Production system and production method for solid product
By introducing liquid phase feeding system, continuous gas production system, gas-liquid reaction system, crystallization system, continuous turntable filter and continuous rotary dryer in solid-state product production, the continuous production process of solid-state products is realized, solving the problem of difficulty in achieving continuous production processes in the existing technology, improving production efficiency and product quality, and reducing safety hazards.
Patent Information
- Application Number
- CN202510138197.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-07
- Publication Date
- 2025-05-09
AI Technical Summary
In industrial production, some solid products need to be produced in multiple steps, especially the gas phase intermediate product needs to be obtained first, and then the liquid phase product is obtained based on the gas phase intermediate product and liquid phase raw material, and finally the solid product can only be obtained after crystallization. The production process is difficult to achieve continuous production process, and manual feeding and other operations are required, which poses safety hazards and low production efficiency problems.
Provide a production system and production method for solid-state products, including a liquid phase feed system, a continuous gas production system, a gas-liquid reaction system, a crystallization system, a continuous turntable filter and a continuous rotary dryer. Through these systems, the continuous production process of liquid phase raw materials, a gas-phase intermediate product, a gas-liquid reaction, crystallization, filtration and drying is realized.
It has achieved the reduction of manual operations, avoiding the risk of harmful gas leakage in the production process, and improving production safety; at the same time, it has improved production efficiency, reduced production costs, improved production stability, reduced batch production differences, and effectively guaranteed product quality.
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Figure CN119960406A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the field of production of solid-state products, and in particular, to a production system and a production method for solid-state products. Background Art
[0002] In the fields of chemical industry, energy, environment and biochemistry, some solid products usually require multiple steps to produce. Take lithium hexafluorophosphate as an example. In industrial production, the preparation reaction of lithium hexafluorophosphate is LiF+PF5→LiPF6, that is, liquid LiF and gaseous PF5 react to generate liquid LiPF6, where gaseous PF5 is obtained by liquid-solid reaction of liquid AHF and solid PCl5. After obtaining liquid LiPF6, solid LiPF6 needs to be obtained through steps such as crystallization. For such solid products that need to first obtain gaseous intermediate products, then obtain liquid products based on gaseous intermediate products and liquid raw materials, and finally obtain solid products through crystallization, in industrial production, manual operations such as feeding are usually required, and the production process is difficult to achieve continuous operation. Summary of the invention
[0003] The present application at least provides a production system and production method for solid-state products, which can realize the continuous production process of liquid raw materials transportation, gas intermediate products transportation, gas-liquid reaction, crystallization, filtration and drying. The continuous production process can reduce manual operation, avoid the risk of leakage of harmful gases in the production process, and improve the safety of the production process; at the same time, automatic continuous operation can improve production efficiency and reduce production costs on the one hand, and on the other hand, it can also improve production stability, reduce differences in batch production, and effectively ensure product quality.
[0004] The present application provides a production system for solid products, which includes a liquid phase feeding system, a continuous gas production system, a gas-liquid reaction system, a crystallization system, a continuous rotary disk filter, and a continuous rotary dryer:
[0005] The discharge port of the liquid phase feeding system is connected to the liquid phase feeding port of the gas-liquid reaction system; the liquid phase feeding system is used to continuously transport liquid phase raw materials to the gas-liquid reaction system;
[0006] The discharge port of the continuous gas production system is connected to the gas phase feed port of the gas-liquid reaction system; the continuous gas production system is used to continuously transport the gas phase intermediate product to the gas-liquid reaction system;
[0007] The discharge port of the gas-liquid reaction system is connected to the feed port of the crystallization system; the gas-liquid reaction system is used to realize the continuous gas-liquid reaction between the liquid raw material and the gas intermediate product to obtain the liquid product, and the crystallization system is used to realize the continuous crystallization of the liquid product to obtain the target crystal;
[0008] The discharge port of the crystallization system is connected to the feed port of the continuous rotary disk filter, and the discharge port of the continuous rotary disk filter is connected to the feed port of the continuous rotary dryer; the continuous rotary disk filter is used to achieve continuous filtration and separation between the target crystal and the crystal mother liquor, and the continuous rotary dryer is used to achieve continuous drying of the target crystal.
[0009] The present application also provides a production method based on the production system, the method comprising:
[0010] The liquid phase raw material is continuously transported to the gas-liquid reaction system through the liquid phase feeding system, and the gas phase intermediate product is continuously transported to the gas-liquid reaction system through the continuous gas production system;
[0011] A continuous gas-liquid reaction between a liquid raw material and a gas intermediate product is achieved through a gas-liquid reaction system to obtain a liquid product;
[0012] Achieving continuous crystallization of the liquid phase product through a crystallization system to obtain target crystals;
[0013] The continuous filtration separation of target crystals and crystal mother liquor is achieved through a continuous rotating disk filter;
[0014] Continuous drying of the target crystals is achieved through a continuous rotary dryer.
[0015] In summary, the present application provides a production system and production method for solid products, which system includes a liquid-phase feeding system, a continuous gas production system, a gas-liquid reaction system, a crystallization system, a continuous turntable filter, and a continuous rotary dryer: the discharge port of the liquid-phase feeding system is connected to the liquid-phase feeding port of the gas-liquid reaction system; the liquid-phase feeding system is used to continuously transport liquid-phase raw materials to the gas-liquid reaction system; the discharge port of the continuous gas production system is connected to the gas-phase feeding port of the gas-liquid reaction system; the continuous gas production system is used to continuously transport gas-phase intermediate products to the gas-liquid reaction system; and the gas-liquid reaction system is used to continuously transport gas-phase intermediate products to the gas-liquid reaction system. The discharge port of the reaction system is connected with the feed port of the crystallization system; the gas-liquid reaction system is used to realize the continuous gas-liquid reaction between the liquid raw material and the gas intermediate product to obtain the liquid product, and the crystallization system is used to realize the continuous crystallization of the liquid product to obtain the target crystal; the discharge port of the crystallization system is connected with the feed port of the continuous rotary filter, and the discharge port of the continuous rotary filter is connected with the feed port of the continuous rotary dryer; the continuous rotary filter is used to realize the continuous filtration and separation between the target crystal and the crystal mother liquor, and the continuous rotary dryer is used to realize the continuous drying of the target crystal. Through the above system, the continuous production process of liquid raw material transportation, gas intermediate product transportation, gas-liquid reaction, crystallization, filtration and drying can be realized. The continuous production process can reduce manual operation, avoid the risk of leakage of harmful gases in the production process, and improve the safety of the production process; at the same time, automatic continuous operation can improve production efficiency and reduce production costs on the one hand, and on the other hand, it can also improve production stability, reduce the difference in batch production, and effectively ensure product quality.
[0016] Other advantages of the present application will be explained in more detail in conjunction with the following description and drawings.
[0017] It should be understood that the above description is only an overview of the technical solution of the present application, so that the technical means of the present application can be generally understood and then implemented according to the contents of the specification. In order to make the above and other purposes, features and advantages of the present application more obvious and easy to understand, the specific implementation methods of the present application are specifically described below by way of example. BRIEF DESCRIPTION OF THE DRAWINGS
[0018] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the following is a brief introduction to the drawings required for use in the embodiments. The drawings herein are incorporated into the specification and constitute a part of the specification. These drawings illustrate embodiments that conform to the present application and are used together with the specification to illustrate the technical solutions of the present application. It should be understood that the drawings only illustrate certain embodiments of the present application and should not be regarded as limiting the scope of protection. For ordinary technicians in this field, other relevant drawings can be obtained based on these drawings without creative work. Moreover, the same reference numerals are used to represent the same components throughout the drawings. In the drawings:
[0019] Figure 1 A schematic diagram of the structure of a production system for solid-state products provided in an embodiment of the present application;
[0020] Figure 2 A schematic diagram of the structure of a cooling cycle crystallizer provided in an embodiment of the present application;
[0021] Figure 3 A schematic diagram of the structure of multiple circulation outlets corresponding to the cooling circulation crystallizer provided in an embodiment of the present application.
[0022] In the drawings, the same or corresponding reference numerals represent the same or corresponding parts.
[0023] Among them, 100-liquid phase feeding system; 1-first dissolving tank; 2-second dissolving tank; 3-first metering pump; 4-second metering pump; 200-continuous gas production 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 circulation crystallizer; 201-paddle; 202-guide tube; 21-continuous rotary disc filter; 22-continuous rotary dryer. DETAILED DESCRIPTION
[0024] The exemplary embodiments of the present application will be described in more detail below with reference to the accompanying drawings. Although the exemplary embodiments of the present application are shown in the accompanying drawings, it should be understood that the present application can be implemented in various forms and should not be limited by the embodiments described herein. On the contrary, these embodiments are provided to enable a more thorough understanding of the present application and to fully convey the scope of the present application to those skilled in the art.
[0025] In the description of the embodiments of the present application, it should be understood that terms such as "including" or "having" are intended to indicate the presence of the disclosed features, numbers, components, parts or a combination thereof in the present specification, and do not exclude the possibility of the presence of one or more other features, numbers, components, parts or a combination thereof.
[0026] Unless otherwise specified, “ / ” means or. For example, A / B can mean A or B. The “and / or” in this article is merely a way to describe the association relationship of associated objects, indicating that three relationships can exist. For example, A and / or B can mean: A exists alone, A and B exist at the same time, and B exists alone.
[0027] The terms "first", "second", etc. are used only to distinguish the same or similar technical features for the convenience of description, and should not be understood as indicating or implying the relative importance or quantity of these technical features. Thus, the features defined by "first", "second", etc. may explicitly or implicitly include one or more of such features. In the description of the embodiments of the present application, unless otherwise specified, the term "plurality" means two or more than two.
[0028] Taking lithium hexafluorophosphate as an example, it is necessary to first obtain a gas phase intermediate product, then obtain a liquid phase product based on the gas phase intermediate product and a liquid phase raw material, and finally obtain a solid product through crystallization. In industrial production, manual operations such as adding materials are usually required, and the production process is difficult to achieve continuity.
[0029] In view of this, the present application provides a production system and production method for solid-state products, which can realize the continuous production process of liquid raw materials transportation, gas intermediate products transportation, gas-liquid reaction, crystallization, filtration and drying. The continuous production process can reduce manual operation, avoid the risk of leakage of harmful gases in the production process, and improve the safety of the production process; at the same time, automatic continuous operation can improve production efficiency and reduce production costs on the one hand, and on the other hand, it can also improve production stability, reduce the differences caused by batch production, and effectively ensure product quality.
[0030] The present application will be described in detail below with reference to the accompanying drawings and in combination with embodiments.
[0031] like Figure 1 As shown, the production system for solid products includes a liquid phase feeding system 100, a continuous gas production system 200, a gas-liquid reaction system 300, a crystallization system 400, a continuous rotary disk filter 21, and a continuous rotary dryer 22:
[0032] The discharge port of the liquid-phase feeding system 100 is connected to the liquid-phase feeding port of the gas-liquid reaction system 300 ; the liquid-phase feeding system 100 is used to continuously transport liquid-phase raw materials to the gas-liquid reaction system 300 .
[0033] Specifically, the liquid raw material usually needs to be dissolved, so 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, that is, the first dissolving tank 1 and the second dissolving tank 2 are used to dissolve the liquid raw material. In actual applications, the first dissolving tank 1 and the second dissolving tank 2 may be provided with a heat exchange jacket or a coil to ensure the dissolution temperature. Accordingly, on the premise of providing the first dissolving tank 1 and the second dissolving tank 2, a corresponding first metering pump 3 and a second metering pump 4 are also provided to realize the quantitative delivery of the liquid raw material. In this embodiment, the continuous delivery of the liquid raw material can be realized by alternating the delivery of multiple dissolving tanks.
[0034] The discharge port of the continuous gas production system 200 is connected to the gas phase feed port of the gas-liquid reaction system 300; the continuous gas production system 200 is used to continuously transport the gas phase intermediate product 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] Relevant reactions can be carried out in the liquid-solid reactor 5 to generate gaseous intermediates. In practical applications, the liquid-solid reactor 5 can be a single-cantilever conical liquid-solid reactor, and the internal stirring paddle is a single-cantilever stirring paddle, which can rotate while revolving around the axis of the liquid-solid reactor 5, thereby achieving 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 set on the outside of the conical cylinder of the liquid-solid reactor 5; a condenser can be set 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, and the gas buffer tank 6 plays a buffering role for the gas phase intermediate product from the liquid-solid reactor 5. A mixing plug-in can be provided inside the gas buffer tank 6, and when the gas phase intermediate product is a multi-component gas, uniform mixing of the multi-component gas can be achieved.
[0038] The discharge port of the gas-liquid reaction system 300 is connected to the feed port of the crystallization system 400; the gas-liquid reaction system 300 is used to realize the continuous gas-liquid reaction between the liquid raw material and the gas intermediate product to obtain the liquid product, and the crystallization system 400 is used to realize the continuous crystallization of the liquid product to obtain the target crystal.
[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. The continuous reaction of the liquid raw material and the gas intermediate product is achieved through multiple groups of gas-liquid reactors and gas-liquid separators, wherein the first gas-liquid reactor 8 is used to achieve complete reaction of the liquid raw material, the first gas-liquid separator 9 is used to achieve recovery of excess gas intermediate products and collection of the liquid products generated by the first gas-liquid reactor 8, and the second gas-liquid reactor 11 realizes the complete reaction of excess gas-phase intermediate products, the second gas-liquid separator 12 realizes the recovery of excess liquid-phase raw materials, the third gas-liquid reactor 14 realizes the complete reaction of excess liquid-phase raw materials, and the first gas-liquid separator 9 also realizes the collection of liquid products produced 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 gas-phase intermediate products and liquid-phase raw materials are fully reacted, and the mixing of liquid-phase raw materials and liquid-phase products is avoided, thereby ensuring product quality, and on the other hand, the maximum utilization of liquid-phase raw materials and gas-phase intermediate products is realized, 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 target crystals.
[0041] The discharge port of the crystallization system 400 is connected to the feed port of the continuous rotary disk filter 21, and the discharge port of the continuous rotary disk filter 21 is connected to the feed port of the continuous rotary dryer 22; the continuous rotary disk filter 21 is used to achieve continuous filtration and separation between the target crystals and the crystal mother liquor, and the continuous rotary dryer 22 is used to achieve continuous drying of the target crystals.
[0042] Specifically, after the target crystals are obtained through the crystallization system 400, in order to ensure the quality of the target crystals, continuous filtration separation between the target crystals and the crystal mother liquor is achieved through a continuous rotary disk filter 21, and continuous drying of the target crystals is achieved through a continuous rotary dryer 22, thereby obtaining the final target crystals.
[0043] Through the above-mentioned production system, the continuous production process of liquid raw material transportation, gas intermediate product transportation, gas-liquid reaction, crystallization, filtration and drying can be realized. The continuous production process can reduce manual operation, avoid the risk of leakage of harmful gases in the production process, and improve the safety of the production process; at the same time, automatic continuous operation can improve production efficiency and reduce production costs on the one hand, and on the other hand, it can also improve production stability, reduce the differences in batch production, and effectively ensure product quality.
[0044] In a possible implementation, the crystallization system 400 includes a primary tubular continuous crystallizer 17 and a secondary circulation crystallization system:
[0045] The discharge port of the gas-liquid reaction system 300 is connected to the feed port of the first-stage tubular continuous crystallizer 17, and the first-stage tubular continuous crystallizer 17 is used to achieve the first-stage cooling crystallization of the liquid phase product;
[0046] The secondary circulation crystallization system includes a circulation pump 18, a cooler 19 and a cooling circulation crystallizer 20. The discharge port of the primary tubular continuous crystallizer 17 is connected to the feed port of the cooler 19, the discharge port of the cooler 19 is connected to the feed port of the cooling circulation crystallizer 20, and a circulation pump 18 is arranged between the circulation outlet of the cooling circulation crystallizer 20 and the feed port of the cooler 19; the cooler 19 is used to meet the cooling demand of the secondary circulation crystallization system, the cooling circulation crystallizer 20 is used to realize crystal generation to obtain target crystals and the discharge of target crystals, and the circulation pump 18 is used to realize the circulation transportation of the crystallization solution including the crystal grains from the circulation outlet of the cooling circulation crystallizer 20 to the cooler 19 and then back to the cooling circulation crystallizer 20.
[0047] Specifically, in order to ensure sufficient crystallization of the liquid phase product, in this embodiment, the crystallization system 400 includes a first-stage tubular continuous crystallizer 17 for first-stage cooling crystallization and a second-stage circulation crystallization system for second-stage cooling crystallization. The first-stage tubular continuous crystallizer 17 can realize the nucleation and growth of crystals; the cooler 19 included in the second-stage circulation crystallization system can be used to realize the cooling demand of the second-stage circulation crystallization system. In practical applications, the cooler 19 can use a single cooling or multiple parallel cooling to improve the cooling efficiency; the cooling circulation crystallizer 20 included in the second-stage circulation crystallization system can realize crystal generation to obtain target crystals and the discharge of target crystals, that is, the generated target crystals can be discharged through the crystal outlet of the cooling circulation crystallizer 20; the circulation pump 18 included in the second-stage circulation crystallization system can provide power for the circulation of the crystallization solution, so that the crystallization solution including fine crystals is discharged from the circulation outlet of the cooling circulation crystallizer 20, passes through the circulation pump 18 to the cooler 19 and then returns to the cooling circulation crystallizer 20 so that the fine crystals grow again into target crystals, that is, the circulation pump 18 can realize the circulation of the crystallization solution to ensure sufficient crystallization.
[0048] It should be noted that, through the secondary circulation crystallization system, the target crystals that meet the requirements can be discharged from the crystal outlet of the cooling circulation crystallizer 20, while the fine grains that do not meet the requirements can be discharged from the circulation outlet of the cooling circulation crystallizer 20, pass through the circulation pump 18 to the cooler 19, and then return to the cooling circulation crystallizer 20 to be crystallized again until they grow into target crystals and are discharged from the crystal outlet of the cooling circulation crystallizer 20.
[0049] In a possible implementation, the bottom of the cooling circulation crystallizer 20 is a W-shaped bottom, a paddle 201 is disposed at the inner center of the cooling circulation crystallizer 20 , and a guide tube 202 is disposed outside the paddle 201 .
[0050] Specifically, Figure 2 As shown, the internal flow pattern of the cooling circulation crystallizer 20 can be changed by the combination of the W-shaped bottom, the paddle 201 and the guide tube 202, so that the internal fluid is divided into an inner liquid column inwardly and an outer liquid column outwardly with the guide tube 202 as the boundary. The paddle 201 can make the inner liquid column always run from top to bottom, and can move smoothly upward after hitting the W-shaped bottom, thereby enhancing the heat exchange effect between the central fluid and the inner wall of the cooling circulation crystallizer 20, improving the temperature uniformity, and allowing the crystal to grow in an environment with the same flow rate and temperature, thereby effectively preventing the occurrence of violent crystallization and crystal doping, improving the consistency and uniformity of the grains, promoting the formation of "spherical" target crystals, and facilitating continuous production.
[0051] In a possible implementation, a heat exchange jacket is provided outside the cooling circulation crystallizer 20, and the heat exchange jacket can further promote the cooling crystallization process and reduce the crystallization time.
[0052] In one possible implementation, considering that the fine grains that do not reach the target crystal size have different sizes, the fine grains of different sizes will have different suspension positions, so the cooling circulation crystallizer 20 can be provided with multiple circulation outlets, and the multiple circulation outlets correspond one-to-one to the suspension positions of multiple crystals with different sizes, and each of the multiple circulation outlets is equipped with a corresponding circulation pump 18 and cooler 19.
[0053] Specifically, Figure 3 As shown, in actual applications, the cooling circulation crystallizer 20 can be provided with two circulation outlets at different heights, the first circulation outlet is provided with a corresponding circulation pump 18A and a cooler 19A, and the second circulation outlet is provided with a corresponding circulation pump 18B and a cooler 19B.
[0054] Through multiple circulation outlets and multiple circulation pumps 18 and multiple coolers 19 corresponding to the multiple circulation outlets, graded cooling of the crystallization solution including grains of different sizes can be achieved. That is, different feed circulation ratios and cooling rates can be set according to the different grain sizes of the grains at different suspension positions, and the growth process of crystals of different sizes can be directionally controlled to enhance the consistency of the crystal form and particle size at the outlet and improve product quality.
[0055] In a possible implementation, a static mixing plug is provided inside the first-stage tubular continuous crystallizer 17, and the static mixing plug has a cutting surface. The static mixing plug with a cutting surface can achieve uniformity of radial temperature distribution in the tube, improve crystallization quality, and strengthen turbulence intensity in the tube to prevent scaling of crystals in the tube from clogging the pipeline.
[0056] In a possible implementation, a heat exchange jacket is disposed outside the first-stage tubular continuous crystallizer 17, and the heat exchange jacket can ensure the cooling requirement during the crystallization process, that is, gradient cooling can be achieved through the external heat exchange jacket.
[0057] In one possible implementation, a filter turntable is provided at the inner bottom end of the continuous turntable filter 21, a distributor is provided at the upper part of the filter turntable, and a discharge baffle is provided at the inner top end of the continuous turntable filter 21; the distributor is used to spray the mixed crystal mother liquor including the target crystals onto the filter turntable, the filter turntable is used to achieve filtering separation between the target crystals and the crystal mother liquor, and the discharge baffle is used to discharge the target crystals that have reached the target height.
[0058] Specifically, a filter turntable is provided at the inner bottom end of the continuous turntable filter 21. The filter turntable can be a circular filter turntable that can rotate 360° in a circle. A distributor is provided on the upper part of the filter turntable. The distributor sprays the mixed crystal mother liquor including the target crystals on the filter turntable. As the filter turntable rotates, the bottom of the filter turntable can be vacuum filtered to achieve filtering and separation between the target crystals and the crystal mother liquor. The separated crystal mother liquor can be discharged from the bottom of the continuous turntable filter 21 and can be recycled to the dissolution tank in the liquid phase feeding system 100 for recycling. The remaining target crystals are accumulated on the filter turntable. After reaching the target height, they can be discharged through the discharge baffle.
[0059] In one possible implementation, the continuous rotary dryer 22 is tilted based on a preset tilt angle, the feed port and the discharge port of the continuous rotary dryer 22 are both provided with a screw conveying device, the interior of the continuous rotary dryer 22 is provided with a lifting plate, the exterior of the continuous rotary dryer 22 is provided with a heat exchange jacket, and the discharge port of the continuous rotary dryer 22 is provided with a protective gas inlet.
[0060] Specifically, the continuous rotary dryer 22 is tilted based on a preset tilt angle, that is, it has a certain tilt angle. The continuous entry and exit process of the target crystal can be realized by the spiral conveying device arranged at the feed port and the discharge port. The continuous rotary dryer 22 is provided with a lifting plate inside to shorten the drying time of the target crystal. The continuous rotary dryer 22 is provided with a heat exchange jacket outside to meet the heating requirements of the target crystal during the drying process. The discharge port of the continuous rotary dryer 22 is provided with a protective gas inlet, and a protective gas such as nitrogen can be introduced into the discharge port through the protective gas inlet so that the gaseous intermediate product volatilized after drying can be discharged from the discharge port.
[0061] In a 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 tail gas exhaust port of the gas-liquid reaction system 300 is connected to the air inlet of the gas-phase intermediate product recovery tower 15, the gas outlet of the gas-phase intermediate product recovery tower 15 is connected to the feed port of the temporary storage tank 16, and the discharge port of the temporary storage tank 16 is connected to the feed port of the liquid-phase feeding system 100; the gas-phase intermediate product recovery tower 15 is used to recover the gas-phase intermediate products remaining in the tail 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.
[0063] Specifically, the gas phase intermediate product recovery tower 15 is used to recover the gas phase intermediate product remaining in the tail gas in the gas-liquid reaction system 300, and other components in the tail gas can be discharged from the top of the gas phase intermediate product recovery tower 15 for tail gas treatment. The temporary storage tank 16 can be used to temporarily store the recovered gas phase intermediate product in liquid form, and the recovered gas phase intermediate product can be temporarily stored in liquid form after condensation. The discharge port of the temporary storage tank 16 is connected to the feed port of the liquid phase feeding system 100, for example, it can be connected to the feed port of the dissolving tank in the liquid phase feeding system 100, so that the solution in the temporary storage tank 16 can be returned to the dissolving tank and used as a solvent to dissolve the solid phase raw material, thereby realizing recycling.
[0064] The following is a method example to illustrate the production method based on the above production system provided by the present application, and the method includes:
[0065] S401 , continuously conveying liquid raw materials to the gas-liquid reaction system 300 through the liquid feeding system 100 , and continuously conveying gas intermediate products to the gas-liquid reaction system 300 through the continuous gas production system 200 .
[0066] S402, realizing a continuous gas-liquid reaction between the liquid raw material and the gas intermediate product through the gas-liquid reaction system 300 to obtain a liquid product.
[0067] S403, achieving continuous crystallization of the liquid phase product through the crystallization system 400 to obtain target crystals.
[0068] S404, achieving continuous filtration separation of target crystals and crystal mother liquor through the continuous rotary disk filter 21.
[0069] S405 , achieving continuous drying of the target crystals through the continuous rotary dryer 22 .
[0070] In a possible implementation, in S403, the liquid phase product is continuously crystallized by the crystallization system 400 to obtain the target crystal, including:
[0071] Performing primary cooling crystallization through a primary tubular continuous crystallizer 17 to obtain a primary crystallization mother liquid including crystal nuclei;
[0072] The primary crystallization mother liquor is first cooled by the cooler 19 and then passes through the cooling circulation crystallizer 20 to generate crystals. The generated target crystals are discharged through the crystal outlet of the cooling circulation crystallizer 20. The crystallization solution including the crystal grains is discharged from the circulation outlet of the cooling circulation crystallizer 20, passes through the circulation pump 18 to the cooler 19, and then returns to the cooling circulation crystallizer 20 so that the crystal grains can grow again to become target crystals.
[0073] Specifically, a first-stage cooling crystallization is performed through the first-stage tubular continuous crystallizer 17 to obtain a first-stage crystallization mother liquor including crystal nuclei. A first-stage cooling crystallization process is performed in the first-stage tubular continuous crystallizer 17 to realize the crystal nucleation process. The temperature reduction gradient can be controlled by using 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 the 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, and the generated target crystals can be discharged through the crystal outlet of the cooling circulation crystallizer 20, wherein the crystallization solution including the grains can be discharged from the circulation outlet of the cooling circulation crystallizer 20 and then pass through the circulation pump 18 to the cooler 19 and then return to the cooling circulation crystallizer 20. Through the circulation process, the fine grains can be further grown until they become target crystals, and then discharged from the crystal outlet of the cooling circulation crystallizer 20. This process can continuously have the entry of the primary crystallization mother liquor and the discharge of the target crystals to achieve continuous crystallization.
[0075] In a possible implementation, in S404, the continuous rotating disk filter 21 is used to achieve continuous filtration separation of target crystals and crystal mother liquor, including:
[0076] Spraying the mixed crystal mother liquor including the target crystal onto the filter turntable through a distributor;
[0077] The target crystals and the crystal mother liquor are filtered and separated by the rotation of the filter turntable and the vacuum operation;
[0078] The separated crystal mother liquor is discharged from the bottom of the continuous rotary disc filter 21 and recycled to the liquid phase feeding system 100 for recycling;
[0079] The target crystals reaching the target height are discharged from the discharge port through the discharge baffle.
[0080] In a possible implementation, in S405, the continuous drying of the target crystals is achieved by the continuous rotary dryer 22, including:
[0081] The continuous feeding of the target crystals is achieved by the screw conveyor at the feed port of the continuous rotary dryer 22 and the rotation of the cylinder;
[0082] The heat exchange jacket of the continuous rotary dryer 22 is used for heating and drying to obtain the target crystal after drying, wherein the protective gas is introduced from the discharge port through the protective gas inlet so that the gas phase intermediate product which has not been completely reacted after drying is discharged from the discharge port;
[0083] The continuous discharge of 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 rotation of the spiral conveying device and the cylinder.
[0085] The target crystals after drying are obtained by heating through the heat exchange jacket of the continuous rotary dryer 22, wherein a protective gas such as nitrogen can be introduced from the discharge port through the protective gas inlet so that the dried incompletely reacted gas intermediate product can be discharged from the discharge port, and the discharged gas intermediate product and protective gas can be introduced into the gas intermediate product recovery tower 15 for recovery, thereby realizing the recycling of the gas intermediate product.
[0086] In a possible implementation, the method includes:
[0087] The tail gas of the gas-liquid reaction system 300 is transported to the gas-phase intermediate product recovery tower 15 to achieve the recovery of the gas-phase intermediate product, and the remaining other components can be subjected to tail gas treatment; the recovered gas-phase intermediate product can enter the temporary storage tank 16 in liquid form for temporary storage, and the solution after temporary storage can be transported to the dissolution tank of the liquid-phase feeding system 100 for recycling.
[0088] The production system and production method provided in the embodiments of the present application are described below using lithium hexafluorophosphate as an example:
[0089] Step 1: Continuous delivery of lithium fluoride solution.
[0090] Step 1-1: Inject solid lithium fluoride and AHF solution into the first dissolution tank 1 and the second dissolution tank 2 respectively, and use an external heat exchange jacket or coil AHF solution to control the temperature and dissolve to form a lithium fluoride solution, wherein the mass ratio of lithium fluoride to hydrogen fluoride is 1:5 to 1:25, and the dissolution temperature is -2 to 16°C.
[0091] Step 1-2: Start the first metering pump 3, control the flow rate, and transport the lithium fluoride solution in the first dissolution tank 1 to the continuous phase main line of the first ejector 7.
[0092] Step 1-3: After the lithium fluoride solution in the first dissolution tank 1 is transported, the first metering pump 3 is closed, and the second metering pump 4 is started to transport the lithium fluoride solution in the second dissolution tank 2 to the continuous phase main line of the first ejector 7.
[0093] Step 1-4: while starting the second metering pump 4, close the first metering pump 3, re-inject the solid lithium fluoride and the AHF solution into the first dissolving tank 1, and repeat the feeding operation; the continuous conveying process of the lithium fluoride solution is realized by the alternating feeding, dissolving and discharging process of the dissolving tank; multiple dissolving tanks can be arranged in parallel, and the feeding and dissolving time is less than the continuous conveying time of the material in a single kettle.
[0094] Step 2: Continuous reaction and transportation of phosphorus pentafluoride gas.
[0095] Step 2-1: Start the phosphorus pentachloride continuous automatic feeding device of the liquid-solid reactor 5, continuously inject phosphorus pentachloride solid, and the feeding process is protected by nitrogen; synchronously and continuously inject AHF solution, start the motor, stir, and carry out liquid-solid reaction of phosphorus pentachloride and hydrogen fluoride in the liquid-solid reactor 5 to produce phosphorus pentafluoride gas; use the heat exchange jacket or coil outside the conical cylinder of the liquid-solid reactor 5 to control the reaction temperature. 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 and revolution speed of the stirring shaft are 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, etc. enters the gas buffer tank 6.
[0097] Step 2-3: The mixed gas is mixed evenly by the mixing plug inside the gas buffer tank 6 to ensure the 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 transport the mixed gas in the 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 and phosphorus pentafluoride gas.
[0100] Step 3-1: The first ejector 7 ejects and mixes the lithium fluoride solution from the dissolution tank and the phosphorus pentafluoride gas from the gas buffer tank 6 and enters the first gas-liquid reactor 8.
[0101] Step 3-2: A gas-liquid reaction of fresh lithium fluoride solution and phosphorus pentafluoride is carried out in the first gas-liquid reactor 8, and the reaction temperature is controlled by an external heat exchange jacket; at the same time, phosphorus pentafluoride gas from the gas buffer tank 6 is injected into the gas replenishment port of the first gas-liquid reactor 8 to ensure that the lithium fluoride solution reacts completely. 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 and the remaining gas (unreacted phosphorus pentafluoride, hydrogen fluoride, hydrogen chloride, and nitrogen) after the reaction in the first gas-liquid reactor 8 enter the first gas-liquid separator 9, and the gas-liquid separation process is completed in the first gas-liquid separator 9.
[0103] Step 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 synchronously transported to the continuous phase main line of the second ejector 10.
[0104] Step 3-5: The second ejector 10 ejects and mixes the lithium fluoride solution from the dissolution tank and the remaining gas separated from the first gas-liquid separator 9 , and the mixture enters the second gas-liquid reactor 11 .
[0105] Step 3-6: The second gas-liquid reactor 11 carries out a gas-liquid reaction between a fresh lithium fluoride solution and the phosphorus pentafluoride gas that has not reacted completely in the first gas-liquid reactor 8, and an excess of lithium fluoride solution is used 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; and the residence time is 0.5 min to 120 min.
[0106] Step 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, and the gas-liquid separation process is completed in the second gas-liquid separator 12.
[0107] Step 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; the fresh gas from the gas buffer tank 6 simultaneously enters the discrete phase side pipeline of the third ejector 13.
[0108] Step 3-9: The third ejector 13 is used to eject and mix the product lithium hexafluorophosphate from the second gas-liquid separator 12 , the remaining lithium fluoride solution and the fresh gas from the gas buffer tank 6 into the third tubular continuous gas-liquid reactor 14 .
[0109] Step 3-10: A gas-liquid reaction is carried out in the third gas-liquid reactor 14 between the lithium fluoride solution that has not been completely reacted in the second gas-liquid reactor 11 and the fresh phosphorus pentafluoride gas. At the same time, the fresh gas from the gas buffer tank 6 enters the gas replenishment port of the third gas-liquid reactor 14. The phosphorus pentafluoride is in excess to ensure that the lithium fluoride solution reacts completely. 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 liquid and the remaining gas after the reaction in the third gas-liquid reactor 14 enter the first gas-liquid separator 9 again; repeat steps 3-4 to 3-10 to achieve continuous gas-liquid reaction.
[0111] Step 4: Exhaust treatment.
[0112] Step 4-1: After separation by the second gas-liquid separator 12, the gas (hydrogen fluoride, hydrogen chloride, nitrogen) enters the gas phase intermediate product recovery tower 15 to achieve the recovery of hydrogen fluoride; the remaining hydrogen chloride and nitrogen enter the subsequent alkali liquid tail gas treatment stage; the top temperature of the recovery tower is -20°C to 15°C; the operating pressure is 0.3MPa to 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 dissolution tank and used as a solvent to dissolve the solid lithium fluoride raw material to achieve 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; a first-stage cooling crystallization process is carried out in the first-stage tubular continuous crystallizer 17 to realize the nucleation process of the crystal, and the cooling gradient is controlled by an external jacket; the first-stage crystallization cooling gradient is 0 to -15°C and -15°C to -30°C; 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 circulation crystallization system.
[0117] Step 5-3: The primary crystallization mother liquor enters the cooling circulation crystallizer 20 through the cooler 19, and the cooler 19 further cools the crystallization mother liquor; the crystal growth process is carried out in the cooling circulation crystallizer 20, and the external heat exchange jacket or coil further strengthens the cooling process; the grown crystals are discharged from the crystal outlet of the cooling circulation crystallizer 20; the crystallization solution containing fine crystals is circulated from the cooling circulation crystallizer 20 outlet through the circulation pump 18 to the cooler 19 and then returned to the cooling circulation crystallizer 20; the fine crystals are further grown through the circulation process until the crystals meet the target requirements and are discharged from the crystal outlet of the cooling circulation crystallizer 20; in this process, the mother liquor is continuously introduced and the formed crystals are discharged, realizing a continuous crystallization process. The secondary crystallization temperature gradient is -30℃~-50℃, the circulating feed ratio is 20~100, the solid content of the outlet crystal solution is 10%~35%, and the residence time is 1h~7h.
[0118] Step 6: Continuous separation of lithium hexafluorophosphate and remaining mother liquor.
[0119] Step 6-1: The formed crystals and the mother liquor enter the continuous rotary disc filter 21, and the lithium hexafluorophosphate crystals and the mother liquor are continuously separated by the rotation and vacuum operation of the internal filter rotary disc.
[0120] Step 6-2: The separated mother liquor (uncrystallized lithium hexafluorophosphate solution and hydrogen fluoride) is discharged from the bottom of the continuous rotary disc filter 21 and recovered to the dissolution tank for recycling.
[0121] Step 6-3: The filtered lithium hexafluorophosphate crystals are continuously discharged from the side of the continuous rotary disk 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 continuous entry and exit process of the crystals is realized by the rotation of the spiral conveying device and the cylinder; the heat exchange jacket or coil outside the continuous rotary dryer 22 is used for heating and drying; after drying, a solid product is obtained; the drying temperature is 20°C to 90°C, and the residence time is 0.5h to 10h.
[0124] Step 7-2: During the continuous drying process, nitrogen 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 can be introduced into the gas phase intermediate product recovery tower 15 for subsequent separation and recovery, thereby realizing the recycling of hydrogen fluoride.
[0125] It can be seen that the present application provides a production system and production method for solid products, which system includes a liquid-phase feeding system, a continuous gas production system, a gas-liquid reaction system, a crystallization system, a continuous turntable filter, and a continuous rotary dryer: the discharge port of the liquid-phase feeding system is connected to the liquid-phase feeding port of the gas-liquid reaction system; the liquid-phase feeding system is used to continuously transport liquid-phase raw materials to the gas-liquid reaction system; the discharge port of the continuous gas production system is connected to the gas-phase feeding port of the gas-liquid reaction system; the continuous gas production system is used to continuously transport gas-phase intermediate products to the gas-liquid reaction system; the gas-liquid reaction The discharge port of the reaction system is connected with the feed port of the crystallization system; the gas-liquid reaction system is used to realize the continuous gas-liquid reaction between the liquid raw material and the gas intermediate product to obtain the liquid product, and the crystallization system is used to realize the continuous crystallization of the liquid product to obtain the target crystal; the discharge port of the crystallization system is connected with the feed port of the continuous rotary filter, and the discharge port of the continuous rotary filter is connected with the feed port of the continuous rotary dryer; the continuous rotary filter is used to realize the continuous filtration and separation between the target crystal and the crystal mother liquor, and the continuous rotary dryer is used to realize the continuous drying of the target crystal. Through the above system, the continuous production process of liquid raw material transportation, gas intermediate product transportation, gas-liquid reaction, crystallization, filtration and drying can be realized. The continuous production process can reduce manual operation, avoid the risk of leakage of harmful gases in the production process, and improve the safety of the production process; at the same time, automatic continuous operation can improve production efficiency and reduce production costs on the one hand, and on the other hand, it can also improve production stability, reduce the difference in batch production, and effectively ensure product quality.
[0126] In the description of this specification, the description with reference to the terms "some possible embodiments", "some embodiments", "examples", "specific examples", or "some examples" means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present application, and the above terms do not necessarily represent the same embodiment or example. Moreover, the described specific features, structures, materials or characteristics may be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art may combine and combine the different embodiments or examples described in this specification and the features of the different embodiments or examples, unless they are contradictory.
[0127] Although the spirit and principle of the present application have been described above with reference to several specific embodiments, it should be understood that the present application is not limited to the disclosed specific embodiments, and the division of various aspects does not mean that the features in these aspects cannot be combined. The present application is intended to cover various modifications and equivalent arrangements included in the spirit and scope of the attached claims.
Claims
1. A production system for solid-state products, characterized in that: The system comprises a liquid phase feeding system (100), a continuous gas production system (200), a gas-liquid reaction system (300), a crystallization system (400), a continuous rotary disk filter (21), and a continuous rotary dryer (22): The discharge port of the liquid-phase feeding system (100) is connected to the liquid-phase feeding port of the gas-liquid reaction system (300); the liquid-phase feeding system (100) is used to continuously transport liquid-phase raw materials to the gas-liquid reaction system (300); The discharge port of the continuous gas production system (200) is connected to the gas phase feed port of the gas-liquid reaction system (300); the continuous gas production system (200) is used to continuously transport the gas phase intermediate product to the gas-liquid reaction system (300); The discharge port of the gas-liquid reaction system (300) is connected to the feed port of the crystallization system (400); the gas-liquid reaction system (300) is used to realize a continuous gas-liquid reaction between a liquid raw material and a gas intermediate product to obtain a liquid product, and the crystallization system (400) is used to realize continuous crystallization of the liquid product to obtain a target crystal; The discharge port of the crystallization system (400) is connected to the feed port of the continuous rotary disk filter (21), and the discharge port of the continuous rotary disk filter (21) is connected to the feed port of the continuous rotary dryer (22); the continuous rotary disk filter (21) is used to achieve continuous filtration separation between target crystals and crystal mother liquor, and the continuous rotary dryer (22) is used to achieve continuous drying of target crystals.
2. The production system for solid-state products according to claim 1, characterized in that: The crystallization system (400) comprises a primary tubular continuous crystallizer (17) and a secondary circulation crystallization system: The discharge port of the gas-liquid reaction system (300) is connected to the feed port of a first-stage tubular continuous crystallizer (17), and the first-stage tubular continuous crystallizer (17) is used to achieve first-stage cooling crystallization of the liquid phase product; The secondary circulation crystallization system comprises a circulation pump (18), a cooler (19) and a cooling circulation crystallizer (20); the discharge port of the primary tubular continuous crystallizer (17) is connected to the feed port of the cooler (19); the discharge port of the cooler (19) is connected to the feed port of the cooling circulation crystallizer (20); a circulation pump (18) is arranged between the circulation outlet of the cooling circulation crystallizer (20) and the feed port of the cooler (19); the cooler (19) is used to meet the cooling requirement of the secondary circulation crystallization system; the cooling circulation crystallizer (20) is used to achieve crystal generation to obtain target crystals and discharge target crystals; the circulation pump (18) is used to achieve the circulation transportation of the crystal solution including the crystal grains from the circulation outlet of the cooling circulation crystallizer (20) to the cooler (19) and then back to the cooling circulation crystallizer (20).
3. The production system for solid products according to claim 2, characterized in that: The equipment bottom of the cooling circulation crystallizer (20) is a W-shaped bottom, a paddle (201) is arranged at the inner center of the cooling circulation crystallizer (20), and a guide tube (202) is arranged outside the paddle (201).
4. The production system for solid-state products according to claim 3, characterized in that: A heat exchange jacket is arranged outside the cooling circulation crystallizer (20).
5. The production system for solid products according to claim 4, characterized in that: The cooling circulation crystallizer (20) is provided with a plurality of circulation outlets, the plurality of circulation outlets corresponding one by one to the suspension positions of a plurality of crystals of different sizes, and each of the plurality of circulation outlets is equipped with a corresponding circulation pump (18) and a cooler (19).
6. The production system for solid products according to claim 2, characterized in that: The first-stage tubular continuous crystallizer (17) is provided with a static mixing plug inside, and the static mixing plug has a cutting surface.
7. The production system for solid products according to claim 6, characterized in that: The first-stage tubular continuous crystallizer (17) is provided with a heat exchange jacket on the outside.
8. The production system for solid-state products according to claim 1, characterized in that: The bottom end of the interior of the continuous rotary disc filter (21) is provided with a filter disc, the top of the filter disc is provided with a distributor, and the top end of the interior of the continuous rotary disc filter (21) is provided with a discharge baffle; the distributor is used to spray a mixed crystal mother liquor including target crystals onto the filter disc, the filter disc is used to achieve filtering separation between the target crystals and the crystal mother liquor, and the discharge baffle is used to discharge the target crystals that have 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 tilted based on a preset tilt angle, the feed port and the discharge port of the continuous rotary dryer (22) are both provided with a screw conveying device, the interior of the continuous rotary dryer (22) is provided with a lifting plate, the exterior of the continuous rotary dryer (22) is provided with a heat exchange jacket, and the discharge port of the continuous rotary dryer (22) is provided with a protective gas inlet.
10. The production system for solid products according to claim 1, characterized in that: The gas-liquid reaction system (300) comprises a gas phase intermediate product recovery tower (15) and a temporary storage tank (16): The tail gas exhaust port of the gas-liquid reaction system (300) is connected to the air inlet of the gas-phase intermediate product recovery tower (15), the gas outlet of the gas-phase intermediate product recovery tower (15) is connected to the feed port of the temporary storage tank (16), and the discharge port of the temporary storage tank (16) is connected to the feed port of the liquid-phase feeding system (100); the gas-phase intermediate product recovery tower (15) is used to recover the gas-phase intermediate products remaining in the tail 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 to 10, characterized in that: The method comprises: Continuously conveying liquid raw materials to a gas-liquid reaction system (300) through a liquid-phase feeding system (100), and continuously conveying gas-phase intermediate products to the gas-liquid reaction system (300) through a continuous gas production system (200); A continuous gas-liquid reaction between a liquid raw material and a gas intermediate product is achieved through the gas-liquid reaction system (300) to obtain a liquid product; Achieving continuous crystallization of the liquid phase product through a crystallization system (400) to obtain target crystals; A continuous filtration separation of target crystals and crystal mother liquor is achieved by a continuous rotating disk filter (21); The continuous drying of the target crystals is achieved by a continuous rotary dryer (22).
12. The production method according to claim 11, characterized in that: The method of achieving continuous crystallization of the liquid phase product by the crystallization system (400) to obtain target crystals comprises: Performing primary cooling crystallization through a primary tubular continuous crystallizer (17) to obtain a primary crystallization mother liquid including crystal nuclei; The primary crystallization mother liquor is first cooled by a cooler (19) and then passes through a cooling circulation crystallizer (20) to generate crystals. The generated target crystals are discharged through the crystal outlet of the cooling circulation crystallizer (20). The crystallization solution including the crystal grains is discharged from the circulation outlet of the cooling circulation crystallizer (20), passes through a circulation pump (18) to the cooler (19), and then returns to the cooling circulation crystallizer (20) so that the crystal grains grow again to become target crystals.
13. The production method according to claim 11, characterized in that: The method of achieving continuous filtration separation of target crystals and crystal mother liquor by using a continuous rotating disk filter (21) comprises: Spraying the mixed crystal mother liquor including the target crystal onto the filter turntable through a distributor; The target crystals and the crystal mother liquor are filtered and separated by the rotation of the filter turntable and the vacuum operation; The separated crystal mother liquor is discharged from the bottom of the continuous rotary disc filter (21) and recycled to the liquid phase feeding system (100) for recycling; The target crystals reaching the target height are discharged from the discharge port through the discharge baffle.
14. The production method according to claim 11, characterized in that: The method of achieving continuous drying of target crystals by a continuous rotary dryer (22) comprises: The continuous feeding of target crystals is achieved by the rotation of the screw conveying device at the feeding port of the continuous rotary dryer (22) and the cylinder; Heating and drying is performed by the heat exchange jacket of the continuous rotary dryer (22) to obtain the target crystal after drying, wherein a protective gas is introduced from the discharge port through the protective gas inlet so that the gas phase intermediate product that has not been completely reacted after drying is discharged from the discharge port; The continuous discharge of target crystals is achieved through the rotation of the screw conveying device at the discharge port of the continuous rotary dryer (22) and the cylinder.
Citation Information
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