CN1384094A - Rectifying process of separating and purifying diethyl carbonate - Google Patents
Rectifying process of separating and purifying diethyl carbonate Download PDFInfo
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- CN1384094A CN1384094A CN 02115936 CN02115936A CN1384094A CN 1384094 A CN1384094 A CN 1384094A CN 02115936 CN02115936 CN 02115936 CN 02115936 A CN02115936 A CN 02115936A CN 1384094 A CN1384094 A CN 1384094A
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Abstract
The rectifying process is for separating and purifying diethyl carbonate (DEC) from ternary DEC-ethanol-water system as raw product of the ethanol liquid phase oxidation and carbonylation process. The rectifying process is performed in a rectifying tower with regular wire mesh corrugated packing and middle inlet for the raw product with certain feeding temperature, reactor temperature and top temperature being set. From the azeotropic mixture from the top of the tower the absolute ethanol is prepared and returned to the oxidation and carbonylation system. The said process can obtain diethyl carbonate product with purity as high as 99.5%.
Description
Technical field
The present invention relates to a kind of from diethyl carbonate-alcohol-water ternary system the method for rectifying separation purifying diethyl carbonate.
Background technology
Diethyl carbonate (Diethyl Carbonate vehicle economy C) is important Organic Chemicals, and purposes is very extensive.No matter be with phosgenation, ester-interchange method, or the synthetic DEC of oxidative carbonylation method all relate to the thick product separation purification problem in synthetic back.In the product of existing phosgenation and ester-interchange method except product DEC, also have ethanol and other alcohol (as methyl alcohol) and ester (as methylcarbonate), make system complicated component to be separated, and easily form polynary azeotropic mixture, more increased and separated the difficulty of purifying.And synthesize DEC with ethanol liquid-phase oxidation carbonylation is a kind of easy novel process, and the thick product of gained is the ternary system that contains diethyl carbonate-alcohol-water, the present invention is directed to the novel process of this synthesizing diethyl carbonate, and the rectifying separation purifying technique of thick product is provided.
Summary of the invention
The object of the present invention is to provide a kind of rectification process to separate diethyl carbonate-alcohol-water ternary system, and can improve the method for diethyl carbonate purity.
With ethanol (C
2H
5OH), carbon monoxide (CO), oxygen (O
2) produce in the technology of diethyl carbonate (DEC) for the raw material oxidative carbonylation, the thick product of gained is DEC-C
2H
5OH-H
2The O three component system, wherein major impurity is C
2H
5OH and H
2O, each constituent mass percentage composition: DEC is 15～20% in the thick product, H
2O is 0～5%, C
2H
5OH is 75～80%.Because H
2O and C
2H
5OH forms azeotropic system, and DEC and C
2H
5OH is azeotropic not, so employing water and ethanol azeotropic method are removed H wherein
2O removes remaining ethanol again, promptly gets the DEC product.
Method processing step of the present invention is as follows:
1. contain DEC-C
2H
5OH-H
2The thick product of O enters in the atmospheric distillation tower that the structured wire corrugated wire gauze packing is housed, and feeding temperature is set in 70～75 ℃, the adding speed 90～110kg/h of thick product, and keep reflux ratio 2～6;
2. the tower still temperature of rectifying tower is set in the boiling point a little more than DEC: 128～132 ℃, tower top temperature is set in a little more than C
2H
5OH and H
2The azeotropic point of O: 77～79 ℃, it is the azeotropic mixture of 0～5% alcohol-water that cat head distillates moisture;
3. distillating cat head moisture according to the industrial alcohol dewatering is the azeotropic mixture dehydration of 0～5% alcohol-water, and the dehydrated alcohol after the dehydration returns the oxidative carbonylation synthesis system;
4. the gas phase of the tower still of rectifying tower and liquid phase place respectively establish a side and adopt a little, and liquid phase place side is adopted a little direct extraction liquid phase diethyl carbonate product, and gas phase place side is adopted an extraction gas-phase carbon diethyl phthalate product, is liquid-phase product after condensation.
What the method for using the extraction of tower still gas phase can guarantee to produce carries out continuously, and effectively reduces the product foreign matter content.When tower steady running, the extraction of product is as the criterion with the temperature of tower bottoms phase point for measuring temperature, adopt with the gas phase side that is higher than the DEC boiling temperature after local normal atmosphere is proofreaied and correct an extraction after condensation the DEC product.
Adopt the method for separating and purifying diethyl carbonate of the present invention, can obtain diethyl carbonate content at tower still extraction point is 99.5% product.
Embodiment example 1.
The atmospheric distillation device is to consisting of diethyl carbonate 15%, ethanol 80%, the thick product of water 5% separates, and the rectifier unit tower diameter is φ 300mm, interior dress structured wire corrugated wire gauze packing, bed stuffing height 15m, 18 of stage number, feed location is the 7th block of plate from top to bottom.70 ℃ of control feeding temperatures, input speed 98kg/h, 132 ℃ of tower still temperature, 78 ℃ of tower top temperatures, reflux ratio 5.Be 3.5kg/h from tower still gas phase extraction mouth (the 17th block of plate from top to bottom) extraction total amount wherein, gas-phase product is cooled to liquid product (colourless) content table composed as follows:
Example 2.
| Cat head | H 2O | ?C 2H 5OH | ?DEC |
| Form | 5％ | 93％ | 2％ |
| Tower still (liquid phase) | H 2O | C 2H 5OH | DEC |
| Form | 0.1％ | 0.2％ | 99.5％ |
The atmospheric distillation device is to consisting of diethyl carbonate 10%, ethanol 85%, the thick product of water 5% separates, and the rectifier unit tower diameter is φ 300mm, interior dress structured wire corrugated wire gauze packing, bed stuffing height 15m, 18 of stage number, feed location is the 7th block of plate from top to bottom.72 ℃ of control feeding temperatures, input speed 98.0kg/h, 131 ℃ of tower still temperature, 79 ℃ of tower top temperatures, reflux ratio 4.Be 3.8kg/h from tower still gas phase extraction mouth (the 17th block of plate from top to bottom) extraction total amount wherein, gas-phase product is cooled to liquid product (colourless) content table composed as follows:
Example 3.
| Cat head | H 2O | C 2H 5OH | DEC |
| Form | 5％ | 93％ | 2％ |
| The tower bottoms phase | H 2O | C 2H 5OH | DEC |
| Form | 0.2％ | 0.4％ | 99.2％ |
The atmospheric distillation device is to consisting of diethyl carbonate 15%, ethanol 80%, the thick product of water 5% separates, and the rectifier unit tower diameter is φ 300mm, interior dress structured wire corrugated wire gauze packing, bed stuffing height 15m, in establish 18 of column plates, feed location is the 7th block of plate from top to bottom.74 ℃ of control feeding temperatures, input speed 104kg/h, 134 ℃ of tower still temperature, 78 ℃ of tower top temperatures, reflux ratio are 2.Be 3.7kg/h wherein from tower bottoms phase extraction mouth (the 18th block of plate from top to bottom) extraction total amount, liquid product (faint yellow) content table composed as follows:
| Cat head | H 2O | ?C 2H 5OH | ?DEC |
| Form | 5％ | ?93％ | ?2％ |
| The tower bottoms phase | H 2O | ?C 2H 5OH | ?DEC |
| Form | 0.5％ | ?0.6％ | ?98.5％ |
Claims (2)
1. the method for a separating and purifying diethyl carbonate the steps include:
1. with the thick product of oxidative carbonylation method synthesizing diethyl carbonate: the ternary system input of diethyl carbonate-alcohol-water is equipped with in the rectifying tower of structured wire corrugated wire gauze packing, sets feeding temperature, the adding speed of thick product, and keep certain reflux ratio;
2. set tower still temperature, the tower top temperature of rectifying tower, it is the azeotropic mixture of 0～5% alcohol-water that cat head distillates moisture;
3. distillating cat head moisture according to the industrial alcohol dewatering is the azeotropic mixture dehydration of 0～5% alcohol-water, and the dehydrated alcohol after the dehydration returns the oxidative carbonylation synthesis system;
4. the gas phase of the tower still of rectifying tower and liquid phase place respectively establish a side and adopt a little, and liquid phase place side is adopted a little direct extraction liquid phase diethyl carbonate product, and gas phase place side is adopted an extraction gas-phase carbon diethyl phthalate product, is liquid-phase product after condensation.
2. by the method for claim 1 indication, it is characterized in that step 1. the feeding temperature of indication be set at 70～75 ℃, the adding speed of thick product is 90～110kg/h, and keeps reflux ratio 2～6; The step 2. tower still temperature of rectifying tower is set at 128～132 ℃, and tower top temperature is set at 77～79 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02115936 CN1384094A (en) | 2002-06-07 | 2002-06-07 | Rectifying process of separating and purifying diethyl carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02115936 CN1384094A (en) | 2002-06-07 | 2002-06-07 | Rectifying process of separating and purifying diethyl carbonate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1384094A true CN1384094A (en) | 2002-12-11 |
Family
ID=4743958
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02115936 Pending CN1384094A (en) | 2002-06-07 | 2002-06-07 | Rectifying process of separating and purifying diethyl carbonate |
Country Status (1)
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|---|---|
| CN (1) | CN1384094A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101367733B (en) * | 2008-10-08 | 2011-12-07 | 西安交通大学 | Heat pump distillation apparatus and process for diethyl carbonate |
| CN105384639A (en) * | 2015-11-11 | 2016-03-09 | 东营市海科新源化工有限责任公司 | Refining purifying device and method used for continuously producing battery grade dimethyl carbonate |
-
2002
- 2002-06-07 CN CN 02115936 patent/CN1384094A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101367733B (en) * | 2008-10-08 | 2011-12-07 | 西安交通大学 | Heat pump distillation apparatus and process for diethyl carbonate |
| CN105384639A (en) * | 2015-11-11 | 2016-03-09 | 东营市海科新源化工有限责任公司 | Refining purifying device and method used for continuously producing battery grade dimethyl carbonate |
| CN105384639B (en) * | 2015-11-11 | 2017-07-14 | 东营市海科新源化工有限责任公司 | Refined purifying plant for continuously producing LITHIUM BATTERY dimethyl carbonate |
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