High-temperature combustion hydrolysis determination device suitable for fluorine in coal

Abstract

The utility model relates to a device for detecting trace harmful elements in coal, in particular to a high-temperature combustion hydrolysis measuring device suitable for fluorine in coal. Comprising a temperature control device, a heating device and a gas path reaction device, the temperature control device comprises a temperature controller and a temperature sensor, the heating device comprises a heating furnace body, two sample testing channels are arranged in the heating furnace body in parallel, heaters are arranged around the sample testing channels, and heat preservation and insulation devices are arranged on the outer sides of the heaters; the heat preservation and insulation device isolates the heater from a furnace body shell of the heating furnace body. According to the utility model, the two groups of sample testing channels are arranged, so that parallel samples are simultaneously tested in the sample testing process, the sample detection accuracy and the testing efficiency are improved, the resources are effectively saved, and the energy consumption is reduced. And meanwhile, the device is provided with a clamping part for the wire and the heater, so that the problem that the wire is overheated due to overlarge conductivity coefficient change is effectively prevented, and the equipment failure rate is reduced.

Description

TECHNICAL FIELD

[0001] The utility model relates to coal trace harmful element detection device, specifically related to a coal fluorine high temperature hydrolysis determination device. BACKGROUND

[0002] The determination method of fluorine in coal is mainly tested through high temperature combustion hydrolysis-fluorine ion selective electrode method, and the method is suitable for the determination of fluorine content in lignite, bituminous coal and anthracite. The test is that the coal sample is combusted and hydrolyzed in the mixed gas stream of oxygen and water vapor, and the fluorine in the coal is all converted into volatile fluorides (such as SF4 and HF) and quantitatively dissolved in water. The fluorine ion concentration in the sample solution is determined by using the fluorine ion selective electrode, and then the fluorine content in the coal sample is calculated.

[0003] At present, the coal fluorine high temperature combustion hydrolysis determination device in use is a single-channel single-group sample test, in order to ensure the accuracy of the measurement result, the determination of fluorine in coal needs to be tested by parallel samples, and the repeatability and accuracy of sample detection are determined by the parallel sample test method. In actual production, parallel sample testing needs to test two hydrolysis devices, which leads to low test efficiency, high energy consumption, and poor repeatability of sample testing due to various factors when testing the two hydrolysis devices. At the same time, the heating components of the existing high temperature combustion hydrolysis device are connected with the wires, and due to the change of the conductance coefficient, the heating component and the wire connection end are often burned out, and the equipment failure rate is frequent.

[0004] Therefore, the inventor makes great improvement and proposes a high temperature combustion hydrolysis determination device suitable for fluorine in coal. The purpose is to solve the problems of low test efficiency, high energy consumption, poor repeatability and frequent equipment failure rate of heating components and wires when using two hydrolysis devices for parallel sample testing. CONTENT OF THE UTILITY MODEL

[0005] In order to solve the above technical problems, the utility model realizes the following technical scheme:

[0006] A high temperature combustion hydrolysis determination device suitable for fluorine in coal, comprising a temperature control device, a heating device and a gas path reaction device, characterized in that the temperature control device comprises a temperature controller and a temperature sensor, the heating device comprises a heating furnace body, two groups of sample test channels are arranged in parallel in the heating furnace body, heaters are arranged around the sample test channels, and heat preservation and insulation devices are arranged outside the heaters to isolate the heaters from the furnace body shell of the heating furnace body.

[0007] The temperature measuring hole is provided below the sample testing channel, and a temperature sensor is installed on the temperature measuring hole, and the temperature measuring probe of the temperature sensor is located in the internal heating area of the heater, and there is a clamping component connected with the lead wire on the heater, the clamping component comprises a clamping sheet, a conductive strip, an insulating gasket, a conductive bolt and a compression spring, the conductive strip is arranged below the clamping sheet, the heater is arranged below the conductive strip, the end of the clamping sheet is provided with a connecting hole, the conductive bolt is arranged on the connecting hole, and the insulating gasket, the compression spring, the fixed sheet, the spring washer and the fixed nut are sequentially arranged on the conductive bolt.

[0008] The heating device is provided with a first constant temperature zone, a second constant temperature zone, a third constant temperature zone and a fourth constant temperature zone, and the gas path reaction device comprises a quartz tube, a water vapor generating device, a silica gel hose, a gas cylinder and a gas flow meter and a reaction condensing device.

[0009] Preferably, the temperature controller comprises a temperature control table and a solid-state relay.

[0010] Preferably, the temperature sensor is an S-shaped platinum-rhodium thermocouple.

[0011] Preferably, the heater is a hollow cylindrical double-spiral silicon-carbon tube.

[0012] Preferably, the quartz tube is installed on the sample testing channel.

[0013] Preferably, one end of the quartz tube is provided with a sample feeding rod, and a sealing component is arranged on the sample feeding rod.

[0014] Preferably, the front end of the gas flow meter is provided with a gas drying device.

[0015] The beneficial effects of the present application are that:

[0016] 1. The two groups of sample testing channels are arranged, so that the parallel samples can be tested at the same time in the sample testing process, the accuracy and testing efficiency of sample detection are improved, resources are effectively saved, and energy consumption is reduced.

[0017] 2. The lead wire and the clamping component of the heater are arranged, so that the problem of overheating of the lead wire due to too large electric conductivity coefficient and high heating temperature is effectively prevented, and the equipment failure rate is greatly reduced.

[0018] 3. The temperature measuring probe of the temperature sensor is arranged in the internal heating area of the heater, so that the temperature measurement is more accurate.

[0019] 4. The heater is provided with different resistance values, so that different constant temperature zones are arranged, the applicability of the equipment is greatly enhanced, and the control requirements of different temperatures in the sample testing process are met. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1The utility model discloses a three-dimensional structure schematic view of the heater 8.

[0021] Figure 2 The utility model discloses a sectional view of the clamping part 12.

[0022] Figure 3 The utility model discloses a three-dimensional structure schematic view of the heater 8.

[0023] Figure 4 The utility model discloses a sectional view of the clamping part 12.

[0024] Figure 5 The utility model discloses a structure schematic view of the gas path reaction device 3.

[0025] Mark: 1-temperature control device, 2-heating device, 3-gas path reaction device, 4-temperature controller, 5-temperature sensor, 6-heating furnace body, 7-sample test channel, 8-heater, 9-heat preservation insulation device, 10-furnace body shell, 11-temperature measuring hole, 12-clamping part, 13-clamping piece, 14-conductive band, 15-insulating gasket, 16-conductive bolt, 17-pressing spring, 18-connection hole, 19-fixing piece, 20-spring washer, 21-fixing nut, 22-first constant temperature area, 23-second constant temperature area, 24-third constant temperature area, 25-fourth constant temperature area, 26-quartz tube, 27-water vapor generating device, 28-silica gel hose, 29-gas cylinder, 30-gas flowmeter, 31-reaction condensing device, 32-water vapor heating furnace, 33-triangular flask, 34-water vapor pipeline, 35-condensing tube, 36-sample feeding rod. DETAILED DESCRIPTION

[0026] The utility model discloses a kind of high-temperature combustion hydrolysis determination device for fluorine in coal suitable for according to the specific implementation mode, structure, characteristics and effect of the utility model, as follows detailed description.

[0027] Refer to the accompanying drawings Figures 1-5The application relates to a high-temperature combustion and hydrolysis determination device for fluorine in coal, which comprises a temperature control device 1, a heating device 2 and a gas path reaction device 3, wherein the temperature control device 1 comprises a temperature controller 4 and a temperature sensor 5, the heating device 2 comprises a heating furnace body 6, two groups of sample test channels 7 are arranged in parallel in the heating furnace body 6, heaters 8 are arranged around the sample test channels 7, heat insulation devices 9 are arranged outside the heaters 8, the heat insulation devices 9 isolate the heaters 8 from a furnace body shell 10 of the heating furnace body 6, and temperature measuring holes 11 are arranged below the sample test channels 7, temperature sensors 5 are arranged on the temperature measuring holes 11, and temperature measuring probes of the temperature sensors 5 are located in internal heating areas of the heaters 8.

[0028] The heating device 2 is provided with a first constant temperature area 22, a second constant temperature area 23, a third constant temperature area 24 and a fourth constant temperature area 25, the gas path reaction device 3 comprises a quartz tube 26, a water vapor generating device 27, a silica gel hose 28, a gas cylinder 29, a gas flow meter 30 and a reaction condensing device 31.

[0029] The temperature control device 1 is a rectangular box body which is formed by sheet metal bending and welding, a control panel is arranged at the front of the rectangular box body, a control box body is fixed on the rear side of the control panel through bolts, the control box body is movably connected with the rectangular box body through slide rails, the control panel and the control box body can move forward and backward along the slide rails, and thus the temperature control elements can be adjusted and maintained in the later period.

[0030] The gas flow meters 30 are arranged on the left and right sides of the control panel, and the temperature controllers 4 are arranged on the side surfaces of the gas flow meters 30. The temperature controller 4 comprises a temperature control table and a solid-state relay, a digital current and voltage meter is arranged on the side surface of the temperature controller 4, the current and voltage values of an output circuit can be displayed in real time, indicator lamps and a power switch are arranged below the temperature controller 4, and a voltage regulating switch is arranged.

[0031] In the control box is provided with temperature control element, temperature control element includes solid state relay, solid state voltage regulator and fuse, solid state relay below is provided with radiator, solid state voltage regulator is controlled through voltage regulator switch, the whole temperature control element is connected through wire, temperature control principle is that temperature sensor 5 connected on temperature controller 4 receives temperature signal, temperature sensor 5 is S type platinum rhodium thermocouple, then through temperature controller 4 control solid state relay, through solid state relay control output circuit's on-off, realize the control to temperature, simultaneously in output circuit series connection voltage regulating device, realize the regulation to output circuit voltage.Warm control device 1 can select Xiamen Yudian control cabinet AI-808P type temperature controller.

[0032] Heating device 2 includes heating furnace body 6 and heater 8, heating furnace body 6 includes furnace shell 10, heat preservation insulation device 9 and sample test channel 7, heat preservation insulation device 9 includes heat insulation paint, heat insulation cotton and refractory hearth, furnace shell 10 is stainless steel sheet metal part, the inside of stainless steel sheet metal part is coated with heat insulation paint, and heat insulation cotton is installed on the heat insulation paint on the inside, and refractory hearth is installed on the heat insulation cotton, the refractory hearth is a cylindrical cavity, sample test channels 7 are provided on the left and right sides of the refractory hearth, quartz tube 26 locking nut is provided on the sample test channel 7, temperature sensing hole 11 is provided below the sample test channel 7, and temperature sensor 5 is installed on the temperature sensing hole 11.

[0033] Heater 8 is a hollow cylindrical double helix silicon carbide tube, the silicon carbide tube is installed in the refractory hearth area, the silicon carbide tube is a non-metallic electric heating element with silicon carbide as the main raw material, in order to realize the first constant temperature zone 22, the second constant temperature zone 23, the third constant temperature zone 24 and the fourth constant temperature zone 25 of the heating device 2, the silicon carbide tube installed in different constant temperature zones will be oxidized, after the oxidation reaction, silicon dioxide will be generated, the resistance value of the silicon carbide tube will be increased, and the resistance value of the silicon carbide tube in different constant temperature zones will be different, under the condition of loading the same current and voltage, the control requirements of different temperatures are realized.

[0034] A clamping part 12 is provided at one end of the silicon carbide tube, the clamping part 12 includes clamping pieces 13, the clamping pieces 13 are two half-circular metal pieces arranged above and below, the radius of the arc surface of the half-circular metal pieces is the same as the radius of the silicon carbide tube, an electrically conductive strip 14 is provided at the joint of the half-circular metal pieces and the silicon carbide tube, the electrically conductive strip 14 is a metal woven piece, the flexibility of the metal woven piece enables the half-circular metal pieces to tightly adhere to the silicon carbide tube, connecting holes 18 are provided at both ends of the half-circular metal pieces, electrically conductive bolts 16 are provided on the connecting holes 18, the electrically conductive bolts 16 are pure copper bolts, high-temperature wires are connected to the elements on the temperature controller 4 through the pure copper bolts.

[0035] Since the heater 8 is a hollow cylindrical double helix silicon-carbon tube, it has the thermal expansion and contraction characteristics when heated, so the conductive bolt 16 cannot be too tight when installed, too tight will cause the heater 8 to be squeezed and broken when heated and expanded, and also cannot be too loose, too loose will easily lead to poor contact, causing the wire to heat and burn out at the connection end. The device is provided with a compression spring 17 installed between the two clamping pieces 13, and the clamping pieces 13 are in close contact with the wire at the connection end through the elastic force of the compression spring 17.

[0036] The gas path reaction device 3 includes a quartz tube 26, a water vapor generating device 27, a silica hose 28, a gas cylinder 29, a gas flow meter 30, and a reaction condensing device 31. The water vapor generating device 27 includes a water vapor heating furnace 32 and a triangular flask 33. A gas drying device is provided at the front end of the gas flow meter 30, which is used to remove the water content of the oxygen in the gas cylinder 29 to prevent the flow meter from entering water vapor and affecting the test results. A sample feeding rod 36 is provided at one end of the quartz tube 26, and a sealing component, which is a high-temperature silica plug, is provided on the sample feeding rod 36.

[0037] The quartz tube 26 is provided with a first branch pipe and a second branch pipe. The first branch pipe is arranged on the upper end face of the quartz tube 26, and oxygen enters the inside of the quartz tube 26 through the first branch pipe. The second branch pipe is arranged on the lower end face of the quartz tube 26, and water vapor enters the inside of the quartz tube 26 through the second branch pipe. The oxygen entering from the first branch pipe mixes with the water vapor entering from the second branch pipe at the front end of the quartz tube 26 to form a mixed gas, which reacts with the coal sample during the test process.

[0038] The triangular flask 33 is placed on the water vapor heating furnace 32, and distilled water is contained in the triangular flask 33. The triangular flask 33 is connected to the second branch pipe of the quartz tube 26 through a water vapor pipeline 34. After the distilled water in the triangular flask 33 is heated and boiled by the water vapor heating furnace 32, water vapor enters the quartz tube 26 through the second branch pipe. A silica hose 28 is connected to the outlet end of the quartz tube 26, and a reaction condensing device 31 is arranged below the silica hose 28. The reaction condensing device 31 includes a condensing pipe 35 and a condensing water inlet and outlet pipe. A volumetric flask is arranged below the condensing pipe 35.

[0039] In use, the quartz tube 26 is installed on the two groups of sample test channels 7, and the circuit, gas path and cooling water path are connected. A small amount of high-temperature resistant cotton is inserted into the gas outlet end of the quartz tube 26. The temperature of the fourth constant temperature zone 25 is increased to 1100℃, and the temperature sensor 5 is located at the center of the fourth constant temperature zone 25. Another group of platinum-rhodium-platinum thermocouples is used to measure the first constant temperature zone 22, the second constant temperature zone 23 and the third constant temperature zone 24, so that the temperature is relatively stable at 300℃, 600℃ and 900℃ in three temperature zones.

[0040] About 300 mL of water was added to the flask 33 and heated to boiling, and the condenser 35 was opened to cool water. The sample push rod 36 was tightly plugged with a silica gel plug, and oxygen was introduced before the water in the flask 33 boiled. The oxygen flow was adjusted to 400 mL / min, and the water vapor generator 27 was adjusted to about 2 mL / min. After the system was checked for leaks, the water vapor and oxygen were introduced and purged for 15 min.

[0041] About 300 mL of water was added to the flask 33 and heated to boiling, and the condenser 35 was opened to cool water. The sample push rod 36 was tightly plugged with a silica gel plug, and oxygen was introduced before the water in the flask 33 boiled. The oxygen flow was adjusted to 400 mL / min, and the water vapor generator 27 was adjusted to about 2 mL / min. After the system was checked for leaks, the water vapor and oxygen were introduced and purged for 15 min.

[0042] The above is only a preferred embodiment of the present application, and is not intended to limit the application in any form. Any modification, equivalent change and modification of the above embodiment, which does not deviate from the technical solution of the present application, and which is based on the technical essence of the present application, still belongs to the scope of the technical solution of the present application.

Claims

1. A device for high temperature combustion hydrolysis determination of fluorine in coal, comprising a temperature control device (1), a heating device (2) and a gas path reaction device (3), characterized in that, The temperature control device (1) comprises a temperature controller (4) and a temperature sensor (5), the heating device (2) comprises a heating furnace body (6), two groups of sample test channels (7) are arranged in parallel in the heating furnace body (6), a heater (8) is arranged around the sample test channel (7), a heat preservation and insulation device (9) is arranged outside the heater (8), and the heat preservation and insulation device (9) isolates the heater (8) from a furnace body shell (10) of the heating furnace body (6); A temperature measuring hole (11) is arranged below the sample test channel (7), the temperature sensor (5) is installed on the temperature measuring hole (11), a temperature measuring probe of the temperature sensor (5) is located in a heating area inside the heater (8), a clamping component (12) connected with a wire is arranged on the heater (8), the clamping component (12) comprises a clamping sheet (13), a conductive belt (14), an insulating gasket (15), a conductive bolt (16) and a compression spring (17), the conductive belt (14) is arranged below the clamping sheet (13), the heater (8) is arranged below the conductive belt (14), the clamping sheet (13) is provided with a connecting hole (18), the conductive bolt (16) is arranged on the connecting hole (18), and the insulating gasket (15), the compression spring (17), a fixed sheet (19), a spring washer (20) and a fixed nut (21) are sequentially installed on the conductive bolt (16); The heating device (2) is provided with a first constant temperature zone (22), a second constant temperature zone (23), a third constant temperature zone (24) and a fourth constant temperature zone (25), and the gas path reaction device (3) comprises a quartz tube (26), a water vapor generating device (27), a silica gel hose (28), a gas cylinder (29), a gas flow meter (30) and a reaction condensing device (31).

2. The apparatus for determination of high temperature combustion hydrolysis of fluorine in coal according to claim 1, characterized in that: The temperature controller (4) comprises a temperature control table and a solid-state relay.

3. The apparatus for determination of high temperature combustion hydrolysis of fluorine in coal according to claim 2, characterized in that: The temperature sensor (5) is an S-shaped platinum-rhodium thermocouple.

4. The apparatus for determination of high temperature combustion hydrolysis of fluorine in coal according to claim 3, characterized in that: The heater (8) is a hollow cylindrical double-spiral silicon-carbon tube.

5. The apparatus for determination of high temperature combustion hydrolysis of fluorine in coal according to claim 4, characterized in that: The quartz tube (26) is installed on the sample test channel (7).

6. The apparatus for determination of high temperature combustion hydrolysis of fluorine in coal according to claim 1, characterized in that: One end of the quartz tube (26) is provided with a sample feeding rod (36), and a sealing component is arranged on the sample feeding rod (36).

7. The apparatus for determination of high temperature combustion hydrolysis of fluorine in coal according to claim 1, characterized in that: The gas flow meter (30) is provided with a gas drying device at the front end.

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