公开(公告)号：US06177593B1

公开(公告)日：2001-01-23

申请号：US09216864

申请日：1998-12-21

申请人： Tadahito Nobori ,  Takaomi Hayashi ,  Katsuhiko Funaki ,  Atsushi Shibahara ,  Isao Hara ,  Shinji Kiyono ,  Kazumi Mizutani ,  Usaji Takaki

发明人： Tadahito Nobori ,  Takaomi Hayashi ,  Katsuhiko Funaki ,  Atsushi Shibahara ,  Isao Hara ,  Shinji Kiyono ,  Kazumi Mizutani ,  Usaji Takaki

IPC分类号： C07F902

CPC分类号： C07F9/065

摘要： The compound [tris(dimethylamino)phosphonioamino]tris[tris(dimethylamino)phosphoranylideneamino]phosphonium dichloride can be prepared by contacting hydrogen chloride with tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium chloride. The phosphonium dichloride compound can be used in a process wherein it is brought into contact with an OH−-form ion exchange resin to prepare tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium hydroxide. Separate processes for separating or isolating the phosphonium chloride compound or isolating the phosphonium hydroxide compound from feed solutions wherein an extraction step is used are also set forth.

摘要翻译： 化合物[三（二甲基氨基）膦酰氨基]三[三（二甲基氨基）亚正膦基氨基]二氯化鏻可以通过使氯化氢与四[三（二甲基氨基）正膦亚基氨基]鏻氯化物接触来制备。 二氯化鏻化合物可以在与OH型离子交换树脂接触以制备四[三（二甲基氨基）正膦亚基氨基]鏻氢氧化物的方法中使用。 还提出了分离或分离氯化鏻化合物或从使用提取步骤的进料溶液中分离氢氧化鏻的分离方法。

公开(公告)号：US06255537B1

公开(公告)日：2001-07-03

申请号：US09289990

申请日：1999-04-13

申请人： Takaomi Hayashi ,  Katsuhiko Funaki ,  Atsushi Shibahara ,  Kazumi Mizutani ,  Isao Hara ,  Shinji Kiyono ,  Tadahito Nobori ,  Usaji Takaki

发明人： Takaomi Hayashi ,  Katsuhiko Funaki ,  Atsushi Shibahara ,  Kazumi Mizutani ,  Isao Hara ,  Shinji Kiyono ,  Tadahito Nobori ,  Usaji Takaki

IPC分类号： C07C4313

CPC分类号： C08G65/2675 ,  C08G65/10 ,  C08G65/2663

摘要： There is provided a process for preparing a poly(alkylene oxide) by using a polymerization initiator which does not cause any problem on preparing and handling in the preparation of the polyalkylene oxide by polymerizing an alkylene oxide compound and does not require a special treatment before the initiation of the polymerization. That is, it is a process of polymerizing the alkylene oxide compound in the presence of a phosphine oxide compound represented by the formula (1): wherein R is 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, or 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—.

摘要翻译： 提供了一种通过使用聚合引发剂制备聚（环氧烷）的方法，该聚合引发剂在通过聚合烯化氧化合物制备聚环氧烷的制备和处理中不会引起任何问题，并且不需要在 引发聚合。 也就是说，它是在式（1）表示的氧化膦化合物存在下使烯化氧化合物聚合的方法：其中R相同或不同，各自代表具有1-10个碳原子的烃基，和 x表示以摩尔比表示的水分子的含量，在0〜5.0的范围内，或在所述氧化膦化合物和活性氢化合物存在下，选自水或具有部分结构式的有机化合物 -OH或-NH-。

公开(公告)号：US6153794A

公开(公告)日：2000-11-28

申请号：US348586

申请日：1999-07-07

申请人： Katsuhiko Funaki ,  Isao Hara ,  Takaomi Hayashi ,  Shinji Kiyono ,  Atsushi Shibahara ,  Kazumi Mizutani ,  Tadahito Nobori ,  Usaji Takaki

发明人： Katsuhiko Funaki ,  Isao Hara ,  Takaomi Hayashi ,  Shinji Kiyono ,  Atsushi Shibahara ,  Kazumi Mizutani ,  Tadahito Nobori ,  Usaji Takaki

IPC分类号： C07F9/53 ,  C07F9/06 ,  C07F9/22 ,  C08G65/26 ,  C07C43/11 ,  C07C69/76

CPC分类号： C07F9/224 ,  C07F9/065 ,  C08G65/2675

摘要： An organic compound which is basic and soluble in an organic solvent, does not have a problem in preparation or handling and exhibits catalytic activity as a basic compound, i.e., a phosphine sulfide represented by formula (1), and a manufacturing process therefor, i.e., manufacturing a phosphine sulfide represented by formula (1), by reacting one molecule of thiophosphoryl chloride with three molecules of a phosphorane represented by formula (2). The phosphine sulfide can be used in a process for effectively manufacturing a poly(alkylene oxide) by polymerizing an alkylene oxide in the presence of the phosphine sulfide or of the phosphine sulfide and an active hydrogen compound selected from water and organic compounds having a partial structure of --OH or --NH--; and 2) a process for manufacturing a 1,2-dioxyethane derivative from an epoxy compound, i.e, manufacturing a 1,2-dioxyethane derivative by reacting an epoxy compound with a carboxylate, carboxylic anhydride, carbonate or phenol compound, respectively, in the presence of the phosphine sulfide.

摘要翻译： 碱性且可溶于有机溶剂的有机化合物在制备或处理中没有问题，并且表现出作为碱性化合物的催化活性，即由式（1）表示的硫化膦及其制备方法，即 制备由式（1）表示的硫化膦，通过使一分子的硫代磷酰氯与由式（2）表示的三价分子的三分子反应。 所述硫化膦可用于通过在硫化膦或硫化氢存在下聚合烯化氧和选自水和具有部分结构的有机化合物的活性氢化合物来有效制造聚（环氧烷）的方法 的-OH或-NH-; 和2）由环氧化合物制造1,2-二氧乙烷衍生物的方法，即分别通过使环氧化合物与羧酸酯，羧酸酐，碳酸酯或酚化合物反应制备1,2-二氧乙烷衍生物 硫化磷的存在。

公开(公告)号：US6130346A

公开(公告)日：2000-10-10

申请号：US289989

申请日：1999-04-13

申请人： Tadahito Nobori ,  Takaomi Hayashi ,  Isao Hara ,  Shinji Kiyono ,  Atsushi Shibahara ,  Katsuhiko Funaki ,  Tatsuhiro Urakami ,  Keisuke Takuma ,  Usaji Takaki

发明人： Tadahito Nobori ,  Takaomi Hayashi ,  Isao Hara ,  Shinji Kiyono ,  Atsushi Shibahara ,  Katsuhiko Funaki ,  Tatsuhiro Urakami ,  Keisuke Takuma ,  Usaji Takaki

IPC分类号： C07B41/04 ,  C07C41/03 ,  C07C67/26 ,  C07C68/06 ,  C07C303/26 ,  C07C309/66 ,  C07C309/73 ,  C07C319/14 ,  C07C323/17 ,  C07C68/00

CPC分类号： C07C319/14 ,  C07B41/04 ,  C07C303/26 ,  C07C41/03 ,  C07C67/26 ,  C07C68/06 ,  C07C2101/14 ,  C07C2102/42

摘要： A process for preparing an organic compound, comprising conducting an organic reaction in the presence of a phosphine oxide represented by formula (1); ##STR1## where R.sup.1 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, exhibiting a high catalytic performance especially in an organic reaction involving an alkylene oxide.

摘要翻译： 一种制备有机化合物的方法，包括在由式（1）表示的氧化膦存在下进行有机反应; 其中R1相同或不同，并且各自表示氢或具有1-10个碳原子的烃基，x是摩尔比为0至5.0的水的量，表现出高的催化性能，特别是在涉及 环氧烷。

公开(公告)号：US06528599B1

公开(公告)日：2003-03-04

申请号：US09549037

申请日：2000-04-13

申请人： Tadahito Nobori ,  Atsushi Shibahara ,  Shinji Kiyono ,  Takaomi Hayashi ,  Katsuhiko Funaki ,  Isao Hara ,  Kazumi Mizutani ,  Usaji Takaki

发明人： Tadahito Nobori ,  Atsushi Shibahara ,  Shinji Kiyono ,  Takaomi Hayashi ,  Katsuhiko Funaki ,  Isao Hara ,  Kazumi Mizutani ,  Usaji Takaki

IPC分类号： C08H200

CPC分类号： C08F297/00 ,  C08F2/38 ,  C08F4/00 ,  C08F220/14 ,  C08F220/28 ,  C08F220/44 ,  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.

摘要翻译： 本发明提供一种制备聚合物的方法，该方法包括在式（1）表示的磷氮烯基鏻化合物的存在下使至少含有极性不饱和化合物的单体进行阴离子聚合:(其中Z-为 活性氢化合物以质子从活性氢化合物中除去并转移到阴离子的形式; a，b，c和d各自表示1或0，但它们都不同时为0; R可以相同或不同， 不同且各自表示具有1-10个碳原子的烃基，并且相同氮原子上的两个R（s）任选地相互结合形成环状结构），或者在磷氮烯基鏻化合物和活性氢化合物 。 所得聚合物的特征在于分子量分布窄。

公开(公告)号：US06444847B1

公开(公告)日：2002-09-03

申请号：US09935655

申请日：2001-08-24

申请人： Tadahito Nobori ,  Isao Hara ,  Katsuhiko Funaki ,  Takaomi Hayashi ,  Atsushi Shibahara ,  Shinji Kiyono ,  Kazumi Mizutani ,  Usaji Takaki

发明人： Tadahito Nobori ,  Isao Hara ,  Katsuhiko Funaki ,  Takaomi Hayashi ,  Atsushi Shibahara ,  Shinji Kiyono ,  Kazumi Mizutani ,  Usaji Takaki

IPC分类号： C07F922

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.

公开(公告)号：US06303815B1

公开(公告)日：2001-10-16

申请号：US09548624

申请日：2000-04-13

申请人： Tadahito Nobori ,  Isao Hara ,  Katsuhiko Funaki ,  Takaomi Hayashi ,  Atsushi Shibahara ,  Shinji Kiyono ,  Kazumi Mizutani ,  Usaji Takaki

发明人： Tadahito Nobori ,  Isao Hara ,  Katsuhiko Funaki ,  Takaomi Hayashi ,  Atsushi Shibahara ,  Shinji Kiyono ,  Kazumi Mizutani ,  Usaji Takaki

IPC分类号： C07F922

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。

公开(公告)号：US6090980A

公开(公告)日：2000-07-18

申请号：US201655

申请日：1998-12-01

申请人： Tadahito Nobori ,  Takaomi Hayashi ,  Katsuhiko Funaki ,  Atsushi Shibahara ,  Isao Hara ,  Shinji Kiyono ,  Kazumi Mizutani ,  Usaji Takaki

发明人： Tadahito Nobori ,  Takaomi Hayashi ,  Katsuhiko Funaki ,  Atsushi Shibahara ,  Isao Hara ,  Shinji Kiyono ,  Kazumi Mizutani ,  Usaji Takaki

IPC分类号： C07F9/06

CPC分类号： C07F9/065

摘要： A process is provided 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 dissolved off at a temperature of 70.degree. 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.

摘要翻译： 提供了从氨基三（二甲基氨基）氯化鏻以高纯度和高收率制备亚氨基三（二甲基氨基）正膦的方法。 氨基三（二甲基氨基）鏻氯化物首先在碱金属或碱土金属的氢氧化物的水溶液中在碱金属或碱土金属的氯化物和氢氧化物微溶于其中的溶剂的存在下反应，由此亚氨基三 （二甲基氨基）正膦。 在反应混合物的70℃或更低的温度下将水溶解后，通过固液分离将固体从这样浓缩的反应混合物中除去。 然后将得到的母液蒸馏得到亚氨基三（二甲基氨基）正膦。

公开(公告)号：US6077930A

公开(公告)日：2000-06-20

申请号：US79230

申请日：1998-05-15

申请人： Tadahito Nobori ,  Shinji Kiyono ,  Takaomi Hayashi ,  Usaji Takaki

发明人： Tadahito Nobori ,  Shinji Kiyono ,  Takaomi Hayashi ,  Usaji Takaki

IPC分类号： C08G63/82 ,  C08G65/26 ,  C08G69/20 ,  C08G77/08 ,  C08G63/08

CPC分类号： C08G69/20 ,  C08G63/823 ,  C08G65/2675 ,  C08G77/08

摘要： A preparation process of a polymer comprising conducting ring-opening polymerization of a 4- to 10-membered ring-opening polymerizable cyclic monomer in the presence of a phosphazenium salt of an active hydrogen compound represented by the chemical formula (1): ##STR1## wherein n is an integer of 1 to 8 and indicates the number of phosphazenium cations, Z.sup.n- is an anion of a n-valent active hydrogen compound derived by releasing n protons from an active hydrogen compound having a maximum of 8 active hydrogen atoms, a, b, c and d are individually a positive integer or 0 and are not all 0 at the same time, R's are the same or different hydrocarbons having 1 to 10 carbon atoms, and two R's located on each common nitrogen atom may be coupled together to form a ring structure; or in the presence of the phosphazenium salt of the active hydrogen compound and the active hydrogen compound is disclosed. The process can prepare polymer by ring-opening polymerization of a 4- to 10-membered ring-opening polymerizable cyclic monomer in the presence of an initiator which causes no specific problem or preparation and handling, contains quite no installic ingredient and has no residual odor.

摘要翻译： 一种聚合物的制备方法，包括在由化学式（1）表示的活性氢化合物的磷氮烯基鏻盐的存在下进行4-至10-元可开环聚合的环状单体的开环聚合：其中n为 1〜8的整数，表示磷氮烯基鏻阳离子的数量，Zn-是通过从具有最多8个活性氢原子的活性氢化合物释放n个质子得到的n价活性氢化合物的阴离子，a，b， c和d分别为正整数或0并且同时不全部为0，R为相同或不同的碳原子数为1〜10的烃，并且位于每个常见氮原子上的两个R可以连接在一起形成 环结构; 或在活性氢化合物的磷腈鎓盐和活性氢化合物的存在下进行。 该方法可以通过在不引起特定问题或制备和处理的引发剂的存在下开环聚合4-至10-元可开环聚合的环状单体来制备聚合物，其中不含安装成分并且没有残留气味 。

公开(公告)号：US06664365B2

公开(公告)日：2003-12-16

申请号：US09366046

申请日：1999-09-03

申请人： Tadahito Nobori ,  Masahiro Kouno ,  Toshiaki Suzuki ,  Kazumi Mizutani ,  Shinji Kiyono ,  Yoshiho Sonobe ,  Usaji Takaki

发明人： Tadahito Nobori ,  Masahiro Kouno ,  Toshiaki Suzuki ,  Kazumi Mizutani ,  Shinji Kiyono ,  Yoshiho Sonobe ,  Usaji Takaki

IPC分类号： C08G6510

CPC分类号： C07F9/065 ,  C07F9/067 ,  C08G65/2675

摘要： The present invention provides a novel salt useful as an active species in an organic reaction and represented by the following chemical formula (1): wherein n stands for an integer of from 1 to 8, Zn− represents an n-valent anion of an active hydrogen compound, a, b, c and d each stands for a positive integer, and Rs represent the same or different hydrocarbon groups. Also disclosed is a simple and efficient process for producing a poly(alkylene oxide) by polymerizing an alkylene oxide compound in the presence of the salt represented by the chemical formula (1).

摘要翻译： 本发明提供了可用作有机反应中的活性物质的新型盐，其由以下化学式（1）表示：其中n表示1至8的整数，Z n表示n价阴离子 的活性氢化合物，a，b，c和d分别表示正整数，Rs表示相同或不同的烃基。 还公开了通过在化学式（1）表示的盐的存在下聚合烯化氧化合物来制备聚（环氧烷）的简单和有效的方法。