公开(公告)号：US06974886B2

公开(公告)日：2005-12-13

申请号：US10511823

申请日：2003-04-24

申请人： Fumio Oi ,  Norio Yanase ,  Takayuki Kitahara ,  Nobuyuki Nate

发明人： Fumio Oi ,  Norio Yanase ,  Takayuki Kitahara ,  Nobuyuki Nate

IPC分类号： C07C315/06 ,  C07C317/22 ,  C07C317/33

CPC分类号： C07C315/06 ,  C07C317/22

摘要： The present invention provides a process for producing dihydroxydiphenylsulfone wherein trihydroxytriphenylsulfone and coloring impurities are effectively removed without altering the isomeric composition of dihydroxydiphenylsulfone. In particular, the present invention provides a process for producing dihydroxydiphenylsulfone comprising the steps of dissolveing or suspending in an aqueous solvent crude dihydroxydiphenylsulfone containing trihydroxytriphenylsulfone, adjusting the pH to 5–7, optionally cooling, and separating the crystalline dihydroxydiphenylsulfone thus precipitated.

摘要翻译： 本发明提供了二羟基二苯砜的制备方法，其中三羟基三苯基砜和着色杂质被有效地除去而不改变二羟基二苯砜的异构体组成。 特别地，本发明提供了二羟基二苯砜的制造方法，其特征在于，将含有三羟基三苯基砜的粗二羟基二苯砜水溶液溶解或悬浮，调节pH至5-7，任选地冷却，分离析出的结晶二羟基二苯砜。

公开(公告)号：US20050272956A1

公开(公告)日：2005-12-08

申请号：US10529074

申请日：2003-09-22

申请人： Eiji Ogata ,  Fumio Oi ,  Norio Yanase ,  Nobuyuki Nate

发明人： Eiji Ogata ,  Fumio Oi ,  Norio Yanase ,  Nobuyuki Nate

IPC分类号： C07C315/00 ,  C07C315/06 ,  C07C317/22

CPC分类号： C07C315/00 ,  C07C315/06 ,  C07C317/22

摘要： The present invention provides a process for producing 4,4′-dihydroxydiphenylsulfone of very high purity. In particular, the present invention provides a process for producing 4,4′-dihydroxydiphenylsulfone of high purity comprising the steps of subjecting phenol in combination with a sulfonating agent or phenolsulfonic acid to a dehydration reaction in the presence of an aromatic nonpolar solvent while suspending the resulting dihydroxydiphenylsulfone therein, mixing the reaction suspension with a polar solvent to at least partially dissolve the dihydroxydiphenylsulfone, and precipitating 4,4′-dihydroxydiphenylsulfone.

摘要翻译： 本发明提供了一种制备非常高纯度的4,4'-二羟基二苯砜的方法。 特别地，本发明提供了一种制备高纯度的4,4'-二羟基二苯基砜的方法，包括以下步骤：在芳族非极性溶剂的存在下使苯酚与磺化剂或苯酚磺酸组合进行脱水反应，同时使 将反应悬浮液与极性溶剂混合至少部分溶解二羟基二苯基砜，并沉淀出4,4'-二羟基二苯基砜。

公开(公告)号：US20050171384A1

公开(公告)日：2005-08-04

申请号：US10511823

申请日：2003-04-24

申请人： Fumio Oi ,  Norio Yanase ,  Takayuki Kitahara ,  Nobuyuki Nate

发明人： Fumio Oi ,  Norio Yanase ,  Takayuki Kitahara ,  Nobuyuki Nate

IPC分类号： C07C315/06 ,  C07C317/22

CPC分类号： C07C315/06 ,  C07C317/22

摘要： The present invention provides a process for producing dihydroxydiphenylsulfone wherein trihydroxytriphenylsulfone and coloring impurities are effectively removed without altering the isomeric composition of dihydroxydiphenylsulfone. In particular, the present invention provides a process for producing dihydroxydiphenylsulfone comprising the steps of dissolveing or suspending in an aqueous solvent crude dihydroxydiphenylsulfone containing trihydroxytriphenylsulfone, adjusting the pH to 5-7, optionally cooling, and separating the crystalline dihydroxydiphenylsulfone thus precipitated.

摘要翻译： 本发明提供了二羟基二苯砜的制备方法，其中三羟基三苯基砜和着色杂质被有效地除去而不改变二羟基二苯砜的异构体组成。 特别地，本发明提供了二羟基二苯砜的制造方法，其特征在于，将含有三羟基三苯基砜的粗二羟基二苯砜水溶液溶解或悬浮，调节pH至5-7，任选地冷却，分离析出的结晶二羟基二苯砜。

公开(公告)号：US07456321B2

公开(公告)日：2008-11-25

申请号：US10529074

申请日：2003-09-22

申请人： Eiji Ogata ,  Fumio Oi ,  Norio Yanase ,  Nobuyuki Nate

发明人： Eiji Ogata ,  Fumio Oi ,  Norio Yanase ,  Nobuyuki Nate

IPC分类号： C07F315/00

CPC分类号： C07C315/00 ,  C07C315/06 ,  C07C317/22

摘要： The present invention provides a process for producing 4,4′-dihydroxydiphenylsulfone of very high purity. In particular, the present invention provides a process for producing 4,4′-dihydroxydiphenylsulfone of high purity comprising the steps of subjecting phenol in combination with a sulfonating agent or phenolsulfonic acid to a dehydration reaction in the presence of an aromatic nonpolar solvent while suspending the resulting dihydroxydiphenylsulfone therein, mixing the reaction suspension with a polar solvent to at least partially dissolve the dihydroxydiphenylsulfone, and precipitating 4,4′-dihydroxydiphenylsulfone.

摘要翻译： 本发明提供了一种制备非常高纯度的4,4'-二羟基二苯砜的方法。 特别地，本发明提供了一种制备高纯度的4,4'-二羟基二苯基砜的方法，包括以下步骤：在芳族非极性溶剂的存在下使苯酚与磺化剂或苯酚磺酸组合进行脱水反应，同时使 将反应悬浮液与极性溶剂混合至少部分溶解二羟基二苯基砜，并沉淀出4,4'-二羟基二苯基砜。

公开(公告)号：US20050272603A1

公开(公告)日：2005-12-08

申请号：US10528784

申请日：2003-09-22

申请人： Fumio Oi ,  Norio Yanase ,  Nobuyuki Nate

发明人： Fumio Oi ,  Norio Yanase ,  Nobuyuki Nate

IPC分类号： B41M5/333 ,  B41M5/337 ,  B41M5/30

CPC分类号： B41M5/3336

摘要： A thermal recording material includes a thermosensitive coloring layer, which is made by applying a dispersion liquid, in which the developer and a coloring dye are dispersed, onto a supporting base, and then drying the base. The developer contains 4,4′-dihydroxydiphenyl sulfone as a major component; and 2,4′dihydroxydiphenyl sulfone, the 4,4′-dihydroxydiphenyl sulfone and the 2,4′-dihydroxydiphenyl sulfone being contained at a weight ratio greater than 90:10 and no more than 100:0, and the developer containing phenolsulfonic acid phenyl ester no more than 1.5% by weight with respect to a sum quantity of the 4,4′-dihydroxydiphenyl sulfone and the 2,4′-dihydroxydiphenyl sulfone. The present invention thus provides a thermal recording material causing less surface texture fogging and is superior in preservation ability, and also provides a developer suitably used as a component of the thermal recording material.

摘要翻译： 热敏记录材料包括通过将其中分散有显色剂和着色染料的分散液施加到支撑基底上，然后干燥基底而制成的热敏着色层。 显影剂含有4,4'-二羟基二苯砜作为主要成分; 和2,4'-二羟基二苯砜，4,4'-二羟基二苯砜和2,4'-二羟基二苯砜以重量比大于90:10且不大于100:0的含量，并含有苯酚磺酸的显影剂 苯基酯相对于4,4'-二羟基二苯基砜和2,4'-二羟基二苯基砜的总量不超过1.5重量％。 因此，本发明提供了一种导致较少表面纹理起雾并且保存能力优异的热敏记录材料，并且还提供了适合用作热敏记录材料的组分的显影剂。

公开(公告)号：US5189223A

公开(公告)日：1993-02-23

申请号：US678332

申请日：1991-05-01

申请人： Eiji Ogata ,  Nobuyuki Nate

发明人： Eiji Ogata ,  Nobuyuki Nate

IPC分类号： C07C315/00 ,  C07C315/04 ,  C07C317/22

CPC分类号： C07C315/04 ,  C07C315/00

摘要： The present invention provides a process for preparing 4,4'-dihydroxydiphenylsulfone which comprises subjecting a phenol and a sulfonating agent to dehydration reaction in the presence of mesitylene as a reaction medium while the produced 4,4'-dihydroxydiphenylsulfone is suspended in the mesitylene, and a process for preparing 4,4'-dihydroxydiphenylsulfone, characterized in that after the foregoing dehydration reaction, the 4,4'-dihydroxydiphenysulfone obtained as suspended in the mesitylene and/or retained in a liquid-free solid form is subjected to reaction for isomerization of 2,4'-dihydroxydiphenylsulfone produced as a by-product into 4,4'-dihydroxydiphenylsulfone with heating at a temperature of not lower than that for isomerization of 2,4'-dihydroxydiphenylsulfone into 4,4'-dihydroxydiphenylsulfone.

摘要翻译： PCT No.PCT / JP90 / 01179 Sec。 371日期1991年5月1日 102（e）1991年5月1日PCT PCT 1990年9月14日PCT公布。 公开号WO91 / 04245 日本1991年4月4日。本发明提供一种4,4'-二羟基二苯砜的制备方法，其包括在作为反应介质的均三甲苯存在下使苯酚和磺化剂进行脱水反应， 二羟基二苯基砜悬浮在均三甲苯中，制备4,4'-二羟基二苯砜的方法，其特征在于，在上述脱水反应后，获得悬浮在均三甲苯中和/或保留在无液体中的4,4'-二羟基二苯砜 使2,4-二羟基二苯基砜的2,4'-二羟基二苯基砜的异构化反应为4,4'-二羟基二苯基砜的2,4'-二羟基二苯砜异构化，在不低于2,4'-二羟基二苯基砜异构化的温度下加热至4， 4'-二羟基二苯砜。

公开(公告)号：US4820831A

公开(公告)日：1989-04-11

申请号：US10095

申请日：1986-12-12

申请人： Eiji Ogata ,  Koji Ono ,  Nobuyuki Nate

发明人： Eiji Ogata ,  Koji Ono ,  Nobuyuki Nate

IPC分类号： C07C315/00 ,  B01J31/02 ,  C07C67/00 ,  C07C313/00 ,  C07C317/22 ,  F15B11/04 ,  C07C147/10

CPC分类号： C07C317/00

摘要： The process of the present invention is a process for preparing 4,4'-dihydroxydiphenyl sulfone by subjecting phenol, and a sulfonating agent or phenolsulfonic acid to a dehydration reaction in the presence of a solvent, subsequently maintaining the reaction system at a temperature of between 100.degree. to 200.degree. C. and removing the solvent from the reaction system to cause the dehydration reaction to further proceed while allowing 4,4'-dihydroxydiphenyl sulfone to separate out and to subject dissolved 2,4'-dihydroxydiphenyl sulfone formed as a by-product to an isomerization reaction for converting the by-product to 4,4'-dihydroxydiphenyl sulfone, and eventually removing the solvent and the unreacted phenol from the system substantially entirely to complete the isomerization reaction, the process being characterized in that an aromatic sulfonic acid represented by the formula ##STR1## wherein X is a halogen atom, n is 0, 1 or 2, and m is 1 of 2 is caused to be present in the reaction system. 4,4'-Dihydroxydiphenyl sulfone can be produced by the process with a high purity and in a high yield.

摘要翻译： PCT No.PCT / JP86 / 00194 Sec。 371日期：1986年12月12日 102（e）日期1986年12月12日PCT提交1986年4月17日PCT公布。 公开号WO86 / 06370 日本1986年11月6日。本发明的方法是通过在溶剂存在下使苯酚和磺化剂或苯酚磺酸进行脱水反应来制备4,4'-二羟基二苯基砜的方法， 反应体系在100〜200℃的温度下，从反应体系中除去溶剂，使脱水反应进一步进行，同时使4,4'-二羟基二苯砜分离出来并使溶解的2,4' - 二羟基二苯砜作为副产物形成异构化反应，用于将副产物转化为4,4'-二羟基二苯基砜，并最终从体系中除去溶剂和未反应的苯酚，完全完全异构化反应，该方法 其特征在于，由式“IMAGE”表示的芳族磺酸，其中X为卤素原子，n为0,1或2，m为2的m为芳族磺酸存在于 反应体系。 4,4'-二羟基二苯砜可以通过高纯度和高收率的方法生产。

公开(公告)号：US5241121A

公开(公告)日：1993-08-31

申请号：US904887

申请日：1992-06-25

申请人： Eiji Ogata ,  Nobuyuki Nate ,  Kazuo Hamano

发明人： Eiji Ogata ,  Nobuyuki Nate ,  Kazuo Hamano

IPC分类号： C07C315/00 ,  C07C315/04 ,  C07C317/22

CPC分类号： C07C315/00 ,  C07C315/04

摘要： A process for preparing 4,4'-dihydroxydiphenylsulfone, the process including heating 4,4'-dihydroxydiphenylsulfone and 2,4'-dihydroxydiphenylsulfone in the presence of an acid catalyst to isomerize the 2,4'-dihydroxydiphenylsulfone into 4,4'-dihydroxydiphenylsulfone, the process being characterized in that a suspension of 4,4'-dihydroxydiphenylsulfone and 2,4'-dihydroxydiphenylsulfone in a liquid dispersing medium is heated for isomerization while the liquid portion is distilled off or a crystal mixture of 4,4'-dihydroxydiphenylsulfone and 2,4'-dihydroxydiphenylsulfone is heated for isomerization to produce 4,4'-dihydroxydiphenylsulfone in the form of crystal powder.

摘要翻译： 一种制备4,4'-二羟基二苯砜的方法，该方法包括在酸催化剂存在下加热4,4'-二羟基二苯砜和2,4'-二羟基二苯砜，使2,4'-二羟基二苯砜异构化成4,4'-二羟基二苯砜， 二氢二苯基砜，其特征在于将4,4'-二羟基二苯基砜和2,4'-二羟基二苯基砜在液体分散介质中的悬浮液加热异构化，同时蒸馏掉液体部分或4,4'-二羟基二苯基砜的结晶混合物， 二羟基二苯砜和2,4'-二羟基二苯砜加热异构化，生成结晶粉末形式的4,4'-二羟基二苯砜。