CN115557467A - System and method for hydrogen production reaction by using wastewater in coal grading manner - Google Patents
System and method for hydrogen production reaction by using wastewater in coal grading manner Download PDFInfo
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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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- C01B2203/12—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 coal grading utilization wastewater hydrogen production reaction system and a coal grading utilization wastewater hydrogen production reaction method, and belongs to the field of wastewater treatment and hydrogen production. The system mainly comprises a plate type reactor, an air inlet buffer tank and an air outlet buffer tank; the plate type reactor is an assembly of an end plate and an inner plate which are designed in a modular mode, the scale enlargement and assembly of the reactor can be easily realized, and a catalyst of the plate type reactor is easy to coat. The whole system is arranged in a waste heat boiler, feed gas enters a plate type reactor from an air inlet buffer tank to react, and gas enters an air outlet buffer tank after the reaction. The fins are arranged inside and outside the air inlet/outlet buffer tank cylinder, so that the technical problems that the dynamic pressure of inlet airflow influences the gas flow rate of the reaction chambers, the synchronous requirement of inlet and outlet gas of each reaction chamber is high, and the heat exchange of the gas in the buffer tank is slow are solved, the purposes of synchronous and stable control of the pressure of the inlet and outlet gas of each reaction chamber and rapid heat transfer of reactants are realized, and the problem of backflow of reaction products in the reaction chambers is solved.
Description
Technical Field
The invention belongs to the field of wastewater treatment and hydrogen production, and particularly relates to a system and a method for hydrogen production reaction by utilizing wastewater in a coal grading manner.
Background
Coal is an important basic energy and raw material, and the development of novel coal chemical technologies such as coal pyrolysis, coal gasification, coal-to-liquid, coal oil substitution and the like has great significance for the clean and efficient utilization of coal. However, in the coal grading utilization process, the waste water production and pollution discharge nodes are more, the waste water production amount is large, the pollutant types are more, the pollutant concentration is high, the toxicity of the waste water is high, the waste water is difficult to degrade biochemically, and the treatment difficulty is extremely high. With increasingly strict requirements on environmental protection, the zero discharge and recycling technology of coal graded utilization wastewater becomes an indispensable part of sustainable development of the modern coal chemical industry.
At present, relatively few researches on wastewater treatment technologies in the coal classification utilization industry are carried out, the coking wastewater treatment technology is mainly used, biochemical treatment is mainly used, and various biological oxidation degradation methods are used for decomposing organic matters into micromolecular substances. The process still has more problems at present, such as great dilution is needed for biochemical treatment, the concentration of the pollutants in the reuse water does not reach the standard, zero emission cannot be realized, the process flow is complex, the occupied area is large, the treatment cost is high, 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 organic matters with complex components such as phenol, naphthalene and the like which are difficult to treat in the coking wastewater cannot be treated. In order to solve the problem that the biochemical treatment cannot realize the standard discharge of the wastewater, CN101508498A discloses that the biochemically treated coking wastewater is deeply treated by adsorption and precipitation, suspended substances in the wastewater can be recovered as fuel, but the treated wastewater still cannot meet the national first-level discharge standard requirement and cannot realize the zero discharge of the wastewater.
In recent years, the research on the high-temperature catalytic reforming of organic pollutants and the high-temperature catalytic cracking of ammonia gas is rapidly developed, and the method provides the treatment of waste water by utilizing coal in a grading way mainly comprising the organic pollutantsA new technical route. A large number of experimental studies have shown that transition metal catalysts of single or multiple metals, such as TiO 2 、Ni/Co-ZrO 2 、NiO/TiO 2 /ZnTiO 3 、Ni/ash/γ-Al 2 O 3 And the hydrogen can be produced by efficiently converting organic pollutants and ammonia gas. 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 the literature that under the optimal reaction conditions, ni/ash/gamma-Al 2 O 3 The catalyst can obtain the conversion rate of organic matters up to 98.6 percent, and the highest hydrogen content in the produced gas reaches 83.8 percent.
In order to realize continuous, efficient and stable conversion of pollutants and further realize zero discharge of wastewater in coal graded utilization, a reaction system capable of large-scale industrial application is urgently needed.
Disclosure of Invention
In order to overcome the defects of the wastewater treatment technology in the existing coal grading utilization industry, the invention provides a system and a method for hydrogen production reaction by utilizing wastewater in coal grading.
The technical scheme of the invention is as follows:
the invention firstly provides a coal grading utilization wastewater hydrogen production reaction system, which comprises:
the plate type reactor comprises an upper end plate, a lower end plate and a plurality of inner plates which are arranged between the two end plates in parallel, wherein the inner plates divide an 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 respectively provided with a hydrogen production catalyst coating layer, 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 and are respectively connected with the air inlets of the reaction chambers through the vent pipes, and fins for heat exchange are arranged on the inner side and the outer side of the barrel body of the air inlet buffer tank; the fins on the inner side of the cylinder are also used for dissipating the kinetic energy of airflow and are circular ring fins;
the structure of the gas outlet buffer tank is the same as that of the gas inlet buffer tank, and the gas outlet buffer tank is connected with the gas outlets of the reaction chambers through vent pipes.
As the preferred scheme of the invention, 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 an air outlet which are used as an air outlet or an air inlet of the reaction chamber surrounded by the end plate.
As a preferable scheme of the invention, the structures of the plurality of inner plates are completely the same; the upper surface and the lower surface 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 inner concave part and the lower inner concave part of the inner plate; the air inlets and air outlets of the two upper and lower adjacent inner plates face opposite directions.
As a preferable scheme of the invention, the end plate and the inner plate of the plate type reactor are fastened by bolts to realize assembly; v-shaped grooves are correspondingly arranged on the mutual contact surfaces between the end plate and the inner plate and between the inner plate and the inner plate; graphite packing is placed in the V-shaped grooves, and the graphite packing has a sealing effect after the plate type reactor is assembled. Preferably, the V-shaped groove is arranged around the inner concave part, so that gas in the reaction chamber is prevented from leaking from the space 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 section.
The invention also provides a method for preparing hydrogen by utilizing waste water by coal classification, which comprises the following steps:
s1: the coal graded wastewater hydrogen production reaction system is arranged in a waste heat boiler, and the heat source of the waste heat boiler is high-temperature pyrolysis gas at 800-1000 ℃; the gas-state and liquid-state coal from the waste heat boiler is conveyed into the air inlet buffer tank by a pipeline in a grading manner, and the waste water absorbs heat in the conveying pipeline and the air inlet buffer tank and is completely gasified;
s2: the air inlet buffer tank dissipates the kinetic energy of gas through the fins in the cylinder body, so that the dynamic pressure of the pipe orifice of the vent pipe of the air inlet buffer tank is eliminated, and the pressure of the pipe orifice of each vent pipe is equal; gas enters each reaction chamber of the plate reactor and reacts on the surface of the hydrogen production catalyst coating layer;
s3: the reacted gas enters a gas outlet buffer tank; and the gas in the gas outlet buffer tank flows out of the coal graded utilization wastewater hydrogen production reaction system after heat exchange and temperature reduction to a target temperature.
Compared with the prior art, the invention has the beneficial effects that at least:
(1) The modular plate type reactor component is designed, the plate type reactor has a simple structure, only the components with two structures of the end plate and the inner plate are needed, the mass production can be conveniently carried out in the production process, and the assembly of a large number of reactors can be easily realized in the assembly process. The modular design ensures that the industrialized scale of the plate type reactor component can be linearly enlarged and the maintenance is rapid.
(2) The catalyst of the plate type reactor is easy to coat, the inner plate and the end plate are only provided with one screwed pipe, and the sharing of the air inlet and the air outlet is realized through matching, so that the number of the air inlet and the air outlet is obviously reduced, the connection points which are easy to happen are reduced, the reliability of the system is improved, and the workload of manufacturing and installing equipment is reduced. The method has the advantages of high conversion rate, quick reaction, overcoming the problems of large mass transfer distance, insufficient reaction, lower conversion rate, long maintenance time and large shutdown loss of the traditional reactor, obtaining the beneficial effects that the reaction system is easy to produce in mass and assemble in batches, can carry out linear amplification, is convenient to maintain and is suitable for large-scale industrial popularization and application.
(3) The invention designs the gas inlet/outlet buffer tank with fins inside and outside, overcomes the technical problems that the dynamic pressure of inlet gas flow affects the gas flow rate of the reaction chambers, the synchronous requirement of inlet and outlet gas 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 and outlet gas of each reaction chamber and the rapid heat transfer of reactants, and solves the problem of the backflow of reaction products in the reaction chambers.
Drawings
FIG. 1 is a schematic structural diagram of a reaction system for producing hydrogen by using wastewater in stages by using coal.
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 screw tube configuration.
Fig. 4 is a schematic view of the structure of the intake buffer tank.
FIG. 5 is an assembly view of the connection between the inlet buffer vessel and the plate reactor.
Fig. 6 is a schematic diagram of the ferrule structure in the embodiment.
FIG. 7 is a schematic diagram of a reaction system for producing hydrogen by using wastewater in stages by using coal according to an embodiment.
FIG. 8 is a schematic view of a reaction system for producing hydrogen by using wastewater in stages by coal according to comparative example 1.
FIG. 9 is a schematic view of a reaction system for producing hydrogen by using wastewater in stages by coal according to comparative example 2.
FIG. 10 is a schematic view of a reaction system for producing hydrogen by using wastewater in stages by coal according to comparative example 3.
In the figure, 1-an air inlet and an air outlet, 2-a V-shaped groove, 3-a bolt hole, 4-a hydrogen production catalyst coating layer, 5-an inner plate, 6-an end plate, 7-a graphite filler, 8-an air inlet buffer tank, 9-an inlet of the air inlet buffer tank, 10-a vent pipe, 11-a fin, 12-a threaded pipe, 13-a clamping sleeve, 14-a metal sealing ring, 15-an outlet of the air outlet buffer tank, 16-an air outlet buffer tank, 17-a concentrated waste liquid tank, 18-a concentrated waste liquid pump, 19-a gas detection valve and 20-a gas chromatograph.
Detailed Description
The invention will be further illustrated and described with reference to specific embodiments. The described embodiments are merely exemplary of the disclosure and are not intended to limit the scope thereof. The technical features of the embodiments of the present invention can be combined correspondingly without mutual conflict.
The reaction system for realizing the hydrogen production by coal grading and utilizing wastewater comprises a plate-type reactor, an air inlet buffer tank 8, an air outlet buffer tank 16, matched connecting and sealing equipment and the like, and is shown in figure 1. The composition and assembly method of the hydrogen production reaction system by using waste water in coal classification are described below.
The key equipment of the wastewater hydrogen production reaction system for coal grading utilization is a plate reactor. The plate type 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 surface and the bottom surface of each reaction chamber are provided with hydrogen production catalyst coating layers 4.
The inner plate 5 and the end plate 6 are both in modular design, the plate type reactor only needs components of two structures 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 and lower end plates 6 have the same structure, the end plate 6 has an inner concave portion, and the bottom surface of the inner concave portion is provided with a hydrogen production catalyst coating layer 4; the structures of the inner plates 5 are completely the same, the upper surface and the lower surface of each inner plate 5 are provided with inner concave parts, and the bottom surfaces of the inner concave parts are provided with hydrogen production catalyst coating layers 4. The plate reactor is constituted by two end plates 6 and a plurality of inner plates 5 which are rotated and overlapped.
As shown in fig. 1 and 2, the end plate of the present invention is disposed opposite to the inner plate and the inner recess between the inner plates up and down, thereby constituting a reaction chamber; the number of reaction chambers is determined by the number of inner plates. The number of reaction chambers can be linearly scaled up according to the wastewater treatment capacity.
The surface of the end plate 6 facing the inside of the plate reactor and the upper surface and the lower surface 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 the hydrogen production catalyst coating layer 4. The catalyst in the hydrogen production catalyst coating layer 4 is a catalyst for steam reforming reaction of organic matters and catalytic cracking reaction of ammonia gas. The catalyst is 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 hydrogen production by reforming 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 reaction that takes place on the surface of the catalyst coated on the plate reactor is:
and (3) phenol steam reforming reaction:
naphthalene steam reforming reaction:
ammonia high-temperature catalytic decomposition reaction:
water gas shift reaction:
methanation reaction:
a budoair 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 of coating the catalyst on the end plate or the inner plate is: thermal spraying of a layer of alpha-Al on the catalyst-coated area of the end plate or inner plate 2 O 3 Coating the nanoparticle matrix with alumina sol and calcining to form gamma-Al 2 O 3 (ii) a Dissolving a catalyst precursor, such as nickel nitrate hexahydrate, tetraisopropyl titanate, and the like, in deionized water under appropriate conditions, followed by stirring at 90 ℃ to remove a portion of the water and form a slurry of appropriate concentration; coating the slurry on a plate type reactor to form a layer of precursor mixture film, then placing the reactor in the air at 500-900 ℃ for roasting for 2-6 hours, and finally naturally cooling at room temperature to form a hydrogen production catalyst coating layer 4 attached to an end plate or an inner plate.
The contact surfaces between the end plate and the inner plate and between the inner plate and the inner plate are correspondingly provided with V-shaped grooves which surround the inner concave part and are used for filling high-temperature-resistant graphite filler 7. The high-temperature resistant graphite packing 7 can realize sealing between plate type reactor components at the temperature higher than 800 ℃. When assembling the plate reactor, according to the plate reactor configuration shown in fig. 1, the end plates 6 and the inner plates 5 are placed by rotation, overlapping, aligning the bolt holes 3 thereon, and the graphite packing 7 is placed in the "V" shaped groove 2 of each plate reactor assembly. Bolts are inserted into the bolt holes 3, the plate type reactor is gradually compacted through synchronous fastening of all groups of bolts and nuts, and at the moment, the graphite packing 7 deforms and completely fills the holes of the V-shaped grooves 2, so that the sealing effect among all plate type reactor components is achieved.
Each reaction chamber is provided with a gas inlet and a gas outlet; the air inlet and the air outlet of the reaction chamber are both positioned in an inner plate or an end plate which is enclosed into the reaction chamber, the air inlet on the inner plate or the end plate is hermetically connected with the air pipe 10 of the air inlet buffer tank 8, and the air outlet on the inner plate or the end plate is hermetically connected with the air 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 an air inlet buffer tank 8.
Because the equipment or system failure usually occurs at the equipment connection or interface, only one end of each end plate 6 is provided with an air inlet and outlet 1 which is used as an air outlet or an air inlet of the reaction chamber surrounded by the end plate; only one end of each inner plate 5 is provided with an air inlet and outlet 1 which is used as an air outlet or an air inlet of the reaction chamber surrounded by the inner plate, and the air inlet and outlet is communicated with the upper concave part and the lower concave part of the inner plate; the air inlets and air outlets 1 of two inner plates 5 adjacent to each other up and down are oppositely oriented. According to the invention, two adjacent reaction chambers separated by the inner plate reduce the number of interfaces by half through sharing the gas inlet and outlet 1, so that the workload in the production and installation processes is reduced, more importantly, the reliability of the plate type reactor system is improved, and the method is very important for improving the safety of the reaction system of which the product is high-concentration hydrogen. The plate type reactor has simple structure, thereby reducing the production difficulty, only two plate type reactor components are used, mass production can be conveniently carried out in the production process, the assembly of a large number of reactors can be easily realized in the assembly process, and errors are not easy to occur. The reactor component manufactured by the method has the advantages of modular equipment, is convenient and quick to overhaul and replace, and can be linearly amplified.
The inlet surge tank 8 and the outlet surge tank 16 of the present invention are identical. Taking the air intake buffer tank as an example, as shown in fig. 4, the air intake buffer tank is cylindrical, a plurality of vent pipes 10 are arranged on the side wall of the cylindrical, and are respectively connected with the air inlets of the reaction chambers through the vent pipes 10, fins 11 for heat exchange are arranged on the inner side and the outer side of the cylinder body of the air intake buffer tank 8, wherein the fins on the inner side of the cylinder body are circular fins and are also used for dissipating the kinetic energy of the air flow. The gas outlet buffer tank 16 is connected with the gas outlet of each reaction chamber through the vent pipe 10. Referring to fig. 1, an inlet 9 of the inlet buffer tank is arranged in the center of one end of the cylinder of the inlet buffer tank 8; an outlet 15 of the gas outlet buffer tank is arranged in the center of one end of the cylinder body of the gas 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 axis direction of the cylinder body.
The plate type reactor component is connected with the gas inlet/outlet buffer tank through the clamping sleeve threads, as shown in figures 3 and 5. The gas inlet and outlet 1 of the plate type reactor component extends outwards to form a threaded pipe 12 with external threads; the clamping sleeve 13 and the metal sealing ring 14 are sequentially placed on the breather pipe 10 of all the air inlet/outlet buffer tanks according to the structure shown in the figure, and then the breather pipe 10 is inserted into the threaded pipe 12 with the external thread of the plate type reactor component. The internal thread of the cutting sleeve 13 is matched with the external thread of the threaded pipe 12, and the outer part of the cutting sleeve is of an outer hexagonal structure as shown in figure 6. The ferrule 13 is screwed together with the plate reactor assembly, and the metal sealing ring 14 in the ferrule 13 can be deformed and the seal between the two connecting pipes can be realized by further fastening.
The pipe orifice pressure difference of the vent pipes 10 of the gas inlet buffer tank 8 and the gas outlet buffer tank 16 determines the gas flow speed of the reaction chambers in the plate reactor, so that the pressure difference between the vent pipe orifices of the gas inlet buffer tank and the gas outlet buffer tank connected with the reaction chamber cavities plays a decisive role in realizing the uniform distribution of gas flow of the reaction chambers. The total pressure at the mouth of the vent pipe is the sum of the static pressure and the dynamic pressure, the influence of gas gravity on the static pressure can be ignored for a storage tank filled with gas close to the normal pressure, that is, the static pressure at each position in the air inlet/outlet buffer tank is equal, but the dynamic pressure at the mouth 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 each vent pipe orifice. On the one hand, reaction system catalyst throughput is stronger, can realize the gaseous processing of great flow, and consequently the admission speed is very fast, and on the other hand, whole reaction system arranges the exhaust-heat boiler in, and the buffer tank that admits air and play gas buffer tank size are less, have strengthened the influence of the air current impact of admitting air to mouth of pipe dynamic pressure. In order to eliminate dynamic pressure, the invention solves the problem of air inflow impact by arranging the circular ring fin at the inner side of the cylinder body of the air inflow buffer tank 8. After the air flow enters the air inlet buffer tank 8, the air flow impacts each layer of fins 11 to form vortex, the kinetic energy of the air flow is dissipated in the vortex and is buffered before flowing to the mouth of the air pipe, and therefore the dynamic pressure of the mouth of the air pipe is reduced to a level far lower than the static pressure of the mouth of the air pipe. Meanwhile, fins on the inner side and the outer side of the cylinder wall of the air inlet buffer tank can remarkably strengthen heat transfer between the inner side and the outer side of the cylinder wall, the time required by the gas in the air inlet buffer tank to reach the target temperature can be remarkably shortened, and the heat of a reaction product in the air outlet buffer tank can be quickly transferred to boiler water of a waste heat boiler. To sum up, the main effect of the buffer tank that admits air and the buffer tank that outgases is:
1. the pressure difference of the inlet and the outlet of each reaction chamber is balanced, the gas distribution of each reaction chamber is realized, and the gas flow in each reaction chamber is regulated.
2. Eliminate the dynamic pressure at the mouth of the vent pipe.
3. The internal and external heat exchange 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 quickly transferred out of the reaction system.
As shown in figure 1, the method for producing hydrogen by using waste water in coal classification by applying the system mainly comprises the following steps:
s1: the coal graded wastewater hydrogen production reaction system is arranged in a waste heat boiler, and the heat source of the waste heat boiler is high-temperature pyrolysis gas at 800-1000 ℃; the gas and liquid coal from the waste heat boiler is conveyed into the air inlet buffer tank 8 by a pipeline in a grading manner, and the waste water absorbs heat in the conveying pipeline and the air inlet buffer tank 8 and is completely gasified;
s2: the air inlet buffer tank 8 dissipates the kinetic energy of the gas through the fins 11 in the cylinder body, so that the dynamic pressure of the pipe openings of the vent pipes 10 of the air inlet buffer tank 8 is eliminated, and the pressure of the pipe openings of the vent pipes 10 is equal; gas enters each reaction chamber of the plate reactor and reacts on the surface of the hydrogen production catalyst coating layer 4;
s3: the reacted gas enters an outlet buffer tank 16; high-temperature reaction products in the gas outlet buffer tank 16 and gases such as unreacted high-temperature water vapor flow out of the coal graded utilization wastewater hydrogen production reaction system after the temperature is reduced to a target temperature through heat exchange.
The temperature of the waste heat boiler is continuously and gradually reduced to 200-400 ℃ of a pyrolysis gas outlet from 800-1000 ℃ of the pyrolysis gas inlet, and the temperature difference between the inside and the outside of the wall of the gas inlet buffer tank 8 can be controlled by arranging the position of the gas inlet buffer tank 8, so that the heat transfer quantity and the temperature of the gas inside the gas inlet can be controlled. Similarly, the temperature of the reaction product and the water vapor in the effluent buffer tank 16 can be lowered to the target temperature by setting the position of the effluent buffer tank 16. The reaction assembly is placed in a region with the temperature of 600-900 ℃, and the activity of the catalyst is high at the temperature. The inlet buffer tank 8 is arranged at a position close to a pyrolysis gas inlet of the waste heat boiler, the temperature of the inlet buffer tank 8 is 800-1000 ℃, the heat exchange rate can be improved by increasing the temperature of the inlet buffer tank 8, and the heat exchange time is shortened. The gas outlet buffer tank 16 is arranged according to the required exhaust temperature, and is used for providing energy for the wastewater pretreatment system for coal classification utilization, and the gas outlet buffer tank 16 is usually arranged in an area with the temperature of 400-600 ℃.
The invention is further illustrated below with reference to several examples. The reaction system used in the example is shown in FIG. 7, and comprises 5 reaction chambers. The waste water of gas and liquid coal grading utilization is sent into the gas inlet buffer tank 8 from the concentrated waste liquid tank 17 through the concentrated waste liquid pump 18, and the gas at the outlet of the gas outlet buffer tank 16 is led out through the gas detection valve 19 and sent into the gas chromatograph 20 for detection.
In the 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 coating zone of a plate reactor assembly (end plate, inner plate) 2 O 3 Then coating aluminium 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 adding NH after full dissolution 4 Adjusting pH of OH solution to 10, slowly adding tetraisopropyl titanate, stirring to obtain uniform mixture, stirring at 90 deg.C, evaporating part of water, grinding into powder, calcining at 750 deg.C for 5 hr, and naturally cooling to room temperature. The catalyst obtained here was powdered TiO 2 /ZnTiO 3 The catalyst powder was added to an aqueous solution containing 10 wt% nickel nitrate, stirred at 90 ℃ and part of the water evaporated to form a slurry of appropriate concentration, porous gamma-Al in the catalyst coating zone of the plate reactor 2 O 3 Coating a uniform thin layer on a carrier substrate, drying at 120 ℃ for 12h to completely remove water seal, roasting at 500 ℃ for 3 h in a plate reactor, and naturally cooling to form 10% NiO/TiO 2 /ZnTiO 3 The plate reactor assembly of (1).
Example (b):
as shown in fig. 7, 2 end plates 6 and 4 inner plates 5 are selected to form a reactor assembly, and the reactor assembly has 5 reaction chambers, wherein the width of each reaction chamber is 10cm, the length of each reaction chamber is 50cm, each reaction chamber has 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 at intervals of 8cm along the axis direction on the inner side and the outer side of the cylinder body, the 8 groups of fins are arranged totally, wherein the fins on the inner side of the cylinder body are circular fins, and the inner circle of each fin is straightDiameter of 8cm, thickness of 3mm, total internal heat exchange area of 2111cm 2 The air inlet/outlet buffer tank is provided with 3 connecting pipes which are respectively connected with the air inlet/outlet pipes of the plate-type reactors through clamping sleeves. For the coal graded utilization wastewater, after primary treatment and wastewater concentration, the quality of the concentrated wastewater is shown in the following table:
the inlet buffer tank 8 and the plate reactor were placed in a constant temperature environment of 900 ℃ and before the test the system was evacuated to remove air from the dead volume and then injected into the system by means of an external concentrated waste liquid pump 18 at a flow rate of 375 mL/h with the addition of 3.75L/h of water vapor. The waste water injected into the system is gasified in the gas inlet buffer tank and heated to 800 ℃ and enters the reaction chamber of the plate reactor to react, and reaction products and unreacted substances are discharged to the gas outlet buffer tank 16. The gas outlet buffer tank 16 is placed in a constant temperature environment of 400 ℃. After all reaction product gas of the gas outlet buffer tank 16 flows out of the gas outlet buffer tank 16, the temperature is reduced to 60 ℃ through a cold trap of a normal-temperature circulating water bath, condensed water is removed, and the components and the flow of residual gas are tested, wherein the components and the concentration of reformed gas are shown in the following table:
the conversion of the wastewater contaminants was found to be 97.22% with a gas flow of 140L/h.
Comparative example 1:
as shown in fig. 8, 2 end plates 6 and 4 inner plates 5 are selected to form a reactor assembly, and there are 5 reaction chambers, each of which has a width of 10cm and a length of 50cm, and each chamber has 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 at intervals of 8cm along the axis direction on the outer side of the cylinder body, the 8 groups of fins are totally arranged, and the fins on the inner side of the cylinder body are slender plates and are arranged along the axis direction, so that the influence on the air flow speed and the dynamic pressure is small. The width of the fin is 7cm, the thickness is 3mm, and the length is 1m3 pieces of heat exchanger are uniformly distributed along the circumference, and the total internal heat exchange area is 2100cm 2 . The air inlet/outlet buffer tank is provided with 3 connecting pipes which are respectively connected with the air inlet/outlet pipes of the plate-type reactors through clamping sleeves. For the coal graded utilization wastewater, after primary treatment and wastewater concentration, the quality of the concentrated wastewater is shown in the following table:
the inlet surge tank and plate reactor assembly were placed in a constant temperature environment of 900 deg.C, the system was evacuated to remove air from the dead volume 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 with the addition of 3.75L/h of water vapor. The waste water injected into the system is gasified in the gas inlet buffer tank and heated to about 800 ℃ and enters the reaction chamber of the plate reactor to react, and reaction products and unreacted substances are discharged to the gas outlet buffer tank 16. The gas outlet buffer tank 16 is placed in a constant temperature environment of 400 ℃. After all reaction product gas of the gas outlet buffer tank 16 flows out of the gas outlet buffer tank 16, the temperature is reduced to 60 ℃ through a cold trap of a normal-temperature circulating water bath, condensed water is removed, and the components and the flow of residual gas are tested, wherein the components and the concentration of reformed gas are shown in the following table:
the conversion of the wastewater contaminants was found to be 77.29% with a gas flow of 111L/h.
Comparative example 2:
as shown in fig. 9, 2 end plates 6 and 4 inner plates 5 are selected to form a reactor assembly, and there are 5 reaction chambers in total, the chamber width is 10cm, the chamber length is 50cm, each chamber has 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, 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 pipe of each plate-type reactor through clamping sleeves. For the coal graded utilization wastewater, after primary treatment and wastewater concentration, the quality of the concentrated wastewater is shown in the following table:
the inlet surge tank and plate reactor package were placed in a 900 ℃ thermostatted environment and prior to testing the system was evacuated to remove air from the dead volume and then injected into the system by an external concentrate waste pump 18 at a rate of 375 mL/h with the addition of 3.75L/h of water vapor. The waste water injected into the system is gasified in the gas inlet buffer tank and heated to 600 ℃ and enters the reaction chamber of the plate reactor to react, and reaction products and unreacted substances are discharged to the gas outlet buffer tank 16. The gas outlet buffer tank 16 is placed in a constant temperature environment of 400 ℃. After all reaction product gas of the gas outlet buffer tank 16 flows out of the gas outlet buffer tank 16, the temperature is reduced to 60 ℃ through a cold trap of a normal-temperature circulating water bath, condensed water is removed, and the components and the flow of residual gas are tested, wherein the components and the concentration of reformed gas are shown in the following table:
the conversion of the wastewater contaminants was found to be 59.52% with a gas flow of 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 formed in total, the width of each chamber is 10cm, the length of each chamber is 50cm, each chamber is provided with 2 catalyst coating layers, 50g of catalyst is attached to each hydrogen production catalyst coating layer, 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 at intervals of 8cm along the axial direction on the inner side and the outer side of the cylinder body, 14 groups of fins are arranged, wherein the fins on the inner side of the cylinder body are circular 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 And 5 connecting pipes are arranged on the gas inlet/outlet buffer tank and are respectively connected with the gas inlet/outlet pipe of each plate-type reactor through a clamping sleeve. For the coal graded utilization wastewater, after primary treatment and wastewater concentration, the quality of the concentrated wastewater is shown in the following table:
the inlet surge tank and plate reactor assembly were placed in a constant temperature environment of 900 c, the system was evacuated to remove air from the dead volume prior to testing and then injected into the system by an external concentrated waste liquid pump 18 at a rate of 675 mL/h with the addition of 6.75L/h of water vapor. The waste water injected into the system is gasified in the gas inlet buffer tank and heated to 800 ℃ and enters the reaction chamber of the plate reactor to react, and reaction products and unreacted substances are discharged to the gas outlet buffer tank 16. The gas outlet buffer tank 16 is arranged in a constant temperature environment of 400 ℃. After all reaction product gas of the gas outlet buffer tank 16 flows out of the gas outlet buffer tank 16, the temperature is reduced to 60 ℃ through a cold trap of a normal-temperature circulating water bath, condensed water is removed, and the components and the flow of residual gas are tested, wherein the components and the concentration of reformed gas are shown in the following table:
the conversion rate of the wastewater pollutants is measured to be 97.00 percent, and the gas flow is 251L/h.
Compared with the comparative 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 circular 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 the comparative examples, 1 and 2, the influence of the fins of the air inlet buffer tank on the heat transfer enhancement effect is obvious, and the air inlet temperature enters the reaction chamber when the air inlet temperature is not raised to the required reaction temperature without the fins, so that the performance of the catalyst is seriously influenced. It can be seen from the comparison of example and comparative example 3 that when the waste liquid flow rate and the number of reaction chambers are increased in proportion, the conversion rate of the waste liquid does not fluctuate significantly, and the components and concentrations of the gaseous products do not fluctuate significantly, indicating that the system can be simply and linearly amplified by using the waste water amount according to the coal scenario.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as limiting the scope of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (10)
1. The utility model provides a coal utilizes waste water hydrogen manufacturing reaction system in grades which characterized in that includes:
the plate type reactor comprises an upper end plate, a lower end plate and a plurality of inner plates which are arranged between the two end plates in parallel, wherein the inner plates divide an 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 respectively provided with a hydrogen production catalyst coating layer, 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 and are respectively connected with the air inlets of the reaction chambers through the vent pipes, and fins for heat exchange are arranged on the inner side and the outer side of the cylinder body 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 airflow and are circular ring fins;
the structure of the gas outlet buffer tank is the same as that of the gas inlet buffer tank, and the gas outlet buffer tank is connected with the gas outlets of the reaction chambers through vent pipes.
2. The system for preparing hydrogen by using waste water in grades by coal as claimed in claim 1, wherein hydrogen production catalyst coating layers are respectively arranged on the surface of the end plate facing the inside of the plate reactor and the upper surface and the lower surface of the inner plate; 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.
3. The system for the hydrogen production reaction by using wastewater in coal classification as claimed in claim 2, wherein the preparation method of the hydrogen production catalyst coating layer comprises the following steps:
thermal spraying of a layer of alpha-Al on the catalyst-coated area of the end plate or inner plate 2 O 3 Coating the nanoparticle matrix with alumina sol and calcining to form gamma-Al 2 O 3 (ii) a Will be hastenedDissolving a precursor of the chemical agent in deionized water, and then stirring under heating to remove part of water and form slurry with proper concentration; 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 a hydrogen production catalyst coating layer attached to an end plate or an inner plate.
4. The system for the hydrogen production by utilizing the wastewater in the coal classification as claimed in claim 1, wherein the assembly is realized by fastening the end plate and the inner plate of the plate reactor through bolts; v-shaped grooves are correspondingly arranged on the mutual contact surfaces between the end plate and the inner plate and between the inner plate and the inner plate; graphite packing is placed in the V-shaped groove, and the graphite packing is sealed after the plate type reactor is assembled.
5. The system for the hydrogen production by utilizing the wastewater in the coal classification as claimed in claim 1, wherein the gas inlet and the gas outlet of the reaction chamber are both positioned in an inner plate or an end plate which is enclosed into the reaction chamber, the gas inlet on the inner plate or the end plate is hermetically connected with the vent pipe of the gas inlet buffer tank, and the gas outlet on the inner plate or the end plate is hermetically connected with the vent pipe of the gas outlet buffer tank.
6. The system for the hydrogen production by utilizing the wastewater in the coal classification as claimed in 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 an air outlet which are used as an air outlet or an air inlet of the reaction chamber surrounded by the end plate.
7. The system for the hydrogen production reaction by utilizing the waste water in the coal classification as claimed in claim 1, wherein the structures of the plurality of inner plates are completely the same; the upper surface and the lower surface 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 inner concave part and the lower inner concave part of the inner plate; the air inlets and air outlets of the two upper and lower adjacent inner plates face opposite directions.
8. The system for the hydrogen production by utilizing the wastewater in the grading manner by the coal as claimed in claim 1, wherein an inlet of the inlet buffer tank is arranged at the center of one end of the cylinder body of the inlet buffer tank; an outlet of the gas outlet buffer tank is arranged in the center of one end of the cylinder body of the gas 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.
9. A method for producing hydrogen by using wastewater in coal classification according to any one of claims 1 to 8, which is characterized by comprising the following steps:
s1: the coal graded wastewater hydrogen production reaction system is arranged in a waste heat boiler, and the heat source of the waste heat boiler is high-temperature pyrolysis gas at 800-1000 ℃; the gas and liquid coal from the waste heat boiler is conveyed into the air inlet buffer tank by a pipeline in a grading manner by utilizing waste water, and the waste water absorbs heat in the conveying pipeline and the air inlet buffer tank and is completely gasified;
s2: the air inlet buffer tank dissipates the kinetic energy of gas through the fins in the cylinder body, so that the dynamic pressure of the pipe orifice of the vent pipe of the air inlet buffer tank is eliminated, and the pressure of the pipe orifice of each vent pipe is equal; gas enters each reaction chamber of the plate reactor and reacts on the surface of the hydrogen production catalyst coating layer;
s3: the reacted gas enters a gas outlet buffer tank; and the gas in the gas outlet buffer tank flows out of the coal graded utilization wastewater hydrogen production reaction system after heat exchange and temperature reduction to a target temperature.
10. The method for preparing hydrogen by utilizing wastewater in stages by coal according to claim 9, characterized in that the temperature of the inlet buffer tank, the plate-type reactor and the outlet buffer tank is controlled by arranging the inlet buffer tank, the plate-type reactor and the outlet buffer tank 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 type reactor is 600-900 ℃; the temperature of the gas outlet buffer tank is 400-600 ℃.
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