CN115557467B - Hydrogen production reaction system and method by utilizing waste water in grading mode through coal - Google Patents
Hydrogen production reaction system and method by utilizing waste water in grading mode through coal Download PDFInfo
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- C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
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- C01B3/38—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts
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- C01B2203/0227—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step
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- C01B2203/12—Feeding the process for making hydrogen or synthesis gas
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- C01B2203/1288—Evaporation of one or more of the different feed components
Abstract
The invention provides a hydrogen production reaction system and method by utilizing waste water in a coal grading manner, belonging to the field of waste water treatment and hydrogen production. The system mainly comprises a plate reactor, an air inlet buffer tank and an air outlet buffer tank; the plate reactor is composed of components of an end plate and an inner plate which are in modularized design, the scale of the reactor can be easily enlarged and assembled, and the catalyst of the plate reactor is easy to coat. The whole system is arranged in the waste heat boiler, raw material gas enters the plate reactor from the gas inlet buffer tank to react, and the gas after the reaction enters the gas outlet buffer tank. Fins are arranged inside and outside the cylinder body of the air inlet/outlet buffer tank, so that the technical problems that the dynamic pressure of the air inlet air flow affects the air flow velocity of the reaction chamber, the synchronous requirement of the air inlet and outlet of each reaction chamber is high, and the heat exchange of the air in the buffer tank is slow are solved, the purposes of synchronous and stable control of the air inlet and outlet pressure of each reaction chamber and rapid heat transfer of reactants are realized, and the problem of backflow of reaction products in the reaction chamber is solved.
Description
Technical Field
The invention belongs to the field of wastewater treatment and hydrogen production, and particularly relates to a reaction system and a method for hydrogen production by using wastewater in a coal grading manner.
Background
The coal is an important basic energy source and raw material, and the development of novel coal chemical technologies such as coal pyrolysis, coal gasification, coal-to-oil, coal substitute oil and the like has great significance for clean and efficient utilization of the coal. However, in the coal classification and utilization process, wastewater production and pollution discharge nodes are more, the wastewater production amount is large, the types and the concentration of pollutants are more, the wastewater toxicity is high, the wastewater is difficult to biochemically degrade, and the treatment difficulty is extremely high. With the increasingly strict environmental protection requirements, the zero emission and recycling technology of the wastewater from the classified utilization of coal becomes an integral part of the sustainable development of the modern coal chemical industry.
At present, the research on wastewater treatment technology in the coal classification utilization industry is relatively less, the coking wastewater treatment technology is mainly used, biochemical treatment is mainly used, and various biological oxidative degradation methods are used for decomposing organic matters into small molecular substances. The technology still has more problems at present, such as large dilution required for biochemical treatment, substandard concentration of pollutants in recycled water, incapability of realizing zero emission, complex technological process, large occupied area, high treatment cost and the like. CN113754167a discloses a process for recovering ammonia from coking wastewater by stripping and adsorbing agent, wherein more than 90% of ammonia can be recovered by controlling pH, temperature and the like, but complex organic matters such as phenol, naphthalene and the like which are difficult to treat in the coking wastewater cannot be treated. Aiming at the problem that the biochemical treatment cannot realize the standard discharge of wastewater, CN101508498A discloses that coking wastewater subjected to the biochemical treatment is deeply treated through adsorption and precipitation, suspended matters in the wastewater can be recycled as fuel, but the treated wastewater still cannot meet the national first-level discharge standard requirement, and the zero discharge of wastewater cannot be realized.
In recent years, research on high-temperature catalytic reforming and high-temperature catalytic cracking of ammonia gas for organic pollutants has been developed rapidly, and a new technical route is provided for the fractional utilization of wastewater treatment of coal mainly containing organic pollutants. A number of experimental studies have shown that single-metal or multi-metal transition metal catalysts, such as TiO 2 、Ni/Co-ZrO 2 、NiO/TiO 2 /ZnTiO 3 、Ni/ash/γ-Al 2 O 3 And the like, can realize the efficient conversion of organic pollutants and ammonia gas to prepare hydrogen. The catalyst for preparing hydrogen by catalytically reforming organic pollutants has extremely high pollutant conversion rate and hydrogen yield under proper reaction conditions. It is reported in literature that Ni/ash/gamma-Al under optimal reaction conditions 2 O 3 The catalyst can obtain the conversion rate of organic matters up to 98.6%, and the hydrogen content in the produced gas is up to 83.8%.
In order to realize continuous, efficient and stable conversion of pollutants and further realize zero emission of wastewater for coal classified utilization, a reaction system capable of being applied to large-scale industrialization is needed.
Disclosure of Invention
The invention provides a hydrogen production reaction system and method by utilizing waste water in a coal grading manner, aiming at overcoming the defects in the waste water treatment technology in the existing coal grading utilization industry.
The technical scheme of the invention is as follows:
the invention firstly provides a reaction system for hydrogen production by using waste water in coal classification, which comprises:
the plate reactor comprises an upper end plate, a lower end plate and a plurality of inner plates which are arranged in parallel between the two end plates, wherein the inner plates divide the area between the two end plates into a plurality of mutually independent reaction chambers; the top surface and the bottom surface of each reaction chamber are provided with hydrogen production catalyst coating layers, and each reaction chamber is provided with an air inlet and an air outlet;
the air inlet buffer tank is cylindrical, a plurality of vent pipes are arranged on the cylindrical side wall, the vent pipes are respectively connected with the air inlets of the reaction chambers, and fins for heat exchange are arranged on the inner side and the outer side of the cylinder of the air inlet buffer tank; the fins on the inner side of the cylinder body are also used for dissipating the kinetic energy of air flow and are annular fins;
the structure of the air outlet buffer tank is the same as that of the air inlet buffer tank, and the air outlet buffer tank is respectively connected with the air outlets of the reaction chambers through the air pipes.
As the preferable scheme of the invention, the structures of the upper end plate and the lower end plate are identical, the end plates are provided with an inner concave part, and the bottom surface of the inner concave part is provided with a hydrogen production catalyst coating layer; only one end of each end plate is provided with an air inlet and outlet which is used as an air outlet or an air inlet of a reaction chamber enclosed by the end plate.
As a preferable scheme of the invention, the structures of the inner plates are identical; the upper and lower surfaces of each inner plate are provided with inner concave parts, the bottom surface of each inner concave part is provided with a hydrogen production catalyst coating layer, only one end of each inner plate is provided with an air inlet and outlet which is used as an air outlet or an air inlet of a reaction chamber enclosed by the inner plate, and the air inlet and outlet are communicated with the upper and lower inner concave parts of the inner plates; the air inlets and outlets of the two adjacent upper and lower inner plates are opposite in orientation.
As a preferable scheme of the invention, the end plate and the inner plate of the plate-type reactor are assembled through bolt fastening; v-shaped grooves are correspondingly formed on the mutual contact surfaces between the end plate and the inner plate and between the inner plate and the inner plate; graphite filler is placed in the V-shaped groove, and the graphite filler has a sealing effect after the plate reactor is assembled. Preferably, the V-shaped groove is arranged around the concave part, so that gas in the reaction chamber is prevented from leaking from between the end plate and the inner plate or between the two inner plates; the V-shaped groove is a groove with a V-shaped cross section.
The invention also provides a method for preparing hydrogen by using waste water in a coal grading way by using the system, which comprises the following steps:
s1: the hydrogen production reaction system by utilizing the waste water in a grading way is arranged in a waste heat boiler, and the heat source of the waste heat boiler is 800-1000 ℃ pyrolysis gas; the waste water from the waste heat boiler is conveyed into the air inlet buffer tank through a pipeline by grading the gas and liquid coal, and the waste water absorbs heat in the conveying pipeline and the air inlet buffer tank to be gasified completely;
s2: the air kinetic energy of the air is dissipated by the air inlet buffer tank through the fins in the cylinder body, so that the dynamic pressure of the mouth of the vent pipe of the air inlet buffer tank is eliminated, and the mouth pressure of each vent pipe is equal; the gas enters into each reaction chamber of the plate reactor and reacts on the surface of the hydrogen-making catalyst coating layer;
s3: the reacted gas enters an air outlet buffer tank; and the gas in the gas outlet buffer tank flows out of the reaction system for hydrogen production by classifying the coal and utilizing the wastewater after heat exchange and temperature reduction are carried out to reach the target temperature.
Compared with the prior art, the invention has the beneficial effects that at least the following steps are included:
(1) The modular plate-type reactor component is designed, the plate-type reactor is simple in structure, only components with two structures of the end plate and the inner plate are needed, mass production can be conveniently carried out in the production process, and assembly of a large number of reactors can be easily realized in the assembly process. The modular design enables the industrialized scale of the plate reactor assembly to be linearly amplified and the maintenance to be rapid.
(2) The catalyst of the plate reactor is easy to coat, the inner plate and the end plate are only provided with one threaded pipe, and the sharing of the air inlet and the air outlet is realized through cooperation, so that the number of the air inlet and the air outlet is obviously reduced, the connection points which are easy to occur accidents are reduced, the reliability of the system is improved, and the manufacturing and mounting workload of equipment is reduced. The method has the advantages of high conversion rate, rapid reaction, capability of overcoming the problems of large mass transfer distance, insufficient reaction, lower conversion rate, long maintenance time and large shutdown loss of the traditional reactor, capability of realizing the easy mass production and batch assembly of the reaction system, capability of linear amplification, convenience in maintenance and repair, and suitability for large-scale industrialized popularization and application.
(3) The invention designs the air inlet/outlet buffer tank with fins inside and outside, solves the technical problems that the dynamic pressure of the inlet air flow affects the flow speed of the gas in the reaction chamber, the synchronous requirement of the inlet air and the outlet air of each reaction chamber is high, and the heat exchange of the gas in the buffer tank is slow, realizes the synchronous and stable control of the pressure of the inlet air and the outlet air of each reaction chamber, and the purpose that the heat transfer of the reactant is rapid, and solves the problem of the backflow of the reaction products in the reaction chamber.
Drawings
FIG. 1 is a schematic diagram of a reaction system for producing hydrogen by classifying coal and utilizing waste water.
Fig. 2 is a schematic structural view of a plate reactor inner plate and a plate reactor end plate structure.
FIG. 3 is a schematic view of a plate reactor threaded tube structure.
Fig. 4 is a schematic view of the structure of the intake buffer tank.
Fig. 5 is an assembly view of the junction of the intake buffer tank and the plate reactor.
Fig. 6 is a schematic view of the ferrule structure in an embodiment.
FIG. 7 is a schematic diagram of a hydrogen production reaction system by utilizing wastewater in coal classification according to an embodiment.
Fig. 8 is a schematic diagram of a reaction system for producing hydrogen by classifying coal and utilizing wastewater according to comparative example 1.
FIG. 9 is a schematic diagram of a reaction system for producing hydrogen by classifying coal and utilizing wastewater according to comparative example 2.
FIG. 10 is a schematic diagram of a reaction system for producing hydrogen from wastewater by classifying coal according to comparative example 3.
In the figure, a 1-gas inlet and outlet, a 2-V-shaped groove, a 3-bolt hole, a 4-hydrogen production catalyst coating layer, a 5-inner plate, a 6-end plate, a 7-graphite filler, an 8-gas inlet buffer tank, a 9-gas inlet buffer tank inlet, a 10-vent pipe, 11-fins, a 12-threaded pipe, a 13-clamping sleeve, a 14-metal sealing ring, a 15-gas outlet buffer tank outlet, a 16-gas outlet buffer tank, a 17-concentrated waste liquid tank, a 18-concentrated waste liquid pump, a 19-gas detection valve and a 20-gas chromatograph.
Detailed Description
The invention is further illustrated and described below in connection with specific embodiments. The described embodiments are merely exemplary of the present disclosure and do not limit the scope. The technical features of the embodiments of the invention can be combined correspondingly on the premise of no mutual conflict.
The reaction system for realizing the hydrogen production by utilizing the wastewater in the coal classification comprises a plate reactor, an air inlet buffer tank 8, an air outlet buffer tank 16, matched connection and sealing equipment and the like, as shown in figure 1. The following describes the composition and assembly method of the hydrogen production reaction system by using waste water in a coal classification mode.
The key equipment of the hydrogen production reaction system by utilizing the waste water in the coal classification is a plate reactor. The plate reactor comprises an upper end plate 6, a lower end plate 6 and a plurality of inner plates 5 which are arranged between the two end plates 6 in parallel, wherein the inner plates 5 divide the area between the two end plates 6 into a plurality of mutually independent reaction chambers; the top and bottom surfaces of each reaction chamber are provided with a hydrogen production catalyst coating layer 4.
The inner plate 5 and the end plate 6 of the invention are both in modularized design, the plate-type reactor only needs components of the end plate and the inner plate, mass production can be conveniently carried out in the production process, and assembly of a large number of reactors can be easily realized in the assembly process. As shown in fig. 2, the upper end plate 6 and the lower end plate 6 have the same structure, the end plate 6 is provided with an inner concave part, and the bottom surface of the inner concave part is provided with a hydrogen production catalyst coating layer 4; the structures of the inner plates 5 are identical, the upper surface and the lower surface of each inner plate 5 are provided with concave parts, and the bottom surfaces of the concave parts are provided with hydrogen production catalyst coating layers 4. The plate reactor is composed of two end plates 6 and a plurality of inner plates 5 by rotation and overlapping.
As shown in fig. 1 and 2, the end plate, the inner plate and the concave part between the inner plates are arranged up and down oppositely, so that a reaction chamber is formed; the number of reaction chambers is determined by the number of inner plates. The number of reaction chambers can be linearly amplified according to the wastewater treatment capacity.
The surface of the end plate 6 facing the inside of the plate reactor and the upper and lower surfaces of the inner plate 5 are both provided with hydrogen production catalyst coating layers 4; so that the top and bottom surfaces of each reaction chamber are provided with a hydrogen-producing catalyst coating layer 4. The catalyst in the hydrogen production catalyst coating layer 4 is a catalyst for steam reforming reaction of organic matter and catalytic cracking reaction of ammonia gas. Such catalysts are mainly TiO 2 、Ni/Co-ZrO 2 、NiO/TiO 2 /ZnTiO 3 、Ni/ash/γAl 2 O 3 The transition metal catalyst of single metal or multiple metals can realize the reforming hydrogen production of organic matters such as tar, phenol, naphthalene, benzene and the like at 450-900 ℃, and the conversion rate under the optimal reaction condition is more than 98%.
The chemical reactions that occur on the coated catalyst surface on the plate reactor are:
phenol steam reforming reaction:
naphthalene steam reforming reaction:
high-temperature catalytic decomposition reaction of ammonia:
water gas shift reaction:
methanation reaction:
budoal reaction:
the hydrogen production catalyst coating layer 4 of the present invention is generally prepared by a coprecipitation method plus an impregnation method. The method for coating the catalyst on the end plate or the inner plate comprises the following steps: thermally spraying a layer of alpha-Al on the catalyst coating area of the end plate or the inner plate 2 O 3 Nanoparticle matrix, coated with aluminum sol and calcined to gamma-Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Dissolving a catalyst precursor such as nickel nitrate hexahydrate, tetraisopropyl titanate and the like in deionized water under proper conditions, and then stirring at 90 ℃ to remove part of water and form a slurry with proper concentration; coating the slurry on a plate reactor to form a layer of precursor mixture film, then placing the reactor in air at 500-900 ℃ for roasting for 2-6 hours, and finally naturally cooling at room temperature to form the hydrogen production catalyst coating layer 4 attached on the end plate or the inner plate.
V-shaped grooves are correspondingly formed on the mutual contact surfaces between the end plate and the inner plate and between the inner plate and the inner plate, and surround the concave part and are used for filling high-temperature-resistant graphite filler 7. The high temperature resistant graphite packing 7 can achieve sealing between the plate reactor components above 800 ℃. When the plate reactor is assembled, according to the plate reactor structure shown in fig. 1, an end plate 6 and an inner plate 5 are placed in a rotating and overlapping manner, the bolt holes 3 on the end plate and the inner plate are aligned, and graphite packing 7 is placed in a V-shaped groove 2 of each plate reactor component. Bolts are inserted into the bolt holes 3, and the plate reactors are gradually compacted through synchronous fastening of the bolt nuts of each group, so that the graphite packing 7 deforms and completely fills the holes of the V-shaped grooves 2, and the sealing effect among the plate reactor components is achieved.
Each reaction chamber is provided with an air inlet and an air outlet; the air inlet and the air outlet of the reaction chamber are positioned in an inner plate or an end plate which encloses the reaction chamber, the air inlet on the inner plate or the end plate is in sealing connection with the vent pipe 10 of the air inlet buffer tank 8, and the air outlet on the inner plate or the end plate is in sealing connection with the vent pipe 10 of the air outlet buffer tank 16. Each reaction chamber has an air inlet and an air outlet, and the flow rate of the gas in the reaction chamber is automatically distributed by the air inlet buffer tank 8.
Because equipment or system faults usually occur at the joints or interfaces of the equipment, only one air inlet and outlet port 1 is arranged at one end of each end plate 6 and is used as an air outlet port or an air inlet port of a reaction chamber enclosed by the air inlet port 1; only one end of each inner plate 5 is provided with an air inlet and outlet port 1 which is used as an air outlet or an air inlet of a reaction chamber enclosed by the inner plate, and the air inlet and outlet port is communicated with the upper concave part and the lower concave part of the inner plate; the air inlets and outlets 1 of the two upper and lower adjacent inner plates 5 are opposite in orientation. According to the invention, the number of the interfaces of two adjacent reaction chambers separated by the inner plate is reduced by half through the shared air inlet and outlet 1, so that the workload in the production and installation process is reduced, and more importantly, the reliability of the plate reactor system is improved, and the safety of the reaction system with high-concentration hydrogen as a product is very important. The plate-type reactor has a simple structure, so that the production difficulty is reduced, the plate-type reactor components are only two, mass production can be conveniently realized in the production process, and the assembly of a large number of reactors can be easily realized in the assembly process and is not easy to make mistakes. The reactor assembly manufactured by the method has the advantages of modularized equipment, is convenient and quick to overhaul and replace, and can be linearly amplified.
The intake buffer tank 8 and the exhaust buffer tank 16 of the present invention are identical. Taking an air inlet buffer tank as an example, as shown in fig. 4, the air inlet buffer tank is cylindrical, a plurality of ventilation pipes 10 are arranged on the side wall of the cylindrical shape, the air inlet buffer tank is respectively connected with the air inlets of the reaction chambers through the ventilation pipes 10, fins 11 for heat exchange are arranged on the inner side and the outer side of the cylinder of the air inlet buffer tank 8, wherein the inner side fins of the cylinder are annular fins, and the annular fins are also used for dissipating the kinetic energy of air flow. The air outlet buffer tanks 16 are connected with the air outlets of the reaction chambers through the air pipes 10, respectively. Referring to fig. 1, an inlet 9 of the air intake buffer tank is arranged at the center of one end of the cylinder of the air intake buffer tank 8; an air outlet buffer tank outlet 15 is arranged in the center of one end of the cylinder body of the air outlet buffer tank 16; the heat exchange fins on the inner side and the outer side of the cylinder body of the air inlet buffer tank and the air outlet buffer tank are arranged along the axial direction of the cylinder body.
The plate reactor assembly is screwed to the inlet/outlet buffer tank by means of a ferrule, as shown in fig. 3 and 5. The air inlet and outlet 1 of the plate reactor assembly is outwardly extended with a threaded pipe 12 with external threads; the ferrule 13 and the metal sealing ring 14 are placed in the illustrated configuration in sequence with the vent tube 10 of all the inlet/outlet buffer tanks, and then the vent tube 10 is inserted into the externally threaded tube 12 of the plate reactor assembly. The internal thread of the cutting sleeve 13 is matched with the external thread of the threaded pipe 12, and the outside of the cutting sleeve is of an external hexagonal structure, as shown in fig. 6. The clamping sleeve 13 is screwed with the plate reactor component through threads, and the metal sealing ring 14 in the clamping sleeve 13 can be deformed and sealing between two connecting pipes can be realized through further fastening.
The difference between the pipe orifices of the vent pipe 10 of the air inlet buffer tank 8 and the air outlet buffer tank 16 determines the gas flow rate of the reaction chamber in the plate reactor, so that the control of the difference between the pipe orifices of the air inlet buffer tank and the air outlet buffer tank connected with the chambers of each reaction chamber plays a decisive role in realizing the uniform distribution of the gas flow of each reaction chamber. The total pressure of the orifice of the vent pipe is the sum of static pressure and dynamic pressure, and the influence of gravity of gas on the static pressure can be ignored for a storage tank filled with gas close to normal pressure, so that the static pressure of each part in the air inlet/outlet buffer tank can be considered to be equal, but the dynamic pressure of the orifice of each vent pipe is different due to the air inlet flow. The gas distribution of each reaction chamber of the reaction system depends on the dynamic pressure of the orifice of each vent pipe. On one hand, the catalyst treatment capacity of the reaction system is higher, and the treatment of the gas with larger flow can be realized, so that the gas inlet speed is higher, and on the other hand, the whole reaction system is arranged in a waste heat boiler, the sizes of the gas inlet buffer tank and the gas outlet buffer tank are smaller, and the influence of the gas inlet airflow impact on the nozzle dynamic pressure is enhanced. In order to eliminate dynamic pressure, the invention solves the problem of inlet air flow impact by arranging the annular fins on the inner side of the cylinder body of the inlet buffer tank 8. After the air flow enters the air inlet buffer tank 8, the air flow impacts the fins 11 of each layer and forms vortex flow, the kinetic energy of the air flow is dissipated in the vortex flow, and the air flow is buffered before flowing to the orifice of the air pipe, so that the dynamic pressure of the orifice of the air pipe is reduced to a level far lower than the static pressure of the orifice of the air pipe. Meanwhile, the fins on the inner side and the outer side of the cylinder wall of the air inlet buffer tank can obviously strengthen heat transfer inside and outside the cylinder wall, the time required for the gas in the air inlet buffer tank to reach the target temperature can be obviously shortened, and the heat of reaction products in the air outlet buffer tank can also be quickly transferred into boiler water of a waste heat boiler. In summary, the main functions of the air inlet buffer tank and the air outlet buffer tank are as follows:
1. and balancing the inlet and outlet pressure differences of each reaction chamber, realizing the gas distribution of each reaction chamber, and regulating the gas flow in each reaction chamber.
2. Eliminating the dynamic pressure of the orifice of the vent pipe.
3. The heat exchange between the inside and the outside of the air inlet/outlet buffer tank is enhanced, the proper reaction temperature and reaction heat are provided for the catalytic reaction, and the heat of the product is rapidly transferred out of the reaction system.
As shown in FIG. 1, the method for producing hydrogen by using waste water through coal classification by using the system disclosed by the invention mainly comprises the following steps:
s1: the hydrogen production reaction system by utilizing the waste water in a grading way is arranged in a waste heat boiler, and the heat source of the waste heat boiler is 800-1000 ℃ pyrolysis gas; the waste water from the waste heat boiler is transported into the air inlet buffer tank 8 through a pipeline by grading the gas and liquid coal, and the waste water absorbs heat in the transportation pipeline and the air inlet buffer tank 8 for complete gasification;
s2: the air kinetic energy of the air is dissipated by the air inlet buffer tank 8 through the fins 11 in the cylinder body, so that the dynamic pressure of the pipe orifice of the air pipe 10 of the air inlet buffer tank 8 is eliminated, and the pipe orifice pressure of each air pipe 10 is equal; the gas enters into each reaction chamber of the plate reactor and reacts on the surface of the hydrogen-making catalyst coating layer 4;
s3: the reacted gas enters an air outlet buffer tank 16; the high-temperature reaction products and unreacted high-temperature steam and other gases in the gas outlet buffer tank 16 flow out of the coal grading utilization wastewater hydrogen production reaction system after heat exchange and temperature reduction to the target temperature.
The temperature of the waste heat boiler continuously and gradually drops from 800-1000 ℃ of the pyrolysis gas inlet to 200-400 ℃ of the pyrolysis gas outlet, and the difference between the inner temperature and the outer temperature of the wall of the air inlet buffer tank 8 can be controlled by arranging the air inlet buffer tank 8, so that the heat transfer quantity and the temperature of the internal gas can be controlled. Similarly, by positioning the vent buffer tank 16, the reaction product and water vapor temperatures within the vent buffer tank 16 may be reduced to target temperatures. The reaction assembly should be placed in a region with a temperature of 600-900 ℃ at which the catalyst activity is strong. The inlet buffer tank 8 is arranged at a position close to the pyrolysis gas inlet of the waste heat boiler, the temperature of the inlet buffer tank is 800-1000 ℃, the heat exchange rate can be improved by improving the temperature of the inlet buffer tank 8, and the heat exchange time is shortened. The effluent buffer tank 16 should be placed according to the desired exhaust temperature to power the coal staged wastewater pretreatment system, typically the effluent buffer tank 16 is placed in a zone at a temperature of 400-600 ℃.
The invention is further illustrated below in connection with several embodiments. The reaction system used in the examples is shown in FIG. 7 and comprises 5 reaction chambers. The waste water from the gas and liquid coal classification is fed into the gas inlet buffer tank 8 from the concentrated waste liquid tank 17 through the concentrated waste liquid pump 18, and the gas from the outlet of the gas outlet buffer tank 16 is led out through the gas detection valve 19 and fed into the gas chromatograph 20 for detection.
In examples and comparative examples, the hydrogen production catalyst coating layer 4 was prepared by exactly the same method as follows: thermal spraying of alpha-Al in the catalyst-coated zone of a plate reactor assembly (end plates, inner plates) 2 O 3 Then coating aluminum sol and roasting to make its surface produce porous gamma-Al 2 O 3 A carrier matrix. Dissolving nickel nitrate hexahydrate in deionized water, and after the nickel nitrate hexahydrate is fully dissolved, using NH 4 Adjusting the pH of the solution to 10 with OH, slowly adding tetraisopropyl titanate, stirring thoroughly to form a homogeneous mixture, stirring the mixture at 90deg.C, and evaporating thoroughlyAnd grinding part of the water into powder, roasting at 750 ℃ for 5 hours, and naturally cooling to room temperature. The catalyst obtained at this time was powdered TiO 2 /ZnTiO 3 Adding the catalyst powder into an aqueous solution containing 10 wt% nickel nitrate, stirring at 90deg.C and evaporating part of the water to form a slurry of suitable concentration, and porous gamma-Al in the catalyst coating zone of the plate reactor 2 O 3 The carrier substrate is coated with a uniform thin layer, the carrier substrate is firstly dried for 12 hours at 120 ℃ to completely remove water seal, then the plate reactor is baked for 3 hours at 500 ℃, and then the 10 percent NiO/TiO can be formed by natural cooling 2 /ZnTiO 3 Is provided.
Examples:
as shown in fig. 7, a reactor assembly is formed by selecting 2 end plates 6 and 4 inner plates 5, wherein the total number of the reaction chambers is 5, the width of each chamber is 10cm, the length of each chamber is 50cm, each chamber is provided with 2 catalyst coating layers, each hydrogen production catalyst coating layer is attached with about 50g of catalyst, and the total catalyst coating amount is about 500g. The diameter of the air inlet/outlet buffer tank is 20cm, the height of the air inlet/outlet buffer tank is 1m, a group of fins are arranged on the inner side and the outer side of the cylinder body at intervals of 8cm along the axial direction, 8 groups of fins are arranged in total, wherein the fins on the inner side of the cylinder body are annular fins, the diameter of the inner circle of each fin is 8cm, the thickness of each fin is 3mm, and the total internal heat exchange area is 2111cm 2 The air inlet/outlet buffer tanks are provided with 3 connecting pipes which are respectively connected with the air inlet/outlet pipes of the plate reactors through cutting sleeves. For the coal classified utilization wastewater, after preliminary treatment and wastewater concentration, the concentrated wastewater quality is shown in the following table:
the intake buffer tank 8 and the plate reactor were placed in a constant temperature environment of 900 c, and the system was evacuated to discharge the air in the dead volume before the test, and then injected into the system at a flow rate of 375 mL/h by the external concentrated waste liquid pump 18 while adding 3.75L/h of water vapor. The wastewater injected into the system is gasified in the air inlet buffer tank to be heated to 800 ℃ and enters the reaction chamber of the plate reactor to react, and the reaction products and unreacted substances are discharged to the air outlet buffer tank 16. The effluent buffer tank 16 is placed in a constant temperature environment at 400 ℃. All reaction product gases of the effluent buffer tank 16 flow out of the effluent buffer tank 16, then are cooled to 60 ℃ through a cold trap of a normal-temperature circulating water bath, condensed water is removed, the components and the flow of residual gases are tested, and the components and the concentration of reformed gases are shown in the following table:
the wastewater contaminant conversion was found to be 97.22% and the gas flow was found to be 140L/h.
Comparative example 1:
as shown in fig. 8, a reactor assembly is formed by selecting 2 end plates 6 and 4 inner plates 5, and the total of the reaction chambers is 5, the chambers are 10cm wide and 50cm long, each chamber is provided with 2 catalyst coating layers, each hydrogen production catalyst coating layer is attached with about 50g of catalyst, and the total catalyst coating amount is about 500g. The diameter of the air inlet/outlet buffer tank is 20cm, the height of the air inlet/outlet buffer tank is 1m, a group of fins are arranged on the outer side of the cylinder body at intervals of 8cm along the axial direction, 8 groups of fins are arranged in total, the fins on the inner side of the cylinder body are slender plates, and the fins are arranged along the axial direction, so that the influence on the air flow speed and dynamic pressure is small. The fin has a width of 7cm, a thickness of 3mm and a length of 1m, 3 fins are uniformly distributed along the circumference, and the total internal heat exchange area is 2100cm 2 . The air inlet/outlet buffer tanks are provided with 3 connecting pipes which are respectively connected with the air inlet/outlet pipes of the plate reactors through cutting sleeves. For the coal classified utilization wastewater, after preliminary treatment and wastewater concentration, the concentrated wastewater quality is shown in the following table:
the intake buffer tank and plate reactor assembly was placed in a constant temperature environment at 900 c, the system was evacuated to vent the dead volume of air prior to testing, and then injected into the system via an external concentrated waste liquid pump 18 at a flow rate of 375 mL/h while adding 3.75L/h of water vapor. The wastewater injected into the system is gasified in the inlet buffer tank to a temperature of about 800 ℃ and enters the reaction chamber of the plate reactor to react, and the reaction products and unreacted materials are discharged to the outlet buffer tank 16. The effluent buffer tank 16 is placed in a constant temperature environment at 400 ℃. All reaction product gases of the effluent buffer tank 16 flow out of the effluent buffer tank 16, then are cooled to 60 ℃ through a cold trap of a normal-temperature circulating water bath, condensed water is removed, the components and the flow of residual gases are tested, and the components and the concentration of reformed gases are shown in the following table:
the wastewater contaminant conversion was measured to be 77.29% and the gas flow was 111L/h.
Comparative example 2:
as shown in fig. 9, a reactor assembly is formed by selecting 2 end plates 6 and 4 inner plates 5, wherein the total number of the reaction chambers is 5, the width of each chamber is 10cm, the length of each chamber is 50cm, each chamber is provided with 2 catalyst coating layers, each hydrogen production catalyst coating layer is attached with about 50g of catalyst, and the total catalyst coating amount is about 500g. The diameter of the air inlet/outlet buffer tank is 20cm, the height is 1m, fins are not arranged on the inner side and the outer side of the cylinder body, 3 connecting pipes are arranged on the air inlet/outlet buffer tank and are respectively connected with the air inlet/outlet pipes of each plate-type reactor through cutting sleeves. For the coal classified utilization wastewater, after preliminary treatment and wastewater concentration, the concentrated wastewater quality is shown in the following table:
the intake buffer tank and plate reactor assembly was placed in a constant temperature environment at 900 c, the system was evacuated to vent the dead volume of air prior to testing, and then injected into the system via an external concentrated waste liquid pump 18 at a flow rate of 375 mL/h while adding 3.75L/h of water vapor. The wastewater injected into the system is gasified in the air inlet buffer tank to be heated to 600 ℃ and enters the reaction chamber of the plate reactor to react, and the reaction products and unreacted substances are discharged to the air outlet buffer tank 16. The effluent buffer tank 16 is placed in a constant temperature environment at 400 ℃. All reaction product gases of the effluent buffer tank 16 flow out of the effluent buffer tank 16, then are cooled to 60 ℃ through a cold trap of a normal-temperature circulating water bath, condensed water is removed, the components and the flow of residual gases are tested, and the components and the concentration of reformed gases are shown in the following table:
the wastewater contaminant conversion was measured to be 59.52% and the gas flow was 86L/h.
Comparative example 3:
the reaction system is shown in FIG. 10. 2 end plates 6 and 8 inner plates 5 are selected to form a reactor assembly, 9 reaction chambers are provided, the chambers are 10cm wide and 50cm long, each chamber is provided with 2 catalyst coating layers, each hydrogen production catalyst coating layer is attached with about 50g of catalyst, and the total catalyst coating amount is about 900g. The diameter of the air inlet/outlet buffer tank is 26cm, the height of the air inlet/outlet buffer tank is 1.7m, a group of fins are arranged on the inner side and the outer side of the cylinder body at intervals of 8cm along the axial direction, 14 groups of fins are arranged in total, wherein the fins on the inner side of the cylinder body are annular fins, the diameter of the inner circle of each fin is 10.4cm, the thickness of each fin is 3mm, and the total heat exchange area is 6243cm 2 The air inlet/outlet buffer tanks are provided with 5 connecting pipes which are respectively connected with the air inlet/outlet pipes of the plate reactors through cutting sleeves. For the coal classified utilization wastewater, after preliminary treatment and wastewater concentration, the concentrated wastewater quality is shown in the following table:
the intake buffer tank and plate reactor assembly was placed in a constant temperature environment at 900 c, the system was evacuated to remove air from the dead volume prior to testing, and then the system was injected with an external concentrated waste liquid pump 18 at a flow rate of 675 mL/h while adding 6.75L/h of water vapor. The wastewater injected into the system is gasified in the air inlet buffer tank to be heated to 800 ℃ and enters the reaction chamber of the plate reactor to react, and the reaction products and unreacted substances are discharged to the air outlet buffer tank 16. The effluent buffer tank 16 is placed in a constant temperature environment at 400 ℃. All reaction product gases of the effluent buffer tank 16 flow out of the effluent buffer tank 16, then are cooled to 60 ℃ through a cold trap of a normal-temperature circulating water bath, condensed water is removed, the components and the flow of residual gases are tested, and the components and the concentration of reformed gases are shown in the following table:
the wastewater contaminant conversion was found to be 97.00% and the gas flow was found to be 251L/h.
As can be seen from the comparison example and the comparison example 1, the arrangement mode of the fins on the inner side of the air inlet buffer tank 8 obviously influences the conversion rate of pollutants, and the annular fins can improve the air inlet distribution of the reaction chamber, so that the conversion performance of the system is improved. As can be seen from comparative examples, comparative example 1 and comparative example 2, the fin of the inlet buffer tank has a significant effect on the heat transfer enhancement effect, and the inlet air temperature is not increased to the desired reaction temperature without the fin, i.e., the inlet air enters the reaction chamber, thereby seriously affecting the performance of the catalyst. The comparison example and the comparison example 3 show that when the flow rate of the waste liquid and the number of the reaction chambers are increased in proportion, the conversion rate of the waste liquid does not obviously fluctuate, the components and the concentration of the gas product do not obviously fluctuate, and the system can be used for carrying out simple linear amplification by utilizing the water quantity of the waste water according to the coal plot.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit of the invention.
Claims (7)
1. A reaction system for producing hydrogen by classifying coal and utilizing waste water, which is characterized by comprising:
the plate reactor comprises an upper end plate, a lower end plate and a plurality of inner plates which are arranged in parallel between the two end plates, wherein the inner plates divide the area between the two end plates into a plurality of mutually independent reaction chambers; the top surface and the bottom surface of each reaction chamber are provided with hydrogen production catalyst coating layers, and each reaction chamber is provided with an air inlet and an air outlet; the structures of the inner plates are identical; the upper and lower surfaces of each inner plate are provided with inner concave parts, the bottom surface of each inner concave part is provided with a hydrogen production catalyst coating layer, only one end of each inner plate is provided with an air inlet and outlet which is used as an air outlet or an air inlet of a reaction chamber enclosed by the inner plate, and the air inlet and outlet are communicated with the upper and lower inner concave parts of the inner plates; the directions of the air inlets and the air outlets of the two adjacent inner plates are opposite;
the air inlet buffer tank is cylindrical, a plurality of vent pipes are arranged on the cylindrical side wall, the vent pipes are respectively connected with the air inlets of the reaction chambers, and fins for heat exchange are arranged on the inner side and the outer side of the cylinder of the air inlet buffer tank; the fins on the inner side of the cylinder body are also used for dissipating the kinetic energy of air flow and are annular fins;
the structure of the air outlet buffer tank is the same as that of the air inlet buffer tank, and the air outlet buffer tank is respectively connected with the air outlets of the reaction chambers through air pipes;
the air inlet and the air outlet of the reaction chamber are both positioned in an inner plate or an end plate which encloses the reaction chamber, the air inlet on the inner plate or the end plate is in sealing connection with a vent pipe of the air inlet buffer tank, and the air outlet on the inner plate or the end plate is in sealing connection with the vent pipe of the air outlet buffer tank;
an inlet buffer tank inlet is formed in the center of one end of the cylinder body of the inlet buffer tank; an outlet of the air outlet buffer tank is arranged at the center of one end of the cylinder body of the air outlet buffer tank; the fins on the inner side and the outer side of the cylinder body of the air inlet buffer tank and the air outlet buffer tank are arranged along the axial direction of the cylinder body.
2. The reaction system for hydrogen production by utilizing waste water in a coal classification manner according to claim 1, wherein the surface of the end plate facing the inside of the plate-type reactor and the upper and lower surfaces of the inner plate are provided with hydrogen production catalyst coating layers; the catalyst in the hydrogen production catalyst coating layer is a catalyst for steam reforming reaction of organic matters and catalytic cracking reaction of ammonia gas.
3. The reaction system for hydrogen production by using waste water in a coal classification as claimed in claim 2, wherein the preparation method of the hydrogen production catalyst coating layer comprises the following steps:
thermally spraying a layer of alpha-Al on the catalyst coating area of the end plate or the inner plate 2 O 3 Nanoparticle matrix, coated with aluminum sol and calcined to gamma-Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Dissolving the catalyst precursor in deionized water, and then stirring under heating to remove part of water and form slurry with proper concentration; and (3) coating the slurry on a catalyst coating area to form a layer of precursor mixture film, then placing the precursor mixture film in air at 500-900 ℃ for roasting for 2-6 hours, and finally naturally cooling at room temperature to form the hydrogen production catalyst coating layer attached on the end plate or the inner plate.
4. The reaction system for hydrogen production by utilizing waste water in coal classification according to claim 1, wherein the end plate and the inner plate of the plate reactor are assembled by fastening bolts; v-shaped grooves are correspondingly formed on the mutual contact surfaces between the end plate and the inner plate and between the inner plate and the inner plate; graphite filler is placed in the V-shaped groove, and the graphite filler is sealed after the plate reactor is assembled.
5. The reaction system for producing hydrogen by utilizing waste water in a coal grading manner according to claim 1, wherein the upper end plate and the lower end plate have the same structure, the end plates are provided with an inner concave part, and the bottom surface of the inner concave part is provided with a hydrogen production catalyst coating layer; only one end of each end plate is provided with an air inlet and outlet which is used as an air outlet or an air inlet of a reaction chamber enclosed by the end plate.
6. A method of producing hydrogen from waste water by coal staged application as claimed in any one of claims 1 to 5, comprising the steps of:
s1: the hydrogen production reaction system by utilizing the waste water in a grading way is arranged in a waste heat boiler, and the heat source of the waste heat boiler is 800-1000 ℃ pyrolysis gas; the waste water from the waste heat boiler is conveyed into the air inlet buffer tank through a pipeline by grading the gas and liquid coal, and the waste water absorbs heat in the conveying pipeline and the air inlet buffer tank to be gasified completely;
s2: the air kinetic energy of the air is dissipated by the air inlet buffer tank through the fins in the cylinder body, so that the dynamic pressure of the mouth of the vent pipe of the air inlet buffer tank is eliminated, and the mouth pressure of each vent pipe is equal; the gas enters into each reaction chamber of the plate reactor and reacts on the surface of the hydrogen-making catalyst coating layer;
s3: the reacted gas enters an air outlet buffer tank; and the gas in the gas outlet buffer tank flows out of the reaction system for hydrogen production by classifying the coal and utilizing the wastewater after heat exchange and temperature reduction are carried out to reach the target temperature.
7. The method for producing hydrogen by using waste water in a classified manner according to claim 5, wherein the temperature of the inlet buffer tank, the plate reactor and the outlet buffer tank is controlled by arranging them at different positions in the waste heat boiler; the temperature of the air inlet buffer tank is 800-1000 ℃, and the temperature of the plate reactor is 600-900 ℃; the temperature of the air outlet buffer tank is 400-600 ℃.
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| CN116216641B (en) * | 2023-05-06 | 2023-08-11 | 浙江百能科技有限公司 | System and method for preparing hydrogen by using waste water in grading manner through high-temperature catalytic coal |
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