CN114073926A - High-temperature reduction reaction device capable of continuous batch production - Google Patents
High-temperature reduction reaction device capable of continuous batch production Download PDFInfo
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- CN114073926A CN114073926A CN202010829835.3A CN202010829835A CN114073926A CN 114073926 A CN114073926 A CN 114073926A CN 202010829835 A CN202010829835 A CN 202010829835A CN 114073926 A CN114073926 A CN 114073926A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0073—Sealings
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/03—Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a high-temperature reduction reaction device capable of realizing continuous batch production, which comprises a sealed heat insulation box, a reaction barrel, a feeding pipeline, a discharging pipeline, a heater, a stirrer, a reducing gas inlet pipeline and an exhaust pipeline. The reaction barrel is arranged in the sealed heat insulation box, and the top and the bottom of the reaction barrel are respectively provided with a feeding hole and a discharging hole. The feeding pipeline penetrates into the sealed heat insulation box and is connected with the feeding hole of the reaction barrel. The discharge pipeline is connected with the discharge port of the reaction barrel and penetrates out of the sealed heat insulation box. The heater is arranged in the sealed heat insulation box and is positioned at the periphery of the reaction barrel. The stirrer penetrates into the sealed heat insulation box and extends into the reaction barrel. The reducing gas inlet pipeline penetrates into the sealed heat insulation box and is connected with the bottom of the reaction barrel. The exhaust pipeline is connected with the top of the reaction barrel and penetrates out of the sealed heat insulation box.
Description
Technical Field
The invention relates to a device, in particular to a high-temperature reduction reaction device capable of realizing continuous batch production.
Background
In the prior art, a tunnel type continuous production high-temperature reaction furnace is commonly used for manufacturing special materials. Taking the production of electrode materials for lithium batteries as an example, a raw material of nano silicon (Si) powder coated with graphite (graphite) particles, for example, is placed in a plurality of containers, and the containers are moved by a conveyor belt through a high-temperature reactor, and heated to a predetermined temperature by the high-temperature reactor, so that silicon in each container can be bonded to a carbon layer, thereby performing surface modification to increase electrical conductivity.
However, since such a tunnel type continuous production high temperature reaction furnace cannot be completely sealed, it is impossible to introduce a special reducing gas (e.g., flammable and explosive gas), and thus the material or product to be manufactured is limited. In addition, since the powder raw material in the container is not stirred, the uniformity of heating is not good, and the contact between the powder raw material and the reducing gas is limited to the surface, and the contact between the powder raw material and the reducing gas is not uniform, so that the uniformity of the product is also challenged.
Disclosure of Invention
In view of the above problems, it is an object of the present invention to provide a high-temperature reduction reactor capable of continuous batch production, which is capable of improving the uniformity of heat reception of the raw material and also has a good contact effect with the reducing gas, and which can be applied to the production process of various materials.
To achieve the above objects, the present invention provides a high temperature reduction reaction apparatus capable of continuous batch production, which comprises a sealed heat insulation box, a reaction barrel, a feeding pipeline, a discharging pipeline, a heater, a stirrer, a reducing gas inlet pipeline and an exhaust pipeline. The reaction barrel is arranged in the sealed heat insulation box, and the top and the bottom of the reaction barrel are respectively provided with a feeding hole and a discharging hole. The feeding pipeline penetrates into the sealed heat insulation box and is connected with the feeding hole of the reaction barrel. The discharge pipeline is connected with the discharge port of the reaction barrel and penetrates out of the sealed heat insulation box. The heater is arranged in the sealed heat insulation box and is positioned at the periphery of the reaction barrel. The stirrer penetrates into the sealed heat insulation box and extends into the reaction barrel. The reducing gas inlet pipeline penetrates into the sealed heat insulation box and is connected with the bottom of the reaction barrel. The exhaust pipeline is connected with the top of the reaction barrel and penetrates out of the sealed heat insulation box.
In one embodiment, the high temperature reduction reaction apparatus further comprises a feed barrel coupled to the reaction barrel through a feed line.
In one embodiment, the reaction barrel is inverted cone shaped.
In one embodiment, the material of the reaction barrel comprises graphite or ceramic, or a combination thereof.
In one embodiment, the stirrer has a stirring rod that extends to a position near the bottom of the reaction tank.
In one embodiment, the stirring rod comprises at least one stirring blade, and the material of the stirring blade comprises graphite or ceramic, or a combination thereof.
In one embodiment, the reducing gas enters the bottom of the reaction barrel through a reducing gas inlet pipeline.
In one embodiment, the high temperature reduction reaction apparatus further includes a vacuum line connected to the reaction tub and extending from the reaction tub to the outside of the sealed heat-insulating box.
In one embodiment, the high temperature reduction reaction device further comprises an inert gas inlet valve and an inert gas outlet valve, the inert gas inlet valve is arranged on the side wall of the sealed heat insulation box, and the inert gas outlet valve is arranged on the top of the sealed heat insulation box.
In one embodiment, the reducing gas entering the reaction tub via the reducing gas inlet line is not parallel to the moving direction of the raw material entering the reaction tub via the feed line.
In one embodiment, the high temperature reduction reaction apparatus further comprises a feeding vacuum line connected to the feeding barrel.
In one embodiment, the high temperature reduction reaction apparatus further comprises at least two discharging barrels respectively connected with the reaction barrel through discharging pipes.
In one embodiment, the high-temperature reduction reaction device further comprises a discharge valve arranged on the discharge pipeline; the material in the reaction barrel enters each discharging barrel in batches through the discharging pipeline by means of switching of the discharging valve.
In one embodiment, the high temperature reduction reaction apparatus further comprises two discharging vacuum pipes respectively connected to the discharging barrels.
As mentioned above, in the high temperature reduction reaction apparatus capable of continuous batch production of the present invention, the reaction vessel is disposed in the sealed heat insulation box, the feed pipe penetrates into the sealed heat insulation box and is connected with the feed port of the reaction vessel, the discharge pipe is connected with the discharge port of the reaction vessel and penetrates out of the sealed heat insulation box, the heater is disposed in the sealed heat insulation box, and is positioned at the periphery of the reaction barrel, the stirrer penetrates into the sealed heat insulation box and extends into the reaction barrel, the reducing gas inlet pipeline penetrates into the sealed heat insulation box and is connected with the bottom of the reaction barrel, and the exhaust pipeline is connected with the top of the reaction barrel and penetrates out of the sealed heat insulation box and other structural designs, so that the raw materials can be fully stirred and heated in the reaction barrel and can also fully contact and react with the reducing gas, therefore, the heating uniformity of the raw materials can be improved, the contact effect with the reducing gas is quite good, and the method can be applied to the manufacturing process of various materials.
In one embodiment of the present invention, the high temperature reduction reaction apparatus can achieve the purpose of continuous batch production and reducing energy consumption caused by temperature increase and decrease.
Drawings
Fig. 1A is a schematic view of a high-temperature reduction reaction apparatus according to an embodiment of the present invention.
FIG. 1B is a schematic diagram of the high-temperature reduction reaction apparatus shown in FIG. 1A.
FIG. 2 is a schematic view of another embodiment of the high-temperature reduction reaction apparatus according to the present invention.
Detailed Description
A high-temperature reduction reaction apparatus capable of continuous batch production according to the present invention will be described with reference to the accompanying drawings, in which like elements are described with like reference numerals.
The high-temperature reduction reaction apparatus (referred to as a high-temperature reduction reaction apparatus for short) capable of continuous batch production of the following examples performs thermal reduction at a high temperature to manufacture a specific material or product. The following description will be made by taking an example in which a nano-silicon powder raw material coated with graphite particles is reacted in a high-temperature reduction reactor, and then silicon is bonded to a carbon layer. Of course, the high temperature reduction reaction apparatus of the present embodiment may also be applied to manufacture other materials or products.
Referring to fig. 1A and fig. 1B, fig. 1A is a schematic diagram of a high temperature reduction reaction device according to an embodiment of the invention, and fig. 1B is an application schematic diagram of the high temperature reduction reaction device of fig. 1A.
The high-temperature reduction reaction device 1 comprises a sealed heat insulation box 11, a reaction barrel 12, a feeding pipeline IP, a discharging pipeline OP, a heater 14, a stirrer 15, a reducing gas inlet pipeline 16 and an exhaust pipeline 17. In addition, the high temperature reduction reaction apparatus 1 of the present embodiment further includes a feeding barrel 13, a vacuum pipeline 18, an inert gas inlet valve 191, an inert gas outlet valve 192, and a feeding vacuum pipeline 132.
The reaction barrel 12 is disposed in the sealed heat insulating box 11. As the name suggests, the sealed heat insulation box 11 can completely seal the reaction barrel 12, so that the high-activity reducing gas for reaction is prevented from leaking out to cause production danger; the sealed heat insulation box 11 can also insulate heat energy, so that the influence of external environment and temperature on the thermal reduction reaction in the reaction barrel 12 is avoided, and meanwhile, the heat energy in the reaction barrel 12 is also prevented from being dissipated outwards. Wherein, the top 121 and the bottom 122 of the reaction barrel 12 are respectively provided with a feeding port I and a discharging port O.
The feeding pipe IP passes through the sealed heat insulation box 11 and is connected with the feeding port I of the reaction barrel 12, and the discharging pipe OP is connected with the discharging port O of the reaction barrel 12 and passes through the sealed heat insulation box 11. In this embodiment, a feeding valve I1 is disposed on the feeding pipeline IP outside the sealed heat-insulating box 11, a discharging valve O1 is also disposed on the discharging pipeline OP outside the sealed heat-insulating box 11, and the discharging pipeline OP is connected to a discharging barrel 20. Therefore, when the thermal reduction reaction of the reaction barrel 12 is completed, the raw material S (labeled in fig. 1B) in the reaction barrel 12, which completes the thermal reduction reaction, can be controlled to enter the discharging barrel 20 through the discharging valve O1. The material of the reaction barrel 12 of the present embodiment may include graphite (which may be artificial graphite) or ceramic, or a combination thereof. The heat transfer efficiency can be increased by the reaction barrel 12 including graphite or ceramic material.
The feed barrel 13 is connected to the reaction barrel 12 through a feed line IP. In some embodiments, the side view of the material feeding barrel 13 may be substantially reverse conical shape, which is beneficial for the material to fall down without excessive residue. The input barrel 13 may hold a reaction precursor, which may be, for example, a powder feedstock. In the present embodiment, the reaction precursor is, for example, but not limited to, nano-silicon powder coated with graphite particles; in various embodiments, the reaction precursor may also be a nano-Silica (SiO) powder coated with graphite particles or other raw materials, depending on the product to be produced. The feeding barrel 13 is provided with a feeding pipeline 131, the feeding pipeline 131 is connected with the feeding barrel 13, the feeding pipeline 131 is provided with a feeding valve 1311, and whether the raw materials enter the feeding barrel 13 or not can be controlled through the feeding valve 1311.
In addition, the feeding vacuum pipeline 132 is connected with the feeding barrel 13, and the feeding vacuum pipeline 132 is provided with a feeding vacuum valve 1321, and whether vacuum pumping is performed or not is controlled through the feeding vacuum valve 1321; the purpose of the evacuation is to keep the reaction mass from coming into contact with oxygen as much as possible when entering the charging basket 13, thereby increasing the reduction efficiency. Therefore, before the material enters the material inlet barrel 13, the material inlet vacuum valve 1321 may be opened to perform vacuum pumping, and the material inlet valve 1311 may be opened after maintaining the high vacuum degree in the material inlet barrel 13, so that the material may rapidly enter the material inlet barrel 13. In addition, in some embodiments, the discharging vacuum pipeline 201 is connected to the discharging barrel 20, and a discharging vacuum valve 2011 is disposed on the discharging vacuum pipeline 201 to control whether to vacuumize through the discharging vacuum valve 2011; the purpose of the vacuum pumping is to keep the material after the reduction reaction from contacting with oxygen when entering the discharging barrel 20. Therefore, before the material after the reduction reaction enters the discharging barrel 20, the discharging vacuum valve 2011 can be opened to vacuumize, the high vacuum degree in the discharging barrel 20 is maintained, and then the discharging valve O1 is opened, so that the raw material can enter the discharging barrel 20.
The heater 14 is disposed in the sealed heat insulating box 11 and is located at the periphery of the reaction tub 12. Here, the heater 14 may heat the reaction barrel 12 so that the raw material S in the reaction barrel 12 may be heated to a high temperature required for the reduction reaction for a certain period of time. In some embodiments, a reflector (such as, but not limited to, a mirror, a reflective sheet, or a reflective film layer) may be further utilized to reflect the heat energy radiated to the side wall 112 of the sealed heat insulating box 11, thereby increasing the heating efficiency.
The agitator 15 is disposed at the top 111 of the sealed and thermally insulated box 11, and penetrates into the top 111 of the sealed and thermally insulated box 11 and extends into the reaction tub 12. Here, the stirrer 15 has a stirring rod 151 and a driver 152 (e.g., a motor), and the driver 152 is linked with the stirring rod 151 and can drive the stirring rod 151 to rotate so as to stir the raw material S in the reaction tank 12. The stirring rod 151 of the present embodiment penetrates the top 111 of the airtight and heat-insulating box 11 and the top 121 of the reaction tub 12, and extends to the position where the reaction tub 12 is close to the bottom 122 thereof, thereby improving the stirring effect of the raw material S in the reaction tub 12.
It should be noted that the side view of the reaction barrel 12 of the present embodiment is, for example, a substantially reverse cone shape, which is beneficial for the raw material to fall down without excessive residue, and at the same time, the stirring degree of the stirring rod 151 can be increased (i.e. the stirring is more uniform), so as to increase the contact time and contact uniformity with the reducing gas. The stirring rod 151 of the present embodiment includes at least one stirring blade 1511, and the material of the stirring blade 1511 may include graphite or ceramic, or a combination thereof. Since the temperature inside the reaction tub 12 is relatively high, the stirring blade 1511 made of graphite or ceramic can prevent the problem that the conventional stirring rod made of nickel stainless steel causes nickel precipitation under high-temperature reducing gas to damage the reaction tub 12.
The reducing gas inlet pipe 16 penetrates the sealed heat insulating box 11 and extends to the bottom 122 of the reaction barrel 12 to be connected with the bottom 122 of the reaction barrel 12. Here, the reducing gas inlet pipe 16 penetrates the sealed heat insulating box 11 from the side wall 112 of the sealed heat insulating box 11. The reducing gas inlet line 16 is provided with a reducing gas inlet valve 161 to control the introduction of the reducing gas a1 into the reaction tub 12. In some application examples, the reducing gas A1 may include, for example, but is not limited to, H2(hydrogen) CH4(methane), C2H2(acetylene), N2(nitrogen), or Ar (argon), or other reducing gas, or a combination thereof, depending on the different starting materials S and products. Taking the present application example as an example, when the raw material S is nano-silicon coated with graphite particles, the introduced reducing gas a1 may be CH4And Ar; when the raw material S is nano-silica coated with graphite particles, the introduced reducing gas A1 can be H2、CH4And Ar, depending on the reaction precursor.
Since the side view of the reaction barrel 12 of the present embodiment is an inverted cone, and the stirring rod 151 extends into the reaction barrel 12, and the reducing gas a1 is also transmitted to the bottom 122 of the reaction barrel 12 through the reducing gas inlet line 16, the raw material S can be stirred to uniformly and sufficiently contact and mix with the reducing gas a1, and the reducing gas a1 entering the reaction barrel 12 through the reducing gas inlet line 16 is not parallel to the moving direction of the raw material S entering the reaction barrel 12 through the feeding line IP (the two are almost opposite directions), and the opposite moving directions also increase the chance of uniform contact, and also increase the heating uniformity of the raw material S.
The exhaust duct 17 is connected to the top 121 of the reaction tank 12, and extends through the top 111 of the sealed heat insulation box 11. The exhaust line 17 is provided with an exhaust valve 171, and the excess reducing gas a1 or reaction by-products in the reaction vessel 12 can be removed by controlling the exhaust valve 171. Further, since the raw material S in the reaction vessel 12 falls down by gravity and moves toward the bottom 122 of the reaction vessel 12, the amount of powder carried along when the exhaust line 17 exhausts can be reduced, thereby reducing the loss of the raw material S and reducing the chance of the raw material S clogging the exhaust line 17. In addition, the sealed design of the reaction barrel 12 and the sealed heat insulation box 11 of the present embodiment can also prevent the danger caused by the leakage of the highly reactive reaction gas, reduce the external oxygen ingress, reduce the reduction efficiency and increase the reaction danger.
The vacuum line 18 is connected to the reaction tub 12 and extends from the reaction tub 12 to the outside of the hermetic heat insulating box 11. The vacuum pipe 18 is provided with a vacuum valve 181 and connected to a vacuum pump (not shown), so as to vacuumize the reaction barrel 12 and prevent the gas inside the reaction barrel 12 not participating in the reaction from damaging the thermal reduction reaction.
Further, an inert gas inlet valve 191 is provided in the side wall 112 of the sealed and heat-insulated box 11, and an inert gas outlet valve 192 is provided in the top 111 of the sealed and heat-insulated box 11. In this embodiment, the inert gas inlet valve 191 and the inert gas outlet valve 192 may be pressure control valves, respectively, and the pressure setting of the inert gas inlet valve 191 and the inert gas outlet valve 192 may control the amount of the inert gas a2 (e.g., Ar) entering the sealed heat insulation box 11, and at the same time, the pressure inside the sealed heat insulation box 11 may be maintained at a slight positive pressure, so as to prevent the outside gas (e.g., oxygen) from entering the sealed heat insulation box 11, thereby preventing the reaction between the material of the reaction barrel 12 and the outside gas, and effectively preventing the danger caused by the leakage of the highly reactive gas. In other embodiments, an inert gas inlet line and an inert gas outlet line may be provided, and valves may be provided to control the inert gas inlet line and the inert gas outlet line, respectively, to maintain the micro-positive pressure in the sealed heat insulation box 11, which is not limited by the invention.
As shown in FIG. 1B, the raw material S is used as the nano-silicon powder for coating the graphite particles, and the introduced reducing gas A1 is CH4And Ar is an example to illustrate the manufacturing process. Firstly, before the thermal reduction reaction, the feeding barrel 13 may be evacuated by the vacuum pump through the feeding vacuum pipeline 132 and the feeding vacuum valve 1321, and the reaction barrel 12 may be evacuated through the vacuum pipeline 18 and the vacuum valve 181, after a certain vacuum degree is reached, the nano-silicon powder raw material S may be fed into the feeding barrel 13 and fed into the reaction barrel 12, the reaction barrel 12 is heated (for example, to 900 ℃ -1200 ℃) by the heater 14 and held for a certain period of time, and the stirrer 15 is started to stir and the reducing gas a1 (for example, CH) is introduced into the reaction barrel while stirring4And Ar) to ensure that the raw material S in the reaction barrel 12 can be fully stirred, mixed and contacted with the reducing gas A1 to carry out thermal reduction reaction, and then the raw material S is discharged to the discharging barrel 20 after reaching the time required by the reaction (the discharging barrel 20 needs to be vacuumized in advance), and the cooling time can be shortened by the jacket design (for example, the water channel is used for cooling) of the discharging barrel 20 and/or a cooling and stirring device; then, before feeding another batch of raw materials S, the feeding barrel 13 is vacuumized through the feeding vacuum pipeline 132 and the feeding vacuum valve 1321, the reaction barrel 12 is vacuumized through the vacuum pipeline 18 and the vacuum valve 181, after a certain vacuum degree is reached, another batch of raw materials S is fed into the feeding barrel 13 and fed into the reaction barrel 12 through the feeding barrel 13, the processes of stirring, introducing the reducing gas a1, maintaining the temperature and the like are repeated, so that the raw materials S in the reaction barrel 12 can be fully stirred, mixed and contacted with the reducing gas a1 to perform thermal reduction reaction, and after the time required by the reaction is reached, the raw materials S are discharged to the discharging barrel 20 (or another discharging barrel) to be cooled, and the like.
In view of the above, in the high temperature reduction reactor 1 of the present embodiment, the reaction barrel 12 is heated by the heater 14, and stirred by the stirrer 15, and the reducing gas a1 is introduced from the bottom of the reaction barrel 12, so that the raw material S can be sufficiently stirred and heated, and can be sufficiently contacted with the reducing gas a1, and therefore, the contact effect with the reducing gas a1 is quite good in addition to increasing the uniformity of the heated raw material S.
Fig. 2 is a schematic view of another embodiment of the high-temperature reduction reaction apparatus according to the present invention. The high-temperature reduction reaction apparatus of the present embodiment is substantially the same as the high-temperature reduction reaction apparatus of the previous embodiment in terms of the component composition and the connection relationship of the components. The difference is that the high temperature reduction reaction device 1 of the present embodiment includes another discharging barrel 21 in addition to the discharging barrel 20. The discharging barrels 20 and 21 are connected to the reaction barrel 12 through a discharging line OP and a discharging valve O1, respectively, and the material after the reduction reaction in the reaction barrel 12 can enter the discharging barrels 20 and 21 in batches through the discharging line OP by switching of the discharging valve O1.
In other words, when the first batch of raw material S is discharged to the discharging barrel 20 for cooling, the feeding and high temperature reduction reaction of the second batch of raw material S can be performed, and then the second batch of raw material S is discharged to the discharging barrel 21 for cooling (the discharging barrel 21 is required to be evacuated through the discharging vacuum pipeline 211 and the discharging vacuum valve 2111), thereby achieving continuous batch production. In some embodiments, a plurality of discharge barrels arranged in a circular shape, for example, may be utilized and rotationally switched to receive the material after the reduction reaction, thereby achieving the purpose of continuous and batch production; in other embodiments, a plurality of discharging barrels can be transported by using a conveyor belt, for example, so as to achieve the purpose of continuous and batch production, and the invention does not limit how many discharging barrels are arranged or transported, as long as the purpose of continuous and batch production can be achieved.
Specifically, in the continuous batch production process, since the reaction barrel 12 is heated to the temperature required for the reaction in the first thermal reduction reaction, the temperature in the reaction barrel 12 is almost the same as the temperature required for the reaction when the second batch of raw material S is fed into the reaction barrel 12, and the heater 14 does not need to be heated from a low temperature to the temperature required for the reaction, so that the energy loss caused by the temperature rise and fall of the heater 14 can be reduced.
The above application examples are for manufacturing electrode material of lithium battery, and the reaction precursor may be Si/SiO2And plating a carbon layer by thermal reduction to improve the surface conductivity, wherein the product is Si/C, and the reaction temperature can be 900-1200 DEG CThe reducing gas may comprise CH4、H2Ar, and mixtures thereof; however, the present invention is not limited thereto, and the high-temperature reduction reaction apparatus of the present invention can be applied to manufacture, for example, a special alloy additive, a ceramic material, or a special alloy thermoelectric material, in various application examples.
For example, the reaction precursor may be chromium oxide (Cr) for the preparation of a special alloy additive2O3) The product of thermal reduction to form carbide is chromium carbide (Cr)3C2) The reaction temperature can be 900-1200 ℃, and the reducing gas can comprise CH4/Ar、H2/Ar。
Taking the application in ceramic materials as an example, the reaction precursor is Si/SiO2The product of thermal reduction to form nitride is silicon nitride (Si)3N4) The reaction temperature may be 1200-1400 deg.C, and the reducing gas may include H2、N2And mixtures thereof.
Taking the application in manufacturing special alloy thermoelectric materials as an example, the reaction precursor is cobalt (Co)/antimony trichloride (SbCl)3) The product of the thermal reduction to form an alloy phase is CoSb3(cobalt ore compounds) at a reaction temperature of between 750 ℃ and 1000 ℃, and the reducing gas may comprise H2/Ar。
Taking another example of the application in manufacturing another battery material, the reaction precursor may be graphite, the product of surface modification and reduction of pore fineness by thermal reduction and coating of carbon layer is graphite/carbon, the reaction temperature may be 600-1000 ℃, and the reducing gas may include CH4/Ar、H2and/Ar. The above application examples are only examples and are not intended to limit the present invention.
In summary, in the high temperature reduction reaction apparatus capable of continuous batch production according to the present invention, the reaction barrel is disposed in the sealed heat insulation box, the feeding pipeline penetrates into the sealed heat insulation box and is connected to the feeding port of the reaction barrel, the discharging pipeline is connected to the discharging port of the reaction barrel and penetrates out of the sealed heat insulation box, the heater is disposed in the sealed heat insulation box, and is positioned at the periphery of the reaction barrel, the stirrer penetrates into the sealed heat insulation box and extends into the reaction barrel, the reducing gas inlet pipeline penetrates into the sealed heat insulation box and is connected with the bottom of the reaction barrel, and the exhaust pipeline is connected with the top of the reaction barrel and penetrates out of the sealed heat insulation box and other structural designs, so that the raw materials can be fully stirred and heated in the reaction barrel and can also fully contact and react with the reducing gas, therefore, the heating uniformity of the raw materials can be improved, the contact effect with the reducing gas is quite good, and the method can be applied to the manufacturing process of various materials.
In one embodiment of the present invention, the high temperature reduction reaction apparatus can achieve the purpose of continuous batch production and reducing energy consumption caused by temperature increase and decrease.
The foregoing is by way of example only, and not limiting. It is intended that all equivalent modifications or variations without departing from the spirit and scope of the present invention shall be included in the appended claims.
Claims (14)
1. A high-temperature reduction reaction device capable of continuous batch production is characterized by comprising:
sealing the heat insulation box;
the reaction barrel is arranged in the sealed heat insulation box, and the top and the bottom of the reaction barrel are respectively provided with a feeding hole and a discharging hole;
the feeding pipeline penetrates into the sealed heat insulation box and is connected with the feeding hole of the reaction barrel;
the discharge pipeline is connected with the discharge port of the reaction barrel and penetrates out of the sealed heat insulation box;
the heater is arranged in the sealed heat insulation box and is positioned at the periphery of the reaction barrel;
the stirrer penetrates into the sealed heat insulation box and extends into the reaction barrel;
a reducing gas inlet pipeline penetrating into the sealed heat insulation box and connected with the bottom of the reaction barrel; and
and the exhaust pipeline is connected with the top of the reaction barrel and penetrates out of the sealed heat insulation box.
2. The high-temperature reduction reaction apparatus according to claim 1, characterized by further comprising:
and the feeding barrel is connected with the reaction barrel through the feeding pipeline.
3. A high-temperature reduction reaction apparatus according to claim 1, wherein the reaction barrel is in an inverted cone shape.
4. A high-temperature reduction reaction apparatus according to claim 1, wherein the reaction vessel is made of graphite or ceramic or a combination thereof.
5. A high-temperature reduction reaction apparatus according to claim 1, wherein the stirrer has a stirring rod extending to a position where the reaction tub is near the bottom.
6. A high-temperature reduction reaction device according to claim 5, wherein the stirring rod comprises at least one stirring blade, and the material of the stirring blade comprises graphite or ceramic, or a combination thereof.
7. A high-temperature reduction reaction apparatus according to claim 1, wherein a reducing gas is introduced into the bottom of the reaction tub from the reducing gas inlet line.
8. The high-temperature reduction reaction apparatus according to claim 1, characterized by further comprising:
and the vacuum pipeline is connected to the reaction barrel and extends from the reaction barrel to the outside of the sealed heat insulation box.
9. The high-temperature reduction reaction apparatus according to claim 1, characterized by further comprising:
the inert gas inlet valve is arranged on the side wall of the sealed heat insulation box; and
and the inert gas outlet valve is arranged at the top of the sealed heat insulation box.
10. A high-temperature reduction reaction apparatus according to claim 1, wherein the reducing gas introduced into the reaction tub through the reducing gas inlet line is not parallel to the moving direction of the raw material introduced into the reaction tub through the feed line.
11. The high-temperature reduction reaction apparatus according to claim 1, characterized by further comprising:
and the feeding vacuum pipeline is connected with the feeding barrel.
12. The high-temperature reduction reaction apparatus according to claim 1, characterized by further comprising:
and the two discharging barrels are respectively connected with the reaction barrel through the discharging pipelines.
13. The high-temperature reduction reaction apparatus according to claim 12, characterized by further comprising:
the discharge valve is arranged on the discharge pipeline;
and by switching the discharge valves, the materials in the reaction barrels enter the discharge barrels in batches through the discharge pipelines.
14. The high-temperature reduction reaction apparatus according to claim 12, characterized by further comprising:
and the two discharging vacuum pipelines are respectively connected with the discharging barrel.
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