CN107032998A - A kind of methyl ethyl carbonate method for continuously synthesizing without catalyst - Google Patents
A kind of methyl ethyl carbonate method for continuously synthesizing without catalyst Download PDFInfo
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- CN107032998A CN107032998A CN201710296483.8A CN201710296483A CN107032998A CN 107032998 A CN107032998 A CN 107032998A CN 201710296483 A CN201710296483 A CN 201710296483A CN 107032998 A CN107032998 A CN 107032998A
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- methyl ethyl
- ethyl carbonate
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- synthetic tower
- continuously synthesizing
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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
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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
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention belongs to the technical field of ester-interchange method anthropogenics, more particularly to a kind of methyl ethyl carbonate method for continuously synthesizing without catalyst.Comprise the following steps：（1）Dimethyl carbonate, ethanol are mixed in proportion, are added to after mixing after heat exchanger is preheated in synthetic tower；（2）Dimethyl carbonate and ethanol in certain temperature, pressure and carry out ester exchange reaction under conditions of existing without catalyst in synthetic tower；（3）Separation, recovery light component at the top of synthetic tower；（4）Collect methyl ethyl carbonate crude product in synthetic tower bottom.The present invention need not add catalyst, it is to avoid the tedious steps such as the selection of catalyst, preparation, separation, recovery, reduce production cost, realize the continuous production of methyl ethyl carbonate.
Description
（One）Technical field
The invention belongs to the technical field of ester-interchange method anthropogenics, more particularly to a kind of methyl ethyl carbonate without catalyst
Ester method for continuously synthesizing.
（Two）Background technology
Methyl ethyl carbonate is a kind of widely used asymmetric carbon ester compound, is mainly used as in the middle of solvent and organic synthesis
Body, the particularly solvent as non-aqueous electrolyte in lithium battery, compared with symmetrical carbonic ester, because it possesses methyl simultaneously
And ethyl, therefore have the advantage of dimethyl carbonate and diethyl carbonate concurrently.During as lithium ion battery electrolyte solvent, due to carbon
Sour methyl ethyl ester viscosity is small, and dielectric constant is big, and the dissolubility to lithium salts is strong, can more improve the energy density and discharge capacity of battery,
Security performance can more be improved and increased the service life, and good low temperature performance.
The synthetic method of methyl ethyl carbonate mainly has phosgenation, oxidative carbonylation and ester-interchange method.Phosgenation raw material severe toxicity,
And the hydrogen chloride severe corrosion equipment produced during the course of the reaction, severe contamination environment, the method is gradually eliminated.
Oxidative carbonylation is not perfect, exist the low, catalyst of selectivity it is expensive, the shortcomings of be difficult to operational control.
Ester-interchange method has dimethyl carbonate and diethyl carbonate, dimethyl carbonate and ethanol and diethyl carbonate and methanol
For three kinds of synthetic routes of raw material, in building-up process, it is important that selecting catalyst, the selection of catalyst, preparation, separation,
Recycling step is cumbersome and cost also has a larger increase.
In summary, all there is certain lack in above mentioned phosgenation, oxidative carbonylation and catalyst ester-interchange method
Fall into.
（Three）The content of the invention
There is provided a kind of methyl ethyl carbonate method for continuously synthesizing without catalyst in order to make up the deficiencies in the prior art by the present invention.
The present invention is achieved through the following technical solutions：
A kind of methyl ethyl carbonate method for continuously synthesizing without catalyst, it is characterised in that：Comprise the following steps：（1）By carbonic acid two
Methyl esters, ethanol are mixed in proportion, are added to after mixing after heat exchanger is preheated in synthetic tower；（2）Dimethyl carbonate and ethanol
In synthetic tower certain temperature, pressure and without catalyst exist under conditions of carry out ester exchange reaction；（3）Synthetic tower top
From, reclaim light component；（4）Collect methyl ethyl carbonate crude product in synthetic tower bottom.
Wherein, synthetic tower charging dimethyl carbonate and ethanol mass ratio are adjusted from 3:1 to 5:1, can obtain methyl ethyl carbonate and
Diethyl carbonate product proportion 5:1 to 9:1.
Further, in synthetic tower in 1.3~1.5MPa of operating pressure.
Further, the temperature in synthetic tower is 200 DEG C ~ 215 DEG C.
Further, the light component of separation is recycled in methanol tank after condenser is condensed at the top of the synthetic tower.
Further, the methyl ethyl carbonate that synthetic tower bottom is collected is recycled to after condenser is condensed in crude product storage tank.
Further, the methyl ethyl carbonate in the crude product storage tank by dealcoholysis, it is de- light and refined after obtain finished product carbonic acid first
Ethyl ester.
The beneficial effects of the invention are as follows：The present invention need not add catalyst, it is to avoid the selection of catalyst, preparation, point
From, reclaim etc. tedious steps, reduce production cost, realize the continuous production of methyl ethyl carbonate.
（Four）Embodiment
Embodiment 1
Comprise the following steps：
（1）Dimethyl carbonate, ethanol are mixed in proportion, are added to after mixing after heat exchanger is preheated in synthetic tower；
（2）Dimethyl carbonate and temperature of the ethanol in synthetic tower are 200 DEG C ~ 215 DEG C, in synthetic tower in operating pressure 1.3
~1.5MPa and without catalyst exist under conditions of carry out ester exchange reaction；
（3）Separation, recovery light component at the top of synthetic tower；
（4）Collect methyl ethyl carbonate crude product in synthetic tower bottom.
Synthetic tower feeds dimethyl carbonate and the adjustment of ethanol mass ratio from 3:1, methyl ethyl carbonate and diethyl carbonate can be obtained
Product proportion 5:1.
The light component of separation is recycled in methanol tank after condenser is condensed at the top of synthetic tower.
The methyl ethyl carbonate that synthetic tower bottom is collected is recycled to after condenser is condensed in crude product storage tank.In crude product storage tank
Methyl ethyl carbonate by dealcoholysis, it is de- light and refined after obtain finished product methyl ethyl carbonate.
Embodiment 2
Comprise the following steps：
（1）Dimethyl carbonate, ethanol are mixed in proportion, are added to after mixing after heat exchanger is preheated in synthetic tower；
（2）Dimethyl carbonate and temperature of the ethanol in synthetic tower are 200 DEG C ~ 215 DEG C, in synthetic tower in operating pressure 1.3
~1.5MPa and without catalyst exist under conditions of carry out ester exchange reaction；
（3）Separation, recovery light component at the top of synthetic tower；
（4）Collect methyl ethyl carbonate crude product in synthetic tower bottom.
Synthetic tower feeds dimethyl carbonate and the adjustment of ethanol mass ratio from 3.5:1, methyl ethyl carbonate and carbonic acid diethyl can be obtained
Ester product proportion 5.8:1.
The light component of separation is recycled in methanol tank after condenser is condensed at the top of synthetic tower.
The methyl ethyl carbonate that synthetic tower bottom is collected is recycled to after condenser is condensed in crude product storage tank.In crude product storage tank
Methyl ethyl carbonate by dealcoholysis, it is de- light and refined after obtain finished product methyl ethyl carbonate.
Embodiment 3
Comprise the following steps：
（1）Dimethyl carbonate, ethanol are mixed in proportion, are added to after mixing after heat exchanger is preheated in synthetic tower；
（2）Dimethyl carbonate and temperature of the ethanol in synthetic tower are 200 DEG C ~ 215 DEG C, in synthetic tower in operating pressure 1.3
~1.5MPa and without catalyst exist under conditions of carry out ester exchange reaction；
（3）Separation, recovery light component at the top of synthetic tower；
（4）Collect methyl ethyl carbonate crude product in synthetic tower bottom.
Synthetic tower feeds dimethyl carbonate and the adjustment of ethanol mass ratio from 4:1, methyl ethyl carbonate and diethyl carbonate can be obtained
Product proportion 6.7:1.
The light component of separation is recycled in methanol tank after condenser is condensed at the top of synthetic tower.
The methyl ethyl carbonate that synthetic tower bottom is collected is recycled to after condenser is condensed in crude product storage tank.In crude product storage tank
Methyl ethyl carbonate by dealcoholysis, it is de- light and refined after obtain finished product methyl ethyl carbonate.
Embodiment 4
Comprise the following steps：
（1）Dimethyl carbonate, ethanol are mixed in proportion, are added to after mixing after heat exchanger is preheated in synthetic tower；
（2）Dimethyl carbonate and temperature of the ethanol in synthetic tower are 200 DEG C ~ 215 DEG C, in synthetic tower in operating pressure 1.3
~1.5MPa and without catalyst exist under conditions of carry out ester exchange reaction；
（3）Separation, recovery light component at the top of synthetic tower；
（4）Collect methyl ethyl carbonate crude product in synthetic tower bottom.
Synthetic tower feeds dimethyl carbonate and the adjustment of ethanol mass ratio from 4.5:1, methyl ethyl carbonate and carbonic acid diethyl can be obtained
Ester product proportion 8.1:1.
The light component of separation is recycled in methanol tank after condenser is condensed at the top of synthetic tower.
The methyl ethyl carbonate that synthetic tower bottom is collected is recycled to after condenser is condensed in crude product storage tank.In crude product storage tank
Methyl ethyl carbonate by dealcoholysis, it is de- light and refined after obtain finished product methyl ethyl carbonate.
Embodiment 5
Comprise the following steps：
（1）Dimethyl carbonate, ethanol are mixed in proportion, are added to after mixing after heat exchanger is preheated in synthetic tower；
（2）Dimethyl carbonate and temperature of the ethanol in synthetic tower are 200 DEG C ~ 215 DEG C, in synthetic tower in operating pressure 1.3
~1.5MPa and without catalyst exist under conditions of carry out ester exchange reaction；
（3）Separation, recovery light component at the top of synthetic tower；
（4）Collect methyl ethyl carbonate crude product in synthetic tower bottom.
Synthetic tower feeds dimethyl carbonate and the adjustment of ethanol mass ratio from 5:1, methyl ethyl carbonate and diethyl carbonate can be obtained
Product proportion 9:1.
The light component of separation is recycled in methanol tank after condenser is condensed at the top of synthetic tower.
The methyl ethyl carbonate that synthetic tower bottom is collected is recycled to after condenser is condensed in crude product storage tank.In crude product storage tank
Methyl ethyl carbonate by dealcoholysis, it is de- light and refined after obtain finished product methyl ethyl carbonate.
The present invention is described by way of example above, but the invention is not restricted to above-mentioned specific embodiment, it is all to be based on
Any change or modification that the present invention is done belong to the scope of protection of present invention.
Claims (7)
1. a kind of methyl ethyl carbonate method for continuously synthesizing without catalyst, it is characterised in that：Comprise the following steps：（1）By carbonic acid
Dimethyl ester, ethanol are mixed in proportion, are added to after mixing after heat exchanger is preheated in synthetic tower；（2）Dimethyl carbonate and second
Alcohol in synthetic tower certain temperature, pressure and without catalyst exist under conditions of carry out ester exchange reaction；（3）At the top of synthetic tower
Separation, recovery light component；（4）Collect methyl ethyl carbonate crude product in synthetic tower bottom.
2. the methyl ethyl carbonate method for continuously synthesizing according to claim 1 without catalyst, it is characterised in that：Synthetic tower enters
Expect dimethyl carbonate and the adjustment of ethanol mass ratio from 3:1 to 5:1, methyl ethyl carbonate and diethyl carbonate product proportion 5 can be obtained:1
To 9:1.
3. the methyl ethyl carbonate method for continuously synthesizing according to claim 1 without catalyst, it is characterised in that in synthetic tower
In 1.3~1.5MPa of operating pressure.
4. the methyl ethyl carbonate method for continuously synthesizing according to claim 1 without catalyst, it is characterised in that in synthetic tower
Temperature be 200 DEG C ~ 215 DEG C.
5. the methyl ethyl carbonate method for continuously synthesizing according to claim 1 without catalyst, it is characterised in that the synthesis
The light component of top of tower separation is recycled in methanol tank after condenser is condensed.
6. the methyl ethyl carbonate method for continuously synthesizing according to claim 1 without catalyst, it is characterised in that synthesis tower reactor
The methyl ethyl carbonate that bottom is collected is recycled to after condenser is condensed in crude product storage tank.
7. the methyl ethyl carbonate method for continuously synthesizing according to claim 6 without catalyst, it is characterised in that the crude product
Methyl ethyl carbonate in storage tank by dealcoholysis, it is de- light and refined after obtain finished product methyl ethyl carbonate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114478250A (en) * | 2021-12-27 | 2022-05-13 | 浙江联盛化学股份有限公司 | Preparation method of methyl ethyl carbonate and co-production of diethyl carbonate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103483200A (en) * | 2013-09-16 | 2014-01-01 | 河北工业大学 | Method for synthesizing ethyl methyl carbonate through ester exchange |
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2017
- 2017-04-28 CN CN201710296483.8A patent/CN107032998A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103483200A (en) * | 2013-09-16 | 2014-01-01 | 河北工业大学 | Method for synthesizing ethyl methyl carbonate through ester exchange |
Non-Patent Citations (2)
| Title |
|---|
| 张巧玲 等: "《化工工艺学》", 30 July 2015, 国防工业出版社 * |
| 舒庆 等: "《生物柴油科学与技术》", 31 December 2012, 冶金工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114478250A (en) * | 2021-12-27 | 2022-05-13 | 浙江联盛化学股份有限公司 | Preparation method of methyl ethyl carbonate and co-production of diethyl carbonate |
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Application publication date: 20170811 |