A tubular reactor for nano-gallium oxide preparation

Abstract

The utility model provides a kind of for nanometer gallium oxide preparation's tubular reactor, including reactor cavity, be located in the feeding port of front end and the discharge port of end. At least two stirring assemblies are equipped in cavity along the axial direction, each stirring assembly includes stirring spindle, is equipped in the push material helical blade of spindle outer periphery and is equipped in the interval position of helical blade paddle, paddle is arranged obliquely to enhance radial and circumferential mixing. Expansion zone is equipped between adjacent stirring assemblies, for flow homogenization. Each stirring assembly is equipped with independent driving device, and heating jacket of subsection independent temperature control is equipped outside reactor. The utility model is designed by multistage combined stirring and controllable temperature field, realizes three-dimensional sufficient mixing and uniform heating in the axial conveying process of solution, effectively solves the problem that traditional tubular reactor is not mixed evenly in nanometer gallium oxide precursor ripening process, temperature distribution is not uniform, is applicable to the large-scale, homogenization preparation of high-performance nanomaterial.

Description

Technical Field

[0001] This utility model relates to the field of semiconductor material preparation equipment technology, and in particular to a tubular reactor for the preparation of nano-gallium oxide. Background Technology

[0002] Gallium oxide nanomaterials refer to gallium oxide nanomaterials with a particle size ranging from 1 to 100 nm. With a band gap of 4.8-5.0 eV, they belong to the category of ultra-wide bandgap semiconductor materials, exhibiting high breakdown electric field, high thermal stability, excellent radiation resistance, and good chemical stability. They have significant application value in optoelectronics, electronics, and catalysis. Chemical precipitation is one of the commonly used methods for preparing gallium oxide nanomaterials. Its main production process includes the preparation of the precursor solution, solution aging, solid-liquid separation and dispersion, and calcination and dispersion of the material. Solution aging is one of the key steps.

[0003] Currently, commonly used maturation equipment employs spiral stirring, but this spiral stirring structure is typically a single spiral. Due to the viscosity of the solution, a single spiral structure can only achieve axial transport, failing to provide sufficient radial stirring and circulation. This results in significant temperature gradients and reaction rate differences during the maturation process, making it difficult for the maturation reaction to proceed uniformly. Therefore, existing tubular reactors struggle to meet the uniform heating and stable reaction conditions required for solution maturation. Utility Model Content

[0004] The purpose of this invention is to provide a tubular reactor for the preparation of nano-gallium oxide, so as to solve the problems of uneven solution mixing and uneven aging reaction caused by the single stirring structure of existing tubular reactors.

[0005] According to the purpose of this utility model, this utility model provides a tubular reactor for the preparation of nano-gallium oxide, including a reactor cavity, a feed port at the front end of the reactor cavity and a discharge port at the end end, and at least two stirring components arranged axially inside the reactor cavity. Each stirring component includes a stirring main shaft, a pushing spiral blade and a paddle agitator blade. The pushing spiral blade is located on the outer periphery of the stirring main shaft, and the paddle agitator blade is located at the interval of the pushing spiral blade.

[0006] Furthermore, the paddle-type tumbling blades are provided with turbulence blocks.

[0007] Furthermore, the shape of the turbulence block is one of hemispherical, prismatic, or airfoil.

[0008] Furthermore, the paddle-type agitator blades are inclined relative to the axis of the stirring main shaft, with an inclination angle of 45°~60°.

[0009] Furthermore, an expansion zone is provided between two adjacent stirring components, and the expansion zone is a straight cylindrical section without a stirring structure.

[0010] Furthermore, each of the stirring components is equipped with an independent drive unit, and each drive unit independently adjusts its rotation speed.

[0011] Furthermore, the reactor cavity is provided with a heating jacket or heating jacket outside, and the heating jacket or heating jacket is divided into multiple independent temperature control zones along the axial direction.

[0012] Furthermore, a gap of 3-10 mm is provided between the outer edge of the pushing spiral blade, the paddle agitator blade and the turbulence block of the stirring assembly and the inner wall of the reactor cavity.

[0013] Furthermore, the stirring spindles are connected by a spindle sleeve connection.

[0014] Furthermore, the reactor cavity is equipped with a temperature sensor and a pressure sensor, and both the feed port and the discharge port are equipped with flow control valves.

[0015] This invention employs at least two axially distributed stirring components, each incorporating a pusher helical blade and an inclined paddle-type agitator with turbulence blocks. This achieves intense radial and circumferential shear mixing of the solution while it is being axially transported, creating a three-dimensional stirring effect. This effectively eliminates temperature and concentration gradients within the reactor, significantly improving the uniformity and consistency of the maturation of the gallium oxide nano-precursor solution. The independently driven structure of each stirring component, along with an intermediate expansion zone, allows for precise intensity and flow rate control at different reaction stages, preventing material stagnation and localized overheating. Combined with a segmented, independently temperature-controlled heating system, this reactor enables flexible optimization of process parameters, resulting in the stable production of gallium oxide nano-materials with narrow particle size distribution and good dispersion. This makes it suitable for the large-scale, uniform preparation of high-performance nanomaterials. Attached Figure Description

[0016] To more clearly illustrate the specific embodiments of this utility model or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this utility model. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0017] Figure 1 This is a schematic diagram of the overall structure of an embodiment of the present utility model; Figure 2 This is a partial structural schematic diagram of the two stirring components in an embodiment of the present invention; Figure 3 This is a three-dimensional structural diagram of the stirring assembly in an embodiment of the present invention.

[0018] In the diagram: 1. Reactor chamber; 2. Feed inlet; 3. Discharge outlet; 4. Expansion zone; 5. Mixing assembly; 511. First mixing spindle; 512. First pusher spiral blade; 513. First paddle agitator blade; 514. Turbulence block; 521. Second mixing spindle; 522. Second pusher spiral blade; 523. Second paddle agitator blade. Detailed Implementation

[0019] The technical solution of this utility model will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of this utility model, not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of this utility model.

[0020] In the description of this utility model, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc., indicating the orientation or positional relationship are based on the orientation or positional relationship shown in the accompanying drawings, and are only for the convenience of describing this utility model and simplifying the description, and are not intended to indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this utility model.

[0021] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the stated features. In the description of this utility model, "a plurality of" means two or more, unless otherwise explicitly specified. Furthermore, the terms "installed," "connected," and "linked" should be interpreted broadly; for example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances.

[0022] Example 1 like Figures 1-3As shown, a tubular reactor for the preparation of nano-gallium oxide includes a reactor cavity 1, with a feed port 2 at the front end and a discharge port 3 at the rear end. Multiple stirring components 5 are arranged axially inside the reactor cavity 1. Flow control valves are respectively installed at the feed port 2 and the discharge port 3.

[0023] Each stirring assembly 5 includes a stirring shaft, a pusher screw blade, and paddle agitators. The stirring shaft axially penetrates the reactor cavity 1. The pusher screw blade is disposed on the outer periphery of the stirring shaft, and the paddle agitators are distributed at intervals between the pusher screw blades. Turbulence blocks are provided on the paddle agitators.

[0024] The spoiler can be hemispherical, prismatic, or airfoil-shaped.

[0025] The paddle-type agitator blades are inclined relative to the axis of the mixing main shaft, with an inclination angle of 45°~60°.

[0026] The paddle-type agitator blades are evenly distributed around the circumference of the mixing shaft.

[0027] In this embodiment, the pusher screw blade is a single-headed screw blade or a double-headed screw blade, and the pitch of the pusher screw blade gradually changes along the material flow direction.

[0028] The various stirring components are connected by a spindle sleeve. A gap of 3-10 mm is left between the stirring components and the inner wall of the reactor chamber.

[0029] An expansion zone is provided between two adjacent mixing components. The expansion zone is a straight cylindrical section without a mixing structure.

[0030] Each mixing component is equipped with an independent drive unit, which can be an independent drive motor or a multi-channel drive mechanism.

[0031] The reactor cavity 1 is provided with a heating jacket or heating jacket outside, and the heating jacket or heating jacket is divided into multiple independent temperature control zones along the axial direction of the reactor cavity.

[0032] Temperature and pressure sensors are installed on reactor chamber 1.

[0033] The stirring shaft is made of corrosion-resistant metal and its surface is polished. Some sections of the stirring shaft are hollow. The inner wall of reactor chamber 1 is coated with a corrosion-resistant coating.

[0034] Example 2 like Figures 1-3As shown in the figure, this embodiment discloses a tubular reactor for the preparation of nano-gallium oxide, comprising a cylindrical reactor chamber 1, with a feed port 2 at the front end and a discharge port 3 at the rear end. Two stirring components 5 are sequentially arranged axially inside the reactor chamber 1, forming an expansion zone 4 between the two stirring components 5. In practical applications, the number of stirring components 5 can be set to two or more depending on the reactor length and process requirements.

[0035] Each stirring assembly 5 includes a stirring shaft, a pusher screw blade, and paddle agitators. The stirring shaft extends axially through the reactor chamber 1. The pusher screw blade is welded or fixed to the outer circumferential surface of the stirring shaft, and is used to push the solution forward axially along the reactor chamber 1. The paddle agitators are fixed to the stirring shaft by support rods and are located at intervals between the pusher screw blades. The paddle agitators are inclined relative to the axis of the stirring shaft, preferably at an angle of 45° to 60°, to generate significant radial and circumferential stirring action based on the axial thrust.

[0036] To further enhance the dispersion effect, multiple turbulence blocks 514 are welded onto the paddle-type tumbling blades. The turbulence blocks 514 can be hemispherical, prismatic, or other shapes, and their function is to create a local high-shear flow field in the area swept by the paddle blades, breaking up agglomerated particles formed in the solution.

[0037] Specifically, in this embodiment, the stirring assembly 5 includes a first stirring assembly and a second stirring assembly, wherein: The first mixing assembly includes a first mixing spindle 511, a first pushing spiral blade 512, and a first paddle-type agitator blade 513. The first stirring shaft 511 is axially arranged along the reactor cavity 1. The first pusher spiral blade 512 is welded or fixed to the outer circumferential surface of the first stirring shaft 511 by a key connection, used to push the solution forward axially along the reactor cavity 1. The first paddle-type agitator blade 513 is fixed to the first stirring shaft 511 by a support rod and is located at intervals between the first pusher spiral blade 512. The first paddle-type agitator blade 513 is inclined relative to the axis of the first stirring shaft 511, preferably at an angle of 45° to 60°, to generate significant radial and circumferential stirring action based on the axial thrust. Multiple turbulence blocks 514 are welded onto the first paddle-type agitator blade 513.

[0038] The second stirring shaft 521 is axially arranged along the reactor cavity 1. The second pusher screw blade 522 is welded or fixed to the outer circumferential surface of the second stirring shaft 521 by key connection, and is used to push the solution forward along the axial direction of the reactor cavity 1. The second paddle agitator blade 523 is fixed to the second stirring shaft 521 by support rod and is located at the interval of the second pusher screw blade 522. The second paddle agitator blade 523 is inclined relative to the axis of the second stirring shaft 521, and the inclination angle is preferably 45°~60°, so as to generate significant radial and circumferential stirring effect based on the axial thrust.

[0039] Each mixing component 5 is connected by a spindle sleeve connection, that is, the front end of the spindle of the subsequent mixing component is inserted into the sleeve at the tail end of the spindle of the preceding mixing component, and torque is transmitted through a coupling or spline. Each mixing component 5 is equipped with an independent drive motor (not shown in the figure), and the speed of each drive motor is independently adjusted by the control system, thereby realizing independent control of the mixing intensity of different sections.

[0040] The outer edge of the pusher screw blade, paddle agitator blade and turbulence block 514 of the stirring assembly 5 is kept 3-10mm away from the inner wall of the reactor cavity 1 to avoid material retention and local overheating caused by mechanical friction.

[0041] Expansion zone 4 is a straight cylindrical section without stirring, and its length is not less than 0.5 times the inner diameter of reactor cavity 1. After being stirred in the previous stirring component, the solution enters expansion zone 4, where the flow rate decreases and the flow tends to be stable, achieving temporary homogenization and diffusion, preparing it for entering the next stirring component.

[0042] The reactor chamber 1 is externally enclosed by a heating jacket, which is divided along the axial direction into multiple independently temperature-controlled heating zones, corresponding to each stirring component 5 and the expansion zone 4, to achieve gradient or uniform control of the reaction temperature. Temperature and pressure sensors are installed on the reactor chamber 1 for real-time monitoring of the internal operating conditions. Flow control valves are installed at both the feed port 2 and the discharge port 3 to regulate the feed and discharge rates. A slag discharge port is also provided at the bottom of the reactor chamber 1 for periodic cleaning of sediment.

[0043] The working process of this utility model is as follows: The solution enters the reactor chamber 1 through the feed port 2 and first enters the first stirring assembly. The first pushing spiral blade 512 of the first stirring assembly pushes the solution forward, while the first paddle-type agitator blade 513 and the turbulence block 514 perform radial and circumferential stirring and shearing on the solution to achieve preliminary mixing and dispersion.

[0044] The solution then enters expansion zone 4, where the flow rate distribution is homogenized, preventing uneven flow caused by the previous stirring from being carried directly into the next stage.

[0045] The solution then enters the second stirring assembly, where it is further mixed and dispersed under the combined action of the second pushing spiral blade 522 and the second paddle-type agitator blade 523. The stirring speed is the same as or different from that of the first stirring assembly, depending on the process requirements.

[0046] The fully matured solution is finally discharged from outlet 3 and enters the subsequent process.

[0047] By adjusting the rotation speed of each stirring component, the temperature of each zone of the heating jacket, and the solution flow rate, precise control of the maturation process can be achieved, thereby obtaining a nano-gallium oxide precursor with uniform particle size distribution and stable performance.

[0048] This invention sets up multiple stirring components, and combines a pusher screw blade and a paddle agitator blade in each stirring component, so that the solution can be fully mixed radially and circumferentially while being transported axially, forming a three-dimensional stirring effect, which significantly improves the uniformity of the ripening reaction; the turbulence blocks set on the paddle agitator blade can form a local high shear zone, effectively breaking up agglomerates in the solution, promoting particle dispersion, and avoiding the formation of large particles. The various stirring components of this invention are connected by a main shaft sleeve and equipped with an independent drive device, which can realize independent and precise control of the stirring speed of each section to adapt to the process requirements of different maturation stages; a gap is left between the stirring components and the inner wall of the reactor cavity to avoid dead corners of solution stagnation and frictional heating; an expansion zone is set between adjacent stirring components to allow the solution to stay briefly, diffuse and homogenize before entering the next stirring component, thereby improving reaction stability and distribution uniformity; This novel tubular reactor has a reasonable structure and flexible control, making it suitable for the large-scale and homogenized preparation of high-performance nanomaterials such as gallium oxide.

[0049] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this utility model, and are not intended to limit it. Although the utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this utility model.

Claims

1. A tubular reactor for the preparation of nano-gallium oxide, characterized in that, The reactor includes a reactor cavity, with a feed port at the front end and a discharge port at the end. At least two stirring components are arranged axially inside the reactor cavity. Each stirring component includes a stirring main shaft, a pushing spiral blade, and a paddle agitator blade. The pushing spiral blade is located on the outer periphery of the stirring main shaft, and the paddle agitator blade is located at the interval between the pushing spiral blade.

2. The tubular reactor for the preparation of nano-gallium oxide according to claim 1, characterized in that, The paddle-type tumbling blades are equipped with turbulence blocks.

3. The tubular reactor for the preparation of nano-gallium oxide according to claim 2, characterized in that, The shape of the turbulence block is one of hemispherical, prismatic, or airfoil.

4. The tubular reactor for the preparation of nano-gallium oxide according to claim 1, characterized in that, The paddle-type agitator blades are inclined relative to the axis of the stirring main shaft, with an inclination angle of 45° to 60°.

5. The tubular reactor for the preparation of nano-gallium oxide according to claim 1, characterized in that, An expansion zone is provided between two adjacent stirring components, and the expansion zone is a straight cylindrical section without a stirring structure.

6. The tubular reactor for the preparation of nano-gallium oxide according to claim 1, characterized in that, Each of the stirring components is equipped with an independent drive unit, and each drive unit can independently adjust its rotation speed.

7. The tubular reactor for the preparation of nano-gallium oxide according to claim 1, characterized in that, The reactor cavity is provided with a heating jacket or heating jacket outside, and the heating jacket or heating jacket is divided into multiple independent temperature control zones along the axial direction.

8. The tubular reactor for the preparation of nano-gallium oxide according to claim 2, characterized in that, The outer edges of the pushing spiral blades, the paddle-type agitator blades, and the turbulence block of the stirring assembly are provided with a gap of 3-10 mm between them and the inner wall of the reactor cavity.

9. The tubular reactor for the preparation of nano-gallium oxide according to claim 1, characterized in that, The stirring spindles are connected by a spindle sleeve connection.

10. The tubular reactor for the preparation of nano-gallium oxide according to claim 1, characterized in that, The reactor chamber is equipped with a temperature sensor and a pressure sensor, and both the feed port and the discharge port are equipped with flow control valves.

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