A hydrothermal kettle synthesis reaction device

Abstract

The utility model relates to the technical field of hydrothermal synthesis experiment, concretely relates to a hydrothermal kettle synthesis reaction device and method, and is suitable for the multi-parameter contrast experiment of chemical, material science, biological engineering and the field. Including box (1), rotating shaft (2), motor 4, controller (11) and reaction kettle body (3), the controller (11) rotates through the control motor 4 drive rotating shaft (2), its characterized in that: the box (1) inner wall sets up microwave parabolic reflector (7), and microwave parabolic reflector (7) and microwave tube (8) constitute microwave focusing heating system, the reaction kettle body (3) is along rotating shaft (2) and presents solid matrix distribution, and the reaction kettle body (3) is in the microwave parabolic reflector (7) radiation area.

Description

Technical Field

[0001] This utility model relates to the field of hydrothermal synthesis experimental technology, specifically to a hydrothermal reactor synthesis reaction apparatus and method, which is applicable to multi-parameter comparative experiments in fields such as chemistry, materials science, and bioengineering. Background Technology

[0002] Traditional hydrothermal synthesis equipment has the following drawbacks:

[0003] Heating with electric heating wires results in a slow heating rate (usually requiring 30-60 minutes), which cannot meet the requirements for rapid temperature response; the efficiency of single sample preparation is low, making it impossible to conduct multi-condition comparative experiments simultaneously; mechanical stirring can easily lead to local overheating or uneven mixing, affecting experimental repeatability; exposed electrical components pose a risk of gas leakage, resulting in insufficient safety.

[0004] Although existing technologies employ a rotating structure, they still rely on traditional heating methods and fail to resolve the core contradiction between rapid heating and uniformity. Summary of the Invention

[0005] The purpose of this invention is to provide a hydrothermal reactor synthesis reaction apparatus and method that features fast heating speed, uniform heating, good processability, and convenient temperature control.

[0006] The purpose of this utility model is achieved as follows: a hydrothermal reactor synthesis reaction device includes a box body (1), a rotating shaft (2), a motor 4, a controller (11), and a reactor body (3). The controller (11) drives the rotating shaft (2) to rotate by controlling the motor 4. The device is characterized in that: a microwave parabolic reflector (7) is provided on the inner wall of the box body (1). The microwave parabolic reflector (7) and the microwave tube (8) constitute a microwave focusing heating system. The reactor body (3) is distributed in a three-dimensional matrix along the rotating shaft (2). The reactor body (3) is located within the radiation area of ​​the microwave parabolic reflector (7).

[0007] The microwave tube (8) emits 2450MHz microwaves, which are transmitted to the parabolic reflector (7) via the waveguide (9).

[0008] The reflector is made of 0.3mm thick aluminum parabolic surface, and the focal length is designed to be 1.2 times the radius of the reactor body (3). Each reactor body or corresponding independent reflector unit can achieve precise energy distribution.

[0009] The motor (4) drives the rotating shaft (2) through the planetary gearbox to achieve a combined revolution and rotation motion.

[0010] The reactor body (3) is evenly distributed in 2-4 layers along the circumference of the rotation axis, with 3-6 per layer.

[0011] The controller (11) and the control panel (12) are set on one side of the housing (1). The controller (11) can preset 50 experimental programs, including parameters such as temperature (room temperature - 250℃), rotation speed (0-500rpm), and time (0-999min).

[0012] The infrared thermometer can monitor the temperature of each reaction vessel in real time and feed it back to the controller (11) to dynamically adjust the microwave power. The controller (11) is a PID controller.

[0013] The focal length of the microwave parabolic reflector (7) and the outer diameter of the reactor body (3) satisfy the geometric relationship f = 1.2D.

[0014] Microwave heating uses pulse modulation mode with a pulse width of 50-500ms and a duty cycle of 10-90%.

[0015] The rotation period of the reactor body (3) and the microwave heating period satisfy the synchronization relationship of T_rot=n×T_mw (n is a natural number).

[0016] In this invention, the rotation and friction of polar molecules occur during microwave heating: Microwave heating utilizes the fact that polar molecules, such as water molecules, change their polar orientation under the influence of a rapidly changing high-frequency electromagnetic field, causing molecular rotation and friction, thereby generating heat. Microwave heating eliminates the need for heat conduction, resulting in extremely fast heating speeds.

[0017] Innovation Point 1: Microwave Direct Heating of Reactive Substances

[0018] The microwave tube heating unit (8) introduces microwave energy into the reactor body (3) through the microwave waveguide (9), and utilizes the resonance effect of microwaves and polar molecules (such as water molecules) in the material to achieve rapid heating (the temperature rise rate can reach 10-15℃ / min), which is 3-5 times higher than the traditional method.

[0019] Innovation Point 2: Energy Focusing Technology

[0020] A microwave parabolic reflector (7) is set around the reactor body (3). By precisely designing the curvature and angle of the reflector, the microwave energy is concentrated in the reactor area, and the energy utilization rate is increased to more than 92%, avoiding energy loss caused by the heating of the inner wall of the box (1).

[0021] Innovation Point 3: Dynamic Rotary Heating System

[0022] The internal rotating shaft (2) drives the reactor body (3) to revolve at a speed of 0.5-10 rpm. At the same time, the reactor body rotates 360° by itself through the planetary gear mechanism, ensuring that the material is continuously irradiated by microwaves during the rotation process, forming an integrated process of "rotation-heating-mixing".

[0023] Innovation Point 4: Intelligent Timing Control

[0024] Configure the programmable controller (11) to dynamically adjust the heating sequence according to experimental requirements:

[0025] Rotation cycle: 0.5-30 minutes / cycle

[0026] Microwave pulse frequency: 1-10Hz. Heating phase angle: 0-360° adjustable. By combining the above parameters, complex heating curves such as gradient heating and staged isothermal heating can be achieved.

[0027] The present invention will be further described below with reference to embodiments thereof: Attached Figure Description

[0028] Figure 1 Example 1: Overall structural schematic diagram (including microwave focusing system)

[0029] Figure 2 Example 2: Overall structural diagram (including microwave focusing system).

[0030] In the diagram: 1. Box body; 2. Internal rotating shaft; 3. Reactor body; 4. Motor; 5. Rotating shaft bearing bracket; 6. Drive unit; 7. Microwave parabolic reflector; 8. Microwave tube; 9. Microwave waveguide; 10. Microwave circuit; 11. Controller; 12. Control panel. Detailed Implementation

[0031] Example 1

[0032] like Figure 1 As shown, a hydrothermal reactor synthesis reaction device includes a housing (1), a rotating shaft (2), a motor 4, a controller (11), and a reactor body (3). The controller (11) drives the rotating shaft (2) to rotate by controlling the motor 4. The device is characterized in that: a microwave parabolic reflector (7) is provided on the inner wall of the housing (1). The microwave parabolic reflector (7) and the microwave tube (8) constitute a microwave focusing heating system. The reactor body (3) is distributed in a three-dimensional matrix along the rotating shaft (2). The reactor body (3) is located within the radiation area of ​​the microwave parabolic reflector (7).

[0033] The microwave tube (8) emits 2450MHz microwaves, which are transmitted to the parabolic reflector (7) via the waveguide (9).

[0034] The microwave parabolic reflector (7) is made of 0.3mm thick aluminum parabolic surface. The focal length is designed to be 1.2 times the radius of the reactor body (3). Each reactor body or corresponding independent reflector unit can achieve precise energy distribution.

[0035] The motor (4) drives the rotating shaft (2) through the planetary gearbox to achieve a combined revolution and rotation motion.

[0036] The reactor body (3) is evenly distributed around the circumference of the rotation axis (3-6 units / layer), with a total of 2-4 layers and a total of 6-24 reaction units.

[0037] The controller (11) and the control panel (12) are set on one side of the housing (1). The controller (11) can preset 50 experimental programs, including parameters such as temperature (room temperature - 250℃), rotation speed (0-500rpm), and time (0-999min).

[0038] The infrared thermometer can monitor the temperature of each reaction vessel in real time and feed it back to the controller (11) to dynamically adjust the microwave power. The controller (11) is a PID controller.

[0039] The focal length of the microwave parabolic reflector (7) and the outer diameter of the reactor body (3) satisfy the geometric relationship f = 1.2D.

[0040] Microwave heating uses pulse modulation mode with a pulse width of 50-500ms and a duty cycle of 10-90%.

[0041] The rotation period of the reactor body (3) and the microwave heating period satisfy the synchronization relationship of T_rot=n×T_mw (n is a natural number).

[0042] Example 2

[0043] like Figure 2 As shown, unlike Example 1, the microwave parabolic reflector (7) and the microwave tube (8) constitute a microwave focusing heating system or there are two sets, distributed on the upper and lower surfaces or the front and back of the box (1).

[0044] In this invention, the rotation and friction of polar molecules occur during microwave heating: Microwave heating utilizes the fact that polar molecules, such as water molecules, change their polar orientation under the influence of a rapidly changing high-frequency electromagnetic field, causing molecular rotation and friction, thereby generating heat. Microwave heating eliminates the need for heat conduction, resulting in extremely fast heating speeds.

[0045] Direct heating: Microwave heating makes the material being heated itself a heat source, eliminating the need for heat conduction. Therefore, even materials with poor thermal conductivity can reach the heating temperature in a very short time.

[0046] Uniform heating: Microwave heating can cause electromagnetic waves to penetrate the surface of an object evenly and simultaneously to generate heat energy. Therefore, the heating uniformity is good and there will be no phenomenon of the outside being burnt while the inside is raw.

[0047] The present invention includes the following technical features:

[0048] Innovation Point 1: Microwave Direct Heating of Reactive Substances

[0049] The microwave tube heating unit (8) introduces microwave energy into the reactor body (3) through the microwave waveguide (9), and utilizes the resonance effect of microwaves and polar molecules (such as water molecules) in the material to achieve rapid heating (the temperature rise rate can reach 10-15℃ / min), which is 3-5 times higher than the traditional method.

[0050] Innovation Point 2: Energy Focusing Technology

[0051] A microwave parabolic reflector (7) is set around the reactor body (3). By precisely designing the curvature and angle of the reflector, the microwave energy is concentrated in the reactor area, and the energy utilization rate is increased to more than 92%, avoiding energy loss caused by the heating of the inner wall of the box (1).

[0052] Innovation Point 3: Dynamic Rotary Heating System

[0053] The internal rotating shaft (2) drives the reactor body (3) to revolve at a speed of 0.5-10 rpm. At the same time, the reactor body rotates 360° by itself through the planetary gear mechanism, ensuring that the material is continuously irradiated by microwaves during the rotation process, forming an integrated process of "rotation-heating-mixing".

[0054] Innovation Point 4: Intelligent Timing Control

[0055] Configure the programmable controller (11) to dynamically adjust the heating sequence according to experimental requirements:

[0056] Rotation cycle: 0.5-30 minutes / cycle

[0057] Microwave pulse frequency: 1-10Hz. Heating phase angle: 0-360° adjustable. By combining the above parameters, complex heating curves such as gradient heating and staged isothermal heating can be achieved.

Claims

1. A hydrothermal reactor synthesis apparatus, comprising a housing (1), a rotating shaft (2), a motor (4), a controller (11), and a reactor body (3), wherein the controller (11) drives the rotating shaft (2) to rotate by controlling the motor (4), characterized in that: The inner wall of the box (1) is provided with a microwave parabolic reflector (7), and the microwave parabolic reflector (7) and the microwave tube (8) constitute a microwave focusing heating system; The microwave parabolic reflector (7) is made of 0.3mm thick aluminum parabolic surface, and its focal length is designed to be 1.2 times the radius of the reactor body (3); The microwave tube (8) emits 2450MHz microwaves, which are transmitted to the parabolic reflector (7) via the waveguide (9). The motor (4) drives the rotating shaft (2) through a planetary gearbox to achieve a combined revolution and rotation motion; The reactor body (3) is evenly distributed in 2-4 layers along the circumference of the rotation axis (2), with 3-6 layers in each layer, forming a three-dimensional matrix distribution, and the reactor body (3) is located in the radiation area of ​​the microwave parabolic reflector (7).

2. The hydrothermal reactor synthesis apparatus according to claim 1, characterized in that: The controller (11) and the control panel (12) are set on one side of the housing (1). The controller (11) is a PID controller and can preset multiple experimental programs including temperature, speed and time.

3. The hydrothermal reactor synthesis apparatus according to claim 1, characterized in that: It also includes an infrared thermometer to monitor the temperature of each reactor body (3) in real time and feed it back to the controller (11), which dynamically adjusts the microwave power.

4. The hydrothermal reactor synthesis apparatus according to claim 1, characterized in that: Microwave heating uses pulse modulation mode with a pulse width of 50-500ms and a duty cycle of 10-90%.

5. A hydrothermal reactor synthesis apparatus according to claim 1, characterized in that: The rotation period of the reactor body (3) and the microwave heating period satisfy the synchronization relationship of T_rot = n × T_mw, where n is a natural number.

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