A system for continuously producing a lithium phosphate product
Patent Information
- Application Number
- CN202521240084.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-17
- Publication Date
- 2026-08-21
- Estimated Expiration
- 2035-06-17
AI Technical Summary
传统工艺中，反应完成后通常采用板框压滤或离心分离，这些方法能耗高、操作不连续且滤饼含水率高，后续干燥能耗大
[0013]有益效果：与现有技术相比，本实用新型的优点为：该磷酸锂产品制备的新系统，通过基于微通道反应器以及分离装置的基础上，集成MVR装置，并针对由硫酸锂和磷酸铵反应生成磷酸锂沉淀的特定工艺，通过将微通道反应器、分离装置以及MVR装置三者进行布设，不仅能够有效缓解于微通道反应器内的磷酸锂沉淀沉积于微通道反应器内，且能够进行充分反应，提高磷酸锂的品质和产量。
Smart Images
Figure CN224656730U_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of systems for the continuous preparation of lithium phosphate products. Background Technology
[0002] Lithium phosphate, as an important inorganic compound, has wide applications in lithium-ion battery cathode materials, catalyst supports, and specialty glasses. Traditional lithium phosphate production processes primarily employ batch reactors; however, this traditional process suffers from numerous technical bottlenecks, such as difficulty in precisely controlling the reaction process; concentrated heat release leading to substandard product parameters; and the need for prolonged settling and separation after the reaction, resulting in low production efficiency. Currently, there is no mature continuous lithium phosphate production technology, especially an integrated system capable of simultaneously addressing key issues such as reaction control and solid-liquid separation. In traditional processes, plate and frame filtration or centrifugation are typically used after the reaction, but these methods are energy-intensive, discontinuous, and result in high moisture content in the filter cake, leading to significant energy consumption for subsequent drying. These problems severely restrict technological advancements and industrial upgrading in lithium phosphate production.
[0003] Based on this, a system for the continuous preparation of lithium phosphate products using a microchannel reactor to achieve precise control of the reaction process is provided. Utility Model Content
[0004] Purpose of the utility model: This utility model provides a new system for preparing lithium phosphate products based on a microchannel reactor, which improves the quality of lithium phosphate products and realizes green production.
[0005] Technical solution: The present invention provides a system for the continuous preparation of lithium phosphate products. The system includes a microchannel reactor that is connected to both a lithium sulfate storage tank and an ammonium phosphate storage tank to react and generate lithium phosphate, a first centrifuge device connected to the discharge port of the microchannel reactor, and an MVR device connected to the mother liquor discharge port of the first centrifuge device.
[0006] The MVR device is also connected to a lithium phosphate concentrate mother liquor storage tank. The inlet port of the lithium phosphate concentrate mother liquor storage tank is connected to the outlet port of the MVR device, and the outlet port of the lithium phosphate concentrate mother liquor storage tank is cyclically connected to the inlet port of the microchannel reactor.
[0007] Furthermore, the system for continuously preparing lithium phosphate products according to this utility model includes a microchannel reactor that is connected to both a lithium sulfate storage tank and an ammonium phosphate storage tank to react and generate lithium phosphate, a first centrifuge device connected to the discharge port of the microchannel reactor, and an MVR device connected to the mother liquor discharge port of the first centrifuge device.
[0008] The MVR device is also connected to a lithium phosphate concentrate mother liquor reaction tank. The inlet port of the lithium phosphate concentrate mother liquor reaction tank is connected to the outlet port of the MVR device and the outlet port of the ammonium phosphate storage tank, respectively. A second centrifuge device is connected to the outlet port of the lithium phosphate concentrate mother liquor reaction tank.
[0009] Furthermore, the solid discharge port of the first centrifugal device of the system is connected to a drying and packaging machine to obtain lithium phosphate products.
[0010] Furthermore, the MVR device of this system is also equipped with a steam condensate storage tank. The inlet port of the steam condensate storage tank is connected to the condensate outlet port of the MVR device, and the outlet port of the steam condensate storage tank is circulated to the microchannel reactor.
[0011] Furthermore, the liquid outlet of the second centrifuge device of the system is connected to a secondary lithium phosphate mother liquor storage tank, and the solid discharge port of the second centrifuge device is circulated to the drying and packaging machine through a pipeline.
[0012] Furthermore, the outlet port of the secondary lithium phosphate mother liquor storage tank of the system is cyclically connected to the inlet port of the microchannel reactor.
[0013] Beneficial effects: Compared with the prior art, the advantages of this utility model are as follows: This new system for preparing lithium phosphate products integrates an MVR device based on a microchannel reactor and a separation device. Targeting the specific process of generating lithium phosphate precipitate from the reaction of lithium sulfate and ammonium phosphate, the arrangement of the microchannel reactor, separation device, and MVR device not only effectively alleviates the deposition of lithium phosphate precipitate within the microchannel reactor but also ensures sufficient reaction, thereby improving the quality and yield of lithium phosphate. Attached Figure Description
[0014] Figure 1 This is a schematic diagram of the system for the continuous preparation of lithium phosphate products according to this invention. Figure 1 ;
[0015] Figure 2 This is a schematic diagram of the system for the continuous preparation of lithium phosphate products according to this invention. Figure 2 . Detailed Implementation
[0016] The technical solution of this utility model will be further described in detail below with reference to the accompanying drawings.
[0017] It should be noted that all components used in this utility model system are known in the art. For example, the microchannel reactor used can be an MT reactor. The centrifuge device can be a scraper centrifuge (vertical Φ1250). The MVR device is a double-effect MVR evaporator. The reaction tank is a reaction vessel, etc., known in the art. The drying and packaging machine can be a DCS-1000-T.
[0018] The system of this invention is used for the continuous preparation of lithium phosphate products, such as... Figure 1 As shown, the system includes storage tanks for storing lithium sulfate and ammonium phosphate separately, namely lithium sulfate tank 1 and ammonium phosphate tank 2, and a microchannel reactor 3 connected to these two raw material tanks for reaction to produce lithium phosphate. The raw materials, ammonium phosphate and lithium sulfate, are filtered separately and then fed into their respective storage tanks, and then proportionally delivered to the microchannel reactor 3 via metering pumps. The microchannels of the microchannel reactor 3 have excellent heat and mass transfer characteristics, preventing excessive temperature buildup and precisely controlling the reaction temperature within a certain range, which is beneficial to the quality of the lithium phosphate product and ensures high safety. The multi-channel structure, with each channel acting as an independent reactor, eliminates the need for scale-up reactors during production expansion; simply increasing the number of reactors in parallel simplifies operation. The system is based on the direct connection of the microchannel reactor 3 to the lithium sulfate tank 1 and ammonium phosphate tank 2, enabling continuous reaction of the pumped raw materials within the tanks, thus forming a continuous product preparation process.
[0019] The suspension generated in the microchannel reactor 3 undergoes primary separation. Specifically, a first centrifuge 4 is connected to the outlet port of the microchannel reactor 3. The solid lithium phosphate obtained after separation by the first centrifuge 4 is discharged from the solid outlet port. A drying and packaging machine 9 is connected to this solid outlet port to obtain the lithium phosphate product through drying and packaging. An MVR device 5 is connected to the mother liquor outlet port of the first centrifuge 4. The lithium phosphate mother liquor obtained after separation by the first centrifuge 4 is concentrated by the MVR device 5, increasing the lithium concentration and causing ammonium sulfate to crystallize out as salt, thereby obtaining solid ammonium sulfate and concentrated lithium phosphate mother liquor (saturated ammonium sulfate and lithium solution).
[0020] The concentrated mother liquor of lithium phosphate is continuously stored in the concentrated mother liquor storage tank 6, which is connected to the outlet port of the MVR device 5. The outlet port of the storage tank is circulated to the inlet port of the microchannel reactor 3 through a connecting pipe. On the one hand, the lithium ions in the concentrated mother liquor of lithium phosphate react with the ammonium phosphate solution in the microchannel reactor 3 again. On the other hand, the concentrated mother liquor of lithium phosphate can be continuously replenished to flush the lithium phosphate precipitate generated in the microchannel reactor 3, so as to prevent the generated lithium phosphate precipitate from depositing in the microchannel reactor 3.
[0021] Simultaneously, a steam condensate storage tank 10 is connected to the MVR device 5, and the inlet port of the steam condensate storage tank 10 is connected to the condensate outlet port of the MVR device 5. The outlet port of the steam condensate storage tank 10 is circulated to the microchannel reactor 3. Using the condensate in the steam condensate storage tank 10, after all the raw materials in the lithium sulfate storage tank 1 and the ammonium phosphate storage tank 2 have reacted, the PLC control system can regulate the condensate in the steam condensate storage tank 10 to circulate water through the microchannel reactor 3 again, preventing the lithium phosphate precipitate generated in the final reaction from depositing inside the microchannel reactor 3, thus achieving the function of flushing the microchannel reactor 3.
[0022] The above system improves yield by recirculating the concentrated lithium phosphate mother liquor back into the microchannel reactor 3. Furthermore, based on the above system setup, it can be further optimized to achieve the same goal of increasing yield.
[0023] Specifically, such as Figure 2 As shown, the system includes a microchannel reactor 3 connected to both a lithium sulfate storage tank 1 and an ammonium phosphate storage tank 2. The outlet port of the microchannel reactor 3 is connected to a first separation device 4. The suspension generated by the reaction is separated by the first separation device 4 to obtain ammonium phosphate solids and lithium phosphate mother liquor. The outlet port of the lithium phosphate mother liquor from the first separation device 4 is connected to an MVR device 5. The MVR device 5 processes the lithium sulfate crystals and concentrated lithium phosphate mother liquor. The outlet port of the concentrated lithium phosphate mother liquor from the MVR device 5 is connected to a lithium phosphate concentrated mother liquor reaction tank 7, which is connected to the ammonium phosphate storage tank 2. This allows lithium ions in the concentrated lithium phosphate mother liquor to react again with ammonium phosphate to generate a lithium phosphate suspension. The outlet port of the lithium phosphate concentrated mother liquor reaction tank 7 is connected to a second centrifuge device 8 to further separate the lithium phosphate solids and the secondary lithium phosphate mother liquor. The solid discharge port of the second centrifuge device 8 is circulated through a pipeline to the drying and packaging machine 9 to dry the lithium phosphate solid and obtain lithium phosphate product. The secondary lithium phosphate mother liquor discharge port of the second centrifuge device 8 is connected through a pipeline to a secondary lithium phosphate mother liquor storage tank 11, and the discharge port of the secondary lithium phosphate mother liquor storage tank 11 can be circulated to the inlet port of the microchannel reactor 3 for further recycling or rinsing of the lithium phosphate precipitate.
[0024] The optimized system's MVR device 5 is also equipped with a steam condensate storage tank 10, whose inlet port is connected to the condensate outlet port of the MVR device 5. The outlet port of the steam condensate storage tank 10 is circulated to the microchannel reactor 3. This allows the condensate to circulate back through the microchannel reactor 3, preventing the lithium phosphate precipitate generated in the final reaction from depositing inside the microchannel reactor 3, thus achieving a flushing effect on the microchannel reactor 3.
[0025] In addition to the components mentioned above, pumps, corresponding valves, and sensors can be installed on the connecting pipelines of this system according to actual needs to coordinate the operation of the entire system. For example, a valve is installed on the pipeline connecting the lithium phosphate concentrate mother liquor reaction tank 7 and the ammonium phosphate storage tank 2, and a sensor is installed inside the lithium phosphate concentrate mother liquor reaction tank 7. When the sensor detects that lithium phosphate concentrate mother liquor has entered the lithium phosphate concentrate mother liquor reaction tank 7, the valve on the pipeline connecting the lithium phosphate reaction tank 7 and the ammonium phosphate storage tank 2 can be opened by controlling the PLC to coordinate the operation of the system.
Claims
1. A system for continuous preparation of lithium phosphate products, characterized in that, The system includes a microchannel reactor (3) connected to both a lithium sulfate storage tank (1) and an ammonium phosphate storage tank (2) to generate lithium phosphate, a first centrifuge device (4) connected to the discharge port of the microchannel reactor (3), and an MVR device (5) connected to the mother liquor discharge port of the first centrifuge device (4). The MVR device (5) is also connected to a lithium phosphate concentrate mother liquor storage tank (6). The inlet port of the lithium phosphate concentrate mother liquor storage tank (6) is connected to the outlet port of the MVR device (5). The outlet port of the lithium phosphate concentrate mother liquor storage tank (6) is cyclically connected to the inlet port of the microchannel reactor (3).
2. A system for continuous preparation of lithium phosphate products, characterized in that, The system includes a microchannel reactor (3) connected to both a lithium sulfate storage tank (1) and an ammonium phosphate storage tank (2) to generate lithium phosphate, a first centrifuge device (4) connected to the discharge port of the microchannel reactor (3), and an MVR device (5) connected to the mother liquor discharge port of the first centrifuge device (4). The MVR device (5) is also connected to a lithium phosphate concentrate mother liquor reaction tank (7). The feed port of the lithium phosphate concentrate mother liquor reaction tank (7) is connected to the liquid outlet port of the MVR device (5) and the discharge port of the ammonium phosphate storage tank (2). A second centrifuge device (8) is connected to the liquid outlet port of the lithium phosphate concentrate mother liquor reaction tank (7).
3. The system for continuous preparation of lithium phosphate products according to claim 1 or 2, characterized in that, The solid discharge port of the first centrifuge device (4) is connected to the drying and packaging machine (9) to obtain lithium phosphate products.
4. The system for continuous preparation of lithium phosphate products according to claim 1 or 2, characterized in that, The MVR device (5) is also connected to a steam condensate storage tank (10). The inlet port of the steam condensate storage tank (10) is connected to the condensate outlet port of the MVR device (5), and the outlet port of the steam condensate storage tank (10) is circulatedly connected to the microchannel reactor (3).
5. The system for continuous preparation of lithium phosphate products according to claim 3, characterized in that, The liquid outlet of the second centrifuge device (8) is connected to a secondary lithium phosphate mother liquor storage tank (11), and the solid discharge port of the second centrifuge device (8) is circulated to the drying and packaging machine (9) through a pipeline.
6. The system for continuous preparation of lithium phosphate products according to claim 5, characterized in that, The outlet port of the secondary lithium phosphate mother liquor storage tank (11) is cyclically connected to the inlet port of the microchannel reactor (3).