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1. 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。

2. 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。

3. 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.

4. 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。

5. 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.

6. 发明授权

US08071819B2 Industrial process for production of high-purity diol 有权
标题翻译：工业生产高纯度二醇的工艺
公开(公告)号：US08071819B2
公开(公告)日：2011-12-06
申请号：US11991292
申请日：2006-12-28
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： C07C31/18 , B01J19/00 , B01D3/00
CPC分类号： C07C29/80 , B01D3/008 , B01D3/009 , B01D3/20 , B01D3/22 , B01D3/32 , C07C29/128 , C07C68/065 , Y02P20/127 , C07C69/96 , C07C31/202
摘要： The invention provides an apparatus and process for producing high-purity diol by taking cyclic carbonate and aliphatic monohydric alcohol as starting materials, continuously feeding the starting materials into column A, carrying out reactive distillation in column A, continuously withdrawing a low boiling point reaction mixture containing a produced dialkyl carbonate and the aliphatic monohydric alcohol from an upper portion of column A, continuously withdrawing a high boiling point reaction mixture containing a produced diol from a lower portion of column A, continuously feeding the high boiling point reaction mixture into distillation column C, distilling off material having a lower boiling point than that of the diol contained in the high boiling point reaction mixture AB as a column top component and/or a side cut component so as to obtain a column bottom component, continuously feeding the column bottom component into distillation column E, and obtaining the diol.
摘要翻译：本发明提供一种以环状碳酸酯和脂肪族一元醇为原料制备高纯度二醇的装置和方法，将原料连续供给到塔A中，在塔A中进行反应性蒸馏，连续取出低沸点反应混合物从塔A的上部含有生成的碳酸二烷基酯和脂肪族一元醇，从塔A的下部连续取出含有生成的二醇的高沸点反应混合物，将高沸点反应混合物连续供给到蒸馏塔C 将沸点低于高沸点反应混合物AB中所含的二醇作为塔顶成分和/或侧馏分成分的材料蒸馏出来，从而得到塔底成分，将塔底成分加入蒸馏塔E中，得到二醇。

7. 发明授权

US07884251B2 Industrial process for separating out by-produced alcohols 有权
标题翻译：用于分离副产物醇的工业过程
公开(公告)号：US07884251B2
公开(公告)日：2011-02-08
申请号：US11660900
申请日：2005-09-12
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： C07C27/10
CPC分类号： B01D3/009 , B01D3/143 , B01D3/16 , C07C29/80 , C07C68/06 , C07C68/08 , Y02P20/127 , Y02P20/582 , C07C69/96 , C07C31/04
摘要： It is an object of the present invention to provide a specific industrial separation process that enables an alcohol to be separated out efficiently and stably for a prolonged period of time from a large amount of a low boiling point reaction mixture containing a 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 aromatic carbonates the 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 using a continuous multi-stage distillation column having a specified structure enabling the above object to be attained.
摘要翻译：本发明的目的是提供一种具体的工业分离方法，其使得能够从大量含有副产物醇的低沸点反应混合物中有效地和稳定地分离出较长时间的醇，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，大量生产芳族碳酸酯。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，在制造芳香族碳酸酯时能够使副产物醇化的具体方法或装置没有公开，使用反应蒸馏系统的工业规模能够在工业规模上有效且稳定地分离出来不小于200公斤/小时。根据本发明，提出了使用具有能够实现上述目的的特定结构的连续多级蒸馏塔的具体方法。

8. 发明申请

US20090253939A1 Process for industrially producing dialkyl carbonate and diol 审中-公开
标题翻译：工业生产碳酸二烷基酯和二醇的方法
公开(公告)号：US20090253939A1
公开(公告)日：2009-10-08
申请号：US11991075
申请日：2006-11-17
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： C07C45/00
CPC分类号： C07C68/065 , B01D3/22 , B01D3/32 , Y02P20/127 , C07C69/96
摘要： It is an object of the present invention to provide a specific process that enables a dialkyl carbonate and a diol to be produced on an industrial scale of not less than 2 ton/hr and not less than 1.3 ton/hr respectively with high selectivity and high productivity stably for a prolonged period of time through a reactive distillation system of taking a cyclic carbonate and an aliphatic monohydric alcohol as starting materials, continuously feeding the starting materials into a continuous multi-stage distillation column in which a catalyst is present, and carrying out reaction and distillation simultaneously in the column. Although there have been many proposals regarding processes for the production of the dialkyl carbonate and the diol through the 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 specific continuous multi-stage distillation column having a specified structure, and a production process using this continuous multi-stage distillation column, according to which the dialkyl carbonate and the diol can be produced on an industrial scale of not less than 2 ton/hr and not less than 1.3 ton/hr respectively each with a selectivity of not less than 95%, preferably not less than 97%, more preferably not less than 99%, stably for not less than 1000 hours, preferably not less than 3000 hours, more preferably not less than 5000 hours.
摘要翻译：本发明的目的是提供一种能够以不低于2吨/小时并且不低于1.3吨/小时的工业规模生产碳酸二烷基酯和二醇的具有高选择性和高的特定方法通过以环状碳酸酯和脂肪族一元醇为起始原料的反应蒸馏系统，稳定地长时间稳定生产，将原料连续供给到存在催化剂的连续多级蒸馏塔中，并进行在柱中同时进行反应和蒸馏。虽然通过反应蒸馏法生产碳酸二烷基酯和二醇的方法有许多提案，但这些都是在规模小，操作时间短的实验室水平上，并没有公开任何关于具体方法或能够在工业规模上批量生产的设备。根据本发明，提供了具有特定结构的特定连续多级蒸馏塔和使用该连续多级蒸馏塔的制备方法，根据该方法可以在工业上生产碳酸二烷基酯和二醇不小于2吨/小时，不小于1.3吨/小时，选择性不低于95％，优选不低于97％，更优选不低于99％，选择性不低于1000 小时，优选不小于3000小时，更优选不小于5000小时。

9. 发明申请

US20090163734A1 Process for producing high-purity diphenyl carbonate on industrial scale 审中-公开
标题翻译：工业规模生产高纯度碳酸二苯酯的工艺
公开(公告)号：US20090163734A1
公开(公告)日：2009-06-25
申请号：US11991382
申请日：2006-12-12
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： C07C68/065 , C07C68/06 , 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-purity diphenyl carbonate required for producing a high-quality high-performance aromatic polycarbonate 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 cyclic carbonate and a phenol. When producing, from a cyclic carbonate and a phenol, a high-purity diphenyl carbonate required for producing a high-quality high-performance aromatic polycarbonate, the above object can be attained by carrying out a process according to the present invention which comprises steps of: (I) producing a dialkyl carbonate and a diol using a reactive distillation column having a specified structure; (II) producing a diphenyl carbonate using two reactive distillation columns each having a specified structure, and (III) 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.
摘要翻译：本发明的目的是提供一种具体方法，其能够大量生产高品质高性能芳族聚碳酸酯所需的高纯度碳酸二苯酯（例如不小于1吨/小时））从环状碳酸酯和苯酚稳定延长的时间（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）。当从环状碳酸酯和苯酚生产高品质高性能芳族聚碳酸酯所需的高纯度碳酸二苯酯时，可以通过进行本发明的方法来实现上述目的，其中包括以下步骤：：（I）使用具有特定结构的反应性蒸馏塔生产碳酸二烷基酯和二醇; （II）使用两个具有特定结构的反应性蒸馏塔制备碳酸二苯酯，（III）使用高沸点材料分离塔A和碳酸二苯酯精制塔B从碳酸二苯酯得到高纯度碳酸二苯酯。

10. 发明申请

US20090137833A1 Process for industrially producing dialkyl carbonate and diol 有权
公开(公告)号：US20090137833A1
公开(公告)日：2009-05-28
申请号：US11991076
申请日：2006-11-17
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 , B01D3/04
CPC分类号： C07C68/065 , B01D3/32 , C07C29/128 , Y02P20/127 , Y02P20/52 , C07C69/96 , C07C31/202
摘要： It is an object of the present invention to provide a specific process that enables a dialkyl carbonate and a diol to be produced on an industrial scale of not less than 2 ton/hr and not less than 1.3 ton/hr respectively with high selectivity and high productivity stably for a prolonged period of time through a reactive distillation system of taking a cyclic carbonate and an aliphatic monohydric alcohol as starting materials, continuously feeding the starting materials into a continuous multi-stage distillation column in which a catalyst is present, and carrying out reaction and distillation simultaneously in the column. Although there have been many proposals regarding processes for the production of the dialkyl carbonate and the diol through the 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 specific continuous multi-stage distillation column having a specified structure, and a production process using this continuous multi-stage distillation column, according to which the dialkyl carbonate and the diol can be produced on an industrial scale of not less than 2 ton/hr and not less than 1.3 ton/hr respectively each with a selectivity of not less than 95%, preferably not less than 97%, more preferably not less than 99%, stably for not less than 1000 hours, preferably not less than 3000 hours, more preferably not less than 5000 hours.

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