Method for hydrothermal kettle synthesis reaction experiment through microwave heating
By adopting microwave heating technology and microwave focusing heating system in the hydrothermal kettle, combined with internal rotational rotation shaft and intelligent timing control, the problems of slow heating speed and uneven heating of traditional hydrothermal synthesis equipment are solved, and the ability of fast, uniform heating and multi-condition comparison experiments are achieved.
Patent Information
- Application Number
- CN202510491041.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-17
- Publication Date
- 2025-06-17
AI Technical Summary
Traditional hydrothermal synthesis equipment has problems such as slow heating speed, low preparation efficiency, uneven heating and insufficient safety, which is difficult to meet the needs of fast temperature response and multi-condition comparison experiments.
Using microwave heating technology, a microwave heating unit is set on the inner wall of the hydrothermal kettle, a microwave parabolic reflective surface and microwave tube are used to form a microwave focusing heating system, and combined with an internal rotational rotation axis and intelligent timing control, a fast, uniform heating and complex heating curve are achieved.
It has achieved 3-5 times the heating speed, improved heating uniformity, increased energy utilization to more than 92%, and has the ability to flexibly adjust and multi-condition comparison experiments, which has improved the efficiency and safety of the experiment.
Smart Images
Figure CN120155155A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of hydrothermal synthesis experiments, and specifically to a method and apparatus for microwave heating in a hydrothermal reactor synthesis reaction experiment, which is applicable to multi-parameter comparative experiments in fields such as chemistry, materials science, and bioengineering. Background Art
[0002] Traditional hydrothermal synthesis equipment has the following defects:
[0003] The heating rate of the electric heating wire heating method is slow (usually 30 - 60 minutes), which cannot meet the demand for rapid temperature response; the preparation efficiency of a single sample is low, and multi-condition comparative experiments cannot be carried out synchronously; mechanical stirring easily causes local overheating or uneven mixing, affecting the repeatability of the experiment; the exposed electrical components pose a risk of gas leakage and lack safety.
[0004] Although a rotating structure is adopted in the prior art, it still relies on the traditional heating method and fails to solve the core contradiction between rapid heating and uniformity. Summary of the Invention
[0005] The purpose of the present invention is to provide a method for microwave heating in a hydrothermal reactor synthesis reaction experiment with fast heating speed, uniform heating, good processability, and convenient temperature adjustment.
[0006] The purpose of the present invention is achieved as follows. A method for microwave heating in a hydrothermal reactor synthesis reaction experiment includes a box body (1) for the hydrothermal reactor synthesis reaction, characterized in that: a microwave heating unit is provided on the inner wall of the box body (1), and the microwave heating unit provides a microwave source for the reaction kettle bodies (3) distributed in a three-dimensional matrix along the rotating shaft (2). The inner-rotating rotating shaft (2) drives the reaction kettle bodies (3) to rotate at a speed of 0.5 - 10 rpm under the control of the controller (11), and the material continuously receives microwave radiation during the rotation of the reaction kettle bodies (3), forming an "rotation - heating - mixing" integrated process.
[0007] The microwave heating unit includes a microwave parabolic reflector (7) and a microwave tube (8), and the reaction kettle bodies (3) are within the radiation area of the microwave parabolic reflector (7).
[0008] The microwave parabolic reflector (7) is made of an aluminum parabolic surface with a thickness of 0.3 mm, and the focal length is designed to be 1.2 times the radius of the reaction kettle bodies (3).
[0009] The reaction kettle bodies (3) are evenly distributed in three circles at intervals along the circumference of the rotating shaft (2), with 2 - 3 in each circle, and there are 3 - 4 circles on the rotating shaft (2).
[0010] The controller (11) is electrically connected to the control panel (12), and the controller (11) and the control panel (12) are arranged on one surface of the box body (1).
[0011] The working principle of the present invention is as follows: In microwave heating, the rotation and friction of polar molecules: Microwave heating utilizes the fact that polar molecules such as water molecules will change their polar orientations under the action of a rapidly changing high-frequency electromagnetic field, resulting in molecular rotation and friction, thereby generating heat. Microwave heating does not require a heat conduction process, so the heating speed is extremely fast.
[0012] The advantages of the present invention are as follows:
[0013] 1: Microwave directly heats the reaction substance
[0014] The microwave tube heating unit (8) is adopted to introduce microwave energy into the reaction kettle body (3) through the microwave waveguide tube (9). By utilizing the resonance effect between the microwave and polar molecules (such as water molecules) in the material, rapid temperature rise can be achieved (the temperature rise rate can reach 10 - 15 °C / min), which is 3 - 5 times higher than the traditional method.
[0015] 2: Energy focusing technology
[0016] A microwave parabolic reflector (7) is arranged outside the reaction kettle body (3). By precisely designing the curvature and angle of the reflector, the microwave energy is concentrated in the reaction kettle area, and the energy utilization rate is increased to more than 92%, avoiding the energy loss caused by the inner wall of the box body (1) heating up.
[0017] 3: Dynamic rotation heating system
[0018] The inner-rotation type rotating shaft (2) drives the reaction kettle body (3) to rotate at a speed of 0.5 - 10 rpm, ensuring that the material continuously receives microwave radiation during the rotation process, forming an integrated process of "rotation - heating - mixing".
[0019] 4: Intelligent timing control
[0020] A programmable controller (11) is set to dynamically adjust the heating timing according to experimental requirements:
[0021] Rotation period: 0.5 - 30 minutes / time
[0022] Microwave pulse frequency: 1 - 10 Hz. The heating phase angle: adjustable from 0 - 360°. Through the above parameter combinations, complex heating curves such as gradient temperature rise and stage constant temperature can be achieved.
[0023] The following further describes the present invention in conjunction with the embodiments of the present invention: Description of the drawings
[0024] Figure 1 : Schematic diagram of the overall structure of Embodiment 1 (including the microwave focusing system)
[0025] Figure 2 : Schematic diagram of the overall structure of Embodiment 2 (including the microwave focusing system).
[0026] In the figure, 1 is the box body; 2 is the inner-rotating shaft; 3 is the reaction kettle body; 4 is the motor; 5 is the rotating shaft bearing bracket; 6 is the drive unit; 7 is the microwave parabolic reflector; 8 is the microwave tube; 9 is the microwave waveguide tube; 10 is the microwave circuit; 11 is the controller. 12 is the control panel. Detailed implementation mode
[0027] Example 1
[0028] As Figure 1 shown, a method of microwave heating for a hydrothermal kettle synthesis reaction experiment includes a box body (1) for the hydrothermal kettle synthesis reaction, and is characterized in that: a microwave heating unit is arranged on the inner wall of the box body (1), and the microwave heating unit provides a microwave source for the reaction kettle bodies (3) distributed in a three-dimensional matrix along the rotating shaft (2). The inner-rotating shaft (2) drives the reaction kettle bodies (3) to rotate at a speed of 0.5 - 10 rpm under the control of the controller (11), and the material continuously receives microwave radiation during the rotation of the reaction kettle bodies (3), forming an "rotation - heating - mixing" integrated process.
[0029] The present invention includes a box body (1), a rotating shaft (2), a motor 4, a controller (11) and a reaction kettle body (3). The controller (11) drives the rotating shaft (2) to rotate by controlling the motor 4. It is characterized in that: a microwave parabolic reflector (7) is arranged on the inner wall of the box body (1), and the microwave parabolic reflector (7) and the microwave tube (8) form a microwave focusing heating system. The reaction kettle bodies (3) are distributed in a three-dimensional matrix along the rotating shaft (2), and the reaction kettle bodies (3) are within the radiation area of the microwave parabolic reflector (7).
[0030] The microwave tube (8) emits 2450 MHz microwaves, which are transmitted to the parabolic reflector (7) through the waveguide tube (9).
[0031] The microwave parabolic reflector (7) is made of an aluminum parabolic surface with a thickness of 0.3 mm, and the focal length is designed to be 1.2 times the radius of the reaction kettle body (3). Each group of reaction kettle bodies or corresponding independent reflection units realizes precise energy distribution.
[0032] The motor (4) drives the rotating shaft (2) through a planetary gearbox to realize a compound motion of revolution + rotation.
[0033] The reaction kettle bodies (3) are evenly distributed along the circumference of the rotating shaft (3 - 6 per layer), with a total of 2 - 4 layers, and a total of 6 - 24 reaction units.
[0034] The controller (11) and the control panel (12) are arranged on one surface of the box body (1). The controller (11) can preset 50 groups of experimental programs, including parameters such as temperature (room temperature - 250 °C), rotation speed (0 - 500 rpm), time (0 - 999 min), etc.
[0035] The infrared thermometer can monitor the temperature of each reactor body in real time and feedback it to the controller (11) to dynamically adjust the microwave power. The controller (11) is a PID controller or the like.
[0036] The focal length of the microwave parabolic reflector (7) and the outer diameter of the reactor body (3) satisfy the geometric relationship of f = 1.2D.
[0037] The microwave heating adopts a pulse modulation mode, with a pulse width of 50 - 500 ms and a duty cycle of 10 - 90%.
[0038] The rotation period of the reactor body (3) and the microwave heating period satisfy the synchronous relationship of T_rot = n × T_mw (n is a natural number).
[0039] Example 2
[0040] As Figure 2 shown, different from Example 1, there are one or two sets of microwave focusing heating systems composed of the microwave parabolic reflector (7) and the microwave tube (8), which are distributed on the upper and lower surfaces or the front and rear surfaces of the box body (1).
[0041] In the microwave heating of the present invention, the rotation and friction of polar molecules: Microwave heating utilizes the fact that polar molecules such as water molecules will change their polar orientations under the action of a rapidly changing high-frequency electromagnetic field, resulting in molecular rotation and friction, thereby generating heat. Microwave heating does not require a heat conduction process, so the heating speed is extremely fast.
[0042] Direct heating: Microwave heating makes the heated material itself become a heating body and does not require a heat conduction process. Therefore, even materials with poor thermal conductivity can reach the heating temperature in a very short time.
[0043] Uniform heating: Microwave heating can uniformly penetrate electromagnetic waves into the object inside and outside at the same time to generate heat energy. Therefore, the heating uniformity is good and there will be no phenomenon of overcooked outside and undercooked inside.
Claims
1. A method for using microwave heating for a hydrothermal reactor synthesis reaction experiment, comprising a housing (1) for hydrothermal reactor synthesis reaction, characterized in that: A microwave heating unit is arranged on the inner wall of the box body (1), and the microwave heating unit provides a microwave source to a reaction kettle body (3) distributed in a three-dimensional matrix along the rotating shaft (2). The inner rotating shaft (2) drives the reaction kettle body (3) to rotate at a speed of 0.5-10 rpm under the control of the controller (11). The material is continuously exposed to microwave radiation during the rotation of the reaction kettle body (3), thereby forming an integrated process of "rotation-heating-mixing".
2. The method for using microwave heating in a hydrothermal reactor synthesis reaction experiment according to claim 1, characterized in that: The microwave heating unit comprises a microwave parabolic reflecting surface (7) and a microwave tube (8), and the reaction kettle body (3) is within the radiation area of the microwave parabolic reflecting surface (7).
3. The method of using microwave heating for a hydrothermal reactor synthesis reaction experiment according to claim 2, characterized in that: The microwave parabolic reflector (7) is a 0.3 mm thick aluminum parabola, and the focal length is designed to be 1.2 times the radius of the reactor body (3).
4. The method of using microwave heating for a hydrothermal reactor synthesis reaction experiment according to claim 1, characterized in that: The reaction kettle body (3) is evenly spaced in three circles along the circumference of the rotating shaft (2), with 2-3 circles in each circle, and there are 3-4 circles on the rotating shaft (2).
5. The method of using microwave heating for a hydrothermal reactor synthesis reaction experiment according to claim 1, characterized in that: The controller (11) is electrically connected to the control screen (12), and the controller (11) and the control screen (12) are arranged on one surface of the box body (1).