Continuous production system and method for condensed nanometer material

Abstract

The invention discloses a continuous production system and method for a condensed nanometer material, and belongs to the technical field of nanometer materials. The continuous production system comprises a gas mixing device and a condensing device which are connected in sequence, the gas mixing device is a Laval nozzle injection pump, and the Laval nozzle injection pump is used for mixing and cooling material steam and injection gas; the condensing device comprises a circulating cooling device and a condensing tank; wherein the air suction end of the Laval nozzle injection pump is connected with the outlet end of the material steam source, the air inlet end of the Laval nozzle injection pump is used for introducing injection gas, and the exhaust end of the Laval nozzle injection pump is connected with the mixed gas inlet of the circulating cooling device; and a bottom end outlet of the circulating cooling device is connected with an inlet of the condensation tank. The system can be accurately regulated and controlled, and nano materials with uniform particle sizes can be continuously and efficiently generated.

Description

Technical Field

[0001] The present invention belongs to the technical field of nanomaterials, and in particular relates to a continuous production system and method of condensed nanomaterials. Background Art

[0002] Nanomaterials, especially nanomaterials, have surpassed traditional materials in many fields and even have unique properties because of their smaller outline size. There are many ways and methods to prepare nanomaterials. In addition to ball milling and chemical deposition, vaporizing the material and then rapidly condensing it to form nanoscale powder is a simple and efficient method. This method is mainly divided into two steps: vaporization and cooling. During the direct cooling process of the vaporized material, due to the lack of effective regulation and dispersion, the unorganized steam molecules may condense at different rates and methods, resulting in the formation of nanopowders with different particle sizes and a wide particle size distribution. This will affect the performance consistency and stability of the nanomaterials, and may not achieve the expected results in practical applications.

[0003] In the traditional nanomaterial condensation preparation process, external refrigerant is used, and heat conduction is used as the dominant mode of heat transfer. Specifically, the refrigerant in the cooling tank is encapsulated in a metal coil. When the material vapor enters the condensation area, the two exchange heat through the coil wall. However, the repeated recrystallization of the attachments on the tube wall affects the condensation efficiency and changes the original fluid channel structure, hindering the smooth flow of material vapor. Therefore, large-scale continuous production is impossible.

[0004] Limited by this heat conduction mode, many problems arise in the process of continuous mass production. First, condensation crystals are concentrated on the outer wall of the condensing coil. The crystallization process presents a significant feature: once nucleated, the surrounding steam molecules quickly attach and crystallize around the core, forming a "snowball" effect, causing the initial crystals to continue to grow and the thickness of the crystal layer to be uneven. On the one hand, as the crystal layer rapidly thickens, the thermal resistance increases significantly, the transfer of cold is hindered, and the heat conduction efficiency drops sharply, and ultimately the low temperature environment required for condensation cannot be maintained, seriously affecting the condensation molding quality of the nanomaterials; on the other hand, the continuously growing, overlapping and thickening recrystallizations gradually occupy the internal space of the condensing coil, changing the original fluid channel structure, and hindering the smooth flow of material vapor and refrigerant until the entire condensing device structure fails and production is interrupted.

[0005] In addition, it is very difficult to clean the thick crystal layer attached to the outer wall of the coil. If you are not careful, it is very easy to cause physical damage to the process pipeline when removing the crystals, which consumes a lot of manpower and time. Frequent maintenance operations also seriously interfere with production continuity, further increasing production costs and reducing production efficiency.

[0006] In general, the technical defect of the traditional condensation method is that it cannot guarantee the efficiency of the condensation process, which makes the preparation of nanomaterials fall into difficulties in many aspects such as quality uniformity, production continuity and cost control. Summary of the invention

[0007] In order to overcome the shortcomings of the above-mentioned prior art, the purpose of the present invention is to provide a continuous production system and method for condensed nanomaterials. The continuous production system and method are aimed at continuous, large-scale and efficient production, and process and produce nanomaterials and their compounds. The method is divided into three steps: vaporization, mixing and condensation, and can accurately control and continuously and efficiently produce nanomaterials with uniform particle size.

[0008] In order to achieve the above object, the present invention adopts the following technical solutions: The present invention provides a continuous production system of condensed nanomaterials, comprising a gas mixing device and a condensing device connected in sequence; the gas mixing device is a Laval nozzle jet pump, and the Laval nozzle jet pump is used for mixing and cooling material vapor and injection gas; the condensing device comprises a circulating cooling device and a condensing tank; wherein the air suction end of the Laval nozzle jet pump is connected to the outlet end of the material vapor source, the air inlet end of the Laval nozzle jet pump is used for introducing injection gas, and the exhaust end of the Laval nozzle jet pump is connected to the mixed gas inlet of the circulating cooling device; the bottom outlet of the circulating cooling device is connected to the inlet of the condensing tank.

[0009] In one implementation process, the circulating cooling device includes a cooling tank, a circulating bypass and a second boosting pump; the two ends of the circulating bypass are respectively connected to the circulating gas outlet at the top end and the circulating gas inlet at the bottom end of the cooling tank, and the second boosting pump is arranged on the circulating bypass; the mixed gas inlet and the circulating gas inlet are respectively opened on both sides of the cooling tank, and the mixed gas inlet and the circulating gas inlet are arranged tangent to the tank body of the cooling tank, and the height of the mixed gas inlet is higher than the height of the circulating gas inlet.

[0010] In one implementation process, the bottom outlet of the cooling tank is connected to the inlet of the condensation tank through an exhaust pipe, and the length of the exhaust pipe is positively correlated with the particle size of the condensed nanomaterial.

[0011] In one implementation process, the material steam source is the material steam generated by heating of a dual-zone heating device, the dual-zone heating device is sequentially divided into internal partitions with a liquefaction device and a vaporization device, the middle part of the liquefaction device and the vaporization device are interconnected; the suction end of the Laval nozzle jet pump is connected to the outlet end of the vaporization device; Alternatively, the source of the material steam is magnesium steam generated in a magnesium smelting process using a Pidgeon method or an electric heating method; the suction end of the Laval nozzle jet pump is connected to the gas outlet in the magnesium steam tank.

[0012] In one implementation process, the liquefaction device and the vaporization device are connected to each other through a connecting pipe; a heat preservation layer or a resistance heating device is arranged outside the connecting pipe.

[0013] In one implementation, the liquefaction device includes a liquefaction furnace and a liquefaction crucible disposed inside the liquefaction furnace; the vaporization device includes a vaporization furnace and a vaporization crucible disposed inside the vaporization furnace; wherein the liquefaction crucible and the vaporization crucible are disposed in communication.

[0014] In one implementation process, the continuous production system further includes a recovery device and a gas recovery device, wherein the recovery device is interconnected with the condensation tank; the recovery device is a pressurized packaging device and / or a glove box; One end of the gas recovery device is connected to the condensing tank, and the other end of the gas recovery device, i.e., the gas outlet end, is connected to the gas inlet end of the Laval nozzle jet pump; the gas recovery device includes a dust removal device, a gas storage tank, and a first booster pump connected in sequence. When the second booster pump of the circulating cooling device is preferably a Laval nozzle jet pump, the gas outlet end of the gas recovery device is connected to the gas inlet end of the second booster pump.

[0015] The present invention also provides a method for continuous production of condensed nanomaterials, based on the above-mentioned continuous production system of condensed nanomaterials, comprising the following steps: After the continuous production system of condensed nanomaterials is evacuated, the protective gas is filled to a preset pressure; The jet gas is charged from the air inlet end of the Laval nozzle jet pump, and at the same time, the material vapor in the material vapor source is sucked in through the air suction end of the Laval nozzle jet pump. The jet gas and the material vapor are mixed in the Laval nozzle jet pump, and the jet gas performs preliminary cooling on the material vapor to realize the physical phase change from gaseous state to liquid state of the material vapor or the reaction product of the jet gas and the material vapor; then, it enters the circulating cooling device along the tangent line of the mixed gas inlet for circulating cooling and sufficient reaction, and then enters the condensation tank for condensation to obtain condensed nanomaterials.

[0016] In one implementation process, when the material steam source is material steam generated by heating with a dual-zone heating device, the dual-zone heating device includes a liquefaction device and a vaporization device. The process of heating and generating material steam with the dual-zone heating device is as follows: Materials are added to the liquefaction device of the dual-zone heating device, and the liquefaction device heats the materials to form molten liquid materials. The molten liquid materials flow to the vaporization device and are heated above the vaporization point to form material steam.

[0017] In one implementation process, when a dual-zone heating device is used to heat the generated magnesium vapor to obtain a condensed nano material as a nano magnesium hydrogen powder material, the continuous production method of the condensed nano material is as follows: After the continuous production system of condensed nanomaterials is evacuated, the protective gas is filled to a preset pressure; Adding magnesium particles into the liquefaction device of the dual-zone heating device, the liquefaction device heats the material to form a molten liquid material, and the molten liquid material flows to the vaporization device and is heated above the vaporization point to form magnesium vapor; Hydrogen is used as the injection gas and the protective gas, and the protective gas hydrogen is blown into the vaporization device. The injection gas hydrogen is charged from the air inlet end of the Laval nozzle injection pump, and the magnesium vapor is sucked in through the air intake end of the Laval nozzle injection pump. The hydrogen and the magnesium vapor are mixed and reacted in the Laval nozzle injection pump to release heat. The injection gas hydrogen performs preliminary cooling on the magnesium vapor to achieve a physical phase change from a gaseous state to a liquid state of a reaction product of the injection gas and the material vapor; then, the mixed gas enters a circulating cooling device along a tangent line of the mixed gas inlet for circulating cooling and sufficient reaction, and then enters a condensation tank for condensation to obtain a nano magnesium hydrogen powder material; Or when the magnesium vapor generated in the magnesium smelting process by the Pidgeon method or the electrothermal method is used to prepare the condensed nano material as a nano magnesium hydrogen powder material, the continuous production method of the condensed nano material is as follows: After the continuous production system of condensed nanomaterials is evacuated, the protective gas is filled to a preset pressure; Hydrogen is used as the injection gas and the protective gas. The injection gas hydrogen is charged from the air inlet end of the Laval nozzle injection pump. At the same time, the magnesium vapor in the magnesium vapor tank is sucked in through the air intake end of the Laval nozzle injection pump. The hydrogen and the magnesium vapor are mixed, reacted and release heat in the Laval nozzle injection pump. The injection gas hydrogen performs preliminary cooling on the magnesium vapor to realize the physical phase change of the reaction product of the injection gas and the material vapor from the gaseous state to the liquid state. The mixture then enters the circulating cooling device along the tangent line of the mixed gas inlet for circulating cooling and sufficient reaction, and then enters the condensation tank for condensation to obtain the nano magnesium hydrogen powder material.

[0018] In another embodiment, a continuous production method for preparing condensed nano-magnesium is provided, wherein the nano-magnesium hydrogen powder material prepared in the above manner is heated to release hydrogen to prepare nano-magnesium.

[0019] In one implementation process, the continuous production system of condensed nanomaterials further includes a harvesting device and a gas recovery device; the gas recovery device includes a dust removal device, a gas storage tank and a gas booster pump, namely a first booster pump; The continuous production method of condensed nanomaterials also includes the steps of harvesting and gas recovery and pressurization circulation after the condensed nanomaterials are prepared; The condensed nanomaterial falls into the recovery device for recovery; the protective gas and the injection gas pass through the dust removal device, the gas storage tank and the gas booster pump in sequence and then enter the Laval nozzle injection pump and the second booster pump of the circulation cooling device to form a gas cycle.

[0020] In one implementation process, the heating method of the liquefaction device and the vaporization device includes a main heating method and an auxiliary heating method; the main heating method is resistance furnace heating, medium high frequency furnace heating or arc furnace heating; the auxiliary heating method is laser heating and / or microwave heating.

[0021] In one implementation, during the continuous production process, the remaining molten liquid material in the liquefaction device always remains in liquid state.

[0022] Compared with the prior art, the present invention has the following beneficial effects: On the one hand, the present invention provides a continuous production system for condensed nanomaterials. In the mixing stage of material vapor and jet gas, the suction end of the Laval nozzle jet pump is connected to the material vapor source outlet, and the jet gas is introduced into the air inlet end. Relying on the special structure inside the Laval nozzle jet pump, the material vapor is fully mixed instantly under the drive of the high-speed airflow in the pump, the cold and hot gases collide and blend, and the heat is quickly transferred, and the temperature is instantly reduced. Compared with the traditional heat conduction condensation, this direct internal mixing cooling method is extremely efficient. It can reduce the temperature of the material vapor in a short time, reduce its molecular activity, effectively suppress the disorder of the steam molecules, ensure consistency, and greatly reduce the particle size difference caused by uneven steam distribution. When the mixed gas shuttles at high speed in the pump, physical changes such as gas expansion and collision occur frequently, which prompts the molecular kinetic energy to be quickly exchanged during mixing and fully react. In this process, the steam molecules quickly adjust their own state, and the steam molecules with uneven energy distribution and chaotic motion state become orderly and easier to transform to a condensed state. By finely adjusting the relevant parameters of the injected gas, the consistency of particle size can be guaranteed, which can effectively improve the performance stability of nanomaterials and perfectly solve the problem that traditional condensation technology cannot guarantee the uniformity, stability and efficiency of the condensation process.

[0023] In addition, when the mixed gas is ejected from the Laval nozzle, the particles are accelerated and can quickly and completely convert energy during the subsequent movement. The accelerated particles have a higher energy conversion efficiency. On the one hand, it further optimizes the condensation conditions, making the steam molecules more thorough in energy conversion, accelerating the condensation process, and allowing the nanopowder to form faster; on the other hand, the uniform energy conversion makes the formed nanopowder particles more dense and uniform, which not only improves product quality, but also provides strong support for meeting the needs of continuous mass production, effectively solving the problem of unstable product quality and difficulty in large-scale continuous production under the traditional condensation mode.

[0024] In addition, the high-speed airflow inside the Laval nozzle jet pump will flush the inner wall of the pipe during operation. This feature effectively prevents the problem of crystal accumulation on the outer wall of the traditional condensing coil, and eliminates a series of drawbacks such as heat transfer obstruction and pipe blockage caused by crystal adhesion. It not only ensures the continuous and efficient transfer of cold energy and maintains a stable condensing environment, but also simplifies the maintenance process of the condensing device, reduces the risk of damage to the process pipeline due to cleaning the crystal layer, reduces production costs, and promotes the steady development of nanomaterial preparation towards industrialization, scale, and high quality.

[0025] Traditional condensation relies on heat conduction between the cooling tank wall and the refrigerant to achieve heat absorption and energy exchange. The contact area is limited to the surface of the tank wall, and the heat exchange path is single. The Laval nozzle jet pump breaks this model, changing external cooling to internal cooling, and changing the limited heat absorption and energy exchange area of ​​the cooling tank wall to three-dimensional chaotic all-round energy exchange. The jet gas is introduced to fully mix with the material vapor in the pump to achieve direct internal cooling. The mixed gas flows at high speed in the pump, and the gas molecules in all directions interact with each other to form a three-dimensional chaotic energy exchange environment. The material vapor molecules are no longer limited to contact with the tank wall for energy exchange, but collide with the cold gas molecules in all directions and transfer heat, which greatly broadens the path of heat absorption and energy exchange, improves the efficiency of heat transfer, and ensures that the material vapor can be cooled more quickly and evenly, creating favorable conditions for precise control of the condensation process, and effectively solving the problem that traditional condensation cannot guarantee the uniformity and efficiency of the condensation process.

[0026] Furthermore, the continuous production system uses a Laval nozzle jet pump and a circulating cooling device as a mixing chamber or a further reaction chamber for material vapor and jet gas, which enables the jet gas charged from the air inlet end and the material vapor sucked in from the air intake end to be fully mixed inside. The mixing is one of the key steps in the process of preparing condensed nanomaterials, which directly affects the subsequent physical phase change from gas to liquid and condensation effect. In addition, after the jet gas enters the Laval nozzle jet pump, it exchanges heat with the high-temperature material vapor, thereby preliminarily cooling the material vapor. This process not only helps to stabilize the state of the material vapor, but more importantly, it promotes the physical phase change from gas to liquid of the reaction product of the material vapor or the jet gas and the material vapor. The gas-liquid phase change is the basis for the formation of condensed nanomaterials. Finally, the multi-stage design of the Laval nozzle jet pump helps to enhance the mixing uniformity of the material and the efficiency of the phase change, thereby improving the yield and quality of the condensed nanomaterials. The device continuously circulates the gas in the cooling tank, thereby achieving a full cycle reaction and a rapid and uniform cooling effect. This circulation method helps to improve condensation efficiency and ensure the rapid and stable generation of nanomaterials.

[0027] The particle size of nanopowders can be controlled by adjusting the injection gas and by adjusting the length of the exhaust duct. Longer exhaust ducts provide more cooling, collision and growth space, which is conducive to the formation of larger nanoparticles, while a longer exhaust duct may promote the formation of smaller particles. This particle size control capability is essential for the preparation of nanopowders with specific particle size requirements. When the exhaust duct length is positively correlated with the particle size of nanopowders, producers can quickly adjust the production line configuration according to the target particle size, which helps to improve production efficiency.

[0028] In the existing vaporization process, the storage tank needs to be periodically charged and continuous production cannot be achieved. Due to the furnace production method, each production needs to go through the processes of heating, heat preservation, and cooling, and the heating and cooling cycle is long; and the raw materials are rapidly gasified in the gasifier, and a large amount of raw materials are rapidly heated in a short period of time, which is easy to cause thermal runaway; the raw materials are directly transformed from solid to gas in the gasifier, and the material state suddenly changes violently, and the temperature rises sharply in a short period of time, which is easy to cause thermal runaway. Based on this, the present invention further adopts the partitioning of the liquefaction device and the vaporization device, which can heat the materials in stages at one time, and avoid too much material from rapidly heating up in a short period of time and causing thermal runaway. The design of interconnected middle parts that can be gradually vaporized makes the generation of material steam more stable, reduces the rapid release of heat caused by large-scale vaporization, and further prevents the occurrence of thermal runaway. The molten liquid material flows to the vaporization device for gradual vaporization. This process is more gentle and reduces the impact on the device caused by the sudden change of the material state. The interconnected setting of the liquefaction device and the vaporization device enables the material to be continuously transformed from liquid to gas during the heating process without interruption or transfer to other equipment, thus realizing continuous production; the interconnected setting can also realize the cascade utilization of thermal energy, shorten the heating time and reduce production costs.

[0029] Furthermore, the interconnection between the middle part of the liquefaction device and the vaporization device can avoid impurities located in the upper and lower parts of the liquefaction device, thereby purifying it. The partitioned liquefaction device ensures that the material forms and maintains a stable molten liquid state during the heating process, avoids the solidification and expansion of the material, and thus protects the heating device from damage.

[0030] The connecting pipe between the liquefaction device and the vaporization device is provided with an insulation layer or a resistance heating device outside to keep warm and adjust the temperature to affect the viscosity and control the flow rate.

[0031] Furthermore, the pressure and charge amount of the injected gas can be adjusted to adjust the mixing process and the initial cooling rate, thereby achieving particle size adjustment.

[0032] On the other hand, the present invention provides a continuous production method for condensed nanomaterials. The mixing and initial cooling process of the injection gas and material vapor in the Laval nozzle jet pump helps to achieve a uniform physical phase change, thereby producing condensed nanomaterials with stable quality.

[0033] The present invention can also ensure the stability of the material during the mixing process by accurately controlling the pressure of the injection gas, and can accurately control the uniformity of the particle size of the nano-powder by adjusting the exhaust pipe between the gas mixing device and the condensing device.

[0034] Furthermore, the method realizes a continuous production mode when heating the generated material steam using a dual-zone heating device, from liquefaction, vaporization, mixing, phase change to condensation, which greatly improves production efficiency. No interruption or batch processing is required, which reduces production cycle and production cost.

[0035] Furthermore, when the method uses magnesium vapor generated during the magnesium smelting process of the Pidgeon method or the electrothermal method to prepare the condensed nanomaterial as a nano magnesium hydrogen powder material, the magnesium vapor is generated under a relatively high temperature and a specific environment during the magnesium smelting process of the Pidgeon method or the electrothermal method. When the magnesium vapor is subsequently reacted with hydrogen to prepare the nano magnesium hydrogen powder material, the high temperature and specific environment help to reduce the introduction of impurities, so that the prepared nano magnesium hydrogen powder material has a higher purity, which is conducive to its application in high-end fields.

[0036] Furthermore, this method is applicable to many different types of materials, and only the liquefaction and vaporization heating temperatures and the type of protective gas need to be adjusted. In addition, the design of the Laval nozzle jet pump allows the flow rate and pressure of the jet gas to be adjusted to suit the characteristics of different material vapors and production requirements.

[0037] Furthermore, the recycling of the shielding gas and the injection gas can reduce gas emissions and meet environmental protection requirements.

[0038] Furthermore, the remaining molten liquid material in the liquefaction device remains in liquid state, which can ensure the continuous flow of the material between the liquefaction and vaporization devices, maintain the liquid phase, prevent solidification expansion from damaging the device, prevent production interruptions due to solidification, and at the same time reduce the energy consumption required to reheat the solidified material, thereby improving energy utilization efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] Figure 1 A schematic diagram of a continuous production system of condensed nanomaterials using a dual-zone heating device provided by an embodiment of the present invention; Figure 2 A schematic flow chart of a continuous production method of condensed nanomaterials provided by one embodiment of the present invention; Figure 3 A schematic diagram of a Laval nozzle jet pump used in the present invention; Figure 4 A schematic diagram of a continuous production system for preparing nano magnesium hydrogen powder material using magnesium vapor generated during magnesium smelting using the Pidgeon method or the electrothermal method provided by another embodiment of the present invention; Among them: 1-dual-zone heating device; 2-liquefaction device; 3-vaporization device; 4-Laval nozzle jet pump; 5-condensation tank; 6-circulation cooling device; 7-harvesting device; 8-dust removal device; 9-gas storage tank; 10-first booster pump; 11-second booster pump; 12-cooling tank; 13-laser system; 14-continuous feeding system; 15-magnesium steam tank; 16-vacuum pump. DETAILED DESCRIPTION

[0040] In order to enable those skilled in the art to understand the characteristics and effects of the present invention, the following is a general description and definition of the terms and expressions mentioned in the specification and claims. Unless otherwise specified, all technical and scientific terms used in the text are the common meanings understood by those skilled in the art for the present invention. In the event of a conflict, the definition in this specification shall prevail.

[0041] The theories or mechanisms described and disclosed herein, whether correct or incorrect, should not limit the scope of the present invention in any way, that is, the present invention can be implemented without being limited by any specific theory or mechanism.

[0042] Herein, all features such as values, quantities, contents and concentrations defined in the form of numerical ranges or percentage ranges are for simplicity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to have included and specifically disclosed all possible sub-ranges and individual values ​​within the ranges.

[0043] In this document, unless otherwise specified, “includes,” “including,” “contains,” “has,” or similar terms cover the meanings of “consisting of” and “mainly consisting of,” for example, “A includes a” covers the meanings of “A includes a and other” and “A only includes a.”

[0044] In this document, in order to make the description concise, not all possible combinations of various technical features in various embodiments or examples are described. Therefore, as long as there is no contradiction in the combination of these technical features, the various technical features in various embodiments or examples can be combined arbitrarily, and all possible combinations should be considered to be within the scope of this specification.

[0045] A continuous production system of condensed nanomaterials provided in one embodiment of the present invention has a structure as follows: Figure 1 As shown, it includes a dual-zone heating device 1, a gas mixing device and a condensing device connected in sequence.

[0046] Dual-zone heating device 1: The internal partitions are sequentially provided with a liquefaction device 2 and a vaporization device 3, and the middle part of the liquefaction device 2 is connected to the vaporization device 3. The dual-zone heating device 1 is a horizontal furnace, and the liquefaction device 2 and the vaporization device 3 are connected in two zones.

[0047] This partitioned setting and staged heating method is conducive to continuous feeding production into the liquefaction device 2, and can effectively prevent the occurrence of thermal runaway. During the production process, the liquefaction device 2 first heats the material to a molten liquid state, so that the vaporized part can be gradually vaporized, thereby realizing continuous production. At the same time, maintaining the liquid phase state of the remaining molten liquid material in the liquefaction device 2 can not only prevent the device from being damaged due to the solidification and expansion of the material, but also avoid the thermal runaway caused by large-scale vaporization. Specifically, the liquefaction device 3 and the vaporization device 4 are set in partitions to heat the material in stages. The liquefaction stage mainly focuses on the melting and uniform heating of the material, while the vaporization stage focuses on heating the molten liquid material to above the vaporization point to form steam. This staged heating method helps to accurately control the temperature and state of the material at different stages. Thermal runaway is usually caused by a rapid heating of the material in a short period of time. The partition setting and gradual vaporization design can effectively disperse and slow down the release of heat, thereby preventing the occurrence of thermal runaway. The connection between the liquefaction device 3 and the vaporization device 4 enables the material to be continuously transformed from liquid to gas during the heating process, which not only simplifies the production process, but also improves the production efficiency and makes continuous production possible.

[0048] In specific implementation, the liquefaction device 2 and the vaporization device 3 are connected to each other through a connecting pipe. In order to prevent the material from cooling and solidifying in the connecting pipe, a thermal insulation layer or a resistance heating device is provided on the outside of the connecting pipe. When the thermal insulation layer is used, a heat-insulating material with good performance such as ceramic fiber insulation cotton can be selected and tightly wrapped on the outside of the connecting pipe to greatly reduce heat loss; if a resistance heating device is used, the resistance wire can be reasonably arranged according to the length and diameter of the connecting pipe, and the heating temperature can be adjusted by accurately controlling the current size to ensure that the material in the connecting pipe always maintains a good flow state. At the same time, the viscosity of the material can be affected by adjusting the temperature, thereby regulating the flow rate.

[0049] The middle part of the liquefaction device 2 is connected to the vaporization device 3, which can effectively purify and prevent the impurities on the top and the deposited impurities on the bottom from entering the vaporization device 3, and facilitate the subsequent slag removal and impurity removal.

[0050] The liquefaction device 2 includes a liquefaction furnace and a liquefaction crucible arranged inside the liquefaction furnace; the vaporization device 3 includes a vaporization furnace and a vaporization crucible arranged inside the vaporization furnace, wherein the liquefaction crucible and the vaporization crucible are connected. Such a connected arrangement can realize the step-by-step controllable continuous vaporization production of materials. In actual operation, the liquefaction furnace and the vaporization furnace can flexibly select the appropriate heating power and temperature control range according to the characteristics of the materials and production requirements. For example, for some materials with a low melting point, the temperature of the liquefaction furnace can be set in a relatively low range, such as 200℃-800℃; while for the vaporization furnace, since the material needs to be heated above the vaporization point, the temperature may be set at 800℃-3000℃. In addition, the heating methods of the liquefaction furnace and the vaporization furnace include a main heating method and an auxiliary heating method, the main heating method is resistance furnace heating, medium-high frequency furnace heating or arc furnace heating; the auxiliary heating method is laser heating and / or microwave heating. In actual production, the heating methods can be flexibly combined according to the properties of the materials and the heating requirements. For example, for some materials that require high temperature uniformity, resistance furnace heating can be used as the main heating method, combined with microwave heating or laser heating as auxiliary heating methods to significantly improve heating efficiency and uniformity.

[0051] Liquefaction can choose a heating scheme according to the situation. For the heating of the crucible in the vaporization zone, microwave-assisted vaporization can be set up at the bottom for difficult-to-melt materials. The crucible material can be a quartz crucible during microwave-assisted vaporization. Laser-assisted vaporization is used at the top to achieve local vaporization. Thanks to the high energy density and precise controllability of the laser, the temperature of the crucible in the vaporization area can be effectively controlled in a lower range. Even for special materials with extremely high vaporization points, this temperature range will not exceed the heat resistance limit of the crucible, thereby eliminating the need for additional strengthening measures to improve the temperature resistance of the crucible and avoiding the increase in process complexity and cost caused by the upgrade of the crucible material. However, laser-assisted vaporization technology is not without shortcomings. It will significantly restrict the scale of production capacity and increase costs in applications. Fiber lasers can be used for metal vaporization, and carbon dioxide lasers can be used for non-metal vaporization.

[0052] For details, see Figure 1 The dual-zone heating device 1 is a vacuum furnace chamber. A continuous feeding system 14 and a laser system 13 are arranged on the top of the vacuum furnace chamber. A plurality of heaters are arranged inside the vacuum furnace chamber. The outlet of the continuous feeding system 14 is connected to the liquefaction device 2. The middle part of the liquefaction device 2 is interconnected with the vaporization device 3. A laser system 13 is arranged above the vaporization device 3. The laser system 13 is connected to the air outlet end of the first booster pump 10. The vaporization device 3 is connected to the air intake end of the Laval nozzle jet pump 4.

[0053] like Figure 3As shown, the gas mixing device is a Laval nozzle jet pump 4, which is used to mix the material steam and the injection gas. The suction end of the Laval nozzle jet pump 4 is connected to the outlet end of the vaporization device 3, the intake end is used to pass the injection gas, and the exhaust end is connected to the condensation device. In the process of mixing the mixed steam and the injection gas, the Laval nozzle jet pump 4 cools the material steam by the injection gas, or similar to magnesium and other similar metals, when hydrogen is used as the injection gas, the material steam reacts with the injection gas to form a mixed gas. This method is simple and efficient, and by adjusting the parameters such as the pressure of the injection gas, controllable continuous production can be achieved.

[0054] In addition, the external water jacket in the Laval nozzle jet pump 4 plays a critical role in thermal management. Figure 3 As shown in the cooling refrigerant inlet and outlet on the left and right sides of the middle, when the device is running, water flows through the external water jacket and, through the principle of heat conduction, promptly removes the heat generated by the pump body during operation, effectively reducing the temperature of the pump body. This cooling measure can ensure that the device can still maintain a stable operating state under high temperature conditions, avoid uneven thermal expansion of materials caused by overheating, and thus prevent thermal deformation of the device, thereby ensuring the reliability and service life of the entire system.

[0055] The injection pressure of the injection gas is adjustable. The injection pressure of the injection gas introduced into the air inlet end of the Laval nozzle injection pump 4 can be flexibly adjusted according to the specific characteristics of the material steam, the requirements of the production process and the different needs of the condensation stage.

[0056] Similarly, the injection temperature of the injection gas is also adjustable. The injection gas temperature can be accurately set according to the initial temperature of the material vapor, the desired condensation temperature range and real-time feedback during the production process.

[0057] Furthermore, the unique structural design of the Laval nozzle jet pump 4 enables it to achieve a multi-stage overlapping suction function. By increasing the suction force step by step, it ensures that the material vapor can be efficiently and completely sucked into the pump.

[0058] On the one hand, in large-scale continuous production, even if the material vapor is generated at a fast rate and a large flow rate, the strong suction force can ensure that it is mixed with the injection gas in time; on the other hand, multi-stage overlapping suction helps to maintain a stable airflow environment in the pump, making the mixing, cooling, condensation and other processes more orderly, further improving the condensation efficiency, ensuring the continuity and efficiency of nanomaterial preparation, and effectively solving the problem of poor production continuity under the traditional condensation mode.

[0059] Condensation device: The condensation device includes a circulating cooling device and a condensation tank 5, the mixed gas inlet of the circulating cooling device is connected to the exhaust end of the Laval nozzle jet pump 4, and the bottom outlet of the circulating cooling device is connected to the inlet of the condensation tank 5. Preferably, the condensation tank 5 is arranged below the circulating cooling device.

[0060] The circulating cooling device includes a cooling tank 12, a circulating bypass and a second boosting pump 11; the two ends of the circulating bypass are respectively connected to the circulating gas outlet at the top and the circulating gas inlet at the bottom of the cooling tank 12, and the second boosting pump 11 is arranged on the circulating bypass; the mixed gas inlet and the circulating gas inlet are respectively opened on both sides of the cooling tank 12, and the mixed gas inlet and the circulating gas inlet are arranged tangent to the tank body of the cooling tank 12, and the height of the mixed gas inlet is higher than the height of the circulating gas inlet.

[0061] The second boost pump 11 is preferably a Laval nozzle jet pump, and the air inlet end of the second boost pump 11 is connected to the air outlet end of the gas recovery device.

[0062] The condensation tank 5 is connected to a circulating cooling device 6, and condensation is performed by combining the condensation tank 5 with the circulating cooling device 6. The circulating cooling device 6 can select a suitable cooling medium, such as water or a specific coolant, as needed, and remove heat through a circulating flow, so that the material vapor entering the condensation tank 5 can be quickly cooled and condensed into condensed nanomaterials. The condensation tank 5 is connected to the gas mixing device, and the circulating cooling device 6 is a cooling tower circulating pump and its corresponding pipelines, which can stably provide cooling support for the condensation process.

[0063] Harvesting device 7: The continuous production system also includes a harvesting device 7, which is interconnected with the condensation tank 5. The harvesting device 7 is a pressurized packaging device and / or a glove box. When a pressurized packaging device is used, the condensed nanomaterials can be packaged and collected under a certain pressure environment, effectively preventing them from contacting with the outside air and causing oxidation or contamination; the glove box can provide a relatively isolated operating space, and the operator can operate through the gloves in the glove box, which is convenient for processing and collecting the condensed nanomaterials, ensuring the quality and safety of the product.

[0064] Gas recovery device: The gas recovery device includes a dust removal device 8, a gas storage tank 9 and a first booster pump 10 connected in sequence; the dust removal device 8 includes a dust collector, a glove box and a vacuum pump 16; the glove box is arranged below the dust collector, the dust collector is connected to the condensation tank 5, the vacuum pump 16 is connected to the dust collector, and the vacuum pump 16 is connected to the gas storage tank 9.

[0065] The inlet end of the gas recovery device is connected to the condensation tank 5, the gas outlet end of the gas recovery device is connected to the air inlet end of the Laval nozzle jet pump 4, and the first booster pump 10 is also connected to the laser system 13 provided on the vaporization device 3. The first booster pump 10 is also connected to the second booster pump 11, and the gas is sent to the Laval nozzle jet pump 4, the laser system 13, and the second booster pump 11 for recycling. The dust collector can effectively remove solid particle impurities in the gas, the gas storage tank 9 is used to store the recovered gas, and the first booster pump 10 pressurizes the gas and sends it back to the air inlet end of the Laval nozzle jet pump 4 or the laser system 13 and the second booster pump 11, so as to realize the recycling of the gas, significantly reduce the production cost, and reduce the impact on the environment.

[0066] All the above-mentioned equipment are equipped with water jackets on the outside to ensure production safety.

[0067] like Figure 2 As shown, based on the above-mentioned continuous production system of condensed nanomaterials, a continuous production method of condensed nanomaterials of the present invention sequentially performs zone heating vaporization, mixed reaction cooling, cycle cooling and condensation, and the specific steps are as follows: Vacuuming and filling: First, the entire system is evacuated to remove air and impurities in the system, and then the protective gas is filled to the preset pressure. For example, the protective gas can be an inert gas such as argon, nitrogen, etc., and the preset pressure can be set to 1 atmosphere or other suitable pressure values ​​according to the specific production process requirements. For some special materials, such as magnesium and other similar metals, hydrogen can be used as a protective gas to generate magnesium hydride as a condensed nanomaterial.

[0068] Material heating: Add material to the liquefaction device 2 of the dual-zone heating device 1, and the liquefaction device 2 heats the material to form molten liquid material through its heating method. The molten liquid material flows to the vaporization device 3 through the connecting pipe, and is further heated to above the vaporization point to form material steam. In this process, the flexibly selected heating method of the liquefaction device 2 and the vaporization device 3 can achieve precise heating according to the characteristics of the material, ensuring the stable conversion of the material.

[0069] Mixing and preliminary cooling: a protective gas is blown into the vaporization device 3, and the injection gas is filled into the air inlet end of the Laval nozzle jet pump 4. At the same time, the material vapor is sucked in through the air suction end of the Laval nozzle jet pump 4. The injection gas and the material vapor are mixed in the Laval nozzle jet pump 4, and the injection gas performs preliminary cooling on the material vapor, so as to realize the physical phase change of the material vapor or the reaction product of the injection gas and the material vapor from gas to liquid.

[0070] Condensation: The material after preliminary cooling enters the circulating cooling device and the condensation tank 5 in the condensation device for condensation to obtain condensed nanomaterials.

[0071] Specifically, the product in the Laval nozzle jet pump 4 enters the circulating cooling device along the mixed gas inlet tangent in the circulating cooling device for circulating cooling and sufficient reaction, and then enters the condensation tank 5 for further condensation to obtain condensed nanomaterials.

[0072] In a specific implementation process, when the condensed nano material is a nano magnesium hydrogen powder material, the continuous production method of the condensed nano material is as follows: After the continuous production system of condensed nanomaterials is evacuated, the protective gas is filled to a preset pressure; Magnesium particles are added to the liquefaction device 2 of the dual-zone heating device 1, and the liquefaction device 2 heats the material to form a molten liquid material, and the molten liquid material flows to the vaporization device 3 and is heated to above the vaporization point to form magnesium vapor; Hydrogen is used as the injection gas and the protective gas, and the protective gas hydrogen is blown into the vaporization device 3. The injection gas hydrogen is filled from the air inlet end of the Laval nozzle jet pump 4, and at the same time, the magnesium vapor is sucked in through the air intake end of the Laval nozzle jet pump 4. The hydrogen and the magnesium vapor are mixed and reacted in the Laval nozzle jet pump 4, and the reaction releases heat. The injection gas hydrogen is used to preliminarily cool the magnesium vapor to achieve a physical phase change from a gaseous state to a liquid state of a reaction product of the injection gas and the material vapor; then, the mixed gas enters a circulating cooling device along a tangent line of the mixed gas inlet for circulating cooling and sufficient reaction, and then enters a condensation tank 5 for condensation to obtain a nano magnesium hydrogen powder material.

[0073] Furthermore, the recovery and gas recovery pressurization cycle: the condensed nanomaterials fall into the recovery device 7 for recovery; the protective gas and the injection gas pass through the dust removal device 8, the gas storage tank 9 and the first booster pump 10 in turn and then enter the Laval nozzle injection pump 4 and the second booster pump 11 to form a gas cycle.

[0074] Furthermore, during the continuous production process, the temperature and material state in the liquefaction device 2 are monitored in real time, and the heating power is adjusted in time to ensure that the remaining molten liquid material in the liquefaction device 2 always remains in liquid state, preventing the remaining material from solidifying and expanding to damage the device, thereby ensuring the continuity and stability of production.

[0075] Another embodiment of the present invention provides a continuous production system of condensed nanomaterials, the structure of which is as follows: Figure 4 As shown, it includes a magnesium vapor tank body 15, a gas mixing device and a condensing device which are connected in sequence.

[0076] The gas mixing device, condensing device, collecting device 7 and gas recovery device are the same as those in the previous embodiment.

[0077] The magnesium steam tank body 15 is provided with an air outlet, and the air outlet in the magnesium steam tank body 15 is connected to the air suction end of the Laval nozzle jet pump 4, and the magnesium steam is sucked by the air suction end of the Laval nozzle jet pump 4.

[0078] The above-mentioned continuous production method includes three steps of vaporization, mixing and condensation. The mixing section is vacuumed through the suction end of the Laval nozzle 4. When magnesium is smelted, after the ore generates magnesium vapor, the magnesium vapor is directly extracted and mixed with the injected gas hydrogen to react, and then condensed to produce nano-magnesium hydrogen powder material. The above-mentioned method is a new magnesium smelting method.

[0079] Specifically, when the magnesium vapor generated in the magnesium smelting process by other methods such as the Pidgeon method or the electrothermal method is used to prepare the condensed nano material as a nano magnesium hydrogen powder material, the continuous production method of the condensed nano material is as follows: After the continuous production system of condensed nanomaterials is evacuated, the protective gas is filled to a preset pressure; Hydrogen is used as the injection gas and the protective gas. The injection gas hydrogen is charged from the air inlet end of the Laval nozzle jet pump 4. At the same time, the magnesium vapor in the magnesium vapor tank body 15 is sucked in through the air intake end of the Laval nozzle jet pump 4. The hydrogen and the magnesium vapor are mixed, reacted and released heat in the Laval nozzle jet pump 4. The injection gas hydrogen is used to preliminarily cool the magnesium vapor to achieve a physical phase change from a gaseous state to a liquid state of a reaction product of the injection gas and the material vapor. The mixture then enters a circulating cooling device along a tangent line of the mixed gas inlet for circulating cooling and sufficient reaction, and then enters a condensation tank 5 for condensation to obtain a nano magnesium hydrogen powder material.

[0080] The produced magnesium hydrogen can be directly used in hydrolysis reaction to generate hydrogen for fuel cells to generate electricity and become fuel cell fuel.

[0081] The traditional Pidgeon method for magnesium refining and some new methods all use heating ore to generate magnesium vapor, which is condensed and recovered as crude magnesium. The new process proposed by the present invention uses hydrogen as the injection gas of the Laval nozzle jet pump 4. The magnesium vapor generated by magnesium refining is sucked from the suction end of the Laval nozzle jet pump 4 and directly mixed with hydrogen to react to generate magnesium hydrogen. Magnesium hydrogen has safe and stable storage and transportation characteristics. When magnesium hydrogen is heated, hydrogen is released and nano-magnesium powder is produced at the same time, thus forming a new magnesium refining method.

[0082] The present invention will be further described below in conjunction with specific embodiments. It should be understood that these embodiments are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms fall within the scope limited by the appended claims of the application equally.

[0083] The following examples use conventional instruments and equipment in the art. The experimental methods in the following examples where specific conditions are not specified are usually carried out under conventional conditions or under conditions recommended by the manufacturer. The various raw materials used in the following examples are conventional commercial products unless otherwise specified, and their specifications are conventional specifications in the art. In the specification of the present invention and the following examples, unless otherwise specified, "%" means weight percentage, "part" means weight part, and ratio means weight ratio.

[0084] Example 1 This embodiment provides a method for continuous production of condensed nanomaterials. In this embodiment, magnesium hydride nanoparticles are produced. The specific steps are as follows: Step 1: System preparation: Use the vacuum pump 16 to evacuate the entire production system pipeline, reduce the pressure to below 30Pa, and remove air and impurities. Then fill the system with hydrogen as a protective gas to make the pressure in the system reach 1 atmosphere.

[0085] Step 2: Material heating and vaporization: Adding materials: After the system is evacuated, magnesium particles are added into the large crucible of the liquefaction furnace of the liquefaction device 2.

[0086] Liquefaction: Start the liquefaction furnace, select a suitable heating method (such as resistance furnace heating, medium-high frequency furnace heating or arc furnace heating, etc.), heat the magnesium particles in the large crucible to the melting point, and melt them into liquid magnesium metal. The liquid magnesium metal flows into the small crucible of the vaporization furnace in the vaporization device 3 connected to the liquefaction device 2.

[0087] Vaporization: Start the vaporization furnace, heat the small crucible to above the vaporization point, and vaporize the liquid magnesium into magnesium vapor. A laser system 13 such as a laser-assisted vaporizer (such as a fiber laser) and a microwave-assisted vaporization device may be used to assist the vaporization.

[0088] Step 3: Mixing reaction and initial cooling: Connection and gas introduction: introduce protective gas hydrogen into the vaporization device 3 to blow magnesium vapor, connect the outlet end of the vaporization device 3 with the suction end of the Laval nozzle jet pump 4, blow hydrogen from the intake end of the Laval nozzle jet pump 4, so that the magnesium vapor is sucked into the jet pump, and the two gases are fully mixed and reacted.

[0089] Mixing reaction and cooling: Hydrogen reacts with magnesium vapor to generate magnesium hydride and releases heat. The mixed gas cools down to form small droplets and becomes spherical due to surface tension. The droplet size and nano-magnesium hydride particle size are controlled by controlling parameters such as the residence time in the pipeline, the temperature in the Laval nozzle jet pump 4, and the injection gas pressure.

[0090] Step 4: Condensation collection: Circulation cooling: The mixed gas discharged from the exhaust end of the Laval nozzle jet pump 4 enters the cooling tank 12 along the tangent of the mixed gas inlet, then enters the circulation bypass through the circulation gas outlet, and then enters the cooling tank 12 again through the circulation gas inlet tangently, and the product falls into the condensation tank 5 from the bottom outlet.

[0091] Condensation: The product from the cooling tank 12 enters the vertically arranged condensation tank 5 for further cooling. Multiple condensation tanks 5 are arranged vertically in succession. The mixed gas enters the condensation tank 5. The circulating cooling device 6 (such as a cooling tower circulating pump and corresponding pipelines, and a suitable cooling medium) is used to cool and condense the magnesium hydride vapor in the mixed gas into nano powder. Multiple condensation tanks 5 can be connected in series to improve the condensation effect.

[0092] Step 5: Harvesting and packaging: The nano-magnesium hydride powder produced after condensation falls vertically into the pressurized packaging equipment or glove box at the lower end to harvest and package the condensed nano-magnesium hydride powder, so that the storage and transportation of magnesium hydride is safe and stable.

[0093] Step 6: Gas recovery and pressurization cycle: Gas filtration: The gas discharged from the condensation tank 5 passes through the dust removal device 8 to remove solid particles.

[0094] Gas circulation treatment: The filtered hydrogen and protective gas enter the gas storage tank 9 and the first booster pump 10, and after being static and pressurized, they are blown into the air inlet end of the Laval nozzle jet pump 4 and the second booster pump 11 vaporization device 3 for recycling.

[0095] In addition, the nano magnesium hydride powder prepared in this embodiment can release hydrogen when heated to above 300° C. to form nano magnesium powder. Heating magnesium hydride will release hydrogen and produce nano magnesium powder at the same time. The above process provides a new magnesium refining method.

[0096] Furthermore, the nano magnesium hydride powder prepared in this embodiment can be directly used for hydrolysis reaction to generate hydrogen for fuel cell power generation and become fuel cell fuel.

[0097] Example 2 This embodiment provides a method for continuous production of condensed nanomaterials. In this embodiment, tin nanoparticles are produced, and argon is used as a protective gas and a spray gas. The differences from the steps in Example 1 are as follows, and the other steps are the same as those in Example 1.

[0098] Step 1: System Preparation The entire production system's equipment pipelines are evacuated using a vacuum pump 16, the pressure is reduced to 50 Pa, air and impurities are removed, and argon is filled in until the system pressure reaches 1 atmosphere.

[0099] Step 2: Material heating and vaporization Adding materials: After the system is evacuated, add tin particles into the large crucible of the liquefaction furnace of the liquefaction device 2.

[0100] Liquefaction: Start the liquefaction furnace and use resistance furnace heating, medium-high frequency furnace heating or arc furnace heating, etc., which can be combined with laser heating and / or microwave heating to heat the tin particles to above the melting point, so that they melt into liquid tin and flow into the small crucible of the vaporization furnace of the vaporization device 3.

[0101] Vaporization: Start the vaporization furnace, heat the small crucible to above the vaporization point of tin, and vaporize the liquid tin into tin vapor. The laser system 13 such as a laser-assisted vaporizer (such as a fiber laser) can be used.

[0102] Step 3: Mixing reaction and initial cooling Connection and gas introduction: introduce argon gas into the vaporization device 3 to blow tin vapor, connect the outlet end of the vaporization device 3 with the suction end of the Laval nozzle jet pump 4, blow argon gas from the intake end of the Laval nozzle jet pump 4, so that the tin vapor is sucked into the pump and mixed.

[0103] Mixing reaction and cooling: Argon gas cools the tin vapor, and the mixed gas forms small droplets and spherical shapes. The droplet size and the particle size of the tin nanoparticles are controlled by controlling the pipeline residence time, the temperature in the Laval nozzle jet pump 4, the jet gas pressure, etc.

[0104] Step 4: Condensation Collection Circulation cooling: The mixed gas discharged from the exhaust end of the Laval nozzle jet pump 4 enters the cooling tank 12 along the tangent of the mixed gas inlet, then enters the circulation bypass through the circulation gas outlet, and then enters the cooling tank 12 again through the circulation gas inlet tangently, and the product falls into the condensation tank 5 from the bottom outlet.

[0105] Condensation: The product from the cooling tank 12 enters a plurality of condensation tanks 5 arranged vertically in a vertical layout, and a circulating cooling device 6 (such as a cooling tower circulating pump and corresponding pipelines, and a suitable cooling medium) is used to cool and condense the tin vapor into tin nanopowder. Multiple condensation tanks 5 can be connected in series.

[0106] Step 5: Harvesting and packaging The condensed tin nanopowder falls into the lower pressure packaging equipment or glove box for collection and packaging.

[0107] Step 6: Gas recovery and pressurization cycle Gas filtration: The gas discharged from the condensation tank 5 passes through the dust removal device 8 to remove solid particles.

[0108] Gas circulation treatment: The filtered hydrogen and protective gas enter the gas storage tank 9 and the first booster pump 10, and after being static and pressurized, they are blown into the air inlet end of the Laval nozzle jet pump 4 and the second booster pump 11 vaporization device 3 for recycling.

[0109] Example 3 This embodiment provides a method for continuous production of condensed nanomaterials. In this embodiment, silver nanoparticles are produced, and argon is used as a protective gas and a spray gas. The differences from the steps in Example 1 are as follows, and the other steps are the same as those in Example 1.

[0110] Step 1: System Preparation The production system pipeline is evacuated to 50Pa by a vacuum pump 16 to remove air and impurities, and argon gas is filled in to make the pressure in the system reach 1 atmosphere.

[0111] Step 2: Material heating and vaporization Adding materials: After the system is evacuated, add silver particles into the large crucible of the liquefaction furnace of the liquefaction device 2.

[0112] Liquefaction: Start the liquefaction furnace, and heat the silver particles to above the melting point by heating with a resistance furnace, a medium-high frequency furnace, or an arc furnace, so that the silver particles are melted into liquid silver and flow into the small crucible of the vaporization furnace of the vaporization device 3.

[0113] Vaporization: Start the vaporization furnace, heat the small crucible to above the vaporization point of silver, and vaporize the liquid silver into silver vapor. This can be done with the help of a laser system 13 such as a laser-assisted vaporizer (such as a fiber laser).

[0114] Step 3: Mixing reaction and initial cooling Connection and gas introduction: introduce argon gas into the vaporization device 3 to blow silver vapor, connect the outlet end of the vaporization device 3 with the suction end of the Laval nozzle jet pump 4, blow argon gas from the intake end of the Laval nozzle jet pump 4, so that the silver vapor is sucked into the pump and mixed.

[0115] Mixing reaction and cooling: Argon gas cools the silver vapor, and the mixed gas forms small droplets and spherical shapes. The droplet size and the size of the silver nanoparticles are controlled by controlling the pipeline residence time, the temperature in the Laval nozzle jet pump 4, and the jet gas pressure.

[0116] Step 4: Condensation Collection Circulation cooling: The mixed gas discharged from the exhaust end of the Laval nozzle jet pump 4 enters the cooling tank 12 along the tangent of the mixed gas inlet, then enters the circulation bypass through the circulation gas outlet, and then enters the cooling tank 12 again through the circulation gas inlet tangently, and the product falls into the condensation tank 5 from the bottom outlet.

[0117] Condensation: The product from the cooling tank 12 enters a plurality of condensation tanks 5 arranged vertically in a vertical layout, and a circulating cooling device 6 (such as a cooling tower circulating pump and corresponding pipelines, and a suitable cooling medium) is used to cool and condense the silver vapor into silver nanopowder. Multiple condensation tanks 5 can be connected in series.

[0118] Step 5: Harvesting and packaging The condensed silver nanopowder falls into the lower pressure packaging equipment or glove box for collection and packaging.

[0119] Step 6: Gas recovery and pressurization cycle Gas filtration: The gas discharged from the condensation tank 5 passes through the dust removal device 8 to remove solid particles.

[0120] Gas circulation treatment: The filtered hydrogen and protective gas enter the gas storage tank 9 and the first booster pump 10, and after being static and pressurized, they are blown into the air inlet end of the Laval nozzle jet pump 4 and the second booster pump 11 vaporization device 3 for recycling.

[0121] Example 4 This embodiment provides a method for continuous production of condensed nanomaterials. In this embodiment, nano silicon particles are produced, silicon is used as raw material, argon is used as protective gas and injection gas, and other steps are the same as those in Example 1.

[0122] Example 5 This embodiment provides a continuous production method for condensed nanomaterials. In this embodiment, nano-silicon dioxide particles are produced. Silicon is used as a raw material, oxygen is used as a protective gas and a spray gas, oxygen and silicon vapor react to generate silicon dioxide, and nano-silicon dioxide particles are obtained. The other steps are the same as those in Example 1.

[0123] The above contents are only for explaining the technical idea of ​​the present invention and cannot be used to limit the protection scope of the present invention. Any changes made on the basis of the technical solution in accordance with the technical idea proposed by the present invention shall fall within the protection scope of the claims of the present invention.

Claims

1. A continuous production system for condensed nanomaterials, characterized in that: It comprises a gas mixing device and a condensing device connected in sequence; the gas mixing device is a Laval nozzle jet pump (4), and the Laval nozzle jet pump (4) is used for mixing material vapor and injection gas and cooling; the condensing device comprises a circulating cooling device and a condensing tank (5); wherein the air suction end of the Laval nozzle jet pump (4) is connected to the outlet end of the material vapor source, the air inlet end of the Laval nozzle jet pump (4) is used for introducing injection gas, and the air discharge end of the Laval nozzle jet pump (4) is connected to the mixed gas inlet of the circulating cooling device; the bottom outlet of the circulating cooling device is connected to the inlet of the condensing tank (5).

2. The continuous production system of condensed nanomaterials according to claim 1, characterized in that: The circulating cooling device comprises a cooling tank (12), a circulating bypass and a second boosting pump (11); The two ends of the circulation bypass are respectively connected to the circulation gas outlet at the top and the circulation gas inlet at the bottom of the cooling tank (12), and the second booster pump (11) is arranged on the circulation bypass; The mixed gas inlet and the circulating gas inlet are respectively provided on both sides of the cooling tank (12), the mixed gas inlet and the circulating gas inlet are arranged tangent to the tank body of the cooling tank (12), and the height of the mixed gas inlet is higher than that of the circulating gas inlet.

3. The continuous production system of condensed nanomaterials according to claim 2, characterized in that: The bottom outlet of the cooling tank (12) is connected to the inlet of the condensation tank (5) via an exhaust pipe, and the length of the exhaust pipe is positively correlated with the particle size of the condensed nanomaterial.

4. The continuous production system of condensed nanomaterials according to claim 1, characterized in that: The material steam source is the material steam generated by heating of a dual-zone heating device (1), the dual-zone heating device (1) is provided with a liquefaction device (2) and a vaporization device (3) in sequence in the internal partitions, the middle part of the liquefaction device (2) and the vaporization device (3) are interconnected; the suction end of the Laval nozzle jet pump (4) is connected to the outlet end of the vaporization device (3); Alternatively, the source of the material steam is magnesium steam generated in a magnesium smelting process using a Pidgeon method or an electric heating method; the suction end of the Laval nozzle jet pump (4) is connected to the gas outlet in the magnesium steam tank (15).

5. The continuous production system of condensed nanomaterials according to claim 4, characterized in that: The liquefaction device (2) and the vaporization device (3) are connected to each other via a connecting pipe; a heat-insulating layer or a resistance heating device is provided outside the connecting pipe; The liquefaction device (2) comprises a liquefaction furnace and a liquefaction crucible arranged inside the liquefaction furnace; the vaporization device (3) comprises a vaporization furnace and a vaporization crucible arranged inside the vaporization furnace; wherein the liquefaction crucible and the vaporization crucible are arranged in communication.

6. The continuous production system of condensed nanomaterials according to claim 1, characterized in that: The continuous production system further comprises a harvesting device (7) and a gas recovery device, wherein the harvesting device (7) is connected to the condensation tank (5); the harvesting device (7) is a pressurized packaging device and / or a glove box; One end of the gas recovery device is connected to a condensation tank (5), and the other end of the gas recovery device is connected to an air inlet end of a Laval nozzle jet pump (4); the gas recovery device comprises a dust removal device (8), a gas storage tank (9), and a first booster pump (10) which are connected in sequence.

7. A method for continuous production of condensed nanomaterials, characterized in that: The continuous production system of condensed nanomaterials according to any one of claims 1 to 6 comprises the following steps: After the continuous production system of condensed nanomaterials is evacuated, the protective gas is filled to a preset pressure; The jet gas is charged from the air inlet end of the Laval nozzle jet pump (4), and at the same time, the material steam in the material steam source is sucked into the Laval nozzle jet pump (4) through the air intake end. The jet gas and the material steam are mixed in the Laval nozzle jet pump (4). The jet gas performs preliminary cooling on the material steam to achieve a physical phase change from gaseous to liquid of the material steam or the reaction product of the jet gas and the material steam. The mixed gas then enters the circulating cooling device along the tangent of the mixed gas inlet for circulating cooling and sufficient reaction, and then enters the condensation tank (5) for condensation to obtain a condensed nanomaterial.

8. The method for continuous production of condensed nanomaterials according to claim 7, characterized in that: When the source of the material steam is material steam generated by heating of a dual-zone heating device (1), the dual-zone heating device (1) comprises a liquefaction device (2) and a vaporization device (3), and the process of heating the material steam generated by the dual-zone heating device (1) is as follows: Materials are added to the liquefaction device (2) of the dual-zone heating device (1), the liquefaction device (2) heats the materials to form molten liquid materials, and the molten liquid materials flow to the vaporization device (3) and are heated to a temperature above the vaporization point to form material vapor.

9. The method for continuous production of condensed nanomaterials according to claim 8, characterized in that: When the magnesium vapor generated by heating with the dual-zone heating device (1) is used to prepare the condensed nano material, which is a nano magnesium hydrogen powder material, the continuous production method of the condensed nano material is as follows: After the continuous production system of condensed nanomaterials is evacuated, the protective gas is filled to a preset pressure; Adding magnesium particles into the liquefaction device (2) of the dual-zone heating device (1), the liquefaction device (2) heats the material to form a molten liquid material, the molten liquid material flows to the vaporization device (3) and is heated to above the vaporization point to form magnesium vapor; Hydrogen is used as the injection gas and the protective gas, and the protective gas hydrogen is blown into the vaporization device (3). The injection gas hydrogen is charged from the air inlet end of the Laval nozzle injection pump (4), and at the same time, the magnesium vapor is sucked in through the air intake end of the Laval nozzle injection pump (4). The hydrogen and the magnesium vapor are mixed and reacted in the Laval nozzle injection pump (4) and release heat. The injection gas hydrogen performs a preliminary cooling of the magnesium vapor to achieve a physical phase change from gas to liquid of the reaction product of the injection gas and the material vapor. The mixture then enters a circulating cooling device along a tangent line of the mixed gas inlet for circulating cooling and sufficient reaction, and then enters a condensation tank (5) for condensation to obtain a nano magnesium hydrogen powder material. Or when the magnesium vapor generated in the magnesium smelting process by the Pidgeon method or the electrothermal method is used to prepare the condensed nano material as a nano magnesium hydrogen powder material, the continuous production method of the condensed nano material is as follows: After the continuous production system of condensed nanomaterials is evacuated, the protective gas is filled to a preset pressure; Hydrogen is used as the injection gas and the protective gas. The injection gas hydrogen is charged from the air inlet end of a Laval nozzle injection pump (4). At the same time, the magnesium vapor in the magnesium vapor tank body (15) is sucked in through the air inlet end of the Laval nozzle injection pump (4). The hydrogen and the magnesium vapor are mixed and reacted in the Laval nozzle injection pump (4) to release heat. The injection gas hydrogen is used to initially cool the magnesium vapor to achieve a physical phase change from a gaseous state to a liquid state of a reaction product of the injection gas and the material vapor. The mixture then enters a circulating cooling device along a tangent line of the mixed gas inlet for circulating cooling and sufficient reaction. The mixture then enters a condensation tank (5) for condensation to obtain a nano magnesium hydrogen powder material.

10. The method for continuous production of condensed nanomaterials according to claim 9, characterized in that: The prepared nano magnesium hydrogen powder material releases hydrogen after heating to prepare nano magnesium.

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