CN116440813A - Preparation method and device of high-purity silicon carbide lining for fluidized bed - Google Patents

Preparation method and device of high-purity silicon carbide lining for fluidized bed Download PDF

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Publication number
CN116440813A
CN116440813A CN202310490325.1A CN202310490325A CN116440813A CN 116440813 A CN116440813 A CN 116440813A CN 202310490325 A CN202310490325 A CN 202310490325A CN 116440813 A CN116440813 A CN 116440813A
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silicon carbide
fluidized bed
purity silicon
lining
movable units
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王建忠
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Xi'an Zhongwei New Material Co ltd
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Xi'an Zhongwei New Material Co ltd
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/24Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
    • B01J8/34Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with stationary packing material in the fluidised bed, e.g. bricks, wire rings, baffles
    • BPERFORMING OPERATIONS; TRANSPORTING
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Abstract

The invention belongs to the technical field of preparation of silicon carbide materials, and particularly relates to a preparation method and a preparation device of a high-purity silicon carbide lining for a fluidized bed, wherein the high-purity silicon carbide lining comprises an outer shell, a deformable inner lining body is arranged in the outer shell, and the inner lining body is connected with the outer shell through an elastic part; the lining body comprises a plurality of movable units which are spliced together, each movable unit is provided with an arc-shaped part, an outer protruding part and an inner protruding part, when all the movable units are gathered together, the movable units can be spliced together, when the movable units are scattered, the distance between the movable units is increased, but after the movable units are scattered, the positions of the outer edges of the movable units still have contact, and boiling materials in a fluidized bed cannot leak out from gaps between the adjacent movable units. The method and the device can prepare the columnar silicon carbide lining, can reduce resource waste and are beneficial to environmental protection.

Description

Preparation method and device of high-purity silicon carbide lining for fluidized bed
Technical Field
The invention belongs to the technical field of preparation of silicon carbide materials, and particularly relates to a preparation method and a device of a high-purity silicon carbide lining for a fluidized bed.
Background
Silicon carbide has good high temperature resistance and corrosion resistance, and high strength, and is prepared by a reaction sintering method generally because of the chemical characteristics of silicon carbide materials and difficult molding. The reaction sintering method comprises the steps of powder preparation, compact pressing, drying, sintering and the like, wherein the parameters involved in the steps are most, such as reasonable raw materials in proportion and powder with a proper particle size are required to be prepared in a powder preparation stage, reasonable pressure conditions and compact size design are required in a compact pressing stage, temperature setting and treatment time setting in the drying and sintering stage are required, and indexes such as hardness of a finished product can be influenced if the design is unreasonable.
Briquette pressing is a critical operation for the preparation of silicon carbide materials, and there are many devices related to briquette pressing in the prior art, such as CN107098702B, CN107127999A, CN211567043U and CN113601894a. However, these devices are mostly adapted to flat plate-type briquettes, and the technical solutions of these patents cannot meet the preparation requirements for briquettes having inconsistent heights or irregular shapes.
The fluidized bed has the working principle that solid powder catalyst is filled in a hollow columnar reactor, gas phase materials enter from the bottom of the reactor to make the powder catalyst in a boiling state, the gas phase materials carry out chemical reaction on the surface of the boiling catalyst, and the reacted gas phase materials are discharged from the top of the reactor. A portion of the catalyst is withdrawn in the middle of the reactor and fresh catalyst is fed in below the reactor. Since some reactions are required to be performed under severe conditions such as high temperature, silicon carbide devices are required to be installed as a liner on the inner wall of a reactor, such as chinese patent CN105617955a. However, the fluidized bed reactor is columnar and the required silicon carbide device liner is also nearly columnar, such as the columnar (annular) liner described in chinese patent CN105617955a, and the prior art lacks a method for preparing columnar silicon carbide liners.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method and a device for a high-purity silicon carbide lining of a fluidized bed, which can prepare a columnar silicon carbide lining
The invention aims to provide a high-purity silicon carbide lining for a fluidized bed, which comprises an outer shell, wherein a deformable lining body is arranged in the outer shell, and the lining body is connected with the outer shell through an elastic part;
the lining body comprises a plurality of movable units which are spliced together, each movable unit is provided with an arc-shaped part, an outer protruding part and an inner protruding part, when all the movable units are gathered together, the movable units can be spliced together, when the movable units are scattered, the distance between the movable units is increased, but after the movable units are scattered, the positions of the outer edges of the movable units still have contact, and boiling materials in a fluidized bed cannot leak out from gaps between the adjacent movable units.
Preferably, the high-purity silicon carbide lining for the fluidized bed is provided with perforations in corresponding positions on the lining body and the outer shell body, and the perforations can be closed by a closing head.
The invention aims to provide a preparation device for a high-purity silicon carbide lining of a fluidized bed, which comprises a support frame, an upper grinding tool, a lower die and a telescopic device, wherein the telescopic device is arranged between the support frame and the upper grinding tool, the lower die is arranged between the upper grinding tool and the support frame, and the lower die is arranged on the support frame.
Preferably, in the above preparation device for a high purity silicon carbide lining of a fluidized bed, the top of the supporting frame is connected with the top of the telescopic device, the bottom of the telescopic device is connected with the upper grinding tool, the lower die is arranged at the bottom of the supporting frame and is located below the upper grinding tool, and along with the extension of the telescopic device, the upper grinding tool can be embedded into a model groove arranged on the lower die.
Preferably, the above preparation device for a high purity silicon carbide lining of a fluidized bed, wherein the mold tank comprises an outer protruding cavity, a middle cavity and an inner protruding cavity which are sequentially communicated, the outer protruding cavity is matched with the outer protruding part in shape, the middle cavity is matched with the arc-shaped part in shape, and the inner protruding cavity is matched with the inner protruding part in shape.
Preferably, in the above preparation device for a high-purity silicon carbide liner of a fluidized bed, the upper grinding tool comprises a supporting plate, the top of the supporting plate is connected with the supporting frame, the bottom of the supporting plate is connected with the top of a fixing rod, the top of an elastic layer is installed at the bottom of the supporting plate and the position where the fixing rod is not arranged, the bottom of the elastic layer is connected with a pressing plate, the shape of the outer wall of the pressing plate is matched with the shape of a model groove, a cavity is arranged between the inner wall of the pressing plate and the elastic layer, an opening is arranged at the position of the pressing plate corresponding to the perforation, and the fixing rod is penetrated in the opening;
the position of the model groove corresponding to the perforation is provided with a vertical cavity, and along with the extension of the telescopic device, the bottom of the fixing rod can be inserted into the vertical cavity in a matched mode.
Preferably, in the preparation device for the high-purity silicon carbide lining of the fluidized bed, the fixing rod is a hollow pipe body inserted into the vertical cavity, and the extrusion block is arranged in the pipe body.
Preferably, the preparation device for the high-purity silicon carbide lining of the fluidized bed is characterized in that the inner wall of the pipe body is provided with lines, and the outer wall of the pipe body is smooth.
The invention aims to provide a preparation method of a high-purity silicon carbide lining for a fluidized bed, which comprises the following steps:
the manufacturing lining body specifically comprises: weighing the raw materials of the lining body according to the proportion, mixing, pressing, forming, drying the biscuit and sintering at high temperature;
manufacturing an outer shell, and forming a perforation on the outer shell;
and connecting an elastic part between the outer shell and the inner lining body to finally prepare the high-purity silicon carbide inner lining.
The invention aims to provide a preparation method of a high-purity silicon carbide lining for a fluidized bed, which comprises the following steps:
the manufacturing lining body specifically comprises: weighing all raw materials of the inner lining body according to the proportion, grinding, mixing, granulating, pressing and forming, pressing a blank of the inner lining body by using the preparation device of the high-purity silicon carbide inner lining for the fluidized bed, drying the blank, and sintering at high temperature;
manufacturing an outer shell, and forming a perforation on the outer shell;
and connecting an elastic part between the outer shell and the inner lining body to finally prepare the high-purity silicon carbide inner lining.
Compared with the prior art, the invention has the following beneficial effects:
the invention develops a deformable inner lining body, which can move towards the outer shell to form a gathering state, and can also move towards the direction far away from the outer shell to form a dispersing state, namely, when the inner lining body is arranged in a vertically arranged fluidized bed reactor, the inner lining body can move back and forth in the horizontal direction or the direction close to the horizontal direction, after the boiled material collides with the inner wall of the inner lining body, the kinetic energy conversion occurs, and a part of the kinetic energy of the boiled material is consumed, so that the excessive boiling of the material can be prevented, namely, the inner lining body simulates the zeolite effect and the bumping is prevented. The material in the lining body can not only move up and down in a boiling way, but also move left and right to a great extent, the kinetic energy of the consumed material is more, the probability of discharging the consumed material from the top of the reactor is reduced, the resource waste is reduced, and the environment is protected. On the other hand, because the elastic component has the elastic action in the horizontal direction on the inner lining body, the elastic component can have the transverse vibration action on the materials, so that the reaction efficiency of the materials in the fluidized bed reactor is not affected, but the probability of discharging the materials from the top of the reactor can be reduced.
The inner lining body comprises a plurality of movable units which are spliced together, boiling materials cannot leak out from gaps between the two movable units, and the boiling materials can only move up and down or collide with the inside of the movable units.
Because the green body in the vertical cavity is used for manufacturing the sealing head, and the sealing head needs to be frequently disassembled and installed, the strength requirement is higher than that of the inner lining body, and the device can simultaneously prepare two green bodies with different compactness and strength, and has strong adaptability. The one-step forming preparation device is high in efficiency, and a blank of the inner lining body and a blank of the closing head are prepared.
The preparation method of the high-purity silicon carbide lining for the fluidized bed has strong practicability and high operability, and is matched with a unique high-purity silicon carbide lining structure and a blank manufacturing device, so that the manufacturing efficiency is high.
Drawings
FIG. 1 is a schematic view of the high purity silicon carbide liner for fluidized bed according to example 1 of the present invention (the liner is in a dispersed state).
Fig. 2 is a schematic view of the high purity silicon carbide liner structure for fluidized bed according to example 1 of the present invention (the liner is in a gathered state).
Fig. 3 is a schematic structural diagram of a movable unit according to embodiment 1 of the present invention.
FIG. 4 is a longitudinal sectional view of an apparatus for preparing a high purity silicon carbide liner for a fluidized bed according to example 2 of the present invention.
Fig. 5 is an operation state diagram of a preparation apparatus of a high purity silicon carbide liner for a fluidized bed according to example 2 of the present invention.
Detailed Description
In order that those skilled in the art will better understand the technical scheme of the present invention, the present invention will be further described with reference to specific embodiments and drawings.
In the description of the present invention, unless otherwise specified, all reagents are commercially available and methods are conventional in the art.
In the description of the present invention, the raw material composition of the high purity silicon carbide liner was the powder composition described in example 1 of CN 107098702B: 1000g of silicon carbide powder, 206g of phenolic resin, 100g of pore-forming agent, 200g of graphite powder, 3000g of ethanol and 50g of surfactant (carbon powder dispersing agent).
Alternatively, the raw materials of the high purity silicon carbide liner are composed of ingredients described in CN108203300 a: a base material, a dispersant, a plasticizer and a lubricant;
the base stock consists of submicron silicon carbide (d50=700 nm) and a sintering aid (d50=1.2 μm), the submicron silicon carbide accounting for 96% of the total weight of the base stock, and the sintering aid accounting for 4% of the total weight of the base stock;
the dispersant accounts for 0.8% of the total weight of the base material, the plasticizer accounts for 2.5% of the total weight of the base material, and the lubricant accounts for 3% of the total weight of the base material;
the sintering aid consists of aluminum nitride, aluminum oxide and yttrium oxide, wherein the aluminum nitride, the aluminum oxide and the yttrium oxide account for 1.4 percent, 1.6 percent and 1 percent of the total weight of the base material;
the dispersing agent is tetramethyl ammonium hydroxide;
the plasticizer is PVA water solution with the mass concentration of 10%;
the lubricant consists of polyethylene glycol and glycerin, wherein the polyethylene glycol accounts for 1.5% of the total weight of the base material, and the glycerin accounts for 1% of the total weight of the base material.
The raw material composition of the reaction sintering silicon carbide ceramic large boat can also adopt the powder composition described in the embodiment 1 of CN 107098702B: 1000g of silicon carbide powder, 206g of phenolic resin, 100g of pore-forming agent, 200g of graphite powder, 3000g of ethanol and 50g of surfactant (carbon powder dispersing agent).
Of course, other silicon carbide material formulations may be selected by those skilled in the art to produce high purity silicon carbide liners without departing from the inventive concepts of the present invention.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention. The terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first", "a second" may include one or more such features, either explicitly or implicitly; in the description of the present invention, unless otherwise indicated, the meaning of "a plurality" is two or more.
Example 1
A high purity silicon carbide liner for a fluidized bed, the structure of which is seen in fig. 1-3, comprising an outer shell 1, the outer shell 1 matching the shape of the portion of the fluidized bed reactor for containing catalyst, to facilitate installation of the outer shell 1 within the fluidized bed reactor. The outer shell 1 is a silicon carbide material or a material which does not participate in a catalytic reaction. The outer shell 1 is not deformable.
The inside of the outer shell 1 is provided with a deformable inner lining body 2, and the inner lining body 2 is connected with the outer shell 1 through an elastic part 3. The inner lining body 2 and the elastic component 3 are matched with each other, and the inner lining body 2 and the elastic component 3 can deform.
The inner wall of the common fluidized bed reactor cannot be deformed, but a plurality of openings are arranged to meet the requirements of sample injection or sample discharge; however, as the gas-phase materials enter from the bottom of the fluidized bed reactor, the powdery catalyst is in a boiling state, the gas-phase materials perform chemical reaction on the surface of the boiling catalyst, the reacted gas-phase materials are discharged from the top of the reactor, the boiling materials continuously move upwards along with the gas in the vertical direction, the moving amplitude in the horizontal direction is small, and then the materials can possibly discharge along with the gas flow from the top of the reactor to cause resource waste, so that the environment protection is not facilitated. Therefore, the invention develops a deformable inner liner 2, the inner liner 2 can move towards the direction of the outer shell 1, so that the inner liner 2 is in a dispersed state shown in fig. 1, the inner liner 2 can move towards the direction away from the outer shell 1, so that the inner liner 2 is in a gathered state shown in fig. 2, that is, the inner liner 2 can move back and forth in the horizontal direction or the direction close to the horizontal direction, after the boiled material collides with the inner wall of the inner liner 2, kinetic energy conversion occurs, a part of kinetic energy of the boiled material is consumed, and excessive boiling of the material can be prevented, namely, the inner liner 2 simulates the zeolite effect and bumping is prevented. The material in the lining body 2 not only can be boiled up and down and move left and right, but also can be moved left and right greatly, the kinetic energy of the consumed material is more, the probability of discharging the consumed material from the top of the reactor is reduced, the resource waste is reduced, and the environment protection is facilitated. On the other hand, because the elastic component has the elastic action in the horizontal direction on the inner lining body, the elastic component can have the transverse vibration action on the materials, so that the reaction efficiency of the materials in the fluidized bed reactor is not affected, but the probability of discharging the materials from the top of the reactor can be reduced.
Illustratively, the elastic member 3 is a spring, an elastic balloon or other material with a telescopic function, the elastic member 3 can be extruded and deformed by the inner liner 2, and when the extrusion force of the inner liner 2 is eliminated, the elastic member 3 can automatically recover the original shape. The elastic member 3 has a vibrating action.
Illustratively, the inner liner body 2 includes a plurality of movable units that are spliced together, for example, two movable units are spliced to form a cylindrical inner liner body 2, and the movable units have a structure shown in fig. 3 and include an arc portion 21, an outer protruding portion 22 and an inner protruding portion 23, and the arc portion 21, the outer protruding portion 22 and the inner protruding portion 23 are integrally formed. When the two movable units move oppositely, the two movable units can be spliced into a cylinder; when the two movable units move backwards, the two movable units can be separated, but the positions of the outer edges still have contact, boiling materials in the fluidized bed cannot leak out from a gap between the two movable units, and the boiling materials can only move up and down or collide with the inside of the movable units.
Illustratively, the inner liner 2 and the outer liner 1 are provided with perforations, and the positions of the perforations on the inner liner 2 and the outer liner 1 are corresponding, so that a pipeline is conveniently installed at the perforations, feeding and discharging operations can be performed through the pipeline, and redundant perforations are closed by the closing head 11.
Example 2
The preparation device for the high-purity silicon carbide lining of the fluidized bed, which is shown in fig. 4-5, comprises a supporting frame 4, an upper grinding tool 5, a lower die 6 and a telescopic device 7. The support frame 4 is supporting role, and telescoping device 7 is installed between support frame 4 and last grinding apparatus 5, and lower mould 6 is located between last grinding apparatus 5 and the support frame 4. The lower die 6 is mounted on the support frame 4. The raw materials for manufacturing the high-purity silicon carbide are positioned in the lower die 6, the telescopic device 7 generates acting force on the upper grinding tool 5 after being extended, the upper grinding tool 5 is driven to move towards the lower die 6, pressure is generated, and the raw materials are pressed into blanks. The telescopic means 7 are pressure-providing, which are electric telescopic rods or hydraulic rods.
The support frame 4 is illustratively a cubic frame, or a frame having a top wall and a bottom wall. The roof of support frame 4 is connected with the top of telescoping device 7, and the bottom of telescoping device 7 is connected with the grinding apparatus 5, and bed die 6 sets up at the support frame 4 diapire to be located the grinding apparatus 5 below. When the expansion device 7 is extended, the upper grinding tool 5 moves downwards, and can be embedded into a model groove 61 arranged on the lower die 6.
In order to prepare the inner liner 2 having a shape matching the inner wall of the fluidized-bed reactor, the mold groove 61 is of a shape matching the movable unit, the mold groove 61 includes an outer protruding cavity 611, a middle cavity 612, and an inner protruding cavity 613, the outer protruding cavity 611, the middle cavity 612, and the inner protruding cavity 613 are sequentially communicated, the outer protruding cavity 611 is matched with the outer protruding portion 22 in shape, the middle cavity 612 is matched with the arc-shaped portion 21 in shape, and the inner protruding cavity 613 is matched with the inner protruding portion 23 in shape. The bottom shape of the upper grinding tool 5 also matches the shape of the mold groove 61.
The upper grinding tool 5 includes a supporting plate 51, a fixing rod 52, an elastic layer 53, and a pressing plate 54, wherein the top of the supporting plate 51 is connected with the bottom of the telescopic device 7, the bottom of the supporting plate 51 is connected with the top of the fixing rod 52, the top of the elastic layer 53 is installed at the position of the bottom of the supporting plate 51, where the fixing rod 52 is not arranged, the bottom of the elastic layer 53 is connected with the pressing plate 54, the shape of the outer wall of the pressing plate 54 is matched with the shape of the model groove 61, and a cavity is formed between the inner wall of the pressing plate 54 and the elastic layer 53. When the inner liner body 2 and the outer casing 1 are provided with perforations, the positions of the pressing plate 54 corresponding to the perforations are provided with openings, each opening is internally provided with a fixing rod 52 in a penetrating manner, the positions of the model grooves 61 corresponding to the perforations are provided with vertical cavities 614, the number of the vertical cavities 614 corresponds to that of the fixing rods 52 one by one, the vertical cavities 614 are shell structures with inner and outer spaces separated, and the bottoms of the fixing rods 52 can be inserted into the vertical cavities 614 in a matched manner.
When the telescopic device 7 is contracted, the vertical cavity 614 is separated from the fixed rod 52, the upper grinding tool 5 is also separated from the model groove 61, and the structure is shown in fig. 4, and the bottom of the fixed rod 52 is positioned near the opening of the pressing plate 54. The raw material for producing the high purity silicon carbide inner liner blank is poured into the mold tank 61, and the raw material for producing the high purity silicon carbide inner liner blank is also contained in the vertical cavity 614. Then the expansion device 7 is extended, the upper grinding tool 5 is gradually close to the model groove 61, the fixing rod 52 is also close to the vertical cavity 614, when the pressing plate 54 is abutted against the raw material for producing the high-purity silicon carbide lining blank in the model groove 61, the fixing rod 52 is abutted against the raw material for producing the high-purity silicon carbide lining blank in the vertical cavity 614, the operation of pressing the blank is carried out, at the moment, the blank in the vertical cavity 614 is separated from the blank in the rest position, the expansion device 7 is contracted in the future, after the upper grinding tool 5 is removed, the blank in the vertical cavity 614 is taken out for producing the closing head 11, and at the moment, the raw material pressure is not in the most solid state, so that the production requirement of low strength requirement of the silicon carbide lining is met.
From one perspective, if the compression plate 54 is in contact with the material of the mold tank 61 for producing the high purity silicon carbide inner liner blank, the fixing rod 52 is in contact with the material of the vertical cavity 614 for producing the high purity silicon carbide inner liner blank, and then the expansion device 7 is further extended, the elastic layer 53 is forced to compress, and in addition, the blocking of the mold tank 61 and the material of the high purity silicon carbide inner liner blank is performed, the downward movement amplitude of the compression plate 54 is smaller than that of the fixing rod 52, and the fixing rod 52 can be inserted into the vertical cavity 614 to press the blank in the vertical cavity 614 more firmly. Because the blanks in the vertical cavity 614 are used for manufacturing the closing head 11, and the closing head 11 needs to be frequently disassembled and installed, the strength requirement is higher than that of the inner lining body 2, and two blanks with different compactness can be simultaneously manufactured by the device provided by the invention, so that the device has strong adaptability.
From another angle, in order to facilitate the removal of the blank in the vertical cavity 614, the bottom of the fixing rod 52, which is used for being inserted into the vertical cavity 614, is a hollow pipe 521, an extrusion block is arranged in the pipe 521, the extrusion block is used for extruding the blank in the vertical cavity 614, the inner wall of the pipe 521 is provided with lines, the outer wall of the pipe 521 is smooth, and the outer wall of the pipe 521 is used for being in contact with the inner wall of the vertical cavity 614, then, along with the compression of the elastic layer 53, the pipe 521 is inserted into the vertical cavity 614, the pipe 521 and the extrusion block are pressed into a blank while the lines are formed on the outer wall of the blank in the pipe 521, and then, when the telescopic device 7 is contracted, the blank 521 is also moved upwards under the action of friction force, and other blanks in the model groove 61 are not worry damaged when the blank is removed from the pipe 521. Moreover, after the outer wall of the blank in the pipe body 521 is textured, the outer wall of the finally manufactured sealing head 11 is textured, so that the firmness of the sealing ring sleeved on the sealing head 11 is better, and the sealing effect of the sealing head 11 in the perforation is also better.
This embodiment has developed a one-shot forming manufacturing apparatus, which is efficient in manufacturing the blank of the inner liner 2 and the blank of the closing head 11.
Example 3
A method of preparing a high purity silicon carbide liner for a fluidized bed, comprising:
manufacturing an inner lining body (2):
1) Weighing all raw materials of the lining body (2) according to the proportion;
2) Ball milling and mixing:
3) And (3) spray granulation:
for a specific method of operation of raw material, ball milling mixing and spray granulation reference is made to the procedure of example 1 of CN108203300 a;
4) And (5) press forming:
performing compression molding of the inner liner body using the apparatus of example 1 or example 2 of the present invention;
5) And (5) biscuit baking:
the pressed biscuit is firstly preserved for 1h at 60 ℃, then is heated to 120 ℃ for 4h, then is heated to 800 ℃ in inert gas environment at the speed of 2 ℃/min, is preserved for 2h, and removes wax substances in the biscuit; the inert gas argon is adopted for protection during the process.
6) Oxidizing and removing carbon in air:
placing the biscuit processed in the step 5) into an oxidation furnace, heating up in the atmospheric environment, heating up to 450 ℃ at 1.5 ℃/min, preserving heat for 2.5 hours, and oxidizing to remove free carbon in the biscuit;
7) High-temperature sintering:
orderly loading the treated biscuit into a hot isostatic pressing sintering furnace, closing a furnace door, opening a vacuum pump to vacuum, heating to 900 ℃ at 5 ℃/min, preserving heat for 40min, closing the vacuum pump, starting to charge argon until the pressure gauge of the sintering furnace shows 0.01bar, heating to 1200 ℃ at 4 ℃/min, and preserving heat for 1.5h; then argon is filled until the pressure gauge shows 5bar, the temperature is increased to 1900 ℃ at 3 ℃/min, and the temperature is kept for 1.5h; then argon is filled until the pressure gauge shows 95bar, the temperature is raised to 1950 ℃ at 1 ℃/min, the temperature is kept for 15min, a heating system is closed, the pressure in the furnace is kept unchanged, the pressure is relieved when the temperature is reduced to 1500 ℃, and then the furnace is cooled to room temperature along with the furnace and opened. Is made into an inner lining body (2).
The outer shell (1) is manufactured by a cylindrical grinding tool in the prior art, for example, the outer shell 1 made of alloy materials is provided with perforations, an elastic component (3) is connected between the outer shell (1) and the inner shell 2, and finally, the high-purity silicon carbide inner liner is manufactured.
It should be noted that, the connection relationships of the components not specifically mentioned in the present invention are all default to the prior art, and the connection relationships of the structures are not described in detail because they do not relate to the invention points and are common applications of the prior art.
It should be noted that, when numerical ranges are referred to in the present invention, it should be understood that two endpoints of each numerical range and any numerical value between the two endpoints are optional, and because the adopted step method is the same as the embodiment, in order to prevent redundancy, the present invention describes a preferred embodiment. While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.

Claims (10)

1. The high-purity silicon carbide lining for the fluidized bed is characterized by comprising an outer shell (1), wherein a deformable inner lining body (2) is arranged inside the outer shell (1), and the inner lining body (2) is connected with the outer shell (1) through an elastic part (3);
the lining body (2) comprises a plurality of movable units which are spliced together, each movable unit is provided with an arc-shaped part (21), an outer protruding part (22) and an inner protruding part (23), when all the movable units are gathered together, the movable units can be spliced together, when the movable units are scattered, the distance between the movable units is increased, but after the movable units are scattered, the positions of the outer edges of the movable units still have contact, and boiling materials in a fluidized bed cannot leak out from gaps between the adjacent movable units.
2. The high-purity silicon carbide lining for a fluidized bed according to claim 1, characterized in that the lining body (2) and the outer shell (1) are provided with perforations at corresponding positions, which can be closed by a closing head (11).
3. A device for preparing a high purity silicon carbide lining for a fluidized bed according to claim 2, comprising a support frame (4), an upper grinding tool (5), a lower die (6) and a telescopic device (7), wherein the telescopic device (7) is installed between the support frame (4) and the upper grinding tool (5), the lower die (6) is located between the upper grinding tool (5) and the support frame (4), and the lower die (6) is installed on the support frame (4).
4. A preparation device for a high purity silicon carbide lining for a fluidized bed according to claim 3, wherein the top of the supporting frame (4) is connected with the top of the telescopic device (7), the bottom of the telescopic device (7) is connected with the upper grinding tool (5), the lower die (6) is arranged at the bottom of the supporting frame (4) and below the upper grinding tool (5), and the upper grinding tool (5) can be embedded into a model groove (61) arranged on the lower die (6) along with the extension of the telescopic device (7).
5. The apparatus for preparing a high purity silicon carbide liner for a fluidized bed as set forth in claim 4, wherein the mold tank (61) comprises an outer protruding cavity (611), a middle cavity (612) and an inner protruding cavity (613) which are sequentially communicated, the outer protruding cavity (611) is matched with the outer protruding portion (22) in shape, the middle cavity (612) is matched with the arc portion (21) in shape, and the inner protruding cavity (613) is matched with the inner protruding portion (23) in shape.
6. The preparation device for the high-purity silicon carbide lining of the fluidized bed according to claim 5, wherein the upper grinding tool (5) comprises a supporting plate (51), the top of the supporting plate (51) is connected with the supporting frame (4), the bottom of the supporting plate (51) is connected with the top of a fixing rod (52), an elastic layer (53) is installed at the position, which is not provided with the fixing rod (52), of the bottom of the supporting plate (51), a pressing plate (54) is connected with the bottom of the elastic layer (53), the shape of the outer wall of the pressing plate (54) is matched with the shape of the model groove (61), a cavity is formed between the inner wall of the pressing plate (54) and the elastic layer (53), an opening is formed in the position, corresponding to the perforation, of the pressing plate (54), and the fixing rod (52) is penetrated in the opening;
the position of the model groove (61) corresponding to the perforation is provided with a vertical cavity (614), and along with the extension of the telescopic device (7), the bottom of the fixing rod (52) can be inserted into the vertical cavity (614) in a matching way.
7. The apparatus for preparing a high purity silicon carbide inner liner for a fluidized bed according to claim 6, wherein the fixing rod (52) is a hollow pipe body (521) inserted into the vertical cavity (614), and a pressing block is arranged in the pipe body (521).
8. The apparatus for preparing a high purity silicon carbide liner for a fluidized bed as set forth in claim 7, wherein the inner wall of the tube body (521) has a grain, and the outer wall of the tube body (521) is smooth.
9. A method of preparing a high purity silicon carbide liner for a fluidized bed according to claim 1 comprising:
the manufacturing lining body (2) specifically comprises: weighing the raw materials of the lining body (2) according to the proportion, mixing, pressing, forming, drying the biscuit and sintering at high temperature;
manufacturing an outer shell (1), and forming a perforation on the outer shell (1);
and an elastic part (3) is connected between the outer shell (1) and the inner lining (2), and finally the high-purity silicon carbide inner lining is manufactured.
10. The method for preparing a high purity silicon carbide liner for a fluidized bed according to claim 8, characterized by preparing an inner liner body (2), in particular comprising: weighing the raw materials of the inner lining body (2) according to the proportion, grinding, mixing, granulating, pressing and forming, pressing a blank of the inner lining body (2) by using the preparation device of the high-purity silicon carbide inner lining for the fluidized bed, drying the blank, and sintering at a high temperature;
manufacturing an outer shell (1), and forming a perforation on the outer shell (1);
and an elastic part (3) is connected between the outer shell (1) and the inner lining (2), and finally the high-purity silicon carbide inner lining is manufactured.
CN202310490325.1A 2023-05-04 2023-05-04 Preparation method and device of high-purity silicon carbide lining for fluidized bed Pending CN116440813A (en)

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