CN111004204A - Process method for preparing vinylene carbonate by using microchannel reactor - Google Patents
Process method for preparing vinylene carbonate by using microchannel reactor Download PDFInfo
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- CN111004204A CN111004204A CN201911349042.5A CN201911349042A CN111004204A CN 111004204 A CN111004204 A CN 111004204A CN 201911349042 A CN201911349042 A CN 201911349042A CN 111004204 A CN111004204 A CN 111004204A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
- C07D317/32—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D317/34—Oxygen atoms
- C07D317/40—Vinylene carbonate; Substituted vinylene carbonates
Abstract
The invention belongs to the technical field of vinylene carbonate, in particular to a process method for preparing vinylene carbonate by using a microchannel reactor, wherein a drying device used in the process method comprises a shell; the upper plate surface of the first plate is communicated with a first cavity and a feed inlet which are enclosed by end covers, a plurality of through holes are arranged at the fixed connection part of the first plate and the side wall of the shell, the through holes are communicated with the first cavity, a first rod is symmetrically arranged on the outer ring of the lower plate of the first plate, the end part of the first rod extends out of a water outlet pipe arranged on the outer ring of the shell, and a liquid vaporization unit is arranged below the first plate; the liquid vaporization unit comprises a spray head, a first pipeline and a nitrogen pipeline; the boiling points of water and the ethylene carbonate liquid are different, so that water in the crude ethylene carbonate liquid is evaporated and removed, and meanwhile, nitrogen is an inert gas, so that the ethylene carbonate liquid is protected, and the ethylene carbonate liquid is prevented from being oxidized by the outside air.
Description
Technical Field
The invention belongs to the technical field of vinylene carbonate, and particularly relates to a process method for preparing vinylene carbonate by using a microchannel reactor.
Background
The lithium ion battery is a novel green energy source, is widely applied to energy storage products such as communication, household appliances, electric tools, electric bicycles, electric automobiles, solar energy, wind energy power generation and the like, and has wide development prospect. The addition of some additives in the lithium ion battery can improve various performances of the battery, the vinylene carbonate is used as an organic film forming additive and an overcharge protection additive of the lithium ion battery electrolyte, has good high and low temperature performances and an anti-flatulence function, and simultaneously the vinylene carbonate can form a compact electrolyte film between a positive electrode and a negative electrode of the lithium battery, so that the charge and discharge efficiency and the cycle life of the lithium battery are improved.
At present, vinylene carbonate preparation methods such as CN201510922630.9 and CN201410546929.4 belong to traditional processes, the general process is to carry out dechlorination on chloroethylene carbonate to obtain a crude product, and then the crude product is refined to obtain the final product vinylene carbonate.
Disclosure of Invention
Aiming at the defects of the prior art and solving the problems of complex and fussy process, more byproducts and higher moisture in the preparation of the vinylene carbonate by using a microchannel reactor, the invention provides a process method for preparing the vinylene carbonate by using the microchannel reactor.
The technical scheme adopted by the invention for solving the technical problems is as follows: the invention relates to a process method for preparing vinylene carbonate by using a microchannel reactor, which comprises the following steps:
s1: uniformly mixing chloroethylene carbonate and an ester solvent to obtain a mixed solution, heating the mixed solution to 25-35 ℃ through a preheater, heating triethylamine to 25-35 ℃ through the preheater, synchronously filling the preheated mixed solution and the triethylamine into a microchannel of a microchannel reactor, heating to 40-50 ℃, and then carrying out mixed reaction for 50-300 s;
s2: after the reactant in the microchannel reactor in the S1 finishes reacting, taking out the reactant from the microchannel reactor, wherein the reactant obtained at this moment is crude ethylene carbonate which contains moisture, and atomizing and removing the moisture in the crude ethylene carbonate liquid by using a drying device to obtain fine ethylene carbonate;
s3: collecting refined ethylene carbonate liquid dried in the step S2, and filling the refined ethylene carbonate liquid and an organic solvent into a storage tank together, wherein the organic solvent can be one or more of diethyl carbonate, dimethyl carbonate, ethyl methyl carbonate and ethylene carbonate, and the storage tank is placed at room temperature and kept in a dark place;
wherein the drying device described in the above method S2 includes a housing; the upper end of the shell is provided with an end cover connected through a bolt, the end cover is symmetrically provided with feed inlets, a first plate for condensing steam is arranged below the feed inlets, the first plate is in a V shape, the middle of the first plate is high, and two sides of the first plate are low; the liquid vaporization unit comprises a spray head, a first pipeline and a nitrogen pipeline; the nitrogen pipeline is positioned below the outer wall of the shell and extends into the shell and is communicated with the inside of the spray head; the spray head is in a circular truncated cone shape, a plurality of outlets for gas-liquid injection are formed in the upper end face of the spray head, nitrogen pipelines positioned in the spray head are symmetrically obliquely and upwards arranged, the lower end of the spray head is communicated with a first pipeline, and the first pipeline is fixedly connected inside the shell through a second rod; a discharge pipe is arranged at the bottom of the shell; the water in the ethylene carbonate is evaporated and removed through the cooperation of the first plate, the first rod and the liquid vaporization unit; when the jet-type gas-liquid mixer is used, firstly, nitrogen gas with the temperature of 120-130 ℃ is introduced into a nitrogen gas pipeline network nozzle, the nitrogen gas is sprayed out from the upper end of the nozzle, then crude ethylene carbonate liquid is thrown into a feeding port on an end cover, the crude ethylene carbonate liquid flows out of a first cavity, then flows into the shell through a through hole on a first plate, the nitrogen gas heats the crude ethylene carbonate liquid in the process that the crude ethylene carbonate liquid flows into the bottom of the shell, the nitrogen gas is cleaned in the nozzle and sprays the nitrogen gas upwards, the nitrogen gas enables negative pressure to be formed in the nozzle, then the negative pressure leads the crude ethylene carbonate liquid at the bottom of the shell to flow into a milling cutter nozzle through a first pipeline, then the nitrogen gas impacts on the crude ethylene carbonate liquid, and the nitrogen gas and the crude ethylene carbonate liquid are discharged; under the marked atmospheric pressure, the boiling point of water is 100 ℃, the boiling point of the ethylene carbonate liquid is 160 ℃, the temperature of nitrogen is between 120 ℃ and 130 ℃, the nitrogen can vaporize the moisture of the crude ethylene carbonate liquid, the vaporized water floats upwards in the shell and is attached to the plate surface of a plate, the vaporized water meets the plate with lower temperature and is condensed into water drops, finally the water drops slide to the joint of a rod and the plate through the inclined plate, and finally the water drops flow out of the water pipe through the rod; the boiling points of water and the ethylene carbonate liquid are different, so that water in the crude ethylene carbonate liquid is evaporated and removed, and meanwhile, nitrogen is an inert gas, so that the ethylene carbonate liquid is protected, and the ethylene carbonate liquid is prevented from being oxidized by the outside air.
Preferably, a rotating impeller is arranged in the spray head; the rotating shaft of the rotating impeller is hinged at the upper end of the spray head; the nitrogen sprayed from the nitrogen pipeline impacts the rotating impeller to push the rotating impeller to rotate, so as to further promote the vaporization of the water in the ethylene carbonate liquid; when the device is used, nitrogen is discharged into the spray head, then the nitrogen impacts the rotating impeller, when crude ethylene carbonate liquid flows into the spray head, the rotating impeller rotates to stir the crude ethylene carbonate liquid, so that bubbles are generated in the crude ethylene carbonate liquid, after the crude ethylene carbonate liquid is sprayed out from the spray head along with the bubbles communicated with the nitrogen, the crude ethylene carbonate liquid is atomized into water drops, and meanwhile, moisture in the crude ethylene carbonate liquid is more beneficial to being vaporized.
Preferably, the lower end of the rotating shaft of the rotating impeller extends out of the lower end of the first pipeline and is connected with the stirring impeller; stirring the ethylene carbonate liquid in the shell by a stirring impeller so as to stir bubbles in the ethylene carbonate and further promote the vaporization of the moisture of the ethylene carbonate liquid; during the use, nitrogen impact is on rotating impeller, rotating impeller rotates and drives stirring impeller through the pivot and rotate, then stirring impeller stirs the crude product ethylene carbonate liquid of casing bottom, produce the bubble in the crude product ethylene carbonate liquid, then in crude product ethylene carbonate liquid gets into the shower nozzle through a pipeline with the bubble together, the crude product ethylene carbonate liquid of bubble that accompanies, after being atomized by nitrogen gas, moisture in the crude product ethylene carbonate liquid is more favorable to by the vaporization, further improve the evaporation rate of moisture in the crude product ethylene carbonate liquid, thereby improve the purity of ethylene carbonate.
Preferably, the lower end surface of the first plate is provided with a plurality of guide strips for guiding water flow, and the guide strips are radially arranged on the lower plate surface of the first plate from the connection part of the first plate and the first rod; the guide strip guides the water condensed on the first plate to flow out of the water outlet pipe from the first rod, so that the condensed water is prevented from dripping into the vinylene carbonate liquid in the shell; when the water-saving device is used, vaporized water is adhered to a first plate, then water drops become larger and larger, then the water drops roll on the plate surface of the first plate and are mutually condensed together, then the water drops slide down to the joint of a first rod and the first plate along the guide strip, and finally the water drops flow out of the water outlet pipe along the first rod; the guide strip guides the condensed water drops on the surface of the first plate to roll, so that the water drops are prevented from directly falling back to the vinylene carbonate liquid in the shell instead of flowing out of the shell when rolling, and the purity of the vinylene carbonate liquid is improved.
Preferably, a liquid storage cavity is formed in the first plate and is communicated with the first cavity and the through hole in the first plate; the condensation of water vapor is further promoted by arranging a liquid storage cavity in the first plate; when the device is used, crude ethylene carbonate liquid is filled into the first cavity from the feeding hole, the temperature of the filled crude ethylene carbonate liquid is 25-35 ℃, then the crude ethylene carbonate liquid flows into the liquid storage cavity, then the crude ethylene carbonate liquid flows into the bottom of the shell from the through hole of the first plate, the liquid storage cavity is filled with the crude ethylene carbonate liquid with the temperature of 25-35 ℃, so that the temperature of the plate surface of the first plate is also kept between 25 and 35 ℃, and when vaporized water is adhered to the plate surface of the first plate, the vaporized water is more beneficial to being condensed into water beads and adhered to the plate surface of the first plate due to the temperature difference between the plate surface temperature of the first plate and the vaporized water; the first plate is cooled through the crude product vinylene carbonate liquid, and the phenomenon that vaporized water loses the effect of condensing vaporized water after continuously heating the first plate and heating is avoided.
Preferably, the nitrogen pipeline is wound on the outer ring of the first pipeline and extends into the air injection channel; winding the carbon dioxide gas pipe on a first pipeline through a nitrogen pipeline, and preheating the ethylene carbonate liquid in the first pipeline; during the use, twine the nitrogen gas pipeline on pipeline one for vaporization blowout moisture is preheated in advance in the shower nozzle, also preheats the crude product ethylene carbonate liquid of casing bottom simultaneously, promotes the vaporization of the moisture in the crude product ethylene carbonate liquid, further improves the evaporation rate of moisture in the crude product ethylene carbonate liquid, thereby improves the purity of ethylene carbonate.
The invention has the technical effects and advantages that:
1. according to the process method for preparing the vinylene carbonate by using the microchannel reactor, water in the crude vinylene carbonate liquid is evaporated and removed by utilizing the difference between boiling points of water and the vinylene carbonate liquid, and meanwhile, nitrogen is an inert gas, so that the vinylene carbonate liquid is protected, and the vinylene carbonate liquid is prevented from being oxidized by external air.
2. The invention relates to a process method for preparing vinylene carbonate by using a microchannel reactor, which comprises the steps of rotating an impeller to stir crude vinylene carbonate liquid to generate bubbles in the crude vinylene carbonate liquid, atomizing the crude vinylene carbonate liquid into water beads to be refined again after the crude vinylene carbonate liquid is sprayed out from a spray head along with bubbles and communicated with nitrogen, and simultaneously, the moisture in the crude vinylene carbonate liquid is more beneficial to being vaporized to further improve the evaporation rate of the moisture in the crude vinylene carbonate liquid, thereby improving the purity of the vinylene carbonate.
3. According to the process method for preparing the vinylene carbonate by using the microchannel reactor, the guide strips guide the condensed water beads on the surface of the first plate to roll, so that the water beads are prevented from directly falling back to the vinylene carbonate liquid in the shell instead of flowing out of the shell when the water beads roll, and the purity of the vinylene carbonate liquid is improved.
Drawings
The invention will be further explained with reference to the drawings.
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a perspective view of a drying apparatus used in the present invention;
FIG. 3 is a cross-sectional view of a drying apparatus used in the present invention;
FIG. 4 is an enlarged view of a portion of FIG. 3 at A;
FIG. 5 is a partial enlarged view at B in FIG. 3;
FIG. 6 is a bottom view of a number plate;
in the figure: the device comprises a shell 1, an end cover 11, a feed inlet 111, a water outlet pipe 12, a discharge pipe 13, a first plate 2, a through hole 21, a first cavity 22, a first rod 23, a guide strip 24, a liquid storage cavity 25, a liquid vaporization unit 3, a spray head 31, a rotating impeller 311, a stirring impeller 312, a first pipeline 32, a second rod 321 and a nitrogen pipeline 33.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
As shown in fig. 1-6, the process for preparing vinylene carbonate by using a microchannel reactor according to the present invention comprises the following steps:
s1: uniformly mixing chloroethylene carbonate and an ester solvent to obtain a mixed solution, heating the mixed solution to 25-35 ℃ through a preheater, heating triethylamine to 25-35 ℃ through the preheater, synchronously filling the preheated mixed solution and the triethylamine into a microchannel of a microchannel reactor, heating to 40-50 ℃, and then carrying out mixed reaction for 50-300 s;
s2: after the reactant in the microchannel reactor in the S1 finishes reacting, taking out the reactant from the microchannel reactor, wherein the reactant obtained at this moment is crude ethylene carbonate which contains moisture, and atomizing and removing the moisture in the crude ethylene carbonate liquid by using a drying device to obtain fine ethylene carbonate;
s3: collecting refined ethylene carbonate liquid dried in the step S2, and filling the refined ethylene carbonate liquid and an organic solvent into a storage tank together, wherein the organic solvent can be one or more of diethyl carbonate, dimethyl carbonate, ethyl methyl carbonate and ethylene carbonate, and the storage tank is placed at room temperature and kept in a dark place;
wherein the drying device described in the above method S2 includes a housing 1; an end cover 11 connected through bolts is arranged at the upper end of the shell 1, feed inlets 111 are symmetrically formed in the end cover 11, a first plate 2 used for condensing steam is arranged below the feed inlets 111, the first plate 2 is in a letter V shape, the first plate 2 is high in the middle and low in two sides, a first cavity 22 formed by the upper plate surface of the first plate 2 and the end cover 11 in a surrounding mode is communicated with the feed inlets 111, a plurality of through holes 21 are formed in the positions, fixedly connected with the side wall of the shell 1, of the first plate 2, the through holes 21 are communicated with the first cavity 22, a first rod 23 is symmetrically arranged on the outer ring of the lower plate of the first plate 2, the end part of the first rod 23 extends out of a water outlet pipe 12 arranged on the outer ring of the shell 1, and a liquid vaporization; the liquid vaporization unit 3 comprises a spray head 31, a first pipeline 32 and a nitrogen pipeline 33; the nitrogen pipeline 33 is positioned below the outer wall of the shell 1, and the nitrogen pipeline 33 extends into the shell 1 and is communicated with the inside of the spray head 31; the spray head 31 is in a circular truncated cone shape, a plurality of outlets for gas-liquid injection are formed in the upper end face of the spray head 31, the nitrogen pipelines 33 located in the spray head 31 are symmetrically arranged obliquely upwards, the lower end of the spray head 31 is communicated with the first pipeline 32, and the first pipeline 32 is fixedly connected inside the shell 1 through the second rod 321; a discharge pipe 13 is arranged at the bottom of the shell 1; the water in the ethylene carbonate is evaporated and removed through the cooperation of the first plate 2, the first rod 23 and the liquid vaporization unit 3; when the device is used, firstly, 120-plus 130 ℃ nitrogen is introduced into the net spray head 31 through the nitrogen pipeline 33, the nitrogen is sprayed out from the upper end of the spray head 31, then crude ethylene carbonate liquid is put into the feed inlet 111 on the end cover 11, the crude ethylene carbonate liquid flows out of the first cavity 22, then the nitrogen flows into the shell 1 through the through hole 21 on the first plate 2, the crude ethylene carbonate liquid is heated by the nitrogen in the process that the crude ethylene carbonate liquid flows into the bottom of the shell 1, the nitrogen is cleaned in the spray head 31 and sprayed upwards to form negative pressure in the spray head 31, then the negative pressure leads the crude ethylene carbonate liquid at the bottom of the shell 1 to be sprayed into the spray head 31 through the first pipeline 32, then the nitrogen impacts on the crude ethylene carbonate liquid, and the nitrogen and the crude ethylene carbonate liquid are discharged from the outlet of the spray head 31 together; under the marked atmospheric pressure, the boiling point of water is 100 ℃, the boiling point of the vinylene carbonate liquid is 160 ℃, the temperature of nitrogen is between 120 ℃ and 130 ℃, the nitrogen can vaporize the moisture of the crude vinylene carbonate liquid, the vaporized water floats upwards in the shell 1 and is attached to the plate surface of the plate 2, the vaporized water meets the plate 2 with lower temperature and is condensed into water drops, finally the water drops slide to the joint of the first rod 23 and the first plate 2 through the inclined plate 2, and finally the water drops flow out of the water pipe 12 through the first rod 23; the boiling points of water and the ethylene carbonate liquid are different, so that water in the crude ethylene carbonate liquid is evaporated and removed, and meanwhile, nitrogen is an inert gas, so that the ethylene carbonate liquid is protected, and the ethylene carbonate liquid is prevented from being oxidized by the outside air.
As an embodiment of the present invention, a rotating impeller 311 is provided in the nozzle 31; the rotating shaft of the rotating impeller 311 is hinged at the upper end of the spray head 31; the nitrogen sprayed from the nitrogen pipeline 33 impacts the rotating impeller 311 to push the rotating impeller 311 to rotate, thereby further promoting the vaporization of the water in the vinylene carbonate liquid; when the device is used, nitrogen is discharged into the spray head 31, then the nitrogen impacts the rotating impeller 311, when crude ethylene carbonate liquid flows into the spray head 31, the rotating impeller 311 rotates to stir the crude ethylene carbonate liquid, so that bubbles are generated in the crude ethylene carbonate liquid, after the crude ethylene carbonate liquid is sprayed out from the spray head 31 along with the bubbles and the nitrogen, atomized water drops of the crude ethylene carbonate liquid are refined again, and meanwhile, moisture in the crude ethylene carbonate liquid is more beneficial to being vaporized.
As an embodiment of the present invention, the lower end of the rotating shaft of the rotating impeller 311 extends out of the lower end of the first pipe 32 and is connected with the stirring impeller 312; stirring the vinylene carbonate liquid in the shell 1 by the stirring impeller 312, so that bubbles are stirred in the vinylene carbonate, and further promoting the vaporization of the moisture of the vinylene carbonate liquid; when the device is used, nitrogen impacts on the rotating impeller 311, the rotating impeller 311 rotates to drive the stirring impeller 312 to rotate through the rotating shaft, then the stirring impeller 312 stirs crude ethylene carbonate liquid at the bottom of the shell 1, bubbles are generated in the crude ethylene carbonate liquid, then the crude ethylene carbonate liquid and the bubbles enter the spray head 31 through the first pipeline 32, the crude ethylene carbonate liquid accompanied by the bubbles is atomized by the nitrogen, moisture in the crude ethylene carbonate liquid is more beneficial to being vaporized, the evaporation rate of the moisture in the crude ethylene carbonate liquid is further improved, and the purity of the ethylene carbonate is improved.
As an embodiment of the present invention, the lower end surface of the first plate 2 is provided with a plurality of guide strips 24 for guiding water flow, and the guide strips 24 are radially arranged on the lower plate surface of the first plate 2 from the connection position of the first plate 2 and the first rod 23; the condensed water on the first plate 2 is guided to flow out of the water outlet pipe 12 from the first rod 23 through the guide strip 24, so that the condensed water is prevented from dripping into the ethylene carbonate liquid in the shell 1 again; when the water-saving device is used, vaporized water is adhered to the first plate 2, then water drops become larger and larger, then the water drops roll on the plate surface of the first plate 2 and are mutually condensed together, then the water drops slide down to the joint of the first rod 23 and the first plate 2 along the guide strip 24, and finally the water drops flow out of the water outlet pipe 12 along the first rod 23; the guide strip 24 guides the condensed water drops on the surface of the first plate 2 to roll, so that the water drops are prevented from directly falling back to the ethylene carbonate liquid in the shell 1 instead of flowing out of the shell 1 when rolling, and the purity of the ethylene carbonate liquid is improved.
As an embodiment of the invention, a liquid storage cavity 25 is formed in the first plate 2, and the liquid storage cavity 25 communicates with the first cavity 22 and the through hole 21 on the first plate 2; the condensation of water vapor is further promoted by arranging a liquid storage cavity 25 in the first plate 2; when the device is used, crude ethylene carbonate liquid is filled into the first cavity 22 from the feeding hole 111, the temperature of the filled crude ethylene carbonate liquid is 25-35 ℃, then the crude ethylene carbonate liquid flows into the liquid storage cavity 25, then the crude ethylene carbonate liquid flows into the bottom of the shell 1 from the through hole 21 of the first plate 2, the temperature of the plate surface of the first plate 2 is kept between 25 and 35 ℃ due to the fact that the crude ethylene carbonate liquid with the temperature of 25-35 ℃ is filled into the liquid storage cavity 25, and when vaporized water is adhered to the plate surface of the first plate 2, the temperature difference between the plate surface temperature of the first plate 2 and the temperature of the vaporized water is reduced, so that the water is beneficial to being condensed into water beads and adhered to the plate surface of the first plate 2; the first plate 2 is cooled through the crude product ethylene carbonate liquid, and the phenomenon that the vaporized water loses the effect of condensing vaporized water after continuously heating the first plate 2 for temperature rise is avoided.
As an embodiment of the present invention, the nitrogen pipeline 33 is wound around the outer ring of the first pipeline 32 and extends into the air injection channel; winding the first pipeline 32 through a nitrogen pipeline 33, and preheating the vinylene carbonate liquid in the first pipeline 32; during the use, twine nitrogen gas pipeline 33 on pipeline 32 for vaporization blowout moisture is preheated in advance in the shower nozzle 31, preheats the crude ethylene carbonate liquid of casing 1 bottom simultaneously, promotes the vaporization of the moisture in the crude ethylene carbonate liquid, further improves the evaporation rate of moisture in the crude ethylene carbonate liquid, thereby improves the purity of ethylene carbonate.
When the device is used, firstly, 120-plus 130 ℃ nitrogen is introduced into the net spray head 31 through the nitrogen pipeline 33, the nitrogen is sprayed out from the upper end of the spray head 31, then crude ethylene carbonate liquid is put into the feed inlet 111 on the end cover 11, the crude ethylene carbonate liquid flows out of the first cavity 22, then the nitrogen flows into the shell 1 through the through hole 21 on the first plate 2, the crude ethylene carbonate liquid is heated by the nitrogen in the process that the crude ethylene carbonate liquid flows into the bottom of the shell 1, the nitrogen is cleaned in the spray head 31 and sprayed upwards to form negative pressure in the spray head 31, then the negative pressure leads the crude ethylene carbonate liquid at the bottom of the shell 1 to be sprayed into the spray head 31 through the first pipeline 32, then the nitrogen impacts on the crude ethylene carbonate liquid, and the nitrogen and the crude ethylene carbonate liquid are discharged from the outlet of the spray head 31 together; under the marked atmospheric pressure, the boiling point of water is 100 ℃, the boiling point of the vinylene carbonate liquid is 160 ℃, the temperature of nitrogen is between 120 ℃ and 130 ℃, the nitrogen can vaporize the moisture of the crude vinylene carbonate liquid, the vaporized water floats upwards in the shell 1 and is attached to the plate surface of the plate 2, the vaporized water meets the plate 2 with lower temperature and is condensed into water drops, finally the water drops slide to the joint of the first rod 23 and the first plate 2 through the inclined plate 2, and finally the water drops flow out of the water pipe 12 through the first rod 23; the boiling points of water and the ethylene carbonate liquid are different, so that water in the crude ethylene carbonate liquid is evaporated and removed, and meanwhile, nitrogen is an inert gas, so that the ethylene carbonate liquid is protected, and the ethylene carbonate liquid is prevented from being oxidized by the outside air; the nitrogen is discharged into the spray head 31, then the nitrogen impacts on the rotating impeller 311, when the crude ethylene carbonate liquid flows into the spray head 31, the rotating impeller 311 rotates to stir the crude ethylene carbonate liquid, so that bubbles are generated in the crude ethylene carbonate liquid, after the crude ethylene carbonate liquid is sprayed out from the spray head 31 together with the nitrogen communicated with the bubbles, the atomized water beads of the crude ethylene carbonate liquid are refined again, and meanwhile, the moisture in the crude ethylene carbonate liquid is more beneficial to being vaporized; nitrogen impacts on the rotating impeller 311, the rotating impeller 311 rotates to drive the stirring impeller 312 to rotate through the rotating shaft, then the stirring impeller 312 stirs crude ethylene carbonate liquid at the bottom of the shell 1, bubbles are generated in the crude ethylene carbonate liquid, then the crude ethylene carbonate liquid and the bubbles enter the spray head 31 through the first pipeline 32, the crude ethylene carbonate liquid accompanied by the bubbles is more beneficial to being vaporized after being atomized by the nitrogen, the evaporation rate of moisture in the crude ethylene carbonate liquid is further improved, and the purity of the ethylene carbonate is improved; the vaporized water is adhered to the first plate 2, then the water drops become larger and larger, then the water drops roll on the plate surface of the first plate 2 and are mutually condensed together, then the water drops slide down to the joint of the first rod 23 and the first plate 2 along the guide strip 24, and finally the water drops flow out of the water outlet pipe 12 along the first rod 23; the guide strip 24 guides the condensed water drops on the surface of the first plate 2 to roll, so that the water drops are prevented from directly falling back to the ethylene carbonate liquid in the shell 1 instead of flowing out of the shell 1 when rolling, and the purity of the ethylene carbonate liquid is improved; crude ethylene carbonate liquid is filled into the first cavity 22 from the feed port 111, the temperature of the filled crude ethylene carbonate liquid is 25-35 ℃, then the crude ethylene carbonate liquid flows into the liquid storage cavity 25, then the crude ethylene carbonate liquid flows into the bottom of the shell 1 from the through hole 21 of the first plate 2, the liquid storage cavity 25 is filled with the crude ethylene carbonate liquid with the temperature of 25-35 ℃, so that the temperature of the plate surface of the first plate 2 is also kept between 25-35 ℃, and when vaporized water is adhered to the plate surface of the first plate 2, the temperature difference between the plate surface temperature of the first plate 2 and the vaporized water is reduced, so that the vaporized water is more conducive to being condensed into water beads and adhered to the plate surface of the first plate 2; the temperature of the first plate 2 is reduced through the crude ethylene carbonate liquid, so that the phenomenon that the vaporized water loses the effect of condensing vaporized water after the temperature of the first plate 2 is continuously heated by the vaporized water is avoided; the nitrogen pipeline 33 is wound on the first pipeline 32, so that moisture sprayed out by vaporization in the spray head 31 is preheated in advance, and meanwhile, crude ethylene carbonate liquid at the bottom of the shell 1 is also preheated, thereby promoting vaporization of moisture in the crude ethylene carbonate liquid, further improving the evaporation rate of moisture in the crude ethylene carbonate liquid, and further improving the purity of ethylene carbonate.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A process method for preparing vinylene carbonate by using a microchannel reactor is characterized by comprising the following steps: the method comprises the following steps:
s1: uniformly mixing chloroethylene carbonate and an ester solvent to obtain a mixed solution, heating the mixed solution to 25-35 ℃ through a preheater, heating triethylamine to 25-35 ℃ through the preheater, synchronously filling the preheated mixed solution and the triethylamine into a microchannel of a microchannel reactor, heating to 40-50 ℃, and then carrying out mixed reaction for 50-300 s;
s2: after the reactant in the microchannel reactor in the S1 finishes reacting, taking out the reactant from the microchannel reactor, wherein the reactant obtained at this moment is crude ethylene carbonate which contains moisture, and atomizing and removing the moisture in the crude ethylene carbonate liquid by using a drying device to obtain fine ethylene carbonate;
s3: collecting refined ethylene carbonate liquid dried in the step S2, and filling the refined ethylene carbonate liquid and an organic solvent into a storage tank together, wherein the organic solvent can be one or more of diethyl carbonate, dimethyl carbonate, ethyl methyl carbonate and ethylene carbonate, and the storage tank is placed at room temperature and kept in a dark place;
wherein the drying device described in the above method S2 comprises a housing (1); the upper end of the shell (1) is provided with an end cover (11) connected through a bolt, the end cover (11) is symmetrically provided with a feed inlet (111), a first plate (2) used for condensing steam is arranged below the feed inlet (111), the first plate (2) is in a letter V shape, the middle of the first plate (2) is high, two sides of the first plate are low, a first cavity (22) defined by the upper plate surface of the first plate (2) and the end cover (11) is communicated with the feed inlet (111), a plurality of through holes (21) are formed in the positions, fixedly connected with the side wall of the shell (1), of the first plate (2), the through holes (21) are communicated with the first cavity (22), a first rod (23) is symmetrically arranged on the lower plate surface ring of the first plate (2), the end part of the first rod (23) extends out of a water outlet pipe (12) arranged on the outer ring of the shell (1), and a liquid vaporization unit (; the liquid vaporization unit (3) comprises a spray head (31), a first pipeline (32) and a nitrogen pipeline (33); the nitrogen pipeline (33) is positioned below the outer wall of the shell (1), and the nitrogen pipeline (33) extends into the shell (1) and is communicated with the inside of the spray head (31); the spray head (31) is in a circular truncated cone shape, a plurality of outlets for gas-liquid injection are formed in the upper end face of the spray head (31), nitrogen pipelines (33) located in the spray head (31) are symmetrically arranged upwards in an inclined mode, the lower end of the spray head (31) is communicated with a first pipeline (32), and the first pipeline (32) is fixedly connected inside the shell (1) through a second rod (321); a discharge pipe (13) is arranged at the bottom of the shell (1); the water in the ethylene carbonate is evaporated and removed through the cooperation of the first plate (2), the first rod (23) and the liquid vaporization unit (3).
2. The process of claim 1 for preparing ethylene carbonate using a microchannel reactor, wherein: a rotating impeller (311) is arranged in the spray head (31); the rotating shaft of the rotating impeller (311) is hinged at the upper end of the spray head (31); the nitrogen gas sprayed from the nitrogen gas pipe (33) impinges on the rotary impeller (311) to drive the rotary impeller (311) to rotate, thereby further promoting vaporization of the water content of the vinylene carbonate liquid.
3. The process of claim 2 for preparing ethylene carbonate using a microchannel reactor, wherein: the lower end of the rotating shaft of the rotating impeller (311) extends out of the lower end of the first pipeline (32) and is connected with a stirring impeller (312); the stirring impeller (312) is used for stirring the ethylene carbonate liquid in the shell (1), so that bubbles are stirred in the ethylene carbonate, and the vaporization of the moisture of the ethylene carbonate liquid is further promoted.
4. The process of claim 1 for preparing ethylene carbonate using a microchannel reactor, wherein: the lower end face of the first plate (2) is provided with a plurality of guide strips (24) for guiding water flow, and the guide strips (24) are radially arranged on the lower plate face of the first plate (2) from the connecting part of the first plate (2) and the first rod (23); the guide strip (24) guides the water condensed on the first plate (2) to flow out of the water outlet pipe (12) from the first rod (23), and the condensed water is prevented from dripping into the ethylene carbonate liquid in the shell (1) again.
5. The process of claim 4 for preparing ethylene carbonate with a microchannel reactor, wherein: a liquid storage cavity (25) is formed in the first plate (2), and the liquid storage cavity (25) is communicated with the first cavity (22) and the through hole (21) in the first plate (2); condensation of water vapour is further promoted by the provision of a reservoir (25) within the first panel (2).
6. The process of claim 1 for preparing ethylene carbonate using a microchannel reactor, wherein: the nitrogen pipeline (33) is wound on the outer ring of the first pipeline (32) and extends into the air injection channel; the ethylene carbonate liquid in the first pipeline (32) is preheated by winding the nitrogen pipeline (33) on the first pipeline (32).
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| CN201911349042.5A CN111004204A (en) | 2019-12-24 | 2019-12-24 | Process method for preparing vinylene carbonate by using microchannel reactor |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115850230A (en) * | 2022-10-25 | 2023-03-28 | 康宁反应器技术有限公司 | Method for preparing vinylene carbonate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115850230A (en) * | 2022-10-25 | 2023-03-28 | 康宁反应器技术有限公司 | Method for preparing vinylene carbonate |
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