CN104774162A - 一种制备硫酸二乙酯的方法 - Google Patents
一种制备硫酸二乙酯的方法 Download PDFInfo
- Publication number
- CN104774162A CN104774162A CN201410009115.7A CN201410009115A CN104774162A CN 104774162 A CN104774162 A CN 104774162A CN 201410009115 A CN201410009115 A CN 201410009115A CN 104774162 A CN104774162 A CN 104774162A
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- CN
- China
- Prior art keywords
- conversion zone
- ethyl sulfate
- sulfuric acid
- cooling section
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000000034 method Methods 0.000 title claims abstract description 52
- DENRZWYUOJLTMF-UHFFFAOYSA-N diethyl sulfate Chemical compound CCOS(=O)(=O)OCC DENRZWYUOJLTMF-UHFFFAOYSA-N 0.000 title abstract 4
- 229940008406 diethyl sulfate Drugs 0.000 title abstract 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 84
- KIWBPDUYBMNFTB-UHFFFAOYSA-N Ethyl hydrogen sulfate Chemical compound CCOS(O)(=O)=O KIWBPDUYBMNFTB-UHFFFAOYSA-N 0.000 claims abstract description 78
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000004821 distillation Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000002699 waste material Substances 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims description 47
- 239000012295 chemical reaction liquid Substances 0.000 claims description 46
- 238000002360 preparation method Methods 0.000 claims description 18
- ROAYSRAUMPWBQX-UHFFFAOYSA-N ethanol;sulfuric acid Chemical compound CCO.OS(O)(=O)=O ROAYSRAUMPWBQX-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- DIMZOVQGUDDSHG-UHFFFAOYSA-N ethene;sulfuric acid Chemical group C=C.OS(O)(=O)=O DIMZOVQGUDDSHG-UHFFFAOYSA-N 0.000 claims description 9
- 239000010808 liquid waste Substances 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 78
- 239000002253 acid Substances 0.000 abstract description 22
- 239000007789 gas Substances 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 abstract 3
- 229960004756 ethanol Drugs 0.000 description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- 238000002156 mixing Methods 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 6
- 239000011541 reaction mixture Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- -1 chlorsulfonic acid-Ethanol Chemical compound 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 239000002274 desiccant Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- VGUWZCUCNQXGBU-UHFFFAOYSA-N 3-[(4-methylpiperazin-1-yl)methyl]-5-nitro-1h-indole Chemical compound C1CN(C)CCN1CC1=CNC2=CC=C([N+]([O-])=O)C=C12 VGUWZCUCNQXGBU-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 239000012021 ethylating agents Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- CJDBRJYSNOSEER-UHFFFAOYSA-N S(=O)(=O)(Cl)Cl.C(C)O Chemical compound S(=O)(=O)(Cl)Cl.C(C)O CJDBRJYSNOSEER-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000006200 ethylation reaction Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
Description
Claims (5)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410009115.7A CN104774162B (zh) | 2014-01-09 | 2014-01-09 | 一种制备硫酸二乙酯的方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410009115.7A CN104774162B (zh) | 2014-01-09 | 2014-01-09 | 一种制备硫酸二乙酯的方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104774162A true CN104774162A (zh) | 2015-07-15 |
| CN104774162B CN104774162B (zh) | 2017-02-08 |
Family
ID=53615967
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410009115.7A Active CN104774162B (zh) | 2014-01-09 | 2014-01-09 | 一种制备硫酸二乙酯的方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104774162B (zh) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020121926A (ja) * | 2019-01-29 | 2020-08-13 | セントラル硝子株式会社 | 含フッ素エーテルの製造方法 |
| CN112194601A (zh) * | 2019-07-08 | 2021-01-08 | 杉杉新材料（衢州）有限公司 | 一种合成硫酸单烃基酯盐衍生物的方法 |
| CN115028555A (zh) * | 2022-07-04 | 2022-09-09 | 武汉青江化工黄冈有限公司 | 一种硫酸二乙酯连续合成工艺 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB175077A (en) * | 1920-11-12 | 1922-02-13 | British Cellulose And Chemical | Improvements in or relating to the manufacture of dialkyl sulphates |
| JPS5182237A (en) * | 1975-01-16 | 1976-07-19 | Nippon Soda Co | 4*4** jikurofuenirusurupponnoseizojiniokeru jimechiruryusannokaishuhoho |
| CN1760179A (zh) * | 2004-10-12 | 2006-04-19 | 山东新华万博化工有限公司 | 硫酸二甲酯的制备工艺 |
| CN101654420A (zh) * | 2008-08-20 | 2010-02-24 | 湖北富驰化工医药股份有限公司 | 复合酸催化脱水制备硫酸二甲酯的生产工艺 |
| CN203247215U (zh) * | 2012-12-26 | 2013-10-23 | 山东兴辉化工有限公司 | 硫酸二甲酯生产余热回收系统 |
-
2014
- 2014-01-09 CN CN201410009115.7A patent/CN104774162B/zh active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB175077A (en) * | 1920-11-12 | 1922-02-13 | British Cellulose And Chemical | Improvements in or relating to the manufacture of dialkyl sulphates |
| JPS5182237A (en) * | 1975-01-16 | 1976-07-19 | Nippon Soda Co | 4*4** jikurofuenirusurupponnoseizojiniokeru jimechiruryusannokaishuhoho |
| CN1760179A (zh) * | 2004-10-12 | 2006-04-19 | 山东新华万博化工有限公司 | 硫酸二甲酯的制备工艺 |
| CN101654420A (zh) * | 2008-08-20 | 2010-02-24 | 湖北富驰化工医药股份有限公司 | 复合酸催化脱水制备硫酸二甲酯的生产工艺 |
| CN203247215U (zh) * | 2012-12-26 | 2013-10-23 | 山东兴辉化工有限公司 | 硫酸二甲酯生产余热回收系统 |
Non-Patent Citations (2)
| Title |
|---|
| 朱建军等: "硫酸二乙酯的合成", 《化工设计》 * |
| 李忠铭: "硫酸二乙酯的合成", 《湖北化工》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020121926A (ja) * | 2019-01-29 | 2020-08-13 | セントラル硝子株式会社 | 含フッ素エーテルの製造方法 |
| JP7181463B2 (ja) | 2019-01-29 | 2022-12-01 | セントラル硝子株式会社 | 含フッ素エーテルの製造方法 |
| CN112194601A (zh) * | 2019-07-08 | 2021-01-08 | 杉杉新材料（衢州）有限公司 | 一种合成硫酸单烃基酯盐衍生物的方法 |
| CN115028555A (zh) * | 2022-07-04 | 2022-09-09 | 武汉青江化工黄冈有限公司 | 一种硫酸二乙酯连续合成工艺 |
| CN115028555B (zh) * | 2022-07-04 | 2023-09-29 | 武汉青江化工黄冈有限公司 | 一种硫酸二乙酯连续合成工艺 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104774162B (zh) | 2017-02-08 |
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Address after: 271000 Shandong city of Tai'an province Dawenkou gypsum Industrial Park Patentee after: TAIAN HANWEI GROUP Co.,Ltd. Address before: 271000 Shandong city of Binzhou province Tai'an Dawenkou gypsum Industrial Park Patentee before: TAIAN HAVAY CHEMICALS Co.,Ltd. |
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Denomination of invention: Method used for preparing diethyl sulfate Effective date of registration: 20200521 Granted publication date: 20170208 Pledgee: Bank of Tai'an Limited by Share Ltd. Pledgor: TAIAN HANWEI GROUP Co.,Ltd. Registration number: Y2020990000498 |
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Denomination of invention: A method for preparing diethyl sulfate Effective date of registration: 20230529 Granted publication date: 20170208 Pledgee: Taixi sub branch of Taian Bank Co.,Ltd. Pledgor: TAIAN HANWEI GROUP Co.,Ltd. Registration number: Y2023980042185 |
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