CN117797755A - Continuous reaction separation device - Google Patents

Abstract

The application relates to a serialization reaction separator, include: a reaction chamber is arranged in the reactor cylinder, and the reaction chamber is provided with a top end and a bottom end which are opposite; the stirring mechanism is arranged at the top end of the reaction chamber and extends from the top end to the bottom end of the reaction chamber; the liquid collecting tank is arranged in the reaction chamber and used for containing mixed solids and liquid, and is connected with the stirring mechanism so as to be driven by the stirring mechanism to rotate; the annular collecting tank is arranged below the liquid collecting tank, one end of the annular collecting tank is connected with the inner wall of the reactor barrel, and the annular collecting tank is provided with a discharge port and an overflow port; the liquid distribution pipe is connected to the bottom end of the liquid collecting groove and extends into the annular collecting groove, and the pushing piece is connected with the stirring mechanism. According to the continuous reaction separation device provided by the application, the solid and the liquid generated in the reaction can be continuously separated without the aid of a solvent.

Description

Continuous reaction separation device

Technical Field

The application relates to the technical field of chemical equipment, in particular to a continuous reaction separation device.

Background

In the process of synthesizing new substances such as chemistry and chemical industry, a large amount of solids are often generated in the liquid phase reaction process, the solids are not expected products, the solids gradually increase along with the continuous progress of the reaction, the viscosity of the whole reaction system is increased, the fluidity is deteriorated, the power consumption of mechanical stirring is increased, and in order to solve the situation, one or more solvents are usually considered to be additionally added, so that the consumption of the solvents is increased, the concentration of expected products in the reaction system is reduced, more separation cost is increased, and even the production efficiency is affected.

Disclosure of Invention

The object of the present application is to provide a continuous reaction separation apparatus which can continuously separate solids and liquids generated in a reaction without the aid of a solvent.

To this end, embodiments of the present application provide a continuous reaction separation device, including: a reaction chamber is arranged in the reactor cylinder, and the reaction chamber is provided with a top end and a bottom end which are opposite; the stirring mechanism is arranged at the top end of the reaction chamber and extends from the top end to the bottom end of the reaction chamber; the liquid collecting tank is arranged in the reaction chamber and used for containing mixed solids and liquid, and is connected with the stirring mechanism so as to be driven by the stirring mechanism to rotate; the annular collecting tank is arranged below the liquid collecting tank, one end of the annular collecting tank is connected with the inner wall of the reactor barrel, and the annular collecting tank is provided with a discharge port and an overflow port; the liquid distribution pipe is connected to the bottom end of the liquid collecting groove and extends into the annular collecting groove, and the pushing piece is connected with the stirring mechanism; when the reaction is separated, the liquid distribution pipe rotates under the drive of the stirring mechanism so as to disperse the solids and the liquid in the liquid collecting tank into the annular collecting tank, the pushing piece pushes the solids to the discharge port to be discharged out of the reactor cylinder, and the liquid is discharged into the reaction cavity from the overflow port.

In one possible implementation, the edge of the annular collecting trough is provided with a toothed overflow weir.

In one possible implementation, the pushing member comprises a fixed connecting rod and a scraping plate, one end of the fixed connecting rod is connected with the stirring mechanism, and the scraping plate is arranged at the other end of the fixed connecting rod and positioned in the annular collecting groove; wherein, the stirring mechanism rotates to drive the fixed connecting rod to rotate, and the fixed connecting rod drives the scraping plate to rotate in the annular collecting groove so as to push solids to the discharge port to be discharged out of the reactor cylinder.

In one possible implementation, the fixed connecting rod is arranged on two sides of the stirring mechanism opposite to the liquid distribution pipe.

In one possible implementation, the stirring mechanism comprises a stirring shaft and stirring blades, the stirring shaft extends from the top end to the bottom end of the reaction chamber, and the stirring blades are provided with a plurality of stirring blades on the stirring shaft.

In one possible implementation, the reactor further comprises a solid discharge member, a solid discharge port is provided on a side wall of the reactor vessel, and the solid discharge member is provided between the discharge port and the solid discharge port.

In one possible implementation, the solid discharging member includes a discharging pipe and a ball valve disposed on the discharging pipe, the discharging pipe is obliquely disposed between the discharge port and the solid discharging port, and the ball valve is used for controlling opening and closing of the discharging pipe.

In one possible implementation, the reactor further comprises a lifting mechanism disposed at an outer bottom end of the reactor vessel and extending into the sump along an outer sidewall of the reactor vessel.

In one possible implementation, the lifting mechanism includes a lifting tube disposed at an outer bottom of the reactor vessel and extending along an outer sidewall of the reactor vessel into the sump, and a lifting pump disposed on the lifting tube for lifting mixed solids and liquids within the reactor vessel along the lifting tube into the sump.

In one possible implementation, the stirring device further comprises a driving mechanism, and the driving mechanism is connected with the stirring mechanism to drive the stirring mechanism to rotate.

According to the continuous reaction separation device provided by the embodiment of the application, the chemical reaction and the solid-liquid separation of reactants can be integrated in one device, so that solid particles generated in the chemical reaction process can be continuously separated, other solvents are reduced or even not added additionally, the equipment investment is reduced, and the economic benefit is increased.

Drawings

In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, a brief description will be given below of the drawings that are needed in the embodiments or the prior art descriptions, and it is obvious that the drawings in the following description are some embodiments of the present application, and that other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art. In addition, in the drawings, like parts are designated with like reference numerals and the drawings are not drawn to actual scale.

FIG. 1 shows a schematic structural diagram of a continuous reaction separation device provided in an embodiment of the present application;

FIG. 2 illustrates a top view of an annular collection trough provided by an embodiment of the present application;

FIG. 3 illustrates a front view of an annular collection trough provided in an embodiment of the present application;

reference numerals illustrate:

1. a reactor cylinder;

21. a stirring shaft; 22. stirring paddles;

3. a liquid collecting tank;

4. an annular collection tank; 41. an overflow weir; 42. an overflow port; 43. a discharge port;

5. a liquid distribution pipe;

61. a fixed connecting rod; 62. a scraper;

71. a discharge pipe; 72. a ball valve;

8. a solids discharge port;

91. a riser; 92. a lift pump;

10. a driving mechanism;

11. a raw material inlet;

12. and a discharge port.

Detailed Description

For the purposes of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present application based on the embodiments herein.

In the synthesis of new materials, such as chemical industry, a large amount of solids are often generated during the liquid phase reaction, and these solids are not desired products, so that these solids need to be separated, and the solids are treated by adding one or more solvents to the reactor and dissolving the solids by the solvents in the prior art, which increases the consumption of the solvents and reduces the concentration of the desired products in the reaction system. The production efficiency is affected; accordingly, embodiments of the present application provide a device capable of continuously separating solid-liquid reactants in a reaction system, without affecting reaction efficiency, while continuously separating solids generated in the reaction.

Example 1

As shown in fig. 1 to 3, the embodiment of the application provides a continuous reaction separation device, which comprises a reactor barrel 1, a stirring mechanism, a liquid collecting tank 3, an annular collecting tank 4, a liquid distribution pipe 5 and a pushing piece, wherein a reaction chamber is arranged inside the reactor barrel 1, and the reaction chamber is provided with a top end and a bottom end from top to bottom; the stirring mechanism is arranged at the top end of the reaction chamber and extends from the top end to the bottom end of the reaction chamber; the liquid collecting tank 3 is arranged in the reaction chamber and used for containing mixed solids and liquid, and the liquid collecting tank 3 is connected with the stirring mechanism so as to be driven by the stirring mechanism to rotate; the annular collecting tank 4 is arranged below the liquid collecting tank 3, one end of the annular collecting tank 4 is connected with the inner wall of the reactor barrel 1, and the annular collecting 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 collecting tank 3 and extends into the annular collecting tank 4, and the pushing piece is connected with the stirring mechanism.

Through the structure, the serialization reaction separator that this application embodiment provided is when the reaction separation, cloth liquid pipe 5 rotates under rabbling mechanism's drive, with solid and liquid in collecting vat 3 spread to annular collecting vat 4 in, the export of cloth liquid pipe 5 is located annular collecting vat 4 all the time, because cloth liquid pipe 5 is rotatory, consequently cloth liquid pipe 5 is with the scattering of mixed solid-liquid reactant one deck to annular collecting vat 4 in, and not carry a fixed position in annular collecting vat 4, avoided annular collecting vat 4's solid-liquid to pile up, the impeller rotates under rabbling mechanism's drive, thereby promote outside solid to annular collecting vat 4's discharge gate 43 discharge reactor barrel 1, liquid then is discharged to the reaction chamber from overflow port 42.

It should be noted that the reaction separation principle of the continuous reaction separation device provided by the application is as follows: in the chemical reaction, solid particles generated in the reaction process are all dispersed in the whole liquid phase system, under the action of gravity and buoyancy, the concentration of the solid particles gradually decreases from bottom to top in a reactor, and before the reaction reaches an expected end point, the solid-liquid mixture cannot be discharged through the bottom.

In an alternative example, the edge of the annular collecting trough 4 provided in the embodiments of the present application is provided with a toothed overflow weir 41. In this embodiment, the overflow weir 41 is an outlet weir, and is located at the bottom of the annular collecting tank 4 after the solids settle, and the liquid is located above the solids and continuously discharged from the overflow port 42 through the overflow weir 41, and when the concentration or amount of solids in the annular collecting tank 4 reaches the theoretical requirement, the pushing member starts to start pushing the solids out of the discharge port 43.

It should be noted that, it is not excluded that a small amount of liquid will be discharged along with the solid, so the continuous reaction separation device provided in the embodiments of the present application needs to perform the recycling solid-liquid separation for a proper number of times.

In addition, it should be noted that before the theoretical requirement of the solid concentration or the solid quantity is not met, the pushing member is not started to work, so that the pushing member provided in the embodiment of the application can move relative to the stirring mechanism so as to lift the pushing member away from the annular collecting tank 4, and thus, the pushing member can be prevented from always pushing the solid in the annular collecting tank 4, and the condition of waiting for the solid concentration or the solid quantity to meet the theoretical requirement is met.

In an alternative example, the pushing member includes a fixed link 61 and a scraper 62, one end of the fixed link 61 is connected to the stirring mechanism, and the scraper 62 is disposed at the other end of the fixed link 61 and located in the annular collecting tank 4; wherein, the stirring mechanism rotates to drive the fixed connecting rod 61 to rotate, and the fixed connecting rod 61 drives the scraping plate 62 to rotate in the annular collecting groove 4 so as to push the solid to the discharge hole 43 to be discharged out of the reactor cylinder 1.

In this embodiment, fixed connecting rod 61 slope sets up between rabbling mechanism and annular collecting vat 4, and fixed connecting rod 61 can rise to perpendicularly with the rabbling mechanism simultaneously, and the impeller level sets up in the reaction chamber when not working promptly, and at the during operation, fixed connecting rod 61 puts down, places scraper blade 62 in annular collecting vat 4 and promotes the solid to discharge.

Or, the end of the fixed connecting rod 61 connected with the stirring mechanism can move up and down relative to the stirring mechanism, when the pushing piece does not work, the fixed connecting rod 61 lifts up from the annular collecting tank 4 along the stirring mechanism, and when the pushing piece works, the fixed connecting rod 61 descends along the stirring mechanism so that the scraping plate 62 is placed in the annular collecting tank 4 to push solids to be discharged.

In an alternative example, the fixed links 61 are provided on both sides of the stirring mechanism opposite to the liquid distribution pipe 5. It should be noted that, although the operation of discharging the solid is not always performed, the operation of inputting the mixed solid-liquid reactant into the annular collecting tank 4 is continuously performed, and when the pushing member is operated, the liquid distribution pipe 5 is still inputting the solid-liquid mixture, so as to avoid the uniform discharge of the reactant, therefore, in the embodiment of the present application, the fixed connecting rod 61 and the liquid distribution pipe 5 are respectively arranged at two sides of the stirring mechanism, and the fixed connecting rod 61 and the liquid distribution pipe 5 have a certain radian and distance, so that the solid discharge and the solid input are avoided being simultaneously performed.

It should be noted that, in practical applications, a person skilled in the art may redesign the relative positions of the fixed connecting rod 61 and the liquid distribution tube 5, for example, the included angle between the fixed connecting rod 61 and the liquid distribution tube 5 is 120 degrees, 90 degrees or 150 degrees, and the like, and since the fixed connecting rod 61 and the liquid distribution tube 5 are driven to rotate by the stirring mechanism, no motion conflict occurs, and therefore, the adjustment and the change of the relative positions of the fixed connecting rod 61 and the liquid distribution tube 5 do not deviate from the principle and the scope of the present application, and should be limited in the protection scope of the present application.

In an alternative example, the stirring mechanism comprises a stirring shaft 21 and stirring blades 22, the stirring shaft 21 extending from the top to the bottom of the reaction chamber, the stirring blades 22 being provided in several numbers on the stirring shaft 21. In this embodiment, stirring paddle 22 is provided with two on (mixing) shaft 21 top-down, stirs the reactant in the reactor barrel 1 through two stirring paddles 22 for reaction rate to not too much occupy the space in the reactor barrel 1, so it is more reasonable to set up two stirring paddles 22. Of course, those skilled in the art may reasonably set the number of stirring paddles 22, and the setting of the number of stirring paddles 22 in the embodiment of the present application is not particularly limited.

In an alternative example, the continuous reaction separation device provided in the embodiment of the present application further includes a solid discharge member, where the solid discharge port 8 is provided on the sidewall of the reactor cylinder 1, and the solid discharge member is provided between the discharge port 43 and the solid discharge port 8.

Further, the solid discharging member includes a discharging pipe 71 and a ball valve 72 provided on the discharging pipe 71, the discharging pipe 71 is obliquely provided between the discharge port 43 and the solid discharging port 8, and the ball valve 72 is used for controlling opening and closing of the discharging pipe 71.

In the embodiment of the application, the discharge pipe 71 is obliquely arranged so as to enable solids in the annular collecting tank 4 to slide into the discharge pipe 71 from the discharge hole 43, a ball valve 72 of the discharge pipe 71 opens a discharge passage, and the solids are fixedly discharged from the solids discharge hole 8 along the discharge pipe 71.

It should be noted that, in practical applications, the solid discharge port 8 may be provided with a recycling member to recycle the recovered solid, and such flexible adjustment and modification should be limited within the scope and spirit of the present application.

In addition, it should be noted that the ball valve 72 may be replaced by another control valve, so long as the opening and closing of the discharge pipe 71 can be ensured, and thus, such adjustment and change of the replacement of the ball valve 72 do not deviate from the principle and scope of the present application, and all such adjustment and change should be limited to the protection scope of the present application.

In an alternative example, the continuous reaction separation device provided in the embodiments of the present application further includes a lifting mechanism disposed at the outer bottom of the reactor cylinder 1 and extending into the sump 3 along the outer sidewall of the reactor cylinder 1.

Further, the lifting mechanism comprises a lifting pipe 91 and a lifting pump 92 arranged on the lifting pipe 91, the lifting pipe 91 is arranged at the outer bottom end of the reactor cylinder 1 and extends into the liquid collecting tank 3 along the outer side wall of the reactor cylinder 1, and the lifting pump 92 is used for lifting the mixed solid and liquid in the reactor cylinder 1 into the liquid collecting tank 3 along the lifting pipe 91.

In an alternative example, the continuous reaction separation device provided in the embodiment of the present application further includes a driving mechanism 10, where the driving mechanism 10 is connected to the stirring mechanism to drive the stirring mechanism to rotate.

In the present embodiment, the reactor vessel 1 is further provided with a raw material inlet 11 for receiving a reaction raw material, and a discharge port 12 for discharging the reactant therein.

Example two

The present embodiment differs from the first embodiment in that the process of solid-liquid reaction separation will be specifically exemplified.

In particular, vinyl chloride carbonate (CEC) is reacted with triethylamine to produce Vinylene Carbonate (VC).

The original operation mode is as follows: in order to solve the problems of increased viscosity and poor fluidity of a reaction system caused by the generation of triethylamine hydrochloride solid particles in the reaction process of CEC and triethylamine, a large amount of dimethyl carbonate (DMC) is generally added into a reaction kettle as a solvent, after the reaction is completed, the solid particles are filtered out through a centrifuge or a plate frame filter press after the complete discharge, enter a washing procedure, and the distilled filtrate is separated and recycled to obtain the product. At the end of the reaction, the DMC accounts for more than 50 percent, CEC is reacted completely, the VC accounts for less than 30 percent, and the solid particles account for about 20 percent.

As shown in fig. 1 to 3, by the continuous reaction separation device provided in the embodiment of the present application, the liquid collecting tank 3 is fixed on the stirring shaft 21, the scraping plate 62 is fixed on the stirring shaft 21 by the fixing connecting rod 61, the liquid collecting tank 3 and the fixing connecting rod 61 can rotate simultaneously along with the stirring shaft 21, the scraping plate 62 is connected with the fixing connecting rod 61 by the connecting component capable of moving up and down, and the scraping plate 62 is located at the upper part of the annular collecting tank 4 when not working.

The solid-liquid mixture is lifted into the liquid collecting tank 3 at the upper part of the reactor cylinder 1 by the lift pump 92 at the bottom of the reactor cylinder 1, the solid-liquid mixture is distributed into the annular collecting tank 4 by the liquid distribution pipe 5 in the liquid collecting tank 3, the annular collecting tank 4 is provided with the toothed overflow weir 41, the liquid returns to the reaction chamber of the reactor cylinder 1 after passing through the overflow weir 41, and the solid is remained in the annular collecting tank 4. When the solid concentration or the solid quantity in the annular collecting tank 4 reaches the theoretical requirement, the lifting pump 92 is stopped, the fixed connecting rod 61 lowers the scraping plate 62, the ball valve 72 is opened, the scraping plate 62 scrapes the solid in the annular collecting tank 4 to the solid discharge port 8, after all solid particles are discharged, the ball valve 72 is closed, the fixed connecting rod 61 lifts the scraping plate 62, the lifting pump 92 is opened, and the next cycle is started. The discharged solid particles can directly enter a washing procedure and can be recycled.

The device has the beneficial effects that: solvent DMC is not added in the reaction kettle, and solid particles are continuously separated in the reaction process. When the reaction is finished, the VC in the reaction kettle accounts for 70% -80%, the solid particles account for 15% -18%, and the rest is unreacted CEC and other byproducts.

In summary, through the continuous reaction separation device provided by the embodiment of the application, the chemical reaction and the solid-liquid separation of reactants can be integrated in one device, so that solid particles generated in the chemical reaction process can be continuously separated, other solvents are reduced or even not added additionally, the equipment investment is reduced, and the economic benefit is increased.

It should be noted that references in the specification to "one embodiment," "an example embodiment," "some embodiments," etc., indicate that the embodiment described may include a particular feature, structure, or characteristic, but every embodiment may not necessarily include the particular feature, structure, or characteristic. Moreover, such phrases are not necessarily referring to the same embodiment. Furthermore, when a particular feature, structure, or characteristic is described in connection with an embodiment, it is submitted that it is within the knowledge of one skilled in the art to effect such feature, structure, or characteristic in connection with other embodiments whether or not explicitly described.

It should be readily understood that the terms "on … …", "above … …" and "above … …" in this disclosure should be interpreted in the broadest sense such that "on … …" means not only "directly on something", but also includes "on something" with intermediate features or layers therebetween, and "above … …" or "above … …" includes not only the meaning "on something" or "above" but also the meaning "above something" or "above" without intermediate features or layers therebetween (i.e., directly on something).

Further, spatially relative terms, such as "below," "beneath," "above," "over," and the like, may be used herein for ease of description to describe one element or feature's relationship to another element or feature as illustrated. Spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. The device may have other orientations (rotated 90 degrees or at other orientations), and the spatially relative descriptors used herein interpreted accordingly.

It should be noted that in this document, relational terms such as "first" and "second" and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.

Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the corresponding technical solutions from the scope of the technical solutions of the embodiments of the present application.

Claims (10)

1. A continuous reaction separation apparatus, comprising:

a reactor cylinder body, wherein a reaction chamber is arranged in the reactor cylinder body, and the reaction chamber is provided with a top end and a bottom end which are opposite;

the stirring mechanism is arranged at the top end of the reaction chamber and extends from the top end to the bottom end of the reaction chamber;

the liquid collecting tank is arranged in the reaction cavity and used for containing mixed solids and liquid, and is connected with the stirring mechanism so as to be driven by the stirring mechanism to rotate;

the annular collecting tank is arranged below the liquid collecting tank, one end of the annular collecting tank is connected with the inner wall of the reactor cylinder, and a discharge port and an overflow port are arranged on the annular collecting tank;

a liquid distribution pipe connected to the bottom end of the liquid collecting tank and extending into the annular collecting tank, and

the pushing piece is connected with the stirring mechanism;

when the reaction is separated, the liquid distribution pipe rotates under the drive of the stirring mechanism so as to disperse the solids and the liquid in the liquid collecting tank into the annular collecting tank, the pushing piece pushes the solids to the discharge port to be discharged out of the reactor cylinder, and the liquid is discharged from the overflow port into the reaction cavity.

2. The apparatus according to claim 1, wherein the annular collecting tank has a toothed overflow weir at the edge thereof.

3. The continuous reaction separation device according to claim 1, wherein the pushing member comprises a fixed connecting rod and a scraper, one end of the fixed connecting rod is connected with the stirring mechanism, and the scraper is arranged at the other end of the fixed connecting rod and is positioned in the annular collecting groove;

the stirring mechanism rotates to drive the fixed connecting rod to rotate, and the fixed connecting rod drives the scraping plate to rotate in the annular collecting groove so as to push solids to the discharge port to be discharged out of the reactor cylinder.

4. The apparatus according to claim 3, wherein the fixed link is disposed on both sides of the stirring mechanism opposite to the liquid distribution pipe.

5. The apparatus according to claim 1, wherein the stirring mechanism comprises a stirring shaft extending from a top end to a bottom end of the reaction chamber and stirring blades provided in a plurality on the stirring shaft.

6. The continuous reaction separation apparatus of claim 1, further comprising a solids discharge member provided with a solids discharge port on a sidewall of the reactor vessel, the solids discharge member being disposed between the discharge port and the solids discharge port.

7. The apparatus according to claim 6, wherein the solid discharge member comprises a discharge pipe and a ball valve provided on the discharge pipe, the discharge pipe being provided obliquely between the discharge port and the solid discharge port, the ball valve being for controlling opening and closing of the discharge pipe.

8. The continuous reaction separation apparatus of claim 1, further comprising a lifting mechanism disposed at an outer bottom end of the reactor vessel and extending into the sump along an outer sidewall of the reactor vessel.

9. The apparatus according to claim 8, wherein the lifting mechanism comprises a lifting pipe and a lifting pump provided on the lifting pipe, the lifting pipe being provided at an outer bottom end of the reactor cylinder and extending into the sump along an outer side wall of the reactor cylinder, the lifting pump being configured to lift the mixed solids and liquids in the reactor cylinder into the sump along the lifting pipe.

10. The apparatus according to any one of claims 1 to 9, further comprising a driving mechanism connected to the stirring mechanism to drive the stirring mechanism to rotate.