Production system for solid-state product and production method

Abstract

The present application provides a production system for a solid-state product and a production method. The system comprises a liquid-phase feeding system, a continuous gas generation system, a gas-liquid reaction system, a crystallization system, a continuous rotary filter, and a continuous rotary dryer. By means of the system, a continuous production process can be achieved, comprising conveying liquid-phase raw materials, conveying gas-phase intermediate products, gas-liquid reaction, crystallization, filtration, and drying. The continuous production process can reduce manual operations, avoid the risk of harmful gas leakage during production, and improve safety during production. Moreover, automatic continuous operations can, in one aspect, improve production efficiency and reduce production costs, and in another aspect, improve production stability, reduce batch-to-batch differences, and effectively guarantee product quality.

Description

A production system and method for solid-state products Technical Field

[0001] This application relates to the field of solid-state product manufacturing, and more specifically, to a manufacturing system and method for solid-state products. Background Technology

[0002] In fields such as chemical engineering, energy, environment, and biochemistry, some solid-state products typically require multiple production steps. Taking lithium hexafluorophosphate (LiPF6) as an example, in industrial production, the reaction for preparing LiPF6 is LiF + PF5 → LiPF6. This means that liquid-phase LiF reacts with gaseous PF5 to generate liquid-phase LiPF6. The gaseous PF5 is obtained from the liquid-solid reaction of liquid-phase AHF with solid-phase PCl5. After obtaining liquid-phase LiPF6, further crystallization and other steps are needed to obtain solid-phase LiPF6. For this type of solid-state product, which requires first obtaining a gaseous intermediate, then using the gaseous intermediate and liquid raw materials to obtain the liquid product, and finally crystallization, manual feeding and other operations are usually required in industrial production, making continuous production difficult. Summary of the Invention

[0003] This application provides at least one production system and method for solid products, which can realize a continuous production process of liquid raw material transportation, gaseous intermediate product transportation, gas-liquid reaction, crystallization, filtration and drying. The continuous production process can reduce manual operation, avoid the risk of leakage of harmful gases during the production process, and improve the safety of the production process. At the same time, the automatic continuous operation can improve production efficiency, reduce production costs, improve production stability, reduce batch production differences, and effectively ensure product quality.

[0004] This application provides a production system for solid products, the system comprising a liquid-phase feeding system, a continuous gas generation system, a gas-liquid reaction system, a crystallization system, a continuous rotary filter, and a continuous rotary dryer.

[0005] The outlet of the liquid phase feed system is connected to the liquid phase feed inlet of the gas-liquid reaction system; the liquid phase feed system is used to continuously feed liquid phase raw materials into the gas-liquid reaction system.

[0006] The outlet of the continuous gas generation system is connected to the gas phase inlet of the gas-liquid reaction system; the continuous gas generation system is used to continuously deliver gas phase intermediate products to the gas-liquid reaction system.

[0007] The outlet of the gas-liquid reaction system is connected to the inlet of the crystallization system; the gas-liquid reaction system is used to realize the continuous gas-liquid reaction between liquid raw materials and gas intermediate products to obtain liquid products, and the crystallization system is used to realize the continuous crystallization of liquid products to obtain target crystals.

[0008] The outlet of the crystallization system is connected to the inlet of the continuous rotary filter, and the outlet of the continuous rotary filter is connected to the inlet of the continuous rotary dryer. The continuous rotary filter is used to achieve continuous filtration and separation between the target crystal and the mother liquor, and the continuous rotary dryer is used to achieve continuous drying of the target crystal.

[0009] This application also provides a production method based on a production system, the method comprising:

[0010] Liquid phase raw materials are continuously fed into the gas-liquid reaction system through a liquid phase feeding system, and gas phase intermediate products are continuously fed into the gas-liquid reaction system through a continuous gas generation system.

[0011] A continuous gas-liquid reaction between liquid-phase raw materials and gas-phase intermediate products is achieved through a gas-liquid reaction system to obtain liquid-phase products.

[0012] The target crystal is obtained by continuous crystallization of the liquid phase product through a crystallization system.

[0013] Continuous filtration and separation of the target crystals and the mother liquor are achieved through a continuous rotating disc filter;

[0014] Continuous drying of the target crystal is achieved through a continuous rotary dryer.

[0015] In summary, this application provides a production system and method for solid products. The system includes a liquid-phase feeding system, a continuous gas generation system, a gas-liquid reaction system, a crystallization system, a continuous rotary filter, and a continuous rotary dryer. The outlet of the liquid-phase feeding system is connected to the liquid-phase inlet of the gas-liquid reaction system; the liquid-phase feeding system continuously feeds liquid-phase raw materials into the gas-liquid reaction system. The outlet of the continuous gas generation system is connected to the gas-phase inlet of the gas-liquid reaction system; the continuous gas generation system continuously feeds gas-phase intermediate products into the gas-liquid reaction system. The system's outlet is connected to the crystallization system's inlet; the gas-liquid reaction system enables continuous gas-liquid reaction between liquid raw materials and gaseous intermediate products to obtain liquid products, while the crystallization system enables continuous crystallization of the liquid products to obtain the target crystals; the crystallization system's outlet is connected to the inlet of a continuous rotary filter, which in turn is connected to the inlet of a continuous rotary dryer; the continuous rotary filter enables continuous filtration and separation between the target crystals and the mother liquor, while the continuous rotary dryer enables continuous drying of the target crystals. Through this system, a continuous production process can be achieved, encompassing the transport of liquid raw materials, the transport of gaseous intermediate products, gas-liquid reaction, crystallization, filtration, and drying. This continuous production process reduces manual operation, avoids the risk of harmful gas leaks, and improves safety. Simultaneously, automated continuous operation improves production efficiency, reduces production costs, enhances production stability, reduces batch-to-batch variations, and effectively ensures product quality.

[0016] Other advantages of this application will be explained in more detail in conjunction with the following description and figures.

[0017] It should be understood that the above description is merely an overview of the technical solution of this application, so as to enable a general understanding of the technical means of this application and to implement it in accordance with the contents of the specification. In order to make the above and other objects, features and advantages of this application more apparent and understandable, specific embodiments of this application are illustrated below. Attached Figure Description

[0018] To more clearly illustrate the technical solutions of the embodiments of this application, the accompanying drawings used in the embodiments will be briefly described below. The accompanying drawings are incorporated in and constitute a part of this specification. These drawings illustrate embodiments conforming to this application and are used together with the specification to explain the technical solutions of this application. It should be understood that the drawings only illustrate certain embodiments of this application and should not be considered as a limitation on the scope of protection. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort. Furthermore, the same reference numerals denote the same components throughout the drawings. In the drawings:

[0019] Figure 1 is a schematic diagram of the structure of a production system for solid-state products provided in an embodiment of this application;

[0020] Figure 2 is a schematic diagram of the structure of the cooling circulation crystallizer provided in the embodiment of this application;

[0021] Figure 3 is a schematic diagram of the structure of multiple circulation outlets corresponding to the cooling circulation crystallizer provided in the embodiment of this application.

[0022] In the accompanying drawings, the same or corresponding reference numerals indicate the same or corresponding parts.

[0023] Among them, 100-liquid phase feed system; 1-first dissolving tank; 2-second dissolving tank; 3-first metering pump; 4-second metering pump; 200-continuous gas generation system; 5-liquid-solid reactor; 6-gas buffer tank; 300-gas-liquid reaction system; 7-first ejector; 8-first gas-liquid reactor; 9-first gas-liquid separator; 10-second ejector; 11-second gas-liquid reactor; 12-second gas-liquid separator; 13-third ejector; 1 4-Third gas-liquid reactor; 15-Gas-phase intermediate product recovery tower; 16-Temporary storage tank; 400-Crystallization system; 17-First-stage tubular continuous crystallizer; 18-Circulation pump; 18A-First circulation pump; 18B-Second circulation pump; 19-Cooler; 19A-First cooler; 19B-Second cooler; 20-Cooling circulating crystallizer; 201-Impeller; 202-Guide cylinder; 21-Continuous rotary filter; 22-Continuous rotary dryer. Detailed Implementation

[0024] Exemplary embodiments of this application will now be described in more detail with reference to the accompanying drawings. While exemplary embodiments of this application are shown in the drawings, it should be understood that this application can be implemented in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided to enable a more thorough understanding of this application and to fully convey the scope of this application to those skilled in the art.

[0025] In the description of embodiments of this application, it should be understood that terms such as “comprising” or “having” are intended to indicate the presence of the disclosed features, numbers, components, portions or combinations thereof in this specification, and do not exclude the possibility of the presence of one or more other features, numbers, components, portions or combinations thereof.

[0026] Unless otherwise stated, " / " means "or". For example, A / B can mean A or B. In this article, "and / or" is merely a way of describing the relationship between related objects, indicating that there can be three relationships. For example, A and / or B can mean: A alone, A and B at the same time, and B alone.

[0027] The terms "first," "second," etc., are used only for ease of description to distinguish identical or similar technical features and should not be construed as indicating or implying the relative importance or number of these technical features. Therefore, a feature defined by "first," "second," etc., may explicitly or implicitly include one or more of that feature. In the description of embodiments of this application, unless otherwise stated, the term "multiple" means two or more.

[0028] Taking lithium hexafluorophosphate as an example, it is necessary to first obtain a gaseous intermediate product, then obtain a liquid product based on the gaseous intermediate product and liquid raw materials, and finally obtain a solid product through crystallization. In industrial production, manual feeding and other operations are usually required, making it difficult to achieve continuous production.

[0029] In view of this, this application provides a production system and method for solid products, which can realize a continuous production process of liquid raw material transportation, gaseous intermediate product transportation, gas-liquid reaction, crystallization, filtration and drying. The continuous production process can reduce manual operation, avoid the risk of leakage of harmful gases during the production process, and improve the safety of the production process. At the same time, the automatic continuous operation can improve production efficiency, reduce production costs, and improve production stability, reduce the differences caused by batch production, and effectively ensure product quality.

[0030] The present application will now be described in detail with reference to the accompanying drawings and embodiments.

[0031] As shown in Figure 1, the production system for solid products includes a liquid-phase feeding system 100, a continuous gas generation system 200, a gas-liquid reaction system 300, a crystallization system 400, a continuous rotary filter 21, and a continuous rotary dryer 22.

[0032] The outlet of the liquid phase feed system 100 is connected to the liquid phase feed port of the gas-liquid reaction system 300; the liquid phase feed system 100 is used to continuously feed liquid phase raw materials to the gas-liquid reaction system 300.

[0033] Specifically, liquid raw materials typically need to be dissolved. Therefore, the liquid feeding system 100 may include a first dissolving tank 1, a first metering pump 3, a second dissolving tank 2, and a second metering pump 4. The first and second dissolving tanks 1 and 2 are used to dissolve the liquid raw materials. In practical applications, heat exchange jackets or coils can be installed externally on the first and second dissolving tanks 1 and 2 to ensure the dissolution temperature. Correspondingly, in addition to providing the first and second dissolving tanks 1 and 2, corresponding first and second metering pumps 3 and 4 are also provided to achieve quantitative delivery of the liquid raw materials. In this embodiment, continuous delivery of the liquid raw materials can be achieved through the alternating delivery of multiple dissolving tanks.

[0034] The outlet of the continuous gas generation system 200 is connected to the gas phase inlet of the gas-liquid reaction system 300; the continuous gas generation system 200 is used to continuously deliver gas phase intermediate products to the gas-liquid reaction system 300.

[0035] Specifically, the continuous gas production system 200 may include a liquid-solid reactor 5 and a gas buffer tank 6.

[0036] The liquid-solid reactor 5 can carry out relevant reactions to generate gaseous intermediate products. In practical applications, the liquid-solid reactor 5 can be a single cantilever cone-shaped liquid-solid reactor with a single cantilever stirring paddle inside. The paddle can rotate on its own axis while revolving around the axis of the liquid-solid reactor 5, which can realize rapid and uniform mixing of materials and rapid removal of reaction heat from the axis to the outer wall of the cone. A heat exchange jacket or coil can be installed on the outside of the cone-shaped body of the liquid-solid reactor 5. A condenser can be installed at the outlet of the liquid-solid reactor 5.

[0037] The inlet of the gas buffer tank 6 can be connected to the gas phase feed port of the gas-liquid reaction system 300. The gas buffer tank 6 buffers the gas phase intermediate product from the liquid-solid reactor 5. A mixing plug can be installed inside the gas buffer tank 6 to achieve uniform mixing of the multi-component gases when the gas phase intermediate product is a multi-component gas.

[0038] The outlet of the gas-liquid reaction system 300 is connected to the inlet of the crystallization system 400; the gas-liquid reaction system 300 is used to realize continuous gas-liquid reaction between liquid raw materials and gas intermediate products to obtain liquid products, and the crystallization system 400 is used to realize continuous crystallization of liquid products to obtain target crystals.

[0039] Specifically, the gas-liquid reaction system 300 may include a first ejector 7, a first gas-liquid reactor 8, a first gas-liquid separator 9, a second ejector 10, a second gas-liquid reactor 11, a second gas-liquid separator 12, a third ejector 13, and a third gas-liquid reactor 14. Through multiple sets of gas-liquid reactors and gas-liquid separators, continuous reaction of liquid-phase raw materials and gas-phase intermediate products is achieved. Specifically, the first gas-liquid reactor 8 ensures complete reaction of the liquid-phase raw materials, the first gas-liquid separator 9 recovers excess gas-phase intermediate products and collects the liquid-phase products generated by the first gas-liquid reactor 8, and the second gas-liquid reactor... The first gas-liquid separator 11 achieves complete reaction of excess gaseous intermediate products, the second gas-liquid separator 12 achieves recovery of excess liquid raw materials, the third gas-liquid reactor 14 achieves complete reaction of excess liquid raw materials, and the first gas-liquid separator 9 also achieves collection of liquid products generated by the second gas-liquid reactor 11 and the third gas-liquid reactor 14. That is, in the continuous reaction process, on the one hand, the gaseous intermediate products and liquid raw materials are fully reacted, and the product quality is guaranteed by avoiding the mixing of liquid raw materials and liquid products. On the other hand, the utilization of liquid raw materials and gaseous intermediate products is maximized, thereby saving production costs.

[0040] After obtaining the liquid phase product, the crystallization system 400 can be used to achieve continuous crystallization of the liquid phase product to obtain the target crystal.

[0041] The outlet of the crystallization system 400 is connected to the inlet of the continuous rotary filter 21, and the outlet of the continuous rotary filter 21 is connected to the inlet of the continuous rotary dryer 22. The continuous rotary filter 21 is used to achieve continuous filtration and separation between the target crystal and the crystal mother liquor, and the continuous rotary dryer 22 is used to achieve continuous drying of the target crystal.

[0042] Specifically, after obtaining the target crystal through the crystallization system 400, in order to ensure the quality of the target crystal, the target crystal and the crystal mother liquor are continuously filtered and separated through the continuous rotating disc filter 21, and the target crystal is continuously dried through the continuous rotary dryer 22, so as to obtain the final target crystal.

[0043] The aforementioned production system enables a continuous production process, including the transport of liquid raw materials, the transport of gaseous intermediate products, gas-liquid reaction, crystallization, filtration, and drying. This continuous production process reduces manual operation, avoids the risk of leakage of harmful gases during production, and improves safety. Furthermore, automated continuous operation increases production efficiency, reduces production costs, enhances production stability, minimizes batch variations, and effectively guarantees product quality.

[0044] In one possible implementation, the crystallization system 400 includes a primary tubular continuous crystallizer 17 and a secondary circulating crystallization system:

[0045] The outlet of the gas-liquid reaction system 300 is connected to the inlet of the primary tubular continuous crystallizer 17, which is used to realize the primary cooling crystallization of the liquid phase product.

[0046] The secondary circulating crystallization system includes a circulating pump 18, a cooler 19, and a cooling circulating crystallizer 20. The outlet of the primary tubular continuous crystallizer 17 is connected to the inlet of the cooler 19, and the outlet of the cooler 19 is connected to the inlet of the cooling circulating crystallizer 20. A circulating pump 18 is installed between the circulation outlet of the cooling circulating crystallizer 20 and the inlet of the cooler 19. The cooler 19 is used to meet the cooling requirements of the secondary circulating crystallization system. The cooling circulating crystallizer 20 is used to generate crystals to obtain the target crystals and discharge the target crystals. The circulating pump 18 is used to realize the circulation transport of the crystallization solution, including the crystal grains, from the circulation outlet of the cooling circulating crystallizer 20 to the cooler 19 and back to the cooling circulating crystallizer 20.

[0047] Specifically, to ensure sufficient crystallization of the liquid phase product, in this embodiment, the crystallization system 400 includes a primary tubular continuous crystallizer 17 for primary cooling crystallization and a secondary circulating crystallization system for secondary cooling crystallization. The primary tubular continuous crystallizer 17 can realize crystal nucleation and growth; the cooler 19 included in the secondary circulating crystallization system can be used to meet the cooling requirements of the secondary circulating crystallization system. In practical applications, the cooler 19 can be used as a single cooler or multiple coolers connected in parallel to improve cooling efficiency; the cooling circulating crystallizer 20 included in the secondary circulating crystallization system can realize crystal generation to obtain the target crystal and the discharge of the target crystal, that is, the generated target crystal can be discharged through the crystal outlet of the cooling circulating crystallizer 20; the circulating pump 18 included in the secondary circulating crystallization system can provide power for the circulation of the crystallization solution, so that the crystallization solution including fine crystal grains is discharged from the circulation outlet of the cooling circulating crystallizer 20, passes through the circulating pump 18 to the cooler 19, and then returns to the cooling circulating crystallizer 20 so that the fine crystal grains can grow again into the target crystal, that is, the circulating pump 18 can realize the circulation transport of the crystallization solution to ensure sufficient crystallization.

[0048] It should be noted that the two-stage circulating crystallization system can discharge the target crystals that meet the requirements from the crystal outlet of the cooling circulating crystallizer 20, while the small crystals that do not meet the requirements can be discharged from the circulation outlet of the cooling circulating crystallizer 20, then passed through the circulation pump 18 to the cooler 19 and returned to the cooling circulating crystallizer 20 for re-crystallization until they grow into the target crystals and are then discharged from the crystal outlet of the cooling circulating crystallizer 20.

[0049] In one possible implementation, the bottom of the cooling circulation crystallizer 20 is W-shaped, and a blade 201 is provided at the center of the interior of the cooling circulation crystallizer 20, with a guide tube 202 provided outside the blade 201.

[0050] Specifically, as shown in Figure 2, the combination of the W-shaped bottom, the blade 201, and the guide tube 202 can change the internal flow pattern of the cooling circulation crystallizer 20. The internal fluid is divided into an inner liquid column and an outer liquid column, with the guide tube 202 as the boundary. The blade 201 allows the inner liquid column to always run from top to bottom, and after hitting the W-shaped bottom, it can move smoothly upwards. This enhances the heat exchange effect between the central fluid and the inner wall of the cooling circulation crystallizer 20, improves temperature uniformity, and allows crystals to grow in an environment with the same flow rate and temperature. This effectively prevents phenomena such as crystallization explosion and crystal doping, improves the consistency and homogenization of the grains, promotes the formation of "quasi-spherical" target crystals, and facilitates continuous production.

[0051] In one possible implementation, a heat exchange jacket is provided on the outside of the cooling circulation crystallizer 20, which can further promote the cooling crystallization process and reduce the crystallization time.

[0052] In one possible implementation, considering that the fine grains that have not reached the target crystal size have different sizes, and the fine grains of different sizes will have different suspension positions, the cooling circulating crystallizer 20 can be provided with multiple circulation outlets. The multiple circulation outlets correspond one-to-one with the suspension positions of multiple crystals of different sizes, and each of the multiple circulation outlets is equipped with a corresponding circulation pump 18 and cooler 19.

[0053] Specifically, as shown in Figure 3, in practical applications, the cooling circulating crystallizer 20 can be equipped with two circulation outlets at different heights. The first circulation outlet is equipped with a corresponding circulation pump 18A and cooler 19A, and the second circulation outlet is equipped with a corresponding circulation pump 18B and cooler 19B.

[0054] Multiple circulation outlets and corresponding circulation pumps 18 and coolers 19 can achieve staged cooling of crystallization solutions containing crystals of different sizes. That is, according to the different particle sizes of crystals at different suspension positions, different feed circulation ratios and cooling rates can be set to directionally control the growth process of crystals of different sizes, enhance the consistency of crystal form and particle size at the outlet, and improve product quality.

[0055] In one possible implementation, a static mixing insert with a cut surface is provided inside the primary tubular continuous crystallizer 17. The static mixing insert with the cut surface can achieve uniform radial temperature distribution within the tube, improving crystallization quality, while simultaneously enhancing turbulence intensity within the tube and preventing crystal scaling and blockage of the pipeline.

[0056] In one possible implementation, a heat exchange jacket is provided on the outside of the primary tubular continuous crystallizer 17. The cooling requirements during the crystallization process can be guaranteed by the heat exchange jacket, that is, gradient cooling can be achieved by the external heat exchange jacket.

[0057] In one possible implementation, a filter disc is provided at the bottom of the continuous rotary filter 21, a distributor is provided at the top of the filter disc, and a discharge baffle is provided at the top of the continuous rotary filter 21. The distributor is used to spray the mixed crystal mother liquor, including the target crystal, onto the filter disc. The filter disc is used to achieve filtration and separation between the target crystal and the crystal mother liquor. The discharge baffle is used to discharge the target crystal that has reached the target height.

[0058] Specifically, the continuous rotary filter 21 has a filter disc at its bottom. The filter disc can be a circular filter disc that rotates 360°. A distributor is installed on the top of the filter disc. The distributor sprays the mixed crystal mother liquor, including the target crystal, onto the filter disc. As the filter disc rotates, the bottom of the filter disc can be vacuum filtered to achieve the separation of the target crystal and the crystal mother liquor. The separated crystal mother liquor can be discharged from the bottom of the continuous rotary filter 21 and can be recycled to the dissolving tank in the liquid phase feeding system 100 for reuse. The remaining target crystal accumulates on the filter disc. After reaching the target height, it can be discharged through the discharge baffle.

[0059] In one possible implementation, the continuous rotary dryer 22 is tilted at a preset tilt angle, and both the inlet and outlet of the continuous rotary dryer 22 are equipped with screw conveyors. The inside of the continuous rotary dryer 22 is equipped with lifting plates, the outside of the continuous rotary dryer 22 is equipped with a heat exchange jacket, and the outlet of the continuous rotary dryer 22 is equipped with a protective gas inlet.

[0060] Specifically, the continuous rotary dryer 22 is tilted at a preset angle, meaning it has a certain tilt angle. The continuous feeding and discharging process of the target crystal can be realized through the screw conveyor devices set at the feed inlet and discharge outlet. The continuous rotary dryer 22 is equipped with lifting plates inside, which can shorten the drying time of the target crystal. The continuous rotary dryer 22 is equipped with a heat exchange jacket outside, which can meet the heating requirements of the target crystal during the drying process. The discharge outlet of the continuous rotary dryer 22 is equipped with a protective gas inlet. Through the protective gas inlet, a protective gas, such as nitrogen, can be introduced into the discharge outlet so that the gaseous intermediate products volatilized after drying can be discharged from the discharge outlet.

[0061] In one possible implementation, the gas-liquid reaction system 300 includes a gas-phase intermediate product recovery tower 15 and a temporary storage tank 16.

[0062] The exhaust port of the gas-liquid reaction system 300 is connected to the inlet of the gas phase intermediate product recovery tower 15, the outlet of the gas phase intermediate product recovery tower 15 is connected to the inlet of the temporary storage tank 16, and the outlet of the temporary storage tank 16 is connected to the inlet of the liquid phase feeding system 100. The gas phase intermediate product recovery tower 15 is used to recover the residual gas phase intermediate products in the exhaust gas of the gas-liquid reaction system 300, and the temporary storage tank 16 is used to temporarily store the recovered gas phase intermediate products in liquid phase form.

[0063] Specifically, the gaseous intermediate product recovery tower 15 is used to recover the residual gaseous intermediate products in the tail gas of the gas-liquid reaction system 300. Other components in the tail gas can be discharged from the top of the gaseous intermediate product recovery tower 15 for tail gas treatment. The temporary storage tank 16 can be used to temporarily store the recovered gaseous intermediate products in liquid form. The recovered gaseous intermediate products can be temporarily stored in liquid form after condensation. The outlet of the temporary storage tank 16 is connected to the inlet of the liquid feed system 100, for example, it can be connected to the inlet of the dissolving tank in the liquid feed system 100, so that the solution in the temporary storage tank 16 can be returned to the dissolving tank as a solvent to dissolve the solid raw materials, thereby realizing recycling.

[0064] The following describes the production method based on the above-described production system provided in this application using method embodiments. The method includes:

[0065] S401. Liquid phase raw materials are continuously fed into the gas-liquid reaction system 300 through the liquid phase feeding system 100, and gas phase intermediate products are continuously fed into the gas-liquid reaction system 300 through the continuous gas generation system 200.

[0066] S402, A continuous gas-liquid reaction between liquid raw materials and gaseous intermediate products is achieved through a gas-liquid reaction system 300 to obtain liquid products.

[0067] S403. Continuous crystallization of the liquid phase product is achieved through the crystallization system 400 to obtain the target crystal.

[0068] S404. The target crystal and the mother liquor are continuously filtered and separated by a continuous rotating disc filter 21.

[0069] S405. Continuous drying of the target crystal is achieved through a continuous rotary dryer 22.

[0070] In one possible implementation, in S403, continuous crystallization of the liquid-phase product is achieved through crystallization system 400 to obtain the target crystal, including:

[0071] A primary cooling crystallization process is performed using a primary tubular continuous crystallizer 17 to obtain a primary crystallization mother liquor containing crystal nuclei.

[0072] The primary crystallization mother liquor is first cooled by cooler 19 and then crystallized by cooling circulation crystallizer 20. The generated target crystal is discharged through the crystal outlet of cooling circulation crystallizer 20. The crystallization solution containing the crystal grains is discharged from the circulation outlet of cooling circulation crystallizer 20 and then pumped by circulation pump 18 to cooler 19 and returned to cooling circulation crystallizer 20 so that the crystal grains can grow again to become the target crystal.

[0073] Specifically, a primary cooling crystallization process is carried out in a primary tubular continuous crystallizer 17 to obtain a primary crystallization mother liquor containing crystal nuclei. The primary cooling crystallization process is carried out in the primary tubular continuous crystallizer 17 to realize the crystal nucleation process. The cooling gradient can be controlled by an external heat exchange jacket.

[0074] The primary crystallization mother liquor from the primary tubular continuous crystallizer 17 can enter the secondary circulation system. The primary crystallization mother liquor is first cooled by the cooler 19, and then crystals are generated by the cooling circulation crystallizer 20. The heat exchange jacket outside the cooling circulation crystallizer 20 can further enhance the cooling process. The generated target crystals can be discharged through the crystal outlet of the cooling circulation crystallizer 20. The crystallization solution, including the crystal grains, can be discharged from the circulation outlet of the cooling circulation crystallizer 20 and then passed through the circulation pump 18 to the cooler 19 and back to the cooling circulation crystallizer 20. Through the circulation process, the fine crystal grains can be further grown until they become the target crystals, and then discharged from the crystal outlet of the cooling circulation crystallizer 20. This process continuously allows the primary crystallization mother liquor to enter and the target crystals to be discharged, thus achieving continuous crystallization.

[0075] In one possible implementation, continuous filtration and separation of the target crystal and the mother liquor are achieved in S404 through a continuous rotating disc filter 21, including:

[0076] The mixed crystal mother liquor, including the target crystals, is sprayed onto the filter disc by a distributor;

[0077] The target crystals and the mother liquor are separated by the rotation of the filter disc and the vacuum operation.

[0078] The separated crystal mother liquor is discharged from the bottom of the continuous rotary filter 21 and recycled back to the liquid phase feed system 100 for reuse;

[0079] The target crystal, having reached the target height, is discharged from the outlet via the discharge baffle.

[0080] In one possible implementation, continuous drying of the target crystal is achieved in S405 via a continuous rotary dryer 22, including:

[0081] The continuous feeding of the target crystal is achieved through the screw conveyor at the feed inlet of the continuous rotary dryer 22 and the rotation of the cylinder.

[0082] The target crystals are obtained by heating and drying through the heat exchange jacket of the continuous rotary dryer 22. Protective gas is introduced from the outlet through the protective gas inlet so that the unreacted gaseous intermediate products after drying are discharged from the outlet.

[0083] The continuous discharge of the target crystals is achieved through the screw conveyor at the discharge port of the continuous rotary dryer 22 and the rotation of the cylinder.

[0084] Specifically, in practical applications, the filtered target crystals can enter the continuous rotary dryer 22, and the continuous entry and exit process of the target crystals can be achieved through the spiral conveyor and the rotation of the cylinder.

[0085] The target crystals are obtained by heating and drying through the heat exchange jacket of the continuous rotary dryer 22. A protective gas, such as nitrogen, can be introduced from the outlet through the protective gas inlet to discharge the unreacted gaseous intermediate products after drying. The discharged gaseous intermediate products and protective gas can be fed into the gaseous intermediate product recovery tower 15 for recovery, thereby realizing the recycling of gaseous intermediate products.

[0086] In one possible implementation, the method includes:

[0087] The tail gas from the gas-liquid reaction system 300 is sent to the gas-phase intermediate product recovery tower 15 to recover the gas-phase intermediate product. The remaining components can be treated as tail gas. The recovered gas-phase intermediate product can be temporarily stored in the liquid phase in the temporary storage tank 16. The temporarily stored solution can be sent to the dissolution tank of the liquid phase feed system 100 for recycling.

[0088] The production system and production method provided in this application embodiment are described below using lithium hexafluorophosphate as an example:

[0089] Step 1: Continuous delivery of lithium fluoride solution.

[0090] Step 1-1: Solid lithium fluoride and AHF solution are injected into the first dissolving tank 1 and the second dissolving tank 2 respectively. The AHF solution is dissolved at a controlled temperature using an external heat exchange jacket or coil to form a lithium fluoride solution. The mass ratio of lithium fluoride to hydrogen fluoride is 1:5 to 1:25, and the dissolution temperature is -2 to 16℃.

[0091] Steps 1-2: Start the first metering pump 3, control the flow rate, and deliver the lithium fluoride solution in the first dissolving tank 1 to the continuous phase main pipeline of the first ejector 7.

[0092] Steps 1-3: After the lithium fluoride solution in the first dissolving tank 1 has been delivered, turn off the first metering pump 3 and start the second metering pump 4 to deliver the lithium fluoride solution in the second dissolving tank 2 to the continuous phase main circuit of the first ejector 7.

[0093] Steps 1-4: While starting the second metering pump 4, turn off the first metering pump 3, and re-inject solid lithium fluoride and AHF solution into the first dissolving tank 1, repeating the feeding operation; the alternating feeding, dissolving and discharging process of the dissolving tank realizes the continuous conveying process of lithium fluoride solution; multiple dissolving tanks can be set up in parallel, and the feeding and dissolving time is less than the continuous conveying time of materials in a single tank.

[0094] Step 2: Continuous reaction and transport of phosphorus pentafluoride gas.

[0095] Step 2-1: Start the continuous automated feeding device for phosphorus pentachloride in liquid-solid reactor 5, continuously injecting solid phosphorus pentachloride under nitrogen protection. Simultaneously, continuously inject AHF solution, start the motor, and begin stirring. The liquid-solid reaction of phosphorus pentachloride and hydrogen fluoride occurs within liquid-solid reactor 5, producing phosphorus pentafluoride gas. The reaction temperature is controlled using the external heat exchange jacket or coils of the conical cylinder of liquid-solid reactor 5. The molar ratio of phosphorus pentachloride to hydrogen fluoride is 1:5.05 to 1:6.65, the reaction temperature of phosphorus pentachloride and hydrogen fluoride is -2 to 16°C, and the rotation speed of the stirring shaft is 1 to 100 rpm.

[0096] Step 2-2: Open the gas outlet of the liquid-solid reactor 5, recover part of the hydrogen fluoride gas through the condenser, and the mixed gas of phosphorus pentafluoride, hydrogen fluoride, hydrogen chloride, nitrogen and other gases enter the gas buffer tank 6.

[0097] Steps 2-3: The mixed gas is uniformly mixed by the mixing plug inside the gas buffer tank 6, ensuring uniformity at the outlet of the gas buffer tank 6. The phosphorus pentafluoride gas content in the mixed gas is 20% to 50%.

[0098] Step 2-4: Start step 2-4 at the same time as starting step 1-2, and deliver the mixed gas in gas buffer tank 6 to the discrete phase side pipeline of the first ejector 7.

[0099] Step 3: Continuous gas-liquid reaction of lithium fluoride solution with phosphorus pentafluoride gas.

[0100] Step 3-1: The first ejector 7 ejects and mixes the lithium fluoride solution from the dissolving tank with the phosphorus pentafluoride gas from the gas buffer tank 6, and then introduces it into the first gas-liquid reactor 8.

[0101] Step 3-2: A gas-liquid reaction of fresh lithium fluoride solution with phosphorus pentafluoride occurs in the first gas-liquid reactor 8, with the reaction temperature controlled by an external heat exchange jacket. Simultaneously, phosphorus pentafluoride gas from the gas buffer tank 6 is injected into the gas supply port of the first gas-liquid reactor 8 to ensure complete reaction of the lithium fluoride solution. The reaction temperature is -20 to 20°C, the reaction pressure is 0.1 MPa to 2 MPa, and the residence time is 0.5 min to 120 min.

[0102] Step 3-3: The mother liquor after reaction in the first gas-liquid reactor 8 and the remaining gas (unreacted phosphorus pentafluoride, hydrogen fluoride, hydrogen chloride, and nitrogen) enter the first gas-liquid separator 9, where the gas-liquid separation process is completed.

[0103] Steps 3-4: The remaining gas after separation by the first gas-liquid separator 9 enters the discrete phase side inlet of the second ejector 10; the lithium fluoride solution in the dissolution tank is simultaneously transported to the continuous phase main pipeline of the second ejector 10.

[0104] Steps 3-5: The second ejector 10 ejects and mixes the lithium fluoride solution from the dissolving tank with the remaining gas separated from the first gas-liquid separator 9, and then introduces it into the second gas-liquid reactor 11.

[0105] Steps 3-6: The second gas-liquid reactor 11 carries out a gas-liquid reaction between fresh lithium fluoride solution and phosphorus pentafluoride gas that has not fully reacted in the first gas-liquid reactor 8. The lithium fluoride solution is in excess to ensure that the phosphorus pentafluoride gas reacts completely. The reaction temperature is controlled by an external heat exchange jacket. The reaction temperature is -20 to 20°C. The reaction pressure is 0.1 MPa to 2 MPa. The residence time is 0.5 min to 120 min.

[0106] Steps 3-7: The mother liquor and the remaining gas (hydrogen fluoride, hydrogen chloride, nitrogen) after the reaction in the second gas-liquid reactor 11 enter the second gas-liquid separator 12, where the gas-liquid separation process is completed.

[0107] Steps 3-8: The mother liquor (product lithium hexafluorophosphate and remaining lithium fluoride solution) separated by the second gas-liquid separator 12 enters the continuous phase inlet of the third ejector 13 from the liquid phase outlet of the second gas-liquid separator 12; fresh gas from the gas buffer tank 6 enters the discrete phase side pipeline of the third ejector 13 simultaneously.

[0108] Steps 3-9: The third ejector 13 is used to eject and mix the lithium hexafluorophosphate product from the second gas-liquid separator 12 with the remaining lithium fluoride solution and the fresh gas from the gas buffer tank 6, and then introduce it into the third tubular continuous gas-liquid reactor 14.

[0109] Steps 3-10: In the third gas-liquid reactor 14, the incompletely reacted lithium fluoride solution from the second gas-liquid reactor 11 undergoes a gas-liquid reaction with fresh phosphorus pentafluoride gas. Simultaneously, fresh gas from the gas buffer tank 6 enters the gas supply port of the third gas-liquid reactor 14. Phosphorus pentafluoride is in excess to ensure complete reaction of the lithium fluoride solution. The reaction temperature is -20 to 20°C, the reaction pressure is 0.1 MPa to 2 MPa, and the residence time is 0.5 min to 120 min.

[0110] Step 3-11: The mother liquor and residual gas after the reaction in the third gas-liquid reactor 14 re-enter the first gas-liquid separator 9; repeat steps 3-4 to 3-10 to achieve continuous gas-liquid reaction.

[0111] Step 4: Exhaust gas treatment.

[0112] Step 4-1: After separation by the second gas-liquid separator 12, the gases (hydrogen fluoride, hydrogen chloride, and nitrogen) enter the gas phase intermediate product recovery tower 15 to recover hydrogen fluoride; the remaining hydrogen chloride and nitrogen enter the subsequent alkaline tail gas treatment stage; the top temperature of the recovery tower is -20℃~15℃; the operating pressure is 0.3MPa~3MPa.

[0113] Step 4-2: The hydrogen fluoride (condensed) recovered by the gas phase intermediate product recovery tower 15 enters the temporary storage tank 16 in liquid form for temporary storage; the solution in the temporary storage tank 16 can be returned to the dissolving tank as a solvent to dissolve the solid lithium fluoride raw material, thereby realizing recycling.

[0114] Step 5: Continuous crystallization of lithium hexafluorophosphate.

[0115] Step 5-1: The mother liquor separated by the first gas-liquid separator 9 in step 3-3 enters the first-stage tubular continuous crystallizer 17; the first-stage cooling crystallization process is carried out in the first-stage tubular continuous crystallizer 17 to realize the crystal nucleation process, and the cooling gradient is controlled by the external jacket; the first-stage crystallization cooling gradient is 0 to -15℃ and -15℃ to -30℃; the solid content of the outlet crystal solution is 3% to 10%, and the residence time is 0.5h to 5h.

[0116] Step 5-2: The primary crystallization mother liquor from the primary tubular continuous crystallizer 17 enters the secondary circulating crystallization system.

[0117] Step 5-3: The primary crystallization mother liquor enters the cooling circulation crystallizer 20 through cooler 19, where cooler 19 further cools the mother liquor. Crystal growth occurs within the cooling circulation crystallizer 20, with external heat exchange jackets or coils further enhancing the cooling process. The grown crystals are discharged from the crystal outlet of the cooling circulation crystallizer 20. The crystallization solution containing fine crystals flows from the circulation outlet of the cooling circulation crystallizer 20 through circulation pump 18 to cooler 19 and then back to the cooling circulation crystallizer 20. This circulation process further grows the fine crystals until they reach the target size and are discharged from the crystal outlet of the cooling circulation crystallizer 20. This continuous process of mother liquor entering and formed crystals exiting achieves continuous crystallization. The secondary crystallization cooling gradient is -30℃ to -50℃, the circulating feed ratio is 20 to 100, the solid content of the outlet crystal solution is 10% to 35%, and the residence time is 1 hour to 7 hours.

[0118] Step 6: Continuous separation of lithium hexafluorophosphate from the remaining mother liquor.

[0119] Step 6-1: The formed crystals and mother liquor enter the continuous rotating disc filter 21. With the rotation of the internal filter disc and the vacuum operation, the lithium hexafluorophosphate crystals and mother liquor are continuously separated.

[0120] Step 6-2: The separated mother liquor (uncrystallized lithium hexafluorophosphate solution and hydrogen fluoride) is discharged from the bottom of the continuous rotary filter 21 and recycled to the dissolving tank for reuse.

[0121] Step 6-3: The filtered lithium hexafluorophosphate crystals are continuously discharged from the side of the continuous rotating disc filter 21.

[0122] Step 7: Continuous drying of lithium hexafluorophosphate crystals.

[0123] Step 7-1: The filtered lithium hexafluorophosphate crystals enter the continuous rotary dryer 22, and the crystals are continuously fed in and out through the rotation of the cylinder via a screw conveyor. The external heat exchange jacket or coil of the continuous rotary dryer 22 is used for heating and drying. After drying, a solid product is obtained. The drying temperature is 20℃~90℃, and the residence time is 0.5h~10h.

[0124] Step 7-2: During the continuous drying process, nitrogen gas is introduced into the continuous rotary dryer 22 from the outlet end, and the hydrogen fluoride gas volatilized during drying is discharged from the inlet end. The discharged hydrogen fluoride and nitrogen gas can be introduced into the gas phase intermediate product recovery tower 15 for subsequent separation and recovery, so as to realize the recycling of hydrogen fluoride.

[0125] Therefore, this application provides a production system and method for solid products. The system includes a liquid-phase feeding system, a continuous gas generation system, a gas-liquid reaction system, a crystallization system, a continuous rotary filter, and a continuous rotary dryer. The outlet of the liquid-phase feeding system is connected to the liquid-phase inlet of the gas-liquid reaction system. The liquid-phase feeding system continuously feeds liquid-phase raw materials into the gas-liquid reaction system. The outlet of the continuous gas generation system is connected to the gas-phase inlet of the gas-liquid reaction system. The continuous gas generation system continuously feeds gas-phase intermediate products into the gas-liquid reaction system. The system's outlet is connected to the crystallization system's inlet; the gas-liquid reaction system enables continuous gas-liquid reaction between liquid raw materials and gaseous intermediate products to obtain liquid products, while the crystallization system enables continuous crystallization of the liquid products to obtain the target crystals; the crystallization system's outlet is connected to the inlet of a continuous rotary filter, which in turn is connected to the inlet of a continuous rotary dryer; the continuous rotary filter enables continuous filtration and separation between the target crystals and the mother liquor, while the continuous rotary dryer enables continuous drying of the target crystals. Through this system, a continuous production process can be achieved, encompassing the transport of liquid raw materials, the transport of gaseous intermediate products, gas-liquid reaction, crystallization, filtration, and drying. This continuous production process reduces manual operation, avoids the risk of harmful gas leaks, and improves safety. Simultaneously, automated continuous operation improves production efficiency, reduces production costs, enhances production stability, reduces batch-to-batch variations, and effectively ensures product quality.

[0126] In the description of this specification, references to terms such as "some possible implementations," "some implementations," "example," "specific example," or "some examples" indicate that a specific feature, structure, material, or characteristic described in connection with that implementation or example is included in at least one implementation or example of this application, and the aforementioned terms do not necessarily refer to the same implementation or example. Furthermore, the described specific features, structures, materials, or characteristics can be combined in any suitable manner in one or more implementations or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different implementations or examples described in this specification, as well as the features of different implementations or examples.

[0127] While the spirit and principles of this application have been described above with reference to several specific embodiments, it should be understood that this application is not limited to the disclosed specific embodiments, and the division of aspects does not imply that features in these aspects cannot be combined. This application is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.

Claims

1. A production system for solid-state products, characterized in that, The system includes a liquid-phase feed system (100), a continuous gas generation system (200), a gas-liquid reaction system (300), a crystallization system (400), a continuous rotary filter (21), and a continuous rotary dryer (22). The outlet of the liquid phase feeding system (100) is connected to the liquid phase inlet of the gas-liquid reaction system (300); the liquid phase feeding system (100) is used to continuously feed liquid phase raw materials into the gas-liquid reaction system (300); The outlet of the continuous gas generation system (200) is connected to the gas phase inlet of the gas-liquid reaction system (300); the continuous gas generation system (200) is used to continuously supply gas phase intermediate products to the gas-liquid reaction system (300); The outlet of the gas-liquid reaction system (300) is connected to the inlet of the crystallization system (400); the gas-liquid reaction system (300) is used to realize continuous gas-liquid reaction between liquid raw materials and gas intermediate products to obtain liquid products, and the crystallization system (400) is used to realize continuous crystallization of liquid products to obtain target crystals. The outlet of the crystallization system (400) is connected to the inlet of the continuous rotary filter (21), and the outlet of the continuous rotary filter (21) is connected to the inlet of the continuous rotary dryer (22). The continuous rotary filter (21) is used to achieve continuous filtration and separation between the target crystal and the crystal mother liquor, and the continuous rotary dryer (22) is used to achieve continuous drying of the target crystal.

2. The production system for solid-state products according to claim 1, characterized in that, The crystallization system (400) includes a primary tubular continuous crystallizer (17) and a secondary circulating crystallization system: The outlet of the gas-liquid reaction system (300) is connected to the inlet of the primary tubular continuous crystallizer (17), which is used to realize the primary cooling crystallization of the liquid phase product. The secondary circulating crystallization system includes a circulating pump (18), a cooler (19), and a cooling circulating crystallizer (20). The outlet of the primary tubular continuous crystallizer (17) is connected to the inlet of the cooler (19), and the outlet of the cooler (19) is connected to the inlet of the cooling circulating crystallizer (20). A circulating pump (18) is provided between the circulation outlet of the cooling circulating crystallizer (20) and the inlet of the cooler (19). The cooler (19) is used to meet the cooling requirements of the secondary circulating crystallization system. The cooling circulating crystallizer (20) is used to generate crystals to obtain target crystals and discharge the target crystals. The circulating pump (18) is used to realize the circulating transport of the crystallization solution including crystal grains from the circulation outlet of the cooling circulating crystallizer (20) to the cooler (19) and back to the cooling circulating crystallizer (20).

3. The production system for solid-state products according to claim 2, characterized in that, The bottom of the cooling circulation crystallizer (20) is W-shaped. A blade (201) is provided in the center of the interior of the cooling circulation crystallizer (20), and a guide tube (202) is provided on the outside of the blade (201).

4. The production system for solid-state products according to claim 3, characterized in that, The cooling circulation crystallizer (20) is provided with a heat exchange jacket on its exterior.

5. The production system for solid-state products according to claim 4, characterized in that, The cooling circulating crystallizer (20) is provided with multiple circulation outlets, each of which corresponds to the suspension position of multiple crystals of different sizes. Each of the multiple circulation outlets is equipped with a corresponding circulation pump (18) and cooler (19).

6. The production system for solid-state products according to claim 2, characterized in that, The primary tubular continuous crystallizer (17) is equipped with a static mixing insert, which has a cut surface.

7. The production system for solid-state products according to claim 6, characterized in that, The external part of the primary tubular continuous crystallizer (17) is provided with a heat exchange jacket.

8. The production system for solid-state products according to claim 1, characterized in that, The continuous rotary filter (21) has a filter disc at its bottom and a distributor at its top. The filter disc has a discharge baffle at its top. The distributor sprays the mixed crystal mother liquor, including the target crystal, onto the filter disc. The filter disc is used to achieve filtration and separation between the target crystal and the crystal mother liquor. The discharge baffle is used to discharge the target crystal that has reached the target height.

9. The production system for solid-state products according to claim 1, characterized in that, The continuous rotary dryer (22) is inclined at a preset tilt angle. Both the inlet and outlet of the continuous rotary dryer (22) are equipped with screw conveyors. The inside of the continuous rotary dryer (22) is equipped with lifting plates. The outside of the continuous rotary dryer (22) is equipped with a heat exchange jacket. The outlet of the continuous rotary dryer (22) is equipped with a protective gas inlet.

10. The production system for solid-state products according to claim 1, characterized in that, The gas-liquid reaction system (300) includes a gas-phase intermediate product recovery tower (15) and a temporary storage tank (16): The exhaust port of the gas-liquid reaction system (300) is connected to the inlet of the gas-phase intermediate product recovery tower (15), the outlet of the gas-phase intermediate product recovery tower (15) is connected to the inlet of the temporary storage tank (16), and the outlet of the temporary storage tank (16) is connected to the inlet of the liquid-phase feeding system (100). The gas-phase intermediate product recovery tower (15) is used to recover the residual gas-phase intermediate products in the exhaust gas of the gas-liquid reaction system (300), and the temporary storage tank (16) is used to temporarily store the recovered gas-phase intermediate products in liquid form.

11. A production method based on the production system according to any one of claims 1-10, characterized in that, The method includes: Liquid raw materials are continuously fed into the gas-liquid reaction system (300) via a liquid-phase feed system (100), and gaseous intermediate products are continuously fed into the gas-liquid reaction system (300) via a continuous gas generation system (200). The continuous gas-liquid reaction between liquid-phase raw materials and gas-phase intermediate products is achieved through the gas-liquid reaction system (300) to obtain liquid-phase products; The target crystal is obtained by continuous crystallization of the liquid phase product through a crystallization system (400); The target crystals and the mother liquor are continuously filtered and separated by a continuous rotating disc filter (21); The continuous drying of the target crystal is achieved by using a continuous rotary dryer (22).

12. The production method according to claim 11, characterized in that, The continuous crystallization of the liquid-phase product through the crystallization system (400) to obtain the target crystal includes: Primary cooling crystallization is carried out through a primary tubular continuous crystallizer (17) to obtain a primary crystallization mother liquor containing crystal nuclei; The primary crystallization mother liquor is first cooled by a cooler (19) and then crystallized by a cooling circulation crystallizer (20). The generated target crystal is discharged through the crystal outlet of the cooling circulation crystallizer (20). The crystallization solution containing the crystal grains is discharged from the circulation outlet of the cooling circulation crystallizer (20), then pumped by a circulation pump (18) to the cooler (19) and then returned to the cooling circulation crystallizer (20) so that the crystal grains can grow again into the target crystal.

13. The production method according to claim 11, characterized in that, The continuous filtration and separation of the target crystal and the mother liquor via a continuous rotating disc filter (21) includes: The mixed crystal mother liquor, including the target crystals, is sprayed onto the filter disc by a distributor; The target crystals and the mother liquor are separated by the rotation of the filter disc and the vacuum operation. The separated crystal mother liquor is discharged from the bottom of the continuous rotary disc filter (21) and recycled back to the liquid phase feed system (100); The target crystal, having reached the target height, is discharged from the outlet via the discharge baffle.

14. The production method according to claim 11, characterized in that, The continuous drying of the target crystal via a continuous rotary dryer (22) includes: The continuous feeding of the target crystal is achieved by the spiral conveying device at the feed inlet of the continuous rotary dryer (22) and the rotation of the cylinder. The target crystals are obtained by heating and drying through the heat exchange jacket of the continuous rotary dryer (22), wherein protective gas is introduced from the outlet through the protective gas inlet so as to discharge the unreacted gaseous intermediate products after drying from the outlet. The continuous discharge of the target crystals is achieved through the spiral conveying device at the discharge port of the continuous rotary dryer (22) and the rotation of the cylinder.

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