A tubular continuous reactor and a device for continuously synthesizing a carbonate precipitate product with adjustable particle size

Abstract

The utility model relates to chemical material synthetic equipment technical field discloses a kind of tubular continuous reactor and particle size adjustable carbonate precipitation product continuous synthesis device. Tubular continuous reactor contains several heat exchange reaction pipes that are sequentially connected along material flow direction, heat exchange reaction pipe includes the reaction pipe body for material flow passage formation reaction channel, and the heat exchange jacket for heat exchange medium circulation is sleeved in its outer periphery, can realize material continuous reaction and accurate temperature control, guarantee reaction stable and efficient. Carbonate precipitation product continuous synthesis device includes above-mentioned tubular continuous reactor, feeding system and centrifugal mixer, feeding system is connected reactor feed inlet through feed pipeline, centrifugal mixer is connected reactor discharge outlet through discharge pipeline, can realize carbonate precipitation product continuous synthesis, and product particle size can be adjusted, improve production efficiency and product uniformity.

Description

Technical Field

[0001] This utility model relates to the field of chemical material synthesis equipment technology, specifically to a tubular continuous reactor and a continuous synthesis device for carbonate precipitate products with adjustable particle size. Background Technology

[0002] Carbonate precipitates (such as calcium carbonate and magnesium carbonate) are widely used in many fields such as chemical engineering, materials science, and pharmaceuticals. Their properties (especially particle size and distribution) have a crucial impact on the quality of downstream products. Currently, the synthesis of carbonate precipitates is mostly carried out using batch reactors.

[0003] In batch reactors, materials are in a static, batch state. Temperature control of the reaction system relies on jackets or internal coils. However, due to the lack of material flow and small heating area, heat transfer and mass diffusion efficiency are low, making it difficult to quickly reach and maintain a uniform target temperature throughout the reactor. This is detrimental to the precise control of crystallization rate and product particle size in temperature-sensitive crystallization processes like carbonate precipitation. Regarding pH adjustment, when reagents are added to adjust the pH, the reagents initially mix with the materials in localized areas. The poor overall flow of the materials makes it difficult for localized pH changes to diffuse quickly and uniformly throughout the reaction system, easily leading to excessively high or low localized pH values. Since carbonate precipitation requires high pH uniformity, fluctuations in localized pH levels result in inconsistent crystallization rates and morphologies in different regions, ultimately leading to a wide and uneven product particle size distribution, making it difficult to adjust the product particle size according to different application requirements.

[0004] Meanwhile, the intermittent production mode of the batch reactor requires a series of steps such as feeding, heating, reaction, cooling and discharging each time, which limits the production efficiency. Moreover, the slight differences in parameters such as temperature and pH between different batches can easily cause product quality fluctuations, making it difficult to ensure batch stability. In large-scale industrial production, the drawbacks of this mode are more prominent, and it cannot efficiently meet the market demand for high-quality, large-scale carbonate precipitation products.

[0005] Therefore, there is an urgent need for a continuous synthesis device for carbonate precipitates that can overcome the shortcomings of existing technologies in temperature control, pH uniformity, and production continuity, so as to achieve continuous production of carbonate precipitates and precisely adjust reaction parameters to control product particle size. Utility Model Content

[0006] The purpose of this invention is to provide a tubular continuous reactor and a continuous synthesis device for carbonate precipitate products with adjustable particle size, enabling continuous production of carbonate precipitate products and allowing precise adjustment of reaction parameters to control product particle size. To achieve the above objective, this invention provides the following technical solution: A tubular continuous reactor includes several heat exchange reaction tubes connected in series along the material flow direction; each heat exchange reaction tube includes a reaction tube body and a heat exchange jacket sleeved around the outer periphery of the reaction tube body; the reaction tube body is used for material flow and forming a reaction channel, and the heat exchange jacket is used for heat exchange medium flow.

[0007] Preferably, a rotating shaft is inserted inside the reaction tube body, the rotating shaft is coaxially distributed with the reaction tube body, and several stirring impellers are sleeved on the rotating shaft.

[0008] Preferably, the stirring impeller includes an impeller body and a locking shaft fixedly connected to the impeller body. One end of the locking shaft is fixedly connected to the impeller body and coaxially distributed. The other end of the locking shaft is provided with an elastic flap. The impeller body and the locking shaft are axially connected and have a shaft hole for the rotating shaft to pass through. The outer periphery of the locking shaft near the impeller body is provided with an external thread.

[0009] Preferably, a locking sleeve is fitted onto the locking shaft. The locking sleeve is a cylindrical structure with openings at both ends, and one end of its inner circumference is provided with an internal thread that matches the external thread.

[0010] Preferably, the reaction tube body is provided with a plurality of anti-backflow components, the anti-backflow components including an annular base and a plurality of arc-shaped guide plates; the annular base has a shaft hole at its center for a rotating shaft to pass through, and the outer peripheral edge of the annular base is fixed to the inner wall of the reaction tube body; the plurality of arc-shaped guide plates are arranged in a ring array below the annular base, the concave surface of the arc-shaped guide plates facing the forward flow direction of the material, and the convex surface facing the backflow direction of the material.

[0011] A continuous synthesis apparatus for carbonate precipitate products with adjustable particle size includes the aforementioned tubular continuous reactor, a feeding system, and a centrifugal mixer; the feeding system is connected to the inlet of the tubular continuous reactor via a feeding pipe, and the centrifugal mixer is connected to the outlet of the tubular continuous reactor via a discharge pipe.

[0012] Preferably, the discharge pipeline is provided with a sampling port and a level gauge interface.

[0013] Preferably, the feeding system includes a plurality of raw material storage containers and a metering pump corresponding to each of the raw material storage containers; the outlet of each raw material storage container is connected to the inlet of the corresponding metering pump through a pipeline, and the outlets of each metering pump are combined and connected to the inlet of the tubular continuous reactor through the feeding pipeline.

[0014] Preferably, the feed pipe is also provided with an exhaust port.

[0015] The beneficial effects of this utility model are: 1. This utility model uses several double-layer jacketed heat exchange reaction tubes connected in series to increase the contact area between the material and the heat exchange medium, improve the efficiency and uniformity of temperature control, and can accurately control the reaction temperature.

[0016] 2. In this invention, the rotating shaft, stirring impeller assembly, and anti-backflow assembly within the reaction tube body work together to enhance material mixing and mass transfer, thereby reducing local fluctuations during pH adjustment. This also prevents material backmixing, providing a stable and uniform reaction environment for carbonate precipitation and crystallization, effectively controlling the product particle size distribution, and meeting the particle size requirements of different scenarios.

[0017] 3. This utility model integrates a continuous feeding system, a tubular continuous reactor, and a centrifugal mixer to form a complete process from raw material transportation and continuous reaction to post-processing, replacing the traditional intermittent production mode and greatly improving production efficiency; at the same time, it avoids quality differences caused by parameter fluctuations between batches, ensuring product quality consistency and better meeting the needs of large-scale industrial production. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the continuous synthesis device for carbonate precipitate products with adjustable particle size according to Embodiment 2 of this utility model; Figure 2 This is a schematic diagram of the feeding system of Embodiment 2 of this utility model; Figure 3 This is a schematic diagram of the discharge pipe and centrifugal mixer of Embodiment 2 of this utility model; Figure 4 This is a schematic diagram of the tubular continuous reactor of Embodiment 1 of this utility model; Figure 5 This is a schematic diagram of the heat exchange reaction tube in Embodiment 1 of this utility model; Figure 6 This is a schematic diagram of the stirring impeller assembly of Embodiment 1 of this utility model; Figure 7 This is a schematic diagram of the anti-backflow component of Embodiment 1 of this utility model.

[0019] Reference numerals: 10-Tubular continuous reactor, 101-Heat exchange reaction tube, 102-Material inlet, 103-Material outlet, 104-Motor, 105-Connecting flange, 106-Reaction tube body, 107-Heat exchange jacket, 108-Heat exchange medium inlet, 109-Heat exchange medium outlet, 110-Rotating shaft, 120-Agitator impeller, 121-Impeller body, 122-Locking shaft, 123-Locking sleeve, 130-Anti-backflow assembly, 131-Annular base, 132-Arc-shaped guide plate, 20-Feeding system, 201-Raw material storage container, 202-First valve, 203-Metering pump, 30-Centrifugal mixer, 40-Feed pipe, 401-Waste gas outlet, 50-Discharge pipe, 501-Sampling port, 502-Level gauge interface, 503-Second valve. Detailed Implementation

[0020] The specific embodiments of this utility model are described below with reference to the accompanying drawings.

[0021] Example 1 like Figures 4 to 7 As shown, this embodiment discloses a tubular continuous reactor 10, which includes several heat exchange reaction tubes 101 connected in series along the material flow direction. The heat exchange reaction tubes 101 are sealed and securely connected by connecting flanges 105, which ensures that the material flows continuously in the tubes without leakage and also facilitates the assembly and maintenance of the reactor.

[0022] The heat exchange reaction tube 101 includes an internal reaction tube body 106 and a heat exchange jacket 107 surrounding the reaction tube body 106. The reaction tube body 106 provides material flow and forms a reaction channel where carbonate precipitation occurs. The heat exchange jacket 107 provides heat exchange medium flow, which enters through the heat exchange medium inlet 108, exchanges heat with the material inside the reaction tube body 106, and then exits through the heat exchange medium outlet 109. The jacket structure increases the heat exchange area, enabling rapid and uniform temperature adjustment of the material inside the reaction tube body 106, providing a suitable and stable temperature environment for the carbonate precipitation reaction. This is crucial for controlling the crystallization rate and product particle size of the carbonate precipitation, avoiding the problem of wide product particle size distribution caused by uneven temperature in traditional batch reactors.

[0023] A rotating shaft 110 is installed inside the reaction tube body 106, coaxially distributed with the reaction tube body 106. Several stirring impellers 120 are mounted on the rotating shaft 110. Both ends of the rotating shaft 110 are connected to motors 104 located at both ends of the tubular continuous reactor 10. When the motors 104 are energized, they drive the rotating shaft 110 to rotate, providing power to the stirring impellers 120, enabling the stirring impellers 120 to stir the materials inside the reaction tube body 106. Stirring enhances the mixing and mass transfer of materials, allowing the reagents to mix more evenly with the materials, avoiding uneven local reactions, helping to control the crystallization process of carbonate precipitation, and ensuring the uniformity of product particle size.

[0024] The impeller 120 includes an impeller body 121 and an elastic valve body fixedly connected to the impeller body 121. The impeller body 121 has a shaft hole through which a rotating shaft 110 passes along the axial direction; the impeller body 121 and the elastic valve body also have shaft holes through which the rotating shaft 110 passes along the axial direction; the outer periphery of the elastic valve body near the impeller body 121 is provided with an external thread; a locking sleeve 123 is fitted on the elastic valve body, the locking sleeve 123 is a cylindrical structure with openings at both ends, and one end of its inner periphery is provided with an internal thread that matches the external thread of the elastic valve body.

[0025] When assembling the impeller 120, the rotating shaft 110 is inserted into the shaft hole of the impeller body 121, and then the locking sleeve 123 is screwed onto the elastic flap of the impeller 120. As the locking sleeve 123 tightens, it gradually conforms to the outer contour of the elastic flap, compressing the elastic flap and causing radial contraction, thereby pressing the rotating shaft 110 into the shaft hole, achieving relative fixation and synchronous rotation between the impeller body 121 and the rotating shaft 110. The rotating impeller body 121 agitates the material, disrupting the crystal growth environment or promoting uniform crystal growth, thus affecting the particle size of the carbonate precipitate.

[0026] The anti-backflow assembly 130 includes an annular base 131 and several arc-shaped guide plates 132. The annular base 131 has a central hole for the rotating shaft 110 to pass through, and its outer periphery is fixed to the inner wall of the reaction tube body 106. Several arc-shaped guide plates 132 are arranged in a ring array below the annular base 131, with the concave surface of the arc-shaped guide plates 132 facing the forward flow direction of the material and the convex surface facing the backflow direction. When the material flows forward, the concave surface of the arc-shaped guide plates 132 guides the material smoothly through; when the material tends to backflow, the convex surface of the arc-shaped guide plates 132 blocks the backflowing material, reducing back-mixing. Preventing back-mixing ensures the continuity and stability of the reaction, allowing the material to react within the reaction tube body 106 according to the set flow direction and reaction time. This helps control the crystallization process of carbonate precipitation and ensures the uniformity of the product particle size distribution.

[0027] Example 2 like Figures 1 to 3 As shown, this embodiment provides a continuous synthesis apparatus for carbonate precipitate products with adjustable particle size, including a tubular continuous reactor 10, a feeding system 20, and a centrifugal mixer 30 as described in Example 1; the feeding system 20 is connected to the inlet of the tubular continuous reactor 10 through a feeding pipe 40, and the centrifugal mixer 30 is connected to the outlet of the tubular continuous reactor 10 through a discharge pipe 50.

[0028] The feeding system 20 is responsible for transporting the raw materials required for the reaction into the tubular continuous reactor 10, ensuring a raw material supply for the continuous reaction. The raw material storage container 201 is used to store the raw materials required for the carbonate precipitation reaction. A first valve 202 is installed on the discharge pipe of the raw material storage container 201. By opening or closing the valve, the flow of raw materials from the raw material storage container 201 is controlled; the flow rate of the raw materials can also be controlled by adjusting the valve opening, achieving precise control of the raw material delivery. This facilitates adjustment of the raw material feed rate according to reaction requirements, ensuring the smooth progress of the reaction. A metering pump 203 corresponds one-to-one with each raw material storage container 201 and is installed on the discharge pipe of each raw material storage container 201. It can accurately deliver the raw materials to the subsequent feed pipe 40 according to the set flow rate.

[0029] The feed pipe 40 collects the raw materials delivered by each metering pump 203 and then transports them into the tubular continuous reactor 10. The discharge ends of each metering pump 203 converge and are connected to the material inlet 102 of the tubular continuous reactor 10 through the feed pipe 40. The feed pipe 40 is also equipped with an exhaust port 401 to discharge the exhaust gas generated during the feeding process, preventing the exhaust gas from accumulating in the pipe and affecting the normal transportation of raw materials or causing safety hazards.

[0030] Centrifugal mixer 30 is connected to the outlet of tubular continuous reactor 10 via discharge pipe 50, and is used for subsequent processing of the carbonate-containing precipitate flowing out of tubular continuous reactor 10. Utilizing centrifugal force, the material is stirred, mixed, or subjected to solid-liquid separation operations to achieve a more uniform particle size distribution of the carbonate precipitate product, or to separate the product from the mother liquor. This further processing of the reacted material improves the quality of the carbonate precipitate product and meets the requirements of different application scenarios.

[0031] The discharge pipe 50 is equipped with a sampling port 501, a level gauge interface 502, and a second valve 503. The sampling port 501 is used to extract a portion of the material from the discharge pipe 50 for testing, in order to monitor the quality of the reaction products in real time. The level gauge interface 502 is used to install a level gauge to monitor the material level within the discharge pipe 50, facilitating material transport control. The second valve 503 is used to control the opening and closing of the discharge pipe 50, allowing the material transport to be opened or closed as needed. Its specific working principle is as follows: Before starting the entire synthesis unit, the debugging and parameter setting of each component are completed according to the particle size requirements of the target carbonate precipitate product. For example, the temperature and circulation rate of the heat exchange medium in the heat exchange jacket 107 and the delivery flow rate of each metering pump 203 are set to provide accurate initial conditions for the reaction process.

[0032] After the device is started, the reaction materials in each raw material storage container 201 flow out slowly under the control of the opening of the first valve 202 and enter the corresponding metering pump 203. The metering pump 203 accurately meteres and delivers the raw materials according to the preset flow parameters to avoid the crystallization process being affected by the material ratio deviation. Subsequently, the different raw materials are initially combined in the feed pipe 40. At this time, the exhaust port 401 on the feed pipe 40 is opened simultaneously to promptly discharge the volatile waste gas generated during the mixing of raw materials or the residual air in the pipe, to prevent the waste gas from interfering with the reaction or causing safety hazards. The initially mixed raw materials are smoothly transported along the feed pipe 40 to the material inlet 102 of the tubular continuous reactor 10.

[0033] After the raw material enters the tubular continuous reactor 10, it flows through the internal channels of several heat exchange reaction tubes 101 that are sealed and connected in series via connecting flanges 105, and begins the carbonate precipitation reaction. During this process, the heat exchange medium (such as hot water, cold water, or heat transfer oil) enters the heat exchange jacket 107 chamber from the heat exchange medium inlet 108, and fully exchanges heat with the material in the reaction tube body 106, absorbing or releasing reaction heat. Then it flows out from the heat exchange medium outlet 109 and is recycled. Through this continuous heat exchange cycle, it is ensured that the material in the reaction tube body 106 is always maintained within a suitable crystallization temperature range, avoiding uneven crystal growth rate caused by excessively high or low local temperatures, which would affect the particle size distribution of the product.

[0034] Meanwhile, the motor 104 is powered on and its output shaft drives the rotating shaft 110, which passes through the center of the heat exchange reaction tube 101, to rotate at high speed. Multiple impellers installed on the rotating shaft 110 rotate synchronously. The impeller body 121 strongly stirs the flowing material, breaking the static state of the material and making the reaction reagents (including the pH adjustment reagents that may be added later) and raw materials uniformly mixed. This avoids the situation where the pH value rises or falls suddenly in a local area due to excessively high reagent concentration, providing a uniform chemical environment for the nucleation and growth of carbonate crystals. Meanwhile, the anti-backflow components 130, which are spaced apart in the heat exchange reaction tube 101, guide the material to flow smoothly in the forward direction through the concave surface of the arc-shaped guide plate 132, while using the convex surface to block the backflow tendency of the material caused by stirring impact or pressure fluctuations. This prevents the reacted material from mixing with the unreacted raw materials, ensuring that the material in each area can complete the crystallization process according to the set reaction time, and further ensuring the consistency of crystal growth.

[0035] After the material completes the preset reaction time and forms a mixture containing carbonate precipitate, it flows out from the material outlet 103 of the tubular continuous reactor 10 and enters the discharge pipe 50. Within the discharge pipe 50, operators can periodically sample small amounts of material through the sampling port 501 to test indicators such as particle size and purity of the precipitated particles. If the particle size deviates from the target value, parameters such as the heat exchange medium temperature, stirring speed, or flow rate of the metering pump 203 can be adjusted in real time. Simultaneously, the level gauge installed at the level gauge interface 502 continuously monitors the material level in the pipe to prevent material overflow due to excessively high levels or subsequent conveying due to excessively low levels. After the material is monitored and regulated within the discharge pipe 50, the second valve 503 opens according to the processing rhythm of the centrifugal mixer 30, conveying the mixture to the centrifugal mixer 30.

[0036] After entering the centrifugal mixer 30, the mixture undergoes initial solid-liquid separation under the centrifugal force generated by high-speed rotation, separating the carbonate precipitate particles from the reaction mother liquor. Simultaneously, the centrifugal force further stirs the material internally, resulting in a more uniform particle size distribution and preventing small particles from agglomerating or large particles from breaking down. Ultimately, a carbonate precipitate product with the required particle size is obtained. The entire production process, from raw material transportation and reaction control to post-processing, forms a complete closed loop. All stages operate continuously, significantly improving production efficiency. Furthermore, through precise control of key parameters such as temperature, stirring, and proportioning, the particle size of the carbonate precipitate product can be flexibly adjusted, effectively ensuring the stability and consistency of product quality.

[0037] In summary, the tubular continuous reactor and the continuous synthesis device for carbonate precipitates with adjustable particle size in this embodiment, through the structural design of the double-jacketed heat exchange reaction tube 101, achieve precise adjustment and uniform control of the reaction temperature. Combined with the efficient mixing effect of the stirring impeller 120 assembly within the reaction tube body 106, local pH fluctuations are effectively avoided, ensuring the stability of the chemical environment of the reaction system. This provides precisely controllable temperature and pH conditions for the crystallization process of carbonate precipitation. Simultaneously, by flexibly adjusting the stirring impeller 120 and reaction parameters, the crystal growth rate and morphology can be specifically controlled, achieving precise adjustment of the carbonate precipitate particle size. The entire device forms a complete and continuous production process from raw material transportation and reaction process to product post-processing, completely overcoming the limitations of traditional intermittent production modes. While ensuring product quality stability and consistency, it significantly improves production efficiency, providing a reliable technical solution for the large-scale, high-quality preparation of carbonate precipitates.

[0038] The above are merely preferred embodiments of this utility model and are not intended to limit the scope of this utility model. Various modifications and variations can be made to this utility model by those skilled in the art. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of this utility model should be included within the protection scope of this utility model.

Claims

1. A tubular continuous reactor, characterized in that, It includes several heat exchange reaction tubes connected in series along the material flow direction; each heat exchange reaction tube includes a reaction tube body and a heat exchange jacket sleeved around the outer periphery of the reaction tube body; the reaction tube body is used to allow material to flow and form a reaction channel, and the heat exchange jacket is used to allow heat exchange medium to flow. A rotating shaft is inserted inside the reaction tube body, and the rotating shaft is coaxially distributed with the reaction tube body. Several stirring impellers are sleeved on the rotating shaft. The stirring impeller includes an impeller body and a locking shaft fixedly connected to the impeller body. One end of the locking shaft is fixedly connected to the impeller body and coaxially distributed. The other end of the locking shaft is provided with an elastic flap. The impeller body and the locking shaft are axially connected and have a shaft hole for the rotating shaft to pass through. The outer periphery of the locking shaft near the impeller body is provided with an external thread.

2. A tubular continuous reactor according to claim 1, characterized in that, A locking sleeve is fitted onto the locking shaft. The locking sleeve is a cylindrical structure with openings at both ends, and one end has an internal thread that matches the external thread.

3. A tubular continuous reactor according to claim 1, characterized in that, The reaction tube body is provided with several anti-backflow components, each including an annular base and several arc-shaped guide plates; the annular base has a shaft hole at its center for a rotating shaft to pass through, and the outer peripheral edge of the annular base is fixed to the inner wall of the reaction tube body; the several arc-shaped guide plates are arranged in a ring array below the annular base, with the concave surface of the arc-shaped guide plates facing the forward flow direction of the material and the convex surface facing the backflow direction of the material.

4. A continuous synthesis apparatus for carbonate precipitates with adjustable particle size, characterized in that, The invention includes a tubular continuous reactor, a feeding system, and a centrifugal mixer as described in any one of claims 1 to 3; the feeding system is connected to the inlet of the tubular continuous reactor via a feeding pipe, and the centrifugal mixer is connected to the outlet of the tubular continuous reactor via a discharge pipe.

5. The continuous synthesis apparatus for carbonate precipitate products with adjustable particle size according to claim 4, characterized in that, The discharge pipe is equipped with a sampling port and a level gauge interface.

6. The continuous synthesis apparatus for carbonate precipitate products with adjustable particle size according to claim 4, characterized in that, The feeding system includes several raw material storage containers and metering pumps corresponding to each of the raw material storage containers. The outlet of each of the raw material storage containers is connected to the inlet of the corresponding metering pump via a pipeline. The outlets of the metering pumps converge and are connected to the inlet of the tubular continuous reactor via the feed pipeline.

7. The continuous synthesis apparatus for carbonate precipitate products with adjustable particle size according to claim 6, characterized in that, The feed pipe is also equipped with an exhaust port.

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