CN103804124A - Preparation method of diethyl carbonate and methylethyl carbonate - Google Patents
Preparation method of diethyl carbonate and methylethyl carbonate Download PDFInfo
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- CN103804124A CN103804124A CN201410076692.8A CN201410076692A CN103804124A CN 103804124 A CN103804124 A CN 103804124A CN 201410076692 A CN201410076692 A CN 201410076692A CN 103804124 A CN103804124 A CN 103804124A
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- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 title claims abstract description 40
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000004821 distillation Methods 0.000 claims description 49
- 238000000066 reactive distillation Methods 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 20
- 239000007858 starting material Substances 0.000 claims description 20
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 abstract description 18
- 238000005265 energy consumption Methods 0.000 abstract description 12
- 239000002994 raw material Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 45
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 33
- 239000000203 mixture Substances 0.000 description 19
- 239000006227 byproduct Substances 0.000 description 9
- 239000000470 constituent Substances 0.000 description 8
- 238000000605 extraction Methods 0.000 description 5
- CXHHBNMLPJOKQD-UHFFFAOYSA-M methyl carbonate Chemical compound COC([O-])=O CXHHBNMLPJOKQD-UHFFFAOYSA-M 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 229960004756 ethanol Drugs 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- -1 methyl ethyl carbonate ester Chemical class 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 125000005911 methyl carbonate group Chemical group 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
- 230000009466 transformation Effects 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/128—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by alcoholysis
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the field of production of chemical products, and particularly relates to a preparation method of diethyl carbonate and methylethyl carbonate. The preparation method comprises the following steps: continuously adding the raw materials including dimethyl carbonate, absolute ethyl alcohol and a catalyst into a first rectifying tower for reactive rectification, wherein the temperature of a tower kettle is controlled to be 80-100 DEG C; adding a substance discharged from the tower kettle of the first rectifying tower into a second rectifying tower for reactive rectification to obtain a diethyl carbonate product, wherein the temperature of the tower kettle is controlled to be 115-130 DEG C; adding the substance discharged from the top of the second rectifying tower into a third rectifying tower for reactive rectification to obtain a methylethyl carbonate (EMC) product, wherein the temperature of the tower kettle is controlled to be 100-115 DEG C. The preparation method provided by the invention is used for preparing diethyl carbonate and methylethyl carbonate by adopting a continuous reactive rectification process, and the parameters such as the operation ratio, the reflux ratio and the like of the rectifying tower need not to be changed after being determined during the whole operation process as long as the feeding process is well controlled, therefore, the energy consumption is relatively low.
Description
Technical field
The present invention relates to Chemicals production field, in particular to the preparation method of a kind of carbonic acid diethyl ester and methyl ethyl carbonate fat.
Background technology
Carbonic acid diethyl ester and methyl ethyl carbonate fat are market outlook Chemicals very widely, the preparation method who generally adopts now prepares carbonic acid diethyl ester and methyl ethyl carbonate fat take dimethyl carbonate (DMC) and methyl alcohol as raw material adopts batch reactive distillation technology, the preparation method of this batch fractionating is because raw material drops in rectifying tower in batches, tower kettle product is down to certain value afterwards by its disposable discharge, therefore in the actual process of preparing carbonic acid diethyl ester and methyl ethyl carbonate fat, as kept overhead product component purity constant, will constantly increase reflux ratio, it is large that energy consumption also becomes thereupon.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of carbonic acid diethyl ester and methyl ethyl carbonate fat, to solve the above problems.
The preparation method that a kind of carbonic acid diethyl ester and methyl ethyl carbonate fat are provided in an embodiment of the present invention, comprises the following steps:
(a) starting material dimethyl carbonate (DMC), dehydrated alcohol (EA) and catalyzer are added continuously in the first rectifying tower and carry out reactive distillation, the tower reactor temperature of the first rectifying tower is controlled at 80-100 ℃;
(b) add Second distillation column to carry out reactive distillation the tower reactor of the first rectifying tower material out, the tower reactor temperature of Second distillation column is controlled at 115-130 ℃; The tower reactor of Second distillation column obtains product carbonic acid diethyl ester (DEC);
(c) add the 3rd rectifying tower to carry out reactive distillation the tower top of Second distillation column material out, the tower reactor temperature of the 3rd rectifying tower is controlled at 100-115 ℃; The tower reactor of the 3rd rectifying tower obtains product methyl ethyl carbonate fat (EMC).
Preferably, the tower top temperature of the first rectifying tower is controlled at 63-65 ℃.
Preferably, the tower top temperature of Second distillation column is controlled at 95-110 ℃.
Preferably, the tower top temperature of the 3rd rectifying tower is controlled at 85-100 ℃.
Preferably, in step (a), the mass ratio of starting material dimethyl carbonate (DMC) and dehydrated alcohol (EA) is between 1:1-0.5.
Preferably, the mass ratio of catalyzer and starting material charging is 0.5-5:100.
Preferably, the trim the top of column of the first rectifying tower is than being 2-5.
Preferably, the trim the top of column of the first rectifying tower is than being 2-5.
Preferably, the trim the top of column of the first rectifying tower is than being 2-5.
A kind of carbonic acid diethyl ester that the embodiment of the present invention provides and the preparation method of methyl ethyl carbonate fat, compared with the method for preparing carbonic acid diethyl ester and methyl ethyl carbonate fat of the prior art, it adopts continuous reaction rectification technology to prepare carbonic acid diethyl ester and methyl ethyl carbonate fat, the operation ratio of rectifying tower, the parameters such as reflux ratio need not be changed in determining whole operating process, as long as control charging well, therefore energy consumption is lower, preparation method's principle of the embodiment of the present invention is: utilize starting material DMC and EA to carry out transesterification reaction, generate carbonic acid diethyl ester, methyl ethyl carbonate fat and by-product carbinol (ME), due to the restriction of self chemical reaction equilibrium, by-product carbinol quality percentage composition accounts for 15%-20% left and right in gross product content.
Accompanying drawing explanation
Fig. 1 shows the preparation flow figure of diethyl carbonate in the embodiment of the present invention and methylcarbonate;
Reference numeral: 1 first rectifying tower, 2 Second distillation columns, 3 strainers, 4 the 3rd rectifying tower.
Embodiment
Also by reference to the accompanying drawings the present invention is described in further detail below by specific embodiment.
(a) starting material dimethyl carbonate (DMC), dehydrated alcohol (EA) and catalyzer are added continuously in the first rectifying tower 1 and carry out reactive distillation, the tower reactor temperature of the first rectifying tower 1 is controlled at 80-100 ℃;
(b) add Second distillation column 2 to carry out reactive distillation the tower reactor of the first rectifying tower 1 material out, the tower reactor temperature of Second distillation column 2 is controlled at 115-130 ℃; The tower reactor of Second distillation column 2 obtains product carbonic acid diethyl ester (DEC);
(c) tower top of Second distillation column 2 material is out added the 3rd rectifying tower 4 carry out reactive distillation, the tower reactor temperature of the 3rd rectifying tower 4 is controlled at 100-115 ℃; The tower reactor of the 3rd rectifying tower 4 obtains product methyl ethyl carbonate fat (EMC).
As shown in Figure 1, the preparation method of the embodiment of the present invention adopts continuous reaction rectification technology to prepare carbonic acid diethyl ester and methyl ethyl carbonate fat, in whole operating process, the parameter such as the operation of rectifying tower ratio, reflux ratio need not be changed once determining, as long as control charging well, therefore energy consumption is lower, the charge ratio of rectifying tower operation and the reflux ratio numerical value during according to general normal running determines, guarantees that gas-liquid two-phase can realize mass transfer and obtain the finished product.
Preferably, in step (a), the tower top temperature of the first rectifying tower 1 is controlled at 63-65 ℃, the light constituent of overhead extraction is mainly the azeotrope of methyl alcohol and DMC, at the bottom of tower, the heavy constituent of extraction is mainly DEC, EMC, in the time that column bottom temperature is lower, also can contain a small amount of EA, methyl alcohol and DMC, controlling tower top temperature is mainly in order better to separate light constituent, guarantees the purity of product.
Preferably, in step (b), the tower top temperature of Second distillation column 2 is controlled at 95-110 ℃, and the light constituent of overhead extraction is mainly EMC, EA, methyl alcohol and DMC, and the restructuring of tower reactor is divided into product D EC, controlling tower top temperature is mainly in order better to separate light constituent, improves product D EC purity.
Preferably, described in step (c), the tower top temperature of the 3rd rectifying tower 4 is controlled at 85-100 ℃, and the light constituent of overhead extraction is mainly tower top methyl alcohol, EA and DMC, and light constituent preferably returns to the first rectifying tower and further reacts, and tower reactor obtains product EMC.
Preferably, in step (a), the mass ratio of starting material dimethyl carbonate (DMC) and dehydrated alcohol (EA) is between 1:1-0.5, in the time that methylcarbonate and ethanol mass ratio are 1:0.5, ethanol synthesis is more complete, methylcarbonate residue is more, product methyl ethyl carbonate ester content is high, diethyl carbonate is less, and in the time that methylcarbonate and ethanol mass ratio are 1:1, dimethyl carbonate is more complete, ethanol residue is more, product diethyl carbonate content is high, Methyl ethyl carbonate is less, therefore charge ratio can make the proportional balancing method of two kinds of products within this scope.
Preferably, in step (a), the mass ratio of catalyzer and starting material charging is 0.5-5:100, the too low effect that does not have catalysis of the consumption of catalyzer, and meeting under certain starting material transformation efficiency condition, increase catalyst levels can raise the cost also can increase the difficulty that subsequent catalyst separates.
Preferably, in step (a), the trim the top of column of the first rectifying tower 1 is than being 2-5, and the EA content in the time that reflux ratio is too low in the tower top of the first rectifying tower is too high, and in the time that reflux ratio is too high, energy consumption is too large.
Preferably, in step (b), the trim the top of column of Second distillation column 2 is than being 2-5, and reflux ratio was lower than 2 o'clock, and the tower top diethyl carbonate content of Second distillation column is too high, and in the time that reflux ratio is too high, energy consumption is too large.
Preferably, in step (c), the trim the top of column of the 3rd rectifying tower 4 is than being 2-5, and reflux ratio was lower than 2 o'clock, and the tower top methyl ethyl carbonate ester content of the 3rd rectifying tower is too high, and in the time that reflux ratio is too high, energy consumption is too large.
Preferably, between step (a) and step (b), increase following steps, the tower reactor of the first rectifying tower 1 material is out introduced into strainer 3 to be filtered and enters Second distillation column 2 for the separation of catalyzer again and carry out reactive distillation, the most handy metal sintering strainer of strainer 3, grow this strainer environmental protection, duration of service and well filtering catalyst of good filtration effect, realize the separation of catalyzer.
Embodiment 1:
By starting material dimethyl carbonate (DMC), dehydrated alcohol (EA), with mass ratio 3:1, catalyzer and raw material quality ratio 10:100 add continuously in the first rectifying tower and carry out reactive distillation, and the tower reactor temperature of the first rectifying tower is controlled at 80 ℃;
Add Second distillation column to carry out reactive distillation the tower reactor of the first rectifying tower material out, the tower reactor temperature of Second distillation column is controlled at 115 ℃; The tower reactor of Second distillation column obtains product carbonic acid diethyl ester (DEC);
Add the 3rd rectifying tower to carry out reactive distillation the tower top of Second distillation column material out, the tower reactor temperature of the 3rd rectifying tower is controlled at 100 ℃; The tower reactor of the 3rd rectifying tower obtains product methyl ethyl carbonate fat (EMC).
In the excessive light constituent that causes tower top of starting material methylcarbonate, DMC content is high, in product, EMC quality percentage composition is 40%, DEC quality percentage composition 10%, by-product carbinol 33%, in product, also contain in addition the mixture of 17%EA, DMC and ME, in bottom product, containing catalyzer needs further to separate.
Embodiment 2:
By starting material dimethyl carbonate (DMC), dehydrated alcohol (EA) with mass ratio 1:0.5, catalyzer and raw material quality ratio 1:200 add continuously and in the first rectifying tower, carry out reactive distillation, the tower reactor temperature of the first rectifying tower is controlled at 100 ℃, and the tower top temperature of the first rectifying tower is controlled at 63 ℃;
Add Second distillation column to carry out reactive distillation the tower reactor of the first rectifying tower material out, the tower reactor temperature of Second distillation column is controlled at 130 ℃; The tower reactor of Second distillation column obtains product carbonic acid diethyl ester (DEC);
Add the 3rd rectifying tower to carry out reactive distillation the tower top of Second distillation column material out, the tower reactor temperature of the 3rd rectifying tower is controlled at 115 ℃; The tower reactor of the 3rd rectifying tower obtains product methyl ethyl carbonate fat (EMC).
Starting material methylcarbonate is excessive a little, and in product, EMC quality percentage composition is at 45%, DEC quality percentage composition 15%, and by-product carbinol 36%, also contains in product in addition and in the mixture bottom product of 4%EA, DMC and ME, contain catalyzer and need further to separate.
Embodiment 3
By starting material dimethyl carbonate (DMC), dehydrated alcohol (EA) with mass ratio 1:1, catalyzer and raw material quality ratio 1:20 add continuously and in the first rectifying tower, carry out reactive distillation, the tower reactor temperature of the first rectifying tower is controlled at 90 ℃, and the tower top temperature of the first rectifying tower is controlled at 65 ℃;
Add Second distillation column to carry out reactive distillation the tower reactor of the first rectifying tower material out, the tower reactor temperature of Second distillation column is controlled at 120 ℃, the tower top temperature of Second distillation column is controlled at 95 ℃, and the tower reactor of Second distillation column obtains product carbonic acid diethyl ester (DEC);
Add the 3rd rectifying tower to carry out reactive distillation the tower top of Second distillation column material out, the tower reactor temperature of the 3rd rectifying tower is controlled at 110 ℃; The tower reactor of the 3rd rectifying tower obtains product methyl ethyl carbonate fat (EMC).
In starting material, ethanol is excessive, and in product, EMC quality percentage composition is at 12%, DEC quality percentage composition 37%, and by-product carbinol 45%, also contains the mixture of 6%EA, DMC and ME in addition in product, and in bottom product, containing catalyzer needs further to separate.
Embodiment 4
By starting material dimethyl carbonate (DMC), dehydrated alcohol (EA) with mass ratio 1:0.8, catalyzer and raw material quality ratio 1:25 add continuously and in the first rectifying tower, carry out reactive distillation, the tower reactor temperature of the first rectifying tower is controlled at 95 ℃, the tower top temperature of the first rectifying tower is controlled at 64 ℃, and reflux ratio is 2;
Add Second distillation column to carry out reactive distillation the tower reactor of the first rectifying tower material out, the tower reactor temperature of Second distillation column is controlled at 118 ℃, and the tower top temperature of Second distillation column is controlled at 110 ℃; The tower reactor of Second distillation column obtains product carbonic acid diethyl ester (DEC);
Add the 3rd rectifying tower to carry out reactive distillation the tower top of Second distillation column material out, the tower reactor temperature of the 3rd rectifying tower is controlled at 108 ℃, and the tower top temperature of the 3rd rectifying tower is controlled at 85 ℃; The tower reactor of the 3rd rectifying tower obtains product methyl ethyl carbonate fat (EMC).
In product, EMC quality percentage composition is at 18%, DEC quality percentage composition 41%, and by-product carbinol 41%, contains further separation of catalyzer in bottom product.
Embodiment 5
By starting material dimethyl carbonate (DMC), dehydrated alcohol (EA) with mass ratio 1:0.8, catalyzer and raw material quality ratio 1:25 add continuously and in the first rectifying tower, carry out reactive distillation, the tower reactor temperature of the first rectifying tower is controlled at 95 ℃, the tower top temperature of the first rectifying tower is controlled at 64 ℃, and reflux ratio is 2;
The tower reactor of the first rectifying tower material is out introduced into strainer to be entered Second distillation column after for the separation of catalyzer again and carries out reactive distillation, the tower reactor temperature of Second distillation column is controlled at 118 ℃, the tower top temperature of Second distillation column is controlled at 100 ℃, and reflux ratio is 5; The tower reactor of Second distillation column obtains product carbonic acid diethyl ester (DEC);
Add the 3rd rectifying tower to carry out reactive distillation the tower top of Second distillation column material out, the tower reactor temperature of the 3rd rectifying tower is controlled at 108 ℃, and the tower top temperature of the 3rd rectifying tower is controlled at 100 ℃, and reflux ratio is 3; The tower reactor of the 3rd rectifying tower obtains product methyl ethyl carbonate fat (EMC).
In product, EMC quality percentage composition is at 19%, DEC quality percentage composition 40%, by-product carbinol 41%.
Embodiment 6
By starting material dimethyl carbonate (DMC), dehydrated alcohol (EA) with mass ratio 1:0.8, catalyzer and raw material quality ratio 1:25 add continuously and in the first rectifying tower, carry out reactive distillation, the tower reactor temperature of the first rectifying tower is controlled at 95 ℃, the tower top temperature of the first rectifying tower is controlled at 64 ℃, and reflux ratio is 5;
The tower reactor of the first rectifying tower material is out introduced into metal sintering strainer to be entered Second distillation column after for the separation of catalyzer again and carries out reactive distillation, the tower reactor temperature of Second distillation column is controlled at 118 ℃, the tower top temperature of Second distillation column is controlled at 105 ℃, and reflux ratio is 3; The tower reactor of Second distillation column obtains product carbonic acid diethyl ester (DEC);
Add the 3rd rectifying tower to carry out reactive distillation the tower top of Second distillation column material out, the tower reactor temperature of the 3rd rectifying tower is controlled at 108 ℃, and the tower top temperature of the 3rd rectifying tower is controlled at 92 ℃, and reflux ratio is 4; The tower reactor of the 3rd rectifying tower obtains product methyl ethyl carbonate fat (EMC).
In product, EMC quality percentage composition is at 18%, DEC quality percentage composition 41%, by-product carbinol 41%.
Embodiment 7
Form with product: EMC quality percentage composition 18% in product, DEC quality percentage composition 41%, by-product carbinol 41% is example, now preparation method of the present invention is contrasted in the energy consumption of producing in same product situation with the preparation method of prior art: specifically see the following form 1:
Table 1 energy consumption comparison sheet
As can be seen from the table, produce equally the product of the above-mentioned composition of 1kg, total energy consumption of the present invention is lower than the total energy consumption of prior art, and the large gross investment of energy consumption also can increase thereupon, and therefore preparation method of the present invention is more energy-conservation.
Preparation method of the present invention, at rectifying tower charging and the whole continous-stables of rectifying tower product extraction, produces thereby realize serialization, and industrial scale can be increased substantially, and commercial production scale is brought up to ton from kiloton; Easy and simple to handle, operator easily grasp production essentials, and labor intensity of operating staff significantly reduces; Methyl ethyl carbonate and diethyl carbonate are realized mass-producing output simultaneously, production economy remarkable benefit.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a preparation method for carbonic acid diethyl ester and methyl ethyl carbonate fat, is characterized in that, comprises the following steps:
(a) starting material dimethyl carbonate (DMC), dehydrated alcohol (EA) and catalyzer are added continuously in the first rectifying tower and carry out reactive distillation, the tower reactor temperature of described the first rectifying tower is controlled at 80-100 ℃;
(b) add Second distillation column to carry out reactive distillation the tower reactor of described the first rectifying tower material out, the tower reactor temperature of described Second distillation column is controlled at 115-130 ℃; The tower reactor of described Second distillation column obtains product carbonic acid diethyl ester (DEC);
(c) add the 3rd rectifying tower to carry out reactive distillation the tower top of described Second distillation column material out, the tower reactor temperature of described the 3rd rectifying tower is controlled at 100-115 ℃; The tower reactor of described the 3rd rectifying tower obtains product methyl ethyl carbonate fat (EMC).
2. preparation method according to claim 1, is characterized in that, described in step (a), the tower top temperature of the first rectifying tower is controlled at 63-65 ℃.
3. preparation method according to claim 1, is characterized in that, described in step (b), the tower top temperature of Second distillation column is controlled at 95-110 ℃.
4. preparation method according to claim 1, is characterized in that, described in step (c), the tower top temperature of the 3rd rectifying tower is controlled at 85-100 ℃.
5. preparation method according to claim 1, is characterized in that, in step (a), the mass ratio of starting material dimethyl carbonate (DMC) and dehydrated alcohol (EA) is between 1:1-0.5.
6. preparation method according to claim 1, is characterized in that, in step (a), the mass ratio of described catalyzer and described starting material charging is 0.5-5:100.
7. preparation method according to claim 1, is characterized in that, in step (a), the trim the top of column of described the first rectifying tower is than being 2-5.
8. preparation method according to claim 1, is characterized in that, in step (b), the trim the top of column of described Second distillation column is than being 2-5.
9. preparation method according to claim 1, is characterized in that, in step (c), the trim the top of column of described the 3rd rectifying tower is than being 2-5.
10. preparation method according to claim 1, it is characterized in that, between step (a) and step (b), increase following steps, the tower reactor of described the first rectifying tower material is out introduced into strainer and filters and enter again described Second distillation column for the separation of catalyzer and carry out reactive distillation.
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Cited By (10)
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| CN105646219A (en) * | 2016-01-24 | 2016-06-08 | 辽宁会福化工有限公司 | Method for catalytically synthesizing diethyl carbonate by means of strong acidic cationic resin |
| CN109096115A (en) * | 2018-07-02 | 2018-12-28 | 赵杰 | A kind of methyl ethyl carbonate preparation process |
| CN110818900A (en) * | 2019-12-12 | 2020-02-21 | 浙江润禾有机硅新材料有限公司 | Method and production system for continuously catalyzing, synthesizing and separating high-purity low-viscosity dimethyl silicone oil |
| CN113248379A (en) * | 2021-06-04 | 2021-08-13 | 重庆微而易科技有限公司 | Method for preparing methyl ethyl carbonate by adopting pipeline continuous reactor |
| CN114436840A (en) * | 2022-02-21 | 2022-05-06 | 江苏思派新能源科技有限公司 | Method for industrially producing methyl ethyl carbonate by reacting diethyl carbonate and dimethyl carbonate |
| WO2022114592A1 (en) | 2020-11-26 | 2022-06-02 | 롯데케미칼 주식회사 | Method for producing heterogeneous linear carbonates using catalyst with excellent solubility |
| WO2022114576A1 (en) | 2020-11-26 | 2022-06-02 | 롯데케미칼 주식회사 | Method for preparing heterologous linear carbonate, with catalyst filtering step introduced thereinto |
| KR20230077543A (en) | 2021-11-25 | 2023-06-01 | 롯데케미칼 주식회사 | Manufacturing method of carbonates |
| KR20230080590A (en) | 2021-11-30 | 2023-06-07 | 롯데케미칼 주식회사 | Manufacturing method of carbonates |
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| WO2023101296A1 (en) | 2021-11-30 | 2023-06-08 | 롯데케미칼 주식회사 | Method for preparing carbonate |
| CN114436840A (en) * | 2022-02-21 | 2022-05-06 | 江苏思派新能源科技有限公司 | Method for industrially producing methyl ethyl carbonate by reacting diethyl carbonate and dimethyl carbonate |
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