A solid-liquid reaction device suitable for prussian blue synthesis
By designing a solid-liquid reaction apparatus suitable for the synthesis of Prussian blue, and employing a dual-path heating and precise feeding module, the problems of high cost and poor performance in the synthesis of Prussian blue were solved, and efficient synthesis and large-scale mass production at low temperatures were achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- SHANDONG HANHANG NEW ENERGY MATERIALS CO LTD
- Filing Date
- 2025-07-14
- Publication Date
- 2026-06-09
AI Technical Summary
Existing technologies for the synthesis of Prussian blue suffer from high costs and poor performance. In particular, the large amount of complexing agent used in the liquid phase method leads to a large amount of wastewater, while the solid phase method produces materials with small particle sizes and is difficult to clean and collect, making it difficult to achieve large-scale mass production.
A solid-liquid reaction apparatus suitable for the synthesis of Prussian blue was designed, employing a dual-path heating system, a precision feeding module, and a stirring system to ensure stable temperature and uniform solid-liquid dispersion. This apparatus includes a solid chute made of breathable material and nitrogen purging, combined with a precision loss-in-weight feeder and a metering pump to achieve precise control of the reaction.
Temperature stability and uniform solid-liquid dispersion were achieved in the synthesis of Prussian blue at low temperatures, reducing costs and improving material properties, making it suitable for industrial production.
Smart Images
Figure CN224332121U_ABST
Abstract
Description
Technical Field
[0001] This utility model belongs to the technical field of battery material synthesis device, specifically relating to a solid-liquid reaction device suitable for the synthesis of Prussian blue. Background Technology
[0002] Common methods for synthesizing Prussian blue include liquid-phase and solid-phase methods. In the liquid-phase method, the reactants are dissolved and pumped into a reaction vessel in liquid form using a metering pump. A pre-added base liquid is added to the vessel, and a co-precipitation reaction occurs under stirring. However, because the reaction of Prussian blue is very rapid, to obtain high-performance Prussian blue sodium electrode materials, a large amount of complexing agent is usually added to slow down the reaction and promote crystal growth. This method results in a large amount of complexing agent in the filtrate after the reaction. The sodium salt of the complexing agent and the reactants have a common ion effect, making it impossible to completely recycle the filtrate for synthesis. Therefore, the wastewater volume is large, the amount of complexing agent used is large, and the production cost of the material is relatively high. The solid-phase synthesis method involves direct solid-phase feeding, mixing, and ball milling, without the need for water dissolution or the addition of complexing agents. The synthesis yield is very high, and the cost is relatively low. However, the Prussian blue-like materials synthesized by this method have small particle sizes, making the cleaning and collection process difficult. In addition, the electrical properties of the material are poor, far inferior to those synthesized by the liquid-phase method.
[0003] Patent CN117843017A proposes a low-cost solid-liquid preparation method for Prussian blue sodium-ion battery cathode materials. However, the synthesis temperature of Prussian blue is relatively low, and it is sensitive to temperature. Furthermore, it requires strict control of the liquid-to-solid ratio and uniform dispersion of the solid feed to ensure that the reaction can synthesize high-quality Prussian blue sodium-ion battery cathode materials. Therefore, developing a reaction device that is suitable for large-scale mass production and can guarantee the performance of material synthesis is of great significance for the industrialization of Prussian blue sodium-ion battery cathode materials. Summary of the Invention
[0004] The purpose of this invention is to provide a solid-liquid reaction apparatus suitable for the synthesis of Prussian blue. It is suitable for the low-temperature reaction of Prussian blue and ensures the stability and accuracy of the temperature during the reaction process. The uniform dispersion of solid and liquid feed ensures precise control of the reaction and produces Prussian blue product material with the same properties as the liquid-liquid method, but at a significantly lower cost. It can be directly applied to industrial production equipment.
[0005] The technical solution adopted by this utility model is:
[0006] A solid-liquid reaction apparatus suitable for the synthesis of Prussian blue, comprising:
[0007] A reaction vessel is a container used for reacting solid and liquid raw materials.
[0008] A stirring system, installed on the reactor, is used to stir solid and liquid raw materials;
[0009] A liquid feeding device, installed on the reactor, is used for feeding liquids;
[0010] A solid feed device, installed on the reactor, is used for feeding solids;
[0011] The quantitative precision feeding module is installed in the liquid feeding device and the solid feeding device to control the feed rate of the liquid feeding device and the solid feeding device.
[0012] Furthermore, the reactor is equipped with dual external coil heating, one of which is steam heating and the other is hot water heating.
[0013] Furthermore, the solid feeding device includes a solid chute, a reducing joint, a star-shaped rotary valve, and a solid feeding inlet device; the solid feeding inlet device is installed on the solid feed port of the reactor, a star-shaped rotary valve is installed between the solid feeding inlet device and the reducing joint, and the reducing joint is externally connected to the solid chute.
[0014] Furthermore, the solid chute is made of a breathable material.
[0015] Furthermore, the solid feed inlet device has multiple nitrogen gas blowing ports evenly distributed on its pipe body, and a dispersion cone is connected to the discharge end of the pipe body.
[0016] Furthermore, the liquid feeding device employs a liquid inlet pipe.
[0017] Furthermore, the quantitative precision feeding module includes a liquid feeding module and a solid feeding module; the liquid feeding module uses a metering pump or a flow meter, and the solid feeding module uses a precision loss-in-weight feeder, which is used to connect the solid chute and the solid feed port.
[0018] Furthermore, the precision loss-in-weight feeder is equipped with a nitrogen inlet above the outlet where it connects to the solid chute.
[0019] Furthermore, the solid feeding device is supported on the ground by a solid feeding bracket.
[0020] Furthermore, a baffle is installed on the outside of the liquid feed pipe located inside the reactor.
[0021] Compared with the prior art, the present invention has the following advantages:
[0022] This invention can precisely control the low-temperature reaction of Prussian blue and ensure the stability and accuracy of the temperature during the reaction process, as well as the uniform dispersion of solid and liquid feed. This precise control of the reaction yields Prussian blue products with the same properties as those produced by the liquid-liquid method, but at a significantly lower cost. It can be directly applied to industrial production facilities, greatly accelerating the industrialization process of Prussian blue. Attached Figure Description
[0023] Figure 1 This is a schematic diagram of the structure of this utility model;
[0024] Figure 2 This is a top view of the present invention;
[0025] Figure 3 This is a schematic diagram of the bottom coil of the reactor of this utility model;
[0026] Figure 4 This is a front view of the solid feed inlet device of this utility model;
[0027] Figure 5 This is a top view of the solid feed inlet device of this utility model;
[0028] Figure 6 This is a schematic diagram of the star-shaped rotary valve of this utility model;
[0029] The components include: 1. Liquid feed pipe; 2. Flow meter; 3. Hot water outlet; 4. Baffle; 5. Solid feed support; 6. Hot water inlet; 7. Pneumatic top valve; 8. Material outlet; 9. Steam inlet; 10. Steam outlet; 11. Solid feed inlet device; 12. Rotary star valve; 13. Reducing connector; 14. Precision loss-in-weight feeder; 15. Nitrogen inlet; 16. Mixing system; 17. Solid feed port; 18. Solid chute; 19. Nitrogen blowing port; 20. Dispersion cone. Detailed Implementation
[0030] To better understand the purpose, structure, and function of this utility model, a more detailed description of this utility model will be provided below with reference to the accompanying drawings.
[0031] like Figure 1 As shown, this utility model provides a solid-liquid reaction apparatus suitable for the synthesis of Prussian blue, including...
[0032] A reaction vessel is a container used for reacting solid and liquid raw materials.
[0033] The stirring system 16 is installed on the reactor and is used to stir solid and liquid raw materials;
[0034] A liquid feeding device, installed on the reactor, is used for feeding liquids;
[0035] A solid feed device, installed on the reactor, is used for feeding solids;
[0036] The quantitative precision feeding module is installed in the liquid feeding device and the solid feeding device to control the feed rate of the liquid feeding device and the solid feeding device.
[0037] like Figure 1 , Figure 3 As shown, the reactor adopts dual-circuit external coil heating. One circuit is steam heating, with a steam inlet 9 and a steam outlet 10. Steam heating is mainly used to rapidly heat the bottom liquid of the reactor to reach the reaction temperature, accelerate the production pace, and improve mass production efficiency. The other circuit is hot water heating, with a hot water inlet 6 and a hot water outlet 3. Hot water heating is mainly used for precise temperature control during the reaction to ensure the temperature stability during the low-temperature synthesis of Prussian blue.
[0038] Steam is supplied to the bottom liquid of the reactor for rapid heating. Once the bottom liquid reaches the reaction temperature, the process is switched to hot water heating to officially start the feeding reaction, ensuring the uniformity of temperature during the reaction process.
[0039] like Figure 1 As shown, the solid feeding device includes a solid chute 18, a reducing connector 13, a star-shaped rotary valve 12, and a solid feeding inlet device 11; the solid feeding inlet device 11 is installed on the solid feed port of the reactor, and a star-shaped rotary valve 12 is installed between the solid feeding inlet device 11 and the reducing connector 13, and the reducing connector 13 is externally connected to the solid chute 18.
[0040] The solid chute 18 is made of a breathable material, preferably a breathable fabric material.
[0041] like Figure 6 As shown, the star-shaped rotary valve 12 is designed to prevent a large amount of water vapor from rising from the reactor and wetting the solid pipes, causing solid materials to accumulate on the pipes and resulting in distorted feeding by the precision loss-in-weight feeder 14.
[0042] like Figure 4 , Figure 5 As shown, the solid feed inlet device 11 has multiple nitrogen blowing ports 19 evenly distributed on its pipe body, and a dispersion cone 20 is connected to the discharge end of the pipe body. With the help of the nitrogen blowing ports 19, the falling solid is dispersed into the reaction vessel. The purpose of setting the nitrogen blowing ports 19 and the dispersion cone 20 is twofold: first, to prevent water vapor from going into the solid feed channel, and second, to make the solid feed dispersion more uniform.
[0043] like Figure 1 As shown, the liquid feeding device uses a liquid feeding pipe 1.
[0044] like Figure 1 , Figure 2As shown, the quantitative precision feeding module includes a liquid feeding module and a solid feeding module. The liquid feeding module uses a metering pump or a flow meter 2. The liquid is fed automatically by a high-precision metering pump or a high-precision flow meter 2 in conjunction with a conveying pump, preferably a mass flow meter. Both the metering pump and the flow meter 2 are connected to the liquid inlet pipe 1. The solid feeding module uses a precision loss-in-weight feeder 14. The precision loss-in-weight feeder 14 is used to connect the solid chute 18 and the solid feed port 17.
[0045] like Figure 1 As shown, a nitrogen inlet 15 is provided above the outlet where the precision loss-in-weight feeder 14 connects to the solid chute 18. The purpose is to prevent a small amount of water vapor in the reactor from entering the screw of the precision loss-in-weight feeder and causing it to clump together with the material, thereby affecting the accuracy of the solid feeding equipment.
[0046] like Figure 1 , Figure 2 As shown, the precision loss-in-weight feeder 14 of the solid feeding device needs to be independently supported on the ground by the solid feeding bracket 5. This is to prevent other vibration sources from interfering with the accuracy of the solid loss-in-weight feeding, thereby isolating vibration sources and ensuring the accuracy of solid feeding.
[0047] like Figure 1 As shown, a baffle 4 is installed on the outside of the liquid feed pipe 1 inside the reactor.
[0048] The bottom of the reactor is provided with a material outlet 8, and a pneumatic upward valve 7 is installed at the material outlet 8.
[0049] It is understood that this utility model has been described through some embodiments, and those skilled in the art will recognize that various changes or equivalent substitutions can be made to these features and embodiments without departing from the spirit and scope of this utility model. Furthermore, under the teachings of this utility model, these features and embodiments can be modified to adapt to specific situations and materials without departing from the spirit and scope of this utility model. Therefore, this utility model is not limited to the specific embodiments disclosed herein, and all embodiments falling within the scope of the claims of this application are within the protection scope of this utility model.
Claims
1. A solid-liquid reaction apparatus suitable for the synthesis of Prussian blue, characterized in that: include A reaction vessel is a container used for reacting solid and liquid raw materials. A stirring system (16) is installed on the reactor and is used to stir solid and liquid raw materials; A liquid feeding device, installed on the reactor, is used for feeding liquids; A solid feed device, installed on the reactor, is used for feeding solids; The quantitative precision feeding module is installed in the liquid feeding device and the solid feeding device to control the feed rate of the liquid feeding device and the solid feeding device.
2. The solid-liquid reaction apparatus for the synthesis of Prussian blue according to claim 1, characterized in that: The reactor is heated by a dual-circuit external coil, one circuit being steam heating and the other being hot water heating.
3. The solid-liquid reaction apparatus for the synthesis of Prussian blue according to claim 1, characterized in that: The solid feeding device includes a solid chute (18), a reducing joint (13), a star-shaped rotary valve (12), and a solid feeding inlet device (11). The solid feeding inlet device (11) is installed on the solid feed port of the reactor. A star-shaped rotary valve (12) is installed between the solid feeding inlet device (11) and the reducing joint (13). The reducing joint (13) is externally connected to the solid chute (18).
4. A solid-liquid reaction apparatus suitable for the synthesis of Prussian blue according to claim 3, characterized in that: The solid chute (18) is made of a breathable material.
5. A solid-liquid reaction apparatus suitable for the synthesis of Prussian blue according to claim 4, characterized in that: The solid feed inlet device (11) has multiple nitrogen blowing ports (19) evenly distributed on its pipe body, and a dispersion cone (20) is connected to the discharge end of the pipe body.
6. A solid-liquid reaction apparatus for the synthesis of Prussian blue according to claim 3, characterized in that: The liquid feeding device uses a liquid feeding pipe (1).
7. A solid-liquid reaction apparatus suitable for the synthesis of Prussian blue according to claim 4, characterized in that: The quantitative precision feeding module includes a liquid feeding module and a solid feeding module; the liquid feeding module uses a metering pump or a flow meter (2), and the solid feeding module uses a precision loss-in-weight feeder (14), which is connected to a solid feed port (17) via a solid chute (18).
8. A solid-liquid reaction apparatus for the synthesis of Prussian blue according to claim 7, characterized in that: The precision loss-in-weight feeder (14) is equipped with a nitrogen inlet (15) above the outlet where it connects to the solid chute (18).
9. A solid-liquid reaction apparatus for the synthesis of Prussian blue according to claim 1, characterized in that: The solid feeding device is supported on the ground by a solid feeding bracket (5).
10. A solid-liquid reaction apparatus for the synthesis of Prussian blue according to claim 6, characterized in that: A baffle (4) is installed on the outside of the liquid feed pipe (1) located inside the reactor.