Experimental device for synthesizing selenium-doped CoZn framework material by hydrothermal method

Abstract

The utility model belongs to the technical field of experimental equipment, and particularly relates to a selenium-doped CoZn frame material hydrothermal synthesis experimental device which is characterized by comprising a base, a premixing tank, a reaction kettle and a diaphragm pump, the reaction kettle is arranged on the base, the premixing tank is arranged on a tank seat on the base, and the diaphragm pump is arranged on the premixing tank. A bottom outlet of the premixing tank is communicated with a feeding hole of the reaction kettle through a pipeline, and a diaphragm pump is arranged on the pipeline; a kettle shell of the reaction kettle is spherical, a stirring shaft is obliquely arranged in the kettle shell, and the deflection angle alpha of the stirring shaft relative to the vertical direction is 30-60 degrees; an electric heating plate, a thermometer and a pressure meter are arranged on the outer wall of the reaction kettle. The reaction kettle has the beneficial effects that the inclined stirring paddle is arranged in the spherical reaction kettle, so that solid metal ions can be prevented from being deposited at the bottom of the reaction kettle to the greatest extent, the doping uniformity can be improved to the greatest extent, an ideal selenium-doped CoZn framework material can be obtained, the reaction can be carried out smoothly, and the repeatability of an experimental process is ensured.

Description

TECHNICAL FIELD

[0001] The utility model belongs to and experimental equipment technical field, especially, it relates to a selenium doped CoZn framework material hydrothermal synthesis experimental device. BACKGROUND

[0002] Hydrothermal synthesis method refers to the method for synthesizing by chemical reaction of substances in aqueous solution under the condition of temperature of 100-1000 DEG C and pressure of 1MPa-1GPa. Under the subcritical and supercritical hydrothermal conditions, because the reaction is at the molecular level, the reaction activity is improved, so the hydrothermal reaction can replace some high-temperature solid-phase reactions. Because the homogeneous nucleation and heterogeneous nucleation mechanism of hydrothermal reaction is different from the diffusion mechanism of solid-phase reaction, new compounds and new materials that cannot be prepared by other methods can be created.

[0003] Doping is an effective method for improving the electrochemical performance of electrode materials, and anion doping can improve the electronic structure of the material and theoretically does not reduce the content of active substances. It has been proved in the prior art that selenium doping and selenium coating can improve the cycle stability of the positive electrode material.

[0004] The Chinese invention patent with application number 202211721037.4 discloses a preparation method and application of selenium-doped positive electrode material, which can improve the electronic conductivity and ion diffusion rate of high-nickel ternary positive electrode material, and the oxygen vacancies caused thereby can inhibit the formation of internal micro-cracks of particles, reduce the dissolution of transition metal ions, and thus improve the cycle performance. At the same time, selenium doping can also effectively inhibit the precipitation of lattice oxygen and improve the safety of high-nickel ternary positive electrode material electrode. The conventional hydrothermal method reaction kettle either has no stirring shaft or has a vertical stirring shaft. For the hydrothermal synthesis reaction of solid metal ions, because of uneven stirring, the problem of uneven doping has always existed in the industry, and has not been effectively solved. UTILITY MODEL CONTENT

[0005] The utility model aims at providing a selenium doped CoZn framework material hydrothermal synthesis experimental device, overcoming the defects of the prior art, adopting a spherical reaction kettle, and built-in inclined stirring paddle, so that the reaction kettle can continuously stir the reactants during the hydrothermal synthesis reaction, avoid the deposition of solid metal ions at the bottom of the reaction kettle, and maximize the uniformity of doping to obtain uniform and stable selenium-doped CoZn framework material.

[0006] To achieve the above-mentioned purpose, the utility model realizes the following technical scheme:

[0007] The application relates to a kind of selenium-doped CoZn framework material hydrothermal synthesis experimental device, including base, premixing groove, reaction kettle and diaphragm pump, the reaction kettle is arranged on the base, the premixing groove is arranged on the groove seat on the base, the bottom outlet of the premixing groove is connected with the feeding port of the reaction kettle through pipeline, and the diaphragm pump is arranged on the pipeline;The kettle shell of the reaction kettle is spherical, a stirring shaft is arranged in the reaction kettle, the stirring shaft is arranged obliquely, the angle alpha of the relative vertical direction is 30-60 DEG, the feeding port of the reaction kettle is arranged at the top of the kettle shell, the discharge port is arranged at the bottom of the kettle shell, and a polytetrafluoroethylene lining is arranged in the kettle shell;An electric heating plate, a thermometer and a pressure gauge are arranged on the outer wall of the reaction kettle.

[0008] Further, a plurality of protruding rib bodies are uniformly arranged on the inner wall of the kettle shell along the horizontal circumferential direction.

[0009] Further, the protruding rib body is a polytetrafluoroethylene strip with a triangular or circular cross section, which is welded along the shape of the inner wall.

[0010] Further, a stirring paddle is arranged on the stirring shaft, and the stirring paddle comprises a clamping frame and guide plates arranged on the left and right of the clamping frame.

[0011] Further, the kettle shell is coated with a rock wool thermal insulation layer.

[0012] Further, a stirring motor is arranged at the top of the premixing groove.

[0013] Further, the diaphragm pump is a JZM-A type mechanical diaphragm pump.

[0014] Compared with the prior art, the application has the following beneficial effects:

[0015] 1) The unique spherical reaction kettle is used, and the oblique stirring paddle is arranged in the spherical reaction kettle, so that the reaction kettle can continuously stir the reactants during the hydrothermal synthesis reaction, the deposition of solid metal ions on the bottom of the reaction kettle can be avoided to the greatest extent, the uniformity of doping can be improved to the greatest extent, and ideal selenium-doped CoZn framework material can be obtained.

[0016] 2) The spherical reaction kettle is used in combination with the diaphragm pump and the premixing groove, the electric heating plate is arranged on the outer surface of the spherical reaction kettle, the experimental conditions of the hydrothermal synthesis can be conveniently realized, the reaction can be smoothly carried out, and the repeatability of the experimental process is ensured. BRIEF DESCRIPTION OF DRAWINGS

[0017] Figure 1 is a structural schematic diagram of an embodiment of the application;

[0018] Figure 2 is Figure 1 a top view.

[0019] Figure 3 is a schematic diagram of the internal structure of the reaction kettle in the embodiment of the application.

[0020] Figure 4 is a stirring paddle structure schematic diagram of the embodiment of the utility model, and

[0021] In the drawing: 1 - base, 2 - premixing tank, 3 - reaction kettle, 4 - diaphragm pump, 5 - tank seat, 6 - pipeline, 7 - stirring shaft, 8 - discharge port, 9 - electric heating plate, 10 - thermometer, 11 - pressure gauge, 12 - rib body, 13 - stirring paddle, 14 - clamping frame, 15 - guide plate, 16 - stirring motor. DETAILED DESCRIPTION

[0022] The technical scheme of the utility model will be described clearly and completely in combination with specific embodiments, and obviously, the described embodiments are part of the embodiments of the utility model, not all the embodiments.

[0023] In order to more clearly illustrate the specific embodiment of the utility model or the technical scheme in prior art, the specific embodiments needed in the description of the specific embodiment or prior art will be simply introduced, and obviously, the specific embodiments in the following description are some embodiments of the utility model, and other specific embodiments can be obtained by those skilled in the art without creative labor on the premise of not paying creative labor.

[0024] The components of the embodiments of the utility model described and shown in the specific embodiments here can be arranged and designed in numerous different configurations. Therefore, the following detailed description of the embodiments of the utility model provided in the specific embodiments is not intended to limit the scope of the claimed utility model, but only represents selected embodiments of the utility model.

[0025] See Figures 1-4 , it is the utility model a selenium doped CoZn frame material hydrothermal synthesis experimental device embodiment structure schematic diagram, including base 1, premixing tank 2, reaction kettle 3 and diaphragm pump 4, be equipped with reaction kettle 3 on base 1, premixing tank 2 is set up on the tank seat 5 on base 1, premixing tank 2 top is equipped with stirring motor 16. The bottom outlet of premixing tank 2 is connected with the feed inlet of reaction kettle 3 through pipeline 6, and diaphragm pump 4 is arranged on the pipeline 6; The kettle shell of reaction kettle 3 is spherical, and the kettle shell is covered with rock wool insulation layer to maintain the temperature during the hydrothermal reaction. Stirring shaft 7 is arranged in the reaction kettle 3, the top end of stirring shaft 7 is connected with speed reducer, and stirring shaft 7 is arranged obliquely, and the angle α relative to the vertical direction is 30-60 °, preferably 30 °, the feed inlet of reaction kettle 3 is arranged at the top of the kettle shell, and the discharge port 8 is arranged at the bottom of the kettle shell, and the cover is arranged at the discharge port 8, and the cover is connected with the discharge port 8 through quick mounting bolt. Polytetrafluoroethylene lining is arranged in the kettle shell; The outer wall of reaction kettle 3 is provided with electric heating plate 9, thermometer 10 and pressure gauge 11, so as to realize the monitoring and control of the hydrothermal reaction process.

[0026] The diaphragm pump 4 is a JZM-A type mechanical diaphragm pump, 0MPa-8.0MPa, which functions to guide the mixture of water and reactant in the premixing tank into the reaction kettle and provide the reaction pressure of the reaction kettle.

[0027] In order to increase the mixing efficiency of the reactants, 6 protruding rib bodies 12 are evenly arranged on the inner wall of the kettle shell along the horizontal circumferential direction. The protruding rib body 12 is a polytetrafluoroethylene strip with a triangular or circular cross section welded along the shape of the inner wall.

[0028] The stirring shaft 7 is provided with a stirring paddle 13, which comprises a clamping frame 14 and a guide plate 15 arranged on the left and right of the clamping frame 14. The obliquely installed stirring shaft 7 can effectively solve the problem of material deposition, and its effect is better than that of the vertically installed stirring shaft.

[0029] Although the embodiments of the utility model have been shown and described, it can be understood by those skilled in the art that various changes, modifications, replacements and variations can be made to these embodiments without departing from the principles and spirits of the utility model, and the scope of the utility model is defined by the appended claims and their equivalents.

Claims

1. An experimental apparatus for the hydrothermal synthesis of selenium-doped CoZn framework materials, characterized in that, The system includes a base, a premixing tank, a reaction vessel, and a diaphragm pump. The reaction vessel is mounted on the base, and the premixing tank is mounted on a trough on the base. The bottom outlet of the premixing tank is connected to the feed inlet of the reaction vessel via a pipeline, and the diaphragm pump is mounted on the pipeline. The reaction vessel has a spherical shell and a stirring shaft inside. The stirring shaft is inclined, with an angle α of 30-60° relative to the vertical direction. The feed inlet of the reaction vessel is located at the top of the shell, and the discharge outlet is located at the bottom of the shell. The shell is lined with polytetrafluoroethylene. The outer wall of the reaction vessel is equipped with an electric heating plate, a thermometer, and a pressure gauge.

2. The experimental apparatus for hydrothermal synthesis of selenium-doped CoZn framework materials according to claim 1, characterized in that, Multiple protruding ribs are evenly arranged along the horizontal circumferential direction on the inner wall of the vessel shell.

3. The experimental apparatus for hydrothermal synthesis of selenium-doped CoZn framework materials according to claim 2, characterized in that, The protruding rib is formed by welding polytetrafluoroethylene strips with triangular or circular cross-sections to the shape of the inner wall.

4. The experimental apparatus for hydrothermal synthesis of selenium-doped CoZn framework materials according to claim 1, characterized in that, The stirring shaft is equipped with a stirring paddle, which includes a clamping frame and guide plates located on the left and right sides of the clamping frame.

5. The experimental apparatus for hydrothermal synthesis of selenium-doped CoZn framework materials according to claim 1, characterized in that, The outer shell of the vessel is covered with a rock wool insulation layer.

6. The experimental apparatus for hydrothermal synthesis of selenium-doped CoZn framework materials according to claim 1, characterized in that, The premix tank is equipped with a stirring motor at the top.

7. The experimental apparatus for hydrothermal synthesis of selenium-doped CoZn framework materials according to claim 1, characterized in that, The diaphragm pump is a JZM-A type mechanical diaphragm pump.

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