CN218160459U - Reduction treatment device for carbon-supported platinum catalyst - Google Patents
Reduction treatment device for carbon-supported platinum catalyst Download PDFInfo
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- CN218160459U CN218160459U CN202222466246.0U CN202222466246U CN218160459U CN 218160459 U CN218160459 U CN 218160459U CN 202222466246 U CN202222466246 U CN 202222466246U CN 218160459 U CN218160459 U CN 218160459U
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Abstract
The utility model discloses a reduction treatment device for carbon-supported platinum catalyst, a reaction tube is of a vertical structure, an upper flange is arranged at the upper end of a quartz tube, and a lower flange is arranged at the lower end of the quartz tube; a sand core used for containing the catalyst pile layer is arranged in the quartz tube, and the sand core is provided with a plurality of pores; the reducing gas input unit and the purging unit are both communicated with the input end of the mixing tank, the output end of the mixing tank is communicated with the upper flange of the reaction tube, and the lower flange of the reaction tube is communicated with the tail gas treatment unit; the heating furnace surrounds the periphery of the reaction tube. The utility model discloses a vertical quartz material's reaction tube to with the catalyst tiling on the psammitolite in the reaction tube, reducing gas from last flange get into the reaction tube in back, can fully contact with the catalytic substance, vertical structure's reaction tube and set up the inside psammitolite that has the aperture simultaneously, avoid the reduction product to pile up and lead to partial catalyst can't react with reducing gas in the catalyst, solved the slow and inhomogeneous problem of reduction speed.
Description
Technical Field
The utility model relates to a hydrogen fuel cell technical field specifically is a reduction processing apparatus for carbon carries platinum catalyst.
Background
The proton exchange membrane fuel cell is a device for directly converting chemical energy into electric energy through electrochemical reaction, wherein the hydrogen fuel cell taking hydrogen as fuel has better application prospect in the fields of new energy automobiles, national defense war industry and the like due to the advantages of environmental friendliness, high energy density, high conversion efficiency and the like. It has the advantages of zero emission, no pollution, high fuel efficiency and the like. The basic reaction principle of the hydrogen fuel cell is that fuel gas hydrogen generates hydrogen oxidation reaction at an anode to lose electrons and change the electrons into protons, the protons are combined with water and then migrate to a cathode through a proton exchange membrane to generate oxygen reduction reaction with oxygen and the electrons from an external circuit to generate water, and the electrons form current through the external circuit to do work outwards. The ORR reaction at the cathode is very slow in kinetics and usually requires the use of a catalyst containing the noble metal platinum (Pt) to accelerate the reaction rate.
In order to save cost, through the development of over twenty years, the catalyst of the hydrogen fuel cell is developed from a catalyst containing pure Pt nano particles to a catalyst containing Pt nano particles loaded by carbon nano tubes (carbon-loaded platinum catalyst for short), and the Pt loading capacity is reduced. One typical preparation procedure for the carbon-supported platinum catalyst is as follows: immersing the carbon nano tube particles in an aqueous solution containing chloroplatinic acid for a period of time, and filtering and collecting to obtain a catalyst primary product. The primary product is treated by the drying equipment to remove free water on the surface of the catalyst, and then transferred to the reduction treatment device. On the reduction treatment device, the chemical substance' chloroplatinic acid aqueous compound (Cl) 6 H 2 Pt.xH 2 O) "at a certain temperature under hydrogen-containing atmosphereAnd reducing the catalyst into a platinum simple substance in the atmosphere to obtain the carbon nano tube supported Pt nano particle catalyst.
In the step of the atmosphere reduction process, HCl and H as byproducts are generated simultaneously while obtaining the platinum simple substance 2 And O. If the by-product does not leave the catalyst surface in time, insufficient reduction of the platinum atoms or a slow chemical reduction rate will result. For particles located at different positions of the catalyst stack, uneven gas diffusion will result in uneven reduction of the platinum atoms.
HCl and H as by-products of the reduction reaction 2 O is weak in corrosivity in a gas state, but is strong in acid hydrochloric acid when condensed into a liquid state, and has strong chemical corrosion performance on metals except gold and zirconium alloy. The price of gold and zirconium alloy is extremely expensive, and at present, quartz pipelines are mostly selected as reactors of devices. However, the quartz material is not a plastic material, but a brittle material, and the brittle material has a property of breaking a fracture when undergoing a small deformation. It is now common for industry suppliers and customers to consider that the upper safe pressure limit in quartz tubes is 0.02MPa (gauge pressure). When the pressure of the gas in the pipe exceeds the upper limit, the gas in the pipe may leak, and a large safety risk exists.
At present, the reduction device adopts a reduction device of a horizontal reaction tube containing a gas circuit and a heating device, and directly puts catalyst particles to be treated into the horizontal reaction tube, or firstly puts the catalyst particles to be treated into a carrying container, and then puts the carrying container into the horizontal reaction tube. Gas enters from one side of the horizontal reaction tube, passes through the catalyst stack layer and is discharged from the other side. Since the catalyst layer generally does not block the entire cross section of the quartz tube, the gas diffuses into the layer at least in part and mostly sweeps over the top of the layer, so that the resistance to gas flow created by the catalyst layer is low and the operating pressure of such devices is near atmospheric. And as the flow rate of the reducing gas increases, most of the gas is still blown over the upper portion or the shallow surface of the catalyst stack layer, and the middle-lower layer of the catalyst stack layer still cannot contact with the fresh reducing gas.
SUMMERY OF THE UTILITY MODEL
The utility model discloses the technical problem that will solve lies in: the problem of insufficient reduction of catalyst particles in a reduction device is solved.
In order to solve the technical problem, the utility model provides a following technical scheme:
a reduction treatment device for a carbon-supported platinum catalyst comprises a reducing gas input unit, a purging unit, a mixing tank, a reaction tube, a heating furnace and a tail gas treatment unit;
the reaction tube is of a vertical structure and comprises a quartz tube, an upper flange and a lower flange; the upper flange is arranged at the upper end of the quartz tube, and the lower flange is arranged at the lower end of the quartz tube; a sand core used for containing the catalyst pile layer is arranged in the quartz tube, and the sand core is provided with a plurality of pores;
the reducing gas input unit and the purging unit are both communicated with the input end of the mixing tank, the output end of the mixing tank is communicated with the upper flange of the reaction tube, and the lower flange of the reaction tube is communicated with the tail gas treatment unit; the heating furnace surrounds the periphery of the reaction tube.
The advantages are that: the utility model discloses a vertical quartz material's reaction tube to with the catalyst tiling on the psammitolite in the reaction tube, reducing gas from last flange get into the reaction tube in the back, can fully contact with the catalytic substance, vertical structure's reaction tube and set up the inside psammitolite that has the aperture simultaneously can make reduction product HCl and H 2 O can flow into the lower end of the reaction tube in time, so that the situation that part of the catalyst can not react with the reducing gas due to the fact that the reducing product is accumulated in the catalyst is avoided, and the problems of slow reducing speed and uneven reducing are solved.
Preferably, the reducing gas input unit includes a reducing gas pipe, a first solenoid valve, a first flow controller, and a first check valve;
the input end of the reducing gas pipe is communicated with the input end of the mixing tank through a pipeline, the first electromagnetic valve, the first flow controller and the first one-way valve are sequentially installed on the pipeline between the reducing gas pipe and the mixing tank respectively, and the flow direction of the first one-way valve is from the reducing gas pipe to the mixing tank.
Preferably, the purge unit includes an inert gas pipe, a second solenoid valve, a second flow controller, and a second check valve;
the input end of the inert gas pipe is communicated with the input end of the mixing tank through a pipeline, the second electromagnetic valve, the second flow controller and the second one-way valve are sequentially installed on the pipeline between the reducing gas pipe and the mixing tank respectively, and the circulation direction of the second one-way valve is from the inert gas pipe to the mixing tank.
Preferably, the tail gas treatment unit comprises an alkali liquor neutralization tank, an adsorption tank and a vacuum pump;
the input end of the alkali liquor neutralization tank is communicated with the lower flange of the reaction tube, the output end of the alkali liquor neutralization tank is communicated with the input end of the adsorption tank, and the output end of the adsorption tank is communicated with the atmosphere after passing through the vacuum pump.
Preferably, the inner cavity surfaces of the upper flange, the lower flange, the mixing tank and the alkali liquor neutralizing tank are all sprayed with polytetrafluoroethylene or modified materials thereof.
Preferably, the hydrogen sensor further comprises a control system, wherein the control system comprises a PLC processor, a touch screen, a first pressure gauge, a second pressure gauge, a first pressure sensor, a second pressure sensor, a first temperature sensor, a second temperature sensor, a third temperature sensor, a fourth temperature sensor, a fifth temperature sensor, a sixth temperature sensor and a hydrogen detector.
The input end of the PLC processor is respectively connected with the touch screen, the first pressure gauge, the second pressure gauge, the first pressure sensor, the second pressure sensor, the first temperature sensor, the second temperature sensor, the third temperature sensor, the fourth temperature sensor, the fifth temperature sensor, the sixth temperature sensor and the hydrogen detector;
the first pressure meter and the first pressure sensor are both arranged on a pipeline between the mixing tank and the reaction tube; the second pressure meter and the second pressure sensor are both arranged on a pipeline between the adsorption tank and the vacuum pump;
the first temperature sensor, the second temperature sensor and the third temperature sensor are respectively inserted into the reaction tube through three openings of the upper flange, and are respectively sleeved in the ceramic sleeve and are respectively inserted into catalyst pile layers with different depths;
the fourth temperature sensor, the fifth temperature sensor and the sixth temperature sensor are respectively and sequentially arranged on three independent hearths of the heating furnace from top to bottom;
the hydrogen detector is positioned on the outer side of the device;
the output end of the PLC processor is connected with the first electromagnetic valve, the first flow controller, the second electromagnetic valve, the second flow controller, the heating furnace, the vacuum pump and the touch screen.
Preferably, the aperture clearance range of the sand core is 10-30 μm, and the inner diameter range of the quartz tube is 30-160mm.
Preferably, O-shaped sealing rings and sealing gaskets are arranged between the upper flange and the quartz tube and between the lower flange and the quartz tube; the O-shaped sealing ring and the sealing washer are made of fluororubber or perfluororubber.
Preferably, the upper flange is provided with four openings, one of the openings is communicated with the output end of the mixing tank through an air inlet, and the other three openings can be respectively inserted into the temperature sensors;
the lower flange is provided with a gas outlet which is communicated with the tail gas treatment unit; the inner bottom surface of the lower flange is conical, and the gradient of the conical shape is less than 170 degrees.
Preferably, the heating furnace adopts three sections of hearths with independent temperature control, the length of a heating zone in the middle of the heating furnace is set to be 3-6 times of the height of a catalyst bed layer in the reaction tube, and the temperature range of the heating furnace is between room temperature and 1000 ℃.
Compared with the prior art, the beneficial effects of the utility model are that:
(1) The utility model discloses a vertical quartz material's reaction tube to with the catalyst tiling on the psammitolite in the reaction tube, reducing gas from last flange get into the reaction tube in the back, can fully contact with the catalytic substance, avoided the insufficient problem of catalyst reduction. Meanwhile, the reaction tube of the vertical structure and the sand core with the small hole in the inner part are arranged, so that the reduction products HCl and H2O can flow into the lower end of the reaction tube in time, the phenomenon that part of the catalyst cannot react with the reduction gas due to the fact that the reduction products are accumulated in the catalyst is avoided, and the problems of slow reduction speed and uneven reduction are solved.
(2) The utility model discloses a material lectotype of seal structure design, inner chamber surface spraying, contact atmosphere of jar in the upper flange of reaction tube, lower flange, blending tank and alkali lye neutralization tank has solved the problem of the corrosivity of reduction product.
(3) The utility model discloses a furnace that the heating furnace adopted the independent accuse temperature of three-section can reach longer constant temperature area, guarantees the temperature homogeneity of catalyst bed.
Drawings
Fig. 1 is a schematic connection diagram of an embodiment of the present invention;
fig. 2 is a schematic view of a reaction tube structure according to an embodiment of the present invention;
FIG. 3 is an enlarged view of a portion A of FIG. 2;
FIG. 4 is an enlarged view of part B of FIG. 2;
FIG. 5 is an enlarged view of portion C of FIG. 2;
FIG. 6 is an enlarged view of a portion D of FIG. 2;
fig. 7 is a top view of an upper flange of a reaction tube according to an embodiment of the present invention;
in the figure: 1. a reducing gas input unit; 11. a reducing gas pipe; 12. a first solenoid valve; 13. a first flow controller; 14. a first check valve; 2. a purging unit; 21. an inert gas pipe; 22. a second solenoid valve; 23. a second flow controller; 24. a second one-way valve; 3. a mixing tank; 4. a reaction tube; 41. a quartz tube; 42. an upper flange; 43. a lower flange; 44. a sand core; 45. clamping a hoop; 46. opening a hole; 47. a support; 48. an air outlet; 49. a sealing gasket; 410. an O-shaped sealing ring; 411. a sleeve; 5. heating furnace; 6. a tail gas treatment unit; 61. an alkali liquor neutralization tank; 62. an adsorption tank; 63. a vacuum pump; 7. a control system; 71. a first pressure gauge; 72. a first pressure sensor; 73. a second pressure gauge; 74. a second pressure sensor; 75. a first temperature sensor; 76. a second temperature sensor; 77. a third temperature sensor; 78. a fourth temperature sensor; 79. a fifth temperature sensor; 710. a sixth temperature sensor; 711. a hydrogen gas detector; 8. polytetrafluoroethylene.
Detailed Description
In order to facilitate the understanding of the technical solutions of the present invention by those skilled in the art, the technical solutions of the present invention will now be further described with reference to the drawings attached to the specification.
The terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, "a plurality" means two or more unless specifically limited otherwise.
Referring to fig. 1, the embodiment discloses a reduction treatment device for a carbon-supported platinum catalyst, which comprises a reducing gas input unit 1, a purging unit 2, a mixing tank 3, a reaction tube 4, a heating furnace 5 and a tail gas treatment unit 6;
the reducing gas input unit 1 includes a reducing gas pipe 11, a first electromagnetic valve 12, a first flow controller 13, and a first check valve 14; the input end of the reducing gas pipe 11 is communicated with the input end of the mixing tank 3 after passing through the first electromagnetic valve 12, the first flow controller 13 and the first check valve 14 in sequence. The reducing gas pipe 11 has pure hydrogen gas or a mixed gas containing hydrogen gas and an inert gas therein, the first electromagnetic valve 12 can control the communication or closing of the reducing gas pipe 11 and the mixing tank 3, the first flow controller 13 can control the flow rate therebetween, and the first check valve 14 can prevent the gas from flowing back into the reducing gas pipe 11 to contaminate the internal gas.
The purge unit 2 includes an inert gas pipe 21, a second electromagnetic valve 22, a second flow controller 23, and a second check valve 24; the input end of the inert gas pipe 21 is communicated with the input end of the mixing tank 3 after passing through the second electromagnetic valve 22, the second flow controller 23 and the second one-way valve 24 in sequence. The inert gas pipe 21 is provided with pure nitrogen or pure argon or a mixed gas of the two, the second electromagnetic valve 22 can control the connection or the disconnection of the inert gas pipe 21 and the mixing tank 3, the second flow controller 23 can control the flow between the two, and the second check valve 24 can prevent the gas from flowing back into the inert gas pipe 21 to pollute the internal gas.
Referring to fig. 2 to 7, the reaction tube 4 is a vertical structure including a quartz tube 41, an upper flange 42 and a lower flange 43; the upper flange 42 is arranged at the upper end of the quartz tube 41 and is fixed with the quartz tube 41 through the hoop 45, the lower flange 43 is arranged at the lower end of the quartz tube 41 and is fixed with the quartz tube 41 through the hoop 45, and the upper flange 42 and the lower flange 43 are fixed with the quartz tube 41 through the detachable hoop 45 structure, so that the disassembly is convenient.
The middle part of the quartz tube 41 is also provided with a sand core 44 for holding a catalyst. The sand core 44 of this embodiment has a pore size of 10 to 30 μm and the quartz tube 41 has an inner diameter of 30 to 160mm. When the reactor is used, the catalyst is poured into the upper part of the sand core 44 of the reaction tube 4, the pile layer is cylindrical in the reaction tube 4, and the pile layer is tightly attached to the inner wall of the reaction tube 4, so that the catalyst is fully reduced.
The upper flange 42 is provided with four openings 46, wherein one opening 46 is an air inlet and is used for being communicated with the output end of the mixing tank 3. Three other openings 46 may be inserted into the temperature sensors, respectively.
The lower flange 43 is provided with an air outlet 48, and the air outlet 48 is communicated with the tail gas treatment unit 6. The bottom surface of the interior of the lower flange 43 is tapered with a slope of less than 170 degrees, so that the reduction product after the catalyst reduction reaction can be collected and output from the gas outlet 48.
The bottom of the reaction tube 4 is also provided with a support 47 for supporting the reaction tube 4.
Meanwhile, in order to ensure the sealing performance inside the quartz tube 41, O-ring seals 410 and sealing gaskets 49 are arranged between the upper flange 42 and the quartz tube 41 and between the lower flange 43 and the quartz tube 41. The O-ring 410 and the gasket 49 are made of a fluorine rubber or a perfluoro rubber.
The quartz tube 41 of the embodiment has the characteristic of resisting corrosion of acid and alkali, and polytetrafluoroethylene 8 or modified materials thereof are sprayed on the inner cavity surfaces of the upper flange 42 and the lower flange 43, so that the upper flange 42 and the lower flange 43 can be ensured to be resistant to corrosion of acid and alkali. The overall apparatus of the reaction tube 4 can thus avoid the problem of corrosion of the equipment by the reduction products HCl and H2O of the chloroplatinic acid hydrate (cl6h2pt.xh2o), and the reaction can be carried out safely without frequent replacement of the equipment.
The heating furnace 5 is surrounded on the periphery of the reaction tube 4, the heating furnace 5 adopts three sections of hearths with independent temperature control, the three sections of independent temperature control can reach a longer constant temperature area, and the temperature uniformity of a catalyst bed layer is facilitated. The length of the heating zone in the middle of the heating furnace 5 is set to be 3-6 times of the height of the catalyst bed in the reaction tube 4. The heating and controlling temperature range of the heating furnace 5 is from room temperature to 1000 ℃.
The tail gas treatment unit 6 comprises an alkali liquor neutralization tank 61, an adsorption tank 62 and a vacuum pump 63; the input end of the alkali liquor neutralization tank 61 is communicated with the gas outlet 48 of the reaction tube 4, the output end is communicated with the input end of the adsorption tank 62, and the output end of the adsorption tank 62 is communicated with the atmosphere after passing through a vacuum pump 63 and is used for discharging tail gas.
The alkali liquor neutralizing tank 61 is made of 316L stainless steel, and the inner cavity surface of the alkali liquor neutralizing tank 61 is sprayed with polytetrafluoroethylene 8 or modified materials thereof, so that the alkali liquor neutralizing tank can resist corrosion of acid and alkali. The inside contains an alkaline solution for neutralizing HCl generated in the reaction tube 4.
The adsorption tank 62 is made of polycarbonate, quartz glass, or the like. An adsorbent is arranged in the adsorption tank 62, and the adsorbent of the quartz inside is active carbon or allochroic silica gel.
The vacuum pump 63 is a corrosion-resistant diaphragm pump, the vacuum degree limit is 200mbar, and the aeration rate is not lower than 120L/min.
It should be noted that the pipelines connecting the devices are made of polytetrafluoroethylene 8 or modified materials thereof, and can resist corrosion of acid and alkali.
The control system 7 comprises a PLC processor, a touch screen, a first pressure gauge 71, a first pressure sensor 72, a second pressure gauge 73, a second pressure sensor 74, a first temperature sensor 75, a second temperature sensor 76, a third temperature sensor 77, a fourth temperature sensor 78, a fifth temperature sensor 79, a sixth temperature sensor 710 and a hydrogen detector 711.
The PLC processor is respectively connected with the touch screen, the first pressure gauge 71, the second pressure gauge 73, the first pressure sensor 72, the second pressure sensor 74, the first temperature sensor 75, the second temperature sensor 76, the third temperature sensor 77, the fourth temperature sensor 78, the fifth temperature sensor 79, the sixth temperature sensor 710 and the hydrogen detector 711.
The first pressure gauge 71 and the first pressure sensor 72 are arranged on the pipeline between the mixing tank 3 and the reaction tube 4 and used for monitoring the pressure value at the upper flange 42; a second pressure gauge 73 and a second pressure sensor 74 are provided on the pipe between the canister 62 and the vacuum pump 63 for monitoring the pressure value at the lower flange 43. Since the gas flow is from the upper flange 42 through the dense stack to the lower flange 43, a pressure differential is created across the stack, and the pressure measurement from the first pressure sensor 72 is generally not lower than the pressure measurement from the second pressure sensor 74.
The first temperature sensor 75, the second temperature sensor 76 and the third temperature sensor 77 are installed in the reaction tube 4, inserted through the three openings 46 of the upper flange 42, respectively, and the first temperature sensor 75, the second temperature sensor 76 and the third temperature sensor 77 measure the temperature of the catalyst stack at different depths, respectively. Specifically, the first temperature sensor 75, the second temperature sensor 76, and the third temperature sensor 77 are all K-type thermocouples, and the outer surface is stainless steel 316L or hastelloy C-276. The thermocouple is placed in a ceramic sleeve 411, and the ceramic sleeve 411 is inserted into the stack to prevent the temperature sensor from contacting corrosive materials.
The fourth temperature sensor 78, the fifth temperature sensor 79 and the sixth temperature sensor 710 are sequentially and respectively installed on three independent hearths of the heating furnace 5 from top to bottom, and are used for monitoring the temperature of the heating furnace 5.
The hydrogen gas detector 711 is located above the device, and the hydrogen gas detector 711 is exposed to the air for detecting the concentration of hydrogen gas that may leak out, thereby confirming whether the device leaks.
The PLC processor is also connected with a first electromagnetic valve 12, a first flow controller 13, a second electromagnetic valve 22, a second flow controller 23, the heating furnace 5, a vacuum pump 63 and a touch screen.
The operation flow of the catalytic reduction apparatus of the present example is as follows:
s1, cleaning the inner wall and the sand core 44 in the reduction reaction tube 4 by using deionized water, and drying by using an oven to remove water molecules.
S2, pouring the catalyst into the upper part of the sand core 44 of the reaction tube 4, and enabling the pile layer to be cylindrical in the reaction tube 4, wherein the pile layer is required to be tightly attached to the inner wall of the reaction tube 4.
And S3, installing the upper flange 42 and the lower flange 43 at the top and the bottom of the reaction tube 4, and fixing a sealing gasket 49 and an O-shaped ring. The ceramic bushings 411 of the three thermocouples are vertically inserted into the reaction tube 4 from the nozzle of the upper flange 42 and immersed inside the bed, and then the thermocouples are put into the ceramic bushings 411 again.
And S4, opening an air inlet valve of the inert gas, allowing the inert gas to enter the reaction tube 4, purging the reaction tube 4 with the inert gas, and closing the air inlet valve of the inert gas after purging.
And S5, opening an air inlet valve of reducing gas, introducing the reducing gas into the reaction tube 4, and heating the heating furnace 5 to the temperature required by the reaction.
And S6, after the catalyst is reduced for a certain time at the temperature and the pressure, finishing the reaction, and closing an air inlet valve of the reducing gas after the temperature of the heating furnace 5 is reduced to be below 50 ℃. And (4) according to the step S4, performing inert gas purging again to discharge flammable and explosive reducing gas.
And S7, after the reaction is finished, opening the upper flange 42, taking out the catalyst bed layer to liquid, and carrying out liquid seal to prevent the influence of oxygen in the air on the catalyst.
In this embodiment, the vertical reaction tube 4 made of quartz is adopted, and the catalyst is laid on the sand core 44 in the reaction tube 4, so that the reducing gas can fully contact with the catalytic material after entering the reaction tube 4 from the upper flange 42, thereby avoiding the problem of insufficient reduction of the catalyst. Meanwhile, the reaction tube 4 with the vertical structure and the sand core 44 with the small holes arranged inside can enable the reduction products HCl and H2O to flow into the lower end of the reaction tube 4 in time, so that the problem that part of the reduction products are accumulated in the catalyst to cause that the catalyst cannot react with the reduction gas is solved, and the problems of slow reduction speed and uneven reduction are solved.
The problem of corrosivity of the reduction product is solved by spraying polytetrafluoroethylene 8 or modified materials thereof on the surfaces of the upper flange 42 of the reaction tube 4, the lower flange 43, the mixing tank 3 and the inner cavity of the alkali liquor neutralization tank 61.
The first temperature sensor 75, the second temperature sensor 76 and the third temperature sensor 77 monitor the temperatures of the catalyst at different depths and send data to the PLC processor, the fourth temperature sensor 78, the fifth temperature sensor 79 and the sixth temperature sensor 710 monitor the temperatures of three independent hearths of the heating furnace 5 and send data to the PLC processor, and the PLC controller can automatically adjust the temperature range of the catalyst during reduction reaction.
It is obvious to a person skilled in the art that the invention is not restricted to details of the above-described exemplary embodiments, but that it can be implemented in other specific forms without departing from the spirit or essential characteristics of the invention. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference signs in the claims are not intended to be construed as limiting the claim concerned.
The above embodiments only show the embodiments of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and for those skilled in the art, a plurality of modifications and improvements can be made without departing from the concept of the present invention, and these modifications and improvements all belong to the protection scope of the present invention.
Claims (10)
1. A reduction treatment apparatus for a carbon-supported platinum catalyst, characterized in that: comprises a reducing gas input unit (1), a purging unit (2), a mixing tank (3), a reaction tube (4), a heating furnace (5) and a tail gas treatment unit (6);
the reaction tube (4) is of a vertical structure and comprises a quartz tube (41), an upper flange (42) and a lower flange (43); the upper flange (42) is arranged at the upper end of the quartz tube (41), and the lower flange (43) is arranged at the lower end of the quartz tube (41); a sand core (44) for containing a catalyst stack layer is arranged in the quartz tube (41), and the sand core (44) is provided with a plurality of pores;
the reducing gas input unit (1) and the purging unit (2) are both communicated with the input end of the mixing tank (3), the output end of the mixing tank (3) is communicated with the upper flange (42) of the reaction pipe (4), and the lower flange (43) of the reaction pipe (4) is communicated with the tail gas treatment unit (6); the heating furnace (5) is surrounded on the periphery of the reaction tube (4).
2. The reduction treatment apparatus for a carbon-supported platinum catalyst according to claim 1, characterized in that: the reducing gas input unit (1) comprises a reducing gas pipe (11), a first electromagnetic valve (12), a first flow controller (13) and a first one-way valve (14);
the input end of the reducing gas pipe (11) is communicated with the input end of the mixing tank (3) through a pipeline, the first electromagnetic valve (12), the first flow controller (13) and the first one-way valve (14) are sequentially installed on the pipeline between the reducing gas pipe (11) and the mixing tank (3) respectively, and the flow direction of the first one-way valve (14) is from the reducing gas pipe (11) to the mixing tank (3).
3. The reduction treatment apparatus for a carbon-supported platinum catalyst according to claim 1, characterized in that: the purging unit (2) comprises an inert gas pipe (21), a second electromagnetic valve (22), a second flow controller (23) and a second one-way valve (24);
the input of inert gas pipe (21) passes through the input intercommunication of pipeline with blending tank (3), install respectively in proper order on the pipeline between reducing gas pipe (11) and blending tank (3) second solenoid valve (22), second flow controller (23) and second check valve (24), the circulation direction of second check valve (24) is from inert gas pipe (21) to blending tank (3).
4. The reduction treatment apparatus for a carbon-supported platinum catalyst according to claim 1, characterized in that: the tail gas treatment unit (6) comprises an alkali liquor neutralization tank (61), an adsorption tank (62) and a vacuum pump (63);
the input end of the alkali liquor neutralization tank (61) is communicated with the lower flange (43) of the reaction tube (4), the output end of the alkali liquor neutralization tank is communicated with the input end of the adsorption tank (62), and the output end of the adsorption tank (62) is communicated with the atmosphere after passing through a vacuum pump (63).
5. The reduction treatment apparatus for a carbon-supported platinum catalyst according to claim 4, characterized in that: the inner cavity surfaces of the upper flange (42), the lower flange (43), the mixing tank (3) and the alkali liquor neutralizing tank (61) are all sprayed with polytetrafluoroethylene (8).
6. The reduction treatment apparatus for a carbon-supported platinum catalyst according to claim 1, characterized in that: the hydrogen-gas hydrogen production system is characterized by further comprising a control system (7), wherein the control system (7) comprises a PLC (programmable logic controller) processor, a touch screen, a first pressure gauge (71), a second pressure gauge (73), a first pressure sensor (72), a second pressure sensor (74), a first temperature sensor (75), a second temperature sensor (76), a third temperature sensor (77), a fourth temperature sensor (78), a fifth temperature sensor (79), a sixth temperature sensor (710) and a hydrogen detector (711),
the input end of the PLC processor is respectively connected with the touch screen, the first pressure gauge (71), the second pressure gauge (73), the first pressure sensor (72), the second pressure sensor (74), the first temperature sensor (75), the second temperature sensor (76), the third temperature sensor (77), the fourth temperature sensor (78), the fifth temperature sensor (79), the sixth temperature sensor (710) and the hydrogen detector (711);
the first pressure gauge (71) and the first pressure sensor (72) are arranged on a pipeline between the mixing tank (3) and the reaction tube (4); the second pressure gauge (73) and the second pressure sensor (74) are arranged on a pipeline between the adsorption tank (62) and the vacuum pump (63);
the first temperature sensor (75), the second temperature sensor (76) and the third temperature sensor (77) are respectively inserted into the reaction tube (4) through three open holes (46) of the upper flange (42), and the first temperature sensor (75), the second temperature sensor (76) and the third temperature sensor (77) are respectively sleeved in a sleeve (411) made of ceramic materials and are respectively inserted into catalyst reactor layers with different depths;
the fourth temperature sensor (78), the fifth temperature sensor (79) and the sixth temperature sensor (710) are respectively and sequentially arranged on three independent hearths of the heating furnace (5) from top to bottom;
the hydrogen detector (711) is positioned outside the device;
the output end of the PLC processor is connected with the first electromagnetic valve (12), the first flow controller (13), the second electromagnetic valve (22), the second flow controller (23), the heating furnace (5), the vacuum pump (63) and the touch screen.
7. The reduction treatment apparatus for a platinum-on-carbon catalyst according to claim 1, characterized in that: the aperture clearance range of the sand core (44) is 10-30 mu m, and the inner diameter range of the quartz tube (41) is 30-160mm.
8. The reduction treatment apparatus for a platinum-on-carbon catalyst according to claim 1, characterized in that: o-shaped sealing rings (410) and sealing gaskets (49) are arranged between the upper flange (42) and the quartz tube (41) and between the lower flange (43) and the quartz tube; the O-shaped sealing ring (410) and the sealing ring (49) are made of fluororubber or perfluororubber.
9. The reduction treatment apparatus for a platinum-on-carbon catalyst according to claim 1, characterized in that: the upper flange (42) is provided with four openings (46), one opening (46) is communicated with the output end of the mixing tank (3) through an air inlet, and the other three openings (46) can be respectively inserted into a temperature sensor;
the lower flange (43) is provided with a gas outlet (48), and the gas outlet (48) is communicated with the tail gas treatment unit (6); the inner bottom surface of the lower flange (43) is conical, and the gradient of the conical shape is less than 170 degrees.
10. The reduction treatment apparatus for a carbon-supported platinum catalyst according to claim 1, characterized in that: the heating furnace (5) adopts three sections of hearths with independent temperature control, the length of a heating zone in the middle of the heating furnace (5) is set to be 3-6 times of the height of a catalyst bed in the reaction tube (4), and the temperature range of the heating furnace (5) is from room temperature to 1000 ℃.
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| CN115425241A (en) * | 2022-09-15 | 2022-12-02 | 安徽科幂仪器有限公司 | Reduction treatment device and method for carbon-supported platinum catalyst |
| CN115425241B (en) * | 2022-09-15 | 2024-06-04 | 安徽科幂仪器有限公司 | Reduction treatment device and method for carbon-supported platinum catalyst |
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