JP7688809B2 - High-temperature resistant liquid reflux and exhaust structure for preparing fine powders by gas phase method - Google Patents

Description

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

The process of preparing fine powder particles using the vapor phase method of evaporation and concentration is a process in which the material to be prepared is first heated at a high temperature to vaporize it, and then solidified and molded from the gaseous state into a liquid state. The fine powder particles to be prepared are tiny substances, and most of the fine powder particles are nano, submicron, or micron powders. Compared to molded particles, they are small in size, 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 likely to condense into liquid or solid, and the liquid is likely to flow out of the crucible, which results in material loss, solid substances are generated, and the discharge port is blocked, affecting production continuity.

The object of the present invention is to provide a high-temperature resistant liquid reflux and exhaust structure for use in preparing fine powders by the vapor phase method, which solves the problem that after vapor is discharged from the cavity of the crucible, the vapor 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 and the generation of solid substances that block the exhaust port and affect production continuity.

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 is characterized in that it includes a pipe that shares 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 backsequence device, and a heat-insulating structure and a case that are sequentially installed on the outside of the pipe, the case having a jacket structure, a cooling liquid inlet and a cooling liquid outlet that communicate with the jacket structure, a lower end of the pipe protruding from the case and inserted into an evaporator and connected to the crucible vapor outlet, an upper end of the pipe connected to the backsequence device, a lower connection part for connecting to a housing of the evaporator is installed at the lower end of the case, and an upper connection part for connecting to the backsequence device is installed at the upper end of the case, the temperature inside the pipe 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 the backsequence device, and the powder material in the liquid phase is liquid-refluxed to the crucible, so that the solid of the powder material to be prepared does not clog the pipe .

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.

Optionally, the crucible vapor outlet in the evaporator, the piping, and the connection port of the backsequence device have the same cross-sectional shape and dimensions, or the cross-sectional shapes and dimensions are different.

Optionally, the internal shape and inner diameter of the cavity at the connection point where the evaporator and 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 case are connected are the same or similar, or are different. If the internal shape and inner diameter of the cavity at the connection point where the evaporator and 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 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 end cases are different.

Optionally, the case is multi-stage connected or shares a case with an adjacent functional structure.

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

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.

This technical proposal involves smoothly transporting high-temperature steam and particles that may have been liquefied or solidified and are accompanied by a carrier gas through piping that shares liquid reflux and exhaust, and connecting them 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 being 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.

FIG. 2 is a schematic diagram of the high-temperature resistant liquid reflux and exhaust structure of the present invention.

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 directions and positional relationships such as "center", "upper", "lower", "left", "right", "front", "rear", "vertical", "horizontal", "inner", and "outer" are based on the directions 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.

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 part of the high-temperature resistant liquid reflux and exhaust structure, and enters the common pipe for 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 pipes, 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 pipes.

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 heat-resistant insulation materials are 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 or 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 a pipe that shares the liquid return and exhaust, and can be connected to the internal piping of other equipment and transferred to the next structure. The liquid that is created when the material to be prepared in this pipe 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 pipe.

As shown in FIG. 1, the present disclosure provides a high-temperature resistant liquid reflux and exhaust structure for use in preparing fine powder by a gas phase method. The high-temperature resistant liquid reflux and exhaust structure for use in preparing fine powder by a gas phase method includes a pipe 9 that shares the liquid reflux and exhaust, and a heat-retaining structure 4 and a case 5 that are sequentially installed on the outside of the pipe 9.

The lower end of the piping 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 piping 9 connects to the back sequence device.

In order to ensure that the structure can be used for a long period of time in the 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.

The inside of pipe 9 is used for both liquid reflux and exhaust. The temperature inside 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 achieve the liquid reflux and exhaust functions.

A heat-retaining structure 4, mainly made of insulating material and high-temperature resistant material, is disposed between the outer wall of the pipe 9 and the case 5. The heat-retaining structure 4 insulates the internal structure and controls the internal temperature to above the melting point of the powder material being 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 quickly melts into a liquid phase and is returned to the crucible. Maintaining a high temperature prevents the solids of the powder material being prepared from clogging the pipe 9.

The case 5 has a jacket structure. The case 5 is provided with a cooling liquid inlet and a cooling liquid outlet that communicate with the jacket structure. Circulating cooling water is supplied inside 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.

The vapor outlet of the crucible 1 in the evaporator, the piping 9, and the connection port of the back sequence device have the same cross-sectional shape and dimensions, or they 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.

The internal shape and inner diameter of the cavity at the connection point where the evaporator and piping 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 point 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 point where the evaporator and piping 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 point where the back sequence device and the case are connected are different, the connection point is a stepped connection, a deformed connection, or the internal shape and inner diameter of the front end case and the rear end case of the case 5 are different. 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, as well as the front and rear connection method, are not used to limit or change the functionality of this high-temperature resistant liquid reflux and exhaust structure.

By extending the lower end of the pipe to the inside of the crucible vapor exhaust structure or within its rim, the reflux liquid flows into the crucible and does not leak out of the crucible.

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, which can prevent the pipe 9 from deforming, breaking, or collapsing 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 device 7 may be provided on the outside of the pipe 9.

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

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

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

Claims (3)

A high-temperature resistant liquid reflux and exhaust structure for preparing fine powder by a gas phase method,
A pipe shared with liquid reflux and exhaust, one end of which is connected to the crucible vapor outlet and the other end of which is connected to a back sequence device;
a heat insulating structure and a case sequentially installed on the outside of the piping, 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 protrudes from the case and is inserted into the evaporator and connected to a crucible vapor outlet, and 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 pipe 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 a crucible;
Ensure that the solids of the powder ingredients being prepared do not block the piping .
A high-temperature resistant liquid reflux and exhaust structure used in the preparation of fine powder by a vapor phase method. The high-temperature resistant liquid reflux and exhaust structure used in the preparation of fine powders by the gas phase method described in claim 1, characterized in that the material of the piping is a material that is unlikely to react physically or chemically with the powder material prepared under high-temperature conditions. 3. A high-temperature resistant liquid reflux and exhaust structure used for preparing fine powder by a gas phase method as described in claim 1 or claim 2, characterized in that the cross-sectional shapes and dimensions of the crucible vapor outlet in the evaporator, the piping, and the connection port of the back-sequence device are the same or different.

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