Magnesium oxide hydrogen storage material preparation equipment and preparation method

Abstract

The invention discloses magnesium oxide hydrogen storage material preparation equipment which comprises a rack, a solid hopper and a liquid hopper are arranged on the rack and connected with a reaction kettle through pipelines, the bottom end of the reaction kettle is connected with a discharging pipe, the discharging pipe is connected with an inlet of a liquid suction pump, and an outlet of the liquid suction pump is connected with a rotary evaporator. According to the present invention, water is adopted as the main material to prepare the product, the whole reaction process is automatic, the preparation efficiency is improved, the reaction safety is increased, the labor cost is reduced, the produced magnesium oxide particles have the large agglomeration, and the magnesium oxide is suitable for being used as the food; and the vacuum generator reduces the air pressure in the rotary evaporator and accelerates the water evaporation speed, so that precipitated magnesium oxide particles are agglomerated, and gaps among agglomerates can further adsorb trace hydrogen, thereby greatly improving the processing efficiency and the production quality.

Description

Technical Field

[0001] The present invention relates to the field of magnesium oxide processing, and particularly to an experimental preparation device and a preparation method for a magnesium oxide hydrogen storage material. Background Art

[0002] Hydrogen is an important carrier for the green and low-carbon transformation. Due to its cleanliness, high efficiency, and sustainability, hydrogen is highly anticipated in the development of new energy. Since hydrogen usually exists in a gaseous state and is flammable, explosive, and easy to disperse, magnesium-based hydrogen storage has become a research direction for hydrogen storage. Magnesium-based materials can not only allow hydrogen to enter and exit freely but also purify hydrogen. Solid-state hydrogen storage enables larger storage and transportation volumes, lower costs, and higher safety. At the same time, hydrogen molecules have strong reducibility and effects on human health, and are also of great importance in food. Through solid-state hydrogen storage products, the hydrogen content in food can also be increased, which has a positive impact on human health and food quality.

[0003] The existing preparation of magnesium-based hydrogen storage materials mainly involves reacting magnesium powder with externally introduced hydrogen to form hydrides (such as MgH2, etc.). Since the alloy material itself requires hydrogen, to increase the hydrogen storage capacity, using magnesium oxide for hydrogen storage becomes a better hydrogen storage material. During preparation, a reaction kettle, a vacuum furnace, a high-temperature heat treatment device, etc. are required to perform processes such as material mixing, heating, constant temperature, and static settlement on the materials. Hydrogen has the characteristics of being flammable, explosive, and easy to disperse. Currently, an electric field generator is installed in the reaction kettle to electrolyze water to produce hydrogen, but the amount of hydrogen produced is small and the air pressure is low, which is not suitable for large-scale production. Summary of the Invention

[0004] To solve the above technical problems, the present invention provides an experimental preparation device for a magnesium oxide hydrogen storage material, including a frame. A solid hopper and a liquid hopper are arranged on the frame. Both the solid hopper and the liquid hopper are connected to a reaction kettle through pipelines. The bottom end of the reaction kettle is connected to a discharge pipe, and the discharge pipe is connected to the inlet of a liquid suction pump. The outlet of the liquid suction pump is connected to a rotary evaporator, and the rotary evaporator is connected to a vacuum generator. An oil temperature machine is also arranged on the frame, and the oil temperature machine is used to provide heat for the rotary evaporator. The pipelines include an air inlet pipe, a liquid inlet pipe, and a feeding pipe, which are used to transport raw materials into the reaction kettle. One end of the air inlet pipe is connected to the reaction kettle, and the port of the air inlet pipe extends to the bottom of the reaction kettle. The other end of the air inlet pipe is connected to an air valve, and the air valve is used to connect to a gas source. Magnesium oxide particles and water enter the reaction kettle through the pipelines and are stirred to enable hydrogen molecules to be adsorbed by the magnesium oxide particles.

[0005] Preferably, a first ball valve and a pressure sensor are further arranged on the air inlet pipe.

[0006] Preferably, one end of the liquid inlet pipe is connected to the reaction kettle, the other end of the liquid inlet pipe is connected to a water storage tank, and a liquid pump and a second ball valve are further arranged on the liquid inlet pipe.

[0007] Preferably, one end of the feeding pipe is connected to the reaction kettle, the other end of the feeding pipe is connected to the solid hopper, and a third ball valve is further arranged on the feeding pipe.

[0008] Preferably, the reaction kettle is connected to an exhaust pipe for discharging the gas in the reaction kettle.

[0009] A method for preparing a magnesium oxide hydrogen storage material comprises the following specific steps:

[0010] S1. Start the reaction kettle, and keep the stirring motor of the reaction kettle running at a low speed;

[0011] S2. Add solid and liquid raw materials into the reaction kettle, pre-mix the solid and liquid in the reaction kettle, and make the liquid raw material reach the preset flow rate;

[0012] S3. After the addition of the solid and liquid raw materials is completed, adjust the stirring motor to run at a high speed, stir the solid and liquid to mix, and at the same time add gas raw materials into the reaction kettle and adjust to the preset air pressure;

[0013] S4. Preheat the oil temperature machine, stop heating after reaching the set temperature, start the vacuum generator, extract the air in the rotary evaporator, so that a negative pressure is formed in the rotary evaporator, and the preset pressure is reached in the rotary evaporator;

[0014] S5. After reaching the preset mixing time, stop supplying the gas raw materials, transport the solid-liquid mixture to the rotary evaporator by a fluid suction pump, evaporate the water, and continuously supply the gas raw materials, set the evaporation temperature and the preset air pressure;

[0015] S6. After reaching the preset evaporation time, the drying step is completed, and the finished product is bagged and collected.

[0016] Preferably, in the step S1, the stirring motor keeps running at a low speed, and the motor percentage is 25%-35%.

[0017] Preferably, in the step S3, the stirring motor is adjusted to run at a high speed, and the motor percentage is 50%-70%.

[0018] The technical effects and advantages of the present invention:

[0019] 1. In the present invention, the product is prepared with water as the main material, no impurities will remain, the overall reaction process is automated, the preparation efficiency is improved, the reaction safety is increased, and the labor cost is reduced.

[0020] 2. In the present invention, the magnesium oxide particles after production have large agglomeration and uniform particles, and are suitable for use as food.

[0021] 3. In the present invention, a vacuum generator reduces the air pressure inside the rotary evaporator, speeds up the water evaporation rate, causes the precipitated magnesium oxide particles to agglomerate into larger-sized agglomerated particles, and the gaps between the agglomerations can further adsorb trace hydrogen. After fully heating to remove the water, agglomerated magnesium oxide particles are obtained, greatly improving the processing efficiency and production quality, and being suitable for mass production. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 is a schematic structural diagram of a test preparation device for a magnesium oxide hydrogen storage material provided by an embodiment of the present application;

[0023] Figure 2 is a top view of the device provided by an embodiment of the present application;

[0024] Figure 3 is a front view of the device provided by an embodiment of the present application with the frame, control box, and oil temperature machine removed.

[0025] In the figure: 1, frame; 2, solid hopper; 3, liquid hopper; 31, water storage tank; 4, pipeline; 41, intake pipe; 411, air valve; 412, first ball valve; 413, pressure sensor; 42, liquid inlet pipe; 421, liquid pump; 422, second ball valve; 43, discharge pipe; 431, third ball valve; 5, reaction kettle; 51, exhaust pipe; 6, fluid suction pump; 61, discharge pipe; 7, rotary evaporator; 8, vacuum generator; 9, oil temperature machine; 10, control box; 11, temperature sensor; 12, manual ball valve. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0026] The present invention will be further described in detail below in conjunction with the drawings and specific embodiments. The embodiments of the present invention are given for purposes of illustration and description, and are not exhaustive or limit the present invention to the disclosed form. Many modifications and variations are obvious to those of ordinary skill in the art. The embodiments are selected and described to better illustrate the principles and practical applications of the present invention, and enable those of ordinary skill in the art to understand the present invention and design various embodiments with various modifications suitable for specific purposes.

[0027] Please refer to Figures 1 to 3 , a test preparation device for a magnesium oxide hydrogen storage material is provided in the invention, including a frame 1, on which a solid hopper 2 and a liquid hopper 3 are arranged. Both the solid hopper 2 and the liquid hopper 3 are connected to a reaction kettle 5 through pipelines 4. The bottom end of the reaction kettle 5 is connected to a discharge pipe 61. The discharge pipe 61 is connected to the inlet of a liquid suction pump 6. The outlet of the liquid suction pump 6 is connected to a rotary evaporator 7. The rotary evaporator 7 is connected to a vacuum generator 8. An oil temperature machine 9 and a control box 10 are also arranged on the frame 1. The oil temperature machine 9 is used to provide heat for the rotary evaporator 7, and the control box 10 is used to control the operation of the device.

[0028] Specifically, the solid hopper 2 is used to add and store magnesium oxide particles and feed them into the reaction kettle 5. The liquid hopper 3 is connected to the water storage tank 31 and is used to add and store water. The magnesium oxide particles and water enter the reaction kettle 5 through the pipeline 4, are fully stirred to disperse the magnesium oxide particles, and hydrogen gas is introduced into the water. Trace hydrogen molecules are adsorbed by the tiny magnesium oxide particles. After the stirring and hydrogen charging process is saturated, the fluid suction pump 6 transports the mixture to the rotary evaporator 7. The oil temperature machine 9 heats the rotary evaporator 7, the water gradually evaporates, and the vacuum generator 8 reduces the air pressure in the rotary evaporator 7 to accelerate the water evaporation rate, causing the precipitated magnesium oxide particles to agglomerate into larger-sized agglomerated particles. The gaps between the agglomerates can further adsorb trace hydrogen gas. After sufficient heating to remove the water, agglomerated magnesium oxide particles are obtained and dried into white fine powder. This fine powder is mixed with one or several flavoring raw materials, and a small amount of hydrogen gas will be released after consumption.

[0029] In this embodiment, the pipeline 4 includes an air inlet pipe 41, a liquid inlet pipe 42, and a blanking pipe 43, which are used to transport raw materials into the reaction kettle 5. One end of the air inlet pipe 41 is connected to the reaction kettle 5, and the port of the air inlet pipe 41 extends to the bottom of the reaction kettle 5, so that the gas entering the reaction kettle 5 can be fully adsorbed by the magnesium oxide particles and can protect the raw materials in the reaction kettle 5 to prevent gas backflow during the mixing and adsorption process. The other end of the air inlet pipe 41 is connected to an air valve 411, and the air valve 411 is used to connect to a gas source. The gas source can be selected as a gas cylinder, and the gas cylinder stores hydrogen gas. A first ball valve 412 and a pressure sensor 413 are also provided on the air inlet pipe 41. When the first ball valve 412 is opened, hydrogen gas enters the reaction kettle 5 through the air inlet pipe 41, and the hydrogen gas flow is monitored by the pressure sensor 413 to adjust the hydrogen gas pressure to 1 - 1.5 kPa.

[0030] One end of the liquid inlet pipe 42 is connected to the reaction kettle 5, and the other end of the liquid inlet pipe 42 is connected to the water storage tank 31. A liquid pump 421 and a second ball valve 422 are also provided on the liquid inlet pipe 42. When the second ball valve 422 is opened and the liquid pump 421 is started, the water in the water storage tank 31 is transported into the reaction kettle 5.

[0031] One end of the blanking pipe 43 is connected to the reaction kettle 5, and the other end of the blanking pipe 43 is connected to the solid hopper 2. A third ball valve 431 is also provided on the blanking pipe 43. When the third ball valve 431 is opened, the magnesium oxide particles fall into the reaction kettle 5 due to gravity.

[0032] The reaction kettle 5 is connected to an exhaust pipe 51, which is used to discharge the gas in the reaction kettle 5 to maintain the pressure balance in the reaction kettle 5. Preferably, the exhaust pipe 51 is provided at the top of the reaction kettle 5.

[0033] Furthermore, a temperature sensor 11 is also provided on the frame 1, and the temperature sensor 11 is used to monitor the oil temperature of the oil temperature machine 9.

[0034] Furthermore, manual ball valves 12 are provided at the connections of the intake pipe 41 and the liquid inlet pipe 42 to the reaction kettle 5, which can be manually closed in case of emergency, thus improving the safety of the equipment.

[0035] The present invention provides a method for preparing a magnesium oxide hydrogen storage material, and the specific steps are as follows:

[0036] S1. Start the reaction kettle, and the stirring motor of the reaction kettle runs at a low speed.

[0037] S2. Add solid and liquid raw materials into the reaction kettle. The solid and liquid are premixed in the reaction kettle, and the liquid raw material reaches the preset flow rate.

[0038] S3. After the addition of the solid and liquid raw materials is completed, adjust the stirring motor to run at a high speed to stir the solid and liquid mixture. At the same time, add gaseous raw materials into the reaction kettle and adjust to the preset air pressure.

[0039] S4. Preheat the oil temperature machine. After heating to the set temperature, stop. Start the vacuum generator to pump out the air in the rotary evaporator, so that a negative pressure is formed in the rotary evaporator, and the preset pressure is reached in the rotary evaporator.

[0040] S5. After reaching the preset mixing time, stop the delivery of the gaseous raw materials. The solid-liquid mixture is transported to the rotary evaporator by a fluid suction pump to evaporate the water, and continuously introduce the gaseous raw materials, and set the evaporation temperature and the preset air pressure.

[0041] S6. After reaching the preset evaporation time, the drying step is completed, and the finished product is bagged and collected.

[0042] In this embodiment, the solid raw material is nano-level magnesium oxide particles, the liquid raw material is water, and the gaseous raw material is hydrogen.

[0043] In this embodiment, in step S1, the stirring motor runs at a low speed, and the motor percentage is 25%-35%. Preferably, the motor percentage is 30%. While adding the solid and liquid raw materials, use low-speed stirring to avoid dusting of the solid raw materials, resulting in backwashing of the raw materials and pollution of the raw materials in the solid hopper 2.

[0044] In this embodiment, in step S2, the liquid raw material is suctioned by a liquid pump. The liquid pump is a 24V explosion-proof and food-grade pump with a flow rate of 1L / min and a polytetrafluoroethylene pump head. The preset flow rate of the liquid raw material is 0.3-0.5L / min to avoid backwashing of the solid raw materials caused by too fast a flow rate.

[0045] In this embodiment, in step S3, the gaseous raw material enters from the bottom of the reaction kettle. The preset air pressure of the gaseous raw material is 1 - 1.5 kPa, which can avoid excessive flow rate during operation caused by excessive pressure, thereby preventing equipment damage or gas waste. Under the action of buoyancy, the bubbles are broken and refined by the stirring paddle and dispersed in the mixture, increasing the contact area and improving the mixing efficiency.

[0046] In this embodiment, in step S3, the stirring motor is adjusted to run at a high speed, and the motor percentage is 50% - 70%. Preferably, the motor percentage is 60%.

[0047] In this embodiment, in step S4, when the oil temperature machine preheats, the temperature rises by 7 - 10 °C per minute until the set temperature of 80 °C - 95 °C is reached and then stops. Preferably, the temperature is 90 °C, which can avoid the dissociation of hydrogen molecules adsorbed by magnesium oxide due to too high temperature.

[0048] In this embodiment, in step S5, a high-power fluid suction pump is used for the fluid suction pump, and a high-power motor is selected to cooperate with a stainless steel pump head because the mixture is a slurry-like material and an ordinary fluid pump cannot suction it.

[0049] In this embodiment, in step S6, the preset evaporation time is 24 h - 36 h. Preferably, the preset evaporation time is 48 h.

[0050] Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art and related fields without creative efforts shall fall within the scope of protection of the present invention. The structures, devices, and operation methods not specifically described and explained in the present invention shall be implemented according to the conventional means in the art without special instructions and limitations.

Claims

1. A test preparation device for magnesium oxide hydrogen storage material, comprising a frame, characterized in that, A solid hopper and a liquid hopper are provided on the frame. Both the solid hopper and the liquid hopper are connected to the reaction kettle through pipelines. The bottom end of the reaction kettle is connected to a discharge pipe. The discharge pipe is connected to the inlet of a liquid suction pump. The outlet of the liquid suction pump is connected to a rotary evaporator. The rotary evaporator is connected to a vacuum generator. An oil temperature machine is also provided on the frame. The oil temperature machine is used to provide heat for the rotary evaporator; The pipeline includes an inlet gas pipe, an inlet liquid pipe and a feeding pipe, which are used to transport raw materials into the reaction kettle. One end of the inlet gas pipe is connected to the reaction kettle, and the port of the inlet gas pipe extends to the bottom of the reaction kettle. The other end of the inlet gas pipe is connected to a gas valve, and the gas valve is used to connect to a gas source; Magnesium oxide particles and water enter the reaction kettle through the pipeline and are stirred to achieve the adsorption of hydrogen molecules by the magnesium oxide particles.

2. The preparation device for a magnesium oxide hydrogen storage material according to claim 1, characterized in that, A first ball valve and a pressure sensor are also provided on the inlet gas pipe.

3. The preparation device for a magnesium oxide hydrogen storage material according to claim 1, wherein One end of the inlet liquid pipe is connected to the reaction kettle, and the other end of the inlet liquid pipe is connected to a water storage tank. A liquid pump and a second ball valve are also provided on the inlet liquid pipe.

4. The preparation device for a magnesium oxide hydrogen storage material according to claim 1, characterized in that, One end of the feeding pipe is connected to the reaction kettle, and the other end of the feeding pipe is connected to the solid hopper. A third ball valve is also provided on the feeding pipe.

5. The preparation device for a magnesium oxide hydrogen storage material according to claim 1, characterized in that, The reaction kettle is connected to an exhaust pipe for discharging the gas in the reaction kettle.

6. A preparation method of a magnesium oxide hydrogen storage material, characterized in that Use the magnesium oxide hydrogen storage material test preparation equipment described in any one of claims 1-5 to process magnesium oxide.

7. The method for preparing the magnesium oxide hydrogen storage material according to claim 6, characterized in that, The specific steps are as follows: S1. Start the reaction kettle, and the stirring motor of the reaction kettle runs at a low speed; S2. Add solid and liquid raw materials into the reaction kettle. The solid and liquid are premixed in the reaction kettle, and the liquid raw material reaches a preset flow rate; S3. After the addition of the solid and liquid raw materials is completed, adjust the stirring motor to run at a high speed to stir the solid and liquid mixture. At the same time, add gas raw materials into the reaction kettle and adjust to a preset air pressure; S4. Preheat the oil temperature machine, stop after heating to the set temperature, start the vacuum generator, and evacuate the air in the rotary evaporator to form a negative pressure in the rotary evaporator, and the pressure in the rotary evaporator reaches a preset pressure; S5. After reaching the preset mixing time, stop transporting the gas raw materials. The solid-liquid mixture is transported to the rotary evaporator by a fluid suction pump to evaporate the water, and continuously introduce the gas raw materials, and set the evaporation temperature and the preset air pressure; S6. After reaching the preset evaporation time, the drying step is completed, and the finished product is bagged and collected.

8. The preparation method of the magnesium oxide hydrogen storage material according to claim 7, characterized in that In step S1, the stirring motor runs at a low speed, and the motor percentage is 25%-35%.

9. The method for preparing the magnesium oxide hydrogen storage material according to claim 7, wherein, In step S3, adjust the stirring motor to run at a high speed, and the motor percentage is 50%-70%.

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