WO2022156227A1

WO2022156227A1 - High-temperature-resistant liquid reflux and air outlet structure for preparing fine powder by gas-phase method

Info

Publication number: WO2022156227A1
Application number: PCT/CN2021/116952
Authority: WO
Inventors: 钟笔
Original assignee: 钟笔
Priority date: 2021-01-25
Filing date: 2021-09-07
Publication date: 2022-07-28
Also published as: TW202229586A; JP2023540814A; TWI820579B

Abstract

The present invention relates to a high-temperature-resistant liquid reflux and air outlet structure for preparing fine powder by a gas-phase method, comprising a channel shared by liquid reflux and air outlet. A thermal preservation structure and a housing are sequentially provided at an outer side of the channel; the lower end of the channel extends out of the housing and is inserted into an evaporator to be connected to a crucible steam outlet; a lower connecting portion is provided at the lower end of the housing to be connected to an evaporator housing; and an upper connecting portion is provided at the upper end of the housing to be connected to a back device. In the technical solution, by means of the design of internal flow conduit connection ports, thermal preservation design, and temperature control, high-temperature steam and possibly liquefied or solidified particles can smoothly pass through the channel shared by liquid reflux and air outlet, and are connected to internal conduits of other devices, so as to be delivered to a next structure.

Description

A high temperature resistant liquid reflux and gas outlet structure for the preparation of fine powder by gas phase method

technical field

The invention belongs to the technical field of fine powder preparation, in particular to a high temperature-resistant liquid reflux and gas outlet structure for the preparation of fine powder by a gas phase method.

Background technique

The process of preparing fine powder particles by evaporation condensation gas phase method is a process in which the material to be prepared is first heated and gasified at high temperature, and then solidified and formed from gaseous state to liquid state. Because the fine powder particles to be prepared are microscopic materials, mostly nano-, sub-micron or micron-scale powders, the formed particles are small in size, very fast in formation, and very high in temperature. Although the technical principle of steam discharge is simple, it is Practical application is very difficult. After the vapor is discharged from the inner cavity of the crucible, it is very easy to condense into liquid or solid in case of condensation. The liquid is easy to flow out of the crucible, resulting in material loss. The appearance of solid can easily cause the outlet to block and affect the continuous production.

SUMMARY OF THE INVENTION

The purpose of the present invention is to provide a high temperature resistant liquid reflux and gas outlet structure for the preparation of fine powder by gas phase method, so as to solve the problem that after the steam is discharged from the inner cavity of the crucible, it is very easy to condense into liquid or solid in case of condensation, and the liquid is easy to flow out of the crucible. In addition, it leads to material loss, and the appearance of solids can easily cause outlet blockage and affect the continuation of continuous production.

The present invention is achieved through the following technical solutions:

A high temperature-resistant liquid return and gas outlet structure for preparing fine powder by a gas phase method, comprising a pipeline for liquid return and gas outlet shared, and a thermal insulation structure and a casing are arranged on the outside of the pipeline in sequence;

The lower end of the pipe extends out of the casing and is inserted into the evaporator to be connected with the crucible evaporation gas outlet;

The lower end of the casing is provided with a lower connecting portion for connecting with the evaporator casing, and the upper end of the casing is provided with an upper connecting portion for connecting with a subsequent device.

Optionally, the material of the pipe is a material that is difficult to produce a physical or chemical reaction with the prepared powder material under high temperature conditions.

Optionally, the temperature inside the pipeline is above the melting point temperature of the prepared powder material, or between the boiling point and the melting point temperature of the prepared powder material.

Optionally, the shape and size of the cross section of the vaporized gas outlet of the crucible in the evaporator, the pipeline and the connection port of the subsequent device are the same in shape and size, or the shape and size of the cross section are different.

Optionally, the inner shape and inner diameter of the inner cavity at the connection between the evaporator and the pipeline, the inner shape and inner diameter of the inner cavity of the outer shell, and the inner shape and inner diameter of the inner cavity at the connection between the subsequent device and the outer shell are the same or similar. Or, the inner shape is not the same as the inner diameter;

If the inner shape and inner diameter are not the same, the connection should be a stepped connection, a gentle deformation connection, or the outer shell should be designed as a transition deformation body of the inner shape and inner diameter of the front and rear shell structures.

Optionally, the casing is connected in multiple sections or shared with casings of adjacent functional structures.

Optionally, the outer shell is of a jacket structure, and a cooling liquid inlet and a cooling liquid outlet communicated with the jacket structure are provided on the outer shell.

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

Optionally, a heating device is provided outside the pipeline.

Optionally, the pipeline is a multi-segment splicing structure, and two adjacent segments are connected by a sub-mother snap; or, the pipeline is a functional segment in an integrated structure of front and rear equipment.

The beneficial effects of the present invention are:

In this technical solution, through the design of the connection port of the internal circulation pipeline, the design of heat preservation and the control of temperature, the high-temperature steam and the particles that may have been liquefied or solidified can smoothly pass through the liquid backflow and the shared gas outlet with the carrier gas, and can be connected with the internal pipelines of other equipment. The connection is fed into the next structure. The solid state of the required preparation material appearing in this pipeline is smoothly melted into a liquid state, or the liquid state produced by the convergence can be returned to the crucible in the high-temperature evaporator through this pipeline.

Description of drawings

FIG. 1 is a schematic structural diagram of the high temperature resistant liquid reflux and gas outlet structure of the present invention.

Description of reference numerals

1. Crucible, 2. Evaporator shell, 3. Lower connecting part, 4. Insulation structure, 5. Shell, 6. Upper connecting part, 7. Heating equipment, 8. Fixed structure, 9. Pipeline, 10. Pipeline and rear The connection port of the sequence device, 11, the connection between the pipeline and the crucible evaporation gas.

Detailed ways

The technical solutions of the present invention will be described in detail by the following examples. The following examples are only exemplary, and can only be used to explain and illustrate the technical solutions of the present invention, but cannot be construed as limitations on the technical solutions of the present invention.

In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "front", "rear", "vertical", "horizontal", "Inner", "outer" and other indications of orientation or positional relationship are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the referred device or element must have a specific orientation, constructed and operated in a particular orientation, and therefore should not be construed as limiting the invention, and the terms "first", "second", and "third" are used for descriptive purposes only and should not be construed as indicating or imply relative importance.

In the description of the present invention, it should be noted that the terms "installed", "connected" and "connected" should be understood in a broad sense, unless otherwise expressly specified and limited, for example, it may be a fixed connection or a detachable connection Connection, or integral connection; may be mechanical connection or electrical connection; may be direct connection, indirect connection through an intermediate medium, or internal communication between two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific situations.

When the powder material is prepared by the evaporation condensation gas phase method, the high temperature steam is formed in the crucible inside the high temperature evaporator. As the carrier gas passes through the crucible vapor outlet and the connection port of the high temperature liquid return and gas outlet structure, it enters the high temperature resistant liquid return and gas outlet shared pipeline, and the high temperature energy carried by the high temperature carrier gas will cause the high temperature liquid return to the internal pipeline of the gas outlet structure. The lumen is maintained above the melting point temperature of the desired preparation material. The powder material vapor carried along with the high-temperature carrier gas is in the liquid return and gas outlet pipeline. Part of the vapor condenses into a liquid state due to the decrease in temperature. The gaseous or liquid particles collide with the inner wall of the internal pipeline and adhere to the high temperature. The powder material in the internal pipeline flows back into the crucible in the liquid phase through the internal pipeline, or the solid phase of the external powder material in the internal pipeline can be quickly melted into a liquid phase and then flow back into the crucible along the pipeline. Maintenance can prevent the occurrence of solids that make powder materials and block the pipeline.

In order to maintain high temperature conditions, this production process is a cyclic production process. The high temperature air flow in the crucible continuously carries heat into the structure, and at the same time, a high temperature-resistant thermal insulation material is provided outside the structure. Moreover, a heating structure (eg, medium frequency heating or resistance wire heating, etc.) can be provided on the outside of the inner pipe structure. In order to protect the internal pipes for long-term work, reinforcement structures can also be provided on other sides to prevent the internal pipes from being deformed or damaged. The high-temperature steam and the particles that may have liquefied or solidified can be smoothly transported to the next structure through the liquid return and gas outlet shared pipelines and the internal pipeline connections of other equipment along with the carrier gas. The solid state of the required preparation material appearing in this pipeline is smoothly melted into a liquid state, or the liquid state generated by the convergence can be returned to the crucible in the high-temperature evaporator through this pipeline.

As shown in FIG. 1 , the present application provides a high-temperature-resistant liquid reflux and gas outlet structure for preparing fine powder by gas phase method, including a pipeline 9 for liquid reflux and gas outlet, and a thermal insulation structure 4 and a casing 5 are arranged on the outside of the pipeline 9 in turn. .

The lower end of the pipe 9 protrudes out of the casing 5 and is inserted into the evaporator to be connected to the crucible evaporation gas outlet. The lower end of the casing 5 is provided with a lower connecting portion 3 for connecting with the evaporator casing 2, the upper end of the casing 5 is provided with an upper connecting portion 6 for connecting with the subsequent device, and the upper end of the pipe 9 is also connected to the subsequent device. device connection.

The material of the pipeline 9 is a material that is not easy to produce physical or chemical reaction with the prepared powder material under high temperature conditions, so as to ensure that its structure can be used for powder preparation cycle production for a long time and does not affect the powder to be prepared. .

The inside of the pipeline 9 is used by liquid return and gas outlet, and the temperature inside the pipeline 9 is above the melting point temperature of the prepared powder material, or between the boiling point and the melting point temperature of the prepared powder material. When the structure realizes the functions of liquid backflow and gas outlet, there is a phenomenon that a part of the powder particles collides and grows in the gas phase or liquid phase.

Between the outer wall of the pipe 9 and the casing 5 is mainly the thermal insulation structure 4, and the thermal insulation structure 4 is made of thermal insulation and high temperature resistant materials. The thermal insulation structure 4 is used for thermal insulation of its internal structure, and the internal temperature is controlled to be above the melting point temperature of the powder material to be prepared, so that the powder material appearing in the pipeline 9 flows back into the crucible in a liquid phase, or is allowed to flow back into the crucible. The solid phase of the powder material in the pipeline 9 can be rapidly melted into a liquid phase and then flow back into the crucible, and the maintenance of high temperature can prevent the phenomenon that the pipeline 9 is blocked by the solid for preparing the powder material.

The casing 5 is a jacket structure, and a cooling liquid inlet and a cooling liquid outlet communicated with the jacket structure are arranged on the casing 5 . Circulating coolant is introduced into the jacket structure to protect the equipment from cooling. The housing 5 can be multi-segmented or shared with housings of adjacent functional structures.

The shape and size of the cross section of the evaporation gas outlet of the crucible 1 in the evaporator, the pipeline 9 and the connection port of the subsequent device are the same, or the shapes and sizes of the cross sections are different. Specifically, it can be selected according to the needs of equipment and use, and the change of the size or ratio or the choice of shape is not considered as other solutions to realize the function of this structure. The inside of the shared pipeline for the outlet and the return can be designed with variable diameter deformation.

The inner shape and inner diameter of the inner cavity at the connection between the evaporator and the pipe 9, the inner shape and inner diameter of the inner cavity of the outer shell 5, and the inner shape and inner diameter of the inner cavity at the connection between the subsequent device and the outer shell are the same or similar, or, The inner shape is not the same as the inner diameter.

If the inner shape and inner diameter are not the same, the connection is a stepped connection, a gentle deformation connection, or the outer shell 5 is designed as a transition deformation body of the inner shape and inner diameter of the front and rear shell structures. The choice of shape, size and proportion can be designed according to the needs of use, not as other solutions for the use of this high temperature resistant liquid return and gas outlet structure function. At the same time, the casing can be connected in multiple sections or shared with the casings of adjacent functional structures. The size, shape and front and rear connection methods of the casing are not intended to limit or change the backflow and air outlet structures.

At the connection 11 between the pipe and the steam outlet of the crucible, the lower end of the pipe needs to be extended into the structure of the steam outlet of the crucible or its edge to ensure that the reflux liquid can flow into the crucible instead of leaking out of the crucible.

Under high temperature conditions, in order to ensure long-term work needs, a fixing structure 8 can be provided on the outer side of the pipeline 9 to prevent the pipeline 9 from being deformed, damaged or collapsed under high temperature. The fixing structure 8 can be made of the same material as the pipe 9, or can be made of other high temperature resistant materials. Furthermore, a heating device 7 may be provided on the outside of the duct 9 .

The pipeline 9 is a multi-segment splicing structure, and two adjacent segments are connected by a sub-mother buckle; or, the pipeline 9 is a functional segment in an integrated structure of front and rear equipment.

Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, and substitutions can be made in these embodiments without departing from the principle and spirit of the invention and variations, the scope of the present invention is defined by the appended claims with full equivalents.

Claims

A high temperature-resistant liquid return and gas outlet structure for preparing fine powder by gas phase method, which is characterized in that it comprises a pipeline for liquid return and gas outlet, and a heat preservation structure and a casing are arranged on the outside of the pipeline in sequence;

The lower end of the pipe extends out of the casing and is inserted into the evaporator to be connected with the crucible evaporation gas outlet;

The lower end of the casing is provided with a lower connecting portion for connecting with the evaporator casing, and the upper end of the casing is provided with an upper connecting portion for connecting with a subsequent device.
The high temperature resistant liquid reflux and gas outlet structure for preparing fine powder by gas phase method according to claim 1, wherein the material of the pipeline is a material that is not easy to produce physical or chemical reaction with the prepared powder material under high temperature conditions.
The high temperature resistant liquid reflux and gas outlet structure for the preparation of fine powder by gas phase method according to claim 1 or 2, characterized in that the temperature inside the pipeline is above the melting point temperature of the prepared powder material, or at the temperature of the prepared powder material. between the boiling and melting points.
The high temperature resistant liquid reflux and gas outlet structure for preparing fine powder by gas phase method according to any one of claims 1 to 3, characterized in that the connection between the crucible evaporation gas outlet, the pipeline and the subsequent device in the evaporator The shape and size of the cross section of the three mouths are the same, or the shape and size of the cross section are different.
The high temperature resistant liquid reflux and gas outlet structure for preparing fine powder by gas phase method according to any one of claims 1 to 4, characterized in that the inner shape and inner diameter of the inner cavity at the connection between the evaporator and the outer shell, the inner cavity of the outer shell The inner shape and inner diameter of the device and the inner shape and inner diameter of the inner cavity at the connection between the subsequent device and the shell are the same or similar, or the inner shape and inner diameter are different;

If the inner shape and inner diameter are not the same, the connection should be a stepped connection, a gentle deformation connection, or the outer shell should be designed as a transition deformation body of the inner shape and inner diameter of the front and rear shell structures.
The high temperature resistant liquid reflux and gas outlet structure for preparing fine powder by gas phase method according to any one of claims 1 to 5, wherein the outer shell is connected in multiple sections or shared with outer shells of adjacent functional structures.
The high temperature resistant liquid reflux and gas outlet structure for preparing fine powder by gas phase method according to any one of claims 1 to 6, wherein the outer shell is a jacket structure, and the outer shell is provided with a connection with the jacket structure coolant inlet and coolant outlet.
The high temperature resistant liquid reflux and gas outlet structure for preparing fine powder by gas phase method according to any one of claims 1 to 7, characterized in that a fixed structure is provided on the outside of the pipeline.
The high temperature resistant liquid reflux and gas outlet structure for preparing fine powder by gas phase method according to any one of claims 1 to 8, characterized in that a heating device is provided outside the pipeline.
The high temperature-resistant liquid reflux and gas outlet structure for preparing fine powder by gas phase method according to any one of claims 1 to 9, wherein the pipeline is a multi-section splicing structure, and a mother card is passed between two adjacent sections. snap connection; or, the pipeline is a functional section in the integrated structure of the front and rear equipment.