CN117772104A - Reaction separation device and method for vinylene carbonate - Google Patents

Reaction separation device and method for vinylene carbonate Download PDF

Info

Publication number
CN117772104A
CN117772104A CN202311814370.4A CN202311814370A CN117772104A CN 117772104 A CN117772104 A CN 117772104A CN 202311814370 A CN202311814370 A CN 202311814370A CN 117772104 A CN117772104 A CN 117772104A
Authority
CN
China
Prior art keywords
vinylene carbonate
reaction
centrifuge
solid
inner cylinder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202311814370.4A
Other languages
Chinese (zh)
Inventor
石鸿伟
唐圆桦
孙文兵
郎波
熊攀
陈真
王春林
张�成
唐倩
靳乾梅
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Donggeng Chemical Technology Co ltd
Original Assignee
Shanghai Donggeng Chemical Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanghai Donggeng Chemical Technology Co ltd filed Critical Shanghai Donggeng Chemical Technology Co ltd
Priority to CN202311814370.4A priority Critical patent/CN117772104A/en
Publication of CN117772104A publication Critical patent/CN117772104A/en
Pending legal-status Critical Current

Links

Landscapes

  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The application relates to a reaction separation device and a reaction separation method of vinylene carbonate, wherein the device comprises the following components: the reaction kettle comprises an inner cylinder and an outer cylinder, an interlayer is formed between the inner cylinder and the outer cylinder, and a solid outlet and a liquid outlet are respectively arranged on the outer side wall of the outer cylinder; the stirring mechanism is arranged in the inner cylinder and extends from the top end to the bottom end of the inner cylinder; the screw driving mechanism is arranged at one side of the bottom end of the outer cylinder; the spiral belt is arranged in the interlayer and spirally wound on the outer side wall of the inner cylinder, and comprises a plurality of liquid outlet holes, and the spiral belt is communicated with the inner cylinder at one side of the bottom end; the method comprises the following steps: adding chloroethylene carbonate and triethylamine into the inner cylinder, and reacting to obtain vinylene carbonate and triethylamine hydrochloride; and starting the screw driving mechanism to enable the vinylene carbonate and triethylamine hydrochloride to rise along the screw belt in a screw way. According to the reaction separation device and method for vinylene carbonate, provided by the application, solids and liquid can be continuously separated, the fluidity of reaction liquid is improved, and the use amount of a solvent is reduced.

Description

Reaction separation device and method for vinylene carbonate
Technical Field
The application relates to the technical field of chemical equipment, in particular to a reaction separation device and a reaction separation method for vinylene carbonate.
Background
The Vinylene Carbonate (VC) has the property of colorless transparent liquid, and is a novel organic film forming additive and overcharge protection additive for lithium ion batteries. The vinylene carbonate is used as the electrolyte additive of the lithium battery, can improve the high-low temperature property of the electrolyte, improve the specific capacity and the cycle life of the battery, has the overcharge protection effect, and is one of the products with the most ideal effect in the electrolyte additive of the lithium battery.
The existing industrial mature synthesis process of Vinylene Carbonate (VC) uses chloroethylene carbonate (CEC) and triethylamine (ET 3N) as raw materials, and removes one molecule of hydrogen chloride in the presence of a solvent in a reaction kettle to obtain vinylene carbonate and triethylamine hydrochloride, and because the triethylamine hydrochloride is insoluble in a VC reaction system, the triethylamine hydrochloride is produced as a solid in the reaction process, and the product VC is a heat-sensitive substance, and a small amount of polymerization can occur at the reaction temperature to produce a polymer with certain viscosity. In the VC reaction process, a large amount of solid triethylamine, VC polymer and raw materials are mixed to form a solid-liquid mixture with poor fluidity, particularly in the late reaction stage, the solid and the polymer are generated in a large amount along with the progress of the reaction, so that the whole reaction system forms a solid-liquid mixture with extremely poor fluidity, and even stirring cannot be operated due to increased resistance.
In order to achieve this, it is common in industry to add dimethyl carbonate, diethyl carbonate, etc. as a diluting solvent for improving the fluidity of the reaction system. In order to ensure the highest possible conversion, the addition of solvent amounts to 4 to 10 times the product, which ultimately results in a reaction product content of only 10 to 20% after the reaction has been completed, which places a great burden on the subsequent separation. The addition of a large amount of solvent also causes great solvent loss in the subsequent working section, and three wastes are finally formed, so that the production cost is obviously increased, and the three wastes are also great. In addition, although a large amount of solvent is added, polymerization of VC products and generation of a large amount of triethylamine hydrochloride are carried out along with the reaction, the fluidity of a reaction system is poor, the mixing effect of fresh triethylamine and a solid-liquid mixture in a reaction kettle is poor, the effect of the later reaction is affected, and side reactions are increased.
Disclosure of Invention
The purpose of the present application is to provide a reaction separation device and a reaction separation method for vinylene carbonate, which can continuously separate solids and liquids generated in the reaction, ensure the fluidity of a reaction liquid in the reaction process, and reduce the use amount of a solvent.
In a first aspect, embodiments of the present application provide a reaction separation device for vinylene carbonate, including: the reaction kettle comprises an inner cylinder and an outer cylinder, an interlayer is formed between the inner cylinder and the outer cylinder, and a solid outlet and a liquid outlet are respectively arranged on the outer side wall of the outer cylinder; the stirring mechanism is arranged in the inner cylinder and extends from the top end to the bottom end of the inner cylinder; the screw driving mechanism is arranged at one side of the bottom end of the outer cylinder; the spiral belt is arranged in the interlayer and spirally wound on the outer side wall of the inner cylinder, and comprises a plurality of liquid outlet holes, and the spiral belt is communicated with the inner cylinder at one side of the bottom end; during reaction separation, the stirring mechanism stirs the solid-liquid reactants mixed in the inner cylinder, the screw driving mechanism drives the solid-liquid reactants mixed in the inner cylinder to rise along the screw belt in a screw mode, liquid falls into the interlayer from the liquid outlet hole, then is discharged from the liquid outlet, and solids rise to the solid outlet along the screw belt to be discharged.
In one possible implementation manner, the device further comprises a solid conveying mechanism and a centrifugal machine, wherein the solid conveying mechanism is arranged at the solid outlet, and the centrifugal machine is connected with the solid conveying mechanism; wherein the solid conveying mechanism is used for conveying the solid discharged from the solid outlet to the centrifugal machine.
In one possible implementation, a solvent adding member is disposed on the centrifuge, the solvent adding member includes a solvent adding container and a solvent adding pipe connected to each other, a cleaning port is formed on the centrifuge, and the solvent adding pipe is communicated with the cleaning port to add solvent into the centrifuge.
In one possible implementation, a return pipe is arranged on the centrifugal machine, and the return pipe is arranged between the centrifugal machine and the reaction kettle so as to communicate the centrifugal machine and the reaction kettle.
In one possible implementation, the device further comprises an annular collecting groove arranged in the inner cylinder, and the top end of the ribbon extends into the annular collecting groove.
In one possible implementation, the device further comprises a retainer ring, and the retainer ring covers the annular collecting groove.
In one possible implementation, the device further comprises a scraper, one end of the scraper is movably connected with the stirring mechanism, and the other end of the scraper is positioned in the annular collecting groove.
In one possible implementation, the device further comprises a dripping component, wherein the dripping component comprises a dripping container and a dripping pipe which are connected with each other, and the dripping pipe is communicated with the reaction kettle so as to drip reactants into the reaction kettle.
In a second aspect, an embodiment of the present application provides a reaction separation method for vinylene carbonate, where the reaction separation device for vinylene carbonate includes: adding chloroethylene carbonate and triethylamine into the inner cylinder, and reacting to obtain vinylene carbonate and triethylamine hydrochloride; starting a screw driving mechanism to enable vinylene carbonate and triethylamine hydrochloride to rise along a screw belt in a screw manner; wherein, vinylene carbonate falls into the interlayer from the liquid outlet hole, and then is discharged from the liquid outlet, and triethylamine hydrochloride rises to the solid outlet along the spiral belt to be discharged.
In one possible implementation, the reaction separation device of vinylene carbonate further comprises a solids conveying mechanism and a centrifuge, the method further comprising: conveying the triethylamine hydrochloride mixed with the liquid to a centrifugal machine through a solid conveying mechanism; the triethylamine hydrochloride of the mixed liquid was subjected to liquid separation by a centrifuge.
In one possible implementation, the centrifuge is provided with a solvent addition member, and the method further comprises: solvent is added to the centrifuge through a solvent addition means to clean the triethylamine hydrochloride.
In one possible implementation, the centrifuge is provided with a return pipe, and the method further includes: and the liquid separated in the centrifugal machine is returned to the reaction kettle through a return pipe.
According to the reaction separation device of vinylene carbonate, which is provided by the embodiment of the application, the chemical reaction and the solid-liquid separation of reactants can be integrated in one device, the liquid outlet holes are formed in the spiral belt, when the solid-liquid separation is carried out, the liquid can be discharged from the liquid outlet holes, the solids can rise into the annular groove through the spiral belt and are discharged through the scraping plate, so that solid particles generated in the chemical reaction process are continuously separated, and the chemical production efficiency is improved.
In addition, the reaction separation method of the vinylene carbonate is further provided on the basis of the reaction separation device of the vinylene carbonate, and the problems of low reaction efficiency, large solvent consumption, multiple side reactions, low conversion rate and the like caused by the difficulty in mixing reaction liquid and triethylamine due to poor fluidity of a reaction system caused by accumulation of triethylamine hydrochloride in the later period of VC reaction are solved by the method. By the method, the mixing effect of VC in the reaction kettle can be obviously improved, the use amount of the solvent is reduced, the VC yield is improved, and the waste liquid production amount is reduced.
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 is a schematic diagram showing the structure of a reaction separation device for vinylene carbonate according to an embodiment of the present application;
FIG. 2 shows a spiral schematic of a ribbon provided by an embodiment of the present application;
fig. 3 shows a schematic distribution diagram of liquid outlet holes according to an embodiment of the present application;
FIG. 4 shows a flow chart of a process for the reactive separation of vinylene carbonate provided in an embodiment of the present application;
reference numerals illustrate:
11. adding solvent into the container; 12. a solvent addition tube;
2. a cleaning port;
3. a centrifuge;
4. a centrifuge motor;
5. a solids discharge orifice;
6. a return pipe;
71. dripping a container; 72. a dropping tube;
8. a driving motor;
91. an inner cylinder; 92. an outer cylinder;
10. a retainer ring;
11. an annular collection tank;
12. a scraper;
131. a stirring shaft; 132. Oblique blade type stirring blade; 133. Propelling stirring blade;
14. a ribbon; 141. A liquid outlet hole;
15. a screw drive mechanism;
16. a solids outlet;
17. a solids conveying mechanism;
18. and a liquid outlet.
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.
The existing mature synthesis process of Vinylene Carbonate (VC) uses chloroethylene carbonate (CEC) and triethylamine (ET 3N) as raw materials, and removes one molecule of hydrogen chloride in the presence of a solvent in a reaction kettle to obtain vinylene carbonate and triethylamine hydrochloride, wherein the chemical equation of the reaction is as follows:
because triethylamine hydrochloride is insoluble in a VC reaction system, triethylamine hydrochloride is generated as a solid in the reaction process, and the product VC is a heat-sensitive substance and can be polymerized in a small amount at the reaction temperature to produce a polymer with certain viscosity. In the VC reaction process, a large amount of solid triethylamine, VC polymer and raw materials are mixed to form a solid-liquid mixture with poor fluidity, particularly in the late reaction stage, the solid and the polymer are generated in a large amount along with the progress of the reaction, so that the whole reaction system forms a solid-liquid mixture with extremely poor fluidity, and even stirring cannot be operated due to increased resistance.
In order to achieve this, dimethyl carbonate, diethyl carbonate, etc. are generally added as a diluting solvent in the prior art for improving the fluidity of the reaction system. The addition of a large amount of solvent leads to extremely large solvent loss in the subsequent working section, three wastes are finally formed, the production cost is obviously increased, in addition, although the addition of a large amount of solvent is carried out, the polymerization of VC products and the generation of a large amount of triethylamine hydrochloride are carried out along with the progress of the reaction, the fluidity of a reaction system is deteriorated, and the effect of the later reaction is further affected.
In order to ensure the fluidity of the reaction solution in the reaction process and reduce the use amount of the solvent, as shown in fig. 1 to 3, the embodiment of the present application provides a reaction separation device for vinylene carbonate, which comprises a reaction kettle, a stirring mechanism, a screw driving mechanism 15 and a screw belt 14: the reaction kettle is of a cylindrical structure and comprises an inner cylinder 91 and an outer cylinder 92, an interlayer is formed between the inner cylinder 91 and the outer cylinder 92, the width of the interlayer is adjustable according to actual conditions, a specific adjustment mode is that an expected space is reserved when the inner cylinder 91 and the outer cylinder 92 are installed, a solid outlet 16 and a liquid outlet 18 are respectively arranged on the outer side wall of the outer cylinder 92, the solid outlet 16 is arranged on one side of the top end of the outer cylinder 92, and the solid outlet 16 is arranged on the outer wall of the outer cylinder 92, but needs to be communicated with the inner cylinder 91 so as to facilitate solid discharge, and the liquid outlet 18 is arranged on one side of the bottom end of the outer cylinder 92 so as to facilitate liquid to naturally flow out of the reaction kettle by virtue of self gravity; the stirring mechanism is arranged in the inner cylinder 91 and extends from the top end to the bottom end of the inner cylinder 91, the spiral driving mechanism 15 is arranged at one side of the bottom end of the outer cylinder 92, and can be a driving device such as a motor, and is electrically connected with the inner cylinder 91 and can drive reactants to flow, the spiral belt 14 is arranged in the interlayer and spirally wound on the outer side wall of the inner cylinder 91, and comprises a plurality of liquid outlet holes 141, and the spiral belt 14 is communicated with the inner cylinder 91 at one side of the bottom end. During reaction separation, the stirring mechanism stirs the solid-liquid reactants mixed in the inner cylinder 91, the screw driving mechanism 15 drives the solid-liquid reactants mixed in the inner cylinder 91 to rise along the screw belt 14 in a screw manner, liquid falls into the interlayer from the liquid outlet 141 and then is discharged from the liquid outlet 18, and solids rise along the screw belt 14 to the solid outlet 16 and are discharged.
In an additional example, the ribbon 14 is a semi-tubular structure that is connected to the outer sidewall of the inner barrel 91. Specifically, the spiral ribbon 14 is a half round tube, the half tubular spiral ribbon 14 is tightly connected with the outer side wall of the inner cylinder 91 through the edge, or is arranged on the outer side wall of the inner cylinder 91 through an integrated forming mode, so that good tightness of the joint of the spiral ribbon 14 and the inner cylinder 91 is ensured, and solid is prevented from falling out of a spiral ascending track of the spiral ribbon 14.
Further, the spiral angle of the spiral belt 14 ranges from 5 ° to 85 °, and in this embodiment, the spiral angle of the spiral belt 14 is preferably 30 °, so that the slope of the spiral belt 14 can be not too steep and not too slow by such arrangement, which is conducive to conveying solids and avoids backflow caused by insufficient conveying of the reaction liquid solids due to unreasonable spiral angle.
Still further, as shown in fig. 3, the liquid outlet holes 141 are arranged on the ribbon 14 at regular triangle intervals, and by such arrangement, the arrangement of the liquid outlet holes 141 is reasonable, the number is proper, and the ribbon 14 is prevented from being jammed due to untimely liquid outflow.
Still further, the aperture of the liquid outlet hole 141 is 0.01mm to 10mm, specifically, the aperture size of the liquid outlet hole 141 can be determined according to the quantity of reactants and the liquid outflow, and preferably, the embodiment of the application can select 5mm holes to carry out liquid outlet, and the 5mm holes meet the requirements of most reactants and liquid flow, and meanwhile, the impurity solid generated under normal conditions can not be smaller than 5mm holes, so that the impurity is prevented from separating from the holes to influence the recovery of the liquid.
Still further, the interval between the adjacent liquid outlet holes 141 is 1mm to 50mm, and as mentioned above, the hole interval between the liquid outlet holes 141 can be determined according to the amount of the reactant and the outflow amount of the liquid, preferably, the interval of 25mm can be selected for setting, and the hole interval of 25mm satisfies the requirement of most of the reactant and the flow amount of the liquid.
In another additional example, the stirring mechanism provided in the embodiments of the present application includes a stirring shaft 131 and a plurality of stirring paddles disposed along an axial direction of the stirring shaft 131.
Further, the stirring blade is a bevel blade stirring blade 132 and/or a push type stirring blade 133, as shown in fig. 1, in this embodiment, the bevel blade stirring blade 132 and the push type stirring blade 133 are combined, the bevel blade stirring blade 132 has a certain inclined radian, and the push type stirring blade 133 can move up and down to stir, so that the reactant can be sufficiently stirred, the reaction is more complete, and the production efficiency is improved.
The stirring shaft 131 of the stirring mechanism needs to be connected to the driving motor 8 so as to power the stirring shaft 131 by the driving motor 8.
In an alternative example, the reaction separation device of vinylene carbonate provided in the embodiment of the present application further includes a solid conveying mechanism 17 and a centrifuge 3, the solid conveying mechanism 17 is disposed at the solid outlet 16, and the centrifuge 3 is connected with the solid conveying mechanism 17; wherein the solids conveying mechanism 17 is used for conveying solids discharged from the solids outlet 16 to the centrifuge 3.
Further, centrifuge 3 that this application embodiment provided is continuous airtight centrifuge, is provided with centrifuge motor 4 on the centrifuge 3, through motor drive centrifuge 3 operation, in addition, still is provided with solid discharge hole 5 on the centrifuge 3, sets up in centrifuge 3's bottom, can discharge the solid through solid discharge hole 5.
In an alternative example, the centrifuge 3 is provided with a solvent adding means including a solvent adding container 11 and a solvent adding pipe 12 connected to each other, the centrifuge 3 is provided with a washing port 2, and the solvent adding pipe 12 communicates with the washing port 2 to add the solvent into the centrifuge 3.
In an alternative example, a return pipe 6 is arranged on the centrifuge 3, the return pipe 6 is arranged between the centrifuge 3 and the reaction kettle to communicate the centrifuge 3 and the reaction kettle, and the return pipe 6 is used for conveying solid-liquid reactants separated in the centrifuge 3, entrained target products, solvents and the like back to the inner barrel 91 of the reaction kettle again for reaction, recycling materials and the like, and saving production cost.
In an alternative example, the reaction separation device for vinylene carbonate provided in the embodiment of the present application further includes an annular collecting groove 11 disposed in the inner cylinder 91, and the top end of the ribbon 14 extends into the annular collecting groove 11.
Further, a retainer ring 10 which is matched with the size of the annular collecting groove 11 is arranged on the annular collecting groove 11, and the retainer ring 10 is covered on the annular collecting groove 11.
Still further, the reaction separation device for vinylene carbonate provided in the embodiment of the present application further includes a scraper 12, one end of the scraper 12 is movably connected with the stirring mechanism, and the other end of the scraper 12 is located in the annular collecting groove 11.
In the embodiment of the present application, the retainer ring 10 can prevent solids from separating from the annular collecting tank 11, and the annular collecting tank 11 can be provided with a discharge port communicated with the solids outlet 16, so that the scraper 12 scrapes the solids, and the scraper 12 provided in the embodiment of the present application is a torsion spring type scraper 12, which has a certain elasticity, a buffering capacity and a good scraping effect; moreover, in the embodiment of the present application, the scraper 12 is obliquely disposed between the stirring mechanism and the annular collecting tank 11 through the connecting rod, and meanwhile, the connecting rod can be lifted up to be vertical to the stirring mechanism, that is, the scraper 12 is horizontally disposed in the inner cylinder 91 when not in operation, and when in operation, the connecting rod is put down, so that the scraper 12 is disposed in the annular collecting tank 11 to push solids to be discharged; or, the end of the connecting rod connected with the stirring mechanism can move up and down relative to the stirring mechanism, when the scraper 12 does not work, the connecting rod lifts up from the annular collecting groove 11 along the stirring mechanism, and when the scraper 12 works, the connecting rod descends along the stirring mechanism so that the scraper 12 is placed in the annular collecting groove 11 to push solids to be discharged.
In an alternative example, as shown in fig. 1, the reaction separation device for vinylene carbonate provided in the embodiment of the present application further includes a dripping member including a dripping container 71 and a dripping pipe 72 connected to each other, and the dripping pipe 72 communicates with the reaction kettle to drip the reactant into the reaction kettle.
According to the reaction separation device for vinylene carbonate, which is provided by the embodiment of the application, chemical reaction and solid-liquid separation of reactants can be integrated in one device, the liquid outlet hole 141 is formed in the spiral belt 14, when solid-liquid separation is performed, liquid can be discharged from the liquid outlet hole 141, solids can rise into the annular groove through the spiral belt 14 and are discharged through the scraping plate 12, so that solid particles generated in the chemical reaction process are continuously separated, and the chemical production efficiency is improved.
In addition, the embodiment of the application further provides a reaction separation method of vinylene carbonate based on the device, and the reaction separation device of vinylene carbonate is adopted, as shown in fig. 4, and the method comprises the following steps:
s1: adding chloroethylene carbonate and triethylamine into the inner cylinder 91, and reacting to obtain vinylene carbonate and triethylamine hydrochloride; the reaction separation device of the vinylene carbonate comprises a dripping component, wherein the dripping component comprises a dripping container 71 and a dripping pipe 72 which are connected with each other, the dripping pipe 72 is communicated with a reaction kettle, and chlorinated ethylene carbonate and triethylamine reactants can be dripped into the reaction kettle through the dripping component;
s2: starting the screw driving mechanism 15 to enable the vinylene carbonate and triethylamine hydrochloride to rise along the screw 14 in a screw mode;
wherein the vinylene carbonate falls into the interlayer from the liquid outlet 141 and is discharged from the liquid outlet 18, and the triethylamine hydrochloride rises along the spiral band 14 to the solid outlet 16 for discharge.
Further, the reaction and separation device of vinylene carbonate comprises a solid conveying mechanism 17 and a centrifuge 3, and according to the solid conveying mechanism 17 and the centrifuge 3, the method further comprises:
s3: conveying the triethylamine hydrochloride of the mixed liquid to the centrifugal machine 3 through a solid conveying mechanism 17;
s4: the liquid separation is carried out on the triethylamine hydrochloride of the mixed liquid through the centrifugal machine 3, wherein the centrifugal machine 3 provided by the embodiment of the application is a continuous sealed centrifugal machine 3, and continuous centrifugation of the triethylamine hydrochloride can be realized.
Further, the centrifuge 3 is provided with a solvent adding member comprising a solvent adding container 11 and a solvent adding tube 12 which are connected with each other, the centrifuge 3 is provided with a cleaning port 2, the solvent adding tube 12 is communicated with the cleaning port 2, and according to the solvent adding member, the method further comprises:
s5: solvent is added to centrifuge 3 by solvent addition means to clean triethylamine hydrochloride.
Further, the centrifuge 3 is provided with a return pipe 6, and according to the return pipe 6, the method further comprises:
s6: the liquid separated in the centrifuge 3 is returned to the reaction vessel through a return pipe 6.
The reaction separation method of the vinylene carbonate is further provided on the basis of the reaction separation device of the vinylene carbonate, and the problems of low reaction efficiency, large solvent consumption, multiple side reactions, low conversion rate and the like caused by difficult mixing of reaction liquid and triethylamine due to poor fluidity of a reaction system caused by accumulation of triethylamine hydrochloride in the later stage of VC reaction are solved by the method. By the method, the mixing effect of VC in the reaction kettle can be obviously improved, the solvent consumption is reduced by more than 50%, the VC yield is improved by about 10%, and the waste liquid yield is reduced by about 10%.
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 (12)

1. A reaction separation device for vinylene carbonate, comprising:
the reaction kettle comprises an inner cylinder and an outer cylinder, an interlayer is formed between the inner cylinder and the outer cylinder, and a solid outlet and a liquid outlet are respectively formed in the outer side wall of the outer cylinder;
the stirring mechanism is arranged in the inner cylinder and extends from the top end to the bottom end of the inner cylinder;
the screw driving mechanism is arranged at one side of the bottom end of the outer cylinder; and
the spiral belt is arranged in the interlayer and spirally wound on the outer side wall of the inner cylinder, and comprises a plurality of liquid outlet holes, and the spiral belt is communicated with the inner cylinder at one side of the bottom end;
when the reaction is separated, the stirring mechanism stirs the solid-liquid reactant mixed in the inner cylinder, the screw driving mechanism drives the solid-liquid reactant mixed in the inner cylinder to rise along the screw belt in a screw way, liquid falls into the interlayer from the liquid outlet hole and then is discharged from the liquid outlet, and solid rises to the solid outlet along the screw belt and is discharged.
2. The reaction separation device of vinylene carbonate according to claim 1, further comprising a solid conveying mechanism and a centrifuge, the solid conveying mechanism being provided at the solid outlet, the centrifuge being connected to the solid conveying mechanism;
wherein the solid conveying mechanism is used for conveying the solid discharged from the solid outlet to the centrifugal machine.
3. The reaction separation device of vinylene carbonate according to claim 2, wherein a solvent adding member is provided on the centrifuge, the solvent adding member includes a solvent adding container and a solvent adding pipe connected to each other, a washing port is provided on the centrifuge, and the solvent adding pipe communicates with the washing port to add a solvent into the centrifuge.
4. The reaction separation device for vinylene carbonate according to claim 2, wherein a return pipe is provided on the centrifuge, and the return pipe is provided between the centrifuge and the reaction kettle to communicate the centrifuge and the reaction kettle.
5. The reaction separation device of vinylene carbonate according to claim 1, further comprising an annular collection groove provided in the inner barrel, the tip of the ribbon extending into the annular collection groove.
6. The reaction separation device of vinylene carbonate according to claim 5, further comprising a retainer ring, wherein the retainer ring covers the annular collection tank.
7. The reaction separation device of vinylene carbonate according to claim 5, further comprising a scraper, wherein one end of the scraper is movably connected to the stirring mechanism, and the other end of the scraper is located in the annular collecting tank.
8. The reaction separation device of vinylene carbonate according to claim 1, further comprising a dropping member including a dropping container and a dropping pipe connected to each other, the dropping pipe being communicated with the reaction kettle to drop a reactant into the reaction kettle.
9. A reaction separation method of vinylene carbonate, characterized in that the reaction separation device of vinylene carbonate according to any one of claims 1 to 8 is employed, comprising:
adding chloroethylene carbonate and triethylamine into the inner cylinder, and reacting to obtain vinylene carbonate and triethylamine hydrochloride;
starting the screw driving mechanism to enable the vinylene carbonate and the triethylamine hydrochloride to rise along the screw belt in a screw way;
wherein, ethylene carbonate falls into the intermediate layer from the liquid outlet hole, discharges from the liquid outlet, and triethylamine hydrochloride rises to the solid outlet along the spiral shell area and discharges.
10. The process for the reactive separation of vinylene carbonate according to claim 9, characterized in that the device for the reactive separation of vinylene carbonate further comprises a solid conveying mechanism and a centrifuge, the process further comprising:
delivering the triethylamine hydrochloride of the mixed liquid to the centrifuge through the solid delivery mechanism;
the triethylamine hydrochloride of the mixed liquid was subjected to liquid separation by the centrifuge.
11. The method for the reaction separation of vinylene carbonate according to claim 10, characterized in that a solvent addition member is provided on the centrifuge, the method further comprising:
adding a solvent to the centrifuge through the solvent adding means to clean the triethylamine hydrochloride.
12. The reaction separation method of vinylene carbonate according to claim 11, characterized in that a return pipe is provided on the centrifuge, the method further comprising:
and the liquid separated in the centrifugal machine is refluxed into the reaction kettle through the reflux pipe.
CN202311814370.4A 2023-12-26 2023-12-26 Reaction separation device and method for vinylene carbonate Pending CN117772104A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202311814370.4A CN117772104A (en) 2023-12-26 2023-12-26 Reaction separation device and method for vinylene carbonate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202311814370.4A CN117772104A (en) 2023-12-26 2023-12-26 Reaction separation device and method for vinylene carbonate

Publications (1)

Publication Number Publication Date
CN117772104A true CN117772104A (en) 2024-03-29

Family

ID=90390409

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202311814370.4A Pending CN117772104A (en) 2023-12-26 2023-12-26 Reaction separation device and method for vinylene carbonate

Country Status (1)

Country Link
CN (1) CN117772104A (en)

Similar Documents

Publication Publication Date Title
CN211913714U (en) Sulfamic acid reation kettle of accurate feeding
CN117772104A (en) Reaction separation device and method for vinylene carbonate
CN107739325B (en) Equipment and process for continuously producing rubber vulcanization accelerator tetramethyl thiuram disulfide
CN206793616U (en) A kind of solid-liquid reaction kettle
TW201925088A (en) Methods, devices, and systems for processing of carbonaceous compositions
CN106986357A (en) A kind of pyrosulfurous acid mother liquid of sodium reclaiming system
CN208829569U (en) It is a kind of for synthesizing the device of trifluoroethanol
CN207845464U (en) A kind of oil field mud processing system
CN117797755A (en) Continuous reaction separation device
CN207072811U (en) A kind of environmentally friendly aluminium polychloride production system
CN112844245A (en) Auger type continuous reaction device and ash removal method thereof
CN218980487U (en) Vacuum pump sewage disposal equipment of rectifying device
CN107673432B (en) Chemical wastewater distillation kettle containing wall-sticking materials
CN206566885U (en) A kind of antioxidant production equipment of catalyst reusable edible
CN220737525U (en) Reaction unit that continuity was leached
CN210994229U (en) Reactor for coal liquefaction
CN219058856U (en) Continuous separation equipment for phenylacetic acid production
CN216890099U (en) Calcium hypochlorite production line
CN110142017A (en) A kind of chlorinated high polymers integration production platform
CN109651138A (en) Adipate monoester continuous producing method
CN103703110B (en) Byproduct white lime discharger
CN210823733U (en) Slurry transfer tank
CN216946493U (en) Real-time desulphurization device for acidized return liquid
CN109534994A (en) Adipate monoester process units of continuous feed and application thereof
CN116870808A (en) Esterification reaction device for ethyl chloroacetate processing

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination