Continuous reaction device and method applied to solid powder material and application

Abstract

The invention provides a continuous reaction device and method applied to a solid powder material and application, the device comprises one or more reactors, when the number of the reactors is multiple, the multiple reactors are connected in parallel and / or in series, each reactor comprises a driving unit, a screw conveying unit and a reaction tube, the screw conveying unit comprises a stirring shaft and a spiral blade arranged on the stirring shaft, the stirring shaft is arranged in the reaction tube in a penetrating manner, the driving unit is positioned outside the reaction tube, is connected with the stirring shaft and drives the stirring shaft to rotate, and a jacket is sleeved outside the reaction tube. The continuous reaction device applied to the solid powder material has the advantages of being high in heat exchange efficiency, small in occupied area and large in treatment capacity, a series of continuous production processes such as loading, production and unloading can be achieved, and the continuous reaction device has the advantages of stirring solid-solid, solid-liquid, liquid-liquid, gas-liquid, gas-liquid, gas-liquid, gas-liquid, gas-liquid, gas-liquid, gas-liquid, gas-liquid, gas-liquid, gas-liquid, gas-liquid, gas-liquid and the method has very good application prospect and large-scale industrial popularization potential in the field of reaction of various phase-state materials such as gas-solid and the like.

Description

Technical Field

[0001] This invention relates to reaction tube technology, and more particularly to a continuous reaction apparatus, method and application for solid powder materials. Background Technology

[0002] Hydrogen energy, as a clean and efficient energy source, holds significant strategic importance in addressing the global energy crisis and environmental pollution. Developing efficient hydrogen storage technologies is crucial for reducing hydrogen costs and enabling large-scale application. Metal hydride solid-state hydrogen storage materials can reversibly absorb and release hydrogen under certain temperature and pressure conditions, offering advantages such as large hydrogen storage capacity, high energy density, safety and convenience, high hydrogen purity, and excellent cycle life performance. They are considered one of the effective means of storing and transporting hydrogen energy in the future. However, hydrogen storage materials exhibit significant thermal effects during preparation and storage. Due to the poor thermal conductivity of powder materials, the heat of hydrogen absorption is difficult to remove effectively and promptly, leading to problems such as particle sintering and agglomeration, which severely affects the hydrogen absorption and desorption reaction rate and cycle life of the storage materials. Traditionally, heat transfer can be enhanced by adding thermally conductive agents to the hydrogen storage material powder, briquetting the powder, and arranging coils or tubes within the container. However, the heat transfer problem remains unresolved, and continuous operation of the device is not yet possible, which seriously hinders the large-scale preparation, application, and promotion of metal hydride solid-state hydrogen storage materials.

[0003] Therefore, there is an urgent need to develop methods for preparing metal hydride hydrogen storage materials, reaction devices, and equipment for their large-scale application. This includes enhancing heat and mass transfer in reactors, increasing hydrogen absorption and desorption reaction rates, device throughput, and material cycle life, to achieve large-scale, continuous, and efficient production. This will greatly promote the application and widespread use of metal hydride hydrogen storage materials in energy storage, chemical, metallurgical, transportation, and construction fields. Summary of the Invention

[0004] The purpose of this invention is to address the aforementioned problems of existing reactors by proposing a continuous reaction device for solid powder materials. This device has the advantages of high heat exchange efficiency, small footprint, and large processing capacity. It can realize a series of continuous production processes such as loading, production, and unloading. It has very good application prospects and potential for large-scale industrial promotion in the field of material reactions involving multiple phases such as solid-solid, solid-liquid, liquid-liquid, gas-liquid, and gas-solid.

[0005] It should be noted that, in this invention, unless otherwise specified, the specific meaning of "comprising" in relation to composition and description includes both open-ended meanings such as "comprising," "including," etc., and closed-ended meanings such as "composed of," "consisting of," etc., and similar meanings.

[0006] To achieve the above objectives, the technical solution adopted by the present invention is: a continuous reaction device for solid powder materials, comprising one or more reactors, wherein when there are multiple reactors, the multiple reactors are connected in parallel and / or in series, and the reactors include a drive unit, a screw conveying unit and a reaction tube;

[0007] The screw conveying unit includes a stirring shaft and helical blades disposed on the stirring shaft, the stirring shaft passing through the reaction tube; or, the screw conveying unit includes two stirring shafts and continuous helical blades disposed between the two stirring shafts, the two stirring shafts being fixed at both ends of the reaction tube respectively;

[0008] The drive unit is located outside the reaction tube and is connected to the stirring shaft to drive the stirring shaft to rotate; the reaction tube is fitted with a jacket.

[0009] Furthermore, the drive unit includes a motor, a reducer, and a sealing structure, which is a magnetic coupler, a mechanical seal, or a packing seal. The motor is connected to the stirring shaft via the reducer, and the sealing structure is used to seal between the reducer and the reaction tube. When the sealing structure uses a magnetic coupler, the motor is connected to the stirring shaft sequentially via the reducer and the magnetic coupler, driving the stirring shaft to rotate. The motor provides power, and the reducer amplifies the motor's output torque before transmitting it to the magnetic coupler. The inner magnet of the magnetic coupler is connected to the stirring shaft, and the outer magnet is connected to the reducer's output shaft. The reducer's output shaft is connected to the stirring shaft inside the reaction tube via a coupling, synchronously transmitting the drive torque.

[0010] Furthermore, the reaction tube is a horizontal, high-temperature and pressure-resistant reactor. The reaction tube is made of high-temperature resistant material and has a high-pressure resistant structure to meet the reaction temperature and pressure requirements for material production.

[0011] Furthermore, a safety valve port is provided on the reaction tube.

[0012] Furthermore, the reaction tube is provided with an inlet and an outlet. The inlet includes one or more of a gas inlet, a liquid inlet, and a solid inlet, and the outlet includes one or more of a gas outlet, a liquid outlet, and a solid outlet. A flow valve is provided on the inlet, and a flow meter is provided on the outlet.

[0013] Furthermore, a temperature sensor and a pressure sensor are installed inside the reaction tube.

[0014] Furthermore, a heat exchange medium is provided within the jacket, including but not limited to heat transfer oil. The jacket heat exchange medium inlet is located near the reaction tube outlet, and the jacket heat exchange medium outlet is located near the reaction tube inlet.

[0015] Furthermore, there are multiple jackets arranged sequentially along the axial direction of the reaction tube, each controlling the temperature independently. The number of jackets is 2-6. The jackets can be independently controlled according to different reaction stages.

[0016] Furthermore, an insulation layer is provided on the outer side of the jacket.

[0017] Furthermore, the jacket is provided with fins to increase the heat dissipation area.

[0018] Furthermore, a gas distributor is axially installed at the bottom inner side of the reaction tube. The height of the gas distributor should be such that it does not interfere with the helical blades.

[0019] Furthermore, the gas distributor is connected to a cold hydrogen inlet. The feed gas (such as hydrogen) enters the reaction tube through the gas inlet and / or the gas distributor. The feed gas entering through the gas distributor agitates the material inside the reaction tube and facilitates heat transfer. When magnesium powder reacts with hydrogen to prepare magnesium hydride or when magnesium hydride is hydrolyzed, hydrogen enters the reaction tube through the gas inlet and the gas distributor.

[0020] Furthermore, the gas distributor includes a stainless steel pipe and a protective net. The protective net is located above the stainless steel pipe and can intercept dust to prevent dust from accumulating at the gas outlet. The lower edge of the stainless steel pipe is provided with a gas outlet.

[0021] Furthermore, the air outlet is tilted downwards, forming an angle of 30-60° (preferably 45°) with the vertical direction.

[0022] Furthermore, the air outlets are symmetrically arranged on both sides of the lower edge of the stainless steel pipe.

[0023] Furthermore, the reaction tube contains spheres, which are selected from steel balls, zirconium balls, ceramics, etc. These spheres can further break down the raw materials, increase heat transfer, prevent dead zones, and also serve as catalyst carriers.

[0024] Furthermore, the spiral blades of the screw conveyor unit are welded to the stirring shaft, and the pitch of the spiral blades is determined by the hydrogen storage / release time of the reactant and the total length of the reaction tube.

[0025] Furthermore, the stirring shaft is a hollow shaft, with rotary joints connecting the input and output ends of the hollow shaft. When the stirring shaft is a hollow shaft, a mechanical seal or a packing seal is selected as the sealing structure.

[0026] Furthermore, a heat exchange medium is circulated through the hollow shaft, including but not limited to heat transfer oil. The heat exchange medium can displace excess reaction heat generated inside the reaction tube, and can also provide a heat source medium during the hydrogen release stage of the reaction tube to heat the inside of the reaction tube and ensure the temperature uniformity of the entire reaction tube.

[0027] Furthermore, the spiral blade is a blade capable of propelling material forward, including but not limited to continuous spiral blades or single diamond-shaped blades.

[0028] When the screw conveyor unit of the present invention includes two stirring shafts and continuous spiral blades:

[0029] Furthermore, the shaft diameter of the continuous helical blades is set as close as possible to the inner wall of the reaction tube.

[0030] Furthermore, the stirring shaft fixed at the drive end of the continuous spiral blades is a hollow shaft, while the other end is a solid shaft, fixed to a thrust bearing. That is, the stirring shaft near the drive unit is a hollow shaft, and the other end is a solid shaft.

[0031] Furthermore, the reactor is also provided with a heat exchange structure, which includes a cooling box, a buffer chamber, and a tube bundle. The cooling box is located outside the reaction tube, the buffer chamber is located inside the reaction tube, and the tube bundle is fixedly installed inside the reaction tube in the hollow part of the continuous spiral blades.

[0032] Furthermore, the tube bundle is a U-shaped tube bundle. A partition is installed in the middle of the hollow shaft, dividing it into upper and lower parts. A partition is also installed in the middle of the buffer cavity, dividing it into upper and lower parts. The cooling box outlet is sequentially connected to the upper part of the hollow shaft, the upper part of the buffer cavity, and the inlet of the U-shaped tube bundle. The U-shaped tube bundle outlet is sequentially connected to the lower part of the buffer cavity, the lower part of the hollow shaft, and the cooling box inlet. The heat exchange medium enters the U-shaped tube bundle through the upper part of the hollow shaft and the upper part of the buffer cavity, and after heat exchange in the U-shaped tube bundle, it exits through the lower part of the buffer cavity and the lower part of the hollow shaft, achieving a circulating return of the cooling medium.

[0033] U-shaped tube bundles facilitate reflux, and because the inlet and outlet of the U-shaped tube are located on the same side, only one end needs to be fitted with a magnetic seal.

[0034] Furthermore, the cooling box is positioned between the sealing structure and the reaction pipe flange to ensure the safety of the sealing structure.

[0035] Furthermore, the hollow shaft is installed in the bearing support, the outer ring of the bearing rotates with the stirring shaft, and the inner ring is fixed in place by the bearing cap; the bearing cap has a hollow shaft opening in the middle, and the bolt holes on the bearing cap are bolted to the buffer cavity.

[0036] Furthermore, the number of reactors is 2-8, preferably 2-4.

[0037] Furthermore, when multiple reactors are connected in series, they are sequentially connected end-to-end. Taking two reactors connected in series as an example, the outlet of the first-stage reactor is connected to the inlet of the second-stage reactor. The reaction tube of the first-stage reactor is fixed above the reaction tube of the second-stage reactor and communicates with it. The second-stage reactor is equipped with legs to jointly support both reactors. The spiral blades of the second-stage reactor push the material in the opposite direction, effectively conveying the material from the first-stage reactor to the inlet of the second-stage reactor. Sufficient installation distance is maintained between the first-stage and second-stage reactors, and each reactor is equipped with an independent heating jacket structure to meet the temperature requirements of each reactor at different reaction stages.

[0038] Furthermore, when multiple reactors are connected in series, a pulverizing device is installed in the pipeline between adjacent reactors.

[0039] Furthermore, the crushing device is a high-speed shear head or a crushing valve. The material exiting the upper-stage reactor is crushed by the high-speed shear or crushing valve and then discharged to the lower-stage reactor. High-speed shearing can crush falling materials (e.g., magnesium powder) through high-speed shearing, refining the material, reducing particle size, accelerating the hydrogen storage rate, and increasing the hydrogen storage density. The crushing valve can shear and crush the material passing through the valve body through the relative movement of the stator and rotor within the valve.

[0040] Furthermore, when multiple reactors are connected in series, level gauges are installed in the pipelines between adjacent reactors. Taking two reactors connected in series as an example, to better monitor the loading and unloading between the two reactors, level gauges are installed in the pipeline between the first-stage reactor and the second-stage reactor, below the high-speed shear head. When the material level in the pipeline is higher than the set value, it is determined whether the stirring shafts of the first-stage and second-stage reactors are rotating. If stirring is still ongoing, it is preliminarily determined that the spiral stirring speed of the second-stage reactor is low, and the stirring shaft speed of the second-stage reactor needs to be increased to speed up the discharge and prevent material accumulation from affecting the entire reaction device. When it is determined that the stirring shaft of the second-stage reactor is not rotating, the first-stage reactor is immediately stopped to prevent the second-stage reactor from getting stuck in the entire second-stage reaction tube due to material accumulation.

[0041] Furthermore, the continuous reaction device applied to solid powder materials also includes a control unit, which is communicatively connected to a temperature sensor, a pressure sensor, a motor, a flow meter, a flow valve, and a level gauge.

[0042] Another objective of this invention is to disclose a continuous reaction method for solid powder materials, comprising the following steps: raw materials enter the reaction tube from the feed inlet, the drive unit drives the stirring shaft with helical blades to rotate, the helical blades rotate with the stirring shaft, and push the raw materials from the reactor feed inlet to the reactor outlet. During this process, the raw materials react under specified temperature, pressure and stirring speed. During the reaction, the raw materials are continuously cut and mixed, and the heat generated during the reaction is removed in time by the heat exchange device.

[0043] Furthermore, the continuous magnesium-based hydrogen storage material pyrolysis hydrogen production reaction conditions include: a temperature of 150-400℃, a pressure of 0.01-1.5MPa, and a stirring shaft speed of 20-40rpm.

[0044] Furthermore, the reaction conditions for hydrogen absorption by continuous magnesium-based hydrogen storage materials include: a temperature of 25-420℃, a pressure of 0.2-10MPa, and a stirring shaft speed of 5-100rpm.

[0045] Furthermore, the continuous magnesium-based hydrogen storage material hydrolysis hydrogen production reaction conditions include: temperature of 30-300℃, pressure of 0.1-2.0 MPa, and stirring shaft speed of 5-100 rpm.

[0046] Another object of the present invention is to disclose the use of a continuous reaction apparatus for solid powder materials in the fields of solid-solid reaction, liquid-solid reaction, gas-solid reaction, liquid-liquid reaction or gas-liquid reaction.

[0047] Furthermore, continuous reaction devices applied to solid powder materials are particularly suitable for hydrogen absorption by magnesium-based hydrogen storage materials (such as the preparation of magnesium hydride), hydrogen production through hydrolysis of magnesium-based hydrogen storage materials, hydrogen production through hydrolysis-pyrolysis coupling of magnesium-based hydrogen storage materials, hydrogen production through pyrolysis of magnesium-based hydrogen storage materials, or thermal storage using thermochemical thermal storage materials. Further, the thermal storage using thermochemical thermal storage materials includes carbonate thermal storage, hydroxide thermal storage, oxide thermal storage, or metal hydride thermal storage, etc.

[0048] Another objective of this invention is to disclose a continuous reaction system for solid powder materials, comprising a raw material silo, an isolation silo, the continuous reaction device for solid powder materials, and a collection tank connected in sequence.

[0049] Furthermore, there are multiple isolation chambers connected in parallel, meaning that the inlet and outlet of each isolation chamber are respectively connected to the raw material silo and the continuous reaction device used for solid powder materials. The isolation chamber is a key piece of equipment for raw material transportation, used for pressure regulation of the raw materials.

[0050] Furthermore, the isolation chamber is equipped with a heating device for heating the raw materials.

[0051] Furthermore, the isolation chamber is connected to an inflation tank and a first gas recovery tank, which are used to replenish or replace the pressure in the isolation chamber.

[0052] Furthermore, the continuous reaction device applied to solid powder materials is placed at an angle of 0 to 20 degrees in the horizontal direction, that is, the feed end of the reaction tube is higher than the discharge end, so as to ensure that the material is completely discharged under the action of stirring and gravity.

[0053] Furthermore, the collection tank is connected to a second gas recovery tank and a filling tank. The collection tank is used to hold the finished product (such as magnesium hydride), and the gas (such as hydrogen) in the collection tank is collected through the second gas recovery tank. The filling tank fills the collection tank with argon gas for inert gas protection.

[0054] Furthermore, a buffer tank is provided between the isolation chamber and the continuous reaction device applied to solid powder materials. When there are multiple isolation chambers, the multiple isolation chambers alternately feed and charge with hydrogen. In order to ensure that the material entering the reactor is uninterrupted, a buffer tank is added between the isolation chamber and the reactor to ensure that the feeding is uninterrupted during the switching process of multiple isolation chambers.

[0055] Furthermore, a cooling tank is provided between the continuous reaction device for solid powder materials and the collection tank.

[0056] Furthermore, the continuous reaction system applied to solid powder materials also includes a heat transfer oil furnace, wherein the heat transfer oil inlet and outlet are respectively connected to the outlet and inlet of the jacket.

[0057] Another objective of this invention is to disclose a continuous reaction method for solid powder materials, comprising the following steps: raw materials in a raw material silo are unloaded by gravity into an isolation chamber; the raw materials are heated and / or pressurized in the isolation chamber before entering a continuous reaction device for solid powder materials; and the reacted materials are collected and stored. This method enables the simultaneous completion of hydrogen storage and release reactions and unloading, thereby realizing a series of continuous production processes including loading, production, and unloading.

[0058] Furthermore, the two isolation chambers are connected in parallel to alternately supply raw materials to the continuous reaction device used for solid powder materials, thereby achieving continuous feeding.

[0059] Furthermore, the raw material enters the reaction tube through the feed inlet, and the drive unit drives the stirring shaft with spiral blades to rotate. The spiral blades rotate with the stirring shaft, pushing the raw material from the reactor feed inlet to the reactor outlet. During this process, the raw material reacts under specified temperature, pressure and stirring speed. The raw material is continuously cut and mixed during the reaction, and the heat generated during the reaction is removed in time by the heat exchange device.

[0060] Furthermore, the gas pipeline connected to the isolation chamber is pressurized or purged as needed by the reaction device.

[0061] Furthermore, the continuous reaction device applied to solid powder materials comprises multiple reactors connected in series and / or in parallel. Each reactor can individually control the reaction temperature and adjust the stirring speed according to the reaction stage to achieve the best mixing effect.

[0062] Another object of the present invention is to disclose the use of a continuous reaction system for solid powder materials in the fields of solid-solid reaction, liquid-solid reaction, gas-solid reaction, liquid-liquid reaction or gas-liquid reaction.

[0063] Furthermore, continuous reaction systems applied to solid powder materials are particularly suitable for hydrogen absorption by magnesium-based hydrogen storage materials (such as the preparation of magnesium hydride), hydrogen production by hydrolysis of magnesium-based hydrogen storage materials, hydrogen production by hydrolysis-pyrolysis coupling of magnesium-based hydrogen storage materials, hydrogen production by pyrolysis of magnesium-based hydrogen storage materials, or thermal storage in the field of thermochemical thermal storage materials.

[0064] Furthermore, the thermochemical thermal storage material includes carbonate thermal storage, hydroxide thermal storage, oxide thermal storage, or metal hydride thermal storage, etc.

[0065] This invention relates to a continuous reaction apparatus, method, and application for solid powder materials, and has the following advantages compared with existing technologies:

[0066] 1) High-efficiency heat exchange;

[0067] The reactor used in this invention is a high-efficiency heat exchange reactor integrating multiple heat transfer structures. The reaction tube is a horizontal tubular structure with a large specific surface area, a large heat transfer area per unit volume, and high heat transfer efficiency. In addition to introducing hydrogen through the reaction gas source inlet, a gas (such as hydrogen) distributor is also installed at the bottom of the reaction tube. This distributor not only purges and loosens the material (such as magnesium powder) on the reactor wall but also allows hydrogen to pass through the material layer from bottom to top, enhancing the heat transfer reaction. When the reaction is violently exothermic, a lower-temperature gas (cold hydrogen) can be introduced through the gas distributor to effectively replace the heat. Inside the reaction tube, the stirring spiral blades continuously tumble and mix the material during the reaction, effectively dissipating the heat from the reaction tube wall. A heat transfer oil jacket is installed outside the reaction tube, and multiple fins are welded to the outer wall of the reaction tube to enhance the heat transfer of the heat from the heat transfer oil to the reaction tube. The stirring shaft can be a hollow shaft, and a heat exchange medium can be introduced inside to homogenize the entire temperature field.

[0068] 2) Applicable to reactions with different reaction times;

[0069] The driving device used in this invention consists of a motor and a reducer. The speed of the stirring shaft can be adjusted by a frequency converter, so the material conveying time in the reaction tube is adjustable, which is suitable for reactions of various reactants with different reaction times.

[0070] 3) Multiple reactors can be freely combined in series and / or parallel;

[0071] Multiple reactors can be freely combined in series and / or parallel. Series connection allows for adjustment of reaction time, while parallel connection allows for adjustment of throughput. The outlet of the upper reactor is connected to the inlet of the lower reactor to achieve series connection, which is suitable for materials with long reaction times. The feeding system connects to the feed inlets of multiple reactors to achieve parallel connection, ensuring large-scale material throughput.

[0072] 4) Wide range of applications;

[0073] This invention has a wide range of applications in continuous reaction devices for solid powder materials, and is suitable for material reactions in various phases such as solid-solid, solid-liquid, liquid-liquid, gas-liquid, and gas-solid.

[0074] 5) Independent temperature control;

[0075] When multiple reactors are connected in series or in parallel, each reactor is independently equipped with a heat transfer oil jacket. The temperature of the reaction tube of each reactor can be independently controlled according to the process requirements of the reaction process, so as to meet the different temperature and pressure requirements of different stages of the reaction.

[0076] 6) Advantages of horizontal containers;

[0077] The reaction tube of this invention is a horizontal reaction vessel, which has a smaller height-to-diameter ratio than a vertical reaction tube of the same volume. After the hydrogen gas is introduced, the pressure drop is small and the gas loss is small, which is beneficial to the rapid reaction of materials and the expansion of product volume.

[0078] 7) Skid-mounted design takes up little space and is easy to scale up;

[0079] Multiple reactors can be connected in series or in parallel, with similar overall structural dimensions, facilitating skid-mounted design and requiring minimal footprint in various engineering applications. Furthermore, they are easily scaled up for large-scale production.

[0080] 8) Different screw types process different types of materials, resulting in a wide range of raw materials that can be processed;

[0081] The reactor of this invention can employ various blade forms, such as continuous spiral blades or single diamond-shaped blades, to push materials in different ways, including plug flow and turbulent mixtures. The reactor is suitable for various materials and reaction conditions requiring different conditions.

[0082] 9) The high-speed shear head removes the oxide layer or magnesium hydride from the surface of magnesium hydride, shortening the reaction time and increasing the hydrogen storage capacity;

[0083] The present invention provides a high-speed shear head in the pipeline between adjacent reactors. The high-speed shear head shears and crushes the material discharged from the outlet, which not only refines the material, but also effectively disperses the material, making it easier for the next stage reactor to uniformly transport the material.

[0084] 10) A sphere is installed inside the reaction tube;

[0085] This invention allows for the addition of spheres within the reaction tube. These spheres move along with the helical blades within the tube, and their rising and falling motion during this movement acts as a crushing and breaking agent for the materials. Furthermore, the spheres can be coated with catalyst components as needed for the material reaction, dynamically participating in the reaction process. As good conductors of heat, the spheres absorb heat within the reaction tube and conduct it during their movement.

[0086] 12) Continuous production: Magnesium powder isolation silo + continuous reaction device (plug flow) applied to solid powder materials;

[0087] This invention relates to a continuous reaction system for solid powder materials. Raw materials are transported from a raw material silo to a reaction apparatus via an isolation chamber, which is a key component for continuous raw material transport. The raw materials are heated and pressurized within the isolation chamber before being transported to the reaction apparatus. Two isolation chambers are connected in parallel with the reaction apparatus, alternately supplying materials to achieve continuous feeding. After feeding into the isolation chambers, the reaction apparatus activates its stirring device under positive pressure. The raw materials react at specified temperature, pressure, and stirring speed. The stirring shaft speed is controlled within the reaction apparatus, causing the spiral blades to push the raw materials horizontally from the inlet to the outlet. Hydrogen storage, release, and unloading are completed simultaneously, thus realizing a series of continuous production processes including loading, production, and unloading. Attached Figure Description

[0088] Figure 1 This is a schematic diagram of the continuous reaction apparatus for solid powder materials applied in Example 1;

[0089] Figure 2 This is a schematic diagram of the continuous reaction apparatus for solid powder materials applied in Example 2;

[0090] Figure 3 This is a schematic cross-sectional view of the reaction tube in Example 2;

[0091] Figure 4 This is a schematic diagram of the continuous reaction system for solid powder materials applied in Example 2;

[0092] Figure 5 This is a schematic diagram of the continuous reaction apparatus for solid powder materials applied in Example 6. Detailed Implementation

[0093] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of this application, and not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of this application without creative effort are within the scope of protection of this application.

[0094] In the description of this application, it should be noted that, unless otherwise expressly specified and limited, the terms "connected" and "linked" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection, an electrical connection, or a connection that allows for mutual communication; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two elements or the interaction between two elements. Those skilled in the art can understand the specific meaning of the above terms in this application according to the specific circumstances. In the description of this application, "multiple" means two or more, unless otherwise expressly and specifically limited. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, features defined with "first" and "second" may explicitly or implicitly include one or more features.

[0095] The following disclosure provides many different implementations or examples for carrying out different structures of this application. To simplify the disclosure of this application, the components and arrangements of specific examples are described below. Of course, these are merely examples and are not intended to limit this application.

[0096] Example 1: Hydrogen production by magnesium hydride pyrolysis

[0097] This embodiment discloses a continuous reaction apparatus for solid powder materials, comprising one or more reactors, the specific number of which depends on the gas demand. In this embodiment, there are two reactors connected in parallel.

[0098] The reactor is as follows Figure 1 As shown, it includes a drive unit, a screw conveying unit, and a reaction tube; the screw conveying unit includes a stirring shaft 9 and spiral blades 8 disposed on the stirring shaft; the stirring shaft 9 passes through the reaction tube; the drive unit is located outside the reaction tube and is connected to the stirring shaft 9, driving the stirring shaft 9 to rotate; the reaction tube is covered by a jacket 6.

[0099] The drive unit includes a motor 1, a reducer 2, and a magnetic coupler 3. The motor 1 is connected to the stirring shaft 9 via the reducer 2 and the magnetic coupler 3, driving the stirring shaft 9 to rotate. The motor 1 provides power, and the reducer 2 amplifies the output torque of the motor before transmitting it to the magnetic coupler 3. The inner magnet of the magnetic coupler 3 is connected to the stirring shaft 9, and the outer magnet is connected to the output shaft of the reducer 2. The output shaft of the reducer 2 is connected to the stirring shaft 9 inside the reactor via a coupling, synchronously transmitting the drive torque.

[0100] The reaction tube is a horizontal, high-temperature, and pressure-resistant reactor. It is made of high-temperature resistant material and has a high-pressure resistant structure to meet the reaction temperature and pressure requirements for material production. A solid feed inlet is located at one end of the reaction tube, through which magnesium hydride enters the reactor. A gas outlet is located at the top, and a solid outlet is located at the bottom of the other end of the reactor. The solid product obtained from the pyrolysis of magnesium hydride is discharged through the solid outlet, and hydrogen gas is discharged through the gas outlet. A flow valve is installed at the solid feed inlet, and a flow meter is installed at the gas outlet. Temperature and pressure sensors are installed inside the reaction tube. A safety valve is also installed on the reaction tube.

[0101] The jacket 6 contains a heat exchange medium, which in this embodiment is heat transfer oil. The heat exchange medium inlet of the jacket 6 is located near the outlet of the reaction tube, and the heat exchange medium outlet of the jacket 6 is located near the inlet of the reaction tube. An insulation layer 4 is provided on the outside of the jacket 6. Fins are provided inside the jacket 6 to increase the heat exchange area.

[0102] The reaction tube is equipped with steel balls, which can further crush the raw materials, increase heat transfer, prevent dead zones, and also serve as a catalyst carrier.

[0103] The spiral blades 8 of the screw conveyor unit are welded to the stirring shaft. The pitch of the spiral blades is determined by the hydrogen storage / release time of the reactants and the total length of the reaction tube. The spiral blades 8 are either continuous spiral blades or single diamond-shaped blades.

[0104] The continuous reaction device for solid powder materials also includes a control unit, which is communicatively connected to a temperature sensor, a pressure sensor, a motor, a flow meter, a flow valve, and a level gauge.

[0105] When the magnesium-based solid hydrogen storage material releases hydrogen, in this embodiment, the hydrogen replacement is completed in the continuous reaction device applied to solid powder materials, and the temperature is preheated to 250°C using the heat transfer oil in the jacket. The valve between the magnesium powder isolation chamber and the feed inlet of the continuous reaction device applied to solid powder materials is opened, and the atmospheric pressure hydrogenated magnesium powder chamber discharges the powder through the isolation chamber into the continuous reaction device applied to solid powder materials.

[0106] The motor is started, driving the reducer and magnetic coupler, which in turn starts the screw conveyor unit. As the stirring shaft moves, the spiral blades push the material and convey it to the reactor outlet. Magnesium powder reacts at a temperature of 340℃, a pressure of 0.3MPa, and a stirring speed of 20rpm. The stirring shaft speed inside the reactor is controlled so that the spiral blades push the magnesium hydride powder horizontally from the feed inlet of the reaction tube to the discharge outlet.

[0107] During pyrolysis, magnesium hydride powder is discharged from the silo by gravity into the reaction unit under constant pressure. The external heat transfer oil system then provides heat to the continuous reaction unit used for solid powder materials. Magnesium hydride has a low thermal conductivity, a high length-to-diameter ratio in the reaction tubes, a large specific surface area, and high thermal efficiency, facilitating heat transfer from the external heat transfer oil into the reaction unit. Furthermore, the spiral blades inside the reaction unit continuously agitate the reaction, transferring heat from the heat transfer oil on the reaction tube walls through the magnesium hydride powder, resulting in a more uniform temperature field throughout the reaction unit. The discharge rate can be controlled by adjusting the stirring speed of the reaction unit according to the reaction state.

[0108] When the hydrogen demand is low, one reactor can be started. When the hydrogen demand is high, multiple reactors can be connected in parallel, and the stroke rate of each reactor can be increased. As the screw propels the material, the hydrogen release reaction and unloading are completed simultaneously, achieving continuous unloading after hydrogen release.

[0109] Example 2: Preparation of magnesium hydride

[0110] This embodiment discloses a continuous reaction system for solid powder materials, the structure of which is as follows: Figure 4 As shown, the system includes a raw material silo 101, an isolation chamber 102, an aeration tank 103, a first gas recovery tank 104, a buffer tank 105, a thermal oil heater 106, a continuous reaction device 107 for solid powder materials, a second gas recovery tank 108, a cooling tank 109, and a collection tank 110. The raw material silo 101, isolation chamber 102, buffer tank 105, continuous reaction device 107 for solid powder materials, cooling tank 109, and collection tank 110 are connected sequentially. The inlet and outlet of the thermal oil heater 106 are respectively connected to the outlet and inlet of the jacket 6 of the continuous reaction device 107 for solid powder materials. The collection tank 110 is also connected to the second gas recovery tank 108 and the aeration tank 103.

[0111] In this embodiment, there are two isolation chambers 102 connected in parallel. The inlet and outlet of each isolation chamber 102 are respectively connected to the raw material chamber 101 and the continuous reaction device 107 for solid powder materials. The isolation chamber is used to regulate the pressure of the raw material. A heating device is also provided in each isolation chamber 102 for heating the raw material. Each isolation chamber 102 is individually connected to an inflation tank 103 and a first gas recovery tank 104 for pressure replenishment or replacement.

[0112] The continuous reaction device applied to solid powder materials, such as Figure 2 As shown, the reactor comprises two reactors connected in series: a primary reactor 7 and a secondary reactor 10. Each reactor includes a drive unit, a screw conveyor unit, and a reaction tube; the screw conveyor unit includes a stirring shaft 9 and helical blades 8 mounted on the stirring shaft, with the stirring shaft 9 passing through the reaction tube; the drive unit is located outside the reaction tube and connected to the stirring shaft 9, driving the stirring shaft 9 to rotate; the reaction tube is fitted with a jacket 6.

[0113] The drive unit includes a motor 1, a reducer 2, and a mechanical seal. The motor is connected to the stirring shaft via the reducer, and the mechanical seal is used to seal between the reducer and the reaction tube. The output shaft of the reducer 2 is connected to the stirring shaft 9 inside the reaction tube via a coupling to synchronously transmit the drive torque.

[0114] The reaction tube is a horizontal, high-temperature and pressure-resistant reactor. It is made of high-temperature resistant material and has a high-pressure resistant structure to meet the reaction temperature and pressure requirements for material production. The first-stage reactor 7 has a solid inlet 16 at one end and a solid conveying port 17 and a gas outlet 15 at the other end. The second-stage reactor 10 has a solid outlet 18 near the solid inlet 16, a gas inlet 14 in the middle, and a gas outlet 15 at the other end. Flow valves are installed in all the inlet pipes, and flow meters are installed in all the outlet pipes. Temperature and pressure sensors are installed inside the reaction tube. A safety valve is also installed on the reaction tube.

[0115] The jacket 6 contains a heat exchange medium, including but not limited to heat transfer oil. The heat exchange medium inlet of the jacket 6 is located near the outlet of the reaction tube, and the heat exchange medium outlet of the jacket 6 is located near the inlet of the reaction tube. An insulation layer 4 is provided on the outer side of the jacket 6. Fins are provided inside the jacket 6 to increase the heat dissipation area.

[0116] like Figure 3As shown, a gas distributor is axially laid on the bottom inner side of the reaction tube 19. The height of the gas distributor should be such that it does not interfere with the spiral blades 8. In this embodiment, the gas distributor includes two 6mm diameter stainless steel tubes 11 and a protective net 12. The protective net is placed above the stainless steel tubes and can intercept dust to prevent dust accumulation at the gas outlet. Gas outlets are symmetrically arranged on both sides of the lower edge of the stainless steel tubes, and the gas outlets are inclined downwards at a 45° angle to the vertical direction. The gas distributor not only purges and loosens the magnesium hydride powder on the reactor wall, but also allows hydrogen gas to pass through the magnesium powder layer from bottom to top for cooling.

[0117] The spiral blades 8 of the screw conveyor unit are welded to the stirring shaft 9. The pitch of the spiral blades 8 is determined by the hydrogen storage / release time of the reactants and the total length of the reaction tube. The stirring shaft 9 is a hollow shaft, with rotary joints connected to its input and output ends. A heat exchange medium flows through the hollow shaft, including but not limited to heat transfer oil. The heat exchange medium can displace excess reaction heat generated in the reaction tube and can also provide a heat source during the hydrogen release stage of the reaction tube, heating the inside of the reaction tube and ensuring temperature uniformity throughout the reaction tube. The spiral blades 8 are either continuous spiral blades or single diamond-shaped blades.

[0118] The reaction tube of the first-stage reactor is fixed above the reaction tube of the second-stage reactor. The solid conveying port 17 of the first-stage reactor 7 is connected to the feed inlet of the second-stage reactor 10. The second-stage reactor is equipped with support legs to jointly support both reactors. The spiral blades of the second-stage reactor push the material in the opposite direction, effectively conveying the material from the first-stage reactor to the feed inlet of the second-stage reactor. Sufficient installation distance is maintained between the first-stage and second-stage reactors. Each reactor is equipped with an independent heating jacket structure to meet the temperature requirements of each reactor at different reaction stages.

[0119] A pulverizing device is installed in the pipeline between the two reactors. The pulverizing device is a high-speed shear head 13. The material in the solid conveying port 17 of the first-stage reactor 7 is crushed by high-speed shearing or a crushing valve and then discharged into the second-stage reactor 10. High-speed shearing can crush the falling magnesium powder material through high-speed shearing, thereby refining the material, cutting and pulverizing the particle size, accelerating the hydrogen storage rate, and increasing the hydrogen storage density.

[0120] To better monitor the loading and unloading between the two-stage reactors, a level gauge is installed in the pipeline between the first-stage and second-stage reactors, below the high-speed shear line. When the detected material level in the pipeline is higher than the set value, it is determined whether the stirring shafts of the first-stage and second-stage reactors are rotating. If stirring is still ongoing, it is preliminarily determined that the spiral stirring speed of the second-stage reactor is low, and the stirring shaft speed of the second-stage reactor needs to be increased to accelerate the discharge and prevent material accumulation from affecting the entire reaction device. If it is determined that the stirring shaft of the second-stage reactor is not rotating, the first-stage reactor is immediately shut down to prevent the second-stage reactor from becoming stuck due to material accumulation within the entire second-stage reaction tube.

[0121] The continuous reaction device for solid powder materials also includes a control unit, which is communicatively connected to a temperature sensor, a pressure sensor, a motor, a flow meter, a flow valve, and a level gauge.

[0122] Applying this embodiment to a continuous reaction system for solid powder materials for the preparation of magnesium hydride includes the following steps:

[0123] The method for preparing magnesium hydride using the above reaction system is as follows: A raw material silo 101 (atmospheric pressure magnesium powder silo) is connected to two isolation silos 102. Under a nitrogen protective atmosphere, after air replacement is completed in both isolation silos 102, the ball valve between the atmospheric pressure magnesium powder silo and the isolation silos 102 is opened for material transport. When one isolation silo 102 is full, the ball valve between the two silos is closed, and the hydrogen inlet valve of the isolation silo 102 is opened. Hydrogen is introduced into the isolation silo 102 through the gas filling tank 103 until the pressure is 0.5 MPa higher than the operating pressure of the reaction apparatus, then the hydrogen valve is closed. The other isolation silo 102 undergoes the same operation. The ball valve between one of the isolation silos 102 and the buffer tank 105 is opened, and the magnesium powder from the isolation silo is loaded into the buffer tank 105. The pressure in the buffer tank is slightly higher than that in the reactor by 0.2 MPa. The magnesium powder is continuously transported from the buffer tank 105 to the continuous reaction apparatus for solid powder materials by gravity and pressure difference. In a continuous reaction device for solid powder materials, the material undergoes a hydrogen storage reaction under certain temperature and pressure. After the reaction is completed, the material enters the cooling tank 109 through the outlet of the reaction device. When a certain cooling temperature is reached, the magnesium powder can be sealed into the collection tank 110.

[0124] In the preparation of magnesium-based solid hydrogen storage materials, before releasing magnesium powder from the atmospheric pressure magnesium powder silo to the isolation chamber, the inert protective gas inside the isolation chamber is vacuum-evacuated and discharged. After discharge, hydrogen gas is introduced into the isolation chamber at a pressure higher than that inside the reaction device. The continuous reaction device for solid powder materials completes the hydrogen replacement and preheats the powder to 150°C using heat transfer oil in the jacket. Initially, the temperature of the heat transfer oil is controlled to allow a core-shell-like structure to form on the surface of the magnesium powder, preventing caking and ensuring subsequent hydrogen storage. The raw material inlet valve between the isolation chamber and the continuous reaction device for solid powder materials is opened, and the magnesium powder is fed into the continuous reaction device for solid powder materials under the combined action of gravity and pressure difference. After the reaction, the material is cooled, collected, and stored.

[0125] When a continuous reaction apparatus for solid powder materials includes a single reactor, the temperature range is controlled between 240 and 420°C depending on the reaction stage. When the apparatus includes multiple reactors connected in series, the temperature of each reactor can be individually controlled according to the preheating and enhanced reaction sections. The first-stage reactor can use a jacketed heating medium to preheat the reaction tubes, with the preheating temperature controlled between 200 and 220°C. After reaching the preheating temperature, the material enters the second-stage reactor through the outlet of the first-stage reactor. The material in the second-stage reactor, having been preheated by the first-stage reactor, has reached the reaction temperature. During the hydrogen storage reaction, the reaction continuously releases heat. The external jacket of the second-stage reactor can use a heat exchange medium to effectively remove heat, controlling the temperature of the enhanced reaction section between 300 and 420°C.

[0126] Each reactor can be configured with different helical blade pitches and stirring speeds depending on the reaction section and temperature. This dual independent setting of temperature and stirring allows for better adaptation to reaction requirements and achieves optimal hydrogen storage performance.

[0127] Specifically, the reaction process in the continuous reaction device for solid powder materials is as follows: The motor is started, driving the reducer and magnetic coupler, which in turn starts the screw conveyor unit. As the stirring shaft moves, the spiral blades push the material, conveying it to the reactor outlet. While the magnesium powder moves spirally with the spiral blades, hydrogen gas is introduced into the reaction gas inlet on the reaction tube. Simultaneously, a hydrogen distributor at the bottom of the reaction tube continuously delivers cold hydrogen into the reaction tube. The horizontal reaction tube has a small diameter, resulting in low hydrogen resistance. The packing material in the reaction tube is controllable, and sufficient gas phase space is reserved to facilitate hydrogen flow within the tube. The magnesium powder reacts at a temperature of 300℃, a pressure of 3.0 MPa, and a stirring speed of 20 rpm. The stirring shaft speed is controlled within the reactor to allow the spiral blades to push the magnesium powder horizontally from the reaction tube inlet to the reaction tube outlet. The discharge pipe of the first-stage reactor connects to the inlet of the second-stage reactor. Before the material flows through the discharge pipe, the high-speed shear head or crushing valve of the discharge pipe is activated to shear and crush the flowing material before it falls into the inlet of the second-stage reactor. The second-stage reactor reverses the material flow, and the magnesium powder is pulverized within the reaction tube, accelerating the hydrogen storage rate and increasing the hydrogen storage density. The heat transfer oil temperature of the second-stage reactor is set to 300℃ to complete hydrogenation under high temperature and high pressure. As the screw propels the material, the hydrogen storage reaction and unloading are completed simultaneously, thus realizing loading and unloading and continuous production.

[0128] Example 3: Hydrolysis of magnesium hydride

[0129] The continuous reaction system for solid powder materials in this embodiment is basically the same as that in Embodiment 2. The difference is that the continuous reaction device for solid powder materials is placed at a 20-degree angle to the horizontal direction, that is, the feed end of the reaction tube is higher than the discharge end, so as to ensure that the material is completely discharged under the action of stirring and gravity.

[0130] During the hydrolysis of magnesium-based solid hydrogen storage materials, the reaction apparatus first completes hydrogen replacement. The raw material inlet valves of the magnesium powder isolation chamber 102 and the continuous reaction apparatus 107 (used for solid powder materials) are then opened. The raw material chamber 101 (also called the atmospheric pressure magnesium hydride powder chamber) releases the powder through the magnesium powder isolation chamber 102 into the continuous reaction apparatus 107. Water is then introduced into the reactor, and the magnesium hydride hydrolyzes to produce hydrogen gas, releasing a large amount of heat energy. The magnesium hydride hydrolysis reaction conditions are 30 degrees Celsius, 20 rpm, and 1.0 MPa.

[0131] In addition, the stirring shaft 9 is a hollow shaft, with heat exchange medium introduced into its inner cavity. Rotary joints 5 are connected to both ends of the hollow shaft. One end of each rotary joint connects to the hollow shaft, and the other end connects to the heat exchange medium inlet pipeline. The rotary joint 5 is a continuous type, with one end connected to the hollow shaft first, then to the reducer output end, and the other end connected to the heat exchange medium outlet pipeline. When the hydrolysis reaction releases a large amount of heat, one pipeline of the heat transfer oil system is used to connect to one end of the rotary joint. After the reaction starts, both pipelines of the heat transfer oil system are cooled, the outer jacket of the reaction tube is cooled, and the heat transfer oil in the hollow shaft of the stirring shaft cools, achieving simultaneous internal and external cooling of the reaction tube. Temperature detection of the inner wall of the reaction tube ensures that the hydrolysis reaction remains at the optimal reaction temperature. The magnesium hydride produced by the reaction moves with the material driven by the screw, and the hydrogen release reaction and unloading are completed simultaneously, thus realizing loading and unloading and continuous production.

[0132] Example 4: Hydrothermal Coupling of Magnesium-Based Solid Hydrogen Storage Materials

[0133] The continuous reaction apparatus for solid powder materials disclosed in Examples 1 and 2 is also suitable for coupled hydrolysis and pyrolysis reactions. The magnesium-based solid hydrogen storage material reacts with water, releasing a large amount of heat, which can be used to pyrolyze magnesium hydride to produce hydrogen. A motor is connected to a reducer, which is a two-end type. One end is connected to a rotary joint, and the other end is connected to a coupling. The coupling connects to the reactor stirring shaft, which is a hollow shaft with a layer of stainless steel wire mesh inside. Magnesium hydride fills the hollow shaft. After the fixed end of the hollow shaft is fixed by bearings, a bearing cap is led out and connected to the cooling water outlet pipeline. The rotary joint at the reducer end is connected to the cooling water inlet pipeline. A control valve is installed on the cooling water inlet pipeline to strictly control the amount of water entering the hollow shaft. The reaction process and the supply of reaction heat are controlled by controlling the water flow. Multiple temperature measuring points are set inside the reaction tube to monitor the temperature in real time. When the temperature exceeds the pyrolysis temperature, the cooling of the external jacket of the reaction tube with heat transfer oil and the cooling water inside the hollow shaft are increased to strictly control the hydrolysis temperature.

[0134] Example 5: Coupling of calcium-based thermal storage materials

[0135] The continuous reaction apparatus for solid powder materials disclosed in Examples 1 and 2 is also suitable for calcium-based coupling. The magnesium hydride hydrogen storage process within the reaction apparatus is exothermic, and the reaction heat should be promptly removed from the container to prevent magnesium hydride caking due to high temperatures. Heat exchange is achieved using heat transfer oil within the reaction apparatus jacket; this heat is a high-grade heat source and easily collected. The heat transfer oil outlet is connected to a calcium-based material heat storage device. Calcium carbonate or calcium hydroxide absorbs heat during the calcination and decomposition process and stores it as chemical energy. During the magnesium hydride hydrogen release process, the reaction product calcium oxide releases heat through carbonation or hydration reactions. Repeating this reaction multiple times achieves heat storage and release cycling during the magnesium hydride hydrogen storage and release process.

[0136] In Examples 2 and 3, the hollow shaft serves only as a channel for heating or heat extraction media. In Examples 4 and 5, the hollow shaft functions as a small reaction chamber, providing heat for the hydrolysis reaction and calcium-based coupled heat storage and release.

[0137] Example 6:

[0138] This embodiment discloses a continuous reaction device for solid powder materials, whose structure is basically the same as that of Embodiment 1, except that the screw conveying unit includes two stirring shafts and continuous spiral blades disposed between the two stirring shafts, and the two stirring shafts are respectively fixed at both ends inside the reaction tube; as shown Figure 5 As shown.

[0139] The shaft diameter of the continuous spiral blade 23 is set as close as possible to the inner wall of the reaction tube.

[0140] The stirring shaft fixed at the drive end of the continuous spiral blades is a hollow shaft, while the other end is a solid shaft, fixed to a thrust bearing. That is, the stirring shaft closer to the drive unit is a hollow shaft, and the other end is a solid shaft.

[0141] The reactor also includes a heat exchange structure comprising a cooling box 24, a buffer chamber 20, and a U-shaped tube bundle 21. The cooling box 24 is located outside the reaction tube. A partition 22 divides the hollow shaft into upper and lower parts. The buffer chamber 20 is located inside the reaction tube and is also divided into upper and lower parts by the partition 22. The U-shaped tube bundle 21 is fixedly inserted into the hollow portion of the continuous spiral blades inside the reaction tube. The cooling box outlet is sequentially connected to the upper part of the hollow shaft, the upper part of the buffer chamber, and the inlet of the U-shaped tube bundle. The U-shaped tube bundle outlet is sequentially connected to the lower part of the buffer chamber, the lower part of the hollow shaft, and the cooling box inlet of the cooling box. The heat exchange medium enters the U-shaped tube bundle through the upper part of the hollow shaft and the upper part of the buffer chamber, and exits through the lower part of the buffer chamber and the lower part of the hollow shaft after heat exchange in the U-shaped tube bundle, thus achieving a circulating return of the cooling medium.

[0142] The drive unit includes a motor, a reducer, and a sealing structure. The motor is connected to the stirring shaft through the reducer and drives the stirring shaft to rotate. The sealing structure is used to seal between the reducer and the reaction tube.

[0143] The cooling box is located between the sealing structure and the reaction pipe flange to ensure the safety of the sealing structure.

[0144] The hollow shaft is installed in the bearing support. The outer ring of the bearing rotates with the stirring shaft, while the inner ring is fixed in place by the bearing cap. The bearing cap has a hollow shaft opening in the middle, and the bolt holes on the bearing cap are bolted to the buffer cavity.

[0145] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A continuous reaction apparatus for solid powder materials, characterized in that, It includes one or more reactors, and when there are multiple reactors, the multiple reactors are connected in parallel and / or in series. The reactor includes a drive unit, a screw conveyor unit and a reaction tube. The screw conveying unit includes a stirring shaft and helical blades disposed on the stirring shaft, the stirring shaft passing through the reaction tube; or, the screw conveying unit includes two stirring shafts and continuous helical blades disposed between the two stirring shafts, the two stirring shafts being fixed at both ends inside the reaction tube respectively; The drive unit is located outside the reaction tube and is connected to the stirring shaft to drive the stirring shaft to rotate; the reaction tube is fitted with a jacket.

2. The continuous reaction apparatus for solid powder materials according to claim 1, characterized in that, The drive unit includes a motor, a reducer, and a sealing structure. The motor is connected to the stirring shaft through the reducer and drives the stirring shaft to rotate. The sealing structure is used to seal between the reducer and the reaction tube.

3. The continuous reaction apparatus for solid powder materials according to claim 1 or 2, characterized in that, The reaction tube is a horizontal high-temperature and pressure-resistant reaction vessel; And / or, the reaction tube is provided with a safety valve port; And / or, the reaction tube is provided with an inlet and an outlet, the inlet including one or more of a gas inlet, a liquid inlet and a solid inlet, and the outlet including one or more of a gas outlet, a liquid outlet and a solid outlet; a flow valve is provided on the inlet and a flow meter is provided on the outlet; And / or, a temperature sensor and a pressure sensor are provided inside the reaction tube; And / or, the jacket is provided with a heat exchange medium, preferably heat transfer oil; And / or, there are multiple jackets, and the multiple jackets are arranged sequentially along the axial direction of the reaction tube; And / or, an insulation layer is provided on the outside of the jacket; And / or, the jacket is provided with fins; And / or, a gas distributor is laid axially at the bottom of the inner side of the reaction tube. Preferably, the gas distributor includes a stainless steel tube and a protective net, with the protective net covering the stainless steel tube. The lower edge of the stainless steel tube is provided with a gas outlet, which is inclined downward at an angle of 30-60° to the vertical direction. And / or, a sphere is provided inside the reaction tube; And / or, the stirring shaft is a hollow shaft, with a rotary joint connecting the inlet and outlet ends of the hollow shaft; a heat exchange medium flows through the hollow shaft, preferably heat transfer oil; And / or, the spiral blade is a blade capable of propelling material forward; preferably, the spiral blade is a continuous spiral blade or a single diamond-shaped blade. When the screw conveyor unit of the present invention includes two stirring shafts and continuous spiral blades: And / or, the shaft diameter of the continuous helical blades is set as close as possible to the inner wall of the reaction tube; And / or, the stirring shaft fixed at the drive end of the continuous spiral blade is a hollow shaft, and the other end is a solid shaft, fixed on a thrust bearing; And / or, the reactor is further provided with a heat exchange structure, the heat exchange structure including a cooling box, a buffer chamber and a tube bundle, the cooling box being located outside the reaction tube, the buffer chamber being located inside the reaction tube, and the tube bundle being fixedly installed inside the reaction tube and in the hollow part of the continuous spiral blades; preferably, the tube bundle is a U-shaped tube bundle, a partition is provided in the middle of the hollow shaft to divide the hollow shaft into upper and lower parts, a partition is provided in the middle of the buffer chamber to divide the buffer chamber into upper and lower parts, the outlet of the cooling box is sequentially connected to the upper part of the hollow shaft, the upper part of the buffer chamber and the inlet of the U-shaped tube bundle, and the outlet of the U-shaped tube bundle is sequentially connected to the lower part of the buffer chamber, the lower part of the hollow shaft and the cooling box inlet of the cooling box; And / or, the cooling box is disposed between the sealing structure and the reaction tube flange; And / or, the hollow shaft is installed in the bearing support, the outer ring of the bearing rotates with the stirring shaft, and the inner ring is fixed in place by the bearing cap; the bearing cap has a hollow shaft opening in the middle, and the bolt holes on the bearing cap are bolted to the buffer cavity.

4. The continuous reaction apparatus for solid powder materials according to any one of claims 1 to 3, characterized in that, When multiple reactors are connected in series, a crushing device is installed in the pipeline between adjacent reactors. Preferably, the crushing device is a high-speed shear head or a crushing valve. And / or, when multiple reactors are connected in series, level gauges are installed in the pipelines between adjacent reactors.

5. A continuous reaction method for solid powder materials, characterized in that, Includes the following steps: The drive unit drives the stirring shaft with spiral blades to rotate, pushing the raw materials from the reactor inlet to the reactor outlet. During the reaction, the raw materials are continuously cut and mixed, and the heat generated during the reaction is removed in time by the heat exchange device.

6. The continuous reaction method for solid powder materials according to claim 5, characterized in that, The continuous pyrolysis hydrogen production reaction conditions for magnesium-based hydrogen storage materials include: temperature of 150-400℃, pressure of 0.01-1.5MPa, and stirring shaft speed of 20-40rpm. And / or, the reaction conditions for continuous magnesium-based hydrogen storage material to absorb hydrogen include: temperature of 25-420℃, pressure of 0.2-10MPa, and stirring shaft speed of 5-100rpm; And / or, the continuous magnesium-based hydrogen storage material hydrolysis hydrogen production reaction conditions include: temperature of 30-300℃, pressure of 0.1-2.0Mpa, and stirring shaft speed of 5-100rpm.

7. A continuous reaction system for solid powder materials, characterized in that, It includes a raw material silo, an isolation silo, a continuous reaction apparatus for solid powder materials as described in any one of claims 1-4, and a collection tank, which are connected in sequence.

8. The continuous reaction system for solid powder materials according to claim 7, characterized in that, The isolation chambers are multiple, and the multiple isolation chambers are connected in parallel; And / or, a heating device is provided inside the isolation chamber; And / or, the isolation chamber is connected to an inflation tank and a first gas recovery tank; And / or, the continuous reaction device applied to solid powder materials is placed at an angle of 0 to 20 degrees in the horizontal direction, so that the outlet is lower than the inlet; And / or, the collection tank is connected to a second gas recovery tank; And / or, a buffer tank is provided between the isolation chamber and the continuous reaction device applied to solid powder materials; And / or, a cooling tank is provided between the continuous reaction device for solid powder materials and the collection tank; And / or, the continuous reaction system applied to solid powder materials further includes a thermal oil furnace, the inlet and outlet of which are connected to the outlet and inlet of the jacket, respectively.

9. A continuous reaction method applied to solid powder materials, characterized in that, Includes the following steps: The raw materials in the raw material silo are unloaded by gravity into the isolation silo. After being heated and / or pressurized in the isolation silo, the raw materials enter the continuous reaction device for solid powder materials. The reacted materials are collected and stored.

10. The use of the continuous reaction apparatus for solid powder materials according to any one of claims 1-4 and the continuous reaction system for solid powder materials according to claim 7 or 8 in the field of solid-solid reaction, liquid-solid reaction, gas-solid reaction, liquid-liquid reaction or gas-liquid reaction, especially in the field of magnesium-based hydrogen storage material reaction.

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