公开(公告)号：US08822715B2

公开(公告)日：2014-09-02

申请号：US13703185

申请日：2011-06-21

申请人： Kiyoharu Hirao ,  Katsuichi Ohtsuki ,  Hiroshi Tsuji ,  Hiroki Sato

发明人： Kiyoharu Hirao ,  Katsuichi Ohtsuki ,  Hiroshi Tsuji ,  Hiroki Sato

IPC分类号： C07F9/12 ,  C09K21/12 ,  B01J27/138 ,  B01J27/125 ,  B01J27/16

CPC分类号： C07F9/12 ,  B01J27/125 ,  B01J27/138 ,  B01J27/16 ,  C09K21/12

摘要： A method for producing an aromatic diphosphate comprising: Step 1 which is a step where a specific aromatic monohydroxy compound having a steric hindrance group at ortho-positions is made to react with phosphorus oxyhalide in the presence of a Lewis acid catalyst and then the unreacted phosphorus oxyhalide is removed under a reduced pressure to give a specific; and Step 2 which is a step where the reaction product obtained in the above step is made to react with a specific aromatic dihydroxy compound in an amount of 0.5 mol to 1 mol of halogen contained in the reaction product in the presence of a Lewis acid catalyst to give a specific aromatic diphosphate.

摘要翻译： 一种制备芳族二磷酸盐的方法，包括：步骤1，其中在路易斯酸催化剂存在下使位于邻位的具有位阻基团的特定芳族单羟基化合物与磷酰卤反应，然后将未反应的磷 在减压下除去卤氧化物，得到特定的; 和步骤2，其中在路易斯酸催化剂存在下使上述步骤中得到的反应产物与特定的芳族二羟基化合物以0.5mol至1mol的反应产物中所含的卤素反应 得到特定的芳族二磷酸酯。

公开(公告)号：US20130090490A1

公开(公告)日：2013-04-11

申请号：US13703185

申请日：2011-06-21

申请人： Kiyoharu Hirao ,  Katsuichi Ohtsuki ,  Hiroshi Tsuji ,  Hiroki Sato

发明人： Kiyoharu Hirao ,  Katsuichi Ohtsuki ,  Hiroshi Tsuji ,  Hiroki Sato

IPC分类号： C07F9/12 ,  C09K21/12

CPC分类号： C07F9/12 ,  B01J27/125 ,  B01J27/138 ,  B01J27/16 ,  C09K21/12

摘要： A method for producing an aromatic diphosphate comprising: Step 1 which is a step where a specific aromatic monohydroxy compound having a steric hindrance group at ortho-positions is made to react with phosphorus oxyhalide in the presence of a Lewis acid catalyst and then the unreacted phosphorus oxyhalide is removed under a reduced pressure to give a specific; and Step 2 which is a step where the reaction product obtained in the above step is made to react with a specific aromatic dihydroxy compound in an amount of 0.5 mol to 1 mol of halogen contained in the reaction product in the presence of a Lewis acid catalyst to give a specific aromatic diphosphate.

摘要翻译： 一种制备芳族二磷酸盐的方法，包括：步骤1，其中在路易斯酸催化剂存在下使位于邻位的具有位阻基团的特定芳族单羟基化合物与磷酰卤反应，然后将未反应的磷 在减压下除去卤氧化物，得到特定的; 和步骤2，其中在路易斯酸催化剂存在下使上述步骤中得到的反应产物与特定的芳族二羟基化合物以0.5mol至1mol的反应产物中所含的卤素反应 得到特定的芳族二磷酸酯。

公开(公告)号：US5679824A

公开(公告)日：1997-10-21

申请号：US685532

申请日：1996-07-24

申请人： Kiyoharu Hirao ,  Shouji Oda ,  Yukio Omoda

发明人： Kiyoharu Hirao ,  Shouji Oda ,  Yukio Omoda

IPC分类号： C09K21/12 ,  B01D9/00 ,  C07F9/12 ,  C08K5/52 ,  C08K5/523 ,  C07F9/09

CPC分类号： C08K5/523 ,  C07F9/12

摘要： A method of pulverizing aromatic phosphates which comprises stressing an oily product of an aromatic phosphate having a purity of 90% or more at a temperature lower by 5.degree. to 100.degree. C. than a melting point of the aromatic phosphate in a temperature-controllable kneader to solidify and pulverize the aromatic phosphate. According to the present invention, aromatic phosphates industrially obtained are able to be solidified and pulverized in a short time in a simple way without being subjected to specific purification. Further, the invention is industrially advantageous in that the solidification and pulverization can be performed successively after production of the aromatic phosphate.

摘要翻译： 一种粉碎芳族磷酸盐的方法，其包括在温度可控的捏合机中，在比所述芳族磷酸酯的熔点低5℃至100℃的温度下，将纯度为90％以上的芳族磷酸酯的油状产物 固化和粉碎芳族磷酸盐。 根据本发明，工业上得到的芳族化合物能够在短时间内以简单的方式固化和粉碎，而不进行特别的纯化。 此外，本发明在工业上的优点在于可以在生产芳族磷酸酯之后连续进行固化和粉碎。

公开(公告)号：US06706907B1

公开(公告)日：2004-03-16

申请号：US10030124

申请日：2002-01-24

申请人： Kiyoharu Hirao ,  Masasuke Oda

发明人： Kiyoharu Hirao ,  Masasuke Oda

IPC分类号： C07F902

CPC分类号： C07F9/025 ,  C07F9/12

摘要： A method of purifying an organic phosphoric ester characterized by treating a crude organic phosphoric ester with an epoxy compound and treating the treated organic phosphoric ester with an alkaline aqueous solution to purify it. The purification method is effective in stably obtaining an organic phosphoric ester reduced in acid value and excellent in heat resistance, hydrolytic resistance, and storage stability, regardless of the kind or amount of the organic phosphoric ester, the treating conditions, etc.

摘要翻译： 一种纯化有机磷酸酯的方法，其特征在于用环氧化合物处理粗有机磷酸酯并用碱性水溶液处理经处理的有机磷酸酯以进行纯化。 纯化方法无论磷酸酯类的种类，用量，处理条件等，均稳定地获得酸值降低，耐热性，耐水解性，贮存稳定性优异的有机磷酸酯。

公开(公告)号：US5880308A

公开(公告)日：1999-03-09

申请号：US761376

申请日：1996-12-09

申请人： Shigeru Kawata ,  Kiyoharu Hirao ,  Kazuo Noguchi

发明人： Shigeru Kawata ,  Kiyoharu Hirao ,  Kazuo Noguchi

IPC分类号： B01J27/06 ,  C07B61/00 ,  C07F9/09 ,  C07F9/12 ,  C08K5/52 ,  C08K5/523 ,  C09K21/12

CPC分类号： C07F9/12

摘要： A process for preparing aromatic bisphosphates includes: a first step of reacting an aromatic monohydroxy compound having a steric hindrance group at the ortho position, with a phosphorus oxyhalide in the presence of a Lewis acid catalyst (a) to yield a reaction mixture containing diarylphosphorohalidate, and a second step of reacting the reaction mixture of the first step with an aromatic dihydroxy compound in the presence of a Lewis acid catalyst (b) to obtain an aromatic bisphosphate, wherein the aromatic monohydroxy compound and the phosphorus oxyhalide are reacted in a molar ratio of 2.0:1.0-1.1 in the first step, and the reaction mixture of the first step is subjected to a distillation treatment before the reaction of the second step, thereby obtaining the aromatic bisphosphate of high purity.

摘要翻译： 一种制备芳族二磷酸盐的方法包括：在路易斯酸催化剂（a）存在下，使在邻位具有位阻基团的芳族单羟基化合物与磷酰卤反应的第一步骤，得到含有二芳基次氯酸盐的反应混合物， 和在路易斯酸催化剂（b）的存在下使第一步反应混合物与芳族二羟基化合物反应得到芳族二磷酸酯的第二步骤，其中芳族单羟基化合物和磷酰卤以摩尔比 为2.0:1.0-1.1，第一步骤的反应混合物在第二步反应之前进行蒸馏处理，从而得到高纯度的芳族二磷酸盐。