CN217410719U - Production device for synthesizing methyl ethyl carbonate by using ethanol and dimethyl carbonate as raw material gas phase and catalytic gas phase reactor - Google Patents
Production device for synthesizing methyl ethyl carbonate by using ethanol and dimethyl carbonate as raw material gas phase and catalytic gas phase reactor Download PDFInfo
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- CN217410719U CN217410719U CN202220017824.XU CN202220017824U CN217410719U CN 217410719 U CN217410719 U CN 217410719U CN 202220017824 U CN202220017824 U CN 202220017824U CN 217410719 U CN217410719 U CN 217410719U
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Abstract
The utility model discloses a production facility and catalytic gas phase reactor of methyl ethyl carbonate is synthesized to feed gas looks with ethanol and dimethyl carbonate, this production facility includes: the vaporizer is used for vaporizing the liquid raw materials of ethanol and dimethyl carbonate; the catalytic gas phase reactor is used for carrying out catalytic gas phase reaction on the ethanol and the dimethyl carbonate; the rough separation tower is used for separating the gas-phase reaction products and extracting a crude product of the methyl ethyl carbonate from the bottom of the tower; and the ethyl methyl carbonate tower is used for purifying the crude ethyl methyl carbonate product and extracting the ethyl methyl carbonate from the top of the tower. The catalytic gas phase reactor comprises a plurality of sections of reaction chambers, wherein a supporting disk for placing a catalyst is respectively arranged in each section of reaction chamber; each section of reaction chamber is respectively provided with an outer jacket positioned on the wall body of the reaction chamber and a heating pipe penetrating through the interior of the reaction chamber. Compared with the prior art, the utility model discloses destruction to the catalyst is few, easily retrieves the regeneration after the inactivation, has that reverse reaction, side reaction are few, and the productivity is high, advantage that product purity is high.
Description
Technical Field
The utility model relates to a production field of methyl ethyl carbonate, concretely relates to with ethanol and methyl carbonate as feed gas phase synthesis methyl ethyl carbonate's apparatus for producing.
Background
The methyl ethyl carbonate is colorless transparent liquid, is insoluble in water, can be used for organic synthesis, and is an excellent solvent of the lithium ion battery electrolyte. Methyl ethyl carbonate can be synthesized by the ester exchange reaction of dimethyl carbonate and ethanol under the catalysis of an acidic or basic catalyst.
The prior production device for synthesizing methyl ethyl carbonate by using ethanol and dimethyl carbonate as raw materials mainly comprises the following two types:
1. the fixed bed process adopts liquid phase reaction in the reactor, and the catalyst is sodium methoxide or solid alkali salt. And (3) feeding the reaction liquid into a first tower to extract methanol, ethanol and dimethyl carbonate, feeding the residual ethyl methyl carbonate and diethyl carbonate at the bottom of the tower, feeding the tower bottom material into a second tower, and extracting ethyl methyl carbonate from the top of the second tower and the residual diethyl carbonate from the bottom of the second tower.
The disadvantages of the process are: 1) the catalyst is easy to break after being soaked in liquid for a long time, and the broken catalyst increases the separation cost; 2) the cost of environmental protection disposal after the catalyst is deactivated is larger; 3) the reaction device is operated intermittently, so that the production efficiency is low; 4) because the reaction is reversible and side reactions occur, the yield of the product is reduced when the raw materials and the reactants stay in the reaction device for a long time, the amount of byproducts is increased, and the production cost is relatively high; 5) the extract at the top of the first tower is a mixture, so that the utilization field is narrow, and the utilization value is low; 6) the residual diethyl carbonate at the bottom of the second tower contains impurities, so that the utilization value is low.
2. The catalytic rectification reaction process adopts liquid phase reaction in the reaction device, and the catalyst is sodium methoxide or resin. The mixture of methanol, ethanol and dimethyl carbonate is extracted from the top of the rectification reaction device, and the extract is not subjected to the next separation and purification operation. And (3) feeding the reaction liquid at the bottom of the rectification reaction device into a first tower to extract the residual methanol, ethanol and dimethyl carbonate, feeding the residual ethyl methyl carbonate and diethyl carbonate at the bottom of the tower into a second tower, extracting ethyl methyl carbonate from the top of the second tower, and extracting the residual diethyl carbonate from the bottom of the second tower.
The disadvantages of this process are: 1) the catalyst is easy to break after being soaked in liquid for a long time, and the broken catalyst increases the separation cost; 2) the cost of environmental protection disposal after the catalyst is deactivated is larger; 3) in order to protect the catalyst, the temperature of the reaction device is not more than 120 ℃, so the reaction rate is slow, the probability of reverse reaction or side reaction is high, and the purification cost of the product is high. 4) Methanol, ethanol and dimethyl carbonate still remain at the bottom of the reaction device; 5) the extract at the top of the first tower is a mixture, so that the utilization field is narrow, and the utilization value is low; 6) the residual diethyl carbonate at the bottom of the second tower contains impurities, so the utilization value is low.
SUMMERY OF THE UTILITY MODEL
The catalyst is easy broken in the technology to above-mentioned fixed bed or catalytic rectification reaction production methyl ethyl carbonate, and the deactivation aftertreatment is with high costs not enough, the utility model aims to provide an use ethanol and methyl carbonate as feed gas phase synthesis methyl ethyl carbonate's apparatus for producing.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
the production device for synthesizing methyl ethyl carbonate by using ethanol and dimethyl carbonate as raw material gas phases comprises:
the vaporizer is used for vaporizing the liquid raw materials of ethanol and dimethyl carbonate;
the catalytic gas phase reactor is used for carrying out catalytic gas phase reaction on the ethanol and the dimethyl carbonate;
the rough separation tower is used for separating the gas-phase reaction products and extracting a crude product of the methyl ethyl carbonate from the bottom of the tower;
and the ethyl methyl carbonate tower is used for purifying the crude ethyl methyl carbonate product and extracting the ethyl methyl carbonate from the top of the tower.
Preferably, the production apparatus further comprises a mixer for mixing the ethanol and the dimethyl carbonate liquid feedstock.
Preferably, the rough separation tower is a packed tower, and the tower top is provided with a condenser 401 and a vacuum pump.
Preferably, the ethyl methyl carbonate tower is a packed tower, a vacuum pump is arranged at the top of the tower, and a reboiler is arranged at the bottom of the tower.
Preferably, the production apparatus further comprises:
the methanol tower is used for separating the materials extracted from the top of the rough separation tower, extracting methanol and dimethyl carbonate from the top of the methanol tower and extracting ethanol from the bottom of the methanol tower;
and the diethyl carbonate tower is used for purifying the material extracted from the bottom of the ethyl methyl carbonate tower and extracting diethyl carbonate from the top of the diethyl carbonate tower.
Preferably, the methanol tower is a packed tower, and the bottom of the tower is provided with a reboiler.
Preferably, the diethyl carbonate column is a packed column, the top of which is provided with a vacuum pump and the bottom of which is provided with a reboiler.
A catalytic gas phase reactor for use in the above production plant, said catalytic gas phase reactor comprising a plurality of reaction chambers, wherein,
a supporting disk for placing a catalyst is respectively arranged in each section of reaction chamber;
each section of reaction chamber is respectively provided with an outer jacket positioned on the wall body of the reaction chamber and a heating pipe penetrating through the interior of the reaction chamber.
Preferably, the body portion of the heating tube is substantially coaxial with the central axis of the reaction chamber.
Preferably, the outer jacket and the heating pipe are heated by steam at 180 ℃, and each section of reaction chamber is provided with an independent temperature control interlocking system.
Preferably, the reaction chamber is vertically fixed on the skirt, the feed inlet is arranged at the bottom of the reaction chamber, and the discharge outlet is arranged at the top of the reaction chamber.
Preferably, the reaction chamber has three segments in total.
The method for synthesizing methyl ethyl carbonate by using ethanol and dimethyl carbonate as raw material gases comprises the following steps:
(1) vaporizing the liquid raw materials of ethanol and dimethyl carbonate by a vaporizer;
(2) sending the vaporized ethanol and the dimethyl carbonate into a catalytic gas phase reactor to perform catalytic gas phase reaction;
(3) feeding the gas-phase reaction product into a rough separation tower for separation, and extracting a crude product of methyl ethyl carbonate from the bottom of the tower;
(4) and (3) feeding the crude product of the methyl ethyl carbonate into a methyl ethyl carbonate tower for purification, and extracting the methyl ethyl carbonate from the tower top.
Preferably, the ethanol and dimethyl carbonate liquid raw materials are mixed and then sent into a vaporizer, the vaporization temperature is 180 ℃, and the molar ratio of the ethanol to the dimethyl carbonate liquid raw materials is 1.1-1.4: 1.
preferably, the temperature of the catalytic gas phase reaction is 160 ℃.
Preferably, the bottom temperature of the rough separation tower is 90 ℃, the top temperature of the rough separation tower is 70 ℃, and the operation is carried out under negative pressure;
preferably, the temperature of the bottom of the ethyl methyl carbonate tower is 110 ℃, the temperature of the top of the ethyl methyl carbonate tower is 90 ℃, and the operation is carried out under negative pressure.
Preferably, the method further comprises the steps of:
extracting a mixture of methanol, ethanol and dimethyl carbonate from the top of the coarse separation tower, sending the mixture into a methanol tower for separation, extracting the methanol and the dimethyl carbonate from the top of the methanol tower, and extracting the ethanol from the bottom of the methanol tower;
extracting a crude product of diethyl carbonate from the bottom of a methyl ethyl carbonate tower, feeding the crude product of diethyl carbonate into a diethyl carbonate tower for purification, and extracting diethyl carbonate from the top of the diethyl carbonate tower.
Preferably, the temperature of the bottom of the methanol tower is 70 ℃, the temperature of the top of the methanol tower is 65 ℃, and the operation is carried out under normal pressure.
Preferably, the temperature of the bottom of the diethyl carbonate is 125 ℃, the temperature of the top of the diethyl carbonate is 100 ℃, and the operation is carried out under negative pressure.
Compared with the prior art, the technical scheme of the utility model have following advantage:
1) the problems of softening and crushing of the catalyst caused by liquid phase reaction are avoided, the loss is obviously reduced, the catalyst is easy to recover and regenerate after being inactivated, and the cost of environmental protection and disposal is greatly reduced;
2) the reaction temperature can be increased to the maximum extent, the effect maximization of the catalyst is ensured, and the reaction rate and the product yield can be improved;
3) the device can realize continuous production, improve the productivity and reduce the investment;
4) the gas phase reaction feeding and discharging are carried out simultaneously, the retention time of the raw materials is short, and the probability of reverse reaction and side reaction is greatly reduced;
5) the yield can be improved by 50 percent and the comprehensive cost of product purification can be reduced by 30 percent by adopting the technology of the utility model with the same investment scale project;
6) the quality of the ethyl methyl carbonate and the diethyl carbonate can reach the battery level (the purity is more than 99.99 percent), the purity of the ethanol can reach more than 99.99 percent, and the impurities brought by the reuse of the ethanol are obviously reduced.
Drawings
FIG. 1 is a schematic flow chart of an apparatus for synthesizing ethyl methyl carbonate by using ethanol and dimethyl carbonate as raw material gases.
FIG. 2 is a schematic diagram of a device for producing crude methyl ethyl carbonate by catalytic gas phase reaction.
FIG. 3 is a schematic diagram of a purification apparatus for crude methyl ethyl carbonate.
FIG. 4 is a schematic view of a separation apparatus for a mixture of methanol, ethanol and dimethyl carbonate.
FIG. 5 is a schematic diagram of a purification apparatus for crude diethyl carbonate.
FIG. 6 is a schematic diagram of the structure of a catalytic gas phase reactor.
Wherein, 1-static mixer, 101-ethanol raw material pump, 102-dimethyl carbonate raw material pump, 2-vaporizer, 3-catalytic gas phase reactor, 301-skirt, 302-feed inlet, (303, 1-303, 2-303) -jacket, 3031-steam inlet, 3032-condensate outlet, (304, 1-304, 2-304) -heating pipe, 3041-steam inlet, 3042-condensate outlet, 305-manhole, 306-safe discharge outlet, 307-discharge outlet, (308, 1-308, 2-308) -temperature measuring port, 309-discharge outlet, 310-manhole, 4-rough separation tower, 401-condenser, 402-primary condenser, 403-secondary condenser, 404-light component buffer tank, 405-rough separation tower vacuum pump, 406-light component reflux pump, 407-heavy component receiving tank, 408-reboiler, 409-circulating pump, 410-heavy component discharge pump, 411-light component receiving tank, 412-light component discharge pump, 5-ethyl methyl carbonate column, 501-primary condenser, 502-secondary condenser, 503-ethyl methyl carbonate buffer tank, 504-ethyl methyl carbonate column vacuum pump, 505-ethyl methyl carbonate reflux pump, 507-tower bottom reboiler, 508-tower bottom circulating pump, 509-tower bottom liquid receiving tank, 510-tower bottom liquid discharge pump, 511-ethyl methyl carbonate receiving tank, 512-ethyl methyl carbonate discharge pump, 6-methanol column, 601-primary condenser, 602-secondary condenser, 603-methanol buffer tank, 604-methanol reflux pump, 605-tower bottom reboiler, 606-tower bottom circulating pump, 607-ethanol receiving tank, 608-ethanol discharge pump, 609-methanol receiving tank, 610-methanol discharge pump, 7-diethyl carbonate column, 701-primary condenser, 702-secondary condenser, 703-diethyl carbonate buffer tank, 704-diethyl carbonate column vacuum pump, 705-diethyl carbonate reflux pump, 706-tower bottom reboiler, 707-tower bottom circulating pump, 708-diethyl carbonate receiving tank and 709-diethyl carbonate discharge pump.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the accompanying drawings and embodiments.
The utility model discloses a device flow schematic diagram that uses ethanol and dimethyl carbonate to synthesize methyl ethyl carbonate for the feed gas phase is shown as figure 1, and apparatus for producing includes:
the mixer is used for uniformly mixing the ethanol and the dimethyl carbonate liquid raw material;
a vaporizer which vaporizes a mixed liquid raw material of ethanol and dimethyl carbonate;
the catalytic gas phase reactor enables the vaporized mixture to enter from the bottom of the reactor and to generate ester exchange reaction under the action of a catalyst in the reactor;
the rough separation tower is used for carrying out preliminary separation on the gas-phase mixture at the top of the reactor in the rough separation tower;
a methyl ethyl carbonate tower, which is used for purifying the materials extracted from the bottom of the coarse separation tower and extracting a battery-grade methyl ethyl carbonate finished product from the top of the tower;
a diethyl carbonate tower for purifying the material extracted from the bottom of the ethyl methyl carbonate tower, extracting a finished diethyl carbonate product from the top of the tower, and intermittently discharging the sewage at the bottom of the tower according to the liquid level condition at the bottom of the tower;
and the methanol tower is used for separating the materials extracted from the top of the coarse separation tower, extracting a mixture of methanol and dimethyl carbonate from the top of the coarse separation tower and extracting an ethanol finished product from the bottom of the coarse separation tower.
Specifically, the schematic diagram of the device for producing crude methyl ethyl carbonate by catalytic gas phase reaction of the utility model is shown in fig. 2, and the molar ratio is 1.1-1.4: 1, keeping excessive ethanol to ensure that dimethyl carbonate reacts completely as much as possible, respectively conveying ethanol and dimethyl carbonate to a static mixer 1 (with a jacket, introducing hot water into the jacket to heat materials) through an ethanol material pump 101 and a dimethyl carbonate material pump 102, allowing the preheated and fully mixed materials to flow into a vaporizer 2 (heating by using steam of 0.6Mpa and 180 ℃) through a pipeline, heating the mixed materials in the vaporizer to vaporize the mixed materials, allowing the vaporized materials to continuously enter from the bottom of a gas phase reactor 3 (heating by using steam of 0.6Mpa and 180 ℃) through a pipeline, continuously discharging a gas phase mixture after reaction from the top of the reactor, directly allowing the gas phase mixture to enter a rough separation tower 4 (a multilayer packed tower, controlling the temperature of the top at 70 ℃ and the temperature of the bottom at 90 ℃) through a pipeline, performing primary separation of products in the tower, and performing primary separation on light components (methanol and dimethyl carbonate) at the top of the rough separation tower, Ethanol and dimethyl carbonate mixture) is condensed by a condenser 401, a first-stage condenser 402 and a second-stage condenser 403 and then enters a light component buffer tank 404, the upper part of the light component buffer tank is connected with a rough component tower vacuum pump 405 through a pipeline, so that the rough component tower is in micro negative pressure operation, the light component in the light component buffer tank is partially returned to the rough component tower through a light component reflux pump 406 through a pipeline, part of the light component is conveyed to a light component receiving tank 411, heavy components (a mixture of ethyl methyl carbonate and diethyl carbonate, namely a crude ethyl methyl carbonate product) at the bottom of the rough component tower are partially extracted to the heavy component receiving tank 407 through a tower bottom circulating pump 409, and part of the heavy components are heated by a tower bottom reboiler 408 and then returned to the rough component tower.
The device for purifying the crude methyl ethyl carbonate to obtain battery-grade methyl ethyl carbonate is shown in fig. 3, the crude methyl ethyl carbonate in the heavy component receiving tank is directly sent to a methyl ethyl carbonate tower 5 (a multilayer packed tower, the top of which is controlled at 90 ℃ and the bottom of which is controlled at 110 ℃) through a heavy component discharging pump 410 through a pipeline, the methyl ethyl carbonate is extracted from the top of the methyl ethyl carbonate tower, and enters a methyl ethyl carbonate buffer tank 503 after being condensed by a first-stage condenser 501 and a second-stage condenser 502, the upper part of the methyl ethyl carbonate buffer tank is connected with a methyl ethyl carbonate tower vacuum pump 504 through a pipeline, so that the methyl ethyl carbonate tower is in micro negative pressure operation, after the sample in the methyl ethyl carbonate buffer tank is qualified in assay and sampling (the purity is more than 99.99 percent), the sample is pumped into the methyl ethyl carbonate receiving tank through a methyl ethyl carbonate reflux pump 505 through a pipeline, and then is taken out through a methyl ethyl carbonate discharging pump 512, if the sample does not reach the standard, the sample flows back to the methyl ethyl carbonate reflux tower through the methyl ethyl carbonate reflux pump 505 through a pipeline, the liquid material at the bottom of the ethyl methyl carbonate tower (diethyl carbonate and impurities, namely crude diethyl carbonate) is partially taken out through a tower bottom circulating pump 508 via a pipeline and sent into a tower bottom liquid receiving tank 509, and part of the liquid material is heated by a tower bottom reboiler 507 and then returned to the ethyl methyl carbonate tower.
The schematic diagram of the apparatus for separating the mixture of light components of methanol, ethanol and dimethyl carbonate is shown in fig. 4, the light components in the light component receiving tank 411 are sent into a methanol tower 6 (multilayer packed tower, normal pressure operation, top temperature control 65 ℃, bottom temperature control 70 ℃) through a light component discharging pump 412, the extract at the top of the tower is condensed by a first-stage condenser 601 and a second-stage condenser 602 and then enters a methanol buffer tank 603, the extract in the methanol buffer tank is partially returned into the methanol tower through a methanol reflux pump 604 through a pipeline, and is partially sent to an azeotrope tank (methanol, dimethyl carbonate azeotrope) or a methanol receiving tank 609 according to the sampling analysis result, the methanol finished product in the methanol receiving tank is taken out through a methanol discharging pump 610, liquid ethanol is retained at the bottom of the methanol tower, and is sent into an ethanol receiving tank 607 through a pipeline through a tower bottom circulating pump 606 after the sampling analysis is qualified (purity is more than 99.99%), and then the liquid is taken out by an ethanol discharging pump 608, and the liquid reserved at the bottom of the tower, which is unqualified in analysis, is sent to a reboiler 605 at the bottom of the tower through a circulating pump 606 at the bottom of the tower through a pipeline and is returned to the methanol tower after being heated.
The schematic diagram of the purification apparatus of crude diethyl carbonate is shown in fig. 5, a crude diethyl carbonate container in a tower bottom liquid receiving tank 509 is sent into a diethyl carbonate tower 7 (multilayer packed tower, top temperature control 100 ℃ and bottom temperature control 125 ℃) through a pipe via a tower bottom liquid discharging pump 510, a tower top extract enters a diethyl carbonate buffer tank 703 after being condensed by a primary condenser 701 and a secondary condenser 702, the upper part of the diethyl carbonate buffer tank is connected with a diethyl carbonate tower vacuum pump 704 through a pipe, so that the diethyl carbonate tower is in micro-negative pressure operation, after sample sampling and assay of samples in the diethyl carbonate buffer tank are qualified (purity is more than 99.99%), the samples are pumped into a diethyl carbonate receiving tank 708 through a pipe via a diethyl carbonate reflux pump 705, and then the samples are taken out by a diethyl carbonate discharging pump 709, and if the samples do not reach the standard, the samples are sent back to the diethyl carbonate tower via the diethyl carbonate reflux pump, the wastewater at the bottom of the tower is sent to a reboiler 706 at the bottom of the tower through a circulating pump 707 at the bottom of the tower by a pipeline, heated and returned to the diethyl carbonate tower, and is discharged intermittently according to the liquid level condition at the bottom of the tower.
Fig. 6 is a schematic structural diagram of the catalytic gas phase reactor of the present invention, which includes three reaction chambers, wherein the three reaction chambers connected in series are vertically and fixedly mounted on the skirt 301, the feed inlet 302 is disposed at the bottom of the three reaction chambers, the discharge outlet 307 is disposed at the top of the three reaction chambers, the top of the three reaction chambers is further provided with a safety discharge outlet 306, and the bottom of the three reaction chambers is provided with a clean outlet 309. The reactor comprises a reaction chamber, a plurality of sections of reaction chambers and a plurality of temperature measuring ports, wherein a support plate for placing a catalyst is arranged in each section of reaction chamber, an outer jacket (303, 1-303, 2-303) for heating the section of reaction chamber is arranged on the wall body of each section of reaction chamber, a heating pipe (304, 1-304, 2-304) penetrating through the section of reaction chamber is arranged on the wall body of each section of reaction chamber, the main body part of the heating pipe is basically coaxial with the central axis of the corresponding section of reaction chamber, the flow of a heating medium is controlled by the outer jacket and the heating pipe through regulating valves arranged on pipelines, each section of reaction chamber is provided with a manhole 305 for people to enter and exit when the catalyst is placed or replaced, and the temperature measuring ports (308, 1-308, 2-308) for measuring the temperature in the reaction chamber, and each temperature measuring port is provided with a temperature sensor. Each temperature sensor is respectively and electrically connected with a controller, and the controller is electrically connected with each outer jacket and the regulating valve of the heating pipe. Each section of reaction chamber is provided with an independent temperature control interlocking system: the temperature of each section of reaction chamber is converted into an electric signal through a temperature sensor and is transmitted to a controller, and the controller sends control signals to the regulating valves of the outer jacket and the heating pipe of each section of reaction chamber according to preset temperature index values. Compared with the liquid phase reaction, the gas phase reaction has short material retention time in the reaction chamber, and has stricter and quicker control requirement on the reaction temperature. The outer jacket of each section of reaction chamber is heated by steam of 0.6Mpa and 180 ℃, the steam enters the outer jacket from a steam inlet 3031, and steam condensate water is discharged from a condensate water outlet 3032. The heating pipe in each section of reaction chamber is heated by steam of 0.6Mpa and 180 ℃, the steam enters the outer jacket from a steam inlet 3041, and steam condensate water is discharged from a condensate water outlet 3042.
The catalyst can adopt the solid basic catalyst used in the liquid phase catalysis transesterification of ethanol and dimethyl carbonate to synthesize methyl ethyl carbonate, such as the catalysts disclosed in CN107473968A, CN109503377A and CN 1900047A.
The catalyst is filled in the wire mesh filler, the wire mesh filler is arranged on the support plate in the reaction chamber, and the catalyst can enter the reaction chamber through the manhole for replacement after being inactivated.
The wire mesh packing is customized to the reaction chamber size.
The utility model discloses a method for synthesizing methyl ethyl carbonate by using ethanol and dimethyl carbonate as raw material gas phase, which comprises the following steps:
(1) the mol ratio of ethanol to dimethyl carbonate liquid raw materials is 1.1-1.4: 1, mixing;
(2) vaporizing the mixed liquid raw materials of ethanol and dimethyl carbonate, wherein the vaporization heating temperature is 180 ℃;
(3) then the vaporized mixture is sent into a catalytic gas phase reactor from the bottom, and gas phase ester exchange reaction is carried out under the catalysis of a solid basic catalyst, wherein the reaction temperature is 160 ℃;
(4) discharging reaction products from the top of the catalytic gas phase reactor, and feeding the reaction products into a coarse separation tower (a multilayer packed tower) for separation, wherein the temperature of the bottom of the tower is 90 ℃, the temperature of the top of the tower is 70 ℃, the micro-negative pressure operation is carried out, a methyl ethyl carbonate crude product is extracted from the bottom of the tower, and light components (a mixture of methanol, ethanol and dimethyl carbonate) are extracted from the top of the tower;
(5) then the extracted crude product of the ethyl methyl carbonate is sent into a ethyl methyl carbonate tower (a multilayer packed tower) for purification, the temperature at the bottom of the tower is 110 ℃, the temperature at the top of the tower is 90 ℃, the micro-negative pressure operation is carried out, the crude product of the diethyl carbonate is extracted at the bottom of the tower, and the battery-grade (the purity is more than 99.99 percent) ethyl methyl carbonate is extracted at the top of the tower;
(6) feeding the extracted diethyl carbonate crude product into a diethyl carbonate tower (a multilayer packed tower) for purification, wherein the temperature at the bottom of the tower is 125 ℃, the temperature at the top of the tower is 100 ℃, the micro negative pressure operation is carried out, battery-grade (with the purity of more than 99.99%) diethyl carbonate is extracted from the top of the tower, and sewage at the bottom of the tower is intermittently discharged according to the liquid level condition;
(7) and (2) sending the light components extracted from the top of the coarse fractionating tower into a methanol tower (a multilayer packed tower) for secondary separation, wherein the temperature at the bottom of the tower is 70 ℃, the temperature at the top of the tower is 65 ℃, the operation is carried out under normal pressure, methanol and dimethyl carbonate are extracted from the top of the tower, and battery-grade ethanol (with the purity of more than 99.99%) is extracted from the bottom of the tower.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described in the foregoing embodiments, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The production device for synthesizing the methyl ethyl carbonate by using the ethanol and the dimethyl carbonate as raw material gas phases is characterized by comprising the following steps of:
the vaporizer is used for vaporizing the liquid raw materials of ethanol and dimethyl carbonate;
the catalytic gas phase reactor is used for carrying out catalytic gas phase reaction on the ethanol and the dimethyl carbonate;
the rough separation tower is used for separating the gas-phase reaction products and extracting a crude product of the methyl ethyl carbonate from the bottom of the tower;
and the ethyl methyl carbonate tower is used for purifying the crude ethyl methyl carbonate and extracting the ethyl methyl carbonate from the top of the tower.
2. The production device according to claim 1, wherein: the production apparatus further comprises a mixer for mixing and preheating the ethanol and dimethyl carbonate liquid feedstock.
3. The production device according to claim 1, wherein:
the rough separation tower is a packed tower, and a condenser and a vacuum pump are arranged at the top of the tower;
the methyl ethyl carbonate tower is a packed tower, a vacuum pump is arranged at the top of the tower, and a reboiler is arranged at the bottom of the tower.
4. The production device according to claim 1, wherein: the production apparatus further includes:
the methanol tower is used for separating the materials extracted from the top of the rough separation tower, extracting methanol and dimethyl carbonate from the top of the methanol tower and extracting ethanol from the bottom of the methanol tower;
and the diethyl carbonate tower is used for purifying the material extracted from the bottom of the ethyl methyl carbonate tower and extracting diethyl carbonate from the top of the diethyl carbonate tower.
5. The production device according to claim 4, wherein:
the methanol tower is a packed tower, and a reboiler is arranged at the bottom of the tower;
the diethyl carbonate tower is a packed tower, a vacuum pump is arranged at the top of the tower, and a reboiler is arranged at the bottom of the tower.
6. A catalytic gas phase reactor for use in the production plant of claim 1, characterized by: the catalytic gas phase reactor comprises a plurality of reaction chambers, wherein,
a supporting disk for placing a catalyst is respectively arranged in each section of reaction chamber;
each section of reaction chamber is respectively provided with an outer jacket positioned on the wall body of the reaction chamber and a heating pipe penetrating through the interior of the reaction chamber.
7. The catalytic gas phase reactor according to claim 6, characterized in that: the reaction chamber is vertically fixed on the skirt, the feed inlet is arranged at the bottom of the reaction chamber, and the discharge outlet is arranged at the top of the reaction chamber.
8. The catalytic gas phase reactor according to claim 6, characterized in that: the main body portion of the heating tube is substantially coaxial with the central axis of the reaction chamber.
9. The catalytic gas phase reactor according to claim 6, characterized in that: the outer jacket and the heating pipe adopt 180 ℃ steam for heating, and each section of reaction chamber is provided with an independent temperature control interlocking system.
10. The catalytic gas phase reactor according to claim 6, characterized in that: the reaction chamber has three sections.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220017824.XU CN217410719U (en) | 2022-01-06 | 2022-01-06 | Production device for synthesizing methyl ethyl carbonate by using ethanol and dimethyl carbonate as raw material gas phase and catalytic gas phase reactor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220017824.XU CN217410719U (en) | 2022-01-06 | 2022-01-06 | Production device for synthesizing methyl ethyl carbonate by using ethanol and dimethyl carbonate as raw material gas phase and catalytic gas phase reactor |
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| CN217410719U true CN217410719U (en) | 2022-09-13 |
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| CN202220017824.XU Active CN217410719U (en) | 2022-01-06 | 2022-01-06 | Production device for synthesizing methyl ethyl carbonate by using ethanol and dimethyl carbonate as raw material gas phase and catalytic gas phase reactor |
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