CN114436840A - Method for industrially producing methyl ethyl carbonate by reacting diethyl carbonate and dimethyl carbonate - Google Patents
Method for industrially producing methyl ethyl carbonate by reacting diethyl carbonate and dimethyl carbonate Download PDFInfo
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- CN114436840A CN114436840A CN202210156538.6A CN202210156538A CN114436840A CN 114436840 A CN114436840 A CN 114436840A CN 202210156538 A CN202210156538 A CN 202210156538A CN 114436840 A CN114436840 A CN 114436840A
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- carbonate
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- ethyl methyl
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- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 title claims abstract description 113
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 title claims abstract description 81
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 69
- 239000000203 mixture Substances 0.000 claims abstract description 45
- 239000003054 catalyst Substances 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000012043 crude product Substances 0.000 claims description 31
- 239000000047 product Substances 0.000 claims description 21
- 238000007670 refining Methods 0.000 claims description 21
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/06—Preparation of esters of carbonic or haloformic acids from organic carbonates
- C07C68/065—Preparation of esters of carbonic or haloformic acids from organic carbonates from alkylene carbonates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for industrially producing methyl ethyl carbonate by reacting diethyl carbonate and dimethyl carbonate, which comprises the following steps: s1, adding diethyl carbonate and dimethyl carbonate into a reaction container to mix, wherein the mass ratio of the diethyl carbonate to the dimethyl carbonate is 1:1-1: 10; s2, adding a catalyst into the reaction container, continuously mixing, heating and pressurizing the reaction container, controlling the reaction temperature to be 10-130 ℃, controlling the reaction pressure to be 0-100KPa, reacting to generate a mixture containing ethyl methyl carbonate, and removing the catalyst; s3, adding the mixture in S2 into a treating tower T1. The invention realizes the technology of producing methyl ethyl carbonate by converting industrial diethyl carbonate, and the technology can continuously and stably operate; and (4) digesting the excess diethyl carbonate to produce the product of methyl ethyl carbonate with larger demand.
Description
Technical Field
The invention relates to the technical field of ethyl methyl carbonate production, in particular to a method for industrially producing ethyl methyl carbonate by reacting diethyl carbonate and dimethyl carbonate.
Background
The methyl ethyl carbonate is an organic compound, has a molecular formula of C4H8O3, 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. The ethyl methyl carbonate should be stored in a cool, ventilated and dry place for storage and transportation according to the regulations of flammable chemicals.
The prior art is used for producing the diethyl carbonate by reacting dimethyl carbonate with ethanol, the products comprise methyl ethyl carbonate and diethyl carbonate, the proportion of the two products is difficult to adjust, and the diethyl carbonate has excessive production capacity.
Therefore, a method for industrially producing the ethyl methyl carbonate by reacting diethyl carbonate and dimethyl carbonate is designed.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for industrially producing ethyl methyl carbonate by reacting diethyl carbonate and dimethyl carbonate.
In order to achieve the purpose, the invention adopts the following technical scheme:
the method for industrially producing the methyl ethyl carbonate by the reaction of diethyl carbonate and dimethyl carbonate comprises the following steps:
s1, adding diethyl carbonate and dimethyl carbonate into a reaction container to mix, wherein the mass ratio of the diethyl carbonate to the dimethyl carbonate is 1:1-1: 10;
s2, adding a catalyst into the reaction container, continuously mixing, heating and pressurizing the reaction container, controlling the reaction temperature to be 10-130 ℃, controlling the reaction pressure to be 0-100KPa, reacting to generate a mixture containing ethyl methyl carbonate, and removing the catalyst;
s3, adding the mixture obtained in the step S2 into a treatment tower T1, removing unreacted diethyl carbonate in the mixture by using a treatment tower T1, obtaining a mixture of ethyl methyl carbonate and dimethyl carbonate at the top of a treatment tower T1, and obtaining a diethyl carbonate crude product at the bottom of the tower;
s4, adding the diethyl carbonate crude product obtained in the tower kettle into the reactor for continuous reaction;
s5, feeding the mixture of ethyl methyl carbonate and dimethyl carbonate into a treating tower T2, and obtaining a crude product of dimethyl carbonate at the top of the treating tower T2;
s6, adding the crude dimethyl carbonate obtained at the top of the treatment tower T2 into a reactor containing crude diethyl carbonate in S4 for reaction;
s7, obtaining a crude product of methyl ethyl carbonate in the tower kettle of the processing tower T2 in S5, and feeding the crude product of methyl ethyl carbonate into a processing tower T3;
s8, refining the processing tower T3 to obtain superior ethyl methyl carbonate, and refining the superior ethyl methyl carbonate continuously entering a processing tower T4 to obtain an electronic grade ethyl methyl carbonate product.
Preferably, the catalyst in S2 is sodium methoxide.
Preferably, the treating column T1 is a diethyl carbonate lightness-removing column.
Preferably, the treatment tower T2 is a methyl ethyl carbonate lightness-removing tower.
Preferably, the treatment tower T3 is a methyl ethyl carbonate refining tower.
Preferably, the treatment column T4 is a ethyl methyl carbonate product column.
Preferably, the mixture of ethyl methyl carbonate obtained in S2 is passed through a filtration system to remove the catalyst.
Compared with the prior art, the invention has the following beneficial effects:
1. diethyl carbonate and dimethyl carbonate react, and the mode, temperature, pressure, proportion, catalyst dosage and the like of a reactor are key points of the reaction stage;
2. a catalyst separation technology, which is how to separate the catalyst in the reaction product after the reaction is finished to obtain a pure mixture;
3. diethyl carbonate separation technology, complete diethyl carbonate separation and recycling technology.
In conclusion, the invention realizes the technology of producing ethyl methyl carbonate by converting industrial diethyl carbonate, and the operation is continuous and stable; and (4) digesting the excess diethyl carbonate to produce the product of methyl ethyl carbonate with larger demand.
Drawings
FIG. 1 is a flow chart of a method for industrially producing ethyl methyl carbonate by reacting diethyl carbonate with dimethyl carbonate according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
With reference to figure 1 of the drawings,
example 1
The method for industrially producing the methyl ethyl carbonate by the reaction of diethyl carbonate and dimethyl carbonate comprises the following steps:
s1, adding diethyl carbonate and dimethyl carbonate into a reaction container to mix, wherein the mass ratio of the diethyl carbonate to the dimethyl carbonate is 1: 2;
s2, adding a catalyst into the reaction vessel, continuously mixing, heating and pressurizing the reaction vessel, controlling the reaction temperature to be 10 ℃ and the reaction pressure to be 20KPa, reacting to generate a mixture containing ethyl methyl carbonate, removing the catalyst, wherein the catalyst in S2 is sodium methoxide, and the mixture of ethyl methyl carbonate obtained in S2 is removed by a filtration system;
s3, adding the mixture in the S2 into a treatment tower T1, removing unreacted diethyl carbonate in the mixture by using a treatment tower T1, obtaining a mixture of ethyl methyl carbonate and dimethyl carbonate at the top of a treatment tower T1, obtaining a crude diethyl carbonate product at the bottom of the tower, and obtaining a diethyl carbonate light-ends removal tower by using a treatment tower T1;
s4, adding the diethyl carbonate crude product obtained in the tower kettle into the reactor for continuous reaction;
s5, feeding the mixture of ethyl methyl carbonate and dimethyl carbonate into a treating tower T2, obtaining a dimethyl carbonate crude product at the top of the treating tower T2, wherein the treating tower T2 is a methyl ethyl carbonate lightness-removing tower;
s6, adding the crude dimethyl carbonate obtained at the top of the treatment tower T2 into a reactor containing crude diethyl carbonate in S4 for reaction;
s7, obtaining a crude product of methyl ethyl carbonate in the tower kettle of the processing tower T2 in the S5, wherein the crude product of methyl ethyl carbonate enters a processing tower T3, and the processing tower T3 is a refining tower of methyl ethyl carbonate;
s8, refining in a treatment tower T3 to obtain high-grade ethyl methyl carbonate, refining the high-grade ethyl methyl carbonate in a treatment tower T4 to obtain an electronic-grade ethyl methyl carbonate product, wherein the treatment tower T4 is a ethyl methyl carbonate product tower.
Example 2
The method for industrially producing the methyl ethyl carbonate by the reaction of diethyl carbonate and dimethyl carbonate comprises the following steps:
s1, adding diethyl carbonate and dimethyl carbonate into a reaction container to mix, wherein the mass ratio of the diethyl carbonate to the dimethyl carbonate is 1: 4;
s2, adding a catalyst into the reaction vessel, continuously mixing, heating and pressurizing the reaction vessel, controlling the reaction temperature at 40 ℃ and the reaction pressure at 40KPa, reacting to generate a mixture containing ethyl methyl carbonate, removing the catalyst, wherein the catalyst in S2 is sodium methoxide, and the mixture of ethyl methyl carbonate obtained in S2 is removed by a filtration system;
s3, adding the mixture in the S2 into a treatment tower T1, removing unreacted diethyl carbonate in the mixture by using a treatment tower T1, obtaining a mixture of ethyl methyl carbonate and dimethyl carbonate at the top of a treatment tower T1, obtaining a crude diethyl carbonate product at the bottom of the tower, and obtaining a diethyl carbonate light-ends removal tower by using a treatment tower T1;
s4, adding the diethyl carbonate crude product obtained in the tower kettle into the reactor for continuous reaction;
s5, feeding the mixture of ethyl methyl carbonate and dimethyl carbonate into a treatment tower T2, obtaining a dimethyl carbonate crude product at the top of the treatment tower T2, wherein the treatment tower T2 is a ethyl methyl carbonate lightness-removing tower;
s6, adding the crude dimethyl carbonate obtained at the top of the treatment tower T2 into a reactor containing crude diethyl carbonate in S4 for reaction;
s7, obtaining a crude product of methyl ethyl carbonate in the tower kettle of the processing tower T2 in the S5, wherein the crude product of methyl ethyl carbonate enters a processing tower T3, and the processing tower T3 is a refining tower of methyl ethyl carbonate;
s8, refining in a treatment tower T3 to obtain high-grade ethyl methyl carbonate, refining the high-grade ethyl methyl carbonate in a treatment tower T4 to obtain an electronic-grade ethyl methyl carbonate product, wherein the treatment tower T4 is a ethyl methyl carbonate product tower.
Example 3
The method for industrially producing the methyl ethyl carbonate by the reaction of diethyl carbonate and dimethyl carbonate comprises the following steps:
s1, adding diethyl carbonate and dimethyl carbonate into a reaction container to mix, wherein the mass ratio of the diethyl carbonate to the dimethyl carbonate is 1: 6;
s2, adding a catalyst into the reaction vessel, continuously mixing, heating and pressurizing the reaction vessel, controlling the reaction temperature to be 70 ℃, controlling the reaction pressure to be 60KPa, reacting to generate a mixture containing ethyl methyl carbonate, removing the catalyst, wherein the catalyst in S2 is sodium methoxide, and the mixture of ethyl methyl carbonate obtained in S2 is removed by a filtration system;
s3, adding the mixture in the S2 into a treatment tower T1, removing unreacted diethyl carbonate in the mixture by using a treatment tower T1, obtaining a mixture of ethyl methyl carbonate and dimethyl carbonate at the top of a treatment tower T1, obtaining a crude diethyl carbonate product at the bottom of the tower, and obtaining a diethyl carbonate light-ends removal tower by using a treatment tower T1;
s4, adding the diethyl carbonate crude product obtained in the tower kettle into the reactor for continuous reaction;
s5, feeding the mixture of ethyl methyl carbonate and dimethyl carbonate into a treating tower T2, obtaining a dimethyl carbonate crude product at the top of the treating tower T2, wherein the treating tower T2 is a methyl ethyl carbonate lightness-removing tower;
s6, adding the crude dimethyl carbonate obtained at the top of the treatment tower T2 into a reactor containing crude diethyl carbonate in S4 for reaction;
s7, obtaining a crude product of methyl ethyl carbonate in the tower kettle of the processing tower T2 in the S5, wherein the crude product of methyl ethyl carbonate enters a processing tower T3, and the processing tower T3 is a refining tower of methyl ethyl carbonate;
s8, refining in a treatment tower T3 to obtain high-grade ethyl methyl carbonate, refining the high-grade ethyl methyl carbonate in a treatment tower T4 to obtain an electronic-grade ethyl methyl carbonate product, wherein the treatment tower T4 is a ethyl methyl carbonate product tower.
Example 4
The method for industrially producing the methyl ethyl carbonate by the reaction of diethyl carbonate and dimethyl carbonate comprises the following steps:
s1, adding diethyl carbonate and dimethyl carbonate into a reaction container to mix, wherein the mass ratio of the diethyl carbonate to the dimethyl carbonate is 1: 8;
s2, adding a catalyst into the reaction vessel, continuously mixing, heating and pressurizing the reaction vessel, controlling the reaction temperature to be 100 ℃, controlling the reaction pressure to be 80KPa, reacting to generate a mixture containing ethyl methyl carbonate, removing the catalyst, wherein the catalyst in S2 is sodium methoxide, and the mixture of ethyl methyl carbonate obtained in S2 is removed by a filtration system;
s3, adding the mixture obtained in the step S2 into a treatment tower T1, removing unreacted diethyl carbonate in the mixture by using a treatment tower T1, obtaining a mixture of ethyl methyl carbonate and dimethyl carbonate at the top of a treatment tower T1, obtaining a diethyl carbonate crude product at the bottom of the tower, and obtaining a diethyl carbonate light-ends removal tower by using a treatment tower T1;
s4, adding the diethyl carbonate crude product obtained in the tower kettle into the reactor for continuous reaction;
s5, feeding the mixture of ethyl methyl carbonate and dimethyl carbonate into a treating tower T2, obtaining a dimethyl carbonate crude product at the top of the treating tower T2, wherein the treating tower T2 is a methyl ethyl carbonate lightness-removing tower;
s6, adding the crude dimethyl carbonate obtained at the top of the treatment tower T2 into a reactor containing crude diethyl carbonate in S4 for reaction;
s7, obtaining a crude product of methyl ethyl carbonate in the tower kettle of the processing tower T2 in the S5, wherein the crude product of methyl ethyl carbonate enters a processing tower T3, and the processing tower T3 is a refining tower of methyl ethyl carbonate;
s8, refining in a treatment tower T3 to obtain high-grade ethyl methyl carbonate, refining the high-grade ethyl methyl carbonate in a treatment tower T4 to obtain an electronic-grade ethyl methyl carbonate product, wherein the treatment tower T4 is a ethyl methyl carbonate product tower.
Example 5
The method for industrially producing the methyl ethyl carbonate by the reaction of diethyl carbonate and dimethyl carbonate comprises the following steps:
s1, adding diethyl carbonate and dimethyl carbonate into a reaction container to mix, wherein the mass ratio of the diethyl carbonate to the dimethyl carbonate is 1: 10;
s2, adding a catalyst into the reaction vessel, continuously mixing, heating and pressurizing the reaction vessel, controlling the reaction temperature to be 130 ℃, controlling the reaction pressure to be 100KPa, reacting to generate a mixture containing ethyl methyl carbonate, removing the catalyst, wherein the catalyst in S2 is sodium methoxide, and the mixture of ethyl methyl carbonate obtained in S2 is removed by a filtration system;
s3, adding the mixture in the S2 into a treatment tower T1, removing unreacted diethyl carbonate in the mixture by using a treatment tower T1, obtaining a mixture of ethyl methyl carbonate and dimethyl carbonate at the top of a treatment tower T1, obtaining a crude diethyl carbonate product at the bottom of the tower, and obtaining a diethyl carbonate light-ends removal tower by using a treatment tower T1;
s4, adding the diethyl carbonate crude product obtained in the tower kettle into the reactor for continuous reaction;
s5, feeding the mixture of ethyl methyl carbonate and dimethyl carbonate into a treating tower T2, obtaining a dimethyl carbonate crude product at the top of the treating tower T2, wherein the treating tower T2 is a methyl ethyl carbonate lightness-removing tower;
s6, adding the crude dimethyl carbonate obtained at the top of the treatment tower T2 into a reactor containing crude diethyl carbonate in S4 for reaction;
s7, obtaining a crude product of methyl ethyl carbonate in the tower kettle of the processing tower T2 in the S5, wherein the crude product of methyl ethyl carbonate enters a processing tower T3, and the processing tower T3 is a refining tower of methyl ethyl carbonate;
s8, refining in a treatment tower T3 to obtain high-grade ethyl methyl carbonate, refining the high-grade ethyl methyl carbonate in a treatment tower T4 to obtain an electronic-grade ethyl methyl carbonate product, wherein the treatment tower T4 is a ethyl methyl carbonate product tower.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (7)
1. The method for industrially producing the methyl ethyl carbonate by the reaction of diethyl carbonate and dimethyl carbonate is characterized by comprising the following steps:
s1, adding diethyl carbonate and dimethyl carbonate into a reaction container to mix, wherein the mass ratio of the diethyl carbonate to the dimethyl carbonate is 1:1-1: 10;
s2, adding a catalyst into the reaction container, continuously mixing, heating and pressurizing the reaction container, controlling the reaction temperature to be 10-130 ℃, controlling the reaction pressure to be 0-100KPa, reacting to generate a mixture containing ethyl methyl carbonate, and removing the catalyst;
s3, adding the mixture in the S2 into a treating tower T1, removing unreacted diethyl carbonate in the mixture by using a treating tower T1, obtaining a mixture of ethyl methyl carbonate and dimethyl carbonate at the top of a treating tower T1, and obtaining a crude product of diethyl carbonate at the bottom of the tower;
s4, adding the diethyl carbonate crude product obtained in the tower kettle into the reactor for continuous reaction;
s5, feeding the mixture of ethyl methyl carbonate and dimethyl carbonate into a treating tower T2, and obtaining a crude product of dimethyl carbonate at the top of the treating tower T2;
s6, adding the crude dimethyl carbonate obtained at the top of the treatment tower T2 into a reactor containing crude diethyl carbonate in S4 for reaction;
s7, obtaining a crude product of methyl ethyl carbonate in the tower kettle of the processing tower T2 in S5, and feeding the crude product of methyl ethyl carbonate into a processing tower T3;
s8, refining the processing tower T3 to obtain superior ethyl methyl carbonate, and refining the superior ethyl methyl carbonate continuously entering a processing tower T4 to obtain an electronic grade ethyl methyl carbonate product.
2. The method for industrially producing ethyl methyl carbonate by the reaction of diethyl carbonate and dimethyl carbonate according to claim 1, wherein the catalyst in S2 is sodium methoxide.
3. The method for industrially producing ethyl methyl carbonate by the reaction of diethyl carbonate and dimethyl carbonate according to claim 1, wherein the treating column T1 is a diethyl carbonate lightness-removing column.
4. The method for industrially producing ethyl methyl carbonate by the reaction of diethyl carbonate and dimethyl carbonate according to claim 1, wherein the treating column T2 is a ethyl methyl carbonate lightness-removing column.
5. The method for industrially producing ethyl methyl carbonate by the reaction of diethyl carbonate and dimethyl carbonate according to claim 1, wherein the treating column T3 is an ethyl methyl carbonate refining column.
6. The method for industrially producing ethyl methyl carbonate by the reaction of diethyl carbonate and dimethyl carbonate according to claim 1, wherein the treating column T4 is a ethyl methyl carbonate product column.
7. The method for industrially producing ethyl methyl carbonate by the reaction of diethyl carbonate and dimethyl carbonate according to claim 1, wherein the mixture of ethyl methyl carbonate obtained in S2 is passed through a filtration system to remove the catalyst.
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