic valve 6 is collected, the controller 18 controls the telescopic device to drive the baffle 4 to be inserted into the furnace tube 2 through the furnace tube slot, meanwhile, the gas supply system stops supplying gas, the reactant container 3 is isolated, then the sampling tube 5 in the furnace tube 2 is manually taken out, the other sampling tube 5 connected with the three-way electromagnetic valve 6 is inserted into the other end of the furnace tube 2, the controller 18 firstly controls the opening of the port of the sampling tube 5 inserted into the furnace tube 2 connected with the three-way electromagnetic valve 6 to start air extraction, then controls the telescopic device to drive the baffle 4 to be retracted into the furnace tube slot from the furnace tube 2, simultaneously, the air supply system supplies air, at the moment, the other sampling tube 5 connected with the three-way electromagnetic valve 6 starts to collect metal vapor, and metal particles formed by the metal vapor when the metal vapor is cooled adhere to the wall surface of the inner cylinder 8 of the condensing part of the sampling tube 5 and are filtered by the outer wall surface of the filter cylinder 12;
when the other sampling tube 5 connected with the three-way electromagnetic valve 6 collects metal vapor, the sampling tube 5 connected with the three-way electromagnetic valve 6 and having collected metal vapor is disassembled, the sampling tube 5 not having collected metal vapor is connected with the three-way electromagnetic valve 6, when the other sampling tube 5 connected with the three-way electromagnetic valve 6 has collected metal vapor, the sampling tube 5 connected with the three-way electromagnetic valve 6 and not having collected metal vapor is inserted into the furnace tube 2 to collect metal vapor, and meanwhile, the sampling tube 5 connected with the three-way electromagnetic valve 6 and having collected metal vapor is disassembled, and a new sampling tube 5 not having collected metal vapor is installed, wherein the mode of collecting metal vapor by each sampling tube 5 is the same and will not be repeated.
According to the test device, the air supply system is used for supplying air to the furnace tube 2, the air in the furnace tube 2 is sucked by the air suction pump 7, the diaphragm pump can be selected by the air suction pump 7, the air quantity in the furnace tube 2 sucked by the air suction pump 7 is larger than the air quantity supplied to the furnace tube 2 by the air supply system, so that negative pressure is formed in the furnace tube 2, air can enter the furnace tube 2 through the annular ring piece 10 with holes of the condensation part, cooling of metal vapor is realized through the air supplied by the air supply system and the air entering from the outside, and meanwhile, under the action of the air suction pump 7, one part of formed metal particles is adhered to the wall surface of the inner tube 8, and the other part of formed metal particles is deposited on the outer wall surface of the filter cylinder 12, so that the metal vapor is prevented from leaking; meanwhile, the application comprises a plurality of sampling pipes 5, when one sampling pipe 5 is collected, the reactant container 3 is isolated by the baffle plate 4, the other sampling pipe 5 is replaced, then the baffle plate 4 is returned to the initial position again, and then the collection process is started again, so that the metal vapor can be dynamically collected without poor dynamic response; the sampling tube 5 is simple in structure, after metal vapor is collected, the cleaning process of the sampling tube 5 is more convenient, collected metal can be recovered only by cleaning the wall surface of the inner tube 8 and the outer wall surface of the filter cartridge 12, and the metal recovery process is more convenient; the device can also continuously collect metal vapor generated at different temperatures, for example, one sampling tube 5 is used for collecting the metal vapor in a certain temperature interval, the other sampling tube 5 is used for collecting the metal vapor in another temperature interval, two sampling tubes 5 can be respectively cleaned, the volatilization amount and volatilization rate of the metal in the two temperature intervals are known, and the device is favorable for researching the volatilization characteristics of the metal, wherein the specific number of the sampling tubes 5 can be set for the experimental device according to actual conditions, for example, if the metal vapor volatilized by a certain metal in four different temperature intervals is required to be collected, four sampling tubes 5 can be set, and the four sampling tubes 5 are respectively used for collecting the metal vapor in different temperature intervals; the test device has higher recovery rate of semi-volatile metal, and the recovery rate of the semi-volatile metal can exceed 90 percent.
As shown in fig. 1, the gas supply system includes a steel cylinder 13, a pressure reducing valve 14, a mass flow controller 15, a surge tank 16, and a gas intake solenoid valve 17;
the steel cylinder 13 stores gas, the steel cylinder 13 is connected with one port of the pressure reducing valve 14, the other port of the pressure reducing valve 14 is connected with the mass flow controller 15, the mass flow controller 15 is connected with the buffer tank 16, the buffer tank 16 is connected with one port of the air inlet electromagnetic valve 17, the other port of the air inlet electromagnetic valve 17 is connected with the furnace tube 2, the controller 18 is electrically connected with the air inlet electromagnetic valve 17, and the controller 18 can control the opening of the air inlet electromagnetic valve 17, so that the gas in the steel cylinder 13 is introduced into the furnace tube 2.
The gas in the steel cylinder 13 may be air, nitrogen or oxygen, the mass flow controller 15 is used for adjusting the flow of the gas entering the furnace tube 2, and the mass flow controller 15 and the air pump 7 are adjusted to make the flow of the gas entering the furnace tube 2 smaller than the air pumping flow of the air pump 7, so that the furnace tube 2 and the condensation part installed in the furnace tube 2 are in a negative pressure state, and the buffer tank 16 is used for buffering the gas. The air inlet electromagnetic valve 17 can be a three-way electromagnetic valve, one port of the air inlet electromagnetic valve 17 is connected with the buffer tank 16, one port is connected with the furnace tube 2, the other port is used as a bypass for emptying, and the air path switching of the air inlet electromagnetic valve 17 is controlled by the controller 18.
In the application, the telescopic device comprises a servo motor, a cam 19 and a connecting rod 20, wherein one end of the cam 19 is connected with one end of the connecting rod 20, the other end of the connecting rod 20 is connected with the baffle 4, the servo motor is connected with the cam 19, the controller 18 is electrically connected with the servo motor, the controller 18 can control the servo motor to drive the cam 19 to rotate, and the connecting rod 20 drives the baffle 4 to be inserted into the furnace tube 2 or to retract into a furnace tube slot from the furnace tube 2. The telescopic device can also be an electric push rod, and the baffle plate is pushed to be inserted into the furnace tube 2 through the electric push rod;
when the sampling tube 5 needs to be replaced, the controller 18 sends a first control instruction to the servo motor, the servo motor drives the cam 19 to rotate, the cam 19 ejects the connecting rod 20, the baffle 4 ejects from the furnace tube slot, the furnace tube 2 is divided into two areas, the reactant container 3 is isolated, when the sampling tube 5 is replaced, the controller 18 firstly sends a second control instruction to the three-way electromagnetic valve 6, the port of the three-way electromagnetic valve 6 connected with the sampling tube 5 inserted into the furnace tube 2 is opened, air suction is started, the controller 18 sends a third control instruction to the servo motor, the servo motor drives the cam 19 to rotate again, the cam 19 drives the connecting rod 20 to retract, the baffle 4 slides downwards from the furnace tube 2 until the end face of the baffle 4 is flush with the inner wall of the furnace tube 2, and metal vapor is collected again.
In the application, the cross section of the cavity in the furnace body 1 can be designed as square, the cross section of the part of the furnace tube 2 in the furnace body 1 is square, so that when the baffle 4 is inserted into the furnace tube 2, the reactant container 3 can be isolated, the cross section of the part of the furnace tube 2 extending out of the furnace body 1 is round, the length of the furnace tube 2 in the furnace body 1 can be designed to be 300-800 mm, the length of the two ends of the furnace tube 2 extending out of the furnace body 1 can be designed to be 30-50 mm, the diameter is 30-50 mm, and the furnace tube slot is positioned at the part of the furnace tube 2 with square cross section and positioned at 1/3 along the length direction of the square part. The furnace body 1 is heated by an electric heating furnace, the inner cylinder 8, the outer cylinder 9 and the baffle plate 4 can be made of quartz glass, corundum, zirconia or high-temperature resistant stainless steel, the reactant container 3 can be made of zirconia, and the reactant container 3 can be made into a square boat shape. The hollow plug 11 is a reducing hollow glass plug, the diameter of the head part of the reducing hollow glass plug is minimum, the diameter of the tail part of the reducing hollow glass plug is maximum, the diameter between the head part and the tail part is gradually changed, the filter cartridge 12 is a filter cartridge 12 made of quartz glass fibers, the filter cartridge 12 is sleeved on the reducing part of the hollow plug 11, an air outlet pipe 21 is arranged at the part, far away from the filter cartridge 12, of the hollow plug 11, and the air outlet pipe 21 is connected with one port of the three-way electromagnetic valve 6.
In the application, the metal vapor collection system further comprises a gas washing cylinder 22, wherein the gas inlet end of the gas washing cylinder 22 is connected with one port of the three-way electromagnetic valve 6, and the gas outlet end is connected with the gas extraction end of the gas extraction pump 7. The gas washing cylinder 22 is used to prevent a trace amount of metal particles from directly flowing into the air through the filter cartridge 12, so that if a trace amount of metal vapor passes through the hollow plug 11, the metal vapor can be discharged to the outside through the gas washing cylinder 22 and then the air pump 7. A silica gel drying bottle can be arranged between the gas washing bottle 22 and the air extracting pump 7, the gas inlet end of the silica gel drying bottle is connected with the gas outlet end of the gas washing bottle 22, the gas outlet end of the silica gel drying bottle is connected with the gas extracting end of the air extracting pump 7, and the silica gel drying bottle is used for drying gas passing through the gas washing bottle 22. A connection hose may be used for connection of the air path in the present test apparatus.
The following describes a process of testing the volatilization rate of lead oxide at 600-1000 ℃ by using the testing device in the application:
0.3g of sodium chloride, 0.025g of lead oxide, 2.7g of silicon dioxide and 2.3g of aluminum oxide are put into a reactant container 3 and are uniformly mixed, wherein the sodium chloride, the silicon dioxide and the aluminum oxide participate in the reaction, the lead oxide can volatilize under the condition of heating, and the reactant container 3 is put into the middle part of a furnace tube 2. One end of the furnace tube 2 is connected with an air inlet electromagnetic valve 17 of an air supply system, and nitrogen is stored in a steel cylinder 13 of the air supply system;
a sampling tube 5 is placed at the other end of the furnace tube 2, a mass flow controller 15 controls the gas flow of nitrogen to be 500ml/ml, an air pump 7 works, a port of the sampling tube 5 in the furnace tube 2 connected with a three-way electromagnetic valve 6 is opened, an electric heating furnace is used for controlling the heating rate to be 10 ℃/min, at the moment, a baffle 4 is in a state of being not inserted into the furnace tube 2, and the sampling tube 5 continuously collects metal vapor in the furnace tube 2;
when the heating temperature reaches 600 ℃, the controller 18 controls the air supply system to stop air supply and controls the baffle plate 4 to be inserted into the furnace tube 2, another sampling tube 5 is replaced, the controller 18 firstly controls the three-way electromagnetic valve 6 to switch the route, then controls the baffle plate 4 to retreat from the furnace tube 2, the air supply system supplies air, and metal vapor in the furnace tube 2 is collected again;
the above process is repeated at 700 deg.c for more than one time, 800 deg.c, 900 deg.c and 1000 deg.c until the whole experimental device is cooled to room temperature and the last sampling tube 5 is taken out. The whole test process uses 6 sampling tubes 5, uses 3% dilute nitric acid solution to wash and soak the inner wall surface of the inner cylinder 8 of the condensing part and the outer wall surface of the filter cylinder 12, finally filters the liquid to obtain 6 lead-containing solution samples, measures the concentration of lead in the solution by using an atomic absorption instrument, and can obtain the volatilization amount and volatilization rate of lead in each time period, and the recovery rate of the lead measured after all data are processed is up to 91%.
The test device has higher recovery rate of metal, can reach more than 90 percent, and can realize dynamic collection of metal vapor; the device has simple structure and convenient operation process, realizes ingenious design of integration of negative pressure sampling and cooling, and solves the problems of complex structure and low recovery rate of the existing test device; the metal vapor generated in the furnace tube 2 can be collected in real time, and the problem of sampling lag existing in the existing test device is solved.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The meaning of "and/or" in the present application means that each exists alone or both exist.
"connected" as used herein means either a direct connection between components or an indirect connection between components via other components.
With the above-described preferred embodiments according to the present application as an illustration, the above-described descriptions can be used by persons skilled in the relevant art to make various changes and modifications without departing from the scope of the technical idea of the present application. The technical scope of the present application is not limited to the description, but must be determined according to the scope of claims.

Claims (8)

1. Can collect tubular furnace test device of metal vapor dynamically, its characterized in that: the tubular furnace test device capable of dynamically collecting metal vapor comprises a horizontal tubular furnace system, a metal vapor collecting system, a gas supply system and a controller;
the horizontal tube furnace system comprises a furnace body, a furnace tube, a reactant container, a baffle and a telescopic device, wherein the reactant container is arranged in the furnace tube, the furnace tube is positioned in the furnace body, two ends of the furnace tube extend out of the furnace body, a furnace body slot is arranged on the side wall of the furnace body, a furnace tube slot is arranged at a position on the furnace tube corresponding to the furnace body slot, the baffle is sequentially inserted into the furnace body slot and the furnace tube slot and is connected with the telescopic device, and the telescopic device can drive the baffle to be inserted into the furnace tube through the furnace tube slot or drive the baffle to retract into the furnace tube slot from the furnace tube;
the metal vapor collecting system comprises a plurality of sampling pipes, a three-way electromagnetic valve and an air pump, wherein each sampling pipe comprises a condensing part and a filtering part, the condensing part comprises an inner cylinder and an outer cylinder, the outer cylinder is sleeved outside the inner cylinder, the end part of the inner cylinder is connected with the end part of the outer cylinder through a ring piece with a hole, the filtering part comprises a hollow plug and a filtering cylinder, the hollow plug is inserted into the inner cylinder at one end of the condensing part, the part of the hollow plug inserted into the inner cylinder is sleeved with the filtering cylinder, the sampling pipe is used for collecting metal vapor, one port of the three-way electromagnetic valve is connected with the air extraction end of the air pump through a pipeline, the other two ports are respectively connected with the two sampling pipes, and the other two ports are respectively connected with the hollow plugs of the two sampling pipes through pipelines;
the air supply system is connected with one end of the furnace tube, when metal vapor is collected, the air supply system supplies air for the furnace tube, the air pump pumps air, the condensing parts of the two sampling tubes connected with the three-way electromagnetic valve are alternately inserted into the other end of the furnace tube, after the other end of the furnace tube is inserted into one of the sampling tubes connected with the three-way electromagnetic valve, the reactant container and the condensing part inserted into the furnace tube are positioned at two sides of the furnace tube slot, the baffle is positioned in the furnace tube slot, the controller controls the opening of the port of the sampling tube inserted into the furnace tube connected with the three-way electromagnetic valve, and simultaneously controls the opening of the air pump connected with the three-way electromagnetic valve, the air pumping quantity of the air pump is larger than the air supply quantity of the air supply system, the condensing parts in the furnace tube and the furnace tube are in a negative pressure state, air enters the furnace tube through the circular ring sheet with holes of the condensing parts, and the air provided by the air and the air supply system cools the metal vapor in the furnace tube, when the metal particles formed by the metal vapor during cooling adhere to the wall surface of the inner cylinder of the condensation part and are filtered by the outer wall surface of the filter cylinder, after one of the sampling pipes connected with the three-way electromagnetic valve is collected, the controller controls the telescopic device to drive the baffle to be inserted into the furnace pipe through the furnace pipe slot, the air supply system stops supplying air, the sampling pipe in the furnace pipe is taken out, the other sampling pipe connected with the three-way electromagnetic valve is inserted into the other end of the furnace pipe, the controller firstly controls the port of the sampling pipe inserted into the furnace pipe and connected with the three-way electromagnetic valve to be opened, then controls the telescopic device to drive the baffle to retract into the furnace pipe slot from the furnace pipe, the air supply system supplies air, the other sampling pipe connected with the three-way electromagnetic valve starts collecting the metal vapor, the sampling pipe connected with the three-way electromagnetic valve and the metal vapor collected is disassembled, connecting sampling pipes which are not used for collecting metal vapor with a three-way electromagnetic valve, wherein the mode of collecting the metal vapor by each sampling pipe connected with the three-way electromagnetic valve is the same;
the air supply system comprises a steel cylinder, a pressure reducing valve, a mass flow controller, a buffer tank and an air inlet electromagnetic valve;
the gas is stored in the steel cylinder, the steel cylinder is connected with one port of the pressure reducing valve, the other port of the pressure reducing valve is connected with the mass flow controller, the mass flow controller is connected with the buffer tank, the buffer tank is connected with one port of the air inlet electromagnetic valve, the other port of the air inlet electromagnetic valve is connected with the furnace tube, and the controller can control the opening of the air inlet electromagnetic valve to enable the gas in the steel cylinder to be introduced into the furnace tube;
the telescopic device comprises a servo motor, a cam and a connecting rod, wherein one end of the cam is connected with one end of the connecting rod, the other end of the connecting rod is connected with the baffle, the servo motor is connected with the cam, the controller can control the servo motor to drive the cam to rotate, and the baffle is driven to be inserted into the furnace tube through the connecting rod or to retract into the furnace tube slot from the furnace tube.
2. The tube furnace test device capable of dynamically collecting metal vapor according to claim 1, wherein: the cross section of the cavity inside the furnace body is square, the cross section of the part of the furnace tube, which is positioned inside the furnace body, is square, and the cross section of the part of the furnace tube, which extends out of the furnace body, is round.
3. The tube furnace test device capable of dynamically collecting metal vapor according to claim 1, wherein: the metal vapor collection system further comprises a gas washing bottle, the gas inlet end of the gas washing bottle is connected with one port of the three-way electromagnetic valve, and the gas outlet end of the gas washing bottle is connected with the gas extraction end of the gas extraction pump.
4. A tube furnace test apparatus capable of dynamically collecting metal vapor according to claim 3, wherein: the metal vapor collection system further comprises a silica gel drying bottle, the air inlet end of the silica gel drying bottle is connected with the air outlet end of the gas washing bottle, and the air outlet end of the silica gel drying bottle is connected with the air exhaust end of the air exhaust pump.
5. The tube furnace test device capable of dynamically collecting metal vapor according to claim 1, wherein: the hollow plug is a reducing hollow glass plug, the filter cartridge is made of quartz glass fibers, the filter cartridge is sleeved on the reducing part of the hollow plug, an air outlet pipe is arranged on the part, away from the filter cartridge, of the hollow plug, and the air outlet pipe is connected with one port of the three-way electromagnetic valve.
6. The tube furnace test device capable of dynamically collecting metal vapor according to claim 1, wherein: the baffle is made of quartz glass, corundum, zirconia or high-temperature-resistant stainless steel.
7. The tube furnace test device capable of dynamically collecting metal vapor according to claim 1, wherein: the width of the furnace tube slot is 0.5-1 mm larger than the thickness of the baffle.
8. The tube furnace test device capable of dynamically collecting metal vapor according to claim 1, wherein: the air extracting pump is a diaphragm pump.
CN201810816836.7A 2018-07-24 2018-07-24 Tubular furnace test device capable of dynamically collecting metal vapor Active CN109030708B (en)

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CN202166582U (en) * 2011-07-20 2012-03-14 夏鸣 Water reaction metal fuel high-temperature experiment apparatus
CN105043967A (en) * 2015-08-31 2015-11-11 西安热工研究院有限公司 Smoke-coal ash synergic corrosion testing device
CN204855328U (en) * 2015-08-31 2015-12-09 西安热工研究院有限公司 Flue gas - coal ash is corrosion test device in coordination
CN108279206A (en) * 2018-03-06 2018-07-13 中山大学 A kind of high-temperature molten salt corrosion pilot system
CN207891404U (en) * 2017-12-18 2018-09-21 昆明理工大学 The experimental facilities of condensing metal steam under a kind of mixed atmosphere
CN208383827U (en) * 2018-07-24 2019-01-15 南京师范大学 It is a kind of can dynamic collection metal vapors tube furnace experimental rig
CN115710014A (en) * 2022-11-04 2023-02-24 重庆大学 Carbon hydrogen raw material coupling abandonment PVC and LCD pyrolysis extraction InCl together 3 In a semiconductor device

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN202166582U (en) * 2011-07-20 2012-03-14 夏鸣 Water reaction metal fuel high-temperature experiment apparatus
CN105043967A (en) * 2015-08-31 2015-11-11 西安热工研究院有限公司 Smoke-coal ash synergic corrosion testing device
CN204855328U (en) * 2015-08-31 2015-12-09 西安热工研究院有限公司 Flue gas - coal ash is corrosion test device in coordination
CN207891404U (en) * 2017-12-18 2018-09-21 昆明理工大学 The experimental facilities of condensing metal steam under a kind of mixed atmosphere
CN108279206A (en) * 2018-03-06 2018-07-13 中山大学 A kind of high-temperature molten salt corrosion pilot system
CN208383827U (en) * 2018-07-24 2019-01-15 南京师范大学 It is a kind of can dynamic collection metal vapors tube furnace experimental rig
CN115710014A (en) * 2022-11-04 2023-02-24 重庆大学 Carbon hydrogen raw material coupling abandonment PVC and LCD pyrolysis extraction InCl together 3 In a semiconductor device

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