Sodium thermal reduction reaction online observation system

Abstract

The utility model discloses a sodium thermal reduction reaction on-line observation system which comprises a reaction device; the reaction device is provided with a transparent observation area and is used for carrying out sodium thermal reduction reaction; the high-definition and high-speed camera is mounted in a manner of being matched with the reaction device and is used for acquiring image data of the sodium thermal reduction reaction through the transparent observation area; the information processing device is connected with the high-definition and high-speed camera and is used for storing and processing the obtained image data; the reaction device comprises a quartz crucible used for containing reaction raw materials for a sodium thermal reduction reaction; the reaction furnace is used for arranging a reaction crucible, the two sides of the reaction furnace are of hollow structures, and transparent quartz glass is arranged in the hollow structures; and the heating device is matched with the reaction furnace and is used for heating the reaction furnace. Real-time image data of the sodium thermal reduction reaction occurring in the reaction device can be dynamically recorded, direct evidences of phase change, particle morphology evolution and reduction reaction mechanism in the reaction process are provided through information processing, and optimization of the reaction process is facilitated.

Description

Technical Field

[0001] This invention belongs to the field of high-temperature metal material preparation technology, specifically relating to an online observation system for sodium thermal reduction reaction. Background Technology

[0002] Sodium thermal reduction is an important metal thermal reduction process widely used in the preparation of high-melting-point metals and their compounds. For example, sodium thermal reduction of potassium fluorotantalate (K₂TaF₇) is one of the important methods for preparing tantalum metal. In traditional processes, this reduction process is usually carried out in a closed reactor, making it difficult for researchers to directly observe the reaction process. They can only infer the reaction mechanism through the analysis of the final product. This approach not only limits the in-depth understanding of reaction kinetics but also affects the precision of process optimization.

[0003] In current technologies, research on high-temperature metal thermal reduction processes mainly relies on indirect detection methods, such as final product composition analysis, thermal analysis (TG / DSC), or theoretical simulation. However, these methods struggle to provide direct evidence of phase changes, particle morphology evolution, and reduction mechanisms during the reaction process. Utility Model Content

[0004] In view of this, some embodiments disclose an online observation system for sodium thermal reduction reactions, including:

[0005] The reaction apparatus has a transparent observation area for the sodium thermal reduction reaction to occur.

[0006] A high-definition, high-speed camera is fitted and installed with the reaction device to acquire image data of the sodium thermal reduction reaction through a transparent observation area.

[0007] An information processing device, connected to a high-definition high-speed camera, is used to store and process the acquired image data.

[0008] Furthermore, some embodiments disclose an online observation system for sodium thermal reduction reactions, the reaction apparatus comprising:

[0009] Quartz crucible, used to set the reaction raw materials for sodium thermal reduction reaction;

[0010] The reactor is used to house the reaction crucible. The two sides of the reactor are hollowed out, and transparent quartz glass is placed inside the hollowed-out structure.

[0011] A heating device, adapted to the reactor, is used to heat the reactor.

[0012] The online observation system for sodium thermal reduction reaction disclosed in some embodiments also includes:

[0013] A wireless communication component configured to wirelessly connect with a high-definition high-speed camera and an information processing device for wirelessly transmitting acquired image data.

[0014] Some embodiments disclose an online observation system for sodium thermal reduction reactions, the information processing device of which includes:

[0015] Communication components for connecting and communicating with the high-definition high-speed camera;

[0016] Information processing components are used to receive, store, and process image data;

[0017] A monitor is used to display image data.

[0018] Some embodiments of the online observation system for sodium thermal reduction reaction also include a gas source assembly for supplying reaction gases to the reaction apparatus.

[0019] The online observation system for sodium thermal reduction reaction disclosed in this embodiment of the invention can dynamically acquire image data of the reaction device, record real-time image data of the sodium thermal reduction reaction occurring in the reaction device, and further store, process and display the data through an information processing component. This facilitates the analysis and characterization of the recorded sodium thermal reduction reaction process, thereby improving the accuracy and precision of data analysis, providing direct evidence of phase changes, particle morphology evolution and reduction reaction mechanism during the reaction process, and helping to optimize the reaction process. Attached Figure Description

[0020] Figure 1 Example 1: Schematic diagram of the composition of the online observation system for sodium thermal reduction reaction.

[0021] Figure Labels

[0022] 1. Reactor 2. Quartz Crucible

[0023] 3 Quartz glass 4 Heating device

[0024] 5. Air supply components 6. High-definition high-speed camera

[0025] 7. Information processing device Detailed Implementation

[0026] The term "embodiment" used herein, as an example, is not necessarily to be construed as superior to or better than other embodiments. Performance testing in these embodiments of the present invention, unless otherwise specified, employs conventional testing methods in the art. It should be understood that the terminology used herein is merely for describing particular implementations and is not intended to limit the scope of the disclosure of these embodiments.

[0027] Unless otherwise stated, the technical and scientific terms used herein have the same meanings as commonly understood by one of ordinary skill in the art to which this invention pertains; other test methods and technical means not specifically noted in this invention refer to test methods and technical means commonly used by one of ordinary skill in the art.

[0028] The terms “basic” and “approximately” used in this document are to describe small fluctuations. For example, they can mean less than or equal to ±5%, such as less than or equal to ±2%, such as less than or equal to ±1%, such as less than or equal to ±0.5%, such as less than or equal to ±0.2%, such as less than or equal to ±0.1%, such as less than or equal to ±0.05%. Numerical data presented or expressed in range format in this document are used for convenience and brevity only, and should therefore be flexibly interpreted to include not only the explicitly listed values ​​that define the range, but also all independent values ​​or subranges contained within that range. For example, a numerical range of “1–5%” should be interpreted to include not only the explicitly listed values ​​from 1% to 5%, but also the independent values ​​and subranges within the indicated range. Thus, this numerical range includes independent values ​​such as 2%, 3.5%, and 4%, and subranges such as 1%–3%, 2%–4%, and 3%–5%, etc. This principle also applies to ranges that list only one value. Furthermore, this interpretation applies regardless of the width of the range or the characteristics described.

[0029] In this document, including in the claims, conjunctions such as "comprising," "including," "with," "having," "containing," "involving," and "accommodating" are understood to be open-ended, meaning "including but not limited to." Only the conjunctions "consisting of" and "composed of" are closed conjunctions.

[0030] To better illustrate the content of this utility model, numerous specific details are provided in the following detailed embodiments. Those skilled in the art should understand that this utility model can be implemented even without certain specific details. In the embodiments, some methods, means, instruments, and equipment well known to those skilled in the art are not described in detail, in order to highlight the main points of this utility model.

[0031] Without conflict, the technical features disclosed in the embodiments of this utility model can be combined arbitrarily, and the resulting technical solution belongs to the content disclosed in the embodiments of this utility model.

[0032] In some embodiments, the online observation system for sodium thermal reduction reaction includes:

[0033] A reaction apparatus; the reaction apparatus has a transparent observation area for conducting a sodium thermal reduction reaction; in some embodiments, the reaction apparatus includes: a quartz crucible for holding the reaction raw materials for the sodium thermal reduction reaction; a reaction furnace for holding the reaction crucible, the sides of the reaction furnace having a hollow structure, and transparent quartz glass being placed inside the hollow structure; and a heating device adapted to the reaction furnace for heating the reaction furnace.

[0034] A high-definition, high-speed camera is fitted and installed with the reaction device to acquire image data of the sodium thermal reduction reaction through a transparent observation area.

[0035] An information processing device, connected to a high-definition high-speed camera, is used to store and process acquired image data; generally, the information processing device includes: a communication component for communicating with the high-definition high-speed camera; an information processing component for receiving, storing, and processing image data; and a display for displaying the image data.

[0036] Some embodiments of the online observation system for sodium thermal reduction reaction also include a wireless communication component configured to wirelessly connect to a high-definition high-speed camera and an information processing device for wirelessly transmitting acquired image data.

[0037] Some embodiments disclose an online observation system for sodium thermal reduction reaction, the information processing device including: a communication component for communicating with the high-definition high-speed camera; an information processing component for receiving, storing and processing image data; and a display for displaying the image data.

[0038] Some embodiments of the online observation system for sodium thermal reduction reaction also include a gas source assembly for supplying reaction gases to the reaction apparatus.

[0039] The technical details are further illustrated below with reference to the embodiments.

[0040] Example 1

[0041] Figure 1 This is a schematic diagram of the composition of the online observation system for sodium thermal reduction reaction disclosed in Example 1.

[0042] In Example 1, the online observation system includes: a reaction device; the reaction device includes a reactor 1 and a quartz crucible 2 disposed inside the reactor 1, the reactor 1 has a hollow structure on both sides, and transparent quartz glass 3 is disposed inside the hollow structure; a heating device 4 is adapted to be disposed below the reactor 1, and the reactor 1 is provided with a gas source assembly 5; a high-definition high-speed camera 6 is disposed on one side of the reaction device, corresponding to the transparent quartz glass 3 of the reactor 1; and an information processing device 7 is connected to the high-definition high-speed camera 6.

[0043] The online observation system in Example 1 is used for online observation of the sodium-thermal reduction of potassium fluorotantalate. The method includes:

[0044] (a) Potassium fluorotantalate (K2TaF7) and basic salts (NaCl, KCl) are mixed in a certain proportion and placed in quartz crucible 2;

[0045] (b) Placing metallic sodium (Na) directly into a quartz crucible 2 containing potassium fluorotantalate (K2TaF7) and basic salts (NaCl, KCl) to ensure that sodium can fully contact the reactants so that a reduction reaction can occur during heating;

[0046] (c) Place the quartz crucible 2 containing the reactants into the transparent perforated reaction furnace 1 on both sides to ensure that the reaction process can be observed in real time during the heating process;

[0047] (d) The furnace body temperature of the reactor 1 is raised to a set temperature range, such as 750-900°C, by means of a heating device, so that the metallic sodium melts and spontaneously undergoes a reduction reaction with potassium fluorotantalate;

[0048] (e) Using a high-speed, high-definition camera, the entire reduction reaction process is recorded in real time, and the images are synchronized to a computer via a data transmission system so that the reaction process can be observed and analyzed in real time.

[0049] (f) After the reduction reaction is complete, stop heating and wait for the system to cool to room temperature. Then, take out the product and analyze and characterize the generated tantalum metal through subsequent processing.

[0050] Example 2

[0051] In Example 2, a sodium thermal reduction experiment was conducted using an online observation system for the sodium thermal reduction reaction, including:

[0052] A 1:1 molar ratio of NaCl to KCl was selected as the base salt. Potassium fluorotantalate (K₂TaF₇) and metallic sodium (Na) were placed together in a transparent quartz crucible, which was then placed inside a furnace with transparent, perforated sides. The heating temperatures were set to 750℃, 800℃, 850℃, and 900℃, respectively. The entire reduction process was recorded using a high-speed, high-definition camera, and the data was acquired and analyzed by a computer.

[0053] Experimental results show that under different temperature conditions, sodium gradually melts and diffuses, undergoing a reduction reaction sequentially upon contact with potassium fluorotantalate, ultimately generating a dispersed product. Image data analysis shows that the system can operate stably under four temperature conditions, completely recording the entire reaction process, verifying its reliability and observational stability under different temperature environments.

[0054] Example 3

[0055] In Example 3, a sodium thermal reduction experiment was conducted using an online observation system for the sodium thermal reduction reaction, including:

[0056] The high-definition high-speed camera was used for observation experiments under two imaging parameters: a resolution of 1920×1080 and a frame rate of 500fps; and a resolution of 3840×2160 (4K) and a frame rate of 1000fps. The remaining experimental conditions were the same as in Example 2, and the experimental temperature was set at 800℃.

[0057] The results show that all key reaction processes were accurately captured under both resolution conditions, verifying that the system can stably record the entire process of sodium thermal reduction reaction and that the camera parameters can be adjusted according to experimental needs to optimize the observation effect.

[0058] Example 4

[0059] In Example 4, a sodium thermal reduction experiment was conducted using an online observation system for the sodium thermal reduction reaction, including:

[0060] The experimental temperature was set at 800℃, and all other experimental conditions were kept consistent with those in Example 2. Three consecutive experiments were conducted under the same conditions, with an interval of 1 hour between each experiment. The recording time for each experiment was 30 minutes. The entire process was recorded using a high-speed, high-definition camera, and the data was analyzed.

[0061] The results show that the image quality of the camera did not degrade under long-term operating conditions, and the data acquisition system operated stably. This demonstrates that the system can maintain stable observation capabilities even under long-term continuous operation.

[0062] The online observation system for sodium thermal reduction reaction disclosed in this embodiment of the invention can dynamically acquire image data of the reaction device, record real-time image data of the sodium thermal reduction reaction occurring in the reaction device, and further store, process and display the data through an information processing component. This facilitates the analysis and characterization of the recorded sodium thermal reduction reaction process, thereby improving the accuracy and precision of data analysis, providing direct evidence of phase changes, particle morphology evolution and reduction reaction mechanism during the reaction process, and helping to optimize the reaction process.

[0063] The technical solutions and technical details disclosed in the embodiments of this utility model are merely illustrative of the inventive concept of this utility model and do not constitute a limitation on the technical solutions of the embodiments of this utility model. Any conventional changes, substitutions or combinations made to the technical details disclosed in the embodiments of this utility model have the same inventive concept as this utility model and are within the protection scope of the claims of this utility model.

Claims

1. A system for online observation of sodium heat reduction reaction, characterized in that, The application relates to a sodium thermal reduction reaction device and a method for monitoring the sodium thermal reduction reaction. The device comprises: a reaction device with a transparent observation area for the sodium thermal reduction reaction; a high-definition high-speed camera mounted on the reaction device for obtaining image data of the sodium thermal reduction reaction through the transparent observation area; 2. The on-line observation system for sodium-thermal reduction reaction according to claim 1, wherein an information processing device connected with the high-definition high-speed camera for storing and processing the obtained image data. The reaction device comprises: a quartz crucible for setting reaction raw materials of the sodium thermal reduction reaction; a reaction furnace for setting the reaction crucible, the two sides of the reaction furnace being hollow structures, and transparent quartz glass being arranged in the hollow structures; 3. The on-line observation system for sodium-thermal reduction reaction according to claim 1, wherein a heating device arranged on the reaction furnace for heating the reaction furnace. The device further comprises:

4. The on-line observation system for sodium-thermal reduction reaction according to claim 1, wherein a wireless communication component configured to be wirelessly connected with the high-definition high-speed camera and the information processing device for wirelessly transmitting the obtained image data. The information processing device comprises: a communication component for connecting and communicating with the high-definition high-speed camera; an information processing component for receiving, storing and processing the image data; 5. The on-line observation system for sodium-thermal reduction reaction according to claim 1, wherein a display for displaying the image data. The device further comprises a gas source component for providing reaction gas to the reaction device.

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