Integrated multi-stage tubular reactor and continuous reaction system

Abstract

The invention provides an integrated multi-stage tubular reactor and a continuous reaction system, and relates to the technical field of chemical equipment, the integrated multi-stage tubular reactor comprises a reaction container, the reaction container is made of a non-metal material; the microwave heating device is arranged in the reaction container and is used for heating a solution in the reaction container; the gas stirring device is arranged in the reaction container and is used for stirring a solution in the reaction container; wherein the microwave heating devices are uniformly distributed in the reaction container. Compared with the prior art, the problem that the crystallinity of ferrous phosphate is not ideal due to uneven heating of the reaction solution can be effectively solved, the crystallization quality of ferrous phosphate is improved, and then the particle uniformity and phase purity of subsequent iron phosphate are improved.

Description

Technical Field

[0001] The invention relates to the technical field of chemical equipment, and in particular to an integrated multi-stage tubular reactor and a continuous reaction system. Background Art

[0002] With the rapid development of new energy vehicles and energy storage markets, the demand for lithium iron phosphate batteries continues to grow. With the development, lithium iron phosphate batteries will occupy a dominant position in the global battery market. As the core material of lithium iron phosphate batteries, the quality of iron phosphate directly affects the electrochemical performance and cycle life of the battery, while ferrous phosphate is an important precursor in the synthesis process of iron phosphate, and its structure and purity play a key role in the performance of the final product.

[0003] In the related art, in order to improve resource utilization, some processes use sulfuric acid slag as raw material to prepare ferrous phosphate. However, in this process, the crystal quality of ferrous phosphate is often not ideal. This low crystal quality of ferrous phosphate may lead to poor particle uniformity of subsequent iron phosphate, which in turn has an adverse effect on the ion diffusion capacity, conductivity and cycle stability of lithium iron phosphate. Summary of the invention

[0004] In order to solve the above problems, the present application provides an integrated multi-stage tubular reactor and a continuous reaction system.

[0005] In a first aspect, the present application provides an integrated multi-stage tubular reactor, which adopts the following technical solution: An integrated multi-stage tubular reactor, comprising: A reaction container, wherein the reaction container is made of a non-metallic material; a microwave heating device, disposed in the reaction container, to heat the solution in the reaction container; and a gas stirring device, disposed in the reaction container, to stir the solution in the reaction container; Wherein, the microwave heating devices are evenly distributed in the reaction container.

[0006] Preferably, the gas stirring device comprises: A nanobubble stirring device is used to generate nano-scale bubbles in the reaction container; and / or a jet stirring device is used to blow gas into the reaction container to stir the solution in the reaction container.

[0007] Preferably, the nanobubble stirring device is located at the bottom side of the reaction container; And / or, the air jet stirring device and the nano bubble stirring device are arranged alternately.

[0008] Preferably, the reaction vessel comprises a main body made of concrete material; And / or, a non-metallic rib mesh structure is provided in the reaction container; And / or, the inner wall of the reaction container is provided with an acid-resistant layer; And / or, there are multiple reaction containers, and adjacent reaction containers are connected via a communication port, and a closing device is provided at the communication port to open or close the communication port; And / or, the reaction container can be switched between a closed state and a connected state; in the closed state, the reaction container is isolated from the outside world; in the connected state, the reaction container is connected to an external device.

[0009] Preferably, the non-metallic reinforcement mesh structure comprises carbon fiber bundles.

[0010] Preferably, the acid-resistant layer is at least one of a ceramic layer and a polytetrafluoroethylene layer.

[0011] Preferably, the reaction container has a first direction and a second direction, and the size of the reaction container in the first direction is larger than the size in the second direction, wherein: The microwave heating devices are evenly spaced and arranged along the first direction; And / or, the gas stirring devices are evenly spaced along the first direction.

[0012] Preferably, at least part of the microwave heating device is arranged on both sides of the reaction container; And / or, at least part of the microwave heating device is arranged inside the reaction container.

[0013] Preferably, the nano bubble stirring device is floatingly connected to the reaction container; the jet stirring device comprises a jet pipe and a jet hose connected thereto, the jet pipe is fixed to the reaction container, and the air outlet end of the jet hose is connected to the nano bubble stirring device; when the jet hose jets, the nano bubble stirring device can be driven to deviate in a direction away from the jet pipe.

[0014] In a second aspect, the present application provides a continuous reaction system, which adopts the following technical solution: A continuous reaction system comprises the integrated multi-stage tubular reactor described in the above technical solution.

[0015] The present invention has the following advantages and beneficial effects: The present application achieves uniform heating and efficient stirring of the solution in the reaction container by providing a microwave heating device and a gas stirring device, thereby optimizing the crystallization quality of ferrous phosphate and improving the subsequent performance of ferric phosphate.

[0016] Among them, the microwave heating devices are evenly distributed in the reaction container, which can heat the reaction solution quickly and evenly, reducing the local overheating or overcooling caused by uneven heat conduction in traditional heating methods, thereby reducing the temperature gradient inside the solution, avoiding the abnormal growth of ferrous phosphate crystal particle size or excessive specific surface area, easy agglomeration and other problems caused by large temperature differences, and improving the crystal integrity and dispersibility of ferrous phosphate.

[0017] In addition, the gas stirring device forms a uniform microscopic flow field in the solution through the disturbance effect and impact of the gas, promotes the material exchange in the solution, and makes the reactants fully mixed, thereby further homogenizing the temperature field, inhibiting the non-uniform nucleation caused by local supersaturation, and improving the crystal stability and particle uniformity of ferrous phosphate.

[0018] The present application can effectively improve the problem of unsatisfactory crystallinity of ferrous phosphate caused by uneven heating, improve the crystallization quality of ferrous phosphate, and then improve the particle uniformity and phase purity of subsequent iron phosphate, and finally enhance the ion diffusion capacity, electrical conductivity and cycle stability of lithium iron phosphate, thereby improving its application performance in lithium-ion batteries. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0020] Figure 1 This is a front view of a reaction vessel according to an embodiment of the present application; Figure 2 is a side view of a reaction container according to an embodiment of the present application; Figure 3 It is a schematic diagram of the structure of the reaction container of the embodiment of the present application; Figure 4 It is a schematic diagram of the structure of an embodiment of the present application.

[0021] The markings in the figure are: 100, reaction container; 110, connecting port; 120, closing device; 130, main body; 200, microwave heating device; 300, gas stirring device; 310, nano bubble stirring device; 320, jet stirring device; 321, jet pipe; 322, jet hose; 400, first direction; 500, second direction. DETAILED DESCRIPTION

[0022] To make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be described in detail below. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other implementation methods obtained by ordinary technicians in this field without creative work belong to the scope of protection of the present invention.

[0023] The terms "first", "second", etc. in the specification and claims of the present application are used to distinguish similar objects, and are not used to describe a specific order or sequence. It should be understood that the data used in this way can be interchangeable under appropriate circumstances, so that the embodiments of the present application can be implemented in an order other than those illustrated or described here, and the objects distinguished by "first", "second", etc. are generally of one type, and the number of objects is not limited. For example, the first object can be one or more. In addition, "and / or" in the specification and claims represents at least one of the connected objects, and the character " / " generally indicates that the objects associated with each other are in an "or" relationship.

[0024] In the process of producing ferrous phosphate, in order to improve resource utilization, sulphuric acid slag is usually used as raw material to prepare ferrous phosphate. However, the inventors found that when the reaction vessel size is large, the traditional heating and stirring method has the problems of uneven heating and insufficient stirring, resulting in uneven temperature distribution inside the reaction solution, and even a temperature difference of 5-10 ° C in different regions. This uneven temperature gradient directly affects the crystallization process of ferrous phosphate, which is likely to lead to problems such as different crystal particle sizes, insufficient crystallinity, excessive specific surface area, and easy agglomeration of particles, thereby affecting the processing performance of ferrous phosphate and its application effect as a positive electrode material.

[0025] In order to solve the above problems, the present invention provides an integrated multi-stage tubular reactor, which uses a microwave heating device to heat the solution and enhances the fluid mixing effect through a gas stirring device. Compared with traditional heating methods, microwave heating has more uniform heat transfer and faster response speed, which can effectively reduce the temperature difference problem. At the same time, due to the use of a gas stirring method, the layout restrictions of mechanical stirring on the heating device are avoided, so that the microwave heating device can be reasonably distributed in the reaction vessel, thereby further improving the temperature uniformity of the reaction solution, improving the crystal quality of ferrous phosphate, and finally optimizing the particle uniformity and phase purity of iron phosphate, providing better protection for the electrochemical performance of lithium iron phosphate batteries.

[0026] The following is combined with Figures 1 to 4 , the integrated multi-stage tubular reactor and continuous reaction system provided by the present application are described in detail through specific embodiments and their application scenarios.

[0027] The first aspect of this embodiment provides a detailed description of the integrated multi-stage tubular reactor.

[0028] Reference Figure 1 , Figure 2 , the embodiment of the present application discloses an integrated multi-stage tubular reactor, including a reaction vessel 100, a microwave heating device 200 and a gas stirring device 300. The reaction vessel 100 is made of non-metallic material, for example, by concrete casting, to ensure that it has good corrosion resistance and structural stability during the production process of ferrous phosphate. In order to further enhance its acid resistance, the inner wall of the reaction vessel 100 is covered with an acid-resistant anti-corrosion layer, which can be a fluorocarbon coating, a fiberglass lining or a special acid-resistant ceramic coating, to effectively resist the corrosion of acidic substances generated during the reaction process and extend the service life of the equipment.

[0029] The microwave heating device 200 is used to perform microwave heating on the solution in the reaction vessel 100, and can achieve uniform heating of the entire reaction solution, thereby effectively reducing the temperature gradient, improving the energy utilization efficiency, and significantly shortening the heating time. Compared with traditional heating methods, microwave heating has higher heating efficiency because microwaves can directly act on the molecules in the solution, especially selectively heating substances with higher dielectric loss. This heating method can heat the reactants more accurately, thereby improving the efficiency of the target reaction, and can avoid contamination of the heating medium and maintain the cleanliness of the reaction system.

[0030] Since microwave heating acts directly on the inside of the substance, it does not rely on a heat transfer medium, greatly reducing the energy loss that may occur during heat transfer. At the same time, it avoids the exchange of substances between the heating medium and the reaction solution, which helps to reduce the occurrence of side reactions. This method not only improves the controllability of the reaction, but also affects certain chemical reaction pathways, which may increase the reaction yield or reduce the activation energy of the reaction and optimize the reaction process. In addition, microwave heating can achieve uniform temperature distribution in a shorter period of time, effectively avoiding local overheating or cooling, making the reaction more stable and ultimately improving the quality of the product.

[0031] In some embodiments, the microwave heating device 200 is evenly distributed in the reaction vessel 100. Exemplarily, the microwave heating device 200 can be evenly distributed around the reaction vessel 100, and a plurality of microwave heating units can be evenly arranged inside the reaction vessel 100. Through this arrangement, microwaves can act on the reaction solution from all directions at the same time, thereby ensuring that the solution in the reaction vessel 100 is evenly and effectively heated. This uniform heating method can significantly improve the temperature consistency of each part of the solution, reduce the temperature difference between different areas, thereby avoiding local overheating or cooling, and ensuring the stability of the reaction environment. This not only helps to improve the uniformity of the reaction, but also effectively improves the crystal quality of ferrous phosphate, reduces the difference in crystal particle size, and improves the purity and availability of the final product.

[0032] The gas stirring device 300 is used to blow air into the reaction solution in the reaction vessel 100, thereby playing the effect of stirring the reaction solution. The gas stirring device 300 causes the solution to form a certain flow in the container by blowing air into the solution in the reaction vessel 100, thereby ensuring the full mixing of the reaction solution. More importantly, the gas stirring device 300 can generate a large number of small bubbles, which play a key role in the production process of ferrous phosphate. Small bubbles can significantly increase the reaction rate, promote the uniform distribution of reactants in the solution, and strengthen the formation of ion exchange and precipitation. The generation and existence of this bubble not only speeds up the synthesis process of ferrous phosphate, but also effectively improves the material transfer process of the reaction solution, and further optimizes the reaction efficiency.

[0033] In addition, since the present solution uses a gas stirring device 300 to stir the reaction solution, there is no need to set a mechanical stirring structure inside the reaction vessel 100, which not only simplifies the design of the equipment, but also saves space, so that the microwave heating device 200 can be more fully arranged inside the reaction vessel 100. Through this design, the temperature difference inside the reaction solution can be effectively reduced, and temperature fluctuations caused by uneven stirring or uneven heat distribution in different regions can be avoided. This optimization scheme can ensure that the temperature of the reaction solution is more uniform, thereby providing a more stable reaction environment for the synthesis of ferrous phosphate.

[0034] Unlike traditional heat transfer heating methods, the microwave heating device 200 can act directly on the inside of the substance without relying on an external heat transfer medium. Traditional heating methods usually produce higher temperatures near the heat source, while areas farther away from the heat source may have lower temperatures, resulting in uneven temperatures inside the reaction solution. Microwave heating avoids this problem. It directly excites the molecules inside the solution through electromagnetic waves, making the heating process more uniform, efficient, and faster. This heating method can fundamentally avoid the temperature difference problem existing in traditional heating methods, ensure that the temperature of each part of the reaction solution is consistent, thereby improving the uniformity and efficiency of the reaction, and further improving the quality and yield of ferrous phosphate crystals.

[0035] Through the synergistic effect of microwave heating and the gas stirring device 300, this solution can provide an efficient and uniform reaction environment, which not only improves the synthesis efficiency of ferrous phosphate, but also enhances the crystal quality of the final product, thereby providing better quality raw materials for subsequent ferrous phosphate preparation.

[0036] In addition, the reaction vessel 100 is made of non-metallic material and combined with a gas stirring method, so that metal impurities are not introduced during the production process of ferrous phosphate, thereby improving the purity of ferrous phosphate. This design avoids the metal ion contamination that may be caused by traditional metal containers or mechanical stirring devices, especially in high temperature or acidic environments, where some metal materials may corrode or dissolve, causing metal impurities to enter the reaction solution and affect the quality of ferrous phosphate. In addition, reducing the introduction of metal impurities helps to improve the applicability of the final product in high-purity application scenarios such as battery materials, while reducing the difficulty of subsequent purification treatments, and improving production efficiency and product competitiveness.

[0037] Reference Figure 1 , Figure 2 According to an optional embodiment, the gas stirring device 300 includes a nano bubble stirring device 310, which is used to generate nano-scale bubbles in the reaction vessel 100. Compared with conventional bubbles, nano-scale bubbles have a higher specific surface area and a longer suspension time, can exist stably in the liquid phase, and gradually dissolve and release gas components, thereby improving the mass transfer efficiency of the gas and making the reaction more complete.

[0038] In some embodiments, the nanobubble stirring device 310 can generate nanobubbles by using microporous aeration, jet mixing or ultrasonic bubble generation. When nanobubbles burst in the liquid, they will generate local micro-flows, which helps to promote the uniform distribution of reactants, thereby enhancing ion exchange and precipitation reactions and improving the crystal quality of ferrous phosphate. In addition, the surface charge characteristics of nanobubbles can also inhibit particle agglomeration, making the generated ferrous phosphate grains more uniform and improving subsequent processing performance.

[0039] In order to optimize the stirring effect, the nano bubble stirring device 310 can be arranged at the bottom or side wall of the reaction vessel 100, and more precise stirring control can be achieved by controlling the gas flow rate, bubble size and distribution mode. This method can not only effectively improve the uniformity of the reaction solution, but also reduce the crystal defects caused by local excess gas or insufficient stirring, and improve the quality stability of the final product.

[0040] Reference Figure 1 , Figure 2 According to an optional embodiment, the gas stirring device 300 includes a jet stirring device 320, which is used to blow gas into the reaction vessel 100 to stir the solution in the reaction vessel 100. The jet stirring device 320 adjusts the gas flow rate and the jet direction so that the blown gas forms turbulent or circulating flow in the liquid, thereby effectively promoting convection and mixing of the solution and improving the uniformity of heating and reaction.

[0041] The continuous blowing of gas can not only prevent solid sedimentation, but also reduce local temperature differences and improve the stability of the reaction system. In addition, by adjusting the arrangement of the jet stirring device 320, such as setting a plurality of jet ports at the bottom or side wall of the reaction vessel 100, the stirring range can be further optimized, so that the solution in the entire reaction area can maintain a uniform flow state, thereby improving the crystal quality of ferrous phosphate and product consistency.

[0042] According to an optional embodiment, the nanobubble stirring device 310 is located at the bottom side of the reaction vessel 100. By means of the bottom arrangement, the nanobubbles can float upward from the lower part of the reaction vessel 100, and continuously contact and burst with the solution during the floating process, thereby enhancing the fluidity and mixing effect of the liquid phase. In addition, the bursting of the nanobubbles can promote the formation of micro-scale turbulence, so that the reaction substances are evenly distributed in the entire solution, improve the crystal quality of ferrous phosphate, and avoid the situation of particle agglomeration or uneven precipitation caused by excessively high or low local solute concentrations.

[0043] Reference Figure 1 , Figure 2 According to an optional embodiment, the jet stirring device 320 and the nano bubble stirring device 310 are staggered. To avoid the gas flows ejected by the two interfering with each other, thereby ensuring the stability and effectiveness of the nano bubbles. Under this arrangement, the jet stirring device 320 is used to provide larger bubbles to form a dominant fluid circulation, while the nano bubble stirring device 310 is used to release nano-scale bubbles to enhance the local microscopic mixing effect. Through the staggered arrangement, the airflow of the jet stirring device 320 can be avoided from directly impacting the nano bubble stirring area, preventing the nano bubbles from being aggregated or broken by large bubbles before they are fully exerted, thereby improving the utilization rate of the bubbles, and enhancing the stirring and mass transfer effects of the reaction solution, so that the crystallization of ferrous phosphate is more uniform.

[0044] According to an optional embodiment, the reaction vessel 100 includes a main body 130 made of concrete. For example, the concrete may be acid-resistant high-performance concrete to enhance its corrosion resistance and prevent the acidic reaction solution from corroding the container main body 130. At the same time, the inner surface of the concrete main body 130 may be covered with an acid-resistant anti-corrosion coating, such as a fluorocarbon coating or a glass flake coating, to further improve the anti-corrosion effect and extend the service life of the reaction vessel 100. In addition, the concrete main body 130 may be designed as a single-layer structure or a multi-layer composite structure according to the reaction requirements to enhance its bearing capacity and heat resistance to adapt to the ferrous phosphate production process under different scales and process conditions.

[0045] According to an optional embodiment, a non-metallic rib mesh structure is provided in the reaction vessel 100. Exemplarily, the rib mesh structure may be made of glass fiber, carbon fiber or other non-metallic materials, and its main purpose is to avoid the shielding effect of metal materials on microwaves while ensuring the structural strength of the reaction vessel 100. Since the reaction solution in the reaction vessel 100 needs to be heated by microwaves, the use of a non-metallic rib mesh structure can effectively reduce the attenuation of microwaves, ensuring that microwaves can evenly penetrate the reaction vessel 100 and act on the substances in the reaction solution, thereby improving the heating effect and heating uniformity. In addition, the non-metallic rib mesh structure has good chemical stability and corrosion resistance, can adapt to high temperature and corrosive reaction media, and extend the service life of the reaction vessel 100.

[0046] According to an optional embodiment, an acid-resistant layer is provided on the inner wall of the reaction vessel 100. The acid-resistant layer is made of a material with strong corrosion resistance, such as polytetrafluoroethylene (PTFE), fluoroplastic coating, ceramic coating or modified epoxy resin coating, so as to effectively resist the erosion of acidic substances that may be generated during the reaction process. By adding an acid-resistant layer to the inner wall of the reaction vessel 100, not only can the service life of the reaction vessel 100 be improved and the maintenance cost caused by corrosion be reduced, but also the reaction vessel 100 can be ensured to maintain good chemical stability during long-term use, avoiding structural damage or performance degradation caused by corrosion. The acid-resistant layer has high high temperature resistance and can remain stable under high temperature reaction conditions, thereby providing more reliable protection for the reaction process.

[0047] Reference Figure 1 , Figure 4According to an optional embodiment, the number of reaction vessels 100 is multiple, and adjacent reaction vessels 100 are connected through a connecting port 110, and a closing device 120 is provided at the connecting port 110 to open or close the connecting port 110. Since the reaction vessel 100 is cast in concrete, a plurality of continuously arranged reaction vessels 100 can be constructed according to the needs of the production process, so that the reactants can flow smoothly at different reaction stages without the need for external pipeline connections between traditional reactors, thereby reducing equipment installation and maintenance costs, and reducing the risk of leakage or blockage that may occur during material transportation. In addition, the setting of the closing device 120 enables each reaction vessel 100 to operate independently according to process requirements, for example, step-by-step control or switching of reaction paths at different reaction stages, improving the flexibility and efficiency of production. Exemplarily, the closing device 120 can adopt a corrosion-resistant gate, an acid-resistant and high-temperature-resistant ball valve or a chemical-resistant diaphragm valve to adapt to the special requirements of the ferrous phosphate production environment, and ensure sealing reliability to avoid cross contamination or unnecessary material loss during the reaction process.

[0048] According to an optional embodiment, the reaction vessel 100 can be switched between a closed state and a connected state; in the closed state, the reaction vessel 100 is isolated from the outside world; in the connected state, the reaction vessel 100 is connected to an external device. In order to improve the quality of ferrous phosphate, when the reaction solution in one reaction vessel 100 is transported to other reaction vessels 100, it is necessary to avoid using a pipeline pump or a conveying device made of a metal material to prevent metal ions from contaminating the reaction solution. Therefore, this scheme adopts a contactless conveying method, by adjusting the closed state and the connected state of the reaction vessel 100, and using the pressure difference to drive the reaction solution to flow, to achieve high-purity delivery of the solution.

[0049] Before delivery, the target reaction container 100 is first switched to a closed state, and the reaction container 100 is pressurized by filling it with an inert gas (such as nitrogen) or by utilizing the liquid level height difference to increase its internal pressure. When the reaction container 100 is connected to the target container, the pressure difference causes the reaction solution to automatically flow into the connected target container, thereby eliminating the need for an additional mechanical pump for delivery and achieving a more gentle and controllable fluid transfer process. In addition, the use of inert gas can prevent the introduction of oxygen or moisture, thereby reducing the possibility of side reactions and improving the purity and stability of the final product.

[0050] In order to further optimize the conveying process, the communication port 110 of the reaction vessel 100 can be set at different positions according to process requirements, such as the bottom or side wall of the container, to adapt to the regulation of different liquid levels and flow directions. The closure device 120 can adopt an acid-resistant and pressure-resistant non-metallic sealing valve, such as a ceramic valve or a polymer composite valve, to ensure long-term use in a strong acid and high temperature environment and reduce maintenance costs. In addition, liquid level sensors and pressure sensors are optionally set on the conveying path to monitor the fluid state in real time, and the conveying parameters are accurately adjusted in combination with the automatic control system to improve the stability and efficiency of production.

[0051] This solution can not only effectively avoid metal ion pollution and improve the purity of ferrous phosphate, but also reduce the use of mechanical equipment, improve the corrosion resistance and long-term operation stability of the system, thereby optimizing the production process and reducing maintenance costs.

[0052] In some embodiments, gas can be injected into the target reaction vessel 100 through the gas stirring device 300, so that the gas pressure in the target reaction vessel 100 increases. Specifically, the gas stirring device 300 can generate an appropriate amount of gas in the reaction vessel 100, and ensure that the gas pressure in the reaction vessel 100 gradually increases by precisely controlling the flow rate and injection position of the gas. When the gas pressure in the reaction vessel 100 reaches a predetermined value, this pressure difference can be used to promote the flow of the reaction solution, prompting the solution to enter other reaction vessels 100 through the connecting port 110, thereby achieving efficient solution transfer.

[0053] In this way, the gas stirring device 300 can not only effectively increase the gas pressure in the reaction vessel 100, but also further optimize the reaction conditions through the interaction between the gas and the liquid. For example, the gas stirring device 300 can generate tiny bubbles, which can play a stirring role in the reaction solution, enhance the solubility and reaction rate of the solute, and contribute to the generation of ferrous phosphate. At the same time, the tiny size of the bubbles helps to improve the contact area between the reactants and further improve the reaction efficiency.

[0054] This solution can not only avoid contact and contamination of metal equipment, but also accurately control the gas pressure in the reaction vessel 100 through gas injection, thereby achieving more flexible and controllable reaction solution transfer. At the same time, this gas injection method also helps to improve the stability of the reaction process, reduce the interference of external mechanical equipment on the reaction solution, and make the production process of ferrous phosphate purer and more efficient.

[0055] According to an optional embodiment, the non-metallic rib mesh structure includes carbon fiber bundles. As a high-strength, low-weight non-metallic material, the carbon fiber bundle has excellent corrosion resistance and tensile strength. Applying the carbon fiber bundle to the non-metallic rib mesh structure of the reaction vessel 100 can not only effectively improve the structural stability of the reaction vessel 100, but also ensure the stable performance of the container under a microwave heating environment.

[0056] Since carbon fiber has excellent electromagnetic transparency, it can not interfere with the penetration of microwaves during microwave heating, ensuring that microwaves can act evenly on the reaction solution. At the same time, the strength of the carbon fiber bundle is sufficient to support the overall structure of the reaction vessel 100, avoiding the electromagnetic shielding effect or corrosion problems that may be caused by the traditional metal rib mesh structure. Therefore, the use of carbon fiber bundles as non-metallic rib mesh structures not only improves the durability and safety of the reaction vessel 100, but also provides support for the microwave heating effect.

[0057] In addition, the use of carbon fiber bundles can also effectively reduce the weight of the reaction vessel 100, reducing manufacturing and transportation costs. Since carbon fiber has a high degree of chemical stability, it can still maintain excellent performance in harsh environments such as high temperature and corrosive solutions, further improving the durability of the reaction vessel 100 and extending its service life.

[0058] According to an optional embodiment, the acid-resistant layer is at least one of a ceramic layer and a polytetrafluoroethylene layer. The ceramic layer has excellent high temperature resistance and corrosion resistance, and can effectively resist the erosion of acidic substances during the reaction process, especially in the production process of ferrous phosphate, the ceramic layer can maintain a stable protective effect under high temperature and strong acid environment. In addition, the ceramic layer also has good mechanical strength, which can enhance the compressive strength and structural stability of the reaction vessel 100.

[0059] The polytetrafluoroethylene layer (PTFE) is a material with extremely high chemical stability, which can resist the corrosion of most acids, alkalis and solvents, and is particularly suitable for environments in contact with corrosive substances. The polytetrafluoroethylene layer is not only corrosion-resistant, but also has a low friction coefficient, which can reduce the adhesion of materials on the inner wall of the reaction vessel 100 and improve the efficiency of the reaction process. In addition, the anti-adhesion properties of polytetrafluoroethylene can effectively avoid the deposition and contamination of materials during the reaction process, thereby maintaining the cleanliness of the reaction vessel 100 and the high quality of ferrous phosphate.

[0060] According to specific needs, one of the ceramic layer and the polytetrafluoroethylene layer or a combination of the two can be selected. The combination of the ceramic layer and the polytetrafluoroethylene layer can provide stronger acid resistance protection. The high temperature tolerance provided by the ceramic layer and the chemical stability of the polytetrafluoroethylene layer complement each other, thereby further improving the service life of the reaction vessel 100 and reducing maintenance costs.

[0061] The design of this acid-resistant layer can not only ensure the long-term stable operation of the reaction vessel 100 in a harsh environment, but also effectively improve the safety and product quality of the ferrous phosphate production process.

[0062] Reference Figure 1 , Figure 2 According to an optional embodiment, the reaction vessel 100 has a first direction 400 and a second direction 500, the size of the reaction vessel 100 in the first direction 400 is larger than the size in the second direction 500, and the microwave heating devices 200 are evenly spaced along the first direction 400. Since the conventional microwave heating device 200 has a certain microwave penetration distance limitation, in order to improve the heating uniformity of the reaction solution, the present application designs the reaction vessel 100 to have a size in the first direction 400 that is larger than the size in the second direction 500. In this way, when the microwave heating devices 200 are evenly spaced along the first direction 400, they can fully cover the entire length of the reaction vessel 100, ensuring that the microwave can evenly penetrate and heat the reaction solution, thereby avoiding the problem of uneven temperature distribution.

[0063] At the same time, since the size of the reaction vessel 100 in the second direction 500 is small, the penetration depth of the microwave in this direction can be more effectively utilized, thereby improving the heating efficiency. In addition, through the uniform distribution of the microwave heating devices 200 and the appropriate size design of the reaction vessel 100, the reaction solution can be heated more evenly in the entire reaction vessel 100, reducing the situation of local overheating or overcooling, which helps to improve the reaction rate and ensure the controllability of the reaction.

[0064] Exemplarily, the reaction vessel 100 is a structure having a rectangular space, wherein the first direction 400 is the length direction of the rectangular parallelepiped, and the second direction 500 is the width direction. The design of the rectangular parallelepiped structure enables the reaction vessel 100 to provide a larger heating area in a limited space, while ensuring the uniform arrangement of the microwave heating device 200 to ensure uniform heating of the reaction solution. This design optimizes the heating effect and helps to improve the reaction efficiency and product quality in the ferrous phosphate production process.

[0065] According to an optional embodiment, the gas stirring devices 300 are evenly spaced along the first direction 400. Since gas stirring can stir the reaction solution through the rise and turbulence of bubbles, this solution evenly arranges the gas stirring devices 300 in the first direction 400 so that the stirring gas can form a uniform flow pattern inside the entire reaction container 100, thereby improving the stirring effect and avoiding the problem of excessive concentration of local gas or insufficient flow.

[0066] In addition, combined with the uniform design of the microwave heating device 200, the reasonable distribution of the gas stirring device 300 can further promote the uniform transfer of heat in the reaction solution and reduce the situation where the reaction rate is affected by local overheating or overcooling. Exemplarily, the gas stirring device 300 can adopt a jet stirring device 320, a nano bubble stirring device 310 or a combination thereof, and is distributed at intervals at the bottom or side wall of the reaction container 100, so as to achieve an efficient and uniform stirring effect.

[0067] Reference Figure 1 , Figure 2 According to an optional embodiment, at least part of the microwave heating device 200 is arranged on both sides of the reaction vessel 100. Since the penetration depth of microwave heating is limited, in order to ensure that the reaction solution is heated evenly, this solution arranges part of the microwave heating device 200 on both sides of the reaction vessel 100 so that the microwave energy can act on the reaction solution from multiple directions, thereby reducing the problem of uneven local heating and improving the overall heating efficiency.

[0068] In addition, the synergistic effect of the microwave heating devices 200 and the gas stirring device 300 evenly spaced in the first direction 400 can further optimize the temperature distribution in the reaction vessel 100, reduce the temperature gradient of the reaction solution, and improve the reaction rate and product quality. Exemplarily, the microwave heating devices 200 can be distributed in a matrix so that the reaction solutions in different regions can be effectively heated to avoid local overheating or insufficient heating.

[0069] Reference Figure 1 , Figure 2 According to an optional embodiment, at least part of the microwave heating device 200 is disposed inside the reaction vessel 100. Since microwave heating directly acts on the inside of a substance through electromagnetic waves, causing its molecules to vibrate and generate heat, it can reduce temperature gradients and improve heating efficiency compared to traditional external heat conduction methods. By distributing the microwave heating devices 200 inside and outside the reaction vessel 100, the microwave field distribution can be further optimized, so that the microwave energy acts on the reaction solution more evenly, reducing local overheating or insufficient heating.

[0070] For example, a non-metallic cover can be provided in the reaction vessel 100, and the microwave heating device 200 is located in the cover, so that the reaction vessel 100 can be better heated and the reaction solution can be prevented from directly contacting the microwave heating device 200. The design of the cover can not only effectively prevent the reaction solution from contacting the microwave heating device 200, but also ensure uniform distribution of microwave energy.

[0071] The cover can be located at the top, bottom, side wall or middle of the reaction vessel 100. If the cover is located at the top, a top heating area can be formed, and microwave energy is radiated from top to bottom, which can effectively penetrate the solution in the entire reaction vessel 100. This arrangement is particularly suitable for reaction vessels 100 with a large depth, which helps to heat the upper and lower layers of the solution and ensure uniform heating.

[0072] If the cover is located at the bottom of the reaction vessel 100, microwave energy is radiated upward from the bottom, which can promote the dissolution of sediments and the uniformity of the bottom reaction. This solution is particularly suitable for processes that require strong stirring or sedimentation of the reaction solution, and can ensure sufficient reaction in the bottom area.

[0073] The arrangement of the side wall integrated cover is suitable for a long reaction vessel 100. Arranging multiple covers on the side wall and integrating the microwave heating device 200 therein can provide uniform heating at multiple points of the long container, thereby avoiding heating dead corners. The side wall arrangement helps to improve the heating efficiency of the reaction vessel 100, especially when processing a large amount of reaction liquid.

[0074] Reference Figure 1 , Figure 2 , if the cover is located in the middle of the reaction vessel 100, a more uniform heating effect can be achieved. By combining the microwave heating device 200 located in the middle of the reaction vessel 100 with the microwave heating device 200 located outside the reaction vessel 100, the heating process can be further optimized to ensure that the temperature distribution of the reaction solution is more uniform. In this arrangement, the middle cover of the reaction vessel 100 can be used as a centralized heating area, and microwaves are radiated from both the outside and the inside of the container. The microwave heating device 200 outside the reaction vessel 100 can radiate the reaction solution from the outside, while the microwave heating device 200 in the middle provides internal heating to the reaction solution through the cover. By combining the two, the problem of uneven temperature caused by the traditional single heating method can be effectively eliminated, thereby improving the reaction efficiency and crystallization quality.

[0075] In addition, the cover can also be designed to be movable, allowing the position of the cover in the reaction vessel 100 to be adjusted as needed. Through the guide rail or support mechanism, the cover can slide in different directions in the reaction vessel 100 to adjust the coverage of microwave heating according to actual needs. This method is suitable for situations where the heating area needs to be adjusted according to different stages in the process.

[0076] Reference Figure 1 , Figure 3According to an optional embodiment, the nano bubble stirring device 310 is connected to the reaction vessel 100 in a floating manner; the jet stirring device 320 includes a jet pipe 321 and a jet hose 322 connected thereto, the jet pipe 321 is fixed to the reaction vessel 100, and the gas outlet end of the jet hose 322 is connected to the nano bubble stirring device 310; when the jet hose 322 jets, the nano bubble stirring device 310 can be driven to deviate in a direction away from the jet pipe 321. The function of the jet pipe 321 is to provide a large amount of gas, which is mainly used to strongly stir the reaction vessel 100 to form larger bubbles. These larger bubbles can produce a violent stirring effect on the solution in the reaction vessel 100. However, if the gas ejected from the jet pipe 321 overlaps with the nano bubbles generated by the nano bubble stirring device 310, it is easy to cause the nano bubbles to be destroyed, thereby affecting the reaction effect. Therefore, by connecting the jet hose 322 to the nano bubble stirring device 310, this situation can be effectively avoided.

[0077] When the gas injection hose 322 injects gas, the injected gas will exert a reverse thrust on the nano bubble stirring device 310, so that the nano bubble stirring device 310 moves away from the gas injection tube 321, thereby reducing the possibility of nano bubbles overlapping with the gas injected from the gas injection tube 321. Through this reverse thrust, the destruction of nano bubbles can be effectively avoided, thereby maintaining the bubble stability during the reaction process and ensuring sufficient stirring of the reaction solution.

[0078] In addition, by adjusting the gas pressure of the gas ejected from the jet pipe 321, the speed of the gas ejected from the jet hose 322 can be indirectly changed, thereby adjusting the reverse thrust applied to the nano bubble stirring device 310. This allows the position of the nano bubble stirring device 310 to be dynamically changed, so that the nano bubbles are distributed more evenly in the reaction vessel 100 and cover a wider area. This change can further improve the stirring effect and increase the contact area between the bubbles and the reaction solution, thereby accelerating the reaction process.

[0079] For example, a spring or elastic member may be provided in the reaction vessel 100, and the nano bubble stirring device 310 is fixed on these elastic members. The spring or elastic member provides a certain elastic effect, and when the nano bubble stirring device 310 is subjected to the reverse thrust generated by the jetting of the jet hose 322, it will be displaced or swung. Through this swing, the position of the nano bubble stirring device 310 can be accurately adjusted, so that it can be more flexibly adapted to different stirring requirements in the reaction vessel 100.

[0080] Reference Figure 3In some embodiments, the jet port of the jet hose 322 faces the jet pipe 321, and such a design can more effectively push the nanobubble stirring device 310 to move to the side away from the jet pipe 321. Specifically, when the jet hose 322 starts to jet, the jetted gas will exert a reverse thrust on the nanobubble stirring device 310, causing the nanobubble stirring device 310 to deviate in the opposite direction of the jet pipe 321. This design can not only dynamically adjust the position of the nanobubble stirring device 310, but also reduce the overlap between the gas jetted from the jet pipe 321 and the nanobubbles, thereby preventing too many nanobubbles from being destroyed.

[0081] In addition, the gas ejected from the jet hose 322 can drive the gas flow while pushing the nano bubble stirring device 310, thereby guiding the gas to flow in the opposite direction, that is, to move to the side away from the nano bubble stirring device 310. This gas flow mode can further reduce the contact amount between the gas ejected from the jet pipe 321 and the nano bubbles, effectively protect the stability of the nano bubbles, and prevent the bubbles from being excessively destroyed during the reaction process, thereby ensuring the effective role of the nano bubbles, enhancing the stirring effect, and improving the reaction efficiency.

[0082] Through this design, the gas flow and bubble distribution in the reaction vessel 100 can be more finely controlled, the working effect of the nanobubble stirring device 310 can be optimized, and the airflow of the jet pipe 321 can be prevented from interfering with the generation and stability of nanobubbles, thereby further improving the quality and reaction rate in the ferrous phosphate production process.

[0083] The first aspect of this embodiment describes a continuous reaction system in detail.

[0084] A continuous reaction system includes the integrated multi-stage tubular reactor in the above embodiment. This enables the continuous reaction system to have the beneficial effects of the integrated multi-stage tubular reactor, which will not be described in detail here.

[0085] With the help of this integrated multi-stage tubular reactor, the flow and temperature of the reactants can be better controlled, so that each link in the continuous reaction process can be effectively managed and optimized, thus avoiding the efficiency loss caused by multiple transfers and switching between equipment in the traditional reaction system. This design improves the contact efficiency between the reactants and the catalyst, heating source and gas, further accelerates the reaction process, effectively increases the reaction rate and product output, and can also reduce material loss and energy consumption between equipment.

[0086] The above description is only a specific implementation mode of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can easily think of changes or substitutions within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. An integrated multi-stage tubular reactor, characterized in that: include: A reaction container (100), wherein the reaction container (100) is made of a non-metallic material; a microwave heating device (200) disposed in the reaction container (100) to heat the solution in the reaction container (100); and a gas stirring device (300) disposed in the reaction container (100) to stir the solution in the reaction container (100); Wherein, the microwave heating devices (200) are evenly distributed in the reaction container (100).

2. The integrated multi-stage tubular reactor according to claim 1, characterized in that: The gas stirring device (300) comprises: A nanobubble stirring device (310) is used to generate nanoscale bubbles in the reaction container (100); and / or a jet stirring device (320) is used to blow gas into the reaction container (100) to stir the solution in the reaction container (100).

3. The integrated multi-stage tubular reactor according to claim 2, characterized in that: The nano bubble stirring device (310) is located at the bottom side of the reaction container (100); And / or, the air jet stirring device (320) and the nano bubble stirring device (310) are arranged alternately.

4. The integrated multi-stage tubular reactor according to claim 1, characterized in that: The reaction container (100) comprises a main body (130) made of concrete material; And / or, a non-metallic rib mesh structure is provided in the reaction container (100); And / or, the inner wall of the reaction container (100) is provided with an acid-resistant layer; And / or, there are a plurality of reaction containers (100), adjacent reaction containers (100) are connected via a communication port (110), and a closing device (120) is provided at the communication port (110) to open or close the communication port (110); And / or, the reaction container (100) can be switched between a closed state and a connected state; in the closed state, the reaction container (100) is isolated from the outside world; in the connected state, the reaction container (100) is connected to an external device.

5. The integrated multi-stage tubular reactor according to claim 4, characterized in that: The non-metallic reinforcement mesh structure includes carbon fiber bundles.

6. The integrated multi-stage tubular reactor according to claim 4, characterized in that: The acid-resistant layer is at least one of a ceramic layer and a polytetrafluoroethylene layer.

7. The integrated multi-stage tubular reactor according to claim 1, characterized in that: The reaction container (100) has a first direction (400) and a second direction (500), and the size of the reaction container (100) in the first direction (400) is greater than the size in the second direction (500), wherein: The microwave heating devices (200) are evenly spaced along the first direction (400); And / or, the gas stirring devices (300) are evenly spaced along the first direction (400).

8. The integrated multi-stage tubular reactor according to claim 7, characterized in that: At least part of the microwave heating device (200) is arranged on both sides of the reaction container (100); And / or, at least a portion of the microwave heating device (200) is disposed inside the reaction container (100).

9. The integrated multi-stage tubular reactor according to claim 2, characterized in that: The nano bubble stirring device (310) is connected to the reaction container (100) in a floating manner; the air jet stirring device (320) comprises an air jet pipe (321) and an air jet hose (322) connected thereto; the air jet pipe (321) is fixed to the reaction container (100); the air outlet end of the air jet hose (322) is connected to the nano bubble stirring device (310); when the air jet hose (322) jets, the nano bubble stirring device (310) can be driven to deviate in a direction away from the air jet pipe (321).

10. A continuous reaction system, characterized in that: An integrated multi-stage tubular reactor comprising any one of claims 1 to 9.

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