High-temperature resistant liquid reflux and exhaust structure for preparing fine powders by gas phase method

Abstract

The present invention relates to a high-temperature resistant liquid reflux and exhaust structure for use in preparing fine powder by a vapor phase method, which includes a pipe shared by the liquid reflux and exhaust, and a heat-insulating structure and a case sequentially installed on the outside of the pipe, the lower end of the pipe protruding from the case and inserted into an evaporator and connected to a crucible vapor outlet, the lower end of the case is equipped with a lower connector for connecting to the evaporator housing, and the upper end of the case is equipped with an upper connector for connecting to a back-sequence device. This technical solution achieves heat-insulating design and temperature control by designing an internal circulation pipe connection port so that high-temperature vapor and potentially liquefied or solidified particles accompanied by a carrier gas can be smoothly transported through the pipe shared by the liquid reflux and exhaust, and connected to the internal pipe of other equipment for transfer to the next structure.

Description

[Technical field]

[0001] The present invention relates to the field of fine powder preparation technology, and in particular to a high-temperature resistant liquid reflux and exhaust structure used in the preparation of fine powder by a gas phase method. [Background technology]

[0002] The process of preparing fine powder particles by the vapor phase method of evaporation and concentration is to first heat the material to be prepared at high temperature to vaporize it, and then solidify and mold it from the gaseous state to the liquid state. The fine powder particles to be prepared are minute substances, and most of the fine powder particles are nano, submicron, and micron powders, which are small in size compared to the molded particles, have a very fast molding speed, and are formed at a very high temperature. Although the principle of steam discharge is simple, it is very difficult to apply in practice. After the steam is discharged from the cavity of the crucible, when it cools down, the steam is easily condensed into liquid or solid, and the liquid is easily discharged from the crucible, which results in material loss, solid substances are generated, and the discharge port is blocked, affecting production continuity. Summary of the Invention [Problem to be solved by the invention]

[0003] The objective of the present invention is to provide a high-temperature resistant liquid reflux and exhaust structure for preparing fine powder by a gas phase method, which solves the problem that after the steam is exhausted from the cavity of the crucible, the steam is likely to condense into liquid or solid when cooled, and the liquid is likely to flow out of the crucible, resulting in material loss, the generation of solid substances, and the clogging of the exhaust port, which affects the continuation of production. [Means for solving the problem]

[0004] The present invention provides a high-temperature resistant liquid reflux and exhaust structure for preparing fine powder by a gas phase method, comprising: The present invention includes a pipe shared with liquid reflux and exhaust, one end of which is connected to a crucible vapor outlet and the other end of which is connected to a back sequence device, and a heat insulation structure and a case sequentially installed on the outside of the pipe, the case being a jacket structure, the case being provided with a cooling liquid inlet and a cooling liquid outlet communicating with the jacket structure, the lower end of the pipe protruding from the case and inserted into an evaporator and connected to the crucible vapor outlet, The upper end of the pipe is connected to the back sequence device, A lower connection part is provided at the lower end of the case for connecting with the housing of the evaporator, and an upper connection part is provided at the upper end of the case for connecting with a back sequence device. The temperature inside the piping is between the melting point temperature and the boiling point temperature of the powder material to be prepared. The powder material in the gas phase present in the pipe is exhausted to a back sequence device, and the powder material in the liquid phase is liquid-backflowed to the crucible, so as to prevent the solid of the powder material to be prepared from clogging the pipe. It is characterized by:

[0005] Optionally, the material of the piping is one that is unlikely to react physically or chemically with the powder material prepared under high temperature conditions.

[0007] Optionally, the crucible vapor outlet in the vaporizer, the piping, and the connection port of the backsequence device may all have the same cross-sectional shape and size, or may all have different cross-sectional shapes and sizes.

[0008] Alternatively, the internal shape and inner diameter of the cavity at the connection point where the evaporator and the case are connected, the internal shape and inner diameter of the cavity of the case, and the internal shape and inner diameter of the cavity at the connection point where the backsequence device and the case are connected may be the same or similar, or they may be different. When the internal shape and inner diameter of the cavity at the connection point where the evaporator and the case are connected, the internal shape and inner diameter of the cavity of the case, and the internal shape and inner diameter of the cavity at the connection point where the backsequence device and the case are connected are different, the connection point is a stepped connection or a deformed connection, or the internal shapes and inner diameters of the front and rear cases are different.

[0009] Optionally, the case is multi-tiered or shares a case with an adjacent functional structure.

[0011] Optionally, a fixed structure is provided on the outside of the piping.

[0013] Optionally, the piping is a multi-section splice structure in which two adjacent sections are connected to each other by snaps, or the piping is a functional section in an integral structure of front and rear end equipment. Effect of the Invention

[0014] This technical proposal involves designing an internal circulation piping connection port to smoothly transport high-temperature steam and particles that may have been liquefied or solidified with the carrier gas through a piping that shares liquid reflux and exhaust, and to connect to the internal piping of other equipment so that they can be transferred to the next structure, thereby realizing heat retention design and temperature control. The liquid that is created when the material to be prepared in this piping smoothly melts from solid to liquid or converges to a liquid state can be returned to the crucible in the high-temperature evaporator through this piping. [Brief description of the drawings]

[0015] [Figure 1] FIG. 2 is a schematic diagram of the high-temperature resistant liquid reflux and exhaust structure of the present invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0016] Please note that there is a term The technical solution of the present invention will be described in detail below through the embodiments, which are merely illustrative and can only be used to describe and illustrate the technical solution of the present invention, and cannot be construed as limiting the technical solution of the present invention. In the description of the present invention, the orientations and positional relationships such as "center", "upper", "lower", "left", "right", "front", "rear", "vertical", "horizontal", "inner", and "outer" are based on the orientations and positional relationships shown in the accompanying drawings, and are intended only to facilitate and simplify the description of the present invention, and do not indicate or suggest that the referenced devices or elements are necessarily required. In addition, the terms "first", "second", and "third" are used for descriptive purposes only and are not to be construed as indicating a particular direction, structure, or operation of the referenced devices or elements. The terms "first", "second", and "third" are used for descriptive purposes only and are not to be understood as indicating or suggesting relative importance. It should be noted that in the description of the present invention, unless otherwise expressly specified and limited, the terms "mounted", "connected" and "coupled" are understood in a broad sense, such as fixed connection, detachable connection, integral connection, mechanical connection, electrical connection, direct connection, indirect connection through an intermediate medium, and internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in the context of the present invention in each case.

[0017] In the preparation of powder materials by the vapor-phase method of evaporation and concentration, high-temperature vapor is formed in the crucible in the high-temperature evaporator. The carrier gas passes through the crucible vapor outlet and the connection of the high-temperature resistant liquid reflux and exhaust structure, and enters the common pipe of the high-temperature resistant liquid reflux and exhaust, and the high-temperature energy carried by the high-temperature carrier gas maintains the cavity of the internal pipe of the high-temperature resistant liquid reflux and exhaust structure at a temperature above the melting point of the material to be prepared. The vapor of the powder raw material carried with the high-temperature carrier gas is in the liquid reflux and exhaust pipe, and some of the vapor is cooled, so it condenses into a liquid state, and the particles in the gas or liquid state collide with and adhere to the inner wall of the internal pipe, and the high temperature causes the powder raw material present in the internal pipe to be returned to the crucible through the internal pipe as a liquid phase, or the solid-phase powder raw material present in the internal pipe to be rapidly dissolved into a liquid phase and returned to the crucible. By maintaining a high temperature, it is possible to prevent the solid matter of the prepared powder raw material from clogging the pipe.

[0018] In order to maintain a high temperature state, this manufacturing process is a circulatory process, and the high-temperature air flow in the crucible always carries heat to the structure, and a heat-resistant heat-insulating material is installed on the outside of this structure. In addition, a heating structure (for example, by medium-frequency heating or resistance wire heating) is provided on the outside of the internal piping structure. In addition, in order to protect the internal piping for a long time, a reinforcing structure can be provided on the other side to prevent deformation and damage of the internal piping. High-temperature steam and particles that may have been liquefied or solidified with the carrier gas can be smoothly transported through the piping that shares the liquid return and exhaust, and can be connected to the internal piping of other equipment to move to the next structure. The liquid that is created when the material to be prepared in this piping is smoothly melted from solid to liquid or converges to a liquid state can be returned to the crucible in the high-temperature evaporator through this piping.

[0019] As shown in Fig. 1, the present disclosure provides a high-temperature resistant liquid reflux and exhaust structure for preparing fine powder by a gas phase method. The high-temperature resistant liquid reflux and exhaust structure for preparing fine powder by a gas phase method includes a pipe 9 for liquid reflux and exhaust in common, and a heat-insulating structure 4 and a case 5 sequentially installed on the outside of the pipe 9.

[0020] The lower end of the pipe 9 protrudes from the case 5 and is inserted into the evaporator and connected to the crucible vapor outlet. A lower connection part 3 for connecting to the housing 2 of the evaporator is provided at the lower end of the case 5, and an upper connection part 6 for connecting to a back sequence device is provided at the upper end of the case 5. The upper end of the pipe 9 is connected to the back sequence device.

[0021] In order to provide a structure that can be used for a long period of time in a powder preparation cycle and does not affect the powder being prepared, the material of the piping 9 is one that is unlikely to react physically or chemically with the powder material being prepared under high temperature conditions.

[0022] The inside of the pipe 9 is used for both liquid reflux and exhaust. The temperature inside the pipe 9 is equal to or higher than the melting point temperature of the powder material being prepared, or between the melting point temperature and the boiling point temperature. In this structure, the gas-liquid collision growth phenomenon of powder particles is partially generated to realize the liquid reflux and exhaust functions.

[0023] Between the outer wall of the pipe 9 and the case 5, a heat-retaining structure 4 mainly made of a heat insulating material and a high-temperature resistant material is arranged. The heat-retaining structure 4 insulates the internal structure and controls the internal temperature to be higher than the melting point of the powder material to be prepared, so that the powder material present in the pipe 9 is returned to the crucible as a liquid phase, or the solid phase powder material in the pipe 9 is quickly melted into a liquid phase and returned to the crucible. Maintaining a high temperature prevents the solid of the powder material to be prepared from clogging the pipe 9.

[0024] The case 5 is a jacket structure. The case 5 is provided with a coolant inlet and a coolant outlet that communicate with the jacket structure. Circulating cooling water is supplied into the jacket structure to cool and protect the equipment. The case 5 may be a multi-section structure, or may be shared with the housing of an adjacent functional structure.

[0025] The vapor outlet of the crucible 1 in the evaporator, the piping 9, and the connection port of the back sequence device may have the same cross-sectional shape and dimensions, or may have different cross-sectional shapes and dimensions. Changes in size, ratio, and shape are not alternatives for functionally realizing this structure. The inside of the piping that shares the liquid return and exhaust can be modified.

[0026] The internal shape and inner diameter of the cavity at the connection part where the evaporator and the pipe 9 are connected, the internal shape and inner diameter of the cavity of the case 5, and the internal shape and inner diameter of the cavity at the connection part where the back sequence device and the case are connected are the same, similar, or different. When the internal shape and inner diameter of the cavity at the connection part where the evaporator and the pipe 9 are connected, the internal shape and inner diameter of the cavity of the case 5, and the internal shape and inner diameter of the cavity at the connection part where the back sequence device and the case are connected are different, the connection part is a stepped connection, a deformed connection, or the internal shape and inner diameter of the case 5 are different between the front end case and the rear end case. The selection of the shape, size, and ratio can be designed according to needs, not as a substitute for using the function of this high temperature resistant liquid reflux and exhaust structure. The case is multi-stage connected, or shared with the case of an adjacent functional structure. The size and shape of the case and the front and rear connection methods are not used to limit or change the function of this high temperature resistant liquid reflux and exhaust structure.

[0027] By extending the lower end of the pipe to the connection port 11 between the piping and the crucible vapor outlet inside the crucible vapor outlet structure or inside its rim, the reflux liquid flows into the crucible and does not leak out of the crucible.

[0028] In order to ensure long-term workability in a high-temperature environment, a fixing structure 8 is installed on the outside of the pipe 9, thereby preventing the pipe 9 from being deformed, damaged, or collapsed under high temperatures. The fixing structure 8 may be made of the same material as the pipe 9, or may be made of another high-temperature resistant material. Furthermore, a heating facility 7 may be provided on the outside of the pipe 9.

[0029] The piping 9 is a multi-section splice structure in which two adjacent sections are connected to each other by snaps, or the piping 9 is a functional section in an integral structure of front and rear end equipment.

[0030] Although embodiments of the present invention have been described, it will be understood by those skilled in the art that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principle and spirit of the present invention, the scope of which is best defined by the appended claims. [Explanation of symbols]

[0031] 1: Crucible 2: Evaporator housing 3: Lower connection part 4: Heat retention structure 5: Case 6: Upper connection part 7:Heating equipment 8:Fixed structure 9: Piping 10: Connection port for piping and back sequence device 11: Connection port for piping and crucible vapor outlet

Claims

1. A high-temperature resistant liquid reflux and exhaust structure used for the preparation of fine powders by the vapor phase method, a pipe that shares liquid reflux and exhaust, with one end connected to the crucible evaporation gas outlet and the other end connected to the back-sequence device, a heat insulation structure and a case sequentially installed outside the pipe, the case having a jacket structure, and a coolant inlet and a coolant outlet communicating with the jacket structure being installed in the case, the lower end of the pipe protruding from the case and inserted into the evaporator and connected to the crucible evaporation gas outlet, and the upper end of the pipe being connected to the back-sequence device, a lower connection part for connecting to the housing of the evaporator being installed at the lower end of the case, and an upper connection part for connecting to the back-sequence device being installed at the upper end of the case, the temperature inside the pipe being between the melting point temperature and the boiling point temperature of the powder material to be prepared, the gaseous-phase powder material present in the pipe being exhausted to the back-sequence device, and the liquid-phase powder material being liquid-refluxed to the crucible, such that the solid matter of the powder material to be prepared does not block the pipe, characterized by a high-temperature resistant liquid reflux and exhaust structure used for the preparation of fine powders by the vapor phase method.

2. The high-temperature resistant liquid reflux and exhaust structure used for the preparation of fine powders by the vapor phase method according to Claim 1, characterized in that the material of the pipe is a material that is difficult to react physically or chemically with the powder material prepared under high-temperature conditions.

3. The high-temperature resistant liquid reflux and exhaust structure used for the preparation of fine powders by the vapor phase method according to Claim 1 or Claim 2, characterized in that the cross-sectional shapes and dimensions of the crucible evaporation gas outlet in the evaporator, the pipe, and the connection port of the back-sequence device are the same, or the cross-sectional shapes and dimensions are different.

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