A reaction kettle
By designing multiple reaction tanks and feed pipes in the reactor, the slow growth of raw materials is achieved, and the structural defects of Prussian blue precipitation in traditional reactors are solved, and the quality and performance of the material are improved.
Patent Information
- Application Number
- CN202421361955.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-06-14
- Publication Date
- 2025-04-04
- Estimated Expiration
- 2034-06-14
AI Technical Summary
When existing reactors precipitate Prussian blue, they often have >10% Fe(CN)6 structural defects, which affect their ion storage and cycling performance.
A reactor is designed, including multiple reaction tanks and feed tubes, which can slowly grow the raw material by electrostatic adsorbing ions with opposite charges, avoiding material vacancy or defects caused by rapid precipitation.
Low defect precipitation of Prussian blue particles is achieved, and its ion storage and cycling performance are improved.
Smart Images

Figure CN222709645U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of chemical reaction devices, in particular to a reaction kettle. Background Art
[0002] A reactor is a container for physical or chemical reactions. Through the structural design and parameter configuration of the container, the heating, evaporation, cooling and low-speed mixing functions required by the process are achieved.
[0003] The existing reactor includes a reaction chamber, a feed port is provided above the reaction chamber, and a stirring device is provided in the reaction chamber. When the Prussian blue is prepared by the existing reactor precipitation method, there are often more than 10% of Fe(CN)6 structural defects. These Fe(CN)6 structural defects will seriously affect the ion storage performance of Prussian blue. Due to the lack of Fe(CN)6, the lattice is prone to chemical bond breakage, lattice distortion or structural collapse during the ion insertion and extraction process, resulting in the attenuation of the cycle performance; at the same time, the unsaturated coordination bonds at the defects will attract a large number of water molecules for coordination, and the oxidative decomposition of water molecules at high potential will lead to a decrease in coulomb efficiency; and the lattice water molecules occupy part of the ion embedding sites, blocking the ion transmission channel, resulting in the deterioration of the material rate performance. The reason for the defects is that the rapid precipitation of the traditional reactor will lead to material vacancies or defects, which needs to be improved. Utility Model Content
[0004] The utility model aims to provide a reaction kettle which can slow down the precipitation speed of raw materials and improve the quality of products.
[0005] The utility model proposes a reaction kettle, comprising a kettle body, a cover plate, a power mechanism, a stirring device, and a plurality of reaction tanks; the cover plate is installed on the top end of the kettle body, and a discharge port is arranged at the bottom end of the kettle body; a plurality of feeding pipes for adding raw materials into the reaction tanks are arranged through the cover plate; the power mechanism is fixedly arranged on the cover plate; the stirring device is located at the center position of the kettle body, and the stirring device is connected to the power mechanism and rotates under the action of the power mechanism; the plurality of reaction tanks are fixedly arranged above the inner side wall of the kettle body, the bottom of the reaction tank is provided with an opening, and the reaction tanks are arranged one by one with the feeding pipes on the cover plate.
[0006] Preferably, the stirring device comprises a stirring shaft and a three-layer stirring paddle arranged on the stirring shaft, and the three-layer stirring paddle comprises an anchor blade, a propeller blade and an inclined blade arranged in sequence from the bottom end to the top end.
[0007] Preferably, the upper end surface of the reaction tank is higher than the inclined blade, and the lower end surface of the reaction tank is located between the propulsion blade and the inclined blade.
[0008] Preferably, the opening at the bottom of the reaction tank is configured as a semi-open spiral opening.
[0009] Preferably, the anchor blade comprises an anchor connecting blade and a transverse blade, the middle portion of the anchor connecting blade is connected to the bottom end of the stirring shaft, the two sides of the upper end of the anchor connecting blade are connected to the transverse blade, and the middle portion of the transverse blade is fixed on the stirring shaft;
[0010] The propulsion blades include a plurality of disc-shaped blades uniformly arranged on the stirring shaft, and the angle between the disc-shaped blades and the horizontal plane is C, and 0°<C<60° is satisfied;
[0011] The inclined blades include a plurality of inclined blades uniformly arranged on the stirring shaft, and the angle between the inclined blades and the horizontal plane is T, which satisfies 10°<T<90°.
[0012] Preferably, the inner diameter of the kettle is L, then the diameter D of the anchor blade satisfies 1 / 2L<D<2 / 3L; the diameter W of the propulsion blade satisfies 1 / 3L<W<1 / 2L; and the diameter S of the inclined blade satisfies 1 / 4L<S<1 / 2L.
[0013] Preferably, there are two reaction tanks, namely a first reaction tank and a second reaction tank;
[0014] The feed pipes are provided with two, namely a first feed pipe and a second feed pipe;
[0015] The relationship between the height dimension h of the first reaction tank and the second reaction tank and the height dimension H of the kettle body is: 1 / 3H<h<1 / 2H;
[0016] The relationship between the diameter size N of the first reaction tank and the second reaction tank and the inner diameter size L of the kettle body is: 1 / 6L <N<1 / 5L。
[0017] Preferably, the bottom end of the kettle body is arranged as a U-shaped bottom, a sealing head is arranged at the center of the bottom end of the kettle body, and a pair of hanging ears are fixedly arranged on the outer side of the kettle body.
[0018] Preferably, a nitrogen pipe is provided through the cover plate, the nitrogen pipe extends into the kettle body, and the bottom end of the nitrogen pipe is located at the lower part of the kettle body.
[0019] Preferably, the power mechanism is a motor reducer with a rotation speed of 0-528 rpm and a linear speed of 0-800 cm / s.
[0020] From the above description of the utility model, it can be seen that the utility model has the following beneficial effects:
[0021] 1. The utility model sets up multiple reaction tanks, and drips raw materials into each reaction tank through a feed pipe, thereby creating a reaction area for the raw materials, which is suitable for the reaction process of chemical substances such as Prussian blue particles. The raw materials grow slowly in the reaction tank by electrostatically adsorbing ions of opposite charges, avoiding material vacancies or defects caused by rapid precipitation in traditional reactors, achieving controllable regulation of Prussian blue particle precipitation, and preparing low-defect Prussian blue materials.
[0022] 2. The bottom of the kettle is set as a U-shaped bottom, and a head is set at the center of the bottom of the kettle to reduce the accumulation of materials at the bottom and improve the mixing and dispersion effect of the slurry.
[0023] 3. A nitrogen pipe is vertically arranged in the kettle body, and the nitrogen pipe passes through the cover plate. Nitrogen can be added into the kettle body through the nitrogen pipe to drive away the oxygen on the surface of the solution, reduce the solubility of oxygen, and thus reduce the oxidation and decomposition of water molecules under high potential, thereby promoting the reaction. BRIEF DESCRIPTION OF THE DRAWINGS
[0024] Figure 1 It is a schematic diagram of the overall structure of a reactor in an embodiment;
[0025] Figure 2 is a schematic structural diagram of the first reaction tank of the embodiment;
[0026] Figure 3 Schematic diagram of the dimensions of the kettle body, the first reaction tank and the second reaction tank of the embodiment;
[0027] Figure 4 is a schematic diagram of the dimensions of an anchor blade, a propeller blade, and a canted blade in an embodiment;
[0028] Figure 5 It is a schematic diagram of the structures of the anchor blade, the propulsion blade and the tilted blade in the embodiment.
[0029] Figure numerals: 1, kettle body; 11, head; 12, discharge port; 13, ear; 14, nitrogen pipe; 2, cover plate; 21, first feed pipe; 22, second feed pipe; 3, power mechanism; 4, first reaction tank; 41, opening; 5, second reaction tank; 6, stirring device; 61, anchor blade; 611, transverse blade; 612, anchor connecting blade; 62, propulsion blade; 621, disc blade; 63, inclined blade; 631, inclined blade; 64, stirring shaft. DETAILED DESCRIPTION
[0030] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present invention clearer and more understandable, the following is a summary of the technical problems, technical solutions and beneficial effects to be solved by the present invention. Figure 1-5It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.
[0031] Reference Figure 1 , Figure 2 and Figure 3 A reactor comprises a reactor body 1, a cover plate 2, a power mechanism 3, a stirring device 6 and two reaction tanks, wherein the two reaction tanks are a first reaction tank 4 and a second reaction tank 5, respectively. The first reaction tank 4 and the second reaction tank 5 are respectively arranged on opposite inner side walls of the reactor body 1, the cover plate 2 is covered on the top of the reactor body 1, the power mechanism 3 is fixedly arranged on the cover plate 2, and the rotating shaft of the power mechanism 3 is vertically penetrated into the reactor body 1, and the stirring device 6 is fixedly arranged on the rotating shaft of the power mechanism 3, so that the stirring device 6 is driven to work by the power mechanism 3.
[0032] The kettle 1 is filled with slurry, and the bottom of the kettle 1 is set to a U-shaped bottom, and a head 11 is set at the center of the bottom of the kettle 1 to prevent the slurry from accumulating at the center of the bottom of the kettle 1, thereby improving the mixing and dispersion effect of the slurry. A discharge port 12 is formed at the bottom of the kettle 1, and a pair of hanging ears 13 are fixedly set on the outside of the kettle 1. The kettle 1 is placed on a stainless steel platform through the hanging ears 13 on both sides, so that the bottom of the kettle 1 is suspended, so as to facilitate the discharge of the discharge port 12 at the bottom of the kettle 1 and the cleaning of the inside of the kettle 1.
[0033] The bottom ends of the first reaction tank 4 and the second reaction tank 5 are both set as semi-open spiral openings 41, that is, the bottom ends of the first reaction tank 4 and the second reaction tank 5 are set as spiral-shaped channels, and the opening 41 is located on the lowermost side at the bottom ends of the first reaction tank 4 and the second reaction tank 5. Through the design of the semi-spiral opening, the reaction raw materials entering the first reaction tank and the second reaction tank slowly flow into the opening 41 through the spiral-shaped channels at the bottom ends. Set the diameter size of the kettle body 1 as "L", set the diameter sizes of the first reaction tank 4 and the second reaction tank 5 as "N", and satisfy 1 / 6L < N < 1 / 5L; set the height sizes of the first reaction tank 4 and the second reaction tank 5 as "h", and set the height size of the kettle body 1 as "H", and make the relationship between the height sizes of the first reaction tank 4 and the second reaction tank 5 and the height size of the kettle body 1 satisfy 1 / 3H < h < 1 / 2H, so as to make the height sizes of the first reaction tank 4 and the second reaction tank 5 match the height size of the kettle body 1. To facilitate the addition of reaction raw materials into the kettle body 1, two feed pipes are vertically arranged through the cover plate 2. The two feed pipes are the first feed pipe 21 and the second feed pipe 22 respectively. Among them, the first feed pipe 21 is located directly above the first reaction tank 4, and the second feed pipe 22 is located directly above the second reaction tank 5; sodium ferrocyanide is dripped into the first reaction tank 4 through the first feed pipe 21, and metal sulfate is dripped into the second reaction tank 5 through the second feed pipe 22.
[0034] Referring to Figure 1 , Figure 4 and Figure 5 , the stirring device 6 includes a stirring shaft 64 and three layers of stirring paddles. The three layers of stirring paddles are respectively an anchor paddle 61, a propeller paddle 62 and an inclined paddle 63. Set the power mechanism 3 as a motor reducer, vertically fix the stirring shaft 64 on the rotating shaft of the motor reducer, and the anchor paddle 61, the propeller paddle 62 and the inclined paddle 63 are all fixedly arranged on the stirring shaft 64 respectively. The stirring speed of the motor reducer is set to 0 - 528 rpm, and the linear velocity of the stirring paddle is 0 - 800 cm / s, so as to keep the slurry in the kettle body 1 at a relatively high reaction rate.
[0035] Among them, the anchor paddle 61 is fixedly arranged at the bottom end of the stirring shaft 64, the propeller paddle 62 is fixedly arranged in the middle of the stirring shaft 64, and the inclined paddle 63 is fixedly arranged at the top end of the stirring shaft 64. Set the diameter size of the anchor paddle 61 as "D", and make the relationship between the diameter size of the anchor paddle 61 and the diameter size of the kettle body 1 satisfy 1 / 2L < D < 2 / 3L. The anchor paddle 61 includes an anchor connecting blade 612 and a cross paddle 611. The middle of the anchor connecting blade 612 is fixedly connected to the bottom end of the stirring shaft 64, both sides of the upper end of the anchor connecting blade 612 are connected to the cross paddle 611, and the middle of the cross paddle 611 is fixed on the stirring shaft 64; the slurry in the kettle body 1 has a good mixing effect through the stirring of the anchor paddle 61.
[0036] Set the diameter dimension of the propeller blade 62 to "W", and make the relationship between the diameter dimension of the propeller blade 62 and the diameter dimension of the kettle body 1 satisfy 1 / 3L < W < 1 / 2L. The propeller blade 62 includes a number of disc-shaped blades 621. After the propeller blade 62 is fixedly arranged on the rotating shaft of the stirring shaft 64, each disc-shaped blade 621 is arranged around the circumference of the stirring shaft 64. Set the angle between the disc-shaped blade 621 and the horizontal plane to "C", and make the angle size between the disc-shaped blade 621 and the horizontal plane satisfy 0° < C < 60°. The position where the propeller blade 62 is arranged is between the bottom ends of the first reaction tank 4 and the second reaction tank 5. By stirring with the propeller blade 62, a weak radial shear force is provided, so that the slurry flow enters and exits the first reaction tank 4 and the second reaction tank 5 from top to bottom.
[0037] Set the diameter dimension of the inclined blade 63 to "S", and make the relationship between the diameter dimension of the inclined blade 63 and the dimension of the kettle body 1 satisfy 1 / 4L < S < 1 / 2L; set the inclined blade 63 to include a number of inclined blades 631, and set the angle between the inclined blade 631 and the horizontal plane to "T", and satisfy 10° < T < 90°. By arranging the inclined blade 631 to be inclined with the horizontal plane, the inclined blade 631 can provide an appropriate shear force to the slurry, so that the crystallinity of the particles in the slurry is improved in the final stage of precipitation, the sphericity is increased, and the particle size distribution of the particles tends to be concentrated.
[0038] During the reaction process, since the unsaturated coordination bonds at the defect sites will attract a large number of water molecules to coordinate, and the oxidation and decomposition of water molecules during battery charging at high potentials will cause the Coulomb efficiency to decrease. In order to reduce the oxidation and decomposition of water molecules in the charged state of the battery. A nitrogen gas pipe 14 is vertically arranged in the kettle body 1, and one end of the nitrogen gas pipe 14 passes through the cover plate 2, and nitrogen gas can be added to the kettle body 1 through the nitrogen gas pipe 14; introducing nitrogen gas into the kettle body 1 can drive away the oxygen on the surface of the solution, reduce the solubility of oxygen, thereby reducing the number of defects and coordinated water in the Prussian blue material itself, avoiding the oxidation and decomposition of water molecules at high charging states, improving the Coulomb efficiency of the battery, and avoiding the situation of battery swelling.
[0039] The specific implementation principle of the embodiment of the present application is: when the liquid level in the kettle body 1 has not reached the lower end of the C-shaped groove, sodium ferrocyanide enters the first reaction tank 4 through the first feed pipe 21, and metal sulfate enters the second reaction tank 5 through the second feed pipe 22. The rotating shaft of the power mechanism 3 rotates to drive the anchor blade 61 to rotate, so that the slurry, sodium ferrocyanide and metal sulfate are uniformly mixed and reacted to form ordinary Prussian blue cubic crystal blocks.
[0040] When the liquid level in the kettle body 1 exceeds the bottom of the first reaction tank 4 and the second reaction tank 5, the propulsion blade 62 rotates to drive the liquid slurry to form two vortices in the first reaction tank 4 and the second reaction tank 5. With the continuous addition of sodium ferrocyanide in the first reaction tank 4 and metal sulfate in the second reaction tank 5, a restricted reaction zone is formed in the first reaction tank 4 and the second reaction tank 5. The vortices in the first reaction tank 4 and the second reaction tank 5 allow the cubic particles to form crystal particles with surface ferrocyanide and metal ion enrichment. Subsequently, the crystals of Prussian blue (negatively charged on the surface) with excess ferrocyanide and Prussian blue (positively charged on the surface) with excess metal ions flow back to the kettle body 1 from the bottom of the first reaction tank 4 and the second reaction tank 5 respectively. And each grows in the first reaction tank 4 and the second reaction tank 5 by electrostatically adsorbing ions of opposite charges. In the process of such reciprocating flow, the assembly and layer-by-layer growth of Prussian blue crystal particles are completed. Since the growth process of each layer of the crystal particles is through electrostatic adsorption in the enriched area with opposite surface charge, it is not easy to produce rapid disordered precipitation and a large number of vacancy defects caused by simultaneous feeding in the same area in conventional reactions, so low-defect Prussian blue materials can be obtained in the liquid phase reaction stage.
[0041] When the liquid level reaches the inclined blade 63, the growth rate of the Prussian blue particles slows down. The radial shearing and axial mixing effects are optimized by the angle design of the inclined blade 631, the particle size distribution of the crystal particles tends to be concentrated, and the crystallinity and sphericity are improved, thereby improving the vibration and compaction density and electrochemical properties, thereby realizing the preparation of low-defect Prussian blue materials.
[0042] The utility model is described above by way of example in conjunction with the accompanying drawings. It is obvious that the specific implementation of the utility model is not limited to the above-mentioned method. As long as various non-substantial improvements are made using the method concept and technical solution of the utility model, or the concept and technical solution of the utility model are directly applied to other occasions without improvement, they are all protected by the utility model.
Claims
1. A reaction kettle, characterized in that: It includes a kettle body, a cover plate, a power mechanism, a stirring device, and a plurality of reaction tanks; The cover plate is installed on the top of the kettle body, and a discharge port is arranged at the bottom of the kettle body; a plurality of feed pipes for adding raw materials into the reaction tank are arranged through the cover plate; The power mechanism is fixedly arranged on the cover plate; The stirring device is located at the center of the kettle body, and is connected to the power mechanism and rotates under the action of the power mechanism; The multiple reaction grooves are fixedly arranged above the inner side wall of the kettle body, the bottom of the reaction grooves is provided with openings, and the reaction grooves are arranged in one-to-one correspondence with the feeding pipes on the cover plate.
2. A reaction kettle according to claim 1, characterized in that: The stirring device comprises a stirring shaft and a three-layer stirring paddle arranged on the stirring shaft, wherein the three-layer stirring paddle comprises an anchor blade, a propulsion blade and an inclined blade which are arranged in sequence from the bottom end to the top end.
3. A reaction kettle according to claim 2, characterized in that: The upper end surface of the reaction tank is higher than the inclined blade, and the lower end surface of the reaction tank is located between the propulsion blade and the inclined blade.
4. A reactor according to any one of claims 1 to 3, characterized in that: The opening at the bottom of the reaction tank is configured as a semi-open spiral opening.
5. A reaction kettle according to claim 2, characterized in that: The anchor blade includes an anchor connection blade and a transverse blade, the middle of the anchor connection blade is connected to the bottom end of the stirring shaft, the two sides of the upper end of the anchor connection blade are connected to the transverse blade, and the middle of the transverse blade is fixed on the stirring shaft; The propulsion blades include a plurality of disc-shaped blades uniformly arranged on the stirring shaft, and the angle between the disc-shaped blades and the horizontal plane is C, and 0°<C<60° is satisfied; The inclined blades include a plurality of inclined blades uniformly arranged on the stirring shaft, and the angle between the inclined blades and the horizontal plane is T, which satisfies 10°<T<90°.
6. A reaction kettle according to claim 5, characterized in that: The inner diameter of the kettle body is L, then the diameter D of the anchor blade satisfies 1 / 2L<D<2 / 3L; the diameter W of the propulsion blade satisfies 1 / 3L<W<1 / 2L; the diameter S of the inclined blade satisfies 1 / 4L<S<1 / 2L.
7. A reaction kettle according to claim 1, characterized in that: There are two reaction tanks, namely the first reaction tank and the second reaction tank; there are two feed pipes, namely the first feed pipe and the second feed pipe; The relationship between the height dimension h of the first reaction tank and the second reaction tank and the height dimension H of the kettle body is: 1 / 3H<h<1 / 2H; The relationship between the diameter size N of the first reaction tank and the second reaction tank and the inner diameter size L of the kettle body is: 1 / 6L <N<1 / 5L。 8. A reaction kettle according to claim 1, characterized in that: The bottom end of the kettle body is arranged as a U-shaped bottom, a sealing head is arranged at the center of the bottom end of the kettle body, and a pair of hanging ears are fixedly arranged on the outer side of the kettle body.
9. A reaction kettle according to claim 1, characterized in that: A nitrogen pipe is provided through the cover plate, and the nitrogen pipe extends into the kettle body, and the bottom end of the nitrogen pipe is located at the lower part of the kettle body.
10. A reaction kettle according to claim 1, characterized in that: The power mechanism is a motor reducer with a rotation speed of 0 to 528 rpm and a linear speed of 0 to 800 cm / s.