CN108003020A - A kind of method for preparing diethy-aceto oxalate as solvent with toluene - Google Patents
A kind of method for preparing diethy-aceto oxalate as solvent with toluene Download PDFInfo
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- CN108003020A CN108003020A CN201711442388.0A CN201711442388A CN108003020A CN 108003020 A CN108003020 A CN 108003020A CN 201711442388 A CN201711442388 A CN 201711442388A CN 108003020 A CN108003020 A CN 108003020A
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- CN
- China
- Prior art keywords
- toluene
- ethanol
- diethy
- aceto oxalate
- solvent
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of method for preparing diethy-aceto oxalate as solvent with toluene, industrial ethanedioic acid, ethanol, toluene are used as raw material, it is made by point water benefit ethanol that feeds, heats up, survey acid, steaming toluene, cooling, vacuum distillation step, the present invention substitutes benzene with toluene, and toluene has insoluble in water, can be with the property of molten ethanol, hypotoxicity, than benzene more resistant to jelly, band outlet capacity is stronger than benzene, makes preparing for diethy-aceto oxalate more environmentally friendly green, pollution-free, improves the production efficiency and yield of diethy-aceto oxalate.
Description
Technical field
The invention belongs to chemical solvent to utilize field, and in particular to a kind of side for preparing diethy-aceto oxalate as solvent with toluene
Method.
Background technology
For diethy-aceto oxalate mainly by being produced with technique of the benzene with water, its technique mainly utilizes benzene and water not at present
Principle that is molten but can dissolving each other with ethanol, a certain amount of oxalic acid, ethanol, benzene are added in reactor, by the physico-chemical property of benzene,
Oxalic acid and ethanol is set to react at a certain temperature, water and the benzene of generation reach azeotropic point, and water is taken out of, so that oxalic acid can with ethanol
The reaction was continued, generates diethy-aceto oxalate.
However, benzene has carcinogenic toxicity, strong toxicity is high to human injury, is unfavorable for prolonged Chemical Manufacture, with environmental protection
Requirement, it is necessary to which the more preferable solvent of environment-friendly function is substituted.
The content of the invention
It is an object of the invention to provide it is a kind of it is environmentally protective, toxicity is low, the high toluene of product yield makees solvent preparation
The method of diethy-aceto oxalate.
The technical solution adopted by the present invention to solve the technical problems is：One kind prepares diethy-aceto oxalate with toluene as solvent
Method, comprise the following steps：
1) feed：Successively by 800kg industrial ethanedioic acids, 1000L ethanol, 1100L toluene solvants input reaction kettle；
2) heating divides water to mend ethanol：Return valve is opened, heating adds 600L ethanol when dividing water to 84 DEG C, continues a point water；
150L ethanol is added when temperature rises to 85 DEG C, continues a point water；When temperature is to 86 DEG C, 150L ethanol is added, continues a point water；
3) acid is surveyed：When temperature is to 96 DEG C, acid is surveyed in sampling, starts to steam toluene when acidity is less than 1.5%；If acidity is high
In 1.5%, added by acidity * 2000L ethanol；
4) toluene is steamed：Start to steam toluene after acidity detection is qualified, to stopping distillation at 140 DEG C；
5) cool down：After steaming toluene, thick ester is obtained with circulating water cooling to less than 80 DEG C blowings；
6) vacuum distillation：Put thick ester into rectifying still, adjustment vacuum to more than 0.95MPa, heating, starts negative pressure essence
Evaporate, collect 45~108 DEG C of solution and do and evaporates head, collected and started to adopt finished product diethy-aceto oxalate after evaporating head, when temperature of reaction kettle extremely
Stop adopting finished product at 140 DEG C, rectifying terminates.
Specifically, the mass fraction of the ethanol is 85%.
The ester-containing amount of diethy-aceto oxalate obtained in the step 6) is more than 99%, and yield is more than 93%.
The invention has the advantages that：The present invention substitutes benzene with toluene, and toluene has insoluble in water, can be with molten ethanol
Property, hypotoxicity, than benzene more resistant to jelly, band outlet capacity is stronger than benzene, makes preparing for diethy-aceto oxalate more environmentally friendly green, pollution-free,
Improve the production efficiency and yield of diethy-aceto oxalate.
Embodiment
It is the specific embodiment of the present invention below, technical scheme is described further, but the present invention
Protection domain is not limited to these embodiments.It is every to be included in the present invention without departing substantially from the change of present inventive concept or equivalent substitute
Protection domain within.
800kg oxalic acid is put into synthesis reactor, is finished after oxalic acid respectively from ethanol head tank and toluene head tank by 1000L
Mass fraction is that 85% ethanol and 1100L toluene are knocked down in synthesis reactor, and valve kettle mouth is shut after the completion of charging, opens steam valve
Door heating divides water, opens return valve, and temperature in the kettle adds 600L ethanol, continue a point water to ethanol head tank is opened at 84 DEG C；
When temperature is to 85 DEG C, 150L ethanol is added, continues a point water；When temperature is to 86 DEG C, 150L ethanol is added, continues a point water；When
Acid is surveyed in temperature to sampling at 96 DEG C, starts to steam toluene when acidity is less than 1.5%, if acidity is higher than 1.5%, by acidity *
2000L ethanol is added, and after qualified, steamed toluene temperature and is stopped steaming toluene to 140 DEG C, with circulating water cooling to 80 DEG C with decentralization
Material.
Put thick ester into rectifying still, pulling vacuum to more than 0.95MPa, heating, starts negative pressure rectifying, collects 45~108 DEG C
Solution do and evaporate head, collected and started to adopt finished product diethy-aceto oxalate after evaporating head, stopped adopting into when temperature of reaction kettle is to 140 DEG C
Product, rectifying terminate.The ester-containing amount of diethy-aceto oxalate of preparation is more than 99%, and yield is more than 93%.
Claims (3)
- A kind of 1. method for preparing diethy-aceto oxalate as solvent with toluene, it is characterised in that comprise the following steps：1) feed：Successively by 800kg industrial ethanedioic acids, 1000L ethanol, 1100L toluene solvants input reaction kettle；2) heating divides water to mend ethanol：Return valve is opened, heating adds 600L ethanol when dividing water to 84 DEG C, continues a point water；Work as temperature Degree adds 150L ethanol when rising to 85 DEG C, continues a point water；When temperature is to 86 DEG C, 150L ethanol is added, continues a point water；3) acid is surveyed：When temperature is to 96 DEG C, acid is surveyed in sampling, starts to steam toluene when acidity is less than 1.5%；If acidity is higher than 1.5%, added by acidity * 2000L ethanol；4) toluene is steamed：Start to steam toluene after acidity detection is qualified, to stopping distillation at 140 DEG C；5) cool down：After steaming toluene, thick ester is obtained with circulating water cooling to less than 80 DEG C blowings；6) vacuum distillation：Put thick ester into rectifying still, adjustment vacuum to more than 0.95MPa, heating, starts negative pressure rectifying, receives The solution of 45~108 DEG C of collection, which is done, evaporates head, has collected and has started to adopt finished product diethy-aceto oxalate after evaporating head, when temperature of reaction kettle is to 140 DEG C When stop adopt finished product, rectifying terminates.
- 2. prepare the method for diethy-aceto oxalate as solvent with toluene as claimed in claim 1, it is characterised in that the ethanol Mass fraction is 85%.
- 3. prepare the method for diethy-aceto oxalate as solvent with toluene as claimed in claim 1, it is characterised in that the step 6) In the obtained ester-containing amount of diethy-aceto oxalate be more than 99%, yield is more than 93%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711442388.0A CN108003020A (en) | 2017-12-27 | 2017-12-27 | A kind of method for preparing diethy-aceto oxalate as solvent with toluene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711442388.0A CN108003020A (en) | 2017-12-27 | 2017-12-27 | A kind of method for preparing diethy-aceto oxalate as solvent with toluene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108003020A true CN108003020A (en) | 2018-05-08 |
Family
ID=62061725
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711442388.0A Pending CN108003020A (en) | 2017-12-27 | 2017-12-27 | A kind of method for preparing diethy-aceto oxalate as solvent with toluene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108003020A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4138587A (en) * | 1976-07-27 | 1979-02-06 | Ube Industries, Ltd. | Process for the preparation of dialkyl oxalates |
-
2017
- 2017-12-27 CN CN201711442388.0A patent/CN108003020A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4138587A (en) * | 1976-07-27 | 1979-02-06 | Ube Industries, Ltd. | Process for the preparation of dialkyl oxalates |
Non-Patent Citations (3)
| Title |
|---|
| 江体乾主编: "《化工工艺手册》", 29 February 1992, 上海科学技术出版社 * |
| 郭三阳: "一次酯化法生产草酸二乙酯的工艺探讨", 《湖南化工》 * |
| 陈力: "反应精馏耦合合成和水解草酸二乙酯工艺研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180508 |