Microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder and its use method

Through microwave induction tube matrix fluidized bed technology, the problems of low efficiency and high energy consumption of traditional degreasing furnaces are solved, and efficient and low-energy degreasing and carbonization of semiconductor materials are achieved, ensuring the purity and morphology integrity of the materials.

CN119680477BActive Publication Date: 2025-09-23SHAOXING JINGCAI TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202411340402.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-09-25
Publication Date
2025-09-23
Estimated Expiration
2044-09-25

AI Technical Summary

Technical Problem

Traditional degreasing furnaces have low degreasing efficiency, high energy consumption and are prone to contamination due to their materials, heating methods and internal structures. They are not suitable for efficient degreasing and carbonization of silicon-based/carbon-based resin powders for semiconductor materials.

Method used

The microwave induction tube matrix fluidized bed is adopted, including a microwave generating unit, a waveguide transmission unit, a fluidized bed pressure vessel, a tube matrix unit, an inert fluidizing gas control unit, a powder collection unit and a condensation recovery unit. Microwave heating technology and inert gas suspension are used to perform degreasing and carbonization to avoid contamination by metal impurities, and efficient separation is achieved through a cyclone separator and a classifying wheel.

Benefits of technology

It improves the degreasing and carbonization efficiency, ensures the material purity and micromorphology, reduces energy consumption, avoids metal impurity pollution, and achieves efficient resin powder degreasing and carbonization.

✦ Generated by Eureka AI based on patent content.

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Abstract

A microwave-inducing tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powders and its use method relate to a microwave-inducing tube matrix fluidized bed and its use method, belonging to the field of specialized equipment for degreasing and carbonizing semiconductor materials. This invention addresses the low degreasing efficiency, high energy consumption, and susceptibility to contamination inherent in conventional degreasing furnaces due to their materials, heating methods, and internal structure. The microwave-inducing tube matrix fluidized bed primarily comprises a microwave generating unit, a waveguide transmission unit, a fluidized bed pressure vessel with a classifying wheel and cyclone separator, a tube matrix unit, an inert fluidizing gas control unit, a precursor resin powder dosing unit, a post-degreasing and carbonization powder collection unit, and a condensation recovery unit. The invention utilizes microwave induction heating technology to facilitate atomic re-alignment, forming an infusible structure. The microwave radiation energy is directly transferred to the absorbing ceramic and resin matrix, significantly improving the degreasing and carbonization efficiency and the in-situ degreasing of the precursor resin micropowder.
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Description

Technical Field

[0001] The invention relates to a microwave induction tube matrix fluidized bed and a use method thereof, and belongs to the field of special equipment for degreasing and carbonizing semiconductor materials. Background Art

[0002] Traditional degreasing furnaces are difficult to apply to the preparation of semiconductor materials due to their material, heating method, and internal structure. The degreasing furnace is mainly made of iron-based alloys. During the degreasing process, due to high-temperature radiation and the contact between the metal cavity and the resin, a large amount of metal impurities such as iron, nickel, chromium, and titanium will inevitably be introduced. The insulation materials are mostly made of silicate fibers or corundum bricks, which will also introduce metal and non-metallic impurities such as sodium, potassium, calcium, aluminum, and boron during the degreasing process. Traditional degreasing furnaces mostly use resistance heating, which has a slow heating rate and cannot pass the viscous flow temperature point. The material will enter a molten state, and the molten resin will have liquid characteristics, converging into a macroscopic resin viscous liquid, which cannot maintain the original morphology of the resin powder. The furnace body structure is basically a square or circular silo. The powder aggregates and cannot be dispersed, the heating is uneven, the degreasing efficiency is low, and the energy consumption is high. Summary of the Invention

[0003] The purpose of the present invention is to solve the technical problems of low degreasing efficiency, high energy consumption and easy contamination caused by the material, heating method and internal structure of traditional degreasing furnaces, and to provide a microwave induction tube matrix fluidized bed suitable for degreasing and carbonization of silicon-based / carbon-based resin powder and its use method.

[0004] The microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder mainly includes:

[0005] A microwave generating unit, a waveguide transmission unit, a fluidized bed pressure vessel with a classifying wheel and a cyclone separator, a tube matrix unit, an inert fluidizing gas control unit, a precursor resin powder quantitative feeding unit, a powder collecting unit after degreasing and carbonizing, and a condensation recovery unit. The fluidized bed pressure vessel with a classifying wheel and a cyclone separator is provided with a discharge port at the upper end, and the discharge port is connected to the powder collecting unit after degreasing and carbonizing. A group of tubes is provided in the tube matrix unit. The tubes are double-layer non-uniform jacketed tubes composed of an inner tube and an outer tube. A jacket is provided between the inner tube and the outer tube. A jacket port is provided at the lower end of the outer tube. The length of the inner tube is 1 / 3-3 / 4 of the length of the outer tube. The layer tubes are conical tubes that are narrow at the bottom and thick at the top. The microwave generating unit is connected to the waveguide transmission unit, and the waveguide transmission unit is connected to the tube matrix unit. The upper end of the outer layer tube is inserted from the lower end of the fluidized bed pressure vessel with a classifying wheel and a cyclone separator into the fluidized bed pressure vessel with a classifying wheel and a cyclone separator. The lower end of the inner layer tube is connected to the precursor resin powder quantitative feeding unit. The jackets of the inner layer tubes and the outer layer tubes of the tube array are connected to the inert fluidizing gas control unit through the jacket port. The upper expansion section of the fluidized bed pressure vessel with a classifying wheel and a cyclone separator is connected to the powder collection unit after degreasing and carbonization. The top of the fluidized bed pressure vessel with a classifying wheel and a cyclone separator is connected to the condensation recovery unit.

[0006] The inner tube has a length of 1-5 meters and is made of isostatically pressed graphite or silicon carbide. The wall thickness of the inner tube is 1-3 mm and the diameter of the inner tube is no greater than 10 cm.

[0007] The diameter of the tubes in the tube matrix unit is no more than 3 cm.

[0008] The diameter of the tubes in the tube matrix unit is no more than 7 cm.

[0009] The wall thickness of the inner tube is 1 to 1.5 mm.

[0010] The distance between two adjacent tubes is 1 to 10 cm.

[0011] The cone angle is 1 to 10 degrees and is adjustable. The ratio of the diameter of the upper end of the inner tube to the diameter of the outer tube is 1:2 to 4:5.

[0012] The method for using the microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder is carried out according to the following steps:

[0013] Semiconductor-grade silicon-carbon composite resin, carbon-based resin, fluorocarbon resin, and fluorosilicone resin are prepared into micron-sized powder materials. Based on a powder processing capacity of 500g to 5000g / hour, the inert fluidizing gas control unit is activated, along with the microwave generator in the microwave generating unit. The output power is adjusted to 80% to 90%, and the carrier gas and auxiliary gas flow rates are coordinated to adjust the suspended powder concentration and residence time to ensure complete degreasing and carbonization of the micropowder. The microwaves generated by the magnetron are transmitted through the waveguide, rapidly raising the temperature of the tube array above the resin's viscous flow point of 200-550°C. Simultaneously, the small amount of microwaves that penetrate the tubes promotes resin rearrangement or further polymerization, thereby achieving infusibility. The carrier gas carries the carbonized powder into the outer tubes of the tubular matrix unit. The high auxiliary gas velocity at the outlet rapidly flushes the degreased, carbonized powder. Simultaneously, the friction between the fluidized powders reduces the adsorption of free carbon and high-molecular organic matter generated during pyrolysis on the particle surfaces. Finally, the pyrolyzed powder, along with the inert fluidizing gas, enters the upper expansion section of the fluidized bed pressure vessel, equipped with a classifier and cyclone separator. Microwave electromagnetic waves are transmitted via waveguide transmission units to the tubular matrix unit for further crosslinking and rearrangement of the resin, achieving infusibility. The introduction of waveguides effectively seals the fluidized bed, preventing the influence of oxygen and nitrogen, which can cause flash explosions and contamination of the precursor resin. Micronized powder material, along with the inert gas, enters the tubular matrix unit from the jacket. Adjusting the powder concentration in the carrier gas and the tube diameter keeps the nanopowder in suspension, allowing it to rearrange upon heating and resist melting at high temperatures. The infusible powder moves in plug flow within the tube. Due to the lack of backmixing, the powder gradually degreases and carbonizes as it rises from the bottom, forming carbon-based particles or silicon-carbon-oxygen particles. Depending on the precursor resin, composite multi-element ceramic particles can also be formed. The carbonized particles encounter the inert gas introduced into the jacket. The inert fluidizing gas control unit maintains a temperature of 200 to -700 degrees Celsius and a flow rate of 0.05 to 0.5 m / s, promoting further friction between the nanopowders and promoting sphericalization. The inert gas also creates a protective space to prevent flash explosions of tar gas clusters. After defatted pyrolysis, the particles enter the upper part of the fluidized bed pressure vessel with a classifying wheel and a cyclone separator along with the inert gas and the organic gas generated by pyrolysis. The particles enter the classifying wheel and the cyclone separator in the fluidized bed pressure vessel with the classifying wheel and the cyclone separator, and finally enter the powder collection unit after defatted carbonization through the discharge port, and then are collected in the powder silo. A small amount of non-condensable gas enters the condensation recovery unit, and a large amount of organic vapor enters the cyclone and powder gas separation in the fluidized bed pressure vessel 3 with the classifying wheel and the cyclone separator, and then enters the condensation recovery unit. After the organic vapor is cooled by the condensation recovery unit, it is collected in the mixed liquid storage tank. The non-condensable gas is incinerated by the incinerator, and the tail gas is washed by the elution tower and purified by the cold dryer, and then converted into high-purity inert gas for recycling.

[0014] The inert gas is argon, helium, nitrogen or hydrogen, and the gas purity is greater than 6N;

[0015] The organic matter is an alkane, an aromatic ring, or a heterocyclic organic matter.

[0016] The fluidized bed pressure vessel with the classifying wheel and the cyclone separator is under normal pressure and negative pressure, and the negative pressure is -60kPa to -95kPa.

[0017] The present invention utilizes microwave induction heating technology to facilitate interatomic re-beating and form an infusible structure. The microwave radiation energy is directly transmitted to the absorbing ceramic and the resin matrix, greatly improving the degreasing carbonization efficiency and the in-situ degreasing effect of the precursor resin micropowder. After carbonization, the carbon microparticles or silicon-carbon-oxygen ceramic particles can ensure purity and microscopic scale.

[0018] This invention has three major innovations. First, the use of high-purity graphite or silicon carbide tubes as the core degreasing and carbonization units prevents contamination from metals and Group III and V elements. Second, because the resin precursor powder is degreased and carbonized while suspended, this solves the problem of resin melting during pyrolysis, which prevents the precursor from maintaining its morphology. Third, the fluidized bed incorporates a tube matrix made of microwave-absorbing materials such as high-purity graphite and silicon carbide ceramics, addressing the issues of low microwave penetration depth and slow resin degreasing and pyrolysis rates. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 This is a schematic diagram of the structure of a microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powders;

[0020] Figure 2 It is a structural diagram of the tube column. DETAILED DESCRIPTION

[0021] The technical solution of the present invention is not limited to the specific embodiments listed below, but also includes any combination of the specific embodiments.

[0022] Specific embodiment 1: This embodiment is suitable for the microwave induction tube matrix fluidized bed for degreasing and carbonizing silicon-based / carbon-based resin powders and mainly includes:

[0023] A microwave generating unit 1, a waveguide transmission unit 2, a fluidized bed pressure vessel 3 with a classifying wheel and a cyclone separator, a tube matrix unit 4, an inert fluidizing gas control unit 5, a precursor resin powder quantitative feeding unit 6, a degreasing and carbonizing powder collecting unit 7 and a condensation recovery unit 8. The fluidized bed pressure vessel 3 with a classifying wheel and a cyclone separator is provided with a discharge port 3-1 at the upper end, and the discharge port 3-1 is connected to the degreasing and carbonizing powder collecting unit 7. The tube matrix unit 4 is provided with a group of tubes 4-3, and the tubes 4-3 are double-layer non-uniform jacketed tubes composed of an inner tube 4-1 and an outer tube 4-2. A jacket 4-4 is provided between the inner tube 4-1 and the outer tube 4-2. A jacket port 4-5 is provided at the lower end of the outer tube 4-2. The length of the inner tube 4-1 is 1 / 3 of the length of the outer tube 4-2. 3 / 4, the inner tube 4-1 is a tapered tube that is narrow at the bottom and thick at the top, the microwave generating unit 1 is connected to the waveguide transmission unit 2, the waveguide transmission unit 2 is connected to the tube matrix unit 4, the upper end of the outer tube 4-2 is inserted from the lower end of the fluidized bed pressure vessel 3 with a classifying wheel and a cyclone separator into the fluidized bed pressure vessel 3 with a classifying wheel and a cyclone separator, the lower end of the inner tube 4-1 is connected to the precursor resin powder quantitative feeding unit 6, the jacket 4-4 of the inner tube 4-1 and the outer tube 4-2 of the tube array 4-3 is connected to the inert fluidizing gas control unit 5 through the jacket port 4-5, the upper expanded section of the fluidized bed pressure vessel 3 with a classifying wheel and a cyclone separator is connected to the powder collection unit 7 after degreasing and carbonization, and the top of the fluidized bed pressure vessel 3 with a classifying wheel and a cyclone separator is connected to the condensation recovery unit 8.

[0024] Specific embodiment 2: This embodiment differs from specific embodiment 1 in that the inner tube 4-1 is 1-5 meters long, made of isostatically pressed graphite or silicon carbide, has a wall thickness of 1-3 mm, and a diameter of no greater than 10 cm. Other aspects are the same as specific embodiment 1.

[0025] Specific embodiment 3: This embodiment differs from specific embodiment 1 or 2 in that the diameter of the tubes 4 - 3 in the tube matrix unit 4 is no greater than 3 cm. Other aspects are the same as specific embodiment 1 or 2.

[0026] Specific embodiment 4: This embodiment differs from specific embodiments 1 to 3 in that the diameter of the tubes 4 - 3 in the tube matrix unit 4 is no greater than 7 cm. Other aspects are the same as specific embodiments 1 to 3.

[0027] Specific embodiment 5: This embodiment differs from specific embodiments 1 to 4 in that the wall thickness of the inner tube 4 - 1 is 1 to 1.5 mm. Other aspects are the same as specific embodiments 1 to 4.

[0028] Specific embodiment 6: This embodiment differs from specific embodiments 1 to 5 in that the distance between two adjacent tubes 4 - 3 is 1 to 10 cm. Other aspects are the same as specific embodiments 1 to 5.

[0029] Specific embodiment 7: This embodiment differs from specific embodiments 1 to 6 in that the cone angle is 1 to 10 degrees and is adjustable, and the ratio of the upper end diameter of the inner tube 4-1 to the diameter of the outer tube 4-2 is 1:2 to 4:5. Other aspects are the same as specific embodiments 1 to 6.

[0030] Specific embodiment eight: The method for using the microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder described in this embodiment and specific embodiment one is as follows:

[0031] Semiconductor-grade silicon-carbon composite resin, carbon-based resin, fluorocarbon resin, and fluorosilicone resin are prepared into micron powder materials. According to the powder processing capacity of 500g to 5000g / hour, the inert fluidizing gas control unit 5 is started, the microwave generator of the microwave generating unit 1 is started, the output power is adjusted to 80% to 90% of the power output, and the microwave electromagnetic wave is transmitted to the tube matrix unit 4 through the waveguide transmission unit 2. The micron powder material enters the tube matrix unit 4 from the jacket 4-4 along with the inert gas, is degreased and carbonized, and the carbonized particles meet the inert gas introduced into the jacket 4-4. The temperature of the inert gas is controlled to be 200 to 700 degrees Celsius and the gas flow rate is controlled to be 0.05 to 0.5m / s by the inert fluidizing gas control unit 5. After degreasing and pyrolysis, the particles are heated and heated. As the inert gas and organic gas generated by pyrolysis enter the upper part of the fluidized bed pressure vessel 3 with a classifying wheel and a cyclone separator, the particles enter the classifying wheel and the cyclone separator in the fluidized bed pressure vessel 3 with the classifying wheel and the cyclone separator, and finally enter the degreasing and carbonizing powder collection unit 7 through the discharge port 3-1, and are then collected in the powder silo. A small amount of non-condensable gas enters the condensation recovery unit 8, and a large amount of organic vapor enters the cyclone and powder-gas separation in the fluidized bed pressure vessel 3 with the classifying wheel and the cyclone separator, and then enters the condensation recovery unit 8. After the organic vapor is cooled by the condensation recovery unit 8, it is collected in the mixed liquid storage tank, the non-condensable gas is incinerated by the incinerator, and the tail gas is washed by the elution tower and purified by the cold dryer, and then converted into high-purity inert gas for recycling.

[0032] Specific embodiment 9: This embodiment differs from specific embodiment 8 in that the inert gas is argon, helium, nitrogen or hydrogen, and the gas purity is greater than 6N; the organic matter is an alkane, aromatic ring, or heterocyclic organic matter.

[0033] Specific embodiment 10: This embodiment differs from specific embodiment 8 or 9 in that the fluidized bed pressure vessel 3 with the classifying wheel and cyclone separator is at normal pressure and negative pressure, wherein the negative pressure is -60kPa to -95kPa. Other aspects are the same as specific embodiment 8.

[0034] The following experiments were used to verify the effects of the present invention:

[0035] Experiment 1:

[0036] Combine Figure 1 、 Figure 2 The microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder mainly includes:

[0037] The invention comprises a microwave generating unit 1, a waveguide transmission unit 2, a fluidized bed pressure vessel 3 with a classifying wheel and a cyclone separator, a tube matrix unit 4, an inert fluidizing gas control unit 5, a precursor resin powder quantitative feeding unit 6, a degreasing and carbonizing powder collecting unit 7 and a condensation recovery unit 8. The fluidized bed pressure vessel 3 with a classifying wheel and a cyclone separator is provided with a discharge port 3-1 at the upper end, and the discharge port 3-1 is connected to the degreasing and carbonizing powder collecting unit 7. The tube matrix unit 4 is provided with a group of tubes 4-3, and the tubes 4-3 are double-layer non-uniform-height jacketed tubes composed of an inner tube 4-1 and an outer tube 4-2. A jacket 4-4 is provided between the inner tube 4-1 and the outer tube 4-2, and a jacket port 4-5 is provided at the lower end of the outer tube 4-2. The length of the inner tube 4-1 is 1 / 2 of the length of the outer tube 4-2. / 3, the inner tube 4-1 is a tapered tube that is narrow at the bottom and thick at the top, the microwave generating unit 1 is connected to the waveguide transmission unit 2, the waveguide transmission unit 2 is connected to the tube matrix unit 4, the upper end of the outer tube 4-2 is inserted from the lower end of the fluidized bed pressure vessel 3 with a classifying wheel and a cyclone separator into the fluidized bed pressure vessel 3 with a classifying wheel and a cyclone separator, the lower end of the inner tube 4-1 is connected to the precursor resin powder quantitative feeding unit 6, the jacket 4-4 of the inner tube 4-1 and the outer tube 4-2 of the tube array 4-3 is connected to the inert fluidizing gas control unit 5 through the jacket port 4-5, the upper expanded section of the fluidized bed pressure vessel 3 with a classifying wheel and a cyclone separator is connected to the powder collection unit 7 after degreasing and carbonization, and the top of the fluidized bed pressure vessel 3 with a classifying wheel and a cyclone separator is connected to the condensation recovery unit 8.

[0038] The inner tube 4 - 1 is 1-5 meters long and is made of isostatically pressed graphite or silicon carbide. The wall thickness of the inner tube 4 - 1 is 1 mm, and the diameter of the inner tube 4 - 1 is 2 cm.

[0039] The wall thickness of the inner tube 4 - 1 is 1 mm.

[0040] The distance between two adjacent tubes 4-3 is 1 cm.

[0041] The cone angle is 10 degrees and is adjustable. The ratio of the diameter of the upper end of the inner tube 4-1 to the diameter of the outer tube 4-2 is 1:2.

[0042] The method for using the microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder is carried out according to the following steps:

[0043] Semiconductor-grade silicon-carbon composite resin, carbon-based resin, fluorocarbon resin, and fluorosilicone resin are prepared into micron-sized powder materials. Based on a powder processing capacity of 5000g / hour, the inert fluidizing gas control unit 5 is activated, along with the microwave generator of the microwave generating unit 1. The output power is adjusted to 80%, and the carrier gas flow rate and auxiliary gas flow rate are coordinated to adjust the suspended powder concentration and residence time to ensure complete degreasing and carbonization of the micropowder. The microwaves generated by the magnetron are transmitted through the waveguide, rapidly raising the temperature of the tube array above the resin's viscous flow point of 200°C. Simultaneously, the small amount of microwaves that penetrate the tubes promotes resin rearrangement or further polymerization, thereby achieving infusibility. The carrier gas carries the carbonized powder into the outer tube 4-2 of the tubular matrix unit 4. Due to the high auxiliary gas flow rate at the outlet, it rapidly flushes the degreased, carbonized powder. Simultaneously, the friction between the fluidized powder reduces the adsorption of free carbon and high-molecular organic matter generated during pyrolysis on the particle surfaces. Finally, the pyrolyzed powder, along with the inert fluidizing gas, enters the upper expanded section of the fluidized bed pressure vessel 3, equipped with a classifier and cyclone separator. Microwave electromagnetic waves are transmitted via the waveguide transmission unit 2 to the tubular matrix unit 4 for further crosslinking and rearrangement of the resin, achieving infusibility. The introduction of the waveguide effectively seals the fluidized bed, preventing the effects of oxygen and nitrogen, which can cause flash explosions and contamination of the precursor resin. Micronized powder material, along with the inert gas, enters the tubular matrix unit 4 from the jacket 4-4. By adjusting the powder concentration in the carrier gas and the tube diameter, the nanopowder is suspended, allowing it to rearrange upon heating, preventing it from melting at high temperatures. The infusible powder moves in plug flow within the tube. Due to the lack of backmixing, the powder gradually degreases and carbonizes as it rises from the bottom, forming carbon-based particles or silicon-carbon-oxygen particles. Depending on the precursor resin, composite multi-element ceramic particles can also be formed. The carbonized particles encounter the inert gas introduced into jacket 4-4. The inert fluidizing gas control unit 5 controls the inert gas temperature to 200 degrees Celsius and the gas flow rate to 0.1 m / s, assisting the nanopowders in further friction and sphericalization. Simultaneously, the inert gas forms a protective space, preventing flash explosions of tar gas clusters. After defatted pyrolysis, the particles enter the upper part of the fluidized bed pressure vessel 3 with a classifying wheel and a cyclone separator along with the inert gas and the organic gas generated by pyrolysis. The particles enter the classifying wheel and the cyclone separator in the fluidized bed pressure vessel 3 with the classifying wheel and the cyclone separator, and finally enter the powder collection unit 7 after defatted carbonization through the discharge port 3-1, and are then collected in the powder silo. A small amount of non-condensable gas enters the condensation recovery unit 8, and a large amount of organic vapor enters the cyclone and powder-gas separation in the fluidized bed pressure vessel 3 with the classifying wheel and the cyclone separator, and then enters the condensation recovery unit 8. After the organic vapor is cooled by the condensation recovery unit 8, it is collected in the mixed liquid storage tank. The non-condensable gas is incinerated in the incinerator, and the tail gas is washed by the leaching tower and purified by the cold dryer, and then converted into high-purity inert gas for recycling.

[0044] The inert gas is argon, and the gas purity is greater than 6N;

[0045] The organic matter is an alkane, an aromatic ring, or a heterocyclic organic matter.

[0046] The fluidized bed pressure vessel 3 with the classifying wheel and the cyclone separator is under negative pressure, which is -60 kPa.

Claims

1. Microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder, characterized by The microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder mainly comprises: A microwave generating unit (1), a waveguide transmission unit (2), a fluidized bed pressure vessel (3) with a classifying wheel and a cyclone separator, a tube matrix unit (4), an inert fluidizing gas control unit (5), a precursor resin powder quantitative feeding unit (6), a degreased carbonized powder collecting unit (7) and a condensation recovery unit (8), wherein the fluidized bed pressure vessel (3) with a classifying wheel and a cyclone separator is provided with a discharge port (3-1) at the upper end, the discharge port (3-1) is connected to the degreased carbonized powder collecting unit (7), the tube matrix unit (4) is provided with a group of tubes (4-3), the tubes (4-3) are double-layer non-uniform jacketed tubes composed of an inner tube (4-1) and an outer tube (4-2), a jacket (4-4) is provided between the inner tube (4-1) and the outer tube (4-2), a jacket port (4-5) is provided at the lower end of the outer tube (4-2), and the length of the inner tube (4-1) is 1 / 4 of the length of the outer tube (4-2). 1 / 3-3 / 4, the inner tube (4-1) is a tapered tube that is narrow at the bottom and thick at the top, the microwave generating unit (1) is connected to the waveguide transmission unit (2), the waveguide transmission unit (2) is connected to the tube matrix unit (4), the upper end of the outer tube (4-2) is inserted from the lower end of the fluidized bed pressure vessel (3) with a classifying wheel and a cyclone separator into the fluidized bed pressure vessel (3) with a classifying wheel and a cyclone separator, and the lower end of the inner tube (4-1) is quantitatively connected to the precursor resin powder. The feeding unit (6) is connected, the inner tube (4-1) and the outer tube (4-2) of the tube array (4-3) are connected to the inert fluidizing gas control unit (5) through the jacket port (4-5), the upper expansion section of the fluidized bed pressure vessel (3) with a classifying wheel and a cyclone separator is connected to the degreased and carbonized powder collection unit (7), and the top of the fluidized bed pressure vessel (3) with a classifying wheel and a cyclone separator is connected to the condensation recovery unit (8).

2. The microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder according to claim 1, characterized in that The inner tube (4-1) is 1-5 meters long and is made of isostatic graphite or silicon carbide. The wall thickness of the inner tube (4-1) is 1-3 mm, and the diameter of the inner tube (4-1) is no more than 10 cm.

3. The microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder according to claim 1, characterized in that The diameter of the tubes (4-3) in the tube matrix unit (4) is no more than 3 cm.

4. The microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder according to claim 1, characterized in that The diameter of the tubes (4-3) in the tube matrix unit (4) is no more than 7 cm.

5. The microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder according to claim 1, characterized in that The wall thickness of the inner tube (4-1) is 1-1.5 mm.

6. The microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder according to claim 1, characterized in that The distance between two adjacent tubes (4-3) is 1~10cm.

7. The microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder according to claim 1, characterized in that The ratio of the diameter of the upper end of the inner tube (4-1) to the diameter of the outer tube (4-2) is 1:2~4:

5.

8. The method for using the microwave induction tube matrix fluidized bed for degreasing and carbonizing silicon-based / carbon-based resin powders as claimed in claim 1, characterized in that The method for using the microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder is carried out according to the following steps: Semiconductor-grade silicon-carbon composite resin, carbon-based resin, fluorocarbon resin, and fluorosilicone resin are prepared into micron powder materials. According to the powder processing amount of 500g~5000g / hour, the inert fluidizing gas control unit (5) is started, the microwave generator of the microwave generating unit (1) is started, the output power is adjusted to 80%~90% of the power output, and the microwave electromagnetic wave is transmitted to the tube matrix unit (4) through the waveguide transmission unit (2). The micron powder material enters the tube matrix unit (4) from the jacket (4-4) along with the inert gas, and is degreased and carbonized. The carbonized particles meet the inert gas introduced into the jacket (4-4). The temperature of the inert gas is controlled to be 200~700 degrees Celsius and the gas flow rate is controlled to be 0.05~0.5m / s through the inert fluidizing gas control unit (5). After degreasing and pyrolysis, the particles are As the inert gas and the organic gas generated by pyrolysis enter the upper part of the fluidized bed pressure vessel (3) with a classifying wheel and a cyclone separator, the particles enter the classifying wheel and the cyclone separator in the fluidized bed pressure vessel (3) with a classifying wheel and a cyclone separator, and finally enter the powder collection unit (7) after degreasing and carbonization through the discharge port (3-1), and are then collected in the powder silo. A small amount of non-condensable gas enters the condensation recovery unit (8), and a large amount of organic vapor enters the cyclone in the fluidized bed pressure vessel (3) with a classifying wheel and a cyclone separator, and after powder and gas separation, enters the condensation recovery unit (8). After the organic vapor is cooled by the condensation recovery unit (8), it is collected in the mixed liquid storage tank, the non-condensable gas is incinerated by the incinerator, and the tail gas is washed by the leaching tower and purified by the cold dryer, and then converted into high-purity inert gas for recycling.

9. The method for using the microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder according to claim 8, characterized in that The inert gas is argon, helium, nitrogen or hydrogen, and the gas purity is greater than 6N; the organic matter is alkane, aromatic ring or heterocyclic organic matter.

10. The method for using the microwave induction tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder according to claim 8, characterized in that The fluidized bed pressure vessel (3) with the classifying wheel and the cyclone separator is under normal pressure and negative pressure, and the negative pressure is -60kPa to -95kPa.

Citation Information

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