Continuous reaction-separation apparatus

Abstract

The application relates to a continuous reaction and separation device, which comprises a reactor barrel, an internal reaction chamber, opposite top and bottom ends, a stirring mechanism arranged at the top end of the reaction chamber and extending from the top end to the bottom end, a liquid collecting tank arranged in the reaction chamber for accommodating mixed solid and liquid, the liquid collecting tank being connected with the stirring mechanism to be driven to rotate by the stirring mechanism, an annular collecting tank arranged below the liquid collecting tank, one end of the annular collecting tank being connected with the inner wall of the reactor barrel, the annular collecting tank being provided with a discharge port and an overflow port, a liquid distribution pipe connected with the bottom end of the liquid collecting tank and extending into the annular collecting tank, and a pushing piece connected with the stirring mechanism. The continuous reaction and separation device provided by the application can continuously separate the solid and liquid generated in the reaction without the help of a solvent.

Description

Technical Field

[0001] This application relates to the field of chemical equipment technology, and in particular to a continuous reaction separation device. Background Technology

[0002] In the process of synthesizing new substances in chemical engineering, a large amount of solids are often produced during liquid-phase reactions. These solids are not the desired products. As the reaction continues, the amount of solids gradually increases, which leads to an increase in the viscosity of the entire reaction system, a decrease in fluidity, and an increase in the power consumption of mechanical stirring. To solve this problem, one or more solvents are usually added. However, this method increases solvent consumption, reduces the concentration of the desired product in the reaction system, increases separation costs, and affects or even reduces production efficiency. Summary of the Invention

[0003] The purpose of this application is to provide a continuous reaction separation device that can continuously separate solids and liquids generated in a reaction without the need for a solvent.

[0004] Therefore, this application provides a continuous reaction separation device, including: a reactor cylinder with a reaction chamber inside, the reaction chamber having a top and a bottom opposite each other; a stirring mechanism disposed at the top of the reaction chamber and extending from the top to the bottom; a collection tank disposed in the reaction chamber for collecting the mixed solids and liquids, the collection tank being connected to the stirring mechanism and rotated by the stirring mechanism; an annular collection tank disposed below the collection tank, one end of the annular collection tank being connected to the inner wall of the reactor cylinder, the annular collection tank having a discharge port and an overflow port; a distribution pipe connected to the bottom of the collection tank and extending into the annular collection tank; and a pushing component connected to the stirring mechanism; during reaction separation, the distribution pipe rotates under the drive of the stirring mechanism to distribute the solids and liquids in the collection tank into the annular collection tank, the pushing component pushes the solids to the discharge port to be discharged out of the reactor cylinder, and the liquids are discharged from the overflow port into the reaction chamber.

[0005] In one possible implementation, the edge of the annular collection trough is provided with a toothed overflow weir.

[0006] In one possible implementation, the actuating component includes a fixed connecting rod and a scraper. One end of the fixed connecting rod is connected to a stirring mechanism, and the scraper is located at the other end of the fixed connecting rod and within an annular collection trough. The stirring mechanism rotates, causing the fixed connecting rod to rotate, which in turn causes the scraper to rotate within the annular collection trough to push the solids to the outlet and discharge them outside the reactor cylinder.

[0007] In one possible implementation, the fixed connecting rod is positioned on both sides of the stirring mechanism, opposite to the liquid distribution pipe.

[0008] In one possible implementation, the stirring mechanism includes a stirring shaft and stirring blades, the stirring shaft extending from the top to the bottom of the reaction chamber, and several stirring blades being arranged on the stirring shaft.

[0009] In one possible implementation, a solid discharge component is also included, with a solid discharge port provided on the side wall of the reactor shell, and the solid discharge component is located between the discharge port and the solid discharge port.

[0010] In one possible implementation, the solid discharge component includes a discharge pipe and a ball valve disposed on the discharge pipe. The discharge pipe is inclined between the discharge port and the solid discharge port, and the ball valve is used to control the opening and closing of the discharge pipe.

[0011] In one possible implementation, a lifting mechanism is also included, which is located at the bottom of the reactor shell and extends along the outer wall of the reactor shell into the collection tank.

[0012] In one possible implementation, the lifting mechanism includes a lifting pipe and a lifting pump mounted on the lifting pipe. The lifting pipe is located at the bottom outer end of the reactor body and extends along the outer side wall of the reactor body into the collection tank. The lifting pump is used to lift the solids and liquids mixed in the reactor body into the collection tank along the lifting pipe.

[0013] In one possible implementation, a drive mechanism is also included, which is connected to the stirring mechanism to drive the stirring mechanism to rotate.

[0014] According to the continuous reaction separation device provided in the embodiments of this application, the chemical reaction and the solid-liquid separation of reactants can be integrated into one device to achieve continuous separation of solid particles generated during the chemical reaction process, reduce or even eliminate the need for additional solvents, reduce equipment investment, and increase economic benefits. Attached Figure Description

[0015] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort. In addition, in the drawings, the same parts use the same reference numerals, and the drawings are not drawn to scale.

[0016] Figure 1 This diagram shows a schematic representation of the continuous reaction separation apparatus provided in an embodiment of this application.

[0017] Figure 2 This shows a top view of the annular collection trough provided in an embodiment of this application;

[0018] Figure 3 This shows a front view of the annular collection trough provided in an embodiment of this application;

[0019] Explanation of reference numerals in the attached figures:

[0020] 1. Reactor shell;

[0021] 21. Stirring shaft; 22. Stirring blades;

[0022] 3. Liquid collection tank;

[0023] 4. Annular collection trough; 41. Overflow weir; 42. Overflow outlet; 43. Discharge outlet;

[0024] 5. Liquid distribution pipe;

[0025] 61. Fixed connecting rod; 62. Scraper;

[0026] 71. Discharge pipe; 72. Ball valve;

[0027] 8. Solid waste discharge outlets;

[0028] 91. Lift pipe; 92. Lift pump;

[0029] 10. Drive mechanism;

[0030] 11. Raw material intake;

[0031] 12. Vent. Detailed Implementation

[0032] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.

[0033] In the synthesis of new substances in chemical and chemical processes, a large amount of solids are often generated during liquid-phase reactions. These solids are not the desired product and therefore need to be separated. Existing technologies handle these solid particles by continuously adding one or more solvents to the reactor to dissolve them. This method increases solvent consumption and reduces the concentration of the desired product in the reaction system, affecting production efficiency. Therefore, this application provides a device capable of continuously separating solid and liquid reactants in a reaction system, continuously separating the solids generated during the reaction without affecting reaction efficiency.

[0034] Example 1

[0035] like Figures 1 to 3 As shown in the figure, this application provides a continuous reaction separation device, including a reactor cylinder 1, a stirring mechanism, a liquid collection tank 3, an annular collection tank 4, a liquid distribution pipe 5, and a pushing component. The reactor cylinder 1 is provided with a reaction chamber, which has a top end and a bottom end from top to bottom. The stirring mechanism is located at the top end of the reaction chamber and extends from the top end to the bottom end. The liquid collection tank 3 is located in the reaction chamber to collect the mixed solid and liquid, and is connected to the stirring mechanism so that it can be driven to rotate by the stirring mechanism. The annular collection tank 4 is located below the liquid collection tank 3, and one end of the annular collection tank 4 is connected to the inner wall of the reactor cylinder 1. The annular collection tank 4 is provided with a discharge port 43 and an overflow port 42. The liquid distribution pipe 5 is connected to the bottom end of the liquid collection tank 3 and extends into the annular collection tank 4. The pushing component is connected to the stirring mechanism.

[0036] With the above structure, in the continuous reaction separation device provided in this application embodiment, the liquid distribution pipe 5 rotates under the drive of the stirring mechanism during reaction separation, so as to distribute the solid and liquid in the liquid collection tank 3 to the annular collection tank 4. The outlet of the liquid distribution pipe 5 is always located in the annular collection tank 4. Since the liquid distribution pipe 5 is rotating, the liquid distribution pipe 5 distributes the mixed solid and liquid reactants layer by layer into the annular collection tank 4, instead of transporting them to a fixed position in the annular collection tank 4, thus avoiding the accumulation of solid and liquid in the annular collection tank 4. The pusher rotates under the drive of the stirring mechanism, thereby pushing the solid to the outlet 43 of the annular collection tank 4 and discharging it out of the reactor cylinder 1, while the liquid is discharged from the overflow port 42 into the reaction chamber.

[0037] It should be noted that the reaction separation principle of the continuous reaction separation device provided in this application is as follows: In a chemical reaction, all solid particles generated during the reaction are dispersed in the entire liquid phase system. Under the action of gravity and buoyancy, the concentration of solid particles gradually decreases from bottom to top in the reactor. Before the reaction reaches the expected endpoint, the solid-liquid mixture must not be discharged through the bottom. Therefore, in the reaction process, this application embodiment provides an independent static sedimentation area, namely the annular collection tank 4, in a timely manner. After the solid particles settle in the annular collection tank 4 and the concentration increases, they can be separated from the entire reaction system under the push of the pusher.

[0038] In an optional example, the annular collection tank 4 provided in this application embodiment is provided with a toothed overflow weir 41 at its edge. In this application embodiment, the overflow weir 41 is an outlet weir, located at the bottom of the annular collection tank 4 after solid sedimentation, while the liquid is located above the solid. The liquid is continuously discharged from the overflow port 42 through the overflow weir 41. When the solid concentration or amount in the annular collection tank 4 reaches the theoretical requirement, the pusher starts to push the solid out of the discharge port 43.

[0039] It should be noted that a small amount of liquid may be discharged along with the solid. Therefore, the continuous reaction separation device provided in this application requires an appropriate number of cycles of solid-liquid separation for solid recycling and reuse.

[0040] Furthermore, it should be noted that the pusher will not start working until the theoretical requirements for solid concentration or solid quantity are met. Therefore, the pusher provided in this embodiment can move relative to the stirring mechanism so that the pusher can be lifted away from the annular collection tank 4. In this way, the pusher can be prevented from pushing the solid within the annular collection tank 4, thus satisfying the above-mentioned condition of waiting for the solid concentration or solid quantity to reach the theoretical requirements.

[0041] In an optional example, the pusher includes a fixed connecting rod 61 and a scraper 62. One end of the fixed connecting rod 61 is connected to the stirring mechanism, and the scraper 62 is disposed at the other end of the fixed connecting rod 61 and located in the annular collection tank 4. The stirring mechanism rotates, causing the fixed connecting rod 61 to rotate. The fixed connecting rod 61 drives the scraper 62 to rotate in the annular collection tank 4 to push the solid to the discharge port 43 and discharge it outside the reactor cylinder 1.

[0042] In this embodiment, the fixed connecting rod 61 is inclined between the stirring mechanism and the annular collection tank 4. At the same time, the fixed connecting rod 61 can be raised to be perpendicular to the stirring mechanism. That is, when the pusher is not working, it is horizontally set in the reaction chamber. When working, the fixed connecting rod 61 is lowered, and the scraper 62 is placed in the annular collection tank 4 to push the solid out.

[0043] Alternatively, the end of the fixed connecting rod 61 connected to the stirring mechanism can move up and down relative to the stirring mechanism. When the pusher is not working, the fixed connecting rod 61 is lifted up along the stirring mechanism away from the annular collection tank 4. When the pusher is working, the fixed connecting rod 61 is lowered along the stirring mechanism so that the scraper 62 is placed in the annular collection tank 4 to push the solid out.

[0044] In an optional example, the fixed connecting rod 61 and the liquid distribution pipe 5 are arranged opposite each other on both sides of the stirring mechanism. It should be noted that although the operation of discharging solids is not continuous, the input of the mixed solid-liquid reactants into the annular collection tank 4 is continuous. When the pusher is working, the liquid distribution pipe 5 is still inputting the solid-liquid mixture. In order to avoid uniform discharge of reactants, the fixed connecting rod 61 and the liquid distribution pipe 5 are placed on both sides of the stirring mechanism, with a certain curvature and distance between them, to avoid the simultaneous discharge and input of solids.

[0045] It should be noted that, in practical applications, those skilled in the art can redesign the relative positions of the fixed connecting rod 61 and the liquid distribution pipe 5. For example, the included angle between the fixed connecting rod 61 and the liquid distribution pipe 5 can be set to 120 degrees, 90 degrees, or 150 degrees, etc. Since both the fixed connecting rod 61 and the liquid distribution pipe 5 are driven to rotate by the stirring mechanism, there will be no motion conflict. Therefore, such adjustments and changes to the relative positions of the fixed connecting rod 61 and the liquid distribution pipe 5 do not deviate from the principles and scope of this application and should be limited to the protection scope of this application.

[0046] In an optional example, the stirring mechanism includes a stirring shaft 21 and stirring blades 22. The stirring shaft 21 extends from the top to the bottom of the reaction chamber, and several stirring blades 22 are arranged on the stirring shaft 21. In this embodiment, two stirring blades 22 are arranged from top to bottom on the stirring shaft 21. By using two stirring blades 22 to stir the reactants in the reactor body 1, the reaction rate is accelerated, and the space occupied in the reactor body 1 is not excessive. Therefore, it is more reasonable to set two stirring blades 22. Of course, those skilled in the art can reasonably set the number of stirring blades 22. This embodiment does not impose a specific limitation on the number of stirring blades 22.

[0047] In an optional example, the continuous reaction separation device provided in this application embodiment further includes a solid discharge component. A solid discharge port 8 is provided on the side wall of the reactor cylinder 1, and the solid discharge component is disposed between the discharge port 43 and the solid discharge port 8.

[0048] Furthermore, the solid discharge component includes a discharge pipe 71 and a ball valve 72 disposed on the discharge pipe 71. The discharge pipe 71 is inclinedly disposed between the discharge port 43 and the solid discharge port 8, and the ball valve 72 is used to control the opening and closing of the discharge pipe 71.

[0049] In this embodiment, the discharge pipe 71 is inclined so that the solid in the annular collection tank 4 can slide from the discharge port 43 into the discharge pipe 71. The ball valve 72 of the discharge pipe 71 opens the discharge channel and is fixedly discharged from the solid discharge port 8 along the discharge pipe 71.

[0050] It should be noted that, in practical applications, recycling components can be installed at the solid discharge outlet 8 to facilitate the recycling of solids. Such flexible adjustments and changes do not deviate from the principles and scope of this application and should be limited to the protection scope of this application.

[0051] Furthermore, it should be noted that the ball valve 72 can be replaced with other control valves, as long as the opening and closing of the discharge pipe 71 can be guaranteed. Therefore, such adjustments and changes to the ball valve 72 do not deviate from the principles and scope of this application and should be limited to the protection scope of this application.

[0052] In an optional example, the continuous reaction separation device provided in this application embodiment further includes a lifting mechanism, which is disposed at the bottom of the reactor cylinder 1 and extends along the outer side wall of the reactor cylinder 1 into the liquid collection tank 3.

[0053] Furthermore, the lifting mechanism includes a lifting pipe 91 and a lifting pump 92 disposed on the lifting pipe 91. The lifting pipe 91 is disposed at the bottom outer end of the reactor body 1 and extends along the outer side wall of the reactor body 1 into the liquid collection tank 3. The lifting pump 92 is used to lift the mixed solids and liquids in the reactor body 1 along the lifting pipe 91 into the liquid collection tank 3.

[0054] In an optional example, the continuous reaction separation device provided in this application embodiment further includes a drive mechanism 10, which is connected to a stirring mechanism to drive the stirring mechanism to rotate.

[0055] In this embodiment of the application, the reactor cylinder 1 is further provided with a raw material inlet 11 for putting in the reaction raw materials and a vent 12 for discharging the internal reactants.

[0056] Example 2

[0057] The difference between this embodiment and Embodiment 1 is that it will provide a specific example to illustrate the process of solid-liquid reaction separation.

[0058] Specifically, the reaction of chloroethylene carbonate (CEC) with triethylamine to produce vinylene carbonate (VC) is taken as an example.

[0059] The original operating procedure: To address the issue of increased viscosity and decreased flowability caused by the formation of triethylamine hydrochloride solid particles during the reaction of CEC and triethylamine, a large amount of dimethyl carbonate (DMC) was typically added to the reactor as a solvent. After the reaction was complete, the entire volume was discharged, and the solid particles were filtered out using a centrifuge or plate and frame filter press. The solid particles were then washed, and the filtrate was distilled to separate the DMC and reused to obtain the product. At the end of the reaction, the proportion of DMC in the reactor was greater than 50%, all CEC had reacted, the VC content in the product was less than 30%, and the solid particle content was approximately 20%.

[0060] like Figures 1 to 3 As shown, in the continuous reaction separation device provided in this application embodiment, the liquid collection tank 3 is fixed on the stirring shaft 21, and the scraper 62 is fixed on the stirring shaft 21 through the fixed connecting rod 61. The liquid collection tank 3 and the fixed connecting rod 61 can rotate simultaneously with the stirring shaft 21. The scraper 62 and the fixed connecting rod 61 are connected by a vertically movable connecting component. When the scraper 62 is not working, it is located at the upper part of the annular collection tank 4.

[0061] A solid-liquid mixture is pumped from the bottom of reactor body 1 to a collection tank 3 at the top of reactor body 1 by a lift pump 92. The mixture is then distributed into an annular collection tank 4 via a distribution pipe 5 in the collection tank 3. The annular collection tank 4 is equipped with a toothed overflow weir 41. After passing through the overflow weir 41, the liquid returns to the reaction chamber of reactor body 1, while the solids remain in the annular collection tank 4. When the solid concentration or quantity in the annular collection tank 4 reaches the theoretical requirement, the lift pump 92 is stopped, the connecting rod 61 lowers the scraper 62, and the ball valve 72 is opened. The scraper 62 scrapes the solids in the annular collection tank 4 to the solid discharge port 8. After all solid particles are discharged, the ball valve 72 is closed, the connecting rod 61 is raised, the lift pump 92 is restarted, and the cycle begins again. The discharged solid particles can be directly recycled and reused in the washing process.

[0062] The advantages of using this device are: no solvent DMC is added to the reactor, and solid particles are continuously separated during the reaction. At the end of the reaction, the proportion of VC in the reactor reaches 70%-80%, the proportion of solid particles is 15%-18%, and the remainder is unreacted CEC and other byproducts.

[0063] In summary, the continuous reaction separation device provided in this application embodiment can integrate chemical reaction and solid-liquid separation of reactants into one device, realize the continuous separation of solid particles generated during the chemical reaction process, reduce or even eliminate the need for additional solvents, reduce equipment investment, and increase economic benefits.

[0064] It should be noted that the terms "one embodiment," "embodiment," "exemplary embodiment," "some embodiments," etc., mentioned in the specification indicate that the described embodiment may include a specific feature, structure, or characteristic, but not every embodiment necessarily includes that specific feature, structure, or characteristic. Furthermore, such phrases do not necessarily refer to the same embodiment. Moreover, when a specific feature, structure, or characteristic is described in connection with an embodiment, implementing such a feature, structure, or characteristic in conjunction with other embodiments, whether explicitly described or not, is within the knowledge scope of those skilled in the art.

[0065] It should be readily understood that the terms “on,” “above,” and “on top of” in this disclosure should be interpreted in the broadest possible sense, such that “on” means not only “directly on something” but also “on something” with an intermediate feature or layer therebetween, and that “above” or “on top of” means not only “on top of something” but also “on top of something” without an intermediate feature or layer therebetween (i.e., directly on something).

[0066] Furthermore, for ease of explanation, spatially relative terms such as "below," "below," "under," "above," and "above" may be used to describe the relationship of one element or feature relative to other elements or features as shown in the figures. Spatially relative terms are intended to encompass different orientations of the device in use or operation other than those shown in the figures. The device may have other orientations (rotated 90 degrees or in other orientations), and the spatially relative descriptive terms used herein may be interpreted accordingly.

[0067] It should be noted that, in this document, relational terms such as "first" and "second" are used merely to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitations, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.

[0068] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this application.

Claims

1. A continuous reaction separation device, characterized in that, include: The reactor cylinder has a reaction chamber inside, and the reaction chamber has a top end and a bottom end. A stirring mechanism is located at the top of the reaction chamber and extends from the top to the bottom of the reaction chamber. A liquid collection tank is disposed in the reaction chamber to collect the mixed solids and liquids. The liquid collection tank is connected to the stirring mechanism so that it can be driven to rotate by the stirring mechanism. An annular collecting trough is located below the liquid collecting trough. One end of the annular collecting trough is connected to the inner wall of the reactor cylinder. The annular collecting trough is provided with a discharge port and an overflow port. A liquid distribution pipe is connected to the bottom end of the liquid collection tank and extends into the annular collection tank. The pushing component is connected to the stirring mechanism; A lifting mechanism is provided at the bottom outer end of the reactor cylinder and extends along the outer side wall of the reactor cylinder into the liquid collection tank; During the reaction separation, the liquid distribution pipe rotates under the drive of the stirring mechanism to distribute the solids and liquids in the liquid collection tank into the annular collection tank. The pusher pushes the solids to the discharge port and discharges them out of the reactor cylinder, while the liquid is discharged from the overflow port into the reaction chamber.

2. The continuous reaction separation device according to claim 1, characterized in that, The annular collection trough is provided with a toothed overflow weir at its edge.

3. The continuous reaction separation device according to claim 1, characterized in that, The pushing component includes a fixed connecting rod and a scraper. One end of the fixed connecting rod is connected to the stirring mechanism, and the scraper is disposed at the other end of the fixed connecting rod and located in the annular collection trough. The stirring mechanism rotates, causing the fixed connecting rod to rotate. The fixed connecting rod then drives the scraper to rotate within the annular collection trough, pushing the solids to the discharge port and discharging them outside the reactor cylinder.

4. The continuous reaction separation device according to claim 3, characterized in that, The fixed connecting rods are positioned on both sides of the stirring mechanism, opposite to the liquid distribution pipe.

5. The continuous reaction separation apparatus according to claim 1, characterized in that, The stirring mechanism includes a stirring shaft and stirring blades. The stirring shaft extends from the top to the bottom of the reaction chamber, and several stirring blades are arranged on the stirring shaft.

6. The continuous reaction separation apparatus according to claim 1, characterized in that, It also includes a solid discharge component, wherein a solid discharge port is provided on the side wall of the reactor cylinder, and the solid discharge component is disposed between the discharge port and the solid discharge port.

7. The continuous reaction separation apparatus according to claim 6, characterized in that, The solid discharge component includes a discharge pipe and a ball valve disposed on the discharge pipe. The discharge pipe is inclined between the discharge port and the solid discharge port, and the ball valve is used to control the opening and closing of the discharge pipe.

8. The continuous reaction separation apparatus according to claim 1, characterized in that, The lifting mechanism includes a lifting pipe and a lifting pump mounted on the lifting pipe. The lifting pipe is located at the bottom outer end of the reactor cylinder and extends along the outer side wall of the reactor cylinder into the liquid collection tank. The lifting pump is used to lift the solids and liquids mixed in the reactor cylinder into the liquid collection tank along the lifting pipe.

9. The continuous reaction separation apparatus according to any one of claims 1 to 8, characterized in that, It also includes a drive mechanism, which is connected to the stirring mechanism to drive the stirring mechanism to rotate.

Images