CN1237067C - 磷酸三乙酯的制备 - Google Patents
磷酸三乙酯的制备 Download PDFInfo
- Publication number
- CN1237067C CN1237067C CNB021524394A CN02152439A CN1237067C CN 1237067 C CN1237067 C CN 1237067C CN B021524394 A CNB021524394 A CN B021524394A CN 02152439 A CN02152439 A CN 02152439A CN 1237067 C CN1237067 C CN 1237067C
- Authority
- CN
- China
- Prior art keywords
- ethanol
- reaction
- distillation
- tower
- weight
- 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.)
- Expired - Fee Related
Links
- 238000002360 preparation method Methods 0.000 title description 4
- UCQFCFPECQILOL-UHFFFAOYSA-N diethyl hydrogen phosphate Chemical compound CCOP(O)(=O)OCC UCQFCFPECQILOL-UHFFFAOYSA-N 0.000 title description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 86
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011541 reaction mixture Substances 0.000 claims abstract description 13
- 238000010992 reflux Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 46
- 238000005406 washing Methods 0.000 claims description 36
- 238000004821 distillation Methods 0.000 claims description 35
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 22
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 22
- 238000009833 condensation Methods 0.000 claims description 10
- 230000005494 condensation Effects 0.000 claims description 10
- 238000005194 fractionation Methods 0.000 claims description 7
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000010943 off-gassing Methods 0.000 abstract 2
- 238000010533 azeotropic distillation Methods 0.000 abstract 1
- 229960004756 ethanol Drugs 0.000 description 32
- 239000000047 product Substances 0.000 description 21
- 239000000203 mixture Substances 0.000 description 16
- 239000002253 acid Substances 0.000 description 7
- 230000001476 alcoholic effect Effects 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 241000282326 Felis catus Species 0.000 description 5
- 239000013505 freshwater Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000007872 degassing Methods 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000012043 crude product Substances 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000008396 flotation agent Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012264 purified product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000003351 stiffener Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000005068 transpiration Effects 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/11—Esters of phosphoric acids with hydroxyalkyl compounds without further substituents on alkyl
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10158135 | 2001-11-27 | ||
| DE10158135.1 | 2001-11-27 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1421448A CN1421448A (zh) | 2003-06-04 |
| CN1237067C true CN1237067C (zh) | 2006-01-18 |
Family
ID=7707117
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021524394A Expired - Fee Related CN1237067C (zh) | 2001-11-27 | 2002-11-27 | 磷酸三乙酯的制备 |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US6673955B2 (und) |
| JP (1) | JP2003160591A (und) |
| CN (1) | CN1237067C (und) |
| DE (1) | DE10253212A1 (und) |
| GB (1) | GB2383795B (und) |
| RU (1) | RU2002131713A (und) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100549130C (zh) * | 2006-01-26 | 2009-10-14 | 江苏雅克化工有限公司 | Tcpp阻燃剂制备方法 |
| CN101775031B (zh) * | 2009-12-22 | 2012-08-29 | 江苏雅克科技股份有限公司 | Tcpp阻燃剂制备方法 |
| CN101941988B (zh) * | 2010-03-04 | 2012-06-27 | 浙江医药股份有限公司维生素厂 | 磷酸二乙酯钠制备磷酸三乙酯的工艺 |
| CN101891761B (zh) * | 2010-07-19 | 2012-07-04 | 吉林大学 | 相转移催化合成磷酸三乙酯的方法 |
| CN102206230B (zh) * | 2011-04-02 | 2014-12-10 | 吉林市永林化工有限公司 | 磷酸三乙酯制备方法 |
| CN102675359B (zh) * | 2012-05-22 | 2015-03-11 | 江苏雅克科技股份有限公司 | 一种制备磷酸三乙酯的方法 |
| CN104447855B (zh) * | 2013-09-18 | 2017-06-06 | 中国石油天然气股份有限公司 | 一种磷酸三乙酯粗品的精馏方法 |
| CN104892666B (zh) * | 2015-06-26 | 2017-03-01 | 四川中萃化工有限公司 | 一种高纯磷酸三丁酯的制备方法 |
| CN105859770B (zh) * | 2016-05-09 | 2019-03-22 | 云南云天化以化磷业研究技术有限公司 | 一种合成磷酸烷基酯的方法 |
| DE102016210484A1 (de) * | 2016-06-14 | 2017-12-14 | Evonik Degussa Gmbh | Verfahren zur Entfeuchtung von feuchten Gasgemischen |
| CN114057787A (zh) * | 2021-11-25 | 2022-02-18 | 浙江万盛股份有限公司 | 一种磷酸三乙酯的制备方法 |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE541145C (de) | 1927-10-13 | 1932-01-14 | I G Farbenindustrie Akt Ges | Verfahren zur Herstellung von Phosphorsaeureestern aliphatischer Alkohole |
| DE899498C (de) | 1944-06-25 | 1954-06-21 | Basf Ag | Verfahren zur Herstellung des Phosphorsaeuretri-(2-aethyl-n-hexyl)-esters |
| JPS5025457B1 (und) * | 1970-10-20 | 1975-08-23 | ||
| JP3323611B2 (ja) | 1993-06-25 | 2002-09-09 | 株式会社日立製作所 | Ｖｔｒ用周波数変換装置 |
| DE19910463B4 (de) * | 1998-03-18 | 2007-05-10 | Lanxess Deutschland Gmbh | Dialkylphosphorsäuren nach der Methanol-Methode |
-
2002
- 2002-11-15 DE DE10253212A patent/DE10253212A1/de not_active Withdrawn
- 2002-11-20 GB GB0227114A patent/GB2383795B/en not_active Expired - Fee Related
- 2002-11-21 JP JP2002337621A patent/JP2003160591A/ja not_active Withdrawn
- 2002-11-22 US US10/302,543 patent/US6673955B2/en not_active Expired - Fee Related
- 2002-11-26 RU RU2002131713/04A patent/RU2002131713A/ru not_active Application Discontinuation
- 2002-11-27 CN CNB021524394A patent/CN1237067C/zh not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1421448A (zh) | 2003-06-04 |
| US6673955B2 (en) | 2004-01-06 |
| GB2383795B (en) | 2004-12-08 |
| RU2002131713A (ru) | 2004-11-27 |
| US20030100788A1 (en) | 2003-05-29 |
| DE10253212A1 (de) | 2003-06-05 |
| GB0227114D0 (en) | 2002-12-24 |
| JP2003160591A (ja) | 2003-06-03 |
| GB2383795A (en) | 2003-07-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1237067C (zh) | 磷酸三乙酯的制备 | |
| CA2234155C (en) | Method for continuously producing a dialkyl carbonate and a diol | |
| US8664453B2 (en) | Multi-stage process and apparatus for recovering dichlorohydrins | |
| EP0984918B1 (en) | Processes for refining butylacrylate | |
| TWI490193B (zh) | 用於二氯丙醇的共沸回收之方法與設備 | |
| EP0390577B1 (en) | Purification and preparation processes for methyl methacrylate | |
| CN1164528A (zh) | (甲基)丙烯酸烷基酯的连续制备方法 | |
| CN102206230B (zh) | 磷酸三乙酯制备方法 | |
| CN1064663C (zh) | 二甲醚和氯甲烷混合物的制备及用水作萃取剂的分馏方法 | |
| CN105050997B (zh) | 通过酯交换制造丙烯酸2‑丙基庚酯的方法 | |
| CN101125795A (zh) | 一种甲酸的制备方法 | |
| US8969601B2 (en) | Method for preparing chlorohydrins composition and method for preparing epichlorohydrin using chlorohydrins composition prepared thereby | |
| US8969631B2 (en) | Method for preparing chlorohydrins composition and method for preparing epichlorohydrin using chlorohydrins composition prepared thereby | |
| CN101357880A (zh) | 一种甘油与氯化氢自催化反应制备二氯丙醇的工艺及系统 | |
| CN100345816C (zh) | 用于进行平衡限制反应的方法 | |
| CN109851490A (zh) | 醋酐催化法连续生产氯乙酸的工艺 | |
| US9035108B2 (en) | Method for preparing chlorohydrins composition and method for preparing epichlorohydrin using chlorohydrins composition prepared thereby | |
| KR100339973B1 (ko) | 메틸아세테이트의 가수분해 방법 및 장치 | |
| US20020177728A1 (en) | Refining processes | |
| US8916732B2 (en) | Method for preparing chlorohydrins and method for preparing epichlorohydrin using chlorohydrins prepared thereby | |
| CN110746453A (zh) | 一种亚磷酸二甲酯的生产工艺及生产装置 | |
| CN100389074C (zh) | N-膦酰基甲基亚氨基二乙酸生产废液中盐酸的回收分离方法 | |
| RU2127252C1 (ru) | Способ получения н-бутилацетата | |
| CN116272736A (zh) | 一种马来酸二乙酯的连续生产方法 | |
| CN115259998A (zh) | 一种适于工业化生产的三溴新戊醇的制备方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |