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1. 发明授权

US4675444A Process for producing aminophenols 失效
标题翻译：生产氨基苯酚的方法
公开(公告)号：US4675444A
公开(公告)日：1987-06-23
申请号：US802182
申请日：1985-11-25
申请人： Fujihisa Matsunaga , Eiji Kato , Tsuyoshi Kimura , Yoichiro Isota
发明人： Fujihisa Matsunaga , Eiji Kato , Tsuyoshi Kimura , Yoichiro Isota
IPC分类号： C07C213/02 , C07C67/00 , C07C213/00 , C07C213/10 , C07C215/76 , C07C85/06
CPC分类号： C07C215/76 , Y02P20/582
摘要： A process for producing an aminophenol, which comprises(A) a step of reacting a dihydric phenol with an aminating reagent in the liquid state under heat in the presence of water and a water-soluble catalyst,(B) a step of removing the unreacted aminating reagent from the reaction mixture, and then precipitating the crude aminophenol from the reaction mixture from which the aminating reagent has been removed, thereby to obtain a crystallization mixture containing the crude aminophenol,(C) a step of separating the crystallization mixture into crystals of the crude aminophenol and the reaction mother liquor containing the catalyst,(D) a step of circulating part or the whole of the reaction mother liquor to the aminating step, and(E) a step of washing the crude aminophenol crystals with a washing liquor to obtain the washed crude aminophenol crystals and the washing mother liquor, and thereafter separating the aminophenol from the washed crude aminophenol crystals and purifying it.
摘要翻译：一种氨基苯酚的制造方法，其包括（A）在水和水溶性催化剂的存在下，在加热下使二元酚与胺化试剂以液态反应的步骤，（B）除去未反应的从反应混合物中制备氨基化试剂，然后从已经除去胺化试剂的反应混合物中沉淀粗氨基苯酚，从而得到含有粗氨基苯酚的结晶混合物，（C）将结晶混合物分离成晶体的步骤粗氨基苯酚和含有催化剂的反应母液，（D）将部分或全部反应母液循环到胺化步骤的步骤，（E）用洗涤液洗涤粗氨基苯酚晶体的步骤，得到洗涤的粗氨基苯酚结晶和洗涤母液，然后从洗涤的粗氨基苯酚晶体中分离出氨基苯酚并进行纯化。

2. 发明授权

US06284931B1 Process for producing 3, 3, 5-trimethylcyclohexylidenebisphenol 有权
标题翻译：制备3,3,5-三甲基亚环己基双酚的方法
公开(公告)号：US06284931B1
公开(公告)日：2001-09-04
申请号：US09421372
申请日：1999-10-20
申请人： Yoichiro Isota , Toru Nakaguchi , Hiroshi Takenaka , Kazuhiko Yao
发明人： Yoichiro Isota , Toru Nakaguchi , Hiroshi Takenaka , Kazuhiko Yao
IPC分类号： C07L3917
CPC分类号： C08G64/06 , C07C37/20 , C07C2601/14 , C08G75/23 , C07C39/17
摘要： A process for producing a 3,3,5-trimethylcyclohexylidenebisphenol, comprising pre-reacting a phenol (A), i.e., phenol whose 2- and 6-positions may be monosubstituted or disubstituted with an alkyl group having 1 to 4 carbon atoms, with 3,3,5-trimethylcyclohexanone (B) at a molar ratio ((A)/(B)) of 3 to 7 in the presence of an acid catalyst until 3,3,5-trimethylcyclohexanone (B) exhibits a degree of conversion of at least 90 mol %; adding the phenol (A) and/or an aromatic hydrocarbon (C) to the thus obtained reaction mixture; and post-reacting the resultant mixture. This process enables not only suppressing a rise of the viscosity of the reaction mixture but also obtaining the desired product at high yield. Therefore, this process is applicable to not only the productivity enhancement in batch processing but also a continuous reaction processing which has been regarded as being difficult.
摘要翻译：一种制备3,3,5-三甲基亚环己基双酚的方法，包括将苯酚（A）即其2-和6-位可以被具有1至4个碳原子的烷基单取代或二取代的苯酚预反应，（A）/（B））的摩尔比为3至7的3,3,5-三甲基环己酮（B）在酸催化剂存在下直至3,3,5-三甲基环己酮（B）显示出转化程度至少90mol％; 向由此得到的反应混合物中加入苯酚（A）和/或芳族烃（C）; 并使所得混合物反应。该方法不仅可以抑制反应混合物的粘度上升，而且能够以高收率得到所需的产物。因此，该方法不仅适用于分批处理的生产率提高，而且适用于被认为难以进行的连续反应处理。

3. 发明授权

US06992227B1 Process for producing 1, 1-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane 有权
标题翻译：制备1,1,1-双（4-羟基苯基）-3,3,5-三甲基环己烷的方法
公开(公告)号：US06992227B1
公开(公告)日：2006-01-31
申请号：US10363797
申请日：2000-09-11
申请人： Kazuhiko Yao , Kenji Ekawa , Yoichiro Isota , Toru Nakaguchi
发明人： Kazuhiko Yao , Kenji Ekawa , Yoichiro Isota , Toru Nakaguchi
IPC分类号： C07L39/17
CPC分类号： C07C37/84 , C07C37/20 , C07C2527/173 , C07C2601/14 , C07C39/17
摘要： A process for production of 1,1-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane which comprises reacting phenol with 3,3,5-trimethylcyclohexanone in the presence of an acid catalyst, separating the resulting phenol adduct crystals of 1,1-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane from the resulting reaction mixture, and removing the phenol from the phenol adduct crystals, wherein the phenol adduct crystals are dissolved in a crystallization solvent comprising an aromatic hydrocarbon solvent and water, crystallizing the crystals of 1,1-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane out of the crystallization solvent, and collecting the crystals by filtration at a temperature of 40–60° C.
摘要翻译：一种生产1,1-双（4-羟基苯基）-3,3,5-三甲基环己烷的方法，其包括在酸催化剂存在下使苯酚与3,3,5-三甲基环己酮反应，将所得苯酚加合物晶体从所得反应混合物中加入1,1-双（4-羟基苯基）-3,3,5-三甲基环己烷，并从苯酚加合物晶体中除去苯酚，其中苯酚加合物晶体溶于包含芳烃溶剂和水，将结晶溶剂中的1,1-双（4-羟基苯基）-3,3,5-三甲基环己烷的结晶结晶，并在40-60℃的温度下过滤收集晶体。

4. 发明授权

US6118029A Process for producing 3,3',5,5'-tetra-t butylbiphenol 失效
标题翻译：制备3,3'，5,5'-四叔丁基联苯酚的方法
公开(公告)号：US6118029A
公开(公告)日：2000-09-12
申请号：US015962
申请日：1998-01-30
申请人： Yoichiro Isota , Kazuhiko Yao , Mikio Kawahara
发明人： Yoichiro Isota , Kazuhiko Yao , Mikio Kawahara
IPC分类号： C07C37/11 , C07C37/14 , C07C39/15 , C07C39/12
CPC分类号： C07C37/14 , C07C37/11 , C07C37/50
摘要： A batch or continuous process produces highly pure 3,3',5,5'-tetra-t-butylbiphenol suitable as a starting material for the synthesis of 4,4'-biphenol. The process for producing 3,3',5,5'-tetra-t-butylbiphenol comprises conducting an oxidation coupling of purified 2,6-di-t-butylphenol(i) or crude 2,6-di-t-butylbiphenol(ii), said crude 2,6-di-t-butylphenol being obtained by reacting isobutylene with phenol in the presence of an aluminum catalyst, and removing the aluminum catalyst. The 2,6-di-t-butylphenol is oxidatively coupled in an alkali metal catalyst mixture comprising (1) an alkali metal catalyst and alkylphenols, or (2) alkali metal catalyst, alkylphenols and phenol to produce 3,3',5,5'-tetra-t-butylbiphenol. The oxidative coupling is conducted together with 10-30% by weight of phenol and/or t-butylphenol per 100% by weight of 2,6-di-t-butylphenol in the presence of an alkali metal catalyst.
摘要翻译：分批或连续方法产生适合作为合成4,4'-联苯酚的起始原料的高纯度3,3'，5,5'-四叔丁基联苯。制备3,3'，5,5'-四叔丁基联苯酚的方法包括纯化的2,6-二叔丁基苯酚（i）或粗2,6-二叔丁基联苯酚（ ii）所述粗制2,6-二叔丁基苯酚是通过异丁烯与酚在铝催化剂存在下反应而得到的，并除去铝催化剂。 2,6-二叔丁基苯酚在碱金属催化剂混合物中氧化偶联，该混合物包括（1）碱金属催化剂和烷基酚，或（2）碱金属催化剂，烷基酚和苯酚，产生3,3' 5'-四叔丁基联苯酚。在碱金属催化剂存在下，每100重量％的2,6-二叔丁基苯酚与10-30重量％的苯酚和/或叔丁基苯酚一起进行氧化偶联。

5. 发明授权

US06673975B1 Method for producing 1,1-bis-(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane 有权
标题翻译： 1,1-双 - （4-羟基苯基）-3,3,5-三甲基环己烷的制备方法
公开(公告)号：US06673975B1
公开(公告)日：2004-01-06
申请号：US10380099
申请日：2003-03-07
申请人： Kazuhiko Yao , Kenji Ekawa , Yoichiro Isota , Toru Nakaguchi
发明人： Kazuhiko Yao , Kenji Ekawa , Yoichiro Isota , Toru Nakaguchi
IPC分类号： C07C3917
CPC分类号： C07C37/20 , C07C37/84 , C07C2527/11 , C07C2601/14 , C07C39/17
摘要： The invention provides a process for production of high purity 1,1-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane (BPTMC) which comprises: (a) a reaction step wherein phenol is reacted with 3,3,5-trimethylcyclohexanone (TMC) in a slurry containing phenol adduct crystals of BPTMC in the presence of an acid catalyst; (b) a neutralization step wherein after the reaction, the resulting reaction mixture in the form of slurry is neutralized with an alkali while heating to convert the slurry to a solution; (c) a primary crystallization and filtration step wherein the resulting solution is cooled and the resulting phenol adduct crystals of BPTMC are collected by filtration; (d) a secondary crystallization and filtration step wherein the adduct crystals obtained in the primary crystallization and filtration step are heated in a crystallization solvent to dissolve the crystals therein to prepare a solution and then the solution is cooled to crystallize BPTMC out of the solution, followed by collecting the crystals of BPTMC by filtration; (e) a filtrate recycling step wherein at least a part of the secondary crystallization filtrate obtained in the secondary crystallization and filtration step is returned to the reaction step. The process provides uncolored high purity BPTMC in high selectivity and in high yield in an industrially stable manner which is substantially free from residual phenol and trace impurities such as sodium, chlorine and sulfur and hence which is suitable for use as raw materials for the production of resins for optical use.
摘要翻译：本发明提供一种生产高纯度1,1-双（4-羟基苯基）-3,3,5-三甲基环己烷（BPTMC）的方法，该方法包括：（a）一个反应步骤，其中苯酚与3,3,5 - 三甲基环己酮（TMC）在含有BPTMC的苯酚加合物晶体的淤浆中，在酸催化剂存在下; （b）中和步骤，其中在反应之后，将所得到的浆料形式的反应混合物用碱中和，同时加热以将浆料转化为溶液; （c）初步结晶和过滤步骤，其中将所得溶液冷却，并通过过滤收集所得到的BPTMC的苯酚加合物晶体; （d）二次结晶和过滤步骤，其中在一次结晶和过滤步骤中获得的加合物晶体在结晶溶剂中加热以溶解其中的晶体，以制备溶液，然后将溶液冷却以使溶液中的BPTMC结晶，然后过滤收集BPTMC晶体; （e）滤液再循环步骤，其中在二次结晶和过滤步骤中获得的至少一部分二次结晶滤液返回到反应步骤。该方法以高选择性提供无色高纯度BPTMC，在工业上稳定地提供高产率方式基本上不含残留的苯酚和痕量杂质如钠，氯和硫，因此适用于生产光学用树脂的原料。

6. 发明授权

US06673974B1 Process for production of 1,1-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane 有权
标题翻译：制备1,1-双（4-羟基苯基）-3,3,5-三甲基环己烷的方法
公开(公告)号：US06673974B1
公开(公告)日：2004-01-06
申请号：US10363706
申请日：2003-03-06
申请人： Kazuhiko Yao , Kenji Ekawa , Yoichiro Isota , Toru Nakaguchi
发明人： Kazuhiko Yao , Kenji Ekawa , Yoichiro Isota , Toru Nakaguchi
IPC分类号： C07C3917
CPC分类号： C07C37/20 , C07C2527/11 , C07C2601/14 , C07C39/17
摘要： A process for production of 1,1-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane which comprises reacting phenol with 3,3,5-trimethylcyclohexanone in the presence of an acid catalyst wherein the reaction of phenol with 3,3,5-trimethylcyclohexanone is started in a slurry comprising phenol adduct crystals of 1,1-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane and hydrated phenol in the presence of an acid catalyst, and then the reaction is continued in the slurry.
摘要翻译：一种生产1,1-双（4-羟基苯基）-3,3,5-三甲基环己烷的方法，包括在酸催化剂存在下使苯酚与3,3,5-三甲基环己酮反应，其中苯酚与3，在酸催化剂存在下，在包含1,1-双（4-羟基苯基）-3,3,5-三甲基环己烷和水合苯酚的苯酚加合物晶体的浆料中开始3,5-三甲基环己酮，然后继续反应在浆液中。

7. 发明授权

US06673973B1 Method of producing 1,1-bis-(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane 有权
标题翻译： 1,1-双 - （4-羟基苯基）-3,3,5-三甲基环己烷的制备方法
公开(公告)号：US06673973B1
公开(公告)日：2004-01-06
申请号：US10363207
申请日：2003-03-06
申请人： Kazuhiko Yao , Kenji Ekawa , Yoichiro Isota , Toru Nakaguchi
发明人： Kazuhiko Yao , Kenji Ekawa , Yoichiro Isota , Toru Nakaguchi
IPC分类号： C07C3917
CPC分类号： C07C37/20 , C07C37/84 , C07C2527/173 , C07C2601/14 , C07C39/17
摘要： A process for production of 1,1-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane which comprises reacting phenol with 3,3,5-trimethylcyclohexanone in the presence of an acid catalyst, adding an aqueous solution of an alkali to the resulting reaction mixture to neutralize it, removing a water phase from the thus neutralized reaction mixture, cooling the resulting oil phase to crystallize phenol adduct crystals of 1,1-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane while obtaining a primary crystallization filtrate, wherein the primary crystallization filtrate is heated to a temperature of 150-250° C. in the presence of an alkali catalyst in an inert gas atmosphere under a reduced pressure to thermally decompose 1,1-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane in the primary crystallization filtrate.
摘要翻译：一种生产1,1-双（4-羟基苯基）-3,3,5-三甲基环己烷的方法，包括在酸催化剂存在下使苯酚与3,3,5-三甲基环己酮反应，加入碱的水溶液向所得反应混合物中和，从由此中和的反应混合物中除去水相，冷却所得油相以结晶1,1-双（4-羟基苯基）-3,3,5-三甲基环己烷的苯酚加合物晶体，同时得到一次结晶滤液，其中在碱性催化剂存在下，在惰性气体气氛中，在减压下将一次结晶滤液加热至150-250℃，热分解1,1-二（4- 羟基苯基）-3,3,5-三甲基环己烷。

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