A co-precipitation experiment integrated device

Abstract

This utility model belongs to the technical field of experimental equipment, and particularly relates to an integrated apparatus for coprecipitation experiments. Its features include a base, a high-pressure magnetically stirred reactor, a peristaltic pump feeding unit, a vacuum pump, and an inert gas storage bottle. The base is respectively equipped with a mounting slot for the high-pressure magnetically stirred reactor, the peristaltic pump feeding unit, the vacuum pump, and the inert gas storage bottle, with the inert gas storage bottle housed within the mounting slot. The peristaltic pump feeding unit is located on the rear upright plate of the base, with at least four hoppers arranged in a row. A peristaltic pump is located below each hopper. The outlet of the peristaltic pump is connected via a manifold and pipeline to the feed valve one of the high-pressure magnetically stirred reactor. The feed valve two of the high-pressure magnetically stirred reactor is connected to the vacuum pump's extraction port. The feed valve three of the high-pressure magnetically stirred reactor is connected to the outlet of the inert gas storage bottle. The beneficial effects of this utility model are: providing more experimental conditions for the preparation process and obtaining more comparative process data.

Description

Technical Field

[0001] This utility model belongs to the field of experimental equipment technology, and in particular relates to an integrated device for coprecipitation experiments. Background Technology

[0002] Coprecipitation refers to a method where a solution contains two or more cations that exist homogeneously in the solution. A precipitant is added, and after a precipitation reaction, a homogeneous precipitate of all components is obtained. This method is an important way to prepare ultrafine powders of composite oxides containing two or more metal elements. In industry, almost all bulk catalysts require precipitation during preparation. They are mostly prepared by adding a precipitant to an aqueous solution of a metal salt to form hydrated oxides or sparingly soluble and slightly soluble metal salts as crystals or gels. These crystals are then precipitated from the solution, separated, and further processed through washing, drying, and calcination.

[0003] Sodium-ion batteries have attracted much attention in the energy storage field in recent years due to their abundant resources, low cost, and safety. Among Ni / Mn-based substrate cathode materials, the triangular prism P2 type exhibits good cycle stability but low specific capacity; the octahedral O3 type has a higher specific capacity but poor cycle stability. Constructing a P2-O3 multiphase structure holds promise for utilizing the advantages of both phases. However, how to regulate and optimize the combination and distribution of the two phases to achieve synergistic enhancement, and how to suppress irreversible phase transitions under high voltage and long cycling, are challenging issues for improving their sodium storage performance.

[0004] Currently, the mainstream international method for preparing ternary cathode materials generally involves a co-precipitation reaction between soluble metal (Ni, Co, Mn) salts and soluble hydroxides (usually sodium hydroxide) to produce a ternary hydroxide precursor, which is then calcined with a lithium source. The composition, sphericity, tap density, particle size, specific surface area, and valence states of the elements in the precursor have a significant impact on the performance of the ternary cathode material. Therefore, the synthesis of the ternary cathode material precursor is the most crucial step in preparing high-performance ternary cathode materials.

[0005] Chinese utility model patent application number 201821659390.3 discloses an integrated system for chemical coprecipitation reaction used to synthesize graded functional materials. The integrated system comprises three parts: a U-shaped mixing system, a chemical coprecipitation reaction system, and a programmable control system. The U-shaped mixing system consists of a U-shaped reactor, an automatic feeding subsystem, and a stirring subsystem. The chemical coprecipitation reaction system consists of a reaction vessel, an automatic feeding subsystem, a temperature control subsystem, a stirring subsystem, an online pH detection and control subsystem, and an online ammonia detection and control subsystem. The programmable control system controls the operation of the U-shaped mixing system and the chemical coprecipitation reaction system. The U-shaped mixing system allows for continuous adjustment of the components of the chemical coprecipitation reactants, thereby synthesizing high-quality graded functional materials.

[0006] Currently, Ni / Mn-based cathode materials with P2-O3 multiphase structures require uniform and consistent phase composition and structural distribution, as well as a stable and continuous P2-O3 phase boundary structure. More experimental conditions are needed in the preparation process to provide a basis for obtaining more comparative process data. Utility Model Content

[0007] The purpose of this invention is to provide an integrated coprecipitation experimental device that overcomes the shortcomings of existing technologies. By integrating a peristaltic pump feeding unit, a vacuum pump, and an inert gas storage bottle into a small high-pressure magnetic stirring reactor, it provides more experimental conditions for the preparation process and obtains more comparative process data.

[0008] To achieve the above objectives, this utility model employs the following technical solution: An integrated coprecipitation experimental apparatus includes a base, a high-pressure magnetically stirred reactor, a peristaltic pump feeding unit, a vacuum pump, and an inert gas storage bottle. The base is equipped with a mounting slot for the high-pressure magnetically stirred reactor, the peristaltic pump feeding unit, the vacuum pump, and the inert gas storage bottle, with the inert gas storage bottle located within the mounting slot. The peristaltic pump feeding unit is located on the rear upright plate of the base, with at least four hoppers arranged in a row. Each hopper has a peristaltic pump positioned below it. The inlet of the peristaltic pump is connected to the outlet of the hopper. The outlet of the peristaltic pump is connected to the feed valve one of the high-pressure magnetically stirred reactor via a manifold and pipeline. The feed valve two of the high-pressure magnetically stirred reactor is connected to the vacuum pump's extraction port. The feed valve three of the high-pressure magnetically stirred reactor is connected to the outlet of the inert gas storage bottle.

[0009] Furthermore, the specifications of the high-pressure magnetic stirring reactor are as follows: stirring constant volume 500-1000ml, heating power 300-600W, and stirring speed 100-2000r / min.

[0010] Furthermore, the inert gas storage bottle is any one of a nitrogen bottle, an argon bottle, or a carbon dioxide bottle, with a capacity of not less than 2 liters and a pressure of not less than 12 MPa.

[0011] Furthermore, the peristaltic pump is a smart flow peristaltic pump CT1000.

[0012] Furthermore, the manifold is connected to the rear upright plate of the base, and is equipped with multiple input pipes and one output pipe. The output pipe is connected to the feed valve of the high-pressure magnetic stirring reactor through a quick connector.

[0013] Furthermore, the vacuum pump is a rotary vane laboratory vacuum pump with a specification of 2XZ-0.5.

[0014] Furthermore, the base is provided with handles on both sides for easy gripping.

[0015] Compared with the prior art, the beneficial effects of this utility model are: By integrating a peristaltic pump feeding unit, a vacuum pump, and an inert gas storage bottle into a small high-pressure magnetically stirred reactor, more experimental conditions are provided for the preparation process, more comparative process data are obtained, and the multiphase structure is optimized to form a P2-O3 phase boundary structure with uniform phase composition and structural distribution and stable continuity. Several representative doping elements were selected in a targeted manner, and the effects of single-element doping and element co-doping on the phase structure, phase boundary structure and sodium storage performance of the prepared P2-O3 multiphase Ni / Mn-based cathode material under different preparation process conditions were systematically investigated. Attached Figure Description

[0016] Figure 1 This is a schematic diagram of the structure of an embodiment of the present utility model; In the diagram: 1-base, 2-high-pressure magnetic stirring reactor, 3-peristaltic pump feeding unit, 4-vacuum pump, 5-inert gas storage bottle, 6-inert gas storage bottle placement tank, 7-rear upright plate, 8-hopper, 9-peristaltic pump, 10-manifold, 11-pipeline, 12-handle. Detailed Implementation

[0017] The technical solution of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are some embodiments of this utility model, but not all embodiments.

[0018] To more clearly illustrate the specific embodiments of this utility model or the technical solutions in the prior art, the accompanying 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 based on these drawings without creative effort. The components of the embodiments of this utility model described and shown in the accompanying drawings can typically be arranged and designed in many different configurations. Therefore, the following detailed description of the embodiments of this utility model provided in the accompanying drawings is not intended to limit the scope of the claimed utility model, but merely represents selected embodiments of the utility model.

[0019] See Figure 1This is a schematic diagram of an embodiment of the coprecipitation experimental integrated device of this utility model, including a base 1, a high-pressure magnetic stirring reactor 2, a peristaltic pump feeding unit 3, a vacuum pump 4, and an inert gas storage bottle 5. The base 1 is respectively provided with the high-pressure magnetic stirring reactor 2, the peristaltic pump feeding unit 3, the vacuum pump 4, and the inert gas storage bottle placement tank 6, and the inert gas storage bottle 5 is placed in the inert gas storage bottle placement tank 6. The peristaltic pump feeding unit 3 is located on the rear upright plate 7 of the base 1, and at least four material bins 8 are arranged in a row. A peristaltic pump 9 is provided below each material bin 8. The inlet of the peristaltic pump 9 is connected to the outlet of the material bin 8. The outlet of the peristaltic pump 9 is connected to the feed valve one of the high-pressure magnetic stirring reactor 2 through the manifold 10 and the pipeline 11. The feed valve two of the high-pressure magnetic stirring reactor 2 (not shown in the figure) is connected to the exhaust port of the vacuum pump 4. The feed valve three of the high-pressure magnetic stirring reactor 2 (not shown in the figure) is connected to the outlet of the inert gas storage bottle 5.

[0020] In this embodiment, the high-pressure magnetically stirred reactor 2 is manufactured by Zhengzhou Ruihan Company with a stirring constant of 500-1000ml, heating power of 300-600W, and a stirring speed of 100-2000r / min that is frequency-adjustable. The heating power and stirring speed can be adjusted and controlled via the control panel. The peristaltic pump 9 is a CT1000 intelligent flow-type peristaltic pump with a 3.5-inch color touchscreen display (Chinese and English), a flow rate of 0.0012-480mL / min, high flow calibration accuracy, and suitability for various applications. The inert gas storage bottle 5 can be any of a nitrogen, argon, or carbon dioxide cylinder, and can be replaced as needed. The bottom of the hopper 8 is connected to the inlet pipe of the peristaltic pump 9 via a quick connector.

[0021] The manifold 10 is connected to the rear upright plate 7 of the base 1, and has multiple input pipes and one output pipe. The output pipe is connected to the feed valve of the high-pressure magnetic stirring reactor 2 via a quick connector. The vacuum pump 4 is a rotary vane laboratory vacuum pump 4, with a specification of 2XZ-0.5 and a pumping speed of 0.5 liters / second. The base 1 has handles 12 on both sides for easy carrying, so that the device can be moved or transferred when needed.

[0022] In this embodiment of the invention, the required solutions of Ni, Mn, and other major transition metal salts, as well as Na2CO3 alkaline solution, are first poured into the silo 8. The dosage of each reagent is set according to the experimental objective. The peristaltic pump is turned on to complete the reagent addition, and the feed valve is closed. The temperature and stirring speed inside the high-pressure magnetically stirred reactor 2 are controlled as needed. The pressure inside the reactor 2 is adjusted using a vacuum pump and an inert gas storage bottle until the experiment is completed. After the material reaction is finished and the temperature drops to room temperature, the high-pressure magnetically stirred reactor 2 can be opened. The mixture is then removed for separation, washing, drying, calcination, and other processing steps, and subsequent performance verification experiments are completed. This embodiment of the device provides more experimental conditions for the preparation process, obtains more comparative process data, and optimizes the multiphase structure to form a uniform and consistent P2-O3 phase boundary structure with stable continuity. This provides experimental equipment support for the upgrading and improvement of P2-O3 multiphase Ni / Mn-based cathode materials.

[0023] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. An integrated apparatus for coprecipitation experiments, characterized in that, The system includes a base, a high-pressure magnetic stirring reactor, a peristaltic pump feeding unit, a vacuum pump, and an inert gas storage bottle. The base is equipped with a mounting slot for the high-pressure magnetic stirring reactor, the peristaltic pump feeding unit, the vacuum pump, and the inert gas storage bottle, with the inert gas storage bottle located in the mounting slot. The peristaltic pump feeding unit is located on the rear upright plate of the base, with at least four hoppers arranged in a row. Each hopper has a peristaltic pump below it. The inlet of the peristaltic pump is connected to the outlet of the hopper. The outlet of the peristaltic pump is connected to the feed valve one of the high-pressure magnetic stirring reactor via a manifold and pipeline. The feed valve two of the high-pressure magnetic stirring reactor is connected to the exhaust port of the vacuum pump. The feed valve three of the high-pressure magnetic stirring reactor is connected to the outlet of the inert gas storage bottle.

2. The integrated coprecipitation experimental apparatus according to claim 1, characterized in that, The specifications of the high-pressure magnetic stirring reactor are: stirring constant volume 500-1000ml, heating power 300-600W, and stirring speed 100-2000r / min.

3. The integrated apparatus for coprecipitation experiments according to claim 1, characterized in that, The inert gas storage bottle is any one of a nitrogen bottle, an argon bottle, or a carbon dioxide bottle, with a capacity of not less than 2 liters and a pressure of not less than 12 MPa.

4. The integrated apparatus for coprecipitation experiments according to claim 1, characterized in that, The peristaltic pump is a smart flow peristaltic pump CT1000.

5. The integrated apparatus for coprecipitation experiments according to claim 1, characterized in that, The manifold is connected to the rear upright plate of the base, and is equipped with multiple input pipes and one output pipe. The output pipe is connected to the feed valve of the high-pressure magnetic stirring reactor through a quick connector.

6. The integrated apparatus for coprecipitation experiments according to claim 1, characterized in that, The vacuum pump is a rotary vane laboratory vacuum pump with a specification of 2XZ-0.

5.

7. The integrated apparatus for coprecipitation experiments according to claim 1, characterized in that, The base has handles on both sides for easy gripping.

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