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1. 发明授权

US4925971A Method for producing aliphatic o-arylurethanes 失效
标题翻译：脂肪族O-芳基氨基甲酸酯的制备方法
公开(公告)号：US4925971A
公开(公告)日：1990-05-15
申请号：US279177
申请日：1988-12-02
申请人： Toshiya Aoki , Hiroshi Ishida , Shinsuke Fukuoka
发明人： Toshiya Aoki , Hiroshi Ishida , Shinsuke Fukuoka
IPC分类号： C07C269/04
CPC分类号： C07C269/04
摘要： A method for producing aliphatic O-arylurethanes by the reaction of an aliphatic primary amine with an aromatic hydroxyl compound and urea. Ammonia produced as a by-product in the reaction is removed during the reaction so that the ammonia concentration of the reaction solution is maintained at 2 wt % or less.

2. 发明授权

US08044226B2 Process for production of high-purity diaryl carbonate 有权
标题翻译：生产高纯度碳酸二芳基酯的方法
公开(公告)号：US08044226B2
公开(公告)日：2011-10-25
申请号：US12508297
申请日：2009-07-23
申请人： Shinsuke Fukuoka , Hironori Miyaji , Hiroshi Hachiya , Kazuhiko Matsuzaki
发明人： Shinsuke Fukuoka , Hironori Miyaji , Hiroshi Hachiya , Kazuhiko Matsuzaki
IPC分类号： C07C69/96
CPC分类号： C08G64/307 , B01D3/009 , B01D3/146 , C07C68/06 , C07C68/08 , Y02P20/127 , Y02P20/582 , C07C69/96
摘要： A high-purity diphenyl carbonate, wherein the diphenyl carbonate is unsubstituted or substituted with a lower hydrocarbon, and has a halogen content of not more than 0.1 ppm, a content of an intermediate boiling point material of not more than 100 ppm, and a content of by-products having a higher boiling point than that of said diphenyl carbonate of not more than 100 ppm. A specific industrially useful process for the production of a high-purity diaryl carbonate in which a diaryl carbonate having low contents of intermediate boiling point and high boiling point impurities is produced is disclosed. As a starting material, a reaction mixture containing an alkyl aryl carbonate obtained through a transesterification reaction between a dialkyl carbonate and an aromatic monohydroxy compound is used. The process in which separation by distillation is carried out uses three distillation columns in a specified order.
摘要翻译：一种高纯度碳酸二苯酯，其中碳酸二苯酯为未取代的或被低级烃取代，卤素含量不超过0.1ppm，中间沸点材料的含量不大于100ppm，含量为的沸点比碳酸二苯酯高的不高于100ppm的副产物。公开了一种生产具有低中值沸点和高沸点杂质含量的碳酸二芳基酯的高纯度碳酸二芳酯的具体的工业上有用的方法。作为起始原料，使用含有通过碳酸二烷基酯和芳族单羟基化合物之间的酯交换反应获得的碳酸烷基芳基酯的反应混合物。通过蒸馏进行分离的方法使用三个蒸馏塔以指定的顺序。

3. 发明申请

US20090209724A1 Process for industrially producing high-quality aromatic polycarbonate 审中-公开
标题翻译：工业生产高品质芳族聚碳酸酯的工艺
公开(公告)号：US20090209724A1
公开(公告)日：2009-08-20
申请号：US11991404
申请日：2006-11-30
申请人： Shinsuke Fukuoka , Hironori Miyaji , Hiroshi Hachiya , Kazuhiko Matsuzaki
发明人： Shinsuke Fukuoka , Hironori Miyaji , Hiroshi Hachiya , Kazuhiko Matsuzaki
IPC分类号： C08G64/06
CPC分类号： C07C68/06 , B01D3/009 , B01D3/32 , C07C68/08 , C08G64/307 , Y02P20/127 , C07C69/96
摘要： It is an object of the present invention to provide a specific process that enables a high-quality high-performance aromatic polycarbonate having excellent mechanical properties and no discoloration to be produced industrially in a large amount (e.g. not less than 1 ton/hr) stably for a prolonged period of time (e.g. not less than 1000 hours, preferably not less than 3000 hours, more preferably not less than 5000 hours) from a dialkyl carbonate and an aromatic dihydroxy compound. When producing the aromatic polycarbonate from the dialkyl carbonate and the aromatic dihydroxy compound, the above object can be attained by carrying out a process according to the present invention which comprises the steps of: (I) producing a diphenyl carbonate using two reactive distillation columns each having a specified structure; (II) obtaining a high-purity diphenyl carbonate from the diphenyl carbonate using a high boiling point material separating column A and a diphenyl carbonate purifying column B each having a specified structure; (III) subsequent producing an aromatic polycarbonate using a guide-contacting downflow type polymerization apparatus having a specified structure from a molten prepolymer obtained from the aromatic dihydroxy compound and the high-purity diphenyl carbonate; and (IV) recycling by-produced phenol into step (I).
摘要翻译：本发明的目的是提供一种能够在工业上大量（例如不低于1吨/小时）稳定地产生具有优异的机械性能和无变色的高品质高性能芳族聚碳酸酯的具体方法从碳酸二烷基酯和芳族二羟基化合物的长时间（例如不小于1000小时，优选不小于3000小时，更优选不小于5000小时）。当从碳酸二烷基酯和芳族二羟基化合物制备芳族聚碳酸酯时，可以通过进行本发明的方法来实现上述目的，其包括以下步骤：（I）使用两个反应蒸馏塔具有指定的结构; （II）使用高沸点材料分离塔A和碳酸二苯酯精制塔B各自具有特定结构，从碳酸二苯酯得到高纯度碳酸二苯酯; （III），然后使用由芳族二羟基化合物和高纯度碳酸二苯酯获得的熔融预聚物，使用具有特定结构的引导接触下流式聚合装置制备芳族聚碳酸酯; 和（IV）将副产物苯酚再循环到步骤（I）中。

4. 发明授权

US07544760B2 Polymerizer device for producing an aromatic polycarbonate 有权
标题翻译：用于生产芳族聚碳酸酯的聚合装置
公开(公告)号：US07544760B2
公开(公告)日：2009-06-09
申请号：US10593394
申请日：2005-06-16
申请人： Shinsuke Fukuoka , Hiroshi Hachiya , Kazuhiko Matsuzaki
发明人： Shinsuke Fukuoka , Hiroshi Hachiya , Kazuhiko Matsuzaki
IPC分类号： C08G64/00 , C08G63/02
CPC分类号： B01J19/24 , B01J2219/00094 , B01J2219/185 , B01J2219/1946 , C08G64/205 , C08G64/307
摘要： It is a task of the present invention to provide a polymerizer device and a polymerizer system which enable the production, by melt transesterification, of a high quality, high performance aromatic polycarbonate (which is colorless and has excellent mechanical properties) from a molten aromatic polycarbonate prepolymer obtained by reacting an aromatic dihydroxy compound with a diaryl carbonate, wherein the polycarbonate can be stably produced on a commercial scale at 1 to 50 t/hr for a long time. In the present invention, this task has been accomplished by a guide-wetting fall polymerizer device (in which a molten prepolymer is allowed to fall along and in contact with a guide, thereby effecting polymerization of the prepolymer) having a specific structure and a polymerizer system comprising such devices. That is, the device and the system have enabled the stable production of a high quality, high performance aromatic polycarbonate as mentioned above at 1 to 50 t/hr for a long time (more than several thousand hours, e.g., as long as 5,000 hours) without fluctuation of the molecular weight thereof.
摘要翻译：本发明的任务是提供一种能够通过熔融酯交换从熔融芳族聚碳酸酯生产高质量，高性能的芳族聚碳酸酯（其是无色且具有优异的机械性能）的聚合反应器装置和聚合反应器系统。通过使芳族二羟基化合物与碳酸二芳酯反应得到的预聚物，其中聚碳酸酯可以长期以1〜50t / hr的规模以商业规模稳定地制造。在本发明中，这个任务已经通过引导润湿下降聚合器装置（其中允许熔融预聚物沿着导向件落下并与导向器接触，从而实现具有特定结构的聚合反应）和聚合反应器包括这种装置的系统。也就是说，该装置和系统使得能够长时间以1至50t / hr稳定地生产如上所述的高质量，高性能的芳族聚碳酸酯（多于几千小时，例如长达5,000小时），其分子量不变。

5. 发明授权

US07531616B2 Process for industrial production of an aromatic carbonate 有权
标题翻译：工业生产芳香族碳酸酯的方法
公开(公告)号：US07531616B2
公开(公告)日：2009-05-12
申请号：US11632170
申请日：2005-07-12
申请人： Shinsuke Fukuoka , Hiroshi Hachiya , Kazuhiko Matsuzaki
发明人： Shinsuke Fukuoka , Hiroshi Hachiya , Kazuhiko Matsuzaki
IPC分类号： C08G64/00 , C08G63/02
CPC分类号： B01D3/146 , B01D3/009 , B01D3/143 , C07C68/06 , C07C68/08 , Y02P20/127 , C07C69/96
摘要： It is an object of the present invention to provide a specific process that enables aromatic carbonates to be produced with high selectivity and high productivity stably for a prolonged period of time on an industrial scale of not less than 1 ton per hour from a dialkyl carbonate and an aromatic monohydroxy compound using two continuous multi-stage distillation columns. Although there have been various proposals regarding processes for the production of aromatic carbonates by means of a reactive distillation method, these have all been on a small scale and short operating time laboratory level, and there have been no disclosures whatsoever on a specific process or apparatus enabling mass production on an industrial scale. According to the present invention, there are provided two specified continuous multi-stage distillation columns, and there is also provided a specific process that enables aromatic carbonates to be produced with high selectivity and high productivity stably for a prolonged period of time on an industrial scale of not less than 1 ton per hour from a dialkyl carbonate and an aromatic monohydroxy compound using a apparatus in which these two continuous multi-stage distillation columns are connected together.
摘要翻译：本发明的目的是提供一种具体方法，其能够以高于1吨/小时的工业规模从碳酸二烷基酯稳定地长时间稳定地制备芳香族碳酸酯，并且使用两个连续多级蒸馏塔的芳族单羟基化合物。尽管通过反应性蒸馏法已经有关于生产芳族碳酸酯的方法的各种建议，但这些方法都已经在小规模和操作时间短的实验室水平上，并且在具体方法或装置上没有公开任何内容实现工业规模的批量生产。根据本发明，提供了两个特定的连续多级蒸馏塔，并且还提供了能够以工业规模长时间稳定地以高选择性和高生产率制备芳族碳酸酯的具体方法使用这两个连续多级蒸馏塔连接在一起的装置，从碳酸二烷基酯和芳族单羟基化合物中不低于1吨/小时。

6. 发明授权

US07528213B2 Method for efficiently producing an aromatic polycarbonate 有权
标题翻译：有效生产芳族聚碳酸酯的方法
公开(公告)号：US07528213B2
公开(公告)日：2009-05-05
申请号：US10592690
申请日：2005-06-14
申请人： Shinsuke Fukuoka , Hiroshi Hachiya , Kazuhiko Matsuzaki
发明人： Shinsuke Fukuoka , Hiroshi Hachiya , Kazuhiko Matsuzaki
IPC分类号： C08G64/00 , C08G63/02
CPC分类号： C08G64/205 , C08G64/307
摘要： It is a task of the present invention to provide a method which enables the production of a high quality, high performance aromatic polycarbonate (which is colorless and has excellent mechanical properties) from a molten aromatic polycarbonate prepolymer obtained from an aromatic dihydroxy compound and a diaryl carbonate, wherein the polycarbonate can be stably produced on a commercial scale at 1 to 50 t/hr for a long time without the need for a large amount of an inert gas. In the present invention, this task has been accomplished by a method for producing an aromatic polycarbonate by the melt transesterification process, in which the prepolymer is caused to absorb a specific amount of an inert gas, followed by polymerization using a guide-wetting fall polymerizer device having a specific structure, whereby a high quality, high performance aromatic polycarbonate as mentioned above can be stably produced on a commercial scale at 1 to 50 t/hr for a long time (more than several thousand hours, e.g., as long as 5,000 hours) without fluctuation of the molecular weight thereof.
摘要翻译：本发明的任务是提供一种能够从由芳族二羟基化合物和二芳基取代的熔融芳族聚碳酸酯预聚物制备高质量，高性能的芳族聚碳酸酯（其为无色且具有优异的机械性能）的方法碳酸酯，其中聚碳酸酯可以长时间以1至50t / hr的规模以商业规模稳定地生产，而不需要大量的惰性气体。在本发明中，通过熔融酯交换法制造芳族聚碳酸酯的方法已经完成了该任务，其中使预聚物吸收特定量的惰性气体，然后使用引导润湿落下聚合反应器进行聚合具有特定结构的装置，由此可以长时间以1至50t / hr的规模以商业规模稳定地生产如上所述的高质量，高性能的芳族聚碳酸酯（多于几千小时，例如长达5,000 小时），其分子量不变。

7. 发明申请

US20080064846A1 Industrial Process for Production of High-Purity Diaryl Carbonate 审中-公开
公开(公告)号：US20080064846A1
公开(公告)日：2008-03-13
申请号：US11661605
申请日：2005-09-01
申请人： Shinsuke Fukuoka , Hironori Miyaji , Hiroshi Hachiya , Kazuhiko Matsuzaki
发明人： Shinsuke Fukuoka , Hironori Miyaji , Hiroshi Hachiya , Kazuhiko Matsuzaki
IPC分类号： C08G64/04 , B01D3/22 , C08G64/30 , B01D3/34
CPC分类号： C07C68/08 , B01D3/143 , B01D3/16 , C07C68/06 , Y02P20/127 , C07C69/96
摘要： It is an object of the present invention to provide a specific process that enables a high-purity diaryl carbonate that can be used as a raw material of a high-quality and high-performance polycarbonate to be produced stably for a prolonged period of time on an industrial scale of not less than 1 ton/hr using as a starting material a reaction mixture containing an alkyl aryl carbonate obtained through a transesterification reaction between a dialkyl carbonate and an aromatic monohydroxy compound. Although there have been various proposals regarding processes for the production of reaction mixtures containing aromatic carbonates by means of a reactive distillation method, these have all been on a small scale and short operating time laboratory level, and there have been no disclosures on a specific process or apparatus enabling mass production on an industrial scale from such a reaction mixture of a high-purity diaryl carbonate that can be used as a raw material of a high-quality and high-performance polycarbonate. According to the present invention, there is provided a specific process that enables a high-purity diaryl carbonate important as a raw material of a high-quality and high-performance polycarbonate to be produced stably for a prolonged period of time on an industrial scale of not less than 1 ton/hr by taking as a starting material a reaction mixture containing an alkyl aryl carbonate that has been obtained through a transesterification reaction between a dialkyl carbonate and an aromatic monohydroxy compound and subjecting this starting material to a transesterification reaction using a reactive distillation column having a specified structure, and then subjecting a high boiling point reaction mixture obtained from the bottom of the reactive distillation column to separation and purification using a high boiling point material separating column A and a diaryl carbonate purifying column B which have specified continuous multi-stage distillation columns.

8. 发明申请

US20080045755A1 Industrial Process For Separating Out By-Produced Alcohol 审中-公开
标题翻译：分离生产酒精的工业过程
公开(公告)号：US20080045755A1
公开(公告)日：2008-02-21
申请号：US11660672
申请日：2005-09-16
申请人： Shinsuke Fukuoka , Hironori Miyaji , Hiroshi Hachiya , Kazuhiko Matsuzaki
发明人： Shinsuke Fukuoka , Hironori Miyaji , Hiroshi Hachiya , Kazuhiko Matsuzaki
IPC分类号： C07C27/28
CPC分类号： C07C29/80 , B01D3/14 , B01D3/146 , C07C29/128 , C07C68/06 , C07C68/08 , Y02P20/127 , Y02P20/582 , C07C69/96 , C07C31/04 , C07C31/202
摘要： It is an object of the present invention to provide a specific industrial separation process that enables a by-produced alcohol to be separated out efficiently and stably for a prolonged period of time from a large amount (not less than 1 ton/hr) of a low boiling point reaction mixture having a specified composition containing the by-produced alcohol when mass-producing aromatic carbonates on an industrial scale by subjecting a dialkyl carbonate and an aromatic monohydroxy compound to transesterification reaction in a reactive distillation column in which a catalyst is present. Although there have been various proposals regarding processes for the production of aromatic carbonates by means of a reactive distillation method, these have all been on a small scale and short operating time laboratory level, and there have been no disclosures whatsoever on a specific process or apparatus enabling mass production on an industrial scale to be carried out stably for a prolonged period of time. Moreover, there have been no disclosures on a specific process or apparatus enabling the alcohol by-produced when producing the aromatic carbonates on an industrial scale using a reactive distillation system to be separated out efficiently and stably for a prolonged period of time on an industrial scale of not less than 200 kg/hr. According to the present invention, there is proposed a specific process that enables the above object to be attained by using the continuous multi-stage distillation column having a specified structure and a large amount (not less than 1 ton/hr) of a low boiling point reaction mixture having a specified composition containing the by-produced alcohol.
摘要翻译：本发明的目的是提供一种具体的工业分离方法，其能够使副产物的醇从大量（不低于1吨/小时）的高效和稳定地分离出来，当通过在其中存在催化剂的反应蒸馏塔中使碳酸二烷基酯和芳族单羟基化合物进行酯交换反应，在工业规模生产芳族碳酸酯时，具有含有副产物醇的指定组成的低沸点反应混合物。尽管通过反应性蒸馏法已经有关于生产芳族碳酸酯的方法的各种建议，但这些方法都已经在小规模和操作时间短的实验室水平上，并且在具体方法或装置上没有公开任何内容使工业规模的大规模生产能够长期稳定进行。此外，在工业规模上使用反应性蒸馏系统生产芳族碳酸酯时能够在工业规模下有效且稳定地分离出长时间的芳族碳酸酯的具体方法或装置不存在任何公开不小于200kg / hr。根据本发明，提出了通过使用具有特定结构和大量（不低于1吨/小时）低沸点的连续多级蒸馏塔来实现上述目的的具体方法具有含有副产物醇的指定组成的点反应混合物。

9. 发明申请

US20070260084A1 Industrial Process for Production of High-Purity Diaryl Carbonate 审中-公开
公开(公告)号：US20070260084A1
公开(公告)日：2007-11-08
申请号：US11661611
申请日：2005-10-17
申请人： Shinsuke Fukuoka , Hironori Miyaji , Hiroshi Hachiya , Kazuhiko Matsuzaki
发明人： Shinsuke Fukuoka , Hironori Miyaji , Hiroshi Hachiya , Kazuhiko Matsuzaki
IPC分类号： C07C69/96 , B01D3/14 , C07C68/08
CPC分类号： B01D3/146 , B01D3/009 , C07C68/06 , C07C68/065 , C07C68/08 , C08G64/307 , Y02P20/127 , Y02P20/582 , C07C69/96
摘要： It is an object of the present invention to provide a specific process that enables a high-purity diaryl carbonate that can be used as a raw material of a high-quality and high-performance polycarbonate to be produced stably for a prolonged period of time on an industrial scale of not less than 1 ton/hr using as a starting material a reaction mixture containing an alkyl aryl carbonate obtained through a transesterification reaction between a dialkyl carbonate and an aromatic monohydroxy compound. Although there have been various proposals regarding processes for the production of reaction mixtures containing aromatic carbonates by means of a reactive distillation method or the like, these have all been on a small scale and short operating time laboratory level, and there have been no disclosures on a specific process or apparatus enabling mass production on an industrial scale from such a reaction mixture of a high-purity diaryl carbonate that can be used as a raw material of a high-quality and high-performance polycarbonate. According to the present invention, there is provided a specific process that enables a high-purity diaryl carbonate substantially not containing intermediate boiling point by-products or high boiling point by-products and important as a raw material of a high-quality and high-performance polycarbonate to be produced stably for a prolonged period of time on an industrial scale of not less than 1 ton/hr by taking as a starting material a reaction mixture containing an alkyl aryl carbonate that has been obtained through a transesterification reaction between a dialkyl carbonate and an aromatic monohydroxy compound and subjecting this starting material to a transesterification reaction using a reactive distillation column, and then subjecting a high boiling point reaction mixture obtained from the bottom of the reactive distillation column to separation/purification by distillation using a high boiling point material separating column A, a diaryl carbonate purifying column B and an intermediate boiling point material separating column C in this order, wherein each of these three columns comprises a specified continuous multi-stage distillation column, the high-purity diaryl carbonate being obtained as a side cut component from said purifying column B.

10. 发明申请

US20070219387A1 Industrial Process for Producing an Aromatic Carbonate 审中-公开
标题翻译：生产芳香族碳酸酯的工业方法
公开(公告)号：US20070219387A1
公开(公告)日：2007-09-20
申请号：US11631862
申请日：2005-07-11
申请人： Shinsuke Fukuoka , Hiroshi Hachiya , Kazuhiko Matsuzaki
发明人： Shinsuke Fukuoka , Hiroshi Hachiya , Kazuhiko Matsuzaki
IPC分类号： C07C69/96
CPC分类号： B01D3/146 , C07C68/06 , C07C68/08 , Y02P20/127 , C07C69/96
摘要： It is an object of the present invention to provide, for the case of continuously producing aromatic carbonates containing a diaryl carbonate as a main product by taking an alkyl aryl carbonate containing specific amounts of a dialkyl carbonate and an aromatic monohydroxy compound as a starting material, in which said alkyl aryl carbonate is obtainable through a transesterification reaction between a dialkyl carbonate and an aromatic monohydroxy compound, using a continuous multi-stage distillation column in which a catalyst is present, and continuously feeding the starting material into the continuous multi-stage distillation column, a specific process that enables the diaryl carbonate to be produced with high selectivity and high productivity stably for a prolonged period of time on an industrial scale of not less than 1 ton per hour. Although there have been various proposals regarding processes for the production of aromatic carbonates by means of a reactive distillation method, these have all been on a small scale and short operating time laboratory level, and there have been no disclosures whatsoever on a specific process or apparatus enabling mass production on an industrial scale. According to the present invention, there is provided a specified continuous multi-stage distillation column, and there is also provided a specific process that enables a diaryl carbonate to be produced with high selectivity and high productivity stably for a prolonged period of time on an industrial scale of not less than 1 ton per hour from an alkyl aryl carbonate containing specific amounts of the dialkyl carbonate and the aromatic monohydroxy compound.
摘要翻译：本发明的目的是提供以含碳酸二烷基酯和芳族单羟基化合物作为起始原料的碳酸烷基芳基酯连续制备含有碳酸二芳基酯作为主要成分的芳族碳酸酯的情况，其中所述烷基芳基碳酸酯可通过碳酸二烷基酯和芳族单羟基化合物之间的酯交换反应获得，使用其中存在催化剂的连续多级蒸馏塔，并将原料连续进料到连续多级蒸馏柱，其特征在于能够以不低于1吨/小时的工业规模长时间稳定地以高选择性和高生产率生产碳酸二芳基酯。尽管通过反应性蒸馏法已经有关于生产芳族碳酸酯的方法的各种建议，但这些都是在小规模和短的操作时间实验室水平上，并且在具体方法或装置上没有公开任何内容实现工业规模的批量生产。根据本发明，提供了一种特定的连续多级蒸馏塔，并且还提供了一种能够在工业上长时间稳定地以高选择性和高生产率制备碳酸二芳基酯的具体方法含有特定量的碳酸二烷基酯和芳族单羟基化合物的碳酸烷基芳基酯不小于1吨/小时。

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