CN113617295A - Reaction furnace and material production process - Google Patents

Reaction furnace and material production process Download PDF

Info

Publication number
CN113617295A
CN113617295A CN202110950826.4A CN202110950826A CN113617295A CN 113617295 A CN113617295 A CN 113617295A CN 202110950826 A CN202110950826 A CN 202110950826A CN 113617295 A CN113617295 A CN 113617295A
Authority
CN
China
Prior art keywords
raw material
cavity
inner tube
reaction
material cavity
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202110950826.4A
Other languages
Chinese (zh)
Other versions
CN113617295B (en
Inventor
朱润良
陈情泽
谢捷洋
何宏平
朱建喜
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangzhou Institute of Geochemistry of CAS
Original Assignee
Guangzhou Institute of Geochemistry of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guangzhou Institute of Geochemistry of CAS filed Critical Guangzhou Institute of Geochemistry of CAS
Priority to CN202110950826.4A priority Critical patent/CN113617295B/en
Publication of CN113617295A publication Critical patent/CN113617295A/en
Application granted granted Critical
Publication of CN113617295B publication Critical patent/CN113617295B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/10Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/008Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/082Controlling processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/087Heating or cooling the reactor
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K17/00Soil-conditioning materials or soil-stabilising materials
    • C09K17/02Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K17/00Soil-conditioning materials or soil-stabilising materials
    • C09K17/02Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
    • C09K17/06Calcium compounds, e.g. lime
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K17/00Soil-conditioning materials or soil-stabilising materials
    • C09K17/02Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
    • C09K17/08Aluminium compounds, e.g. aluminium hydroxide
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Soil Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Muffle Furnaces And Rotary Kilns (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The application relates to the field of equipment manufacturing, in particular to a reaction furnace and a material production process. The reaction furnace comprises: the inner pipe is provided with a first material cavity and is provided with a discharge hole; the first driving piece is connected with the inner pipe; the outer pipe is sleeved outside the inner pipe, and a second material cavity is formed between the inner pipe and the outer pipe; and the second driving piece is connected with the outer pipe. The inner pipe and the outer pipe are driven to rotate, so that the material in the first material cavity can enter the second material cavity through the discharge hole, and is mixed and reacted with the material in the second material cavity; the atmosphere of the reaction cavity can be controlled by ventilating the air inlet pipe; has the functions of improving the mixing uniformity and controlling the reaction rate and the reaction atmosphere; can be applied to the process which has the regulation and control requirement on the mixing process or the reaction process; in addition, a large amount of materials can be added into the first material cavity and the second material cavity, and the reaction furnace can be applied to large-scale production of materials.

Description

Reaction furnace and material production process
Technical Field
The application relates to the field of equipment manufacturing, in particular to a reaction furnace and a material production process.
Background
The high-temperature solid-phase reaction method is a process method which comprises the steps of uniformly mixing reactants to generate a precursor or an amorphous product, and then roasting at high temperature (200-1000 ℃) to completely react and crystallize the product, and is commonly used for preparing nano materials and the like. For example, silicon nanomaterials are widely used in the fields of lithium ion batteries, solar cells, cermet sintering, composites, refractories, etc. due to their excellent physicochemical properties; the preparation of the silicon nano material by the metallothermic reduction method is usually carried out in a high-temperature atmosphere furnace. For example, soil conditioners (materials added to soil to improve physical, chemical or biological properties of soil) can be used for heavy metal passivation, ph adjustment, water retention and air permeability improvement, and the like; in the preparation process, the components are usually activated by baking or slightly heated to make the components combined more firmly. For the above solid-phase reaction, atoms and ions of each component participating in the reaction are limited by cohesive force of crystals and cannot move freely as in the liquid-phase or gas-phase reaction, and fineness and uniformity of powder are very important for the progress of the solid-phase reaction. The progress of the solid phase reaction at high temperatures is often difficult to control and therefore has an adverse effect on the reaction products.
Disclosure of Invention
An object of the embodiments of the present application is to provide a reaction furnace and a material production process, which aim to solve the problem that the reaction process of the high temperature solid phase reaction is not easy to control.
The present application provides in a first aspect a reaction furnace comprising:
the inner tube is provided with a first material cavity, and a discharge hole which penetrates through the inner tube and is communicated with the first material cavity is formed in the inner tube;
the first driving piece is connected with the inner pipe and is used for driving the inner pipe to rotate;
the outer pipe is sleeved outside the inner pipe and is rotationally connected with the inner pipe, and a second material cavity is formed between the inner pipe and the outer pipe; and
and the second driving piece is connected with the outer pipe and is used for driving the outer pipe to rotate.
The inner pipe is driven to rotate by the first driving piece, the outer pipe is driven to rotate by the second driving piece, so that materials in the first material cavity can enter the second material cavity through the discharge hole, and the materials are reacted or mixed in the second material cavity; the reaction furnace can adjust the particle size and the quality of the material in the first material cavity entering the second material cavity, and has the effect of controlling the mixing or reaction rate; can be applied to the process which has the regulation and control requirement on the mixing process or the reaction process; in addition, a large amount of materials can be added into the first material cavity and the second material cavity, and the reaction furnace can be applied to large-scale production of materials.
In some embodiments of the first aspect of the present application, the inner tube is provided with stirring blades on a side thereof adjacent to the outer tube.
In some embodiments of the first aspect of the present application, the stirring blade includes an extension portion connected to the inner tube, the extension portion extending in a direction perpendicular to an axial direction of the inner tube, and a stirring portion connected to a free end of the extension portion, the stirring portion extending in a direction parallel to the axial direction of the inner tube.
In some embodiments of the first aspect of the present application, the reaction furnace further includes a heating element, the heating element is sleeved outside the outer tube, and the heating element is rotatably connected to the outer tube.
In a second aspect of the application, a material production process based on the above reaction furnace is provided, which comprises the following steps:
placing a first raw material in the first material cavity, and placing a second raw material in the second material cavity;
the heating assembly heats the first feedstock and the second feedstock;
rotating the inner pipe and the outer pipe, and introducing protective gas into the first material cavity or the second material cavity;
the first raw material enters the second raw material cavity through the material hole to react with the second raw material.
In some embodiments of the second aspect of the present application, the first feedstock comprises a clay mineral and a salt, the second feedstock comprises at least one of magnesium, aluminum, sodium, potassium, calcium, and zinc, and the salt comprises NaCl, LiCl, KCl, CaCl2、ZnCl2、MgCl2At least one of (1).
In some embodiments of the second aspect of the present application, the clay mineral is montmorillonite and the salt is NaCl; the second raw material is magnesium; the heating assembly heats the first raw material and the second raw material to 600-700 ℃.
The magnesium metal in the first material cavity can slowly and uniformly enter the second material cavity to react with montmorillonite and NaCl; the controllability of the whole reaction process is good, and the reaction speed can be controlled according to the aperture size of the discharge hole, the rotating speed of the inner tube and the rotating speed of the outer tube. The magnesium metal slowly enters the second material cavity, so that the influence on the appearance of a final product due to high local reaction heat can be avoided.
In some embodiments of the second aspect of the present application, the flow rate of the shielding gas introduced into the first material chamber or the second material chamber is 1 to 10L/min.
In some embodiments of the second aspect of the present application, after the first raw material enters the second raw material chamber through the material hole and reacts with the second raw material, the method further includes:
washing the reaction product with acid, leaching the solid phase with HF, and drying.
In some embodiments of the second aspect of the present application, the first raw material is a clay mineral; the second raw material is a soil additive;
optionally, the first raw material is palygorskite; the second raw material is potassium dihydrogen phosphate;
optionally, the rotating speed of the inner pipe is 60-140r/min, and the rotating speed of the outer pipe is 20-50 r/min.
In the reaction process, the monopotassium phosphate in the first material cavity can slowly and uniformly enter the second material cavity to react with the palygorskite; the effects of slow release and slow reaction are achieved, and the polyphosphate in the obtained soil conditioner can be uniformly distributed on the surface of the palygorskite.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort.
FIG. 1 is a schematic view showing an internal structure of a reaction furnace provided in an embodiment of the present application;
FIG. 2 is a schematic structural diagram of a housing provided by an embodiment of the present application;
fig. 3 shows a schematic structural diagram of a heating assembly provided in an embodiment of the present application.
Icon: 100-a reaction furnace; 110-an inner tube; 111-a first material chamber; 112-discharge hole; 113-stirring blade; 120-an outer tube; 121-second material chamber; 122-a housing; 123-rotating shaft sleeve; 130-a first driving member; 140-a second drive member; 150-a heating assembly; 151-heating element; 152-an insulating layer; 160-support frame.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. The components of the embodiments of the present application, generally described and illustrated in the figures herein, can be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present application, presented in the accompanying drawings, is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the embodiments of the present application, it should be understood that the terms "center", "inside", "outside", and the like refer to orientations or positional relationships based on those shown in the drawings, or orientations or positional relationships that are conventionally arranged when products of the application are used, or orientations or positional relationships that are conventionally understood by those skilled in the art, and are used for convenience of description and simplification of the description, but do not refer to or imply that the referred devices or elements must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the application.
Furthermore, the terms "first," "second," and the like are used merely to distinguish one description from another, and are not to be construed as indicating or implying relative importance.
In the description of the embodiments of the present application, it should also be noted that, unless otherwise explicitly stated or limited, the terms "disposed," "mounted," and "connected" are to be construed broadly, and may for example be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present application can be understood in a specific case by those of ordinary skill in the art.
Example 1
Fig. 1 is a schematic diagram illustrating an internal structure of a reaction furnace 100 according to an embodiment of the present invention, and referring to fig. 1, the embodiment provides a reaction furnace 100, and the reaction furnace 100 is suitable for a high-temperature solid-phase reaction, and it should be noted that the application of the reaction furnace 100 is not limited in the present application, and for example, the reaction furnace 100 may be used for a liquid-solid reaction, or the reaction furnace 100 may also be used for mixing materials and stirring materials.
The reaction furnace 100 includes an inner tube 110, an outer tube 120, a first driving member 130, a second driving member 140, and a heating assembly 150. The first driving member 130 is connected to the inner tube 110 for driving the inner tube 110 to rotate, and the second driving member 140 is connected to the outer tube 120 for driving the outer tube 120 to rotate. The outer tube 120 is sleeved outside the inner tube 110, and a second material chamber 121 is formed between the outer tube 120 and the inner tube 110. The heating assembly 150 is used to heat the inner tube 110 and the outer tube 120.
The inner tube 110 has a first material chamber 111 therein, and the inner tube 110 is provided with an outlet through which a material can be charged into the first material chamber 111 and a cover for opening and closing the opening.
In this embodiment, the inner tube 110 is cylindrical, the outlet of the inner tube 110 is disposed at one end of the inner tube 110, the first driving member 130 is connected to one end of the inner tube 110, and the first driving member 130 can drive the inner tube 110 to rotate.
A plurality of discharge holes 112 are distributed on the inner tube 110 at intervals, and the discharge holes 112 penetrate through the inner tube 110 and are communicated with the first material cavity 111, so that the materials in the first material cavity 111 can be discharged through the discharge holes 112.
In the embodiment, the diameter of the discharging hole 112 is 1 to 5mm, for example, 1mm, 2mm, 3mm, 4mm or 5 mm. The discharge holes 112 are distributed along the length direction of the inner pipe 110 and are also distributed along the circumferential direction of the inner pipe 110.
It should be noted that in other embodiments of the present application, the inner tube 110 may have other shapes, such as a prism shape, a bent tube shape, etc.; accordingly, the shape of the first material chamber 111 is not limited in this application.
In addition, the diameter of the discharge hole 112 may be set according to the particle size in the first material cavity 111 or the reaction speed in the reaction process, and is not limited to the above 1-5 mm, and may be, for example, 0.5mm, 6mm, 7mm, 10mm, and the like; the number of the discharge holes 112 and the distance between two adjacent discharge holes 112 may also be set according to specific requirements, which is not limited in the present application.
In some embodiments of the present application, the inner tube 110 is further provided with an air intake hole for communicating with an air intake assembly; gas, such as reaction gas or shielding gas, may be introduced into the inner tube 110 through the gas inlet holes. It should be noted that, for the embodiment that does not require the gas to be introduced, the inner tube 110 may not be provided with the gas inlet.
In this embodiment, the outer surface of the inner tube 110 is further provided with a stirring blade 113; the stirring blade 113 is located on the outer surface of the inner tube 110 far from the first material chamber 111.
In the present embodiment, the stirring vanes 113 include an extended portion connected to the inner tube 110, the extended portion extending in a direction perpendicular to the axial direction of the inner tube 110, and a stirring portion extending in a direction parallel to the axial direction of the inner tube 110. The stirring part is connected with the free end of the extension part. The extension part is perpendicular to the stirring part. For example, in some embodiments, the extension is connected to the middle of the stirring section and the stirring vanes 113 are generally T-shaped, it being understood that in some embodiments, the extension may be connected to the end of the stirring section and the stirring vanes 113 are generally inverted L-shaped.
The stirring blade 113 is positioned in the second material cavity 121, and in the rotating process of the inner pipe 110, the stirring blade 113 and the inner pipe 110 rotate synchronously, so that the material in the second material cavity 121 is stirred; the stirring part extends along the direction parallel to the axial direction of the inner tube 110, the extending direction of the stirring part is perpendicular to the centrifugal force of the materials, and the stirring part can intercept the materials moving towards the direction far away from the inner tube 110 due to the centrifugal force, so that the system in the second material chamber 121 is more uniform.
In other embodiments of the present application, the stirring blade 113 may have other shapes, for example, a helical blade, a curved rod, or the like. Or, in some usage scenarios where the requirement on the uniformity of the material is not high, the reaction furnace 100 may not be provided with the stirring blade 113.
The outer tube 120 is sleeved outside the inner tube 110, the inner tube 110 extends into the outer tube 120 from one end of the outer tube 120, and a second material chamber 121 is defined between the inner tube 110 and the outer tube 120. The inner tube 110 is rotatably connected to the outer tube 120. in this embodiment, the inner tube 110 is connected to the outer tube 120 by a bearing, so that the inner tube 110 can rotate relative to the outer tube 120.
As mentioned above, in some embodiments of the present application, the outer tube 120 is further provided with an intake aperture in communication with the intake assembly; gas, such as reaction gas or protective gas, may be introduced into the second material chamber 121 through the gas inlet. It should be noted that for embodiments where gas introduction is not required, the outer tube 120 may not be provided with gas inlets.
In this embodiment, the outer tube 120 is a circular tube, the outer tube 120 and the inner tube 110 are coaxially disposed, the outer tube 120 is made of 310S stainless steel tube, and both ends of the outer tube 120 are fixed and sealed by flanges.
It should be noted that in other embodiments of the present application, the outer tube 120 may have other shapes, such as a prism shape, a bent tube shape, etc.; the material of the outer tube 120 may also be selected as desired.
In this embodiment, the first driving element 130 and the second driving element 140 are both motors, the first driving element 130 is in transmission connection with the inner tube 110 through a gear pair, and the second driving element 140 is in transmission connection with the outer tube 120 through a gear pair.
It should be noted that, in other embodiments of the present application, the first driving element 130 and the second driving element 140 may be connected to the inner tube 110 and the outer tube 120 respectively through other transmission connection manners, so that the first driving element 130 and the second driving element 140 can drive the inner tube 110 and the outer tube 120 to rotate respectively.
Referring to fig. 1 again, in the present embodiment, an outer casing 122 is further sleeved outside the outer tube 120, and the outer casing 122 is connected to the outer tube 120 through a rotating shaft sleeve 123, so that the outer casing 122 and the outer tube 120 can rotate relatively.
In other embodiments of the present application, the reaction furnace 100 may not be provided with the outer casing 122.
Fig. 2 shows a schematic structural diagram of a housing 122 provided in an embodiment of the present application, please refer to fig. 2, in this embodiment, the housing 122 is formed by two semicircular plates which are rotatably connected, the outer tube 120 is detachably connected to the housing 122, a buckle is disposed on the housing 122, and the semicircular plates are detachably connected through the buckle, so as to open the housing 122, and thus install the outer tube 120 into the housing 122.
Fig. 3 shows a schematic structural diagram of a heating assembly 150 provided in an embodiment of the present application, please refer to fig. 1 and 3, in which the heating assembly 150 mainly functions to heat the outer tube 120 and the inner tube 110, so as to heat the materials in the first material chamber 111 and the second material chamber 121.
In the present embodiment, the heating assembly 150 includes a heating element 151 and an insulating layer 152, the heating element 151 is connected to the outer casing 122, and the insulating layer 152 is disposed around the outer circumference of the outer casing 122. For example, the heating element 151 may be a heating wire or a silicon carbide rod.
The heat is transferred to second material chamber 121 through outer shell 122, outer tube 120, and then to first material chamber 111 through inner tube 110 by heating element 151. The insulating layer 152 can prevent a large amount of heat loss and increase heat utilization rate.
It should be noted that in other embodiments of the present application, the heating assembly 150 may be other mechanisms capable of supplying heat, for example, the heating assembly 150 may be a heat exchange sleeve, the outer tube 120 and the inner tube 110 are heated by the heat exchange sleeve, and the heating assembly 150 may be set according to the target heating temperature of the materials in the first material chamber 111 and the second material chamber 121.
In this embodiment, the reaction furnace 100 is provided with a support frame 160 for supporting the heating assembly 150, and the support frame 160 is connected to the heating assembly 150. It should be noted that, in some embodiments, the support frame 160 is not necessary, and the reaction furnace 100 may not be provided with the support frame 160.
In some embodiments of the present application, if the first material chamber 111 and the second material chamber 121 do not need to be heated, the reaction furnace 100 may not be provided with the heating assembly 150, in other words, the heating assembly 150 is not necessary in some embodiments.
In this embodiment, the reaction furnace 100 may further include a controller connected to the heating elements 151 of the heating assembly 150 to control the temperature of the materials in the first material chamber 111 and the second material chamber 121.
Further, a controller may be connected to the first driving member 130 and the second driving member 140, and the controller controls the output power of the first driving member 130 and the second driving member 140 to control the rotation speed of the inner tube 110 and the outer tube 120.
The reaction furnace 100 provided by the embodiment of the application has at least the following advantages:
the inner tube 110 is driven to rotate by the first driving member 130, the outer tube 120 is driven to rotate by the second driving member 140, so that the material in the first material cavity 111 can enter the second material cavity 121 through the discharge hole 112, and the material is reacted or mixed in the second material cavity 121; the reaction furnace 100 provided by the application can adjust the particle size and the mass of the material in the first material cavity 111 entering the second material cavity 121, and has the function of controlling the mixing or reaction rate; can be applied to the process which has the regulation and control requirement on the mixing process or the reaction process; in addition, a large amount of materials can be added into the first material cavity and the second material cavity, and the reaction furnace can be applied to large-scale production of materials.
The following description is made taking as an example the use of the reaction furnace 100 provided in the embodiment of the present application.
Referring to example 1, the process for preparing a material in the reaction furnace 100 of example 1 may include the following steps:
placing the first raw material in the first material cavity 111 and placing the second raw material in the second material cavity 121; the heating assembly 150 heats the first and second raw materials; rotating the inner tube 110 and the outer tube 120, and introducing protective gas into the first material cavity or the second material cavity; the first raw material enters the second raw material chamber 121 through the material holes 112 to react with the second raw material.
It should be noted that, in the present application, the step "placing the first raw material in the first material chamber 111" and the step "placing the second raw material in the second material chamber 121" do not have a sequence, and may be performed simultaneously or separately according to requirements.
In the preparation process, protective gas can be introduced into the first material cavity, and protective gas can also be introduced into the second material cavity.
Two examples are made below for the material prepared by the reactor 100.
Example 2
Embodiment 2 provides a process for preparing a material in the reaction furnace 100 shown in embodiment 1, which mainly comprises the following steps:
step S1: placing clay minerals and salts in the second material cavity 121; wherein the salt can be NaCl, LiCl, KCl, CaCl2、ZnCl2、MgCl2At least one of; for example, the salt may be NaCl; the clay mineral is montmorillonite. In other embodiments of the present application, the clay mineral is not limited to montmorillonite, and may be kaolinite, illite, or the like.
Illustratively, the mass ratio of montmorillonite to NaCl is 1: (0.1 to 5), for example, 1:0.1, 1:0.5, 1:2, 1:2.5, 1:3, 1:4, 1:5 and the like can be given.
Step S2: placing the second raw material in the first material chamber 111; the second raw material includes at least one of magnesium, aluminum, sodium, potassium, calcium, and zinc, for example, the second raw material is metallic magnesium.
Illustratively, the mass ratio of magnesium to montmorillonite is (0.4-3): 1, for example, can be 0.4:1, 0.5:1, 0.6:1, 0.9:1, 1.2:1, 1.5:1, 2:1, 2.4:1, 3:1, and the like.
It should be noted that step S1 and step S2 do not have a sequential order.
The heating element 150 heats the outer tube 120 at a temperature of 550-.
Introducing protective gas into the first material cavity 111, or introducing protective gas into the second material cavity 121; as an example, the shielding gas may be N2Ar, He, etc. Illustratively, the inlet speed of the shielding gas may be 1-10L/min, such as 1L/min, 2L/min, 3L/min, 4L/min, 5L/min, 6L/min, 7L/min, 8L/min, 9L/min, 10L/min, and so on.
Driving the inner tube 110 and the outer tube 120 to rotate; illustratively, the rotation speed of the inner tube 110 can be 160-240r/min, such as 160r/min, 170r/min, 180r/min, 190r/min, 200r/min, 210r/min, 220r/min, 230r/min, 240r/min, etc.; the outer tube 120 may rotate at a speed of 30-80r/min, such as 30r/min, 40r/min, 50r/min, 60r/min, 70r/min, 80r/min, and so forth.
The reaction time of the material in the reaction furnace 100 may be 4 to 10 hours, for example, 4 hours, 5 hours, 6 hours, 7 hours, 8 hours, or 9 hours, etc.
In some embodiments, after the reaction in the reaction furnace 100 is completed, the solid phase is leached with HF after washing the reaction product with an acid, and then dried. For example, washing with HCl may be employed.
For example, in this embodiment, the preparation process is as follows:
500g of montmorillonite and 2500g of NaCl are placed in a second material cavity 121, 300g of magnesium metal is uniformly mixed and then placed in a first material cavity 111, argon is introduced into the first material cavity 111, and the airflow speed is 6L/min; heating unit 150 heats the interior of first material chamber 111 to 650 ℃. The rotating speed of the inner pipe 110 is 200r/min, and the rotating speed of the outer pipe 120 is 60 r/min; the reaction was carried out for 5 hours and then allowed to cool naturally.
And taking out a product after reaction, respectively cleaning the product with distilled water and 1mol/L HCl, then leaching the product with 1 wt% HF, washing the product with ultrapure water to be neutral, and drying the product in vacuum at the temperature of 60 ℃ to obtain the nano silicon material. The nano silicon material is in a porous structure, and the contained nano silicon has high purity and larger specific surface area.
The preparation method based on the reaction furnace 100 provided by the embodiment has at least the following advantages:
in the reaction process, the magnesium metal in the first material cavity 111 can slowly and uniformly enter the second material cavity 121 to react with montmorillonite and NaCl; the controllability of the whole reaction process is better, and the speed of the reaction can be controlled according to the aperture size of the discharge hole 112, the rotating speed of the inner tube 110 and the rotating speed of the outer tube 120.
The metal magnesium gradually enters the second material cavity 121 from the discharge hole 112 in a liquid or gaseous state and then reacts with montmorillonite in a contact manner, so that excessive heat generated by the reaction of a large amount of magnesium powder and montmorillonite is effectively avoided, and the generated nano silicon is prevented from melting or generating a mixed phase; further, the stirring of the stirring blade 113 in the second material chamber 121 can prevent the accumulation of heat in the reaction system, and simultaneously make the contact of reactants more uniform; the reaction process can be regulated and controlled by controlling the conditions of air flow, rotating speed, opening size of the inner pipe wall and the like.
Example 3
Embodiment 3 provides a process for preparing a material in the reaction furnace 100 shown in embodiment 1, which mainly comprises the following steps:
step S1: placing clay minerals in the second material cavity 121;
step S2: placing a soil additive in the first material chamber 111;
illustratively, the clay mineral is palygorskite and the soil additive is monopotassium phosphate; for example, the mass ratio of palygorskite to monopotassium phosphate is (15-28: 5), and may be, for example, 15:5, 18:5, 20:5, 22:5, 23:5, 25:5, 28:5, and the like.
Step S1 is not in sequence with step S2.
Driving the inner tube 110 and the outer tube 120 to rotate; illustratively, the rotational speed of the inner tube 110 may be 60-140r/min, such as 60r/min, 70r/min, 80r/min, 90r/min, 100r/min, 110r/min, 120r/min, 130r/min, 140r/min, and so forth; the outer tube 120 may rotate at a speed of 20-50r/min, for example, 20r/min, 22r/min, 26r/min, 30r/min, 35r/min, 40r/min, 50r/min, and so on.
The heating assembly 150 heats the outer tube 120 to make the temperature in the second material chamber 121 be 250-320 ℃, for example, 250 ℃, 260 ℃, 270 ℃, 280 ℃, 290 ℃, 300 ℃, 320 ℃ and so on.
The reaction time in the reaction furnace 100 may be 1 to 4 hours, for example, 1 hour, 2 hours, 3 hours, 4 hours, or the like.
For example, in this embodiment, the preparation process is as follows:
2200g of palygorskite are placed in a second material cavity 121, 500g of potassium dihydrogen phosphate is placed in a first material cavity 111, the rotating speed of an inner pipe 110 is 100r/min, and the rotating speed of an outer pipe 120 is 30 r/min.
Heating assembly 150 heats the interior of first material chamber 111 to 280 ℃. And naturally cooling after reacting for 2h to obtain the palygorskite-loaded polyphosphate soil conditioner. The soil conditioner has a rod-like shape, and phosphorus is uniformly loaded on the surface of the palygorskite.
The preparation method based on the reaction furnace 100 provided by the embodiment has at least the following advantages:
in the reaction process, the monopotassium phosphate in the first material cavity 111 can slowly and uniformly enter the second material cavity 121 to react with the palygorskite; the effects of slow release and slow reaction are achieved, and the polyphosphate in the obtained soil conditioner can be uniformly distributed on the surface of the palygorskite.
In detail, in the reaction furnace 100, the monopotassium phosphate in the inner tube 110 is firstly melted, then gradually released to be mixed with the palygorskite for reaction and combination, and under the stirring action, the palygorskite-based soil conditioner uniformly loaded with polyphosphate is finally generated, so that the problem of nonuniform loading caused by nonuniform and uncontrollable traditional high-temperature solid-phase reaction is solved; in addition, the existing two-step reaction of mixing and reheating firstly is improved into one-step preparation by adopting the reaction furnace 100, so that the reaction process is simplified.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (10)

1. A reaction furnace, comprising:
the inner tube is provided with a first material cavity, and a discharge hole which penetrates through the inner tube and is communicated with the first material cavity is formed in the inner tube;
the first driving piece is connected with the inner pipe and is used for driving the inner pipe to rotate;
the outer pipe is sleeved outside the inner pipe and is rotationally connected with the inner pipe, and a second material cavity is formed between the inner pipe and the outer pipe; and
and the second driving piece is connected with the outer pipe and is used for driving the outer pipe to rotate.
2. The reactor furnace of claim 1, wherein the inner tube is provided with stirring blades on a side thereof adjacent to the outer tube.
3. The reactor according to claim 2, wherein the stirring blade includes an extension part connected to the inner tube, the extension part extending in a direction perpendicular to an axial direction of the inner tube, and a stirring part connected to a free end of the extension part, the stirring part extending in a direction parallel to the axial direction of the inner tube.
4. The reactor according to any one of claims 1 to 3, further comprising a heating element, wherein the heating element is sleeved outside the outer tube, and the heating element is rotatably connected to the outer tube.
5. A material production process based on the reaction furnace of claim 4, characterized by comprising:
placing a first raw material in the first material cavity, and placing a second raw material in the second material cavity;
the heating assembly heats the first feedstock and the second feedstock;
rotating the inner pipe and the outer pipe, and introducing protective gas into the first material cavity or the second material cavity;
the first raw material enters the second raw material cavity through the material hole to react with the second raw material.
6. The material production process according to claim 5,
the first raw material comprises clay mineral and salt, the second raw material comprises at least one of magnesium, aluminum, sodium, potassium, calcium and zinc, and the salt comprises NaCl, LiCl, KCl, CaCl2、ZnCl2、MgCl2At leastOne kind of the medicine.
7. The material production process according to claim 6,
the clay mineral is montmorillonite, and the salt is NaCl; the second raw material is magnesium; the heating assembly heats the first raw material and the second raw material to 600-700 ℃.
8. The material production process according to claim 6,
and the flow speed of the protective gas introduced into the first material cavity or the second material cavity is 1-10L/min.
9. The material production process according to claim 6, wherein after the first raw material enters the second raw material chamber through the material hole and reacts with the second raw material, the process further comprises:
washing the reaction product with acid, leaching the solid phase with HF, and drying.
10. The material production process according to claim 5,
the first raw material is clay mineral; the second raw material is a soil additive;
optionally, the first raw material is palygorskite; the second raw material is potassium dihydrogen phosphate;
optionally, the rotating speed of the inner pipe is 60-140r/min, and the rotating speed of the outer pipe is 20-50 r/min.
CN202110950826.4A 2021-08-18 2021-08-18 Reaction furnace and material production process Active CN113617295B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110950826.4A CN113617295B (en) 2021-08-18 2021-08-18 Reaction furnace and material production process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110950826.4A CN113617295B (en) 2021-08-18 2021-08-18 Reaction furnace and material production process

Publications (2)

Publication Number Publication Date
CN113617295A true CN113617295A (en) 2021-11-09
CN113617295B CN113617295B (en) 2022-08-09

Family

ID=78386473

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110950826.4A Active CN113617295B (en) 2021-08-18 2021-08-18 Reaction furnace and material production process

Country Status (1)

Country Link
CN (1) CN113617295B (en)

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001085333A2 (en) * 2000-05-05 2001-11-15 Saudi Basic Industries Corporation An apparatus for the controlled optimized addition of reactants in continuous flow reaction systems and methods of using the same
US20120258857A1 (en) * 2011-04-11 2012-10-11 Saudi Arabian Oil Company Auto thermal reforming (atr) catalytic structures
WO2014042410A1 (en) * 2012-09-11 2014-03-20 주식회사 아이제이피에스 Jacket and reactor using same
CN107720816A (en) * 2017-11-14 2018-02-23 黄林海 A kind of high-temperature tubular reactor for being used to produce rutile titanium dioxide
CN207493679U (en) * 2017-08-29 2018-06-15 广元瑞峰新材料有限公司 A kind of reaction kettle
CN108246221A (en) * 2018-03-29 2018-07-06 睦化(上海)流体工程有限公司 Micropore is vortexed casing mixing reactor and its application
CN110305664A (en) * 2019-01-14 2019-10-08 深圳屹米达环保科技有限公司 Soil conditioner and preparation method thereof and application method
CN210826998U (en) * 2019-09-29 2020-06-23 成都市路桥工程股份有限公司 Asphalt aggregate drying device for road and bridge
US20200276555A1 (en) * 2016-12-16 2020-09-03 Commissariat A L'energie Atomique Et Aux Energies Alternatives Reactor for the hydrothermal oxidation treatment of an organic material in a reaction medium
CN112107881A (en) * 2020-09-29 2020-12-22 内蒙古麦维生物科技有限公司 Device for saponifying and extracting ergosterol

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001085333A2 (en) * 2000-05-05 2001-11-15 Saudi Basic Industries Corporation An apparatus for the controlled optimized addition of reactants in continuous flow reaction systems and methods of using the same
US20120258857A1 (en) * 2011-04-11 2012-10-11 Saudi Arabian Oil Company Auto thermal reforming (atr) catalytic structures
WO2014042410A1 (en) * 2012-09-11 2014-03-20 주식회사 아이제이피에스 Jacket and reactor using same
US20200276555A1 (en) * 2016-12-16 2020-09-03 Commissariat A L'energie Atomique Et Aux Energies Alternatives Reactor for the hydrothermal oxidation treatment of an organic material in a reaction medium
CN207493679U (en) * 2017-08-29 2018-06-15 广元瑞峰新材料有限公司 A kind of reaction kettle
CN107720816A (en) * 2017-11-14 2018-02-23 黄林海 A kind of high-temperature tubular reactor for being used to produce rutile titanium dioxide
CN108246221A (en) * 2018-03-29 2018-07-06 睦化(上海)流体工程有限公司 Micropore is vortexed casing mixing reactor and its application
CN110305664A (en) * 2019-01-14 2019-10-08 深圳屹米达环保科技有限公司 Soil conditioner and preparation method thereof and application method
CN210826998U (en) * 2019-09-29 2020-06-23 成都市路桥工程股份有限公司 Asphalt aggregate drying device for road and bridge
CN112107881A (en) * 2020-09-29 2020-12-22 内蒙古麦维生物科技有限公司 Device for saponifying and extracting ergosterol

Also Published As

Publication number Publication date
CN113617295B (en) 2022-08-09

Similar Documents

Publication Publication Date Title
CN106495161B (en) A method of nano-silicon is prepared based on metal intervention metallothermic reduction
JP5113081B2 (en) Lithium manganese phosphate cathode material for lithium secondary battery
JP6579237B2 (en) Method for producing positive electrode active material for lithium secondary battery
KR20000028989A (en) Niobium Powder and a Process for the Production of Niobium and/or Tantalum Powders
CN113617295B (en) Reaction furnace and material production process
JP6182673B2 (en) Method for producing lithium iron phosphate
CN105280920B (en) The devices, systems, and methods made for lithium cell cathode material
CN101794881A (en) Method for preparing anode material of lithium ion batteries by one-step microwave sintering
CN101293671A (en) Process for preparing bismuth oxide, and the apparatus therefor
JP5176222B2 (en) Vertical firing furnace and firing method using the same
TW202222679A (en) Improved synthesis of olivine lithium metal phosphate cathode materials
CN106981653B (en) Preparation method of nano spinel type nickel-doped lithium manganate material
EP2565158B1 (en) Method for manufacturing a lithium transition metal phosphate
CN104178809A (en) Method for preparing low metal boron master alloy by use of metallurgy method
CN205294851U (en) Graphite purification furnace
JP3446390B2 (en) Method for producing lithium cobaltate
CN110433744B (en) Fluorescent powder preparation device and preparation method
US20220209222A1 (en) Method and System for High-Yield Dynamic Crystallization Manufacturing of Battery Materials
CN219385399U (en) Graphite resistance furnace
CN216924921U (en) Lithium hydroxide monohydrate drying device
CN211921303U (en) Continuous smelting furnace body suitable for thermal state doping of quartz powder and multiple rare earth elements
CN106745332A (en) Combustion method quickly prepares nanometer spinel type nickel ion doped material
CN208087234U (en) A kind of ammonium paratungstate calciner
JP7491659B2 (en) Lithium hydroxide hydrate, method for producing lithium hydroxide hydrate, and method for producing lithium nickel composite oxide
JP2021183550A (en) Lithium disilicate-containing lithium-containing silicon oxide and method for producing the same

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant