Microwave induction array tube matrix fluidized bed suitable for degreasing and carbonizing silicon-based / carbon-based resin powder and use method of microwave induction array tube matrix fluidized bed
Through microwave induction tube matrix fluidized bed technology, the problems of low degreasing efficiency, high energy consumption and easy contamination of traditional degreasing furnaces are solved, and the high-efficiency, low energy consumption and impurity-free resin degreasing carbonization process is achieved.
Patent Information
- Application Number
- CN202411340402.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-25
- Publication Date
- 2025-03-25
- Estimated Expiration
- 2044-09-25
AI Technical Summary
Traditional degreasing furnaces have problems such as low degreasing efficiency, high energy consumption and easy staining due to materials, heating methods and internal structures.
The microwave induction column tube matrix fluidized bed is used to achieve non-fused degreasing and carbonization of the resin through microwave heating technology. The column tube matrix unit and an inert fluidized gas control unit are used to ensure the efficiency and purity of the degreasing process.
It improves the degreasing carbonization efficiency, reduces energy consumption, avoids contamination of metal impurities, and ensures the in-situ degreasing effect of resin powder and the purity and microscopic scale of the particles after carbonization.
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Figure CN119680477A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a microwave induction tube matrix fluidized bed and a use method thereof, belonging 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 materials, heating methods, and internal structures. 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 cross the viscous flow temperature point. The material will appear in a molten state, and the molten resin will have liquid characteristics and gather into a macroscopic resin viscous liquid, which cannot maintain the original morphology of the resin micropowder. 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 the traditional degreasing furnace, and to provide a microwave induction tube matrix fluidized bed suitable for degreasing and carbonization of silicon-based / carbon-based resin powder and a method of using the same.
[0004] The microwave induction tube matrix fluidized bed suitable for degreasing and carbonization of 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 degreasing and carbonizing powder collecting unit 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 degreasing and carbonizing powder collecting unit. A group of tubes is provided in the tube matrix unit. The tubes are double-layer non-equal-height 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 tube is a conical tube that is 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 into the fluidized bed pressure vessel with a classifying wheel and a cyclone separator from the lower end of 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 tube and the outer layer tube 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, is made of isostatic graphite or silicon carbide, has a wall thickness of 1-3 mm, and has a diameter of no more 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 the cone angle is adjustable. The ratio of the upper end diameter of the inner tube to the outer tube diameter 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 powder materials. According to the powder processing capacity of 500g to 5000g / hour, the inert fluidizing gas control unit is started, the microwave generator of the microwave generating unit is started, and its output power is adjusted to 80% to 90% of the power output, and the carrier gas flow rate and auxiliary gas flow rate are coordinated to adjust the concentration and residence time of the suspended powder to ensure the complete degreasing and carbonization of the micropowder. After the microwaves generated by the magnetron are transmitted through the waveguide, the temperature of the tube array is quickly raised to cross the resin viscous flow temperature point of 200-550 degrees Celsius. At the same time, a small amount of microwaves that penetrate promote the rearrangement or further polymerization of the resin, thereby achieving infusibility. The carrier gas carries the carbonized powder into the outer tube of the tube matrix unit. Due to the high flow rate of the auxiliary gas at the outlet, the degreased carbonized powder is quickly flushed. At the same time, the mutual friction of the fluidized powder reduces the adsorption of free carbon and high molecular organic matter produced during pyrolysis on the particle surface. Finally, the pyrolyzed powder and the inert fluidized gas enter the upper expansion section of the fluidized bed pressure vessel with a classifier and a cyclone separator, and transmit the microwave electromagnetic wave to the tube matrix unit through the waveguide transmission unit for further cross-linking of the resin and rearrangement to achieve infusible characteristics. The introduction of the waveguide can better seal the fluidized bed and prevent the influence of oxygen and nitrogen, which may cause flash explosions and contamination of the precursor resin. The micron powder material enters the tube matrix unit from the jacket with the inert gas. By adjusting the concentration of the powder in the carrier gas and the tube diameter, the nano powder is suspended, and then rearranged by heat to achieve no melting at high temperatures. The infusible powder moves in a plug flow in the tube. Since there is no back-mixing process, the powder gradually degreases and carbonizes during the rising process from the bottom to form carbon-based particles or silicon-carbon-oxygen particles. It can also form composite multi-element ceramic particles due to the difference in precursor resins. The carbonized particles meet the inert gas introduced into the jacket. Through the inert fluidizing gas control unit, the temperature of the inert gas is controlled to 200 to -700 degrees Celsius and the gas flow rate is 0.05 to 0.5 m / s, which helps the nano-powders to further rub against each other and promote spheroidization. At the same time, the inert gas forms a protective space to prevent the tar gas cluster from flashing. 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 the 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 in the fluidized bed pressure vessel 3 with the classifying wheel and the cyclone separator, and after the powder and gas are separated, 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 eluted 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 at normal pressure and negative pressure, and the negative pressure is -60kPa to -95kPa.
[0017] The present invention utilizes microwave induction heating technology to facilitate atomic 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. The carbonized carbon microparticles or silicon carbon oxygen ceramic particles can ensure purity and microscopic scale.
[0018] The main innovations of the present invention are three. First, the use of high-purity graphite tubes or silicon carbide tubes as the degreasing carbonization core unit can avoid the contamination of metals and group III and V elements. Second, since the resin precursor powder is degreased and carbonized in a suspended state, the problem of melting during the resin pyrolysis process and thus being unable to maintain the precursor morphology can be solved. Third, the fluidized bed is built with a tube matrix unit made of high-purity graphite, silicon carbide ceramics and other absorbing materials, which solves the problem of low microwave penetration depth and slow resin degreasing pyrolysis speed. BRIEF DESCRIPTION OF THE DRAWINGS
[0019] Figure 1 It is a schematic diagram of the structure of a microwave induction tube matrix fluidized bed suitable for degreasing and carbonization of silicon-based / carbon-based resin powders;
[0020] Figure 2 It is a schematic diagram of the structure of the tube array. DETAILED DESCRIPTION
[0021] The technical solution of the present invention is not limited to the specific implementation modes listed below, but also includes any combination of the specific implementation modes.
[0022] Specific implementation method 1: This implementation method is suitable for the microwave induction tube matrix fluidized bed for degreasing and carbonization of silicon-based / carbon-based resin powder 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. A group of tubes 4-3 is provided in the tube matrix unit 4. 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 inner tube 4-1 of the tube array 4-3 and the jacket 4-4 of the outer tube 4-2 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 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 is different from specific embodiment 1 in that the inner tube 4-1 is 1-5 meters long, made of isostatic graphite or silicon carbide, has a wall thickness of 1-3 mm, and has a diameter of no more than 10 cm. Others are the same as specific embodiment 1.
[0025] Specific implementation method 3: This implementation method is different from specific implementation methods 1 or 2 in that the diameter of the tubes 4 - 3 in the tube matrix unit 4 is not greater than 3 cm. The rest is the same as specific implementation methods 1 or 2.
[0026] Specific embodiment 4: This embodiment is different from specific embodiments 1 to 3 in that the diameter of the tubes 4 - 3 in the tube matrix unit 4 is not greater than 7 cm. The rest is the same as specific embodiments 1 to 3.
[0027] Specific implementation mode 5: This implementation mode is different from specific implementation modes 1 to 4 in that the wall thickness of the inner tube 4 - 1 is 1 to 1.5 mm. The rest is the same as specific implementation modes 1 to 4.
[0028] Specific implementation example 6: This implementation example is different from specific implementation examples 1 to 5 in that the distance between two adjacent tube arrays 4 - 3 is 1 to 10 cm. The rest is the same as specific implementation examples 1 to 5.
[0029] Specific embodiment 7: This embodiment is different from specific embodiments 1 to 6 in that the cone angle is 1 to 10 degrees, and the cone angle 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 carbonization of silicon-based / carbon-based resin powder described in this embodiment and specific embodiment one is carried out according to the following steps:
[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 amount 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, 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 to 700 degrees Celsius and the gas flow rate is controlled to be 0.05 to 0.5 m / s through the inert fluidizing gas control unit 5. After degreasing and pyrolysis, the particles 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 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 eluted by the elution tower and purified by the cold dryer, and then converted into high-purity inert gas for recycling.
[0032] Specific implementation method 9: This implementation method is different from specific implementation method 8 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.
[0033] Specific embodiment 10: This embodiment is different from specific embodiment 8 or 9 in that the fluidized bed pressure vessel 3 with a classifying wheel and a cyclone separator is at normal pressure and negative pressure, and the negative pressure is -60 kPa to -95 kPa. The rest is the same as specific embodiment 8.
[0034] The following experiments were used to verify the effect of the present invention:
[0035] Experiment 1:
[0036] Combination Figure 1 , Figure 2 The microwave induction tube matrix fluidized bed suitable for degreasing and carbonization of 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. 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. 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 expansion 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 has a length of 1-5 meters and is made of isostatic 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 layer 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 upper end diameter 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 powder materials. According to the powder processing capacity of 5000g / hour, the inert fluidizing gas control unit 5 is started, the microwave generator of the microwave generating unit 1 is started, and its output power is adjusted to 80% of the power output, and the carrier gas flow rate and the auxiliary gas flow rate are coordinated to adjust the concentration and residence time of the suspended powder to ensure the complete degreasing and carbonization of the micropowder. After the microwaves generated by the magnetron are transmitted through the waveguide, the temperature of the tube array is quickly raised to cross the resin viscosity flow temperature point of 200 degrees Celsius. At the same time, a small amount of microwaves that penetrate promote the rearrangement or further polymerization of the resin, thereby achieving infusibility. The carrier gas carries the carbonized powder into the outer tube 4-2 of the tube matrix unit 4. Due to the high flow rate of the auxiliary gas at the outlet, the degreased carbonized powder is quickly flushed. At the same time, the mutual friction of the fluidized powder reduces the adsorption of free carbon and high molecular organic matter produced during pyrolysis on the particle surface. Finally, the pyrolyzed powder and the inert fluidized gas enter the upper expansion section of the fluidized bed pressure vessel 3 with a classifier and a cyclone separator, and transmit the microwave electromagnetic wave to the tube matrix unit 4 through the waveguide transmission unit 2 for further cross-linking of the resin and rearrangement to achieve infusible properties. The introduction of the waveguide can better seal the fluidized bed and prevent the influence of oxygen and nitrogen, thereby causing flash explosions and contamination of the precursor resin. The micron powder material enters the tube matrix unit 4 from the jacket 4-4 with the inert gas. By adjusting the concentration of the powder in the carrier gas and the adjustment of the tube diameter, the nano powder is suspended, and then rearranged by heat to achieve no melting at high temperatures. The infusible powder moves in a plug flow in the tube. Since there is no back-mixing process, the powder gradually degreases and carbonizes during the rising process from the bottom to form carbon-based particles or silicon-carbon-oxygen particles. It can also form composite multi-element ceramic particles due to the difference in precursor resins. The carbonized particles meet the inert gas introduced into the jacket 4-4. The inert gas temperature is controlled to 200 degrees Celsius and the gas flow rate is 0.1m / s through the inert fluidizing gas control unit 5, which assists the nanopowders to further rub against each other and promote spheroidization. At the same time, the inert gas forms a protective space to prevent the tar gas mass from flashing. 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 the 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 then are 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 the classifying wheel and the cyclone separator, and after the powder and gas are separated, 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 eluted by the elution 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, and the negative pressure is -60 kPa.
Claims
1. A microwave induction tube matrix fluidized bed suitable for degreasing and carbonization of silicon-based / carbon-based resin powders, characterized in that 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 and 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 thereof, and the discharge port (3-1) The tube matrix unit (4) is connected to a powder collecting unit (7) after degreasing and carbonization. A group of tubes (4-3) is provided in the tube matrix unit (4). 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). A jacket opening (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). 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 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).
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) has a length of 1-5 meters 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 not greater 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 greater 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 layer tube (4-1) is 1 to 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 tube arrays (4-3) is 1 to 10 cm.
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 cone angle is 1 to 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 to 4:
5.
8. The method for using the microwave induction tube matrix fluidized bed suitable 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 500 g to 5000 g / 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, and is degreased and carbonized. The carbonized particles meet the inert gas introduced into the jacket (4-4). The inert gas temperature is controlled to be 200 to 700 degrees Celsius and the gas flow rate is controlled to be 0.05 to 0.5 m / s through the inert fluidizing gas control unit (5). After degreasing and pyrolysis, the particles 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 then are 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 a mixed liquid storage tank, the non-condensable gas is incinerated by an incinerator, and the tail gas is eluted by an elution tower and purified by a cold dryer, and then converted into a 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 7, 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, 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 7, characterized in that The fluidized bed pressure vessel (3) with a classifying wheel and a cyclone separator is at normal pressure and negative pressure, and the negative pressure is -60 kPa to -95 kPa.
Citation Information
Patent Citations
Multistage fluidized bed steam reforming apparatus and method of treating waste resin
CN106732306A
Process for preparing highly pure silicon granules
CN1216288A
Carbon activation in a microwave fluidized bed process
US20140056799A1
Fluidized-bed reactor and process for preparing granular polycrystalline silicon
US20170158516A1
Fluid bed apparatus and method of operating such apparatus
WO2006067544A1