CN114719185A - Hydrogen slurry reaction device and hydrogen storage and discharge method - Google Patents
Hydrogen slurry reaction device and hydrogen storage and discharge method Download PDFInfo
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- CN114719185A CN114719185A CN202210334601.0A CN202210334601A CN114719185A CN 114719185 A CN114719185 A CN 114719185A CN 202210334601 A CN202210334601 A CN 202210334601A CN 114719185 A CN114719185 A CN 114719185A
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- 150000002431 hydrogen Chemical class 0.000 claims abstract description 33
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000001471 micro-filtration Methods 0.000 claims abstract description 12
- 230000008859 change Effects 0.000 claims abstract description 10
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Images
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C11/00—Use of gas-solvents or gas-sorbents in vessels
- F17C11/005—Use of gas-solvents or gas-sorbents in vessels for hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
- C01B3/0078—Composite solid storage mediums, i.e. coherent or loose mixtures of different solid constituents, chemically or structurally heterogeneous solid masses, coated solids or solids having a chemically modified surface region
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C13/00—Details of vessels or of the filling or discharging of vessels
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C13/00—Details of vessels or of the filling or discharging of vessels
- F17C13/04—Arrangement or mounting of valves
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C5/00—Methods or apparatus for filling containers with liquefied, solidified, or compressed gases under pressures
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C7/00—Methods or apparatus for discharging liquefied, solidified, or compressed gases from pressure vessels, not covered by another subclass
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2205/00—Vessel construction, in particular mounting arrangements, attachments or identifications means
- F17C2205/03—Fluid connections, filters, valves, closure means or other attachments
- F17C2205/0302—Fittings, valves, filters, or components in connection with the gas storage device
- F17C2205/0323—Valves
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2221/00—Handled fluid, in particular type of fluid
- F17C2221/01—Pure fluids
- F17C2221/012—Hydrogen
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2250/00—Accessories; Control means; Indicating, measuring or monitoring of parameters
- F17C2250/03—Control means
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Hydrogen, Water And Hydrids (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The embodiment of the invention provides a hydrogen slurry reaction device and a hydrogen storage and discharge method, wherein the reaction device comprises: the device comprises a first body, a second body, a heating component and a microfiltration component, wherein the hydrogen storage material circulates in the first body and the second body to perform hydrogen storage reaction and hydrogen discharge reaction. The invention absorbs and releases hydrogen by coupling of the liquid organic material and the solid alloy powder, simultaneously utilizes the solid alloy powder as a catalyst for hydrogen storage reaction and hydrogen release reaction of the liquid organic material, utilizes the liquid organic material as a dispersion carrier of the solid alloy powder, and can adjust the mass ratio of the liquid organic material and the solid alloy powder and the flow of the liquid organic material according to the change of the particle size distribution of the solid alloy powder by considering the pulverization influence of the solid alloy powder, thereby adjusting the operation parameters, increasing the contact area of hydrogen and the hydrogen storage material, realizing the optimization of operation and achieving the optimal airspeed and reaction efficiency.
Description
Technical Field
The invention relates to the technical field of hydrogen energy storage and discharge, in particular to a hydrogen slurry reaction device and a hydrogen storage and discharge method.
Background
In hydrogen energy application, the storage and release of hydrogen as required are important problems influencing the safety and cost of hydrogen, how to store hydrogen becomes a popular research direction, the most widely applied gaseous hydrogen storage at present has the problems of poor safety and low hydrogen storage density, and in large-scale hydrogen energy storage application, the storage tank has explosion risk and the storage tank with an ultra-large volume can cause great increase of occupied area and management cost; and the hydrogen gas is not released thoroughly by the hydrogen gas storage tank, so that certain hydrogen gas allowance loss is caused, and the release speed is slowed down due to the reduction of the residual pressure of the gas cylinder in the later stage of the hydrogen release process.
In the existing research, organic liquid and solid alloy are used as hydrogen storage materials, wherein although the solid alloy or the organic liquid and the like are used as the hydrogen storage materials to realize large-scale and long-period storage of hydrogen and can be stored at normal temperature and normal pressure, and the safety is high, the organic liquid hydrogen storage not only faces the problems of poor hydrogen absorption and desorption dynamic performance and high temperature requirement, but also has small contact area with the hydrogen and low hydrogen storage efficiency. When solid alloy is used for storing hydrogen, although gaps are formed among the solid alloys, the solid alloys have larger contact area of hydrogen compared with organic liquid hydrogen storage, but the contact area of the solid alloys and the hydrogen storage efficiency are gradually reduced along with pulverization of the solid alloys within 100 reaction periods of work, namely pulverization from 50-100 micrometers of average particle size to about 1 micrometer. Therefore, how to provide a hydrogen slurry reaction device to achieve the storage and release of hydrogen gas as required and achieve the optimal space velocity and reaction efficiency is a technical problem to be solved urgently by those skilled in the art.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art.
Therefore, the invention aims to provide a hydrogen slurry reaction device, wherein a hydrogen storage material circularly performs hydrogen storage reaction and hydrogen discharge reaction in a first body and a second body, the hydrogen is absorbed and discharged through coupling of a liquid organic material and solid alloy powder, the solid alloy powder is used as a catalyst for the hydrogen storage reaction and the hydrogen discharge reaction of the liquid organic material, the liquid organic material is used as a dispersing carrier of the solid alloy powder, and the mass ratio of the liquid organic material to the solid alloy powder and the flow of the liquid organic material can be adjusted according to the change of the particle size distribution of the solid alloy powder in consideration of the pulverization influence of the solid alloy powder, so that the operating parameters are adjusted, the contact area of hydrogen and the hydrogen storage material is increased, the optimization of operation is realized, and the optimal space velocity and the reaction efficiency are achieved.
In order to achieve the above object, an embodiment of the present invention provides a hydrogen slurry reaction apparatus, including:
a first body comprising a volume of hydrogen storage material therein;
a second body having an input end connected with an output end of the hydrogen storage material of the first body and an output end connected with an input end of the hydrogen storage material of the first body; the hydrogen storage material is circulated in the first body and the second body;
a heating unit that heat-treats the first body and the second body, respectively; and
a microfiltration component; the input end of the hydrogen storage material is connected with the output end of the second body, the output end of the hydrogen storage material is connected with the input end of the hydrogen storage material of the first body, and the hydrogen storage material is used for screening and filtering the circulating hydrogen storage material.
In some embodiments, a hydrogen inlet and a first hydrogen outlet are arranged in a height direction of the first body in an opposite manner; and a second hydrogen outlet is formed in the second body.
In some embodiments, the reaction device further comprises a plurality of sampling windows dispersed on the connecting line of the first body and the second body.
In some embodiments, the hydrogen storage material comprises a liquid organic material and a solid alloy powder in a mass ratio of 5-10: 1; wherein the liquid organic material is an aromatic liquid organic material; the solid alloy powder is rare earth AB5At least one of a type alloy, a zirconium-based alloy, a titanium-based alloy, a vanadium-based alloy, and a magnesium-based alloy.
In some embodiments, the first body further comprises a first charging port and a second charging port; the first filling port is used for inputting the liquid organic material into the first body; the second charging port is used for inputting the solid alloy powder into the first body.
In some embodiments, the first body and the second body are both provided with a sewage draining outlet, and the sewage draining outlet is used for draining the used hydrogen storage material.
An embodiment according to the present invention also provides a hydrogen storage control method, including the steps of:
assembling a reaction apparatus as described in any of the above embodiments;
introducing a certain flow of liquid organic material and solid alloy powder into the first body until the liquid organic material and the solid alloy powder stably circulate in the first body and the second body;
heating the first body and the second body and then introducing hydrogen with certain pressure into the first body;
periodically monitoring the particle size of the solid alloy powder, and adjusting the mass ratio of the liquid organic material to the solid alloy powder and the flow rate of the liquid organic material according to the change of the particle size of the solid alloy powder.
In some embodiments, the initial volumetric flow rate Q of the liquid organic material0＝V*TOF；
Wherein Q0The unit is L/min; v is the sum of the volumes of the first body and the second body, and the unit is L; TOF is the space velocity of hydrogen storage reaction and hydrogen discharge reaction of the liquid organic material and the solid alloy powder, and the unit is min-1；
TOF＝k*ml/mg；
Wherein k is a rate constant of hydrogen storage reaction and hydrogen discharge reaction of the liquid organic material and the solid alloy powder in min-1；mlIs the mass of the liquid organic material in kg; m isgIs the mass of the solid alloy powder in kg.
In some embodiments, the method of adjusting the mass ratio of liquid organic material to the solid alloy powder according to the change in particle size of the solid alloy powder comprises:
when the particle diameter d of the solid alloy powdermAnd its primary particle size d0In a ratio of 1: when the particle diameter is 20-50, the particle diameter is d0The solid alloy powder has an alternative particle diameter dmThe solid alloy powder of (2) has a particle diameter of dmThe mass of the solid alloy powder is taken as a reference, and the mass percentage of the replaced solid alloy powder is 20-80%;
obtaining a relation of the particle size of the solid alloy powder in the newly formed hydrogen storage material-space velocity-flow of the liquid organic material;
TOFregulating device＝f(d)；
Wherein TOFRegulating deviceSpace velocity in min for hydrogen storage and hydrogen discharge for the newly formed hydrogen storage material-1(ii) a Q ═ f (d), Q being the volume flow rate of the liquid organic material, in units of L/min;
Qregulating device＝V*TOFRegulating device＝V*f(d)
Wherein QRegulating deviceThe volume flow of the liquid organic material after adjustment is in L/min; TOFRegulating deviceFor newly forming said hydrogen storage materialThe space velocity of hydrogen storage reaction and hydrogen discharge reaction is in min-1(ii) a V is the sum of the volumes of the first body and the second body, and the unit is L.
In some embodiments, Q is definedRegulating device>2Q0When the temperature of the water is higher than the set temperature,
wherein QRegulating deviceIs the regulated volume flow of the liquid organic material; q0Is the initial volumetric flow rate of the liquid organic material; m islIs the initial mass of the liquid organic material; m isgIs the initial mass of the solid alloy powder; m isl. toneThe mass of the liquid organic material adjusted according to the particle size of the solid alloy powder; m is a unit ofg tiao (a Chinese character of 'g')The quality of the solid alloy powder is adjusted according to the particle size of the solid alloy powder.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
fig. 1 is a schematic structural diagram of a hydrogen slurry reaction apparatus according to an embodiment of the present invention.
FIG. 2 is a schematic structural diagram of a hydrogen slurry reactor according to still another embodiment of the present invention.
FIG. 3 is a schematic structural diagram of a hydrogen slurry reactor according to another embodiment of the present invention.
FIG. 4 is a schematic structural diagram of a hydrogen slurry reactor according to still another embodiment of the present invention.
Fig. 5 is a flowchart of a hydrogen storage control method of a hydrogen slurry reactor according to an embodiment of the present invention.
Reference numerals:
a reaction apparatus 100;
a first body 1; a hydrogen inlet 11; a first hydrogen outlet 12; a first charge inlet 13; a second charge inlet 14; a sewage discharge port 15;
a second body 2; a second hydrogen outlet 21; a valve 22;
a heating assembly 3;
a microfiltration component 4;
a sampling window 5.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to examples. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other technical solutions obtained by a person skilled in the art based on the embodiments of the present invention belong to the protection scope of the present invention.
Specifically, as shown in fig. 1 to 5, the present invention is directed to a hydrogen slurry reactor 100, in which a hydrogen storage material circulates in a first body 1 and a second body 2 to perform a hydrogen storage reaction and a hydrogen discharge reaction, hydrogen is absorbed and discharged by coupling a liquid organic material and a solid alloy powder, and considering the pulverization effect of the solid alloy powder, the mass ratio of the liquid organic material to the solid alloy powder and the flow rate of the liquid organic material can be adjusted according to the change of the particle size distribution of the solid alloy powder, the contact area between hydrogen and the hydrogen storage material is increased, the optimization of operation is achieved, and the optimal space velocity and reaction efficiency are achieved.
To achieve the above object, as shown in fig. 1, an embodiment of the present invention provides a hydrogen slurry reaction apparatus 100, including: a first body 1, a second body 2, a heating assembly 3 and a microfiltration assembly 4; wherein, a certain volume of hydrogen storage material is filled in the first body 1, and the output end of the hydrogen storage material of the first body 1 is connected with the input end of the hydrogen storage material of the second body 2; the output end of the hydrogen storage material of the second body 2 is connected with the input end of the hydrogen storage material of the first body 1; the hydrogen storage material may circulate within the first body 1 and the second body 2. The hydrogen storage material is a slurry having fluidity and capable of circulating in the first body 1 and the second body 2, and the hydrogen slurry reaction apparatus 100 in this embodiment further includes a pump device capable of delivering the hydrogen storage material to smoothly circulate in the first body 1 and the second body 2. In the embodiment, the hydrogen storage material circulates in the first body 1 and the second body 2, so that the contact surface between the hydrogen and the hydrogen storage material is further increased, and the proceeding degree of the hydrogen storage reaction and the hydrogen discharge reaction is improved.
The heating assembly 3 in this embodiment can heat the first body 1 and the second body 2, and those skilled in the art can understand that hydrogen storage reaction and hydrogen desorption reaction using hydrogen storage materials need to be performed at a certain temperature and pressure, and the heating assembly 3 in this embodiment can be a heating jacket, a heating pipe, or other devices with heating function and controllable temperature, and can heat the first body 1 and the second body 2 to provide suitable temperature and pressure for the hydrogen storage materials circulating in the first body 1 and the second body 2, so as to perform hydrogen storage reaction or hydrogen desorption reaction.
The microfiltration component 4 is used for sieving and filtering the circulating hydrogen storage material, the input end of the hydrogen storage material is connected with the output end of the hydrogen storage material of the second body 2, and the output end of the hydrogen storage material of the first body 1. Understandably, the inside micro-filtration net that sets up of microfiltration subassembly 4 can sieve the hydrogen storage material and go out unqualified hydrogen storage material screening, prevents that unqualified hydrogen storage material from continuing at first body 1 and second body 2 inner loop, and then influences hydrogen storage reaction and the reaction efficiency of putting hydrogen.
It should be noted that in this embodiment, the first body 1, the second body 2 and the microfiltration component 4 are all provided with a valve 22 on the pipeline, and as shown in fig. 2 in particular, the valve 22 is provided to facilitate flow control and sampling.
In some embodiments, a hydrogen inlet 11 and a first hydrogen outlet 12 are formed in the first body 1 in a height direction; the second body 2 is provided with a second hydrogen outlet 21.
It is easy to understand that the present embodiment is described by taking as an example that the height direction of the first body 1 coincides with the up-down direction, which is shown in fig. 1.
Specifically, as shown in fig. 1, a first hydrogen outlet 12 for releasing hydrogen is formed above the first body 1, and a hydrogen inlet 11 for allowing hydrogen to enter is formed below the first body 1. Understandably, a certain volume of hydrogen storage material can be accommodated in the first body 1, hydrogen is introduced from the hydrogen inlet 11 of the first body 1, the pressure of the introduced hydrogen is controlled by the compressor and the valve 22, the heating assembly 3 is utilized to enable the first body 1 and the second body 2 to reach a certain temperature, and then hydrogen storage reaction can be carried out, and the hydrogen storage material is circulated in the first body 1 and the second body 2, so that the contact surface between the hydrogen and the hydrogen storage material is further increased, and the hydrogen storage reaction efficiency is improved; similarly, the second body 2 in this embodiment is provided with a second hydrogen outlet 21, and if a hydrogen discharge reaction occurs, only the corresponding temperature and pressure need to be changed, and the hydrogen released by the hydrogen storage material is collected through the first hydrogen outlet 12 and the second hydrogen outlet 21.
In some embodiments, the hydrogen storage material comprises a liquid organic material and a solid alloy powder in a mass ratio of 5-10: 1; wherein the liquid organic material is an aromatic liquid organic material; the solid alloy powder is rare-earth AB5At least one of a type alloy, a zirconium-based alloy, a titanium-based alloy, a vanadium-based alloy, and a magnesium-based alloy.
Illustratively, the mass ratio of the liquid organic material to the solid alloy powder in the hydrogen storage material is 5:1, 6:1, 7:1, 8:1, 9:1, 10:1, or any range therebetween. Wherein, when the mass ratio of the liquid organic material to the solid alloy powder of the hydrogen storage material is too low (for example, the mass ratio is less than 5), the solid particles are insufficiently dispersed, the liquid-solid contact is deteriorated to cause the reaction efficiency to be lowered, and the solid utilization rate to be lowered; when the mass ratio of the liquid organic material to the solid alloy powder is too high (for example, the mass ratio is higher than 10), the solid alloy powder is too small in unit volume, the hydrogen storage and discharge amount of the device is low, and the processing capacity of the device is reduced. Preferably, the primary particle size d of the solid alloy powder in the hydrogen storage material0Is 50-100 μm, e.g. primary particle size d of solid alloy powder 050, 60, 70, 80, 90, 100 microns or any range therebetween.
Specifically, the aromatic liquid organic material comprises at least one of benzene series, carbazole series and indole series; wherein for example benzene is selected from cyclohexaneAt least one of methylcyclohexane, benzene, toluene, and the like; exemplary carbazole groups may be selected from, for example, at least one of ethylcarbazole, tetrahydrocarbazole, octahydrocarbazole, dodecahydrocarbazole, and the like; exemplary indoles can be selected from N-ethyl indole, N-methyl indole, and the like. The solid alloy in this example is a rare earth alloy AB5Type alloys such as LaNi5Zirconium-based alloys such as ZrMn2Titanium-based alloys such as TiFe, vanadium-based alloys such as VFe, magnesium-based alloys such as Mg2Ni, and the like.
For example, in this embodiment, the hydrogen storage material is N-ethyl indole as the liquid organic material, LaNi5When the alloy powder is solid alloy powder, the temperature of the hydrogen storage reaction is 160-190 ℃, and the pressure is 2-10 MPa; the temperature of the hydrogen discharge reaction is 170-220 ℃, and the pressure is 0.1-1 MPa; further examples are ethyl carbazole as liquid organic material, Mg2When Ni is solid alloy powder, the temperature of the hydrogen storage reaction is 200-250 ℃, and the pressure is 2-10 MPa; the temperature of the hydrogen discharge reaction is 220-300 ℃, and the pressure is 0.1-1 MPa; further example is toluene as liquid organic material, LaNi5When the alloy powder is solid alloy powder, the temperature of the hydrogen storage reaction is 200-250 ℃, and the pressure is 2-10 MPa; the temperature of the hydrogen discharge reaction is 300-350 ℃, and the pressure is 0.1-1 MPa.
The embodiment of the invention realizes the coupling hydrogen absorption and desorption of the liquid organic material and the solid alloy powder, and simultaneously utilizes the solid alloy powder as a catalyst of the liquid organic material for hydrogen storage reaction and hydrogen desorption reaction, and the liquid organic material serves as a dispersion carrier of the solid alloy powder. The embodiment realizes the fluidization operation of the hydrogen storage material formed by the liquid organic material and the solid alloy powder, increases the contact area of gas, liquid and solid, and improves the reaction efficiency; the hydrogen storage material is circulated through the first body 1 and the second body 2, so that the separation of fine powder substances of solid alloy powder and a continuous phase, namely liquid organic materials is avoided, the energy consumption is reduced, the reaction part is further enlarged, and the reaction proceeding degree is improved.
In some embodiments, the first body 1 further comprises a first charging port 13 and a second charging port 14; the first inlet 13 is used for inputting liquid organic material into the first body 1; the second charge inlet 14 is used for feeding solid alloy powder into the first body 1.
Specifically, as shown in fig. 1 and fig. 2, in this embodiment, the liquid organic material is introduced into the lower portion of the first body 1 through the first charging port 13 and the solid alloy powder through the second charging port 14, under the flow lifting action of the liquid organic material, the solid-liquid mixture is uniformly dispersed in the first body 1, enters the second body 2 through the pipeline, and circulates back into the first body 1 from the second body 2, and the hydrogen storage material composed of the liquid organic material and the solid alloy powder forms stable solid-liquid distribution and circulation between the first body 1 and the second body 2. Advantageously, a valve 22 is provided at the first inlet port 13, by means of which valve 22 the flow of liquid organic material can be regulated, and a tap is provided at the second inlet port 14, by means of which tap the discharge of solid alloy powder can be regulated.
In some embodiments, as shown in fig. 3 in particular, the first body 1 and the second body 2 are both provided with a sewage draining outlet 15, and the sewage draining outlet 15 is used for draining the used hydrogen storage material. Understandably, in 100 reaction cycles of work, the solid alloy powder with the average particle size of 50-100 microns can be pulverized to about 1 micron, and the pulverization is shown to have the effects of reducing the hydrogen storage and discharge speed, reducing the particle size, deteriorating the separation effect and the like. The drain outlet 15 may be used to discharge all of the solid alloy powder and the liquid organic material, the properties of which are not satisfactory after a period of use. Specifically, the method comprises the following steps: the hydrogen inlet 11, the first inlet port 13 and the second inlet port 14 may be closed, and the hydrogen storage material in the first body 1 may be discharged from the sewage drain 159 by blowing gas from the first hydrogen outlet 12.
In some embodiments, the reaction apparatus 100 further comprises a plurality of sampling windows 5, the sampling windows 5 being dispersed on the connecting lines of the first body 1 and the second body 2.
Specifically, as shown in fig. 4, a certain particle size limit value may be set for the solid alloy powder, when the solid alloy powder passes through a plurality of reaction cycles, the pulverization degree of the solid alloy powder is periodically and periodically detected, if the pulverization degree of the particle size of the solid alloy powder reaches the limit value, it indicates that the hydrogen storage and release rate is decreased, the particle size is decreased, and the separation effect is deteriorated, and the microfiltration module 4 may be used to screen out the solid alloy powder in the circulating hydrogen storage material, and then a new solid alloy powder with excellent functions may be replenished. The method specifically comprises the following steps: periodically detecting the pulverization degree of the solid alloy powder through the sampling window 5, and when the real-time analysis result of the particle size of the solid alloy powder shows that the particle size is reduced to a particle size limit value, opening the pipe valve 22 between the second body 2 and the microfiltration module 4, removing a part of the solid alloy powder through the microfiltration module 4, and simultaneously supplementing an equal amount of new solid alloy powder with excellent functions from the lower part of the second charging port 14 of the first body 1, wherein the replacement rate of the solid alloy powder is preferably 20-80%. In the embodiment, the influence of solid alloy powder pulverization on the catalytic efficiency and the hydrogen absorption and desorption reaction rate is considered, the particle size is analyzed in real time by arranging the sampling port, and the operation parameters are adjusted accordingly, so that the optimization of operation is realized.
As shown in fig. 5, according to an embodiment of the present invention, there is also provided a hydrogen storage control method including the steps of:
s1, assembling the reaction device 100 in any one of the above embodiments;
s2, introducing a certain flow of liquid organic material and solid alloy powder into the first body 1 until the liquid organic material and the solid alloy powder stably circulate in the first body 1 and the second body 2;
s3, heating the first body 1 and the second body 2, and introducing hydrogen with certain pressure into the first body 1;
and S4, periodically monitoring the particle size of the solid alloy powder, and adjusting the mass ratio of the liquid organic material to the solid alloy powder and the flow rate of the liquid organic material according to the change of the particle size of the solid alloy powder.
Specifically, in S1, the hydrogen slurry reactor 100 in any of the above embodiments is connected by piping, and a suitable hydrogen storage material is selected, wherein the initial mass ratio of the liquid organic material to the solid alloy powder is preferably 5 to 10:1, primary particle diameter d of solid alloy powder0Preferably 50-100 micrometers (see the above description, and will not be described again), in the hydrogen slurry reaction apparatus 100 of the present embodiment, the sum of the volumes of the first body 1 and the second body 2 is the total volume V.
The method for determining the initial flow rate of the liquid organic material at a certain flow rate comprises the following steps:
and detecting the hydrogen storage (or hydrogen discharge) isotherm of the hydrogen storage material system at the selected hydrogen storage temperature and pressure (or hydrogen discharge temperature and pressure), namely a hydrogen storage amount-time curve (or hydrogen discharge amount-time curve), wherein the detection method is a conventional method and is not repeated.
The first-order kinetic fitting is carried out on the isothermal line of hydrogen storage (or hydrogen discharge) to obtain the speed constant k (min) of the hydrogen storage reaction or the hydrogen discharge reaction-1)：
dc/ct＝k(ce-c)
c is the concentration of the reaction product of hydrogen storage (or hydrogen discharge) at time t in kg/L, ceThe concentration of hydrogen storage (or hydrogen discharge) reaction products when the reaction reaches the equilibrium is expressed in kg/L;
the space velocity of hydrogen storage reaction and hydrogen discharge reaction between the liquid organic material and the solid alloy powder, TOF ═ k × ml/mg；
Wherein k is the speed constant unit of min for hydrogen storage reaction and hydrogen discharge reaction of the liquid organic material and the solid alloy powder-1；mlIs the mass of the liquid organic material, and the unit is Kg; m isgIs the mass of the solid alloy powder, and the unit is kg;
according to the velocity constant k (min) of hydrogen storage reaction or hydrogen discharge reaction-1) And space velocity TOF (min) of hydrogen storage reaction and hydrogen discharge reaction of the liquid organic material and the solid alloy powder-1) The initial volume flow Q of the liquid organic material can be obtained0；
Q0＝V*TOF；
Wherein Q0The unit is L/min; v is the sum of the volumes of the first body 1 and the second body 2, and the unit is L; TOF is the space velocity of hydrogen storage reaction and hydrogen discharge reaction of the liquid organic material and the solid alloy powder, and the unit is min-1。
In some embodiments, the method for adjusting the mass ratio of the liquid organic material to the solid alloy powder according to the change in the particle size of the solid alloy powder in S4 includes:
firstly, the pulverization degree of the solid alloy powder can be analyzed in a real-time analysis mode, namely, the particle size value of the analyzed solid alloy powder is measured, and the method specifically comprises the following steps: the sampling is performed from the sampling window 5, and the analysis can be performed in an online or offline manner, for example, the analysis can be performed in an online manner by means of a focused beam reflection measurement technique, a particle video microscope technique, and the like; the off-line method can be performed by means of a laser particle size analyzer, zeta potential analyzer, etc., i.e., the analysis frequency of the particle size of the solid alloy powder is preferably 10 to 30 min/time.
Wherein the volume flow rate Q ═ f (d) of the liquid organic material;
mass flow rate M ═ g (d) of the solid alloy powder;
secondly, when the particle diameter d of the solid alloy powdermWith its primary particle size d0In a ratio of 1: 20-50, e.g. primary particle size d of the solid alloy powder in this example0Preferably 50-100 microns, and the particle size of the solid alloy powder detected in real-time analysis at the present stage is dmWhen the particle size is 1-5 microns, the available particle size is d0Has an alternative particle diameter dmThe solid alloy powder of (1), wherein the substitution amount is in terms of particle diameter dmBased on the mass of the solid alloy powder of (b), the particle diameter of the substitute is d0The solid alloy powder of (2) has a particle diameter of dm20-80% by mass of the solid alloy powder.
When a new particle diameter d is added0Obtaining a relation of particle size of solid alloy powder in the newly formed hydrogen storage material-airspeed-flow of the liquid organic material;
i.e., the value d after the formation of a new hydrogen storage material in the present hydrogen slurry reaction apparatus 1000And dmThe particle size of the space velocity TOF is determined according to the methodRegulating deviceFor solid alloy powders and corresponding TOFRegulating deviceFitting numerical values to obtain a relational expression
TOFRegulating device＝f(d)；
Wherein TOFRegulating deviceSpace velocity in min for hydrogen storage and hydrogen discharge for the newly formed hydrogen storage material-1(ii) a Q ═ f (d), Q is the flow rate of the liquid organic material, in units of L/min;
Qregulating device＝V*TOFRegulating device＝V*f(d)
Wherein QRegulating deviceThe volume flow of the adjusted liquid organic material is L/min; TOFRegulating deviceSpace velocity in min for hydrogen storage and hydrogen discharge for the newly formed hydrogen storage material-1(ii) a V is the sum of the volumes of the first body 1 and the second body 2, in units L.
In some embodiments, to avoid excessive flow of liquid organic material, Q is definedRegulating device>2Q0When the temperature of the water is higher than the set temperature,
wherein QRegulating deviceIs the regulated volume flow of the liquid organic material; q0Is the initial volumetric flow rate of the liquid organic material; m islIs the initial mass of liquid organic material; m isgIs the initial mass of the solid alloy powder; m isl. toneThe quality of the liquid organic material adjusted according to the particle size of the solid alloy powder; m isg tiao (a Chinese character of 'g')The quality of the solid alloy powder is adjusted according to the particle size of the solid alloy powder.
The hydrogen storage control method of the hydrogen slurry reaction apparatus 100 in this embodiment considers the influence of pulverization of the solid alloy powder on the catalytic efficiency and the hydrogen absorption reaction and hydrogen desorption reaction rates, adjusts the mass ratio of the liquid organic material to the solid alloy powder and the flow rate of the liquid organic material according to the change of the particle size distribution of the solid alloy powder, adjusts the operation parameters accordingly, increases the contact area of hydrogen and the hydrogen storage material, realizes the optimization of operation, and achieves the optimal space velocity and reaction efficiency.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A hydrogen slurry reaction apparatus, comprising:
a first body comprising a volume of hydrogen storage material therein;
a second body having an input end connected with an output end of the hydrogen storage material of the first body and an output end connected with an input end of the hydrogen storage material of the first body; the hydrogen storage material is circulated in the first body and the second body;
a heating unit that heat-treats the first body and the second body, respectively; and
a microfiltration component; the input end of the hydrogen storage material is connected with the output end of the second body, the output end of the hydrogen storage material is connected with the input end of the hydrogen storage material of the first body, and the hydrogen storage material is used for screening and filtering the circulating hydrogen storage material.
2. The reaction device according to claim 1, wherein a hydrogen inlet and a first hydrogen outlet are formed in the first body in a height direction in an opposite manner; and a second hydrogen outlet is formed in the second body.
3. The reactor device of claim 1 or 2, further comprising a plurality of sampling windows dispersed on the connecting line of the first body and the second body.
4. A reaction device according to claim 3, wherein the hydrogen storage material comprises a liquid in a mass ratio of 5-10:1Bulk organic materials and solid alloy powders; wherein the liquid organic material is an aromatic liquid organic material; the solid alloy powder is rare earth AB5At least one of a type alloy, a zirconium-based alloy, a titanium-based alloy, a vanadium-based alloy, and a magnesium-based alloy.
5. The reactor device of claim 4, wherein the first body further comprises a first charging port and a second charging port; the first filling port is used for inputting the liquid organic material into the first body; the second charging port is used for inputting the solid alloy powder into the first body.
6. The reaction device as claimed in claim 3, wherein the first body and the second body are both provided with a sewage draining outlet for draining the used hydrogen storage material.
7. A hydrogen storage control method is characterized by comprising the following steps:
assembling the reaction device of any one of claims 1-6;
introducing a certain flow of liquid organic material and solid alloy powder into the first body until the liquid organic material and the solid alloy powder stably circulate in the first body and the second body;
heating the first body and the second body and then introducing hydrogen with certain pressure into the first body;
periodically monitoring the particle size of the solid alloy powder, and adjusting the mass ratio of the liquid organic material to the solid alloy powder and the flow rate of the liquid organic material according to the change of the particle size of the solid alloy powder.
8. The method of claim 7,
initial volume flow rate Q of the liquid organic material0＝V*TOF；
Wherein Q0The unit is L/min; v is the first body and the second bodyThe sum of the volumes of the two bodies is expressed in L; TOF is the space velocity of hydrogen storage reaction and hydrogen discharge reaction of the liquid organic material and the solid alloy powder, and the unit is min-1；
TOF＝k*ml/mg；
Wherein k is a rate constant of hydrogen storage reaction and hydrogen discharge reaction of the liquid organic material and the solid alloy powder in min-1；mlIs the mass of the liquid organic material in kg; m isgIs the mass of the solid alloy powder in kg.
9. The method of claim 7, wherein adjusting the mass ratio of liquid organic material to the solid alloy powder based on the change in particle size of the solid alloy powder comprises:
when the particle diameter d of the solid alloy powdermWith its primary particle size d0In a ratio of 1: when the particle diameter is 20-50, the particle diameter is d0The solid alloy powder has an alternative particle diameter dmThe solid alloy powder of (2) has a particle diameter of dmThe mass of the solid alloy powder is taken as a reference, and the mass percentage of the replaced solid alloy powder is 20-80%;
obtaining a relation of the particle size of the solid alloy powder in the newly formed hydrogen storage material-space velocity-flow of the liquid organic material;
TOFregulating device＝f(d)；
Wherein TOFRegulating deviceSpace velocity in min for hydrogen storage and hydrogen discharge for the newly formed hydrogen storage material-1(ii) a Q ═ f (d), Q is the volume flow rate of the liquid organic material, in units of L/min;
Qregulating device＝V*TOFRegulating device＝V*f(d)
Wherein QRegulating deviceThe volume flow of the liquid organic material after adjustment is in L/min; TOFRegulating deviceSpace velocity in min for hydrogen storage and hydrogen discharge for the newly formed hydrogen storage material-1(ii) a V is the sum of the volumes of the first body and the second body, and the unit isL。
10. Method according to claim 9, characterized in that Q is definedRegulating device>2Q0When the temperature of the water is higher than the set temperature,
wherein QRegulating deviceIs the regulated volume flow of the liquid organic material; q0Is the initial volumetric flow rate of the liquid organic material; m islIs the initial mass of the liquid organic material; m isgIs the initial mass of the solid alloy powder; m isl. toneThe mass of the liquid organic material adjusted according to the particle size of the solid alloy powder; m isg tiao (a Chinese character of 'g')The quality of the solid alloy powder is adjusted according to the particle size of the solid alloy powder.
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