CN218532810U - Device for preparing nano composite hydrogen storage material - Google Patents
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- CN218532810U CN218532810U CN202222584444.7U CN202222584444U CN218532810U CN 218532810 U CN218532810 U CN 218532810U CN 202222584444 U CN202222584444 U CN 202222584444U CN 218532810 U CN218532810 U CN 218532810U
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Abstract
The invention provides a device for preparing a nano-composite hydrogen storage material, which comprises a ball mill; the aerosol generator is connected with the bottom of the ball mill and used for generating aerosol which is combined with raw materials in the ball mill to form the nano-composite hydrogen storage material; and the vacuumizing device is connected with the ball mill and used for adjusting the air pressure in the ball mill. The nano composite hydrogen storage material prepared by the device has the advantages of obviously increased hydrogen storage amount, obviously accelerated hydrogen absorption and desorption rate and more stable cycle performance.
Description
Technical Field
The utility model relates to a hydrogen storage material technical field especially relates to a device of preparation nanometer composite hydrogen storage material.
Background
The mechanical ball milling method is one of the important methods for nano hydrogen storage material and processing. The mixing and refining of the materials are realized through frequent collision of the grinding balls, the grinding tank and the particles, and the generated metastable phase and amorphous phase can obviously improve the surface activity of the hydrogen storage alloy, so that the dynamics and the thermodynamic properties of the hydrogen storage material are improved. The mechanical ball milling method has simple operation process, low cost and high efficiency, and is one of the ideal methods for preparing the nano hydrogen storage material.
The attritor mill among the prior art includes: the device comprises a shell, a grinding barrel, a grinding ball unit and a control unit; the grinding barrel is fixedly arranged in the shell and positioned at the middle lower part of the shell, and the grinding barrel is used for placing grinding balls and grinding materials to be treated; the ball milling unit comprises a motor, a milling shaft and a rotary vane, the milling shaft is connected with an output shaft of the motor, the rotary vane is arranged on the milling shaft, and the ball milling unit is used for ball milling balls and grinding materials; the control unit is used for controlling the operation of the ball milling unit.
Although mechanical ball milling methods can rapidly refine the particles to the desired particle size range. However, the conventional mechanical ball milling method has an obvious physical limit, when the particle size is reduced to about 500nm and then ball milling is continued, the high temperature generated by ball milling easily causes particle agglomeration and grain growth, so that the material loses the nano structure, and the activity is difficult to further improve. This is because the milling of the material into the ultra-fine milling range creates a balance between the tendency of the milled product particles to re-agglomerate and break up, making the milling process more and more difficult. Therefore, the single ball milling method faces the development bottleneck in preparing high-performance nano functional powder.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a device for preparing a nano composite hydrogen storage material, which solves the problem that the mechanical ball milling method in the prior art has obvious physical limit.
In one aspect of the invention, an apparatus for preparing a nanocomposite hydrogen storage material is provided, comprising a ball mill;
the aerosol generator is connected with the bottom of the ball mill and used for generating aerosol which is combined with raw materials in the ball mill to form the nano-composite hydrogen storage material;
and the vacuumizing device is connected with the ball mill and is used for adjusting the air pressure in the ball mill.
Has the beneficial effects that: the ball mill is used for ball-milling raw materials to prepare nano-scale raw materials; the aerosol generator is used for preparing aerosol, so that the nano-scale raw material and the aerosol react to prepare the nano-composite hydrogen storage material; the vacuumizing device is used for vacuumizing and reducing the gas pressure in the ball mill, so that the phenomenon that the reaction of raw materials and aerosol is influenced due to overhigh gas pressure in the ball mill is avoided.
Further, the ball mill includes:
the cylinder body is connected with a vacuumizing device;
the transmission shaft is rotatably arranged in the barrel body and is arranged along the vertical direction, a material guide cavity is formed in the bottom side of the transmission shaft, a plurality of material distribution holes communicated with the material guide cavity are uniformly distributed in the outer wall of the bottom side of the transmission shaft, and the aerosol generator is communicated with the material guide cavity and is rotatably connected with the transmission shaft.
Has the beneficial effects that: the barrel is used for containing raw materials. The rotary shaft is used for stirring the raw materials in the ball mill, the material guide cavity is used for guiding the aerosol in and discharging the aerosol from the material distribution hole, the direct contact between the aerosol and the raw materials is facilitated, and violent collision is generated, so that the aerosol can quickly absorb heat generated in the ball milling process, the low-boiling-point solvent in the aerosol is quickly evaporated into gas under the combined action of kinetic energy and heat energy, and the generated superfine solute particles are uniformly distributed on the inner surface and the outer surface of the raw materials, so that the contact area and the reaction rate are greatly improved. The aerosol is sprayed out from the side wall material distribution hole of the transmission shaft, so that the potential safety hazard caused by instantaneous overlarge pressure in the cavity in the blowing-in process due to the fact that the air hole is blocked by particle powder sedimentation when the opening is located at the bottom is avoided.
Further, the aerosol generator comprises:
the input unit comprises a solution input unit and a gas input unit, the solution input unit is used for introducing a solution, and the gas input unit is used for introducing a gas;
the compression unit is connected with the solution input unit and the gas input unit and is used for compressing the introduced solution and/or gas;
and the output unit is connected between the compression unit and the transmission shaft, communicated with the material guide cavity and used for guiding the compressed solution and/or gas into the material guide cavity.
Has the advantages that: the input unit is used for inputting solution and gas, the compression unit is used for mixing the solution and the gas and generating certain pressure, and the solution and the gas generate certain air pressure under the action of the compression unit to form aerosol spray. The output unit is used for outputting the aerosol to the material guide cavity.
Further, the output unit includes
The spray head is connected with the output end of the compression unit and used for spraying aerosol;
and one end of the outlet pipe is communicated with the spray head, and the other end of the outlet pipe is communicated with the material guide cavity and used for conveying aerosol.
Has the beneficial effects that: the spray head is used for leading the compressed solution and the compressed gas in the compression unit to be in an aerosol form and leading the aerosol to a material guide cavity of the cylinder body.
Further, a first electronic valve for controlling the flow rate of the aerosol is arranged on the outlet pipe.
Has the advantages that: the first electronic valve is used for controlling the flow rate of the aerosol, so that the accurate control of the reaction is facilitated, and the smooth proceeding of the reaction is facilitated.
Furthermore, an exhaust port is formed in the top of the cylinder body, and the vacuumizing device is connected with the exhaust port of the cylinder body.
Has the advantages that: the exhaust port is favorable for exhausting gas generated in the grinding mill, so that the safety of reaction is ensured, and meanwhile, the phenomenon that the reaction speed is reduced or the reaction is hindered due to excessive gas in the grinding mill is avoided. The vacuumizing device can accelerate the discharge of gas in the grinding machine and improve the reaction efficiency.
Further, a second electronic valve used for maintaining the vacuum degree in the cylinder body is arranged between the exhaust port and the vacuum pumping device.
Has the beneficial effects that: the second electronic valve is used for controlling the opening and closing of the exhaust port, and the second electronic valve is opened when the exhaust is needed; the second electronic valve is closed when it is desired to maintain the atmosphere and pressure within the mill.
Furthermore, a nano-filtration membrane for filtering gas is arranged in the exhaust port.
Has the advantages that: the nanofiltration membrane only permeates gas, so that the loss of solid materials is avoided.
Further, the side wall of the cylinder body is provided with a cooling cavity for reducing the temperature in the cylinder body.
Has the advantages that: the cooling cavity is favorable for reducing the temperature in the cylinder in the reaction process, and avoids the influence of overhigh temperature on the reaction process.
Furthermore, a temperature measurer for detecting the temperature in the cylinder is arranged on the side wall of the cylinder.
Has the advantages that: for detecting the temperature within the barrel.
The technical principle of the invention is as follows: the inventor finds in previous experiments that the solute particles can be uniformly distributed on the surface of the nanoparticle raw material by adding the raw material into a ball mill for ball milling, blowing a solution from the top of the ball mill, and gasifying the solvent at a local high temperature generated by the ball milling. However, since the solution is blown in from the top, the solute cannot directly contact the raw material after being sprayed from the spray can, but needs to be fully contacted with the raw material through molecular diffusion, thereby reducing the contact rate and the combination rate of the solute and the raw material. Therefore, the inventor makes further improvement on the basis, the solution is blown in from the bottom, so that after the solute is sprayed out, the solute is directly contacted with the raw material under the action of air pressure and generates violent collision, the heat generated in the ball milling process is quickly absorbed, the solvent is quickly evaporated into gas under the combined action of kinetic energy and heat energy, and the generated superfine solute particles are uniformly distributed on the inner surface and the outer surface of the raw material particles, so that the contact rate and the combination rate are greatly improved. The inventor also unexpectedly finds that the hydrogen storage performance of the hydrogen storage material prepared by the method is obviously improved, and compared with the method of blowing the solution from the top, the hydrogen storage material prepared by the method has the advantages of obviously increased hydrogen storage amount, obviously accelerated hydrogen absorption and desorption rate and more stable cycle performance under the same condition. This may be due to the fact that such externally injected mechanical and chemical energy changes the size, morphology and microstructure of the particles. Specifically, the contact distance between the solution sprayed from the bottom and the raw material is shorter than that of top blowing, and the solution is in more violent direct collision, so that a larger stirring force is generated, the particles are more fully deformed, crushed, welded and refined in the ball milling process, and the particle stress, strain, defects, nano grain boundaries and phase boundaries are generated in a large quantity, so that the particle activity is greatly improved, and even multiphase chemical reactions are induced.
In addition, the skilled person usually does not choose bottom blowing because the pressure in the pipeline is too high instantaneously when the solution is blown in due to the easy blockage of the bottom air hole caused by powder sedimentation, and the potential safety hazard such as deflagration is easily generated. The traditional ball mill is further improved, the solution is blown in from the bottom through the wall of the transmission shaft, the problem of blockage caused by powder sedimentation is avoided while the same preparation effect is ensured, and the potential safety hazard in the production and preparation process is solved.
Meanwhile, the solution is gasified to absorb heat in the system, a good heat dissipation effect is achieved when the solution is discharged from the top, and the problem that the dehydrogenation reaction is carried out in advance due to overheating in the preparation process of the material, so that the loss of hydrogen storage capacity is caused is avoided.
Compared with the prior art, the invention has the following beneficial effects:
(1) The nano composite hydrogen storage material of the invention has the advantages of obviously increased hydrogen storage capacity, obviously accelerated hydrogen absorption and desorption rate and more stable cycle performance.
(2) Compared with the ball milling physical limit (about 500 nm), the grain diameter of the solute in the obtained aerosol is smaller and is only 20-50nm in a solvent volatilization mode, the activity is greatly improved, and hydrogen can be easily discharged/charged through a low-temperature path.
(3) Compared with the theoretical contact interfacial area between the solute and the raw material after the top blowing, the theoretical contact interfacial area of the material prepared by the bottom blowing is 5-10 times that of the top blowing; the dense superfine solute particles on the surface can improve the contact probability of the solute particles and hydrogen, thereby increasing the density of active sites, shortening the diffusion distance of hydrogen atoms in the hydrogen releasing/charging process and reducing the hydrogen releasing/charging reaction barrier; the reaction kinetics condition of the low temperature discharging/charging path speed limiting step (formula 5) can be greatly improved.
(4) The nano solute particles are fully contacted with the nano raw material particles and have certain binding force, thereby effectively avoiding the agglomeration of the raw material particles, being beneficial to maintaining the uniform grain size (100-150 nm) of the raw material phase in the discharge/charging circulation process and improving the circulation stability of the hydrogen storage performance of the composite material.
(5) The nano composite material is prepared by adopting a mode of high-energy ball milling in cooperation with bottom blowing aerosol spraying, so that the thermodynamics of raw materials are unstable, the reaction is facilitated, the hydrogen absorption and desorption kinetics can be improved, and compared with a material prepared by top blowing, a bottom blowing preparation sample realizes more rapid hydrogen absorption and desorption.
In conclusion, the nano-composite hydrogen storage material of the invention provides enough specific surface area and enough attachment sites, so that the activity is greatly improved, and the speed limit step of the low-temperature hydrogen discharge/charging path is greatly improved; the probability of hydrogen contact is improved, the diffusion distance of hydrogen atoms in the hydrogen discharging/charging process is shortened, and the hydrogen discharging/charging reaction potential barrier is reduced; the solute nanoparticles and the raw material nanoparticles are fully contacted and have certain binding force, so that the agglomeration of the raw material particles is effectively avoided, and the uniform size of the raw material grains is maintained.
Drawings
FIG. 1 shows the preparation of LiBH in example 1 of the present invention 4 Modified MgH 2 Schematic representation of an apparatus for nanocomposite hydrogen storage material.
FIG. 2 is a graph showing the results of the cycle stability test in test example 2 of the present invention.
In the above drawings: 1. a barrel; 2. a drive shaft; 3. an exhaust port; 4. an exhaust pipe; 5. a vacuum pump; 6. a second electronic valve; 7. a ball mill controller; 8. a motor; 9. a material distribution hole; 10. an impeller; 11. an inner wall; 12. an outer wall; 13. a cooling chamber; 14. a container; 15. an inlet tube; 16. a gas compressor; 17. a spray head; 18. an outlet pipe; 19. a first electronic valve; 20. an air inlet; 21. a coolant inlet; 22. and a cooling liquid outlet.
Detailed Description
The technical solution of the present invention is further described with reference to the drawings and the embodiments.
EXAMPLE 1 preparation of LiBH 4 Modified MgH 2 Device for nano composite hydrogen storage material
Preparation of LiBH of the invention 4 Modified MgH 2 The device for nano-composite hydrogen storage material comprises an attritor mill, an aerosol generator and a vacuum extractor.
The vertical ball mill comprises a cylinder body 1 and a transmission shaft 2, wherein the cylinder body 1 comprises a top, a side wall and a bottom. The top is provided with an exhaust port 3, the nano-film is arranged at the exhaust port 3 to prevent the materials from being exhausted along with the gas, the exhaust port 3 is communicated with a vacuum pump 5 through an exhaust pipe 4, and a second electronic valve 6 used for controlling the vacuum degree in the cylinder is arranged on the exhaust pipe 4. The transmission shaft 2 is rotatably arranged in the cylinder body 1 and is arranged along the vertical direction, a material guide cavity is formed in the bottom side of the transmission shaft 2, and a plurality of material distribution holes 9 communicated with the material guide cavity are uniformly distributed on the outer wall of the bottom side of the transmission shaft. The outer wall of the bottom side of the transmission shaft is provided with an impeller 10 for stirring materials. The other end of the transmission shaft 2 penetrates through the top of the cylinder body 1 and is connected with a motor 8, and the motor 8 is connected with a ball mill controller 7. The ball mill controller 7 is used for controlling parameters such as the rotating speed and time of the ball mill. The lateral wall of the cylinder body 1 is of a double-layer structure and comprises an inner wall 11 and an outer wall 12, a cooling cavity 13 capable of reducing the temperature of the cylinder body is arranged between the inner wall 11 and the outer wall 12, cooling liquid is contained in the cooling cavity 13, and the cooling liquid used in the embodiment is water. The outer wall 12 is provided with a coolant inlet 21 on one side and a coolant outlet 22 on the other side. A temperature measurer is arranged on the side wall of the cylinder body 1 and used for detecting the temperature in the cylinder body 1.
The aerosol generator comprises a container 14, an inlet pipe 15, a gas compressor 16, a spray head 17 and an outlet pipe 18, wherein the side wall of the gas compressor 16 is provided with a gas inlet 20 for inputting high-purity argon; the bottom end of a gas compressor 16 is connected with an inlet pipe 15 through an LiBH 4 The container 14 for the/THF solution is connected. The top of the gas compressor 16 is communicated with a spray head 17, one end of the spray head 17, which is far away from the gas compressor 16, is communicated with an outlet pipe 18, and one end of the outlet pipe 18, which is far away from the spray head 17, is communicated with the material guide cavity and is rotationally connected with the transmission shaft 2. The outlet pipe 18 is provided with a first electronic valve 19 for controlling the flow and start and stop of the aerosol generator. The gas compressor 16 is used to compress high purity argon and LiBH 4 THF solution was mixed and pressurized.
The second electronic valve 6, the first electronic valve 19 and the ball mill controller 7 are provided with an organic electronic module.
When in use, the method comprises the following steps: 1. the weight percentage of the composite material is 100 percent: magnesium hydride (MgH) 2 ) 66wt.%, lithium borohydride (LiBH) 4 ) 33.5wt.%, graphite grinding aid 0.5%; 66g of MgH 2 Adding the powder into a vertical ball mill, and grinding the powder into MgH 2 Adding 6600g of grinding balls into the mixture according to the mass ratio of 100. And starting the vacuum pump 5 to pump air out of the cylinder 1, then closing the vacuum pump 5, and keeping vacuum in the ball mill. The second electronic valve 19 is opened and high purity argon is added through the gas inlet 20 in the side wall of the gas compressor 16 to fill the inside of the attritor mill with argon. Starting a motor 8 of the vertical ball mill, setting the ball milling rotating speed to be 600rpm, setting the time to be 6h, and starting the motor8 drive the transmission shaft 2 to rotate, the transmission shaft 2 drives the impeller 10 to stir the grinding balls and the MgH 2 Make the grinding ball repeatedly impact MgH 2 So that the cold welding and the fracture are continuously generated.
2. In the ball milling process, liBH is prepared 4 The THF solution (2) having a concentration of 0.5mol/L was charged into the vessel 14. Turning on the power supply of the aerosol generator, setting the aerosol fluidity at 500ml/min, introducing argon (Ar) gas from the gas inlet 20, compressing high purity argon gas by the gas compressor 16, and charging LiBH in the container 14 4 The THF solution is pressed through the inlet tube 15 into the gas compressor 16, argon and LiBH 4 The THF solution is mixed and compressed in a gas compressor 16, the THF solution is sprayed out from a spray head 17 to form aerosol, the aerosol flows in an outlet pipe 18, enters a material guide cavity through the bottom of the ball milling tank and is sprayed out from a material distribution hole 9 into the cylinder body 1 at a constant speed. During the grinding process, high-speed collision between grinding balls, between the grinding balls and the wall of the vessel and between the grinding balls and the impeller 10 can generate local high temperature of 200-250 ℃ and strong physical force of 5-10 GPa at the collision point. When the aerosol touches the grinding ball and MgH 2 When in particle, THF solvent with boiling point of 66 ℃ can be vaporized instantly, and nanometer LiBH with superfine particle size 4 Solute particles are uniformly dispersed and loaded in the nano MgH under the action of stirring force 2 The surface of the particles; meanwhile, mgH is enabled by strong physical force generated by ball milling 2 The particles are continuously fractured and cold welded, resulting in partially ultrafine LiBH 4 The particles are coated on MgH 2 In the granules, thereby obtaining uniformly mixed MgH 2 Loaded ultra-fine LiBH 4 Like a hemp ball of LiBH 4 /MgH 2 A nanocomposite material.
The vacuum pump 5 works intermittently, and the air pressure in the tank is reduced, so that more aerosol can be sprayed in subsequently. In the whole preparation process, flowing water is introduced between the inner wall and the outer wall of the ball mill to prevent the temperature in the tank from being overhigh.
LiBH paired by FESEM and X-ray diffraction 4 /MgH 2 The nano composite material is characterized to obtain LiBH 4 Has a particle diameter of 50nm, mgH 2 The particle diameter of the particles is about 600nm, mgH 2 Has a grain size of 150nm, and has a LiBH 4 Modified MgH 2 Specific surface of nano composite hydrogen storage materialProduct of 15m 2 /g。
Example 2LiBH 4 Modified MgH 2 Preparation of nano composite hydrogen storage material
1. Based on the mass of the composite material as 100%: 58wt.% of magnesium hydride, 41wt.% of lithium borohydride and 1% of graphite grinding aid; mgH is added 2 Adding the mixture into an attritor mill for ball milling, and reducing the particle size by using a mechanical milling principle. The ball material ratio is: 80, 1, the rotating speed is as follows: the time at 800rpm was: 7h;
2. blowing LiBH from the bottom of the ball mill tank through Ar gas 4 THF solution, and gasifying the solvent by utilizing heat generated by ball milling to ensure that nano LiBH with ultra-fine particle size 4 Solute particles are uniformly distributed in MgH 2 Nano particle surface to obtain LiBH 4 Modified MgH 2 A nanocomposite hydrogen storage material. The LiBH 4 The THF solution had a concentration of 1.25mol/L and the gas feed rates were: 750ml/min.
LiBH paired by FESEM and X-ray diffraction 4 /MgH 2 Characterizing the nano composite material to obtain LiBH 4 Has a particle diameter of 35nm 2 The particle diameter of the particles is about 500nm, mgH 2 Has a grain size of 120nm, liBH 4 Modified MgH 2 The specific surface area of the nano-composite hydrogen storage material is 45m 2 /g。
Example 3LiBH 4 Modified MgH 2 Preparation of nano composite hydrogen storage material
1. The weight percentage of the composite material is 100 percent: 50wt.% of magnesium hydride, 48wt.% of lithium borohydride and 2% of graphite grinding aid; mgH is added 2 Adding the mixture into an attritor mill for ball milling, and reducing the particle size of the mixture by utilizing a mechanical milling principle. The ball material ratio is: 60; the rotating speed is as follows: 1000rpm; the time is as follows: 8h;
2. blowing LiBH from the bottom of the ball mill tank through Ar gas 4 THF solution, and gasifying the solvent by utilizing heat generated by ball milling to ensure that nano LiBH with ultra-fine particle size 4 Solute particles are uniformly distributed in MgH 2 Nano particle surface to obtain LiBH 4 Modified MgH 2 A nanocomposite hydrogen storage material. The LiBH 4 The THF solution had a concentration of 2mol/L and the gas feed rate was:1000ml/min。
LiBH paired by FESEM and X-ray diffraction 4 /MgH 2 Characterizing the nano composite material to obtain LiBH 4 Has a particle diameter of 20nm and MgH 2 The particle diameter of the particles is about 450nm, mgH 2 Has a grain size of 100nm 4 Modified MgH 2 The specific surface area of the nano-composite hydrogen storage material is 60m 2 /g。
Comparative example
Similar to example 3, except that Ar gas and LiBH were blown from the top of the jar mill 4 THF solution.
Test example 1 detection of Hydrogen storage kinetics
The detection method comprises the following steps: performing DSC test by setting different temperature rise rate gradients (2-10 ℃/min), drawing a DSC curve to find out the peak temperature, and using a formula:
wherein T is p Beta is the peak temperature and the heating rate respectively, a is the conversion of Mg into MgH 2 Fraction of, E a To activation energy, F KAS (a) A function representing the conversion fraction, R is a gas constant, and the apparent activation energy E is calculated a The hydrogen evolution dynamic performance of the composite material is expressed;
by setting different temperature gradients (100-300 ℃), filling H with different pressures 2 (2-5 MPa) and respectively recording the change of the hydrogen adsorption amount along with the time, finally drawing a curve of the change of the hydrogen adsorption/desorption amount along with the time under different conditions, and utilizing a formula:
ln[-ln(1-α)]＝n ln k+n ln t
wherein a is the conversion of Mg to MgH at the time of t 2 K is an effective kinetic parameter, n is an Avrami index, and the activation energy E is calculated a Reference is made to the literature for details on the determination of the hydrogen absorption kinetics of composite materials (Zhang L.et.)al, applied Surface Science,2020, 504. The results are shown in Table 1.
Test example 2 detection of cycling stability
The detection method comprises the following steps: the optimum hydrogen absorption/desorption conditions are obtained through hydrogen storage kinetic performance detection, the hydrogen absorption/desorption process is repeated on the composite material under the conditions, the total hydrogen absorption/desorption amount of the composite material in each process is recorded, a hydrogen absorption/desorption total amount data graph is drawn successively, the change trend of the data graph is observed and calculated, and the cycle stability of the composite material is determined, and the detailed content can refer to the reference in the test example 1. The results are shown in FIG. 2 and Table 1.
TABLE 1 Performance test results
| Group of | Example 3 | Comparative example |
| First hydrogen evolution (wt.%) at 265 deg.C | 5.8 | 5.6 |
| Time (h) to complete release of |
1 | 6 |
| Hydrogen storage capacity (wt.%) after 10 cycles | 96.5 | 70.9 |
| After 10 times of circulation, the hydrogen release quantity is reduced to (wt.%) | 5.6 | 3.97 |
From the above results, it can be seen that: the hydrogen storage material prepared in example 3 had a primary hydrogen release of 5.8wt.% higher than the hydrogen storage material prepared in the comparative example of 5.6wt.%; the time 1h required for the hydrogen storage material prepared in example 3 to completely absorb and desorb hydrogen is significantly shorter than that of the comparative example preparation material 6h; after ten hydrogen absorption and desorption cycles, the hydrogen storage capacity of the material prepared in the example 3 can still be kept to be 96.5 percent, while the hydrogen storage material prepared in the comparative example only remains 70.9 percent. The hydrogen evolution of the material prepared in example 3 decayed to 5.6% compared to only 3.97% for the hydrogen storage material prepared in the comparative example. It can be seen that the performance of the hydrogen storage material prepared in example 3 is significantly due to the hydrogen storage material prepared in the comparative example. The performance of the hydrogen storage materials prepared in examples 1-2 was tested to be similar to that of example 3.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (10)
1. An apparatus for preparing a nanocomposite hydrogen storage material, comprising:
a ball mill;
the aerosol generator is connected with the bottom of the ball mill and used for generating aerosol which is combined with raw materials in the ball mill to form the nano-composite hydrogen storage material;
and the vacuumizing device is connected with the ball mill and used for adjusting the air pressure in the ball mill.
2. An apparatus for producing a nanocomposite hydrogen storage material as claimed in claim 1, wherein: the ball mill comprises:
the cylinder body is connected with a vacuumizing device;
the transmission shaft is rotatably arranged in the barrel body and is arranged along the vertical direction, a material guide cavity is formed in the bottom side of the transmission shaft, a plurality of material distribution holes communicated with the material guide cavity are uniformly distributed in the outer wall of the bottom side of the transmission shaft, and the aerosol generator is communicated with the material guide cavity and is rotatably connected with the transmission shaft.
3. An apparatus for preparing a nanocomposite hydrogen storage material according to claim 2, wherein: the aerosol generator comprises:
the input unit comprises a solution input unit and a gas input unit, the solution input unit is used for introducing a solution, and the gas input unit is used for introducing a gas;
the compression unit is connected with the solution input unit and the gas input unit and is used for compressing the introduced solution and/or gas;
and the output unit is connected between the compression unit and the transmission shaft, communicated with the material guide cavity and used for guiding the compressed solution and/or gas into the material guide cavity.
4. An apparatus for preparing a nanocomposite hydrogen storage material as claimed in claim 3, wherein: the output unit comprises
The spray head is connected with the output end of the compression unit and is used for spraying aerosol;
and one end of the outlet pipe is communicated with the spray head, and the other end of the outlet pipe is communicated with the material guide cavity and used for conveying aerosol.
5. An apparatus for preparing a nanocomposite hydrogen storage material as claimed in claim 4, wherein: and the outlet pipe is provided with a first electronic valve for controlling the flow rate of the aerosol.
6. An apparatus for producing a nanocomposite hydrogen storage material as claimed in claim 2, wherein: an exhaust port is formed in the top of the cylinder body, and the vacuumizing device is connected with the exhaust port of the cylinder body.
7. An apparatus for preparing a nanocomposite hydrogen storage material as claimed in claim 6, wherein: and a second electronic valve for maintaining the vacuum degree in the cylinder is arranged between the exhaust port and the vacuum pumping device.
8. An apparatus for preparing a nanocomposite hydrogen storage material according to claim 6, wherein: and a nano filter membrane for filtering gas is arranged in the exhaust port.
9. An apparatus for preparing a nanocomposite hydrogen storage material according to claim 2, wherein: the side wall of the cylinder body is provided with a cooling cavity for reducing the temperature in the cylinder body.
10. An apparatus for preparing a nanocomposite hydrogen storage material according to claim 2, wherein: and a temperature measurer for detecting the temperature in the cylinder is arranged on the side wall of the cylinder.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115650156A (en) * | 2022-09-28 | 2023-01-31 | 重庆镁储新材料科技有限公司 | LiBH 4-modified MgH2 nano composite hydrogen storage material and preparation method and application thereof |
| CN116062684A (en) * | 2023-03-16 | 2023-05-05 | 浙江大学 | Device and method for increasing hydrogenation reaction speed of material in mixed gas containing hydrogen and inert impurity gas |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115650156A (en) * | 2022-09-28 | 2023-01-31 | 重庆镁储新材料科技有限公司 | LiBH 4-modified MgH2 nano composite hydrogen storage material and preparation method and application thereof |
| CN116062684A (en) * | 2023-03-16 | 2023-05-05 | 浙江大学 | Device and method for increasing hydrogenation reaction speed of material in mixed gas containing hydrogen and inert impurity gas |
| CN116062684B (en) * | 2023-03-16 | 2024-04-26 | 浙江大学 | Device and method for increasing hydrogenation reaction speed of material in mixed gas containing hydrogen and inert impurity gas |
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Effective date of registration: 20230509 Address after: 518107 b2-1908, building b1b2, Guangming science and Technology Park, Fenghuang community, Fenghuang street, Guangming District, Shenzhen, Guangdong Patentee after: Guangdong Guoyan Technology Research Center Co.,Ltd. Address before: No. 1-3-1, Building 2, International Maker Port Park, No. 130 Xiazhong Dukou, Shapingba District, Chongqing 400050 Patentee before: Chongqing magnesium storage new material technology Co.,Ltd. |