A continuous fluidized gas-solid reaction apparatus

Abstract

The present application relates to a kind of continuous fluidized gas-solid reaction device, including heating chamber and the fluidized gas-solid reaction mechanism being arranged in heating chamber.Heating chamber contains shell plate and heating element, fluidized gas-solid reaction mechanism includes wall plate, multiple fluidized reaction cavities and corresponding gas pipeline, adjacent fluidized reaction cavities are communicated by the passage of bottom, and the top and bottom wall plate of reaction mechanism are staggered and arranged with upper baffle and lower baffle, and upper baffle and lower baffle form a serpentine curved flow channel in fluidized reaction cavity together, and powder is driven to flow in flow channel by the height difference between cavity body.The present application sets up multiple fluidized reaction cavities, so that powder flows in fluidized state for a long distance, and the inner and outer surfaces of porous powder are continuously and stably deposited for a long time in fluidized and flowing state, which well meets the requirements of industrial scale production.Meanwhile, different deposition reaction gases can be replaced in different reaction cavities, which has flexible and extensive adaptability.

Description

Technical Field

[0001] This invention relates to the field of gas-solid fluidization, and more specifically to a continuous fluidized gas-solid reaction apparatus. Background Technology

[0002] Fluidized bed reactors are a common type of gas-solid reactor or vapor deposition equipment. When used for vapor deposition, large deposition volumes require long deposition times, necessitating intermittent operation. Especially when deposition requires high temperatures, heating and cooling consume significant time and energy.

[0003] CN2035354U describes a continuous fluidized bed solid-phase reactor suitable for solid-phase reaction operations of modified starch with reaction temperatures below 200℃, feed moisture content below 13%, and starch particle size of 30-400μm.

[0004] In the process of preparing silicon-carbon composites by silane deposition, the fluidized bed device needs to ensure continuous and stable deposition of porous carbon powder on its inner and outer surfaces for a long time at a certain high temperature. Different deposition reaction gases also need to be changed at different stages, while ensuring operational safety. Currently, there is no commercially available continuous reaction device suitable for preparing silicon-carbon composites by silane deposition. Therefore, this invention proposes a continuous fluidized gas-solid reaction device. Summary of the Invention

[0005] To address the problem that existing fluidized bed gas-solid reactors cannot achieve large-scale production of silicon-carbon composite materials through continuous, stable, and long-term deposition on the inner and outer surfaces of porous carbon powder, this invention proposes a continuous fluidized bed gas-solid reactor. The specific technical solution is as follows:

[0006] A continuous fluidized gas-solid reaction apparatus includes a heating chamber and a fluidized gas-solid reaction mechanism disposed within the heating chamber. The heating chamber includes a shell plate and a heating element. The fluidized gas-solid reaction mechanism includes a wall plate, multiple fluidized reaction chambers, and corresponding gas pipelines. Adjacent fluidized reaction chambers are connected through a channel at the bottom. Upper and lower baffles are alternately arranged at the top and bottom of the wall plate. The upper and lower baffles together form a serpentine flow channel within the fluidized reaction chamber. The powder is propelled to flow within the flow channel by the height difference of the powder between the chambers.

[0007] Furthermore, the shell plate includes an outer shell plate, an insulation material layer, and an inner shell plate. The insulation material layer is disposed in the interlayer between the outer shell plate and the inner shell plate, and the heating element is installed on the inner shell plate.

[0008] Furthermore, the fluidized gas-solid reaction mechanism also includes a feed inlet, a discharge outlet, a carrier gas pipe, a reaction gas pipe, a gas distribution plate, an exhaust pipe, and a pulse backflush gas pipe. The gas distribution plate is located on the lower side of the wall panel. The heating chamber and the wall panel have feed inlets and discharge outlets. The pulse backflush gas pipe and the exhaust pipe are both located on the upper side of the fluidized gas-solid reaction mechanism. The carrier gas pipe and the reaction gas pipe are both located on the lower side of the fluidized gas-solid reaction mechanism. The reaction gas pipe inlet is equipped with a reaction gas solenoid valve, and the carrier gas pipe inlet is equipped with a carrier gas solenoid valve.

[0009] Furthermore, the height of the lower baffle in the fluidized reaction chamber decreases sequentially from the side closer to the feed inlet to the side closer to the discharge outlet.

[0010] Furthermore, each fluidized reaction chamber is equipped with a gas distribution plate and a gas chamber below it; the gas chamber is enclosed by the gas distribution plate and the gas chamber wall panel, and each gas chamber is equipped with a flow control valve on its lower side.

[0011] Furthermore, each fluidized reaction chamber is equipped with one or more pairs of filters on its upper side, and each filter is equipped with a backflushing and discharge control valve on its upper side.

[0012] Furthermore, an inert gas is introduced into the space between the heating chamber and the fluidized gas-solid reaction mechanism.

[0013] Furthermore, the fluidized gas-solid reactor can be used independently as a single unit or in series with multiple units.

[0014] The beneficial effects of this invention are as follows:

[0015] 1. This invention enables continuous large-scale production with simultaneous feeding and discharging of materials.

[0016] 2. The present invention can control the residence time of powder in the fluidized gas-solid reaction mechanism by adjusting the feeding speed and gas flow rate, and at the same time control the deposition and reaction quality by controlling the concentration of fluidized reaction gas.

[0017] 3. This invention can uniformly change the reaction or deposition gas of each fluidized gas-solid reaction mechanism, and can also change the deposition or reaction gas of different chambers in each fluidized gas-solid reaction mechanism separately, thus having a wider range of product performance adaptability. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other configuration schemes can be obtained based on these drawings without creative effort.

[0019] 1. AppendixFigure 1 This is a schematic diagram of the single-unit structure of the continuous fluidized gas-solid reaction device in Example 1, wherein the single-unit fluidized reaction chamber is schematically divided into five chambers.

[0020] 2. Appendix Figure 2 This is a schematic diagram of the equipment consisting of three fluidized gas-solid reactors connected in series, as shown in Example 3.

[0021] In the diagram: 1. Outer shell; 2. Insulation material layer; 3. Inner shell; 4. Heating element; 5. Feed inlet; 6. Exhaust pipe; 7. Pulse backflush pipe; 8. Discharge port; 9. Carrier gas solenoid valve; 10. Carrier gas pipe; 11. Reaction gas pipe; 12. Reaction gas solenoid valve; 13. Gas chamber wall panel; 14. Gas distribution plate; 15. Wall panel; 16. Powder movement trajectory; 17. Single-unit fluidized gas-solid reaction device one; 18. Single-unit fluidized gas-solid reaction device two; 19. Single-unit fluidized gas-solid reaction device three; 101. Flow control valve; 102. Flow control valve; 103. Flow control valve; 104. Flow control valve; 201. Gas chamber; 202. Gas chamber; 203. Gas chamber; 204. Gas chamber; 301. First lower partition; 302. Second lower partition; 303. Third lower partition; 304. Fourth lower partition; 401. First upper partition; 402. Second upper partition; 403. Third upper partition; 404. Fourth upper partition; 501a. Filter; 501b. Filters; 502a, Filter; 502b, Filter; 503a, Filter; 503b, Filter; 504a, Filter; 504b, Filter; 505a, Filter; 505b, Filter; 605a, Filter; 605b, Filter; 601a, Control Valve; 601b, Control Valve; 602a, Control Valve; 602b, Control Valve; 603a, Control Valve; 603b, Control Valve; 604a, Control Valve; 604b, Control Valve. Detailed Implementation

[0022] In the description of this invention, it should be understood that the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicating orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, are only for the convenience of describing the invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the invention. Furthermore, the terms "first," "second," etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined with "first," "second," etc., may explicitly or implicitly include one or more of that feature. In the description of this invention, unless otherwise stated, "a plurality of" means two or more.

[0023] The present invention provides the following specific embodiments of a continuous fluidized gas-solid reaction apparatus:

[0024] Example 1:

[0025] As attached Figure 1 As shown, a continuous fluidized gas-solid reaction apparatus includes a heating chamber and a fluidized gas-solid reaction mechanism disposed within the heating chamber. The heating chamber includes a shell plate and heating elements 4, which are used to heat and maintain the reaction temperature within the reaction mechanism between 30°C and 700°C. The fluidized gas-solid reaction mechanism is disposed within the heating chamber. The fluidized gas-solid reaction mechanism includes wall plates 15 and multiple fluidized reaction chambers. Adjacent fluidized reaction chambers are connected by a channel at the bottom. Upper and lower partitions are staggered between the top and bottom wall plates 15. The upper and lower partitions together form a serpentine flow channel within the fluidized reaction chamber. The powder is propelled to flow along a powder movement trajectory 16 by the height difference between the chambers.

[0026] Furthermore, it also includes an exhaust pipe 6, a pulse backflush pipe 7, a carrier gas pipe 10, and a reaction gas pipe 11. A gas distribution plate 14 is located on the lower side of the wall panel 15. The heating chamber and the side of the wall panel 15 have inlet 5 and outlet 8. The pulse backflush pipe 7 and the exhaust pipe 6 are both located on the upper side of the fluidized gas-solid reaction mechanism, and the carrier gas pipe 10 and the reaction gas pipe 11 are both located on the lower side of the fluidized gas-solid reaction mechanism. A reaction gas solenoid valve 12 is installed at the inlet of the reaction gas pipe 11, and a carrier gas solenoid valve 9 is installed at the inlet of the carrier gas pipe 10. The shell plate includes an outer shell plate 1, a thermal insulation material layer 2, and an inner shell plate 3. The thermal insulation material layer 2 is located in the interlayer between the outer shell plate 1 and the inner shell plate 3. The heating element 4 is installed on the inner shell plate 3.

[0027] Furthermore, the fluidized bed is divided into five smaller chambers: chamber A, chamber B, chamber C, chamber D, and chamber E. Adjacent fluidized bed chambers are separated by a first upper partition 401, a second upper partition 402, a third upper partition 403, and a fourth upper partition 404, respectively. Each upper partition has a powder flow channel between its lower part and the gas distribution plate 14. Chambers B, C, D, and E are respectively equipped with a first lower partition 301, a second lower partition 302, a third lower partition 303, and a fourth lower partition 304. 4. Each lower baffle divides its fluidization reaction chamber into two equal parts; the upper heights of the first lower baffle 301, the second lower baffle 302, the third lower baffle 303, and the fourth lower baffle 304 decrease sequentially, driving the flow of powder through the height difference between the cavities. A gas chamber wall 13 is provided on the lower side of the gas distribution plate 14; a gas chamber 201 is provided on the lower side of cavity A, a gas chamber 202 is provided on the lower side of cavity B, a gas chamber 203 is provided on the lower side of cavity C, and a gas chamber 204 is provided on the lower side of cavity D. A gas chamber 205 is located on the lower side of chamber E. Each gas chamber is enclosed by a gas distribution plate 14 and a gas chamber wall panel 13. A flow control valve 101 is located on the lower side of gas chamber 201, gas chamber 202, gas chamber 203, gas chamber 204, and gas chamber 205. These flow control valves are used to adjust the fluidization state of the powder within each chamber. Filters 501a and 501b are located on the upper side of chamber A, chamber B, chamber C, chamber D, and chamber E. Filters 505a and 505b are used during exhaust and backflushing processes. The powder filtration system includes control valves 601a, 601b, 602a, 602b, 603a, 603b, 604a, 604b, 505a, and 605b. Each filter has multiple pairs of filters on its upper side, and the number of control valves corresponds to the number of filters. Inert gas is introduced into the space between the heating chamber and the fluidized gas-solid reaction mechanism.

[0028] Solid powder is added to the fluidized gas-solid reaction mechanism through the feed port 5. The powder is first distributed to each chamber of the fluidized gas-solid reaction mechanism by the carrier gas. The heating system is turned on to make the material temperature in the fluidized gas-solid reaction mechanism reach the temperature required for reaction or deposition. The required reaction gas is mixed into the carrier gas to start the reaction. At the same time, the powder is fed and discharged. After a transition period, qualified and stable continuous production can be achieved.

[0029] Example 2:

[0030] Solid powder is added to the fluidized gas-solid reaction mechanism through the feed port 5. The powder is first distributed to each chamber of the fluidized gas-solid reaction mechanism by the carrier gas. The heating element 4 is turned on to make the material temperature in the fluidized gas-solid reaction mechanism reach the temperature required for reaction or deposition. Different carrier gases and different reaction gases are introduced into the five chambers A, B, C, D and E as needed. The material is fed and discharged at the same time. After a transition period, qualified and stable continuous production can be achieved.

[0031] Example 3:

[0032] like Figure 2 As shown, a device consisting of three fluidized gas-solid reaction units connected in series is used. Referring to Example 1, the three fluidized gas-solid reaction units are loaded sequentially. The heating system is turned on so that the material temperature in each fluidized gas-solid reaction unit reaches the temperature required for reaction or deposition. A mixture of nitrogen and silane gas is introduced into the single fluidized gas-solid reaction unit 17 and the single fluidized gas-solid reaction unit 28, and a mixture of nitrogen and acetylene gas is introduced into the single fluidized gas-solid reaction unit 319. Material is added and discharged simultaneously. After a transition period, qualified and stable continuous production can be achieved.

[0033] The solid powders used in this invention include, but are not limited to, porous carbon powder, carbon powder, graphite powder, silica powder, and silicon powder; the reaction gases include, but are not limited to, silane, disilane, trichlorosilane, methylaluminum, methyllithium, butylaluminum, butyllithium, acetylene, and ethylene; and the carrier gases include, but are not limited to, hydrogen, nitrogen, argon, and helium. An important application of this invention is in the preparation process of silicon-carbon composites formed by the deposition of silane in porous carbon.

[0034] This invention controls the residence time of powder in the fluidized gas-solid reaction mechanism by adjusting the feeding rate and gas flow rate, and controls the deposition and reaction quality by controlling the concentration of the fluidized reaction gas, thereby achieving batch production control. This invention can uniformly change the reaction or deposition gas in each fluidized gas-solid reaction mechanism, or individually change the deposition or reaction gas in different chambers within each fluidized gas-solid reaction mechanism, exhibiting wide adaptability.

[0035] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments, nor is it limited to the production of silicon-carbon composite materials. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claimed invention.

Claims

1. A continuous fluidized gas-solid reaction apparatus, characterized in that: It includes a heating chamber and a fluidized gas-solid reaction mechanism installed in the heating chamber. The heating chamber includes a shell plate and a heating element (4). The fluidized gas-solid reaction mechanism includes a wall plate (15), multiple fluidized reaction chambers and corresponding gas pipelines. Adjacent fluidized reaction chambers are connected through a channel at the bottom. Upper and lower partitions are staggered between the top and bottom wall plates (15). The upper and lower partitions together form a serpentine flow channel in the fluidized reaction chamber. The powder is pushed to flow in the flow channel by the height difference of the powder between the chambers. From the side near the feed inlet (5) to the side near the discharge outlet (8), the height of the lower partition of the fluidized reaction chamber decreases sequentially.

2. The continuous fluidized gas-solid reaction apparatus according to claim 1, characterized in that: An inert gas is introduced into the space between the heating chamber and the fluidized gas-solid reaction mechanism.

3. The continuous fluidized gas-solid reaction apparatus according to claim 1, characterized in that: It can be used independently by one set of devices or in series by multiple sets of devices.

4. The continuous fluidized gas-solid reaction apparatus according to claim 1, characterized in that: The shell plate includes an outer shell plate (1), a thermal insulation material layer (2), and an inner shell plate (3). The thermal insulation material layer (2) is disposed in the interlayer between the outer shell plate (1) and the inner shell plate (3), and the heating element (4) is installed on the inner shell plate (3).

5. A continuous fluidized gas-solid reaction apparatus according to claim 1, characterized in that: The fluidized gas-solid reaction mechanism includes a feed inlet (5), a discharge outlet (8), a carrier gas pipe (10), a reaction gas pipe (11), a gas distribution plate (14), an exhaust pipe (6), and a pulse backflush pipe (7). The gas distribution plate (14) is located on the lower side of the wall panel (15). The heating chamber and the wall panel (15) have feed inlets (5) and discharge outlets (8). The pulse backflush pipe (7) and the exhaust pipe (6) are both located on the upper side of the fluidized gas-solid reaction mechanism. The carrier gas pipe (10) and the reaction gas pipe (11) are both located on the lower side of the fluidized gas-solid reaction mechanism. The inlet of the reaction gas pipe (11) is equipped with a reaction gas solenoid valve (12), and the inlet of the carrier gas pipe (10) is equipped with a carrier gas solenoid valve (9).

6. A continuous fluidized gas-solid reaction apparatus according to claim 1, characterized in that: Each fluidized reaction chamber is equipped with a gas distribution plate (14) and a gas chamber below it; the gas chamber is formed by the gas distribution plate (14) and the gas chamber wall panel (13), and each gas chamber is equipped with a flow control valve on its lower side.

7. A continuous fluidized gas-solid reaction apparatus according to claim 1, characterized in that: Each fluidized reaction chamber is equipped with one or more pairs of filters on its upper side, and each filter is equipped with a backflushing and discharge control valve on its upper side.

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