CN214486909U - A kind of vertical reaction furnace and preparation device for preparing silicon monoxide - Google Patents
A kind of vertical reaction furnace and preparation device for preparing silicon monoxide Download PDFInfo
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- CN214486909U CN214486909U CN202022952433.0U CN202022952433U CN214486909U CN 214486909 U CN214486909 U CN 214486909U CN 202022952433 U CN202022952433 U CN 202022952433U CN 214486909 U CN214486909 U CN 214486909U
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Abstract
本实用新型公开了一种用于制备一氧化硅的竖式反应炉及制备装置，本实用新型通过在竖式反应炉的中心管中通入氩气，从中心管下部穿过反应器内的原料层，一方面有利于原料内部均匀分散，减少物料烧结团聚，另一方面及时将一氧化硅气体产物带出，提高产物逸出率，从而提高生产效率；一氧化硅制备装置冷却收集器分别设置了多孔陶瓷挡板、微孔金属挡板和无孔金属侧壁来分别拦截未反应的原料粉末和凝结一氧化硅产物，形成原料粉尘收集室、第一产物收集室和第二产物收集室，提高产物纯度，实现了一氧化硅粉体的连续制备。
The utility model discloses a vertical reaction furnace and a preparation device for preparing silicon monoxide. In the utility model, argon gas is introduced into the central tube of the vertical reaction furnace, and the lower part of the central tube passes through the inner tube of the reactor. The raw material layer, on the one hand, is conducive to the uniform dispersion of the raw materials and reduces the sintering and agglomeration of the materials; Porous ceramic baffles, microporous metal baffles and non-porous metal sidewalls are provided to intercept unreacted raw material powder and condensed silicon monoxide products respectively, forming a raw material dust collection chamber, a first product collection chamber and a second product collection chamber , improve the product purity, and realize the continuous preparation of silicon monoxide powder.
Description
Technical Field
The utility model belongs to the technology of SiO preparation, concretely relates to a vertical reacting furnace and preparation facilities for preparing SiO.
Background
At present, the commercial cathode material of the lithium ion battery is generally a graphite material, the theoretical specific capacity of the graphite material is 372mAh/g, and the demand of the fields of rapidly developed consumer electronics products, new energy automobiles and the like on the high energy density of the battery cannot be met. The theoretical specific capacity of the silicon-based material reaches 4200mAh/g, and the silicon-based material is a key material for developing next-generation high-specific-energy lithium ion batteries. However, the silicon has the problems of large volume effect and poor cycle performance in the cycle process. The silicon monoxide integrates the characteristics of large specific capacity and stable cycle, and is one of ideal materials for the cathode of the lithium ion battery.
Most of traditional SiO production equipment is a single vacuum furnace, raw materials are accumulated in a furnace body, the distance between a material center region and a furnace wall heating source is far, heat transfer and reaction efficiency is inconsistent with the peripheral region of the raw materials, so that the yield is low, the energy consumption is high, the batch stability is poor, and a product is usually a SiO block and needs to be further crushed to be suitable for a powder material for battery manufacturing, so that the process flow is increased, and the manufacturing cost is increased.
SUMMERY OF THE UTILITY MODEL
The utility model provides a technical problem be: aiming at the problems of low production efficiency, poor product consistency and the like in the existing silicon monoxide production equipment, the vertical reaction furnace and the preparation device for preparing the silicon monoxide are provided.
The utility model discloses a following technical scheme realizes:
the vertical reaction furnace for preparing the silicon monoxide comprises a furnace body, a central pipe and a reaction heater;
the furnace body is vertically arranged, the central tube is vertically fixed in the furnace body, an annular space formed between the inner wall of the furnace body and the outer wall of the central tube is a reaction bin for preparing silicon monoxide by reaction, the reaction bin is communicated with a first vacuum pump, and the reaction heater is arranged on the furnace body on the outer wall of the reaction bin in a surrounding manner;
the continuous blanking device is arranged at the top of the furnace body and is in butt joint with the reaction bin, the inner tube cavity of the central tube is communicated with the inert gas input tube, the central tube is provided with a plurality of air holes communicated with the reaction bin, and the reaction bin is led out of the furnace body and is provided with an inert gas output tube.
A vertical reacting furnace for preparing silicon monoxide in the above scheme, it is further, furnace body inner wall bottom sets up the funnel inclined plane, the bottom on funnel inclined plane forms decurrent counter bore, the center tube bottom is inserted and is inlayed in this counter bore, center tube upper portion is equipped with the locating lever outward, the center tube passes through the support location between locating lever and the furnace body inner wall.
The vertical reaction furnace for preparing the silicon monoxide in the scheme is further provided with a hoisting hole on the top of the central tube.
The utility model discloses an among the vertical reaction furnace for preparing silicon monoxide, the furnace body includes outer jar and the pot bottom and the upper cover plate of sealed assembly at outer tank bottoms portion and top respectively, form the reaction chamber between the inner wall of outer jar and the center tube, the upper cover plate corresponds reaction chamber annular cross section and is equipped with a plurality of charge inlets, corresponds the center tube and is equipped with the air inlet of introducing the inert gas input tube, reaction heater arranges around outer jar outer wall to wrap up in the outer layer and set up the heat preservation.
The vertical reaction furnace for preparing the silicon monoxide in the scheme is further characterized in that the continuous blanking device comprises a storage bin and a plurality of blanking pipes, the blanking pipes are communicated with the charging openings of the upper cover plate in a one-to-one butt joint mode, all the blanking pipes are connected with the storage bin in a junction mode, the storage bin is connected with a second vacuum pump, and a feeding valve is arranged between the storage bin and the blanking pipes.
The utility model also discloses a preparation device for preparing the silicon monoxide, which comprises a cooling collector and the vertical reaction furnace;
the cooling collector comprises a raw material dust collecting chamber, a first product collecting chamber and a second product collecting chamber which are sequentially connected in series, the raw material dust collecting chamber is provided with a condensation air inlet and is separated from the first product collecting chamber through a porous baffle plate, the first product collecting chamber is separated from the second product collecting chamber through a microporous baffle plate, the aperture of the microporous baffle plate is smaller than that of the porous baffle plate, a nonporous metal side wall is arranged in the second product collecting chamber, a condensation air outlet is arranged in the second product collecting chamber, and the raw material dust collecting chamber, the first product collecting chamber and the second product collecting chamber are connected with a third vacuum pump;
an inert gas input pipe of the vertical reaction furnace is connected with an inert gas tank, an inert gas output pipe of the vertical reaction furnace is in butt joint with a condensation gas inlet of a cooling collector through a condensation pipe, and a condensation gas outlet of the cooling collector is connected to an inert gas collecting tank;
the inert gas output pipe is provided with a first valve, the inert gas input pipe is provided with a second valve, and the condensation gas outlet is provided with a third valve.
In the preparation device for preparing SiO in the above scheme, further, the aperture on the porous baffle is 0.1-1mm, and the aperture on the microporous baffle is 1-100 μm.
In the preparation apparatus for preparing SiO in the above scheme, a gas heater is further arranged between the inert gas tank and the inert gas input pipe.
A preparation facilities for preparing silicon monoxide among the above-mentioned scheme, it is further, the bottom of raw materials dust collection room, first result collection room and second result collection room is equipped with first bleeder valve, second bleeder valve and third bleeder valve respectively.
The utility model discloses compare with current monogamy production facility, have following beneficial effect:
(1) the loading capacity of a single tank can be improved by increasing the inner diameter of the outer tank of the furnace body and the outer diameter of the central pipe, so that the yield of the silicon monoxide in the single tank is improved;
(2) because the space distance of the furnace body is within the reasonable reaction depth, the central area of the furnace body is provided with the central pipe for replacement to form the annular reaction bin, the heating distance of the reaction heater to the raw materials in the reaction bin is more reasonable and uniform, and the good heat transfer and the high reaction efficiency can be effectively maintained;
(3) argon is introduced into the central tube, and the argon passes through the raw material layer from the lower part of the central tube, so that the uniform dispersion of the interior of the raw material is facilitated, the sintering and agglomeration of the material are reduced, and the silicon monoxide gas product is taken out in time, so that the product escape rate is improved, and the production efficiency is improved;
(4) the cooling end is respectively provided with a porous ceramic baffle, a microporous metal baffle and a nonporous metal side wall to respectively intercept unreacted raw material powder and a condensed silicon monoxide product to form a raw material dust collecting chamber, a first product collecting chamber and a second product collecting chamber, so that the product purity is improved, and the direct preparation of the silicon monoxide powder is realized;
(5) utilize continuous unloader to feed in raw material, realized continuous production, the center tube can promote the automatic discharge that dismantles the slag charge that realizes not reacting through mechanical system, effectively reduces the intensity of labour in the production process, improves productivity.
To sum up, the utility model provides a vertical reacting furnace for preparing SiO improves the inside homodisperse of raw materials and conducts heat, improves SiO and spills over efficiency, and holistic SiO preparation facilities can realize the continuous preparation of SiO powder, and the product uniformity is good.
The present invention will be further described with reference to the accompanying drawings and the following detailed description.
Drawings
FIG. 1 is a schematic view of a vertical reactor for preparing SiO according to example I.
FIG. 2 is a schematic structural diagram of a second embodiment of a production apparatus for producing SiO.
Reference numbers in the figures: 1-continuous blanking device, 11-storage bin, 12-blanking pipe, 2-vertical reaction furnace, 20-reaction bin, 21-outer tank, 22-upper cover plate, 221-charging hole, 222-air inlet, 23-tank bottom cover, 24-supporting seat, 25-central pipe, 251-positioning rod, 252-hoisting hole, 253-air hole, 26-reaction heater, 27-heat preservation layer, 28-condensation pipe, 3-cooling collector, 31-porous baffle, 311-raw material dust collection chamber, 32-microporous baffle, 321-first product collection chamber, 33-nonporous metal side wall, 331-second product collection chamber, 34-condensation air inlet, 35-condensation air outlet, 4-argon tank, 41-gas heater, 42-argon gas collecting tank, 51-first vacuum pump, 52-second vacuum pump, 53-third vacuum pump, 61-feeding valve, 62-first valve, 63-second valve, 64-third valve, 65-first discharge valve, 66-second discharge valve and 67-third discharge valve.
Detailed Description
Example one
Referring to fig. 1, the vertical reactor in the figure is a specific embodiment of the present invention, and the silicon and silica are used in the reduction reaction under vacuum condition to produce and prepare silicon monoxide, and specifically includes a storage silo 11, a blanking pipe 12, an outer tank 21, an upper cover plate 22, a tank bottom cover 23, a supporting seat 24, a central pipe 25, a reaction heater 26, a heat insulation layer 27, a first vacuum pump 51, a second vacuum pump 52 and a feeding valve 61.
Specifically, the vertical setting of furnace body of vertical reacting furnace 2 sets up center tube 25 at the inside vertical fixed setting of furnace body, and the annular space that forms between the outer wall of furnace body inner wall and center tube 25 is reaction storehouse 20 of reaction preparation silicon monoxide, and reaction storehouse 20 and first vacuum pump 51 intercommunication establish the vacuum reaction environment in reaction storehouse 20 through first vacuum pump 51, encircle to set up reaction heater 26 at the outer wall of furnace body 25, reach reaction temperature through reaction heater 26 to reaction storehouse 20 heating. The continuous blanking device 1 is arranged at the top of the furnace body and is in butt joint with the reaction bin 20, continuous blanking of silicon and silicon dioxide raw material pellets is realized through the continuous blanking device 1, an inner cavity of the central tube 25 is communicated with an inert gas input tube, inert gas is input into the central tube 25 through the inert gas input tube, a plurality of air holes 253 communicated with the reaction bin 20 are arranged on the central tube 25, an inert gas output tube is led out of the reaction bin 20 to the outside of the furnace body, inert gas (such as argon) enters the reaction bin 20 through the air holes on the central tube 25, the inert gas does not participate in the reduction reaction in the reaction bin 20, silicon monoxide steam generated by the reaction in the reaction bin 20 is output through the inert gas output tube through the inert gas, and a silicon monoxide product is obtained by separation from the inert gas.
The furnace body in this embodiment includes an outer tank 21, an upper cover plate 22 and a tank bottom cover 23, the outer tank 21 is a cylinder, the bottom of the outer tank 21 is welded with support legs, the whole furnace body is kept in a vertical state by the support legs, the upper cover plate 22 is hermetically assembled on the top of the outer tank 21, the tank bottom cover 23 is hermetically assembled on the bottom of the outer tank 21, the outer tank 21 is sealed up and down, a reaction chamber 20 is formed between the inner wall of the outer tank 21 and a central tube 25, the upper cover plate 22 is fixed with the top of the outer tank 21 by a flange structure, the upper cover plate 22 is provided with a plurality of feed inlets 221 corresponding to the annular cross section of the reaction chamber 20, the feed inlets 221 are at least two, the diameter of the feed inlets 221 is smaller than or equal to the difference between the inner diameter and the outer diameter of the annular cross section of the reaction chamber 20, the central tube 25 is provided with an air inlet 222 for introducing inert gas, the reaction heater 26 adopts an electromagnetic heating coil arranged around the outer wall of the outer tank, and the outer layer of the reaction heater 26 is wrapped with a heat insulation material to form a heat insulation layer 27, so that heat dissipation is prevented, and the reaction temperature is kept constant.
The funnel inclined plane is set to bottom the furnace body inner wall of outer jar 21, the bottom on funnel inclined plane forms decurrent counter bore, the bottom of center tube 25 is fixed to be inserted and is inlayed in this counter bore, with outer jar 21 concentric location, center tube 25 upper portion outwards is equipped with a plurality of locating levers 251 along radial, the upper portion of center tube 25 is passed through and is supported the location between locating lever 251 and the furnace body inner wall of outer jar 21, guarantee vertical coaxial between center tube 25 and the outer jar 21, the top and the upper cover plate 22 butt of center tube 25, be equipped with a plurality of hole for hoist 252 along the circumferencial direction at the top of center tube 25, be convenient for carry out the dismouting through the hoist and mount to center tube 25.
In the present embodiment, the material of the outer tank 21 is preferably centrifugally cast from heat-resistant Ni — Cr steel; the wall thickness of the outer tank 21 is 30mm-50mm, and the inner diameter is 800mm-2000 mm; a circle of flange skirt edge with the width of 50-80mm is processed at the upper end of the outer tank 21, 6-24 through holes with the aperture of 18-30mm are uniformly drilled on the flange along the circumference, and the positions of the drilled holes are the same as the positions of the drilled holes on the upper cover plate; the lower part of the outer tank 21 is funnel-shaped, the inclination angle theta value of the inclined plane of the funnel-shaped upper part is between 45 degrees and 60 degrees, the diameter of the cylindrical part of the funnel-shaped lower neck is 10-20mm larger than the outer diameter of the central pipe, so that the central pipe 25 can be conveniently inserted, the outer tank 21 is welded with a supporting seat 24 for positioning the central pipe 25 in the funnel-shaped lower neck cylinder, a bottom flange is welded at the bottom of the funnel-shaped lower neck, 6-24 through holes with the aperture of 18-30mm are drilled on the bottom flange, and the bottom flange is fixedly assembled with the tank bottom cover 23 through flanges and bolts.
The thickness of the upper cover plate 22 is 30-50mm, the material is preferably one of 45# steel or A3 steel, and a water cooling jacket is welded on the upper cover plate; the outer diameter of the upper cover plate 22 is equal to the outer diameter of the top flange of the outer tank 21; a circular groove is formed in the matching area of the inner side of the upper cover plate 22 and the flange of the outer tank 21 and used for placing a sealing ring, and the sealing ring is made of silicon rubber; the top flanges of the upper cover plate 22 and the outer tank 21 are drilled with 6-24 through holes with the aperture of 18-30mm along the circumference, bolts simultaneously penetrate through the holes on the flange of the outer tank 21 and are locked with the holes on the upper cover plate 22, and the tight connection between the outer tank 21 and the upper cover plate 22 is realized through bolt connection.
The thickness of the tank bottom cover 23 is 30-50mm, the material is preferably one of 45# steel or A3 steel, and a water cooling jacket is welded on the tank bottom cover; the outer diameter of the tank bottom cover 23 is equal to the outer diameter of a bottom flange of the funnel-shaped lower neck of the outer tank 21; a circular groove for placing a sealing ring is formed in the matching area of the inner side of the tank bottom cover 23 and the flange of the outer tank 21, and the sealing ring is made of silicon rubber; 6-24 through holes with the aperture of 18-30mm are drilled at the position of the tank bottom cover 23 corresponding to the bottom flange of the outer tank 21, bolts simultaneously penetrate through the holes on the bottom flange of the outer tank 21 and are locked with the holes on the tank bottom cover 23, and the tight connection between the lower part of the outer tank 21 and the tank bottom cover 23 is realized through bolt connection.
The material of the central tube 25 is preferably formed by centrifugally casting heat-resistant Ni-Cr steel; the wall thickness of the central tube 25 is 30mm-50mm, the outer diameter of the central tube 25 is determined according to the inner diameter of the outer tank, and the radial distance between the outer wall of the central tube 25 and the inner wall of the outer tank 21 is controlled to be 500 mm-1000 mm; three positioning rods 251 which are used for positioning the central tube 25 in the outer tank 21 and are not inclined are welded on the same horizontal plane at the upper end of the central tube 25, and the length of each positioning rod 251 is 5-10mm shorter than the distance between the outer wall of the central tube 25 and the inner wall of the outer tank 21; three hoisting holes 252 are drilled at the top of the central tube 25, and external hoisting equipment can conveniently hook the holes through the hoisting holes 252 so as to hoist the central tube from the interior of the furnace body.
The continuous unloader 1 that sets up on the vertical reacting furnace of this embodiment includes storage silo 11 and a plurality of unloading pipe 12, the charge door 221 that sets up on unloading pipe 12 and the upper cover plate 22 docks the intercommunication one by one, the quantity of unloading pipe 12 and charge door 221 is designed according to furnace body diameter size, guarantee that raw material pellet passes through charge door 221 and at the inside even blanking of reaction bin 20, all unloading pipe 12 concentrate with storage silo 11 tandem, storage silo 11 is fixed to be set up in the top of unloading pipe 12, utilize the automatic unloading of gravity of raw material pellet, storage silo 11 is connected with second vacuum pump 52, and be equipped with feed valve 61 between storage silo 11 and unloading pipe 12, establish the vacuum environment of storage silo 11 in the unloading in-process through second vacuum pump 52, the coordinated control of feed valve 61, can realize the continuous automatic unloading of reaction bin in the production reaction process.
The thickness of the outer walls of a storage bin 11 and a blanking pipe 12 of the continuous blanking device 1 is 30-50mm, the material is preferably one of 45# steel or A3 steel, the upper part of the storage bin 11 is a straight cylinder with a sealing cover at the upper part, the lower part of the storage bin is connected with at least two blanking pipes 12 distributed along the circumference in a branching mode, the blanking pipes 12 are welded on a feed inlet 221 of an upper cover plate 22 in a seamless mode, and a water cooling sleeve is welded on the outer side of each blanking pipe.
Example two
Referring to FIG. 2, there is shown an embodiment of the present invention for preparing SiO, which is based on the vertical reactor of example one and combines with a cooling collector 3 to realize continuous production and preparation of SiO powder. The system specifically comprises a vertical reaction furnace 2, a cooling collector 3, an argon gas tank 4, a gas heater 41, an argon gas collecting tank 42, a third vacuum pump 53, a first valve 62, a second valve 63, a third valve 64, a first discharge valve 65, a second discharge valve 66 and a third discharge valve 67 in the first embodiment. In the embodiment, the vertical reaction furnace 2 is connected with the cooling collector 3 to process the output inert gas and SiO steam mixed gas, and the SiO steam carried by the inert gas is collected in the cooling collector 3 by cooling and condensing.
Specifically, the cooling collector 3 includes a raw material dust collecting chamber 311, a first product collecting chamber 321 and a second product collecting chamber 331 which are sequentially connected in series, a condensation air inlet 34 is arranged on the raw material dust collecting chamber 311, the raw material dust collecting chamber 311 and the first product collecting chamber 321 are separated by a porous baffle 31, raw material powder particles mixed in mixed air flow are filtered in the raw material dust collecting chamber 311, a plurality of pore channels arranged on the porous baffle 31 communicate the raw material dust collecting chamber 311 with the first product collecting chamber 321, the first product collecting chamber 321 and the second product collecting chamber 331 are separated by a microporous baffle 32 to ensure that inert gas can normally pass through, a plurality of pore channels arranged on the microporous baffle 32 communicate the first product collecting chamber 321 with the second product collecting chamber 331, a non-porous metal side wall 33 is arranged in the second product collecting chamber 331, as the SiO vapor in the mixed gas flow passes through the first product collecting chamber 321 and the second product collecting chamber 331, the SiO vapor gradually cools and condenses into powder, and the powder is collected in the first product collecting chamber 321 and the second product collecting chamber 331, and the second product collecting chamber 331 is provided with a condensation gas outlet 35 for discharging the residual inert gas. The raw material dust collection chamber 311, the first product collection chamber 321, and the second product collection chamber 331 are connected to a third vacuum pump 53, and a vacuum environment inside the cooling collector 3 is established by the third vacuum pump 53, thereby preventing the oxidation of the silicon monoxide.
In the embodiment, the inert gas for preparing and producing the silicon monoxide adopts argon, an inert gas input pipe of the vertical reaction furnace 2 is connected with an argon tank 4, a gas heater 41 is arranged between the argon tank 4 and the inert gas input pipe, the argon entering the vertical reaction furnace 2 is preheated and heated by the gas heater 41 to prevent the argon from entering the furnace to reduce the reaction temperature, an inert gas output pipe of the vertical reaction furnace 2 is butted with a condensation gas inlet 34 of a cooling collector 3 by a condensation pipe 28, mixed gas flow output from the vertical reaction furnace 2 is pre-condensed and cooled by the condensation pipe 28, a condensation gas outlet 35 of the cooling collector 3 is connected to an argon collecting tank 42, the argon collecting tank 42 can be provided with pumping equipment to provide power for the argon inside the cooling collector 3 in a vacuum negative pressure state, and the collected argon tail gas is subjected to dust removal, impurity removal and purification, can be conveyed and stored into the argon tank 4 again for cyclic utilization; in this embodiment, a first valve 62 is provided on the inert gas outlet pipe of the vertical reactor 2, a second valve 63 is provided on the inert gas inlet pipe of the argon gas tank 4, and a third valve 64 is provided on the condensation gas outlet of the cooling collector 3.
The thickness of the outer wall of the cooling collector 3 is 30-50mm, the material is preferably one of 45# steel or A3 steel, a porous baffle plate 31, a microporous baffle plate 32 and a non-porous metal side wall 33 are respectively arranged in the cooling collector 3 from the air inlet end of the condenser pipe 28, wherein the porous baffle plate 31 is a porous ceramic baffle plate with the thickness of 30-50mm, the material is preferably one of corundum and silicon carbide, the pore size is 0.1-1mm, and the porosity is 20-80%; the microporous baffle 32 is a microporous metal baffle with the thickness of 30-50mm, the material is preferably one of 45# steel or A3 steel, the aperture is a through hole penetrating through the baffle, the aperture size is 1-100 μm, and the porosity is 10-50%; the non-porous metal side wall 33 is made of metal, no pore channel is arranged on the non-porous metal side wall, the outer wall of the cooling collector is formed by airflow impacting on the surface of the non-porous metal side wall, a cooling coil or a cooling water jacket can be arranged inside the non-porous metal side wall 33, the cooling and condensation conditions are provided for SiO steam impacting on the non-porous metal side wall, and the condensation air outlet 35 is arranged above the non-porous metal side wall 33.
Argon gas coming out from a gas hole at the lower part of a central pipe 25 of the vertical reaction furnace 2 passes through a raw material layer in the reaction bin 20 and then carries silicon monoxide vapor out, the argon gas flows out from an inert gas output pipe at the upper part of an outer tank and enters the cooling collector 3 after being preliminarily condensed by a condensing pipe 28, and firstly reaches the porous ceramic baffle plate, the argon gas input from the vertical reaction furnace 2 contains silicon monoxide vapor and simultaneously mixes a part of raw material particles, the aperture of the microporous baffle plate 32 in the cooling collector 3 of the embodiment is smaller than that of the porous baffle plate 31, when mixed gas flow enters the first product collecting chamber 321 from the raw material dust collecting chamber 311, gaseous argon gas and silicon monoxide vapor can normally pass through a pore channel on the porous baffle plate 31 and enter the first product collecting chamber 321, and the mixed raw material particles in the gas can be blocked and filtered in the raw material dust collecting chamber 311 by the porous baffle plate 31, reducing impurities subsequently entering the SiO product. The SiO in the first and second product collecting chambers 321 and 331 condenses into solid powder with the gradual decrease of temperature, and the solid powder is collected in the first and second product collecting chambers 321 and 331, wherein the SiO vapor continues to flow with the argon gas and reaches the microporous metal baffle plate, and most of the SiO gas is deposited on the side wall of the microporous metal baffle plate on one side of the first product collecting chamber in powder form; the argon carries the residual SiO gas to further flow to the non-porous metal side wall in the second product collection chamber 331, the residual SiO gas is deposited and collected in the second product collection chamber, and the argon is reserved from the upper condensation gas outlet 35 and enters a gas circulation system for recycling. The first discharge valve 65, the second discharge valve 66, and the third discharge valve 67 are provided at the bottom of the raw material dust collection chamber 311, the first product collection chamber 321, and the second product collection chamber 331, respectively, and discharge the respective collection chambers.
When the pore channels on the porous baffle 31 and the microporous baffle 32 are blocked, the inside of the cooling collector 3 can be back-blown through the condensation gas outlet 35 by controlling the gas-pumping equipment of the argon gas collecting tank 42.
The process for the continuous preparation of SiO powder in this example was as follows:
in the first step, the vertical reactor and the cooling collector are assembled, and all valves are kept closed. Specifically, the continuous blanking device 1 is hoisted to the upper part of the vertical reaction furnace 2, the upper cover plate 22 is tightly connected with the top flange of the outer tank 21 through bolts, and the blanking pipe 12 of the continuous blanking device 1 is aligned to the annular reaction bin 20 between the outer tank 21 and the central pipe 25; the tank bottom cover 23 is tightly connected with a bottom flange of the outer tank 21 by bolts; the first valve 62 connected to the condensation duct 28 is closed to disconnect the shaft reactor 2 from the cooling collector 3.
Secondly, adding the pre-pressed silicon and silicon dioxide raw material pellets into a storage bin from the upper opening part of the continuous discharging device 1 through a belt conveyor or a manual mode, closing the storage bin after the materials are fully charged, and starting a first vacuum pump 51 and a second vacuum pump 52 to enable the pressure in the storage bin 11 and the reaction bin 20 to reach a vacuum negative pressure environment of 1-1000 Pa; opening the feeding valve 61 on the storage bin 11 to enable the raw material pellets to fall into the reaction bin 20 through the discharging pipe 12, closing the feeding valve 61 after the reaction bin 20 is filled to two thirds, opening the upper opening of the storage bin 11 to break vacuum, continuously filling the raw material pellets into the storage bin for later use, and repeating the processes of vacuumizing and discharging when the reaction of the raw materials in the reaction bin is finished to realize continuous discharging.
Thirdly, opening a third vacuum pump 53, vacuumizing the interior of the cooling collector to 1-1000Pa, simultaneously starting a reaction heater to heat the reaction bin, when the temperature reaches 1100-1500 ℃, opening a second valve, preheating inert gas in an inert gas tank to the reaction temperature through a gas heater, introducing the inert gas into a reaction bin from a gas inlet on an upper cover plate through a central pipe, introducing silicon monoxide product steam generated by the reaction into a cooling collector through a condensing pipe along with gas flow, filtering unreacted raw materials mixed in the gas flow in a raw material dust collecting chamber by a porous baffle, condensing the silicon monoxide steam in a first product collecting chamber and a second product collecting chamber by the microporous baffle and a non-porous metal side wall to obtain silicon monoxide powder, allowing the inert gas to flow out of a condensing gas outlet, introducing the inert gas into the inert gas collecting tank through a pipeline, purifying and conveying the inert gas into the inert gas tank for recycling;
opening a third vacuum pump 53, vacuumizing the interior of the cooling collector 3 to 1-1000Pa, simultaneously starting a reaction heater 26 to heat the reaction bin 20 of the outer tank 21, opening a second valve 63 when the temperature reaches the reaction temperature of 1100-1500 ℃, preheating argon in the argon tank 4 to the reaction temperature through a gas heater 41, introducing the argon into the reaction bin 20 from a gas inlet 222 on the upper cover plate through an inert gas input pipe, and controlling the flow of the argon to be 1-10L/h; the silicon monoxide product steam generated by the reaction enters the cooling collector 3 through the condensation gas inlet 34 along with the argon gas flow through the condensation pipe 28; unreacted raw materials in the gas flow are filtered by the porous baffle 31 in the raw material dust collection chamber 311, SiO vapor is condensed by the microporous baffle 32 and the non-porous metal side wall 33 in the first product collection chamber 321 and the second product collection chamber 331 to form SiO powder, inert gas flows out from the condensing gas outlet 35, enters the inert gas collection tank 42 through a pipeline, and is conveyed to an inert gas tank for recycling after purification.
And fourthly, respectively collecting unreacted raw materials and silicon monoxide powder products in a raw material dust collecting chamber 311, a first product collecting chamber 321 and a second product collecting chamber 331, after the materials are filled to two thirds in any one collecting chamber, closing a first valve 62, a second valve 63 and a third valve 64, closing an argon tank, stopping argon circulation, opening a discharge valve of the corresponding collecting chamber for discharging, after the discharging is finished, closing the discharge valve, opening the first valve 62, the second valve 63 and the third valve 64 again, starting argon circulation, continuously collecting reaction products, and realizing the continuous production of the silicon monoxide powder through the continuous discharging and the continuous discharging in the first step.
When the vertical reaction furnace 2 needs to be cleaned or overhauled, the upper cover plate 22 and the continuous blanking device 1 connected to the upper cover plate 22 are moved away, the central tube 25 is slowly lifted from the furnace body, and then the vertical reaction furnace can be cleaned or overhauled through a manhole arranged on the furnace body or the bottom cover 23 of the tank is detached; and after the cleaning or the maintenance is finished, reassembling the vertical reaction furnace according to the first step, and performing continuous production operation again.
Through the process steps of the embodiment, the obtained silicon monoxide powder has high purity, does not contain silicon or silicon dioxide impurities, has particle sizes ranging from submicron to micron, is 0.5-5 mu m, is suitable for being directly used as a negative electrode raw material of a lithium ion battery, and does not need to be further crushed. Because the annular reactor is matched with the argon circulating system, the reaction efficiency is greatly improved, and the yield is doubled compared with that of the traditional single vacuum furnace.
The above description is only exemplary of the present invention and should not be construed as limiting the present invention, and any modification, equivalent replacement or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
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| CN202022952433.0U CN214486909U (en) | 2020-12-08 | 2020-12-08 | A kind of vertical reaction furnace and preparation device for preparing silicon monoxide |
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| CN202022952433.0U CN214486909U (en) | 2020-12-08 | 2020-12-08 | A kind of vertical reaction furnace and preparation device for preparing silicon monoxide |
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| CN112495336A (en) * | 2020-12-08 | 2021-03-16 | 中南大学 | Vertical reaction furnace for preparing silicon monoxide, preparation device and preparation process |
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Effective date of registration: 20230802 Address after: 672100 East of Industrial Avenue, Yanpo Area, Fortune Industrial Park, Xiangcheng Town, Xiangyun County, Dali Bai Autonomous Prefecture, Yunnan Province Patentee after: Dali Chenyu energy storage new material Co.,Ltd. Address before: Yuelu District City, Hunan province 410083 Changsha Lushan Road No. 932 Patentee before: CENTRAL SOUTH University |