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CN113617295B - Reaction furnace and material production process - Google Patents

Reaction furnace and material production process Download PDF

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Publication number
CN113617295B
CN113617295B CN202110950826.4A CN202110950826A CN113617295B CN 113617295 B CN113617295 B CN 113617295B CN 202110950826 A CN202110950826 A CN 202110950826A CN 113617295 B CN113617295 B CN 113617295B
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raw material
inner pipe
cavity
material cavity
pipe
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CN113617295A (en
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朱润良
陈情泽
谢捷洋
何宏平
朱建喜
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Guangzhou Institute of Geochemistry of CAS
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Guangzhou Institute of Geochemistry of CAS
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    • 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

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  • 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)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Muffle Furnaces And Rotary Kilns (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

一种反应炉和物料生产工艺A kind of reaction furnace and material production process

技术领域technical field

本申请涉及设备制造领域,具体而言,涉及一种反应炉和物料生产工艺。The present application relates to the field of equipment manufacturing, and in particular, to a reaction furnace and a material production process.

背景技术Background technique

高温固相反应法是先使反应物混合均匀,生成一种前体物或非晶态产物,然后高温(200~1000℃)焙烧,使反应进行完全并使产物晶化的工艺方法,该方法常用于纳米材料等的制备。例如,硅纳米材料因具有优良的理化性能而被广泛应用于锂离子电池、太阳能电池、金属陶瓷烧结、复合材料、耐火材料等领域;金属热还原法制备硅纳米材料,常在高温气氛炉中进行。例如,土壤调理剂(加入土壤中以改善土壤物理、化学或生物性状的物料)可用于重金属钝化、酸碱度调节、保水性和透气性改善等;其制备过程中,常通过焙烧以活化其组分,或是稍加热使组分结合更牢固。对上述固相反应来说,参加反应各组分的原子和离子受到晶体内聚力的限制,不能像在液相或气相反应中那样自由地迁移运动,粉体细度和均匀程度对固相反应的进行极为重要。高温下固相反应进程往往难以控制,因此会对反应产物造成不良影响。The high-temperature solid-phase reaction method is to mix the reactants evenly to generate a precursor or amorphous product, and then calcinate at a high temperature (200-1000 ° C) to complete the reaction and crystallize the product. Commonly used in the preparation of nanomaterials. For example, silicon nanomaterials are widely used in lithium-ion batteries, solar cells, cermet sintering, composite materials, refractory materials and other fields due to their excellent physical and chemical properties. conduct. For example, soil conditioners (materials added to soil to improve soil physical, chemical or biological properties) can be used for heavy metal passivation, pH adjustment, water retention and air permeability improvement, etc.; Divide, or slightly heat to make the components bind more firmly. For the above solid-phase reactions, the atoms and ions participating in the reaction components are limited by crystal cohesion and cannot move freely as in liquid or gas-phase reactions. It is extremely important to proceed. The progress of solid-phase reactions at high temperatures is often difficult to control and thus adversely affects the reaction products.

发明内容SUMMARY OF THE INVENTION

本申请实施例的目的在于提供一种反应炉和物料生产工艺,其旨在改善高温固相反应的反应过程不易控制的问题。The purpose of the embodiments of the present application is to provide a reaction furnace and a material production process, which aims to improve the problem that the reaction process of the high-temperature solid-phase reaction is not easy to control.

本申请第一方面提供一种反应炉,所述反应炉包括:A first aspect of the present application provides a reaction furnace, the reaction furnace comprising:

内管,所述内管具有第一物料腔,所述内管开设有贯穿所述内管并与所述第一物料腔连通的出料孔;an inner tube, the inner tube has a first material cavity, and the inner tube is provided with a discharge hole that penetrates the inner tube and communicates with the first material cavity;

第一驱动件,所述第一驱动件与所述内管连接并用于驱动所述内管转动;a first driving member, the first driving member is connected with the inner tube and used to drive the inner tube to rotate;

外管,所述外管套设于所述内管外且与所述内管转动连接,所述内管与所述外管之间形成第二物料腔;以及an outer tube, the outer tube is sleeved outside the inner tube and is rotatably connected with the inner tube, and a second material cavity is formed between the inner tube and the outer tube; and

第二驱动件,所述第二驱动件与所述外管连接并用于驱动所述外管转动。A second driving member, the second driving member is connected with the outer tube and used to drive the outer tube to rotate.

通过第一驱动件驱动内管转动,第二驱动件驱动外管转动,使第一物料腔内的物料可以通过出料孔进入第二物料腔,使物料在第二物料腔内反应或者混合;本申请提供的反应炉可以调节第一物料腔内的物料进入第二物料腔内的粒径以及质量,具有控制混合或者反应速率的作用;可以应用于对混合过程或者反应过程有调控需要的工艺;此外,第一、第二物料腔内可大量加入物料,反应炉可以应用于材料的规模化生产。The inner tube is driven to rotate by the first driving member, and the outer tube is driven by the second driving member to rotate, so that the material in the first material cavity can enter the second material cavity through the discharge hole, so that the material can react or mix in the second material cavity; The reaction furnace provided by the application can adjust the particle size and quality of the materials in the first material cavity entering the second material cavity, and has the effect of controlling the mixing or reaction rate; it can be applied to processes that need to regulate the mixing process or the reaction process. ; In addition, a large amount of materials can be added to the first and second material chambers, and the reaction furnace can be applied to large-scale production of materials.

在本申请第一方面的一些实施例中,内管靠近所述外管的一侧设置搅拌叶片。In some embodiments of the first aspect of the present application, a stirring blade is provided on a side of the inner tube close to the outer tube.

在本申请第一方面的一些实施例中,搅拌叶片包括延伸部和搅拌部,所述延伸部与所述内管连接,所述延伸部沿与所述内管轴线方向垂直的方向延伸,所述搅拌部与所述延伸部的自由端连接,所述搅拌部沿与所述内管轴线方向平行的方向延伸。In some embodiments of the first aspect of the present application, the stirring blade includes an extension part and a stirring part, the extension part is connected with the inner pipe, the extension part extends in a direction perpendicular to the axial direction of the inner pipe, so The stirring part is connected to the free end of the extending part, and the stirring part extends in a direction parallel to the axial direction of the inner tube.

在本申请第一方面的一些实施例中,反应炉还包括加热组件,所述加热组件套设于所述外管外,所述加热组件与所述外管转动连接。In some embodiments of the first aspect of the present application, the reaction furnace further includes a heating component, the heating component is sleeved outside the outer tube, and the heating component is rotatably connected to the outer tube.

在申请第二方面提供一种基于上述反应炉的物料生产工艺,包括:A second aspect of the application provides a material production process based on the above-mentioned reaction furnace, comprising:

将第一原料置于所述第一物料腔,将第二原料置于所述第二物料腔;placing the first raw material in the first material cavity, and placing the second raw material in the second material cavity;

所述加热组件加热所述第一原料和所述第二原料;the heating assembly heats the first raw material and the second raw material;

转动所述内管和所述外管,向所述第一物料腔或者所述第二物料腔通入保护气体;Rotate the inner tube and the outer tube, and pass protective gas into the first material cavity or the second material cavity;

所述第一原料通过所述物料孔进入所述第二物料腔与所述第二原料反应。The first raw material enters the second material cavity through the material hole to react with the second raw material.

在本申请第二方面的一些实施例中,所述第一原料包括黏土矿物和盐,所述第二原料包括镁、铝、钠、钾、钙和锌中的至少一种,所述盐包括NaCl、LiCl、KCl、CaCl2、ZnCl2、MgCl2中的至少一种。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, aluminium, sodium, potassium, calcium and zinc, and the salt comprises At least one of NaCl, LiCl, KCl, CaCl 2 , ZnCl 2 , and MgCl 2 .

在本申请第二方面的一些实施例中,所述黏土矿物为蒙脱石,所述盐为NaCl;所述第二原料为镁;所述加热组件加热所述第一原料和所述第二原料至600-700℃。In some embodiments of the second aspect of the present application, the clay mineral is montmorillonite, the salt is NaCl; the second raw material is magnesium; the heating component heats the first raw material and the second raw material Raw material to 600-700°C.

第一物料腔的金属镁可以比较缓慢且均匀地进入第二物料腔内与蒙脱石、NaCl反应;整个反应过程可控性较佳,可以根据出料孔的孔径大小和内管转速、外管转速控制反应进行的快慢。金属镁缓慢进入第二物料腔内可以避免因为局部反应热量较高而影响最终产物的形貌。The magnesium metal in the first material cavity can enter the second material cavity relatively slowly and evenly to react with montmorillonite and NaCl; the whole reaction process is better controllable, and can be adjusted according to the diameter of the discharge hole and the rotation speed of the inner tube, the outer Tube speed controls how fast the reaction proceeds. The slow entry of metal magnesium into the second material cavity can avoid affecting the morphology of the final product due to the high local reaction heat.

在本申请第二方面的一些实施例中,向所述第一物料腔或所述第二物料腔通入的保护气体的流速为1~10L/min。In some embodiments of the second aspect of the present application, the flow rate of the protective gas introduced into the first material chamber or the second material chamber is 1-10 L/min.

在本申请第二方面的一些实施例中,第一原料通过所述物料孔进入所述第二物料腔与所述第二原料反应完成后,还包括:In some embodiments of the second aspect of the present application, after the first raw material enters the second material cavity through the material hole and the reaction with the second raw material is completed, the method further includes:

采用酸洗涤反应产物后将固相采用HF浸出,然后干燥。After washing the reaction product with acid, the solid phase was leached with HF and then dried.

在本申请第二方面的一些实施例中,所述第一原料为黏土矿物;所述第二原料为土壤添加剂;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;

可选地,所述第一原料为坡缕石;所述第二原料为磷酸二氢钾;Optionally, the first raw material is palygorskite; the second raw material is potassium dihydrogen phosphate;

可选地,所述内管的转速为60-140r/min,所述外管的转速为20-50r/min。Optionally, the rotational speed of the inner tube is 60-140 r/min, and the rotational speed of the outer tube is 20-50 r/min.

在反应过程中,第一物料腔的磷酸二氢钾可以比较缓慢且均匀地进入第二物料腔内与坡缕石反应;达到缓慢释放且缓慢反应的效果,得到的土壤调理剂中聚磷酸盐可以比较均匀地分布于坡缕石表面。During the reaction process, potassium dihydrogen phosphate in the first material cavity can relatively slowly and uniformly enter the second material cavity to react with palygorskite; to achieve the effect of slow release and slow reaction, the polyphosphate in the obtained soil conditioner It can be distributed evenly on the palygorskite surface.

附图说明Description of drawings

为了更清楚地说明本申请实施例的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,应当理解,以下附图仅示出了本申请的某些实施例,因此不应被看作是对范围的限定,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他相关的附图。In order to illustrate the technical solutions of the embodiments of the present application more clearly, the following drawings will briefly introduce the drawings that need to be used in the embodiments. It should be understood that the following drawings only show some embodiments of the present application, and therefore do not It should be regarded as a limitation of the scope, and for those of ordinary skill in the art, other related drawings can also be obtained according to these drawings without any creative effort.

图1示出了本申请实施例提供的反应炉的内部结构示意图;FIG. 1 shows a schematic diagram of the internal structure of the reaction furnace provided in the embodiment of the present application;

图2示出了本申请实施例提供的外壳的结构示意图;FIG. 2 shows a schematic structural diagram of a housing provided by an embodiment of the present application;

图3示出了本申请实施例提供的加热组件的结构示意图。FIG. 3 shows a schematic structural diagram of a heating assembly provided by an embodiment of the present application.

图标:100-反应炉;110-内管;111-第一物料腔;112-出料孔;113-搅拌叶;120-外管;121-第二物料腔;122-外壳;123-转动轴套;130-第一驱动件;140-第二驱动件;150-加热组件;151-加热元件;152-保温层;160-支撑架。Icon: 100-reaction furnace; 110-inner pipe; 111-first material chamber; 112-discharge hole; 113-stirring blade; 120-outer pipe; 121-second material chamber; 122-shell; 123-rotating shaft Cover; 130-first driving part; 140-second driving part; 150-heating assembly; 151-heating element; 152-thermal insulation layer; 160-support frame.

具体实施方式Detailed ways

为使本申请实施例的目的、技术方案和优点更加清楚,下面将结合本申请实施例中的附图,对本申请实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本申请一部分实施例,而不是全部的实施例。通常在此处附图中描述和示出的本申请实施例的组件可以以各种不同的配置来布置和设计。In order to make the purposes, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be described clearly and completely below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments It is a part of the embodiments of the present application, but not all of the embodiments. The components of the embodiments of the present application generally described and illustrated in the drawings herein may be arranged and designed in a variety of different configurations.

因此,以下对在附图中提供的本申请的实施例的详细描述并非旨在限制要求保护的本申请的范围,而是仅仅表示本申请的选定实施例。基于本申请中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本申请保护的范围。Thus, the following detailed description of the embodiments of the application provided in the accompanying drawings is not intended to limit the scope of the application as claimed, but is merely representative of selected embodiments of the application. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the protection scope of the present application.

应注意到:相似的标号和字母在下面的附图中表示类似项,因此,一旦某一项在一个附图中被定义,则在随后的附图中不需要对其进行进一步定义和解释。It should be noted that like numerals and letters refer to like items in the following figures, so once an item is defined in one figure, it does not require further definition and explanation in subsequent figures.

在本申请实施例的描述中,需要理解的是,术语“中心”“内”、“外”等指示的方位或位置关系为基于附图所示的方位或位置关系,或者是该申请产品使用时惯常摆放的方位或位置关系,或者是本领域技术人员惯常理解的方位或位置关系,仅是为了便于描述本申请和简化描述,而不是指示或暗示所指的设备或元件必须具有特定的方位、以特定的方位构造和操作,因此不能理解为对本申请的限制。In the description of the embodiments of the present application, it should be understood that the orientation or positional relationship indicated by the terms "center", "inside", "outside", etc. is based on the orientation or positional relationship shown in the accompanying drawings, or is based on the use of the product of the application The orientation or positional relationship that is usually placed at times, or the orientation or positional relationship that is commonly understood by those skilled in the art, is only for the convenience of describing the present application and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific Orientation, construction and operation in a particular orientation, and therefore should not be construed as a limitation of the present application.

此外,术语“第一”、“第二”等仅用于区分描述,而不能理解为指示或暗示相对重要性。Furthermore, the terms "first", "second", etc. are only used to differentiate the description and should not be construed to indicate or imply relative importance.

在本申请实施例的描述中,还需要说明的是,除非另有明确的规定和限定,术语“设置”、“安装”、“连接”应做广义理解,例如,可以是固定连接,也可以是可拆卸连接,或一体地连接;可以是机械连接,也可以是电连接;可以是直接相连,也可以通过中间媒介间接相连,可以是两个元件内部的连通。对于本领域的普通技术人员而言,可以具体情况理解上述术语在本申请中的具体含义。In the description of the embodiments of the present application, it should also be noted that, unless otherwise expressly specified and limited, the terms "arrangement", "installation" and "connection" should be understood in a broad sense, for example, it may be a fixed connection, or a It is a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected, or indirectly connected through an intermediate medium, or it can be the internal communication between two components. For those of ordinary skill in the art, the specific meanings of the above terms in this application can be understood in specific situations.

实施例1Example 1

图1示出了本申请实施例提供的反应炉100的内部结构示意图,请参阅图1,本实施例提供一种反应炉100,本申请提供的反应炉100适用于高温固相反应,需要说明的是,在本申请并不对反应炉100的用途进行限定,例如,其可以用于液固反应,或者,反应炉100也可以用于物料的混合以及物料的搅拌等。FIG. 1 shows a schematic diagram of the internal structure of a reaction furnace 100 provided by an embodiment of the present application. Please refer to FIG. 1 . This embodiment provides a reaction furnace 100. The reaction furnace 100 provided by the present application is suitable for high-temperature solid-phase reaction. It needs to be explained However, the application does not limit the application of the reaction furnace 100, for example, it can be used for liquid-solid reaction, or the reaction furnace 100 can also be used for material mixing and material stirring.

反应炉100包括内管110、外管120、第一驱动件130、第二驱动件140以及加热组件150。第一驱动件130与内管110连接,用于驱动内管110转动,第二驱动件140与外管120连接,用于驱动外管120转动。外管120套设于内管110外,外管120与内管110之间形成第二物料腔121。加热组件150用于为内管110、外管120加热。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 cavity 121 is formed between the outer tube 120 and the inner tube 110 . The heating assembly 150 is used for heating the inner tube 110 and the outer tube 120 .

内管110内有第一物料腔111,内管110设置有出口和用于开闭所述开口的盖体,通过出口可向第一物料腔111内装填物料。Inside the inner tube 110 is a first material cavity 111 , the inner tube 110 is provided with an outlet and a cover for opening and closing the opening, and the first material cavity 111 can be filled with materials through the outlet.

在本实施例中,内管110为圆柱形,内管110的出口设置于内管110的一端,第一驱动件130与内管110的一端连接,第一驱动件130可驱动内管110转动。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 .

内管110上间隔分布多个出料孔112,出料孔112贯穿内管110并与第一物料腔111连通,可以使第一物料腔111内的物料经过出料孔112排出。A plurality of discharge holes 112 are distributed on the inner pipe 110 at intervals. The discharge holes 112 penetrate through the inner pipe 110 and communicate with the first material cavity 111 , so that the material in the first material cavity 111 can be discharged through the discharge holes 112 .

在本实施例中,出料孔112的直径为1~5mm,例如可以为1mm、2mm、3mm、4mm或者5mm等等。出料孔112沿内管110长度方向分布的同时还沿内管110的周向分布。In this embodiment, the diameter of the discharge hole 112 is 1-5 mm, for example, it may be 1 mm, 2 mm, 3 mm, 4 mm, or 5 mm, and so on. The discharge holes 112 are distributed along the length direction of the inner pipe 110 and also distributed along the circumferential direction of the inner pipe 110 .

需要说明的是,在本申请的其他实施例中,内管110可以为其他形状,例如可以为棱柱形或者弯管形等;相应地,本申请也不对第一物料腔111的形状进行限定。It should be noted that, in other embodiments of the present application, the inner tube 110 may be in other shapes, such as a prismatic shape or a curved tube shape; accordingly, the present application does not limit the shape of the first material cavity 111 .

此外,出料孔112的直径可以根据第一物料腔111内的粒径或者在反应过程中反应的快慢等设置,不仅限于上述的1~5mm,例如可以为0.5mm、6mm、7mm、10mm等等;出料孔112的数量以及相邻两个出料孔112之间的距离也可以根据具体需求进行设置,本申请不对其进行限定。In addition, the diameter of the discharge hole 112 can be set according to the particle size in the first material cavity 111 or the speed of the reaction in the reaction process, and is not limited to the above-mentioned 1-5 mm, for example, it can be 0.5 mm, 6 mm, 7 mm, 10 mm, etc. etc.; the number of discharge holes 112 and the distance between two adjacent discharge holes 112 can also be set according to specific requirements, which are not limited in this application.

在本申请的一些实施例中,内管110还设置有用于与进气组件连通的进气孔;可以通过进气孔向内管110通入气体,例如通入反应气体或者保护气体。需要说明的是,对于不需要通入气体的实施例而言,内管110可以不设置进气孔。In some embodiments of the present application, the inner pipe 110 is further provided with an air inlet for communicating with the air inlet assembly; gas, such as reacting gas or protective gas, can be introduced into the inner pipe 110 through the air inlet. It should be noted that, for the embodiment that does not need to pass gas, the inner pipe 110 may not be provided with an air inlet hole.

在本实施例中,内管110的外表还设置有搅拌叶113;搅拌叶113位于内管110远离第一物料腔111的外表面。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 away from the first material cavity 111 .

在本实施例中,搅拌叶113包括延伸部和搅拌部,延伸部与内管110连接,延伸部沿与内管110轴线方向垂直的方向延伸,搅拌部沿与内管110轴线方向平行的方向延伸。搅拌部与延伸部的自由端连接。延伸部与搅拌部相互垂直。例如,在一些实施例中,延伸部与搅拌部的中部连接,搅拌叶113大致为T形,可以理解的是,一些实施例中,延伸部可以与搅拌部的端部连接,搅拌叶113大致为倒L形。In this embodiment, the stirring blade 113 includes an extension part and a stirring part, the extension part is connected to the inner pipe 110 , the extension part extends in a direction perpendicular to the axial direction of the inner pipe 110 , and the stirring part is in a direction parallel to the axial direction of the inner pipe 110 extend. The stirring part is connected to the free end of the extension part. The extension part and the stirring part are perpendicular to each other. For example, in some embodiments, the extension part is connected to the middle of the stirring part, and the stirring blade 113 is approximately T-shaped. It is understood that, in some embodiments, the extending part may be connected to the end of the stirring part, and the stirring blade 113 is approximately T-shaped. Inverted L shape.

搅拌叶113位于第二物料腔121内,内管110转动的过程中,搅拌叶113与内管110同步转动,从而搅动第二物料腔121内的物料;搅拌部沿与内管110轴线方向平行的方向延伸,搅拌部的延伸方向与物料的离心力垂直,搅拌部可以拦截因离心力而朝远离内管110方向运动的物料,使第二物料腔121内的体系更均匀。The stirring blade 113 is located in the second material cavity 121. During the rotation of the inner pipe 110, the stirring blade 113 rotates synchronously with the inner pipe 110, thereby stirring the material in the second material cavity 121; the stirring part is parallel to the axis direction of the inner pipe 110. The extension direction of the stirring part is perpendicular to the centrifugal force of the material, and the stirring part can intercept the material moving away from the inner tube 110 due to the centrifugal force, so that the system in the second material cavity 121 is more uniform.

需要说明的是,在本申请的其他实施例中,搅拌叶113可以为其他形状,例如可以为螺旋的叶片或者弯曲形的杆状等。或者,在一些对物料的均匀性要求不高的使用场景,反应炉100可以不设置搅拌叶113。It should be noted that, in other embodiments of the present application, the stirring blade 113 may be in other shapes, for example, may be a spiral blade or a curved rod shape or the like. Alternatively, in some usage scenarios that do not require high material uniformity, the reaction furnace 100 may not be provided with the stirring blade 113 .

外管120套设于内管110外,内管110从外管120的一端伸入外管120内,内管110与外管120之间围成第二物料腔121。内管110与外管120转动连接,在本实施例中,内管110与外管120通过轴承连接,使内管110能相对外管120转动。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 cavity 121 is formed between the inner tube 110 and the outer tube 120 . The inner tube 110 and the outer tube 120 are rotatably connected. In this embodiment, the inner tube 110 and the outer tube 120 are connected by a bearing, so that the inner tube 110 can rotate relative to the outer tube 120 .

承上所述,在本申请的一些实施例中,外管120还设置有与进气组件连通的进气孔;可以通过进气孔向第二物料腔121通入气体,例如通入反应气体或者保护气体。需要说明的是,对于不需要通入气体的实施例而言,外管120可以不设置进气孔。Continuing from the above, in some embodiments of the present application, the outer pipe 120 is further provided with an air intake hole communicating with the air intake assembly; gas, for example, a reaction gas can be introduced into the second material chamber 121 through the air intake hole or protective gas. It should be noted that, for the embodiment that does not need to pass gas, the outer pipe 120 may not be provided with an air inlet hole.

在本实施例中,外管120为圆形管,外管120与内管110同轴设置,外管120的材质为310S不锈钢管,外管120两端用法兰固定密封。In this embodiment, the outer tube 120 is a circular tube, the outer tube 120 and the inner tube 110 are coaxially arranged, the material of the outer tube 120 is a 310S stainless steel tube, and both ends of the outer tube 120 are fixed and sealed with flanges.

需要说明的是,在本申请的其他实施例中,外管120可以为其他形状,例如可以为棱柱形或者弯管形等;外管120的材质也可以根据需求进行选择。It should be noted that, in other embodiments of the present application, the outer tube 120 may be in other shapes, such as a prismatic shape or an elbow shape, etc.; the material of the outer tube 120 may also be selected according to requirements.

在本实施例中,第一驱动件130和第二驱动件140均为电机,第一驱动件130通过齿轮副与内管110传动连接,第二驱动件140通过齿轮副与外管120传动连接。In this embodiment, the first driving member 130 and the second driving member 140 are both motors, the first driving member 130 is drivingly connected to the inner tube 110 through a gear pair, and the second driving member 140 is drivingly connected to the outer tube 120 through a gear pair .

需要说明的是,在本申请的其他实施例中,第一驱动件130和第二驱动件140可以通过其他传动连接方式分别与内管110、外管120连接,使第一驱动件130与第二驱动件140能分别驱动内管110、外管120转动。It should be noted that, in other embodiments of the present application, the first driving member 130 and the second driving member 140 may be respectively connected to the inner tube 110 and the outer tube 120 through other transmission connection methods, so that the first driving member 130 and the The two driving members 140 can respectively drive the inner tube 110 and the outer tube 120 to rotate.

请再次参阅图1,在本实施例中,外管120外还套设有外壳122,外壳122与外管120通过转动轴套123连接,使外壳122能与外管120相对转动。Referring to FIG. 1 again, in this embodiment, the outer tube 120 is further sleeved with a casing 122 , and the casing 122 and the outer tube 120 are connected by a rotating shaft sleeve 123 , so that the casing 122 and the outer tube 120 can rotate relative to each other.

需要说明的是,在本申请的其他实施例中,反应炉100也可以不设置外壳122。It should be noted that, in other embodiments of the present application, the outer shell 122 may not be provided in the reaction furnace 100 .

图2示出了本申请实施例提供的外壳122的结构示意图,请参阅图2,在本实施例中,外壳122通过两个半圆弧形的板转动连接而成,外管120与外壳122可拆卸连接,外壳122上设置有卡扣,半圆弧形的板通过卡扣可拆卸连接,从而打开外壳122,从而将外管120安装入外壳122。FIG. 2 shows a schematic structural diagram of the housing 122 provided by the embodiment of the present application. Please refer to FIG. 2 . In this embodiment, the housing 122 is formed by rotating and connecting two semi-circular arc plates, and the outer tube 120 and the housing 122 can be connected For detachable connection, the shell 122 is provided with a buckle, and the semi-circular arc-shaped plate is detachably connected through the buckle, so as to open the shell 122 and install the outer tube 120 into the shell 122 .

图3示出了本申请实施例提供的加热组件150的结构示意图,请参阅图1和图3,加热组件150主要作用在于为外管120与内管110加热,从而对位于第一物料腔111和第二物料腔121内的物料加热。FIG. 3 shows a schematic structural diagram of a heating assembly 150 provided by an embodiment of the present application. Please refer to FIGS. 1 and 3 . The heating assembly 150 is mainly used to heat the outer tube 120 and the inner tube 110 , thereby heating the first material chamber 111 and the material in the second material chamber 121 is heated.

在本实施例中,加热组件150包括加热元件151和保温层152,加热元件151与外壳122连接,保温层152围设于外壳122的外周。例如,加热元件151可以为加热丝或是硅碳棒。In this embodiment, the heating assembly 150 includes a heating element 151 and an insulating layer 152 , the heating element 151 is connected to the casing 122 , and the insulating layer 152 is arranged around the outer periphery of the casing 122 . For example, the heating element 151 may be a heating wire or a silicon carbide rod.

通过加热元件151加热,然后热通过外壳122、外管120传递至第二物料腔121,然后再通过内管110传递至第一物料腔111。保温层152可避免大量热量损失,增加热利用率。It is heated by the heating element 151 , and then the heat is transferred to the second material chamber 121 through the outer shell 122 and the outer tube 120 , and then transferred to the first material chamber 111 through the inner tube 110 . The thermal insulation layer 152 can avoid a large amount of heat loss and increase the heat utilization rate.

需要说明的是,在本申请的其他实施例中,加热组件150可以为其他可以供热的机构,例如加热组件150可以为换热套管,通过换热套管对外管120与内管110加热等等,可以根据第一物料腔111和第二物料腔121内物料的目标加热温度设置加热组件150。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 through which the outer tube 120 and the inner tube 110 are heated And so on, the heating component 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 .

在本实施例中,反应炉100设置有用于支撑加热组件150的支撑架160,支撑架160与加热组件150连接。需要说明的是,在一些实施例中,支撑架160并非是必要的,反应炉100可以不设置支撑架160。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 with 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 .

在本申请的一些实施例中,如果第一物料腔111和第二物料腔121无须加热,反应炉100可以不设置加热组件150,换言之,加热组件150在一些实施例中并非是必要的。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 element 150 , in other words, the heating element 150 is not necessary in some embodiments.

在本实施例中,反应炉100可以还包括控制器,控制器与加热组件150的加热元件151连接从而控制第一物料腔111和第二物料腔121内物料的温度。In this embodiment, the reaction furnace 100 may further include a controller, which is connected to the heating element 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 .

进一步地,控制器还可以与第一驱动件130、第二驱动件140连接,控制器通过控制第一驱动件130、第二驱动件140的输出功率从而控制内管110和外管120的转速。Further, the controller can also be connected with the first driving member 130 and the second driving member 140 , and the controller controls the rotational speed of the inner tube 110 and the outer tube 120 by controlling the output power of the first driving member 130 and the second driving member 140 . .

本申请实施例提供的反应炉100至少具有以下优点:The reaction furnace 100 provided in the embodiment of the present application has at least the following advantages:

通过第一驱动件130驱动内管110转动,第二驱动件140驱动外管120转动,使第一物料腔111内的物料可以通过出料孔112进入第二物料腔121,使物料在第二物料腔121内反应或者混合;本申请提供的反应炉100可以调节第一物料腔111内的物料进入第二物料腔121内的粒径以及质量,具有控制混合或者反应速率的作用;可以应用于对混合过程或者反应过程有调控需要的工艺;此外,第一、第二物料腔内可大量加入物料,反应炉可以应用于材料的规模化生产。The inner tube 110 is driven to rotate by the first driving member 130, and the outer tube 120 is driven by the second driving member 140 to rotate, so that the material in the first material cavity 111 can enter the second material cavity 121 through the discharge hole 112, so that the material in the second material cavity 121 Reaction or mixing in the material cavity 121; the reaction furnace 100 provided by the present application can adjust the particle size and quality of the material in the first material cavity 111 entering the second material cavity 121, and has the effect of controlling the mixing or reaction rate; it can be applied to The mixing process or the reaction process needs to be controlled; in addition, a large amount of materials can be added to the first and second material chambers, and the reaction furnace can be applied to the large-scale production of materials.

以下就本申请实施例提供的反应炉100的使用做出示例进行描述。The following describes an example of the use of the reaction furnace 100 provided in the embodiments of the present application.

请参阅实施例1,实施例1所示的反应炉100制备物料的工艺,可以包括以下步骤:Please refer to Embodiment 1. The process for preparing materials in the reaction furnace 100 shown in Embodiment 1 may include the following steps:

将第一原料置于第一物料腔111,将第二原料置于第二物料腔121;加热组件150加热第一原料和第二原料;转动内管110和外管120,向第一物料腔或者第二物料腔通入保护气体;第一原料通过物料孔112进入第二物料腔121与第二原料反应。The first raw material is placed in the first material chamber 111, and the second raw material is placed in the second material chamber 121; the heating component 150 heats the first and second raw materials; the inner tube 110 and the outer tube 120 are rotated to move toward the first material chamber Or the second material cavity is passed into the protective gas; the first material enters the second material cavity 121 through the material hole 112 to react with the second material.

需要说明的是,在本申请中,步骤“将第一原料置于第一物料腔111”与步骤“将第二原料置于第二物料腔121”没有先后顺序,可以同时进行或者按照需求分别进行。It should be noted that, in this application, the steps of "putting the first raw material in the first material chamber 111" and the step of "putting the second raw material in the second material chamber 121" have no order, and can be performed simultaneously or separately according to requirements. conduct.

在制备过程中,可以向第一物料腔通入保护气体,也可以向第二物料腔内通入保护气体。In the preparation process, the protective gas can be introduced into the first material cavity, and the protective gas can also be introduced into the second material cavity.

以下就反应炉100制备物料做出两个示例。Two examples are given below for the preparation of materials in the reactor 100 .

实施例2Example 2

实施例2提供一种实施例1所示的反应炉100制备物料的工艺,主要包括以下步骤:Embodiment 2 provides a process for preparing materials in the reaction furnace 100 shown in Embodiment 1, which mainly includes the following steps:

步骤S1:将黏土矿物和盐置于第二物料腔121;其中,盐可以为NaCl、LiCl、KCl、CaCl2、ZnCl2、MgCl2中的至少一种;例如,盐可以为NaCl;黏土矿物为蒙脱石。需要说明的是,在本申请的其他实施例中,黏土矿物也不仅限于蒙脱石,例如可以为高岭石、伊利石等。Step S1: placing clay minerals and salts in the second material chamber 121; wherein the salts can be at least one of NaCl, LiCl, KCl, CaCl 2 , ZnCl 2 , and MgCl 2 ; for example, the salts can be NaCl; clay minerals For montmorillonite. It should be noted that, in other embodiments of the present application, the clay minerals are not limited to montmorillonite, for example, kaolinite, illite and the like.

作为示例性地,蒙脱石和NaCl的质量比为1:(0.1-5),例如可以为1:0.1、1:0.5、1:2、1:2.5、1:3、1:4、1:5等等。As an example, the mass ratio of montmorillonite and NaCl is 1:(0.1-5), for example, it can be 1:0.1, 1:0.5, 1:2, 1:2.5, 1:3, 1:4, 1: 5 and so on.

步骤S2:将第二原料置于第一物料腔111;第二原料包括镁、铝、钠、钾、钙和锌中的至少一种,例如,第二原料为金属镁。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 metal magnesium.

作为示例性地,镁和蒙脱石的质量比为(0.4-3):1,例如可以为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等等。As an example, the mass ratio of magnesium to montmorillonite is (0.4-3):1, for example, it 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, etc.

需要说明的是,步骤S1与步骤S2没有先后顺序。It should be noted that, step S1 and step S2 are not in sequence.

加热组件150对外管120加热,加热的温度可以为550-800℃,例如可以为550℃、580℃、600℃、610℃、620℃、630℃、640℃、650℃、660℃、670℃、680℃、690℃、700℃、730℃、760℃、800℃等等。The heating assembly 150 heats the outer tube 120, and the heating temperature can be 550-800°C, for example, 550°C, 580°C, 600°C, 610°C, 620°C, 630°C, 640°C, 650°C, 660°C, 670°C , 680°C, 690°C, 700°C, 730°C, 760°C, 800°C, etc.

向第一物料腔111内通入保护气体,或者,向第二物料腔121内通入保护气体;作为示例性地,保护气体可以为N2、Ar、He等气体。作为示例性地,保护气体的进气速度可以为1~10L/min,例如可以为1L/min、2L/min、3L/min、4L/min、5L/min、6L/min、7L/min、8L/min、9L/min、10L/min等等。A shielding gas is introduced into the first material chamber 111, or a shielding gas is introduced into the second material chamber 121; as an example, the shielding gas may be N 2 , Ar, He or other gases. As an example, the inlet speed of the shielding gas may be 1-10L/min, for example, it may be 1L/min, 2L/min, 3L/min, 4L/min, 5L/min, 6L/min, 7L/min, 8L/min, 9L/min, 10L/min, etc.

驱动内管110和外管120转动;作为示例性地,内管110的转速可以为160-240r/min,例如可以为160r/min、170r/min、180r/min、190r/min、200r/min、210r/min、220r/min、230r/min、240r/min等等;外管120的转速可以为30-80r/min,例如可以为30r/min、40r/min、50r/min、60r/min、70r/min、80r/min等等。Drive the inner tube 110 and the outer tube 120 to rotate; as an example, the rotation speed of the inner tube 110 may be 160-240r/min, for example, may be 160r/min, 170r/min, 180r/min, 190r/min, 200r/min , 210r/min, 220r/min, 230r/min, 240r/min, etc.; the rotation speed of the outer tube 120 can be 30-80r/min, for example, it can be 30r/min, 40r/min, 50r/min, 60r/min , 70r/min, 80r/min and so on.

物料在反应炉100内的反应时间可以为4-10h,例如可以为4h、5h、6h、7h、8h或者9h等等。The reaction time of the material in the reaction furnace 100 can be 4-10h, for example, it can be 4h, 5h, 6h, 7h, 8h or 9h and so on.

在一些实施例中,反应炉100内反应完成后,采用酸洗涤反应产物后将固相采用HF浸出,然后干燥。例如,可以采用HCl酸洗涤。In some embodiments, after the reaction in the reaction furnace 100 is completed, the reaction product is washed with acid, the solid phase is leached with HF, and then dried. For example, HCl acid wash can be used.

例如,在本实施例中,制备工艺如下:For example, in this embodiment, the preparation process is as follows:

将500g蒙脱石和2500g NaCl置于第二物料腔121,将300g金属镁均匀混合后放置于第一物料腔111,向第一物料腔111通入氩气,气流速度为6L/min;加热组件150将第一物料腔111内加热至650℃。内管110转速为200r/min,外管120转速为60r/min;反应5h然后自然冷却。500g of montmorillonite and 2500g of NaCl were placed in the second material chamber 121, 300g of magnesium metal was evenly mixed and placed in the first material chamber 111, and argon was introduced into the first material chamber 111, and the air flow rate was 6L/min; heating assembly 150 heats the inside of the first material chamber 111 to 650°C. The rotational speed of the inner tube 110 is 200 r/min, and the rotational speed of the outer tube 120 is 60 r/min; the reaction is performed for 5 hours and then cooled naturally.

取出反应后的产物,分别用蒸馏水和1mol/L HCl清洗,然后用1wt%HF浸出,然后用超纯水洗涤至中性,并在60℃下真空干燥,即可得到纳米硅材料。该纳米硅材料呈多孔结构,所含纳米硅纯度高,具有较大的比表面积。The reacted products were taken out, washed with distilled water and 1 mol/L HCl respectively, then leached with 1 wt% HF, washed with ultrapure water until neutral, and dried in vacuum at 60 °C to obtain nano-silicon materials. The nano-silicon material has a porous structure, contains high-purity nano-silicon, and has a larger specific surface area.

本实施例提供的基于反应炉100的制备方法至少具有以下优点:The preparation method based on the reaction furnace 100 provided in this embodiment has at least the following advantages:

在反应过程中,第一物料腔111的金属镁可以比较缓慢且均匀地进入第二物料腔121内与蒙脱石、NaCl反应;整个反应过程可控性较佳,可以根据出料孔112的孔径大小和内管110转速、外管120转速控制反应进行的快慢。During the reaction process, the metal magnesium in the first material cavity 111 can enter the second material cavity 121 relatively slowly and uniformly to react with montmorillonite and NaCl; The size of the aperture, the rotational speed of the inner tube 110 and the rotational speed of the outer tube 120 control the speed of the reaction.

金属镁以液态或气态形式从出料孔112逐步进入到第二物料腔121,然后与蒙脱石接触反应,有效避免了大量镁粉与蒙脱石反应产生的过量热量,从而避免生成的纳米硅熔融或者产生杂相;进一步地,第二物料腔121内的搅拌叶113的搅拌能防止反应体系中热量的累积,同时使反应物接触更均匀;通过气流、转速、内管壁的开口大小等条件的控制,可调控该反应的进程。The metal magnesium enters the second material cavity 121 from the discharge hole 112 in a liquid or gaseous state gradually, and then contacts and reacts with the montmorillonite, which effectively avoids the excess heat generated by the reaction between a large amount of magnesium powder and the montmorillonite, thereby avoiding the generated nanometer The silicon melts or generates a miscellaneous 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 at the same time make the contact of the reactants more uniform; Under the control of other conditions, the process of the reaction can be regulated.

实施例3Example 3

实施例3提供一种实施例1所示的反应炉100制备物料的工艺,主要包括以下步骤:Embodiment 3 provides a process for preparing materials in the reaction furnace 100 shown in Embodiment 1, which mainly includes the following steps:

步骤S1:将黏土矿物置于第二物料腔121;Step S1: placing clay minerals in the second material cavity 121;

步骤S2:将土壤添加剂置于第一物料腔111;Step S2: placing the soil additive in the first material cavity 111;

作为示例性地,黏土矿物为坡缕石,土壤添加剂为磷酸二氢钾;例如,坡缕石和磷酸二氢钾的质量比为(15-28):5,例如可以为15:5、18:5、20:5、22:5、23:5、25:5、28:5等等。As an example, the clay mineral is palygorskite, and the soil additive is potassium dihydrogen phosphate; for example, the mass ratio of palygorskite and potassium dihydrogen phosphate is (15-28):5, for example, it can be 15:5, 18: 5, 20:5, 22:5, 23:5, 25:5, 28:5, etc.

步骤S1与步骤S2没有先后顺序。Step S1 and step S2 are not in order.

驱动内管110和外管120转动;作为示例性地,内管110的转速可以为60-140r/min,例如可以为60r/min、70r/min、80r/min、90r/min、100r/min、110r/min、120r/min、130r/min、140r/min等等;外管120的转速可以为20-50r/min,例如可以为20r/min、22r/min、26r/min、30r/min、35r/min、40r/min、50r/min等等。Drive the inner tube 110 and the outer tube 120 to rotate; as an example, the rotation speed of the inner tube 110 may be 60-140r/min, for example, may be 60r/min, 70r/min, 80r/min, 90r/min, 100r/min , 110r/min, 120r/min, 130r/min, 140r/min, etc; , 35r/min, 40r/min, 50r/min and so on.

加热组件150对外管120加热,使第二物料腔121内的温度为250-320℃,例如可以为250℃、260℃、270℃、280℃、290℃、300℃、320℃等等。The heating component 150 heats the outer tube 120 so that the temperature in the second material chamber 121 is 250-320°C, such as 250°C, 260°C, 270°C, 280°C, 290°C, 300°C, 320°C and so on.

在反应炉100内的反应时间可以为1-4h,例如可以为1h、2h、3h、4h等等。The reaction time in the reaction furnace 100 can be 1-4h, for example, it can be 1h, 2h, 3h, 4h and so on.

例如,在本实施例中,制备工艺如下:For example, in this embodiment, the preparation process is as follows:

将2200g坡缕石置于第二物料腔121,将500g磷酸二氢钾置于第一物料腔111,内管110转速为100r/min,外管120转速为30r/min。2200g palygorskite was placed in the second material chamber 121, 500g potassium dihydrogen phosphate was placed in the first material chamber 111, the inner tube 110 was rotated at 100 r/min, and the outer tube 120 was rotated at 30 r/min.

加热组件150将第一物料腔111内加热至280℃。反应2h后自然冷却即得到坡缕石负载聚磷酸盐土壤调理剂。该土壤调理剂具有棒状形貌,磷在坡缕石表面均匀负载。The heating component 150 heats the first material chamber 111 to 280°C. The palygorskite-loaded polyphosphate soil conditioner was obtained by natural cooling after 2 hours of reaction. The soil conditioner has a rod-like morphology, and phosphorus is uniformly loaded on the palygorskite surface.

本实施例提供的基于反应炉100的制备方法至少具有以下优点:The preparation method based on the reaction furnace 100 provided in this embodiment has at least the following advantages:

在反应过程中,第一物料腔111的磷酸二氢钾可以比较缓慢且均匀地进入第二物料腔121内与坡缕石反应;达到缓慢释放且缓慢反应的效果,得到的土壤调理剂中聚磷酸盐可以比较均匀地分布于坡缕石表面。During the reaction process, the potassium dihydrogen phosphate in the first material cavity 111 can relatively slowly and uniformly enter the second material cavity 121 to react with palygorskite; the effect of slow release and slow reaction is achieved, and the obtained soil conditioner is polymerized in Phosphate can be relatively evenly distributed on the palygorskite surface.

详细地,在反应炉100内,内管110内的磷酸二氢钾先熔融,然后逐步释放与坡缕石混合、反应结合,在搅拌作用下,最终生成均匀负载聚磷酸盐的坡缕石基土壤调理剂,避免了传统高温固相反应因为不均匀不可控导致负载不均匀的问题;此外,本申请中将现有的先混合再加热的两步反应改良为采用反应炉100的一步制备,简化反应流程。In detail, in the reaction furnace 100, the potassium dihydrogen phosphate in the inner tube 110 is first melted, and then gradually released and mixed with the palygorskite to react and combine. The soil conditioner avoids the problem of uneven loading caused by the uneven and uncontrollable traditional high-temperature solid-phase reaction; in addition, in the present application, the existing two-step reaction of mixing first and then heating is improved to a one-step preparation using the reaction furnace 100, Simplify the reaction process.

以上所述仅为本申请的优选实施例而已,并不用于限制本申请,对于本领域的技术人员来说,本申请可以有各种更改和变化。凡在本申请的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本申请的保护范围之内。The above descriptions are only preferred embodiments of the present application, and are not intended to limit the present application. For those skilled in the art, the present application may have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of this application shall be included within the protection scope of this application.

Claims (9)

1. A process for the production of materials based on a reaction furnace, characterized in that it comprises:
the inner pipe is provided with a first material cavity, and a discharge hole which penetrates through the inner pipe and is communicated with the first material cavity is formed in the inner pipe;
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;
the second driving piece is connected with the outer pipe and is used for driving the outer pipe to rotate; and
the heating assembly is sleeved outside the outer pipe and is rotationally connected with the outer pipe;
the production process 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;
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, CaCl 2 、ZnCl 2 、MgCl 2 At least one of (1).
2. The reactor-based material production process of claim 1, wherein a stirring blade is provided at a side of the inner tube adjacent to the outer tube.
3. The reactor-based material production process according to claim 2, wherein 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.
4. The process for producing a reaction furnace-based material according to claim 1,
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 ℃.
5. The process for producing a reaction furnace-based material according to claim 1,
and the flow speed of the protective gas introduced into the first material cavity or the second material cavity is 1-10L/min.
6. The process for producing materials based on reaction furnace as claimed in claim 1, wherein after the first raw material enters the second 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.
7. A process for the production of a material based on a reaction furnace, characterized in that the reaction furnace comprises:
the inner pipe is provided with a first material cavity, and a discharge hole which penetrates through the inner pipe and is communicated with the first material cavity is formed in the inner pipe;
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;
the second driving piece is connected with the outer pipe and is used for driving the outer pipe to rotate; and
the heating assembly is sleeved outside the outer pipe and is rotationally connected with the outer pipe;
the production process 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;
the first raw material is clay mineral; the second raw material is a soil additive.
8. The reactor-based material production process of claim 7, wherein the first raw material is palygorskite; the second raw material is potassium dihydrogen phosphate.
9. The process for producing a reaction furnace-based material according to claim 7,
the rotating speed of the inner pipe is 60-140r/min, and the rotating speed of the outer pipe is 20-50 r/min.
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