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1. 发明授权

US6444847B2 Process for preparing phosphine oxides and process for purifying the same 有权
标题翻译：制备氧化膦的方法及其纯化方法
公开(公告)号：US6444847B2
公开(公告)日：2002-09-03
申请号：US93565501
申请日：2001-08-24
申请人： MITSUI CHEMICALS INC
发明人： NOBORI TADAHITO , HARA ISAO , FUNAKI KATSUHIKO , HAYASHI TAKAOMI , SHIBAHARA ATSUSHI , KIYONO SHINJI , MIZUTANI KAZUMI , TAKAKI USAJI
IPC分类号： C07F9/535 , C07F9/02 , C07F9/22
CPC分类号： C07F9/025 , C07F9/224
摘要： A process for preparing phosphine oxides by reacting iminophosphoranes with phosphorus oxytrichloride by which highly purified phosphine oxides can be obtained industrially in a higher yield. Specifically, phosphine oxides are prepared in such a manner that iminophosphoranes are reacted with phosphorus oxytrichloride using an aprotic organic solvent with permittivity 2.2 or more at 20° C. as a solvent under special reaction conditions to give a liquid reaction product containing phosphine oxides and aminophosphonium chlorides which are yielded as a by-product at the same time as the phosphine oxides, and the above described chlorides are removed from the above described liquid reaction product by a solid-liquid separation process, and the solution having been subjected to the solid-liquid separation process is washed with water.
摘要翻译：通过使亚氨基磷腈与三氯氧化磷反应来制备氧化膦的方法，通过该方法可以以更高的产率在工业上获得高度纯化的氧化膦。具体地说，在特殊的反应条件下，使亚氨基磷腈与二氧化磷与二氯化磷反应，使用介电常数为2.2以上，介电常数为2.2以上的溶剂，作为溶剂，在特殊的反应条件下反应生成含有氧化膦和氨基鏻的液体反应产物与氧化膦同时作为副产物生成的氯化物，并且通过固液分离方法从上述液体反应产物中除去上述氯化物，并将溶液经受固体 - 液体分离过程用水洗涤。

2. 发明专利

DE60020900D1 未知
公开(公告)号：DE60020900D1
公开(公告)日：2005-07-28
申请号：DE60020900
申请日：2000-04-12
申请人： MITSUI CHEMICALS INC
发明人： NOBORI TADAHITO , SHIBAHARA ATSUSHI , KIYONO SHINJI , HAYASHI TAKAOMI , FUNAKI KATSUHIKO , HARA ISAO , MIZUTANI KAZUMI , TAKAKI USAJI
IPC分类号： C08F2/00 , C08F2/38 , C08F4/00 , C08F4/04 , C08F220/14 , C08F220/28 , C08F220/44 , C08F297/00 , C08F297/02
摘要： The present invention provides a method of preparing a polymer, which comprises subjecting a monomer containing at least a polar unsaturated compound to anionic polymerization in the presence of a phosphazenium compound represented by the formula (1): (wherein Z is an anion of an active hydrogen compound in the form where a proton is eliminated from the active hydrogen compound and transferred to the anion; a, b, c and d each represents 1 or 0, but all of them are not simultaneously 0; and R may the same or different and each represents a hydrocarbon group having 1 to 10 carbon atoms, and two R(s) on the same nitrogen atom are optionally combined each other to form a cyclic structure), or in the presence of the phosphazenium compound and the active hydrogen compound. The resulting polymer is characterized by narrow molecular weight distribution.

3. 发明专利

DE60013644T2 未知
公开(公告)号：DE60013644T2
公开(公告)日：2005-02-03
申请号：DE60013644
申请日：2000-04-12
申请人： MITSUI CHEMICALS INC
发明人： NOBORI TADAHITO , HARA ISAO , FUNAKI KATSUHIKO , HAYASHI TAKAOMI , SHIBAHARA ATSUSHI , KIYONO SHINJI , MIZUTANI KAZUMI , TAKAKI USAJI
IPC分类号： C07F9/535 , C07F9/02 , C07F9/22
摘要： The invention provides for purifying phosphine oxides which may be prepared in such a manner that iminophosphoranes are reacted with phosphorus oxytrichloride using an aprotic organic solvent with permittivity 2.2 or more at 20 DEG C as a solvent under specical reaction conditions to give a liquid reaction product containing phosphine oxides and aminophosphonium chlorides which are yielded as a by-product at the same time as the phosphine oxides. The above described chlorides are removed from the above described liquid reaction product by the solid-liquid separation process, and the solution having been subjected to the solid-liquid separation process is washed with water.

4. 发明专利

DE69808227D1 未知
公开(公告)号：DE69808227D1
公开(公告)日：2002-10-31
申请号：DE69808227
申请日：1998-12-03
申请人： MITSUI CHEMICALS INC
发明人： NOBORI TADAHITO , HAYASHI TAKAOMI , FUNAKI KATSUHIKO , SHIBAHARA ATSUSHI , HARA ISAO , KIYONO SHINJI , MIZUTANI KAZUMI , TAKAKI USAJI
IPC分类号： C07F9/06
摘要： In a process for preparing iminotris(dimethylamino)phosphorane at high purity and high yield from aminotris(dimethylamino)phosphonium chloride, Aminotris(dimethylamino)phosphonium chloride is first reacted with an aqueous solution of the hydroxide of an alkali metal or alkaline earth metal in the presence of a solvent in which the chloride and hydroxide of the alkali metal or alkaline earth metal are sparingly soluble, whereby iminotris(dimethylamino)phosphorane is formed. After water is driven off at a temperature of 70 DEG C or lower from the reaction mixture, solids are removed from the thus-concentrated reaction mixture by solid-liquid separation. The resultant mother liquor is then distilled to obtain iminotris(dimethylamino)phosphorane in high yield and of high purity.

5. 发明专利

DE60004915D1 未知
公开(公告)号：DE60004915D1
公开(公告)日：2003-10-09
申请号：DE60004915
申请日：2000-04-12
申请人： MITSUI CHEMICALS INC
发明人： NOBORI TADAHITO , HARA ISAO , FUNAKI KATSUHIKO , HAYASHI TAKAOMI , SHIBAHARA ATSUSHI , KIYONO SHINJI , MIZUTANI KAZUMI , TAKAKI USAJI
IPC分类号： C07F9/535 , C07F9/02 , C07F9/22
摘要： The invention provides for purifying phosphine oxides which may be prepared in such a manner that iminophosphoranes are reacted with phosphorus oxytrichloride using an aprotic organic solvent with permittivity 2.2 or more at 20 DEG C as a solvent under specical reaction conditions to give a liquid reaction product containing phosphine oxides and aminophosphonium chlorides which are yielded as a by-product at the same time as the phosphine oxides. The above described chlorides are removed from the above described liquid reaction product by the solid-liquid separation process, and the solution having been subjected to the solid-liquid separation process is washed with water.

6. 发明专利

DE69809696T2 未知
公开(公告)号：DE69809696T2
公开(公告)日：2003-07-31
申请号：DE69809696
申请日：1998-12-22
申请人： MITSUI CHEMICALS INC
发明人： NOBORI TADAHITO , HAYASHI TAKAOMI , FUNAKI KATSUHIKO , SHIBAHARA ATSUSHI , HARA ISAO , KIYONO SHINJI , MIZUTANI KAZUMI , TAKAKI USAJI
IPC分类号： C07F9/02 , C07F9/06
摘要： A raw material is provided which permits preparation of tetrakisÄtris(dimetHylamino)phosphoranylideneaminoÜphosphonium hydroxide by an extremely simple process. The raw material, Ätris(dimethylamino)phosphonioaminoÜtrisÄtris(dimethylamino)phosphoran ylidene aminoÜphosphonium dichloride is prepared by bringing hydrogen chloride into contact with tetrakisÄtris(dimethylamino)phosphoranylideneaminoÜphosphonium chloride and adding the former on the latter. TetrakisÄtris(dimethylamino)phosphoranylideneaminoÜphosphonium hydroxide is prepared by bringing an aqueous solution of the dichoride into contact with an OH -form ion exchange resin. A separation process, is provided in which tetrakisÄtris(dimethylamino)phosphoranylideneaminoÜphosphonium chloride is separated from solution by extracting it out, as Ätris(dimethylamino)phosphonioaminoÜtrisÄtris(dimethylamino)phosphoran ylidene aminoÜphosphonium dichloride, into a water phase. An isolation process is also provided, in which an aqueous solution of Ätris(dimethylamino)phosphonioaminoÜtrisÄtris(dimethylamino)phosphoran ylidene aminoÜphosphonium dichloride is neutralized so that tetrakisÄtris(dimethylamino)phosphoranylideneaminoÜphosph onium chloride is regenerated and precipitated as a solid.

7. 发明专利

DE69808227T2 未知
公开(公告)号：DE69808227T2
公开(公告)日：2003-01-23
申请号：DE69808227
申请日：1998-12-03
申请人： MITSUI CHEMICALS INC
发明人： NOBORI TADAHITO , HAYASHI TAKAOMI , FUNAKI KATSUHIKO , SHIBAHARA ATSUSHI , HARA ISAO , KIYONO SHINJI , MIZUTANI KAZUMI , TAKAKI USAJI
IPC分类号： C07F9/06
摘要： In a process for preparing iminotris(dimethylamino)phosphorane at high purity and high yield from aminotris(dimethylamino)phosphonium chloride, Aminotris(dimethylamino)phosphonium chloride is first reacted with an aqueous solution of the hydroxide of an alkali metal or alkaline earth metal in the presence of a solvent in which the chloride and hydroxide of the alkali metal or alkaline earth metal are sparingly soluble, whereby iminotris(dimethylamino)phosphorane is formed. After water is driven off at a temperature of 70 DEG C or lower from the reaction mixture, solids are removed from the thus-concentrated reaction mixture by solid-liquid separation. The resultant mother liquor is then distilled to obtain iminotris(dimethylamino)phosphorane in high yield and of high purity.

8. 发明专利

SG78346A1 A process for preparing an organic compounds 未知
公开(公告)号：SG78346A1
公开(公告)日：2001-02-20
申请号：SG1999001839
申请日：1999-04-15
申请人： MITSUI CHEMICALS INC
发明人： NOBORI TADAHITO , HAYASHI TAKAOMI , HARA ISAO , KIYONO SHINJI , SHIBAHARA ATSUSHI , FUNAKI KATSUHIKO
IPC分类号： C07B41/04 , C07C41/03 , C07C67/26 , C07C68/06 , C07C303/26 , C07C309/66 , C07C309/73 , C07C319/14 , C07C323/17
摘要： A process for preparing an organic compound, comprises conducting an organic reaction in the presence of a phosphine oxide represented by formula (1); where R is the same or different and each represents a hydrogen or hydrocarbon group with 1 to 10 carbon atoms, and x is the amount of water as a molar ratio which is 0 to 5.0. The phosphine oxide can exhibit a high catalytic performance, especially in organic reactions involving alkylene oxides.

9. 发明专利

ID25576A 未知
公开(公告)号：ID25576A
公开(公告)日：2000-10-19
申请号：ID20000287
申请日：2000-04-13
申请人： MITSUI CHEMICALS INC
发明人： NOBORI TADAHITO , SHIBAHARA ATSUSHI , KIYONO SHINJI , HAYASHI TAKAOMI , FUNAKI KATSUHIKO , HARA ISAO , MIZUTANI KAZUMI , TAKAKI USAJI
IPC分类号： C08G63/82 , C08G69/20

10. 发明专利

ID22463A 未知
公开(公告)号：ID22463A
公开(公告)日：1999-10-21
申请号：ID990346
申请日：1999-04-16
申请人： MITSUI CHEMICALS INC
发明人： HAYASHI TAKAOMI , FUNAKI KATSUHIKO , SHIBAHARA ATSUSHI , MIZUTANI KAZUMI , HARA ISAO , KIYONO SHINJI , NOBORI TADAHITO , TAKAKI USAJI
IPC分类号： C08G65/10 , C08G65/26 , C08G65/28
摘要： Poly(alkylene oxide) which does not contain any metallic component and does not leave an odor is prepared simply and efficiently, by a process using a polymerization initiator which does not cause any problems in preparing and handling in the preparation of the polyalkylene oxide by polymerizing an alkylene oxide compound, and does not require special treatment before the initiation of the polymerization. In the process, the alkylene oxide compound is polymerized in the presence of a phosphine oxide compound represented by the formula (1): wherein Rs are the same or different and each represents a hydrocarbon group having 1 to 10 carbon atoms, and x represents an amount of water molecules contained in terms of a molar ratio and is within a range from 0 to 5.0. If desired, the alkylene oxide compound can be polymerized in the presence of said phosphine oxide compound and an active hydrogen compound selected from water or an organic compound having a partial structural formula -OH or -NH-.

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