CN113072530A - Device and method for producing electronic-grade ethylene carbonate - Google Patents
Device and method for producing electronic-grade ethylene carbonate Download PDFInfo
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- CN113072530A CN113072530A CN202110294426.2A CN202110294426A CN113072530A CN 113072530 A CN113072530 A CN 113072530A CN 202110294426 A CN202110294426 A CN 202110294426A CN 113072530 A CN113072530 A CN 113072530A
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- 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
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Abstract
The invention relates to a device and a method for producing electronic-grade ethylene carbonate, which solve the problems that reaction heat is not removed in time, the conversion rate of epoxy compounds is not high, the product purity can not meet the requirements of electronic-grade products and the like in the prior art. The synthesis process comprises the steps of carrying out homogeneous esterification reaction on ethylene oxide, carbon dioxide and an ionic liquid catalyst in a reactor, and feeding the crude ethylene carbonate subjected to flash evaporation into a refining unit to obtain electronic-grade ethylene carbonate. The production equipment comprises a catalyst buffer tank, a reactor, a flash tank, a flash vapor receiving tank, a crude ethylene carbonate refining tower, a catalyst recovery tower and an ethylene carbonate refining tower. The conversion rate of the ethylene oxide is not lower than 99.5%, the highest yield of the ethylene carbonate is 99.7%, and the electronic-grade ethylene carbonate with the purity not lower than 99.99% is obtained, so that the industrial problem is well solved, and the method can be used for the industrial production of the ethylene carbonate, and achieves the purposes of energy conservation and environmental protection.
Description
Technical Field
The invention relates to the technical field of ethylene carbonate production, in particular to a device and a method for producing electronic-grade ethylene carbonate.
Background
The ethylene carbonate is a raw material of a solvent and a surfactant with excellent performance, particularly has better dissolving effect on a plurality of polymers and resins, can be used as an organic synthesis intermediate, is used as a raw material for synthesizing furazolidone, is used as a water glass series sizing agent, a fiber finishing agent and other fiber processing agents, can be used as a spinning solution on textile, can be directly used as a solvent for removing acid gas and an additive of concrete, and can also be used as a plastic foaming agent and a stabilizer for synthesizing lubricating oil. Besides, the ethylene carbonate can also be used as a high-energy battery electrolyte with high added value. With the increasing demand of electrolyte, the dosage of high-purity ethylene carbonate is higher and higher.
In recent years, researchers in various countries have conducted many studies on the synthesis of carbonates, and many new synthesis methods and new catalysts have been discovered, and the main production methods of ethylene carbonate include phosgene method, transesterification method, halohydrin method, ethylene oxide and carbon dioxide synthesis method. The phosgene method has the defects of long process flow, low yield, high cost and the like, and the phosgene has high toxicity and serious pollution and is basically stopped being used in developed countries. The transesterification method is a method for producing ethylene carbonate by transesterification of diethyl carbonate (or dimethyl carbonate) and ethylene glycol. The product of the ethylene carbonate produced by the process is not easy to separate and purify, and the synthesis cost of the catalyst is high. The halohydrin method is a method for generating ethylene carbonate from halohydrin and carbon dioxide in an organic solvent under the catalysis of a catalyst. The raw materials and the catalyst needed by the process are high in price, the reaction raw material chloroethanol is harmful to the environment, the reaction conditions are harsh, the yield is low, and the actual production is not facilitated. The method for preparing the ethylene carbonate by directly esterifying the carbon dioxide and the ethylene oxide serving as raw materials is an efficient, green and environment-friendly method for synthesizing novel intermediate ester, provides a new way for chemically utilizing carbon dioxide resources, can obtain obvious economic benefits and social benefits, is generally regarded by all countries, and is suitable for large-scale industrial production.
In order to increase the mass transfer and heat transfer effects, CN201410214132.4 provides a production method for preparing propylene carbonate or ethylene carbonate by tubular reaction of carbon dioxide and propylene oxide or ethylene oxide, the tubular synthesis reactor has good mass transfer effect, full gas-liquid contact, timely heat exchange of reaction heat, large operation flexibility of the device, and stable operation in a wider output range.
CN201911393119.9 provides a method for preparing ethylene carbonate by a circulating jet mixing method. The method is carried out in a circulating jet mixing reactor by taking ethylene oxide and carbon dioxide as raw materials, wherein the catalyst is one or more of a bimetallic catalyst, a late transition metal catalyst, an alkaline earth metal catalyst, amino acid, phosphotungstic acid, silicotungstic acid, germanium tungstic acid and arsenic tungstic acid, the conversion rate of the ethylene oxide can reach more than 90 percent and even more than 99 percent, and the process has the advantages of uniform material mixing, high reaction speed and high process safety.
CN200910080322.0 relates to a method for preparing ethylene carbonate, the raw materials are gas mixture obtained by ethylene oxidation and ethylene carbonate solution, ethylene carbonate is generated under the action of catalyst, the catalyst is carbonate and alkyl imidazole salt, the conversion rate of ethylene oxide is 96-99%; the selectivity is 97-99%, the ethylene oxide in the mixed gas is directly oxidized by the ethylene as the raw material, the ethylene oxide does not need to be separated and rectified to obtain the product ethylene oxide, and the cost is saved.
CN201910976767.0 through ethylene oxide and carbon dioxide in a single-stage or multi-stage bubble column for esterification, through stripping, refining unit to obtain 99.9w% ethylene carbonate, the invention through the bubble column structure optimization, effectively improved the bubble distribution uniformity in the column, effectively reduced ethylene oxide dissolution degree, reduced side reaction, increased ethylene oxide and carbon dioxide utilization ratio.
At present, in the prior art, reaction heat is not removed in time, the conversion rate of epoxy compounds is not high, the product purity cannot meet the requirement of electronic grade products, the product purity needs to be further improved, and a device and a method for obtaining high-purity and high-conversion-rate ethylene carbonate are provided.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a device and a method for producing electronic-grade ethylene carbonate, so that high-purity ethylene carbonate is obtained, high conversion rate of raw materials is realized, and industrial-grade ethylene carbonate is obtained at the same time.
The invention provides a device for producing electronic-grade ethylene carbonate, which comprises a catalyst buffer tank, a reactor, a flash tank, a flash evaporation gas receiving tank, a crude ethylene carbonate refining tower, a catalyst recovery tower and an ethylene carbonate refining tower, wherein the catalyst buffer tank is connected with the reactor;
the top of the reactor is provided with a first reactor feeding hole, the bottom of the reactor is provided with a reactor discharging hole, the middle part of the reactor is provided with a second reactor feeding hole, and the inside of the reactor is provided with a cooling coil pipe;
the middle part of the flash tank is provided with a flash tank feeding hole which is connected with the reactor discharging hole, the top part of the flash tank is provided with a gas phase discharging hole, the upper part of the flash tank is provided with a liquid phase returning hole, and the bottom part of the flash tank is provided with a flash tank discharging hole;
the middle part of the flash evaporation gas receiving tank is provided with a flash evaporation gas receiving tank feeding port which is connected with the gas phase discharging port, the top part of the flash evaporation gas receiving tank is provided with a gas phase discharging port, and the bottom part of the flash evaporation gas receiving tank is provided with a flash evaporation gas receiving tank discharging port which is connected with the liquid phase returning port;
a crude ethylene carbonate feeding hole is formed in the lower part of the crude ethylene carbonate refining tower and is connected with a discharging hole of the flash tank, a first outlet of the crude ethylene carbonate refining tower is formed in the top of the crude ethylene carbonate refining tower, and a second outlet of the crude ethylene carbonate refining tower is formed in the bottom of the crude ethylene carbonate refining tower;
the lower part of the catalyst recovery tower is provided with a catalyst recovery tower feed inlet which is connected with a second outlet of the crude ethylene carbonate refining tower, the top of the catalyst recovery tower feed inlet is provided with a first outlet of the catalyst recovery tower, and the bottom of the catalyst recovery tower feed inlet is provided with a second outlet of the catalyst recovery tower which is connected with the catalyst buffer tank;
the lower part of the ethylene carbonate refining tower is provided with an ethylene carbonate refining tower feed inlet which is connected with the first outlet of the catalyst recovery tower, the top of the ethylene carbonate refining tower is provided with a first outlet of the ethylene carbonate refining tower, and the bottom of the ethylene carbonate refining tower is provided with a second outlet of the ethylene carbonate refining tower.
The invention also provides a method for producing the ethylene carbonate by the device, which comprises the following steps:
s1, feeding the ethylene oxide into a reactor through a first feed inlet of the reactor, feeding the catalyst into the reactor through a catalyst buffer tank and the first feed inlet of the reactor in sequence, feeding the carbon dioxide into the reactor through a second feed inlet of the reactor, and carrying out a homogeneous esterification reaction on the ethylene oxide and the carbon dioxide in the reactor to obtain a product, wherein the product comprises crude ethylene carbonate, ethylene glycol and diethylene glycol, and simultaneously generates a large amount of heat, and the heat is transferred through a cooling coil pipe, and the product is fed into a flash tank from a discharge outlet of the reactor;
s2, separating unreacted carbon dioxide and crude ethylene carbonate in the flash tank, enabling a gas phase after flash evaporation to enter a flash evaporation gas receiving tank through a gas phase discharge port, emptying non-condensable gas through a gas phase emptying port, returning liquid into the flash tank through a flash evaporation gas receiving tank discharge port and a liquid phase return port in sequence, and enabling a product after flash evaporation to enter a refining unit through a flash evaporation tank discharge port;
s3, dividing a material at a first outlet of the crude ethylene carbonate refining tower into two streams, returning one stream as a circulating stream to the flash tank, introducing the other stream to a first outlet of the ethylene carbonate refining tower, introducing a material extracted at a second outlet of the crude ethylene carbonate refining tower into a catalyst recovery tower, separating an ionic liquid catalyst in the catalyst recovery tower, introducing the material extracted at the first outlet of the catalyst recovery tower into the ethylene carbonate refining tower, introducing a material rich in the catalyst extracted at the second outlet of the catalyst recovery tower into the catalyst buffer tank for recycling, mixing the material extracted at the first outlet of the ethylene carbonate refining tower with the material extracted at the first outlet of the crude ethylene carbonate refining tower to obtain an industrial-grade ethylene carbonate product, and extracting electronic-grade ethylene carbonate at the second outlet of the ethylene carbonate refining tower.
Preferably, in S1, the temperature of the reactor is 130-180 ℃ and the pressure is 3.5-5.5 MPa (a).
Preferably, in S2, the temperature of the flash tank is 110-140 ℃, and the pressure is 0.1-0.35MPa (a).
Preferably, in S2, the temperature of the flash evaporation gas receiving tank is 50-80 ℃, and the pressure is 0.1-0.35MPa (a).
Preferably, in S3, the temperature of the crude ethylene carbonate refining tower is 130-180 ℃, the pressure is-0.1-0.35 MPa (a), the reflux ratio is 5-15, and the number of plates is 30-60.
Preferably, in S3, the temperature of the catalyst recovery column is 140 ℃ and 200 ℃, the pressure is-0.1 to 0.35MPa (a), the reflux ratio is 8 to 20, and the number of trays is 20 to 50.
Preferably, in S3, the temperature of the ethylene carbonate refining tower is 140-180 ℃, the pressure is-0.1-0.35 MPa (a), the reflux ratio is 6-12, and the number of plates is 15-40.
Preferably, the catalyst is an ionic liquid; the ionic liquid is at least one of tetraethylammonium bromide, methyl triphenyl phosphonium iodide, methyl triphenyl phosphonium bromide and 1-ethyl-3-methylimidazole bromine salt.
Preferably, the mass ratio of carbon dioxide to ethylene oxide feed is from 1.05 to 2: 1; the mass of the outlet material of the catalyst buffer tank is 0.01-0.05% of the feeding amount of the ethylene oxide, and the feeding amount of the fresh catalyst is 1-5% of the mass of the outlet material of the catalyst buffer tank; the recovery amount of the circulating flow is 65-85% of the recovery amount of the first outlet of the crude ethylene carbonate refining tower.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, ethylene oxide, carbon dioxide and an ionic liquid catalyst are subjected to homogeneous reaction in a reactor, and the electronic-grade ethylene carbonate is obtained through flash evaporation and refining processes.
2. The conversion rate of the ethylene oxide is not less than 99.5 percent, the highest yield of the ethylene carbonate is 99.7 percent, the purity of the industrial-grade ethylene carbonate product is not less than 99.5 percent, the purity of the electronic-grade ethylene carbonate product is not less than 99.99 percent (the total content of the ethylene glycol and the diethylene glycol is less than or equal to 50ppm, and the water content is less than or equal to 40 ppm), the product purity meets the index requirement of the electrolytic cell solvent, the industrial-grade ethylene carbonate is obtained, the yield can be adjusted according to the requirement, the product yield is high, and good technical effects are obtained.
Drawings
Fig. 1 is a schematic structural view of embodiment 1 of the present invention.
Wherein, the system comprises a V1-catalyst buffer tank, an R1-reactor, a V2-flash tank, a V3-flash gas receiving tank, a T1-crude ethylene carbonate refining tower, a T2-catalyst recovery tower and a T3-ethylene carbonate refining tower.
1-a first reactor feeding port, 2-a second reactor feeding port, 3-a reactor discharging port, 4-a flash tank feeding port, 5-a gas phase discharging port, 6-a gas phase emptying port, 7-a liquid phase returning port, 8-a flash tank discharging port, 9-a crude ethylene carbonate feeding port, 10-a first crude ethylene carbonate refining tower outlet, 11-a second crude ethylene carbonate refining tower outlet, 12-a catalyst recovery tower feeding port, 13-a first catalyst recovery tower outlet, 14-a second catalyst recovery tower outlet, 15-an ethylene carbonate refining tower feeding port, 16-an ethylene carbonate refining tower outlet, 17-an ethylene carbonate refining tower outlet, 18-a distributor and 19-a cooling coil.
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 explained below by combining the specific drawings.
Example 1
An apparatus for producing electronic-grade ethylene carbonate, referring to fig. 1, comprises a catalyst buffer tank V1, a reactor R1, a flash tank V2, a flash gas receiving tank V3, a crude ethylene carbonate refining tower T1, a catalyst recovery tower T2 and an ethylene carbonate refining tower T3;
the top of the reactor R1 is provided with a first reactor feed inlet 1, the bottom is provided with a reactor discharge outlet 3, the middle part is provided with a second reactor feed inlet 2, carbon dioxide enters the reactor R1 from the second reactor feed inlet 2 and is uniformly distributed on the distributor 18, and two sections of cooling coils 19 are arranged inside the reactor R1.
The middle part of flash tank V2 is equipped with flash tank feed inlet 4, links to each other with reactor discharge gate 3, and the top is equipped with gaseous phase discharge gate 5, and upper portion is equipped with liquid phase and returns mouth 7, and the bottom is equipped with flash tank discharge gate 8.
The middle part of the flash evaporation gas receiving tank V3 is provided with a flash evaporation gas receiving tank feed inlet which is connected with a gas phase discharge port 5, the top part is provided with a gas phase vent 6, and the bottom part is provided with a flash evaporation gas receiving tank discharge port which is connected with a liquid phase return port 7.
The lower part of the crude ethylene carbonate refining tower T1 is provided with a crude ethylene carbonate feed inlet 9 which is connected with a discharge outlet 8 of the flash tank, the top part is provided with a first outlet 10 of the crude ethylene carbonate refining tower, and the bottom part is provided with a second outlet 11 of the crude ethylene carbonate refining tower.
The lower part of the catalyst recovery tower T2 is provided with a catalyst recovery tower feed inlet 12 which is connected with a second outlet 11 of the crude ethylene carbonate refining tower, the top is provided with a first outlet 13 of the catalyst recovery tower, the bottom is provided with a second outlet 14 of the catalyst recovery tower, and the second outlet is connected with a catalyst buffer tank V1.
The lower part of the ethylene carbonate refining tower T3 is provided with an ethylene carbonate refining tower feed inlet 15 which is connected with a first outlet 13 of the catalyst recovery tower, the top part is provided with a first outlet 16 of the ethylene carbonate refining tower, and the bottom part is provided with a second outlet 17 of the ethylene carbonate refining tower.
In the implementation of the embodiment, ethylene oxide and an ionic liquid catalyst enter a reactor R1 through a first feed inlet 1 of the reactor, carbon dioxide enters a reactor R1 through a second feed inlet 2 of the reactor, the ethylene oxide and the carbon dioxide undergo a homogeneous esterification reaction in the reactor R1 to generate ethylene carbonate, ethylene glycol, diethylene glycol and the like, a large amount of heat is generated at the same time, heat is removed through a cooling coil 19, and the reacted materials enter a flash tank V2 from a discharge outlet 3 of the reactor;
separating unreacted carbon dioxide and ethylene carbonate in a flash tank V2, feeding the gas phase after flash evaporation into a flash evaporation gas receiving tank V3 through a gas phase discharge port 5, emptying the non-condensable gas through a gas phase emptying port 6, returning the liquid into the flash tank V2 through a flash evaporation gas receiving tank discharge port, and feeding the crude ethylene carbonate material after flash evaporation into a refining unit through a flash tank discharge port 8;
the material extracted from the first outlet 10 of the crude ethylene carbonate refining tower is divided into two streams, one stream is returned to a flash tank V2 as a circulating stream, the other stream is led to a first outlet 16 of the ethylene carbonate refining tower, the material extracted from the second outlet 11 of the crude ethylene carbonate refining tower enters a catalyst recovery tower T2, the separation of the ionic liquid catalyst is realized in a catalyst recovery tower T2, the material extracted from the first outlet 13 of the catalyst recovery tower enters an ethylene carbonate refining tower T3, the material rich in the catalyst is extracted from the second outlet 14 of the catalyst recovery tower and enters a catalyst buffer tank V1 for recycling, the material extracted from the first outlet 16 of the ethylene carbonate refining tower is mixed with the material extracted from the first outlet 10 of the crude ethylene carbonate refining tower to be used as an industrial-grade ethylene carbonate product, and the second outlet 17 of the ethylene carbonate refining tower extracts electronic-grade ethylene carbonate.
Example 2
Electronic grade ethylene carbonate was produced using the apparatus obtained in example 1:
the feeding amount of ethylene oxide is 839Kg/h, the feeding amount of carbon dioxide is 883Kg/h, the ionic liquid catalyst is methyl triphenyl phosphonium iodide, the mass flow of fresh catalyst is 0.0125Kg/h, the temperature of reactor R1 is 160 ℃, the pressure is 5MPa (a), the material after homogeneous esterification reaction in reactor R1 enters a flash tank V2, the temperature of flash tank V2 is 130 ℃, the pressure is 0.1MPa (a), the mass flow of crude ethylene carbonate extracted from the flash tank V2 is 2118Kg/h, the material enters a crude ethylene carbonate refining tower T1, the temperature of crude ethylene carbonate refining tower T1 is 150 ℃, the pressure is-0.1 MPa (a), the number of plates is 50, the reflux ratio is 7.5, the crude ethylene carbonate feeding position is at a 35 th plate, the mass flow of the material at a first outlet 10 of the crude ethylene carbonate refining tower is 224Kg/h, the material is divided into two streams, one stream is a circulating flash tank returning V2, one of the streams is led to a first outlet 16 of a ethylene carbonate refining tower, wherein the mass flow of a circulating stream is 44.8Kg/h, the mass flow of a material extracted from a second outlet 11 of a crude ethylene carbonate refining tower is 1894Kg/h, the stream enters a catalyst recovery tower T2, the temperature of a catalyst recovery tower T2 is 150 ℃, the pressure is-0.1 MPa (a), the number of trays is 40, the reflux ratio is 15, the feeding position is at a 27 th plate, the mass flow of a material extracted from a first outlet 13 of the catalyst recovery tower is 1630Kg/h, the stream enters a ethylene carbonate refining tower T3, the mass flow of a material rich in catalyst extracted from a second outlet 14 of the catalyst recovery tower is 264Kg/h, the material is returned to a catalyst buffer tank V1 for recycling, the temperature of the ethylene carbonate refining tower T3 is 150 ℃, the pressure is-0.1 MPa (a), the number of trays is 40, the reflux ratio is 10, the feeding position is at a, the mass flow of the material extracted from the first outlet 16 of the ethylene carbonate refining tower is 380Kg/h, and the material is mixed with one stream of the first outlet 10 of the crude ethylene carbonate refining tower to obtain the industrial-grade ethylene carbonate with the mass fraction of 99.81%, the mass flow is 424Kg/h, and the electronic-grade ethylene carbonate with the mass fraction of 99.996% is extracted from the second outlet 17 of the ethylene carbonate refining tower, and the mass flow is 1250 Kg/h.
In summary, in the method for producing ethylene carbonate, the conversion rate of ethylene oxide is 99.65%, the yield of ethylene carbonate is 99.6%, the purity of industrial-grade ethylene carbonate is 99.81%, and the purity of electronic-grade ethylene carbonate is 99.996% (the total content of ethylene glycol and diethylene glycol is 20ppm, and the water content is 10 ppm).
Example 3
Electronic grade ethylene carbonate was produced using the apparatus obtained in example 1:
the feeding amount of ethylene oxide is 839Kg/h, the feeding amount of carbon dioxide is 1191Kg/h, the ionic liquid catalyst is methyl triphenyl phosphonium iodide, the mass flow of fresh catalyst is 0.0125Kg/h, the temperature of reactor R1 is 150 ℃, the pressure is 5MPa (a), the material after homogeneous esterification reaction in reactor R1 enters a flash tank V2, the temperature of flash tank V2 is 130 ℃, the pressure is 0.1MPa (a), the mass flow of crude ethylene carbonate extracted from the flash tank V2 is 2120Kg/h, the material enters a crude ethylene carbonate refining tower T1, the temperature of crude ethylene carbonate refining tower T1 is 150 ℃, the pressure is-0.1 MPa (a), the number of plates is 45, the reflux ratio is 8, the feeding position of crude ethylene carbonate is at the 32 th plate, the mass flow of the material at the first outlet 10 of the crude ethylene carbonate refining tower is 224Kg/h, the material is divided into two streams, one stream is a circulating return stream to the flash tank V2, one of the two streams is led to a first outlet 16 of a ethylene carbonate refining tower, wherein the mass flow of a circulating stream is 44.8Kg/h, the mass flow of a material extracted from a second outlet 11 of a crude ethylene carbonate refining tower is 1896Kg/h, the circulating stream enters a catalyst recovery tower T2, the temperature of the catalyst recovery tower T2 is 150 ℃, the pressure is-0.1 MPa (a), the number of trays is 40, the reflux ratio is 12, the feeding position is at a 20 th tray, the mass flow of a material extracted from a first outlet 13 of the catalyst recovery tower is 1630Kg/h, the catalyst recovery tower T3 is fed, the mass flow of a material rich in catalyst is extracted from a second outlet 14 of the catalyst recovery tower and is 266Kg/h, the material is returned to a catalyst buffer tank V1 for recycling, the temperature of the ethylene carbonate refining tower T3 is 150 ℃, the pressure is-0.1 MPa (a), the number of trays is 35, the reflux ratio is 8.5, the feeding position is, the mass flow of the material extracted from the first outlet 16 of the ethylene carbonate refining tower is 380Kg/h, and the material is mixed with one stream of the first outlet 10 of the crude ethylene carbonate refining tower to obtain the industrial-grade ethylene carbonate with the mass fraction of 99.88%, the mass flow is 424Kg/h, and the electronic-grade ethylene carbonate with the mass fraction of 99.998% is extracted from the second outlet 17 of the ethylene carbonate refining tower, and the mass flow is 1250 Kg/h.
As described above, in the process for producing ethylene carbonate, the ethylene oxide conversion is 99.7%, the ethylene carbonate yield is 99.7%, the purity of industrial-grade ethylene carbonate is 99.88%, and the purity of electronic-grade ethylene carbonate is 99.998% (the total content of ethylene glycol and diethylene glycol is 10ppm, and the water content is 5 ppm).
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent structures made by using the contents of the present specification and the drawings can be directly or indirectly applied to other related technical fields, and are within the scope of the present invention.
Claims (10)
1. The device for producing electronic-grade ethylene carbonate is characterized by comprising a catalyst buffer tank, a reactor, a flash tank, a flash evaporation gas receiving tank, a crude ethylene carbonate refining tower, a catalyst recovery tower and an ethylene carbonate refining tower;
the top of the reactor is provided with a first reactor feeding hole, the bottom of the reactor is provided with a reactor discharging hole, the middle part of the reactor is provided with a second reactor feeding hole, and the inside of the reactor is provided with a cooling coil pipe;
the middle part of the flash tank is provided with a flash tank feeding hole which is connected with the reactor discharging hole, the top part of the flash tank is provided with a gas phase discharging hole, the upper part of the flash tank is provided with a liquid phase returning hole, and the bottom part of the flash tank is provided with a flash tank discharging hole;
the middle part of the flash evaporation gas receiving tank is provided with a flash evaporation gas receiving tank feeding port which is connected with the gas phase discharging port, the top part of the flash evaporation gas receiving tank is provided with a gas phase discharging port, and the bottom part of the flash evaporation gas receiving tank is provided with a flash evaporation gas receiving tank discharging port which is connected with the liquid phase returning port;
a crude ethylene carbonate feeding hole is formed in the lower part of the crude ethylene carbonate refining tower and is connected with a discharging hole of the flash tank, a first outlet of the crude ethylene carbonate refining tower is formed in the top of the crude ethylene carbonate refining tower, and a second outlet of the crude ethylene carbonate refining tower is formed in the bottom of the crude ethylene carbonate refining tower;
the lower part of the catalyst recovery tower is provided with a catalyst recovery tower feed inlet which is connected with a second outlet of the crude ethylene carbonate refining tower, the top of the catalyst recovery tower feed inlet is provided with a first outlet of the catalyst recovery tower, and the bottom of the catalyst recovery tower feed inlet is provided with a second outlet of the catalyst recovery tower which is connected with the catalyst buffer tank;
the lower part of the ethylene carbonate refining tower is provided with an ethylene carbonate refining tower feed inlet which is connected with the first outlet of the catalyst recovery tower, the top of the ethylene carbonate refining tower is provided with a first outlet of the ethylene carbonate refining tower, and the bottom of the ethylene carbonate refining tower is provided with a second outlet of the ethylene carbonate refining tower.
2. A method for producing ethylene carbonate according to claim 1, comprising the steps of:
s1, feeding the ethylene oxide into a reactor through a first feed inlet of the reactor, feeding the catalyst into the reactor through a catalyst buffer tank and the first feed inlet of the reactor in sequence, feeding the carbon dioxide into the reactor through a second feed inlet of the reactor, and carrying out a homogeneous esterification reaction on the ethylene oxide and the carbon dioxide in the reactor to obtain a product, wherein the product comprises crude ethylene carbonate, ethylene glycol and diethylene glycol, and simultaneously generates a large amount of heat, and the heat is transferred through a cooling coil pipe, and the product is fed into a flash tank from a discharge outlet of the reactor;
s2, separating unreacted carbon dioxide and crude ethylene carbonate in the flash tank, enabling a gas phase after flash evaporation to enter a flash evaporation gas receiving tank through a gas phase discharge port, emptying non-condensable gas through a gas phase emptying port, returning liquid into the flash tank through a flash evaporation gas receiving tank discharge port and a liquid phase return port in sequence, and enabling a product after flash evaporation to enter a refining unit through a flash evaporation tank discharge port;
s3, dividing a material at a first outlet of the crude ethylene carbonate refining tower into two streams, returning one stream as a circulating stream to the flash tank, introducing the other stream to a first outlet of the ethylene carbonate refining tower, introducing a material extracted at a second outlet of the crude ethylene carbonate refining tower into a catalyst recovery tower, separating an ionic liquid catalyst in the catalyst recovery tower, introducing the material extracted at the first outlet of the catalyst recovery tower into the ethylene carbonate refining tower, introducing a material rich in the catalyst extracted at the second outlet of the catalyst recovery tower into the catalyst buffer tank for recycling, mixing the material extracted at the first outlet of the ethylene carbonate refining tower with the material extracted at the first outlet of the crude ethylene carbonate refining tower to obtain an industrial-grade ethylene carbonate product, and extracting electronic-grade ethylene carbonate at the second outlet of the ethylene carbonate refining tower.
3. The method as claimed in claim 2, wherein in S1, the temperature of the reactor is 130-180 ℃ and the pressure is 3.5-5.5 MPa (a).
4. The method as claimed in claim 2, wherein in S2, the flash tank has a temperature of 110 ℃ and 140 ℃ and a pressure of 0.1-0.35MPa (a).
5. The method of claim 2, wherein in S2, the flash gas receiving tank has a temperature of 50-80 ℃ and a pressure of 0.1-0.35mpa (a).
6. The method as claimed in claim 2, wherein in S3, the temperature of the crude ethylene carbonate refining column is 130-180 ℃, the pressure is-0.1-0.35 MPa (a), the reflux ratio is 5-15, and the number of plates is 30-60.
7. The method as claimed in claim 2, wherein in S3, the temperature of the catalyst recovery column is 140 ℃ and 200 ℃, the pressure is-0.1 to 0.35MPa (a), the reflux ratio is 8 to 20, and the number of trays is 20 to 50.
8. The method as claimed in claim 2, wherein in S3, the temperature of the ethylene carbonate refining column is 140 ℃ and 180 ℃, the pressure is-0.1 to 0.35MPa (a), the reflux ratio is 6 to 12, and the number of plates is 15 to 40.
9. The method of claim 2, wherein the catalyst is an ionic liquid; the ionic liquid is at least one of tetraethylammonium bromide, methyl triphenyl phosphonium iodide, methyl triphenyl phosphonium bromide and 1-ethyl-3-methylimidazole bromine salt.
10. The method of claim 2, wherein the carbon dioxide to ethylene oxide feed mass ratio is from 1.05 to 2: 1; the mass of the outlet material of the catalyst buffer tank is 0.01-0.05% of the feeding amount of the ethylene oxide, and the feeding amount of the fresh catalyst is 1-5% of the mass of the outlet material of the catalyst buffer tank; the recovery amount of the circulating flow is 65-85% of the recovery amount of the first outlet of the crude ethylene carbonate refining tower.
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| CN202110294426.2A CN113072530B (en) | 2021-03-19 | 2021-03-19 | Device and method for producing electronic-grade ethylene carbonate |
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| CN113072530A true CN113072530A (en) | 2021-07-06 |
| CN113072530B CN113072530B (en) | 2021-12-21 |
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