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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

US08093437B2 Industrial process for production of diol 有权
标题翻译：生产二醇的工业过程
公开(公告)号：US08093437B2
公开(公告)日：2012-01-10
申请号：US11991419
申请日：2007-01-19
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： C07C29/128 , B01D3/009 , B01D3/22 , B01D3/32 , C07C68/065 , Y02P20/127 , C07C69/96 , C07C31/202
摘要： The invention provides an apparatus and process for producing a diol by taking a cyclic carbonate and an 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 as a column top component and a side cut component so as to obtain a column bottom component, continuously feeding the column bottom component into column C, and obtaining the diol.
摘要翻译：本发明提供一种通过以环状碳酸酯和脂肪族一元醇为原料制备二醇的装置和方法，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中所含的二醇的沸点的材料作为塔顶成分和侧馏分，蒸馏出塔底成分，将塔底成分连续供给塔C ，得到二醇。

7. 发明授权

US08058465B2 Process for industrially producing dialkyl carbonate and diol 有权
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：US08058465B2
公开(公告)日：2011-11-15
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
CPC分类号： C07C68/065 , B01D3/32 , C07C29/128 , Y02P20/127 , Y02P20/52 , C07C69/96 , C07C31/202
摘要： A process for industrially producing dialkyl carbonate and a diol continuously through a reactive distillation system is disclosed. The process includes the steps 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, carrying out reaction and distillation simultaneously in the column, continuously withdrawing a low boiling point reaction mixture containing the produced dialkyl carbonate from an upper portion of the column in a gaseous form, and continuously withdrawing a high boiling point reaction mixture containing the diol from a lower portion of the column in a liquid form. 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.
摘要翻译：公开了一种通过反应蒸馏系统连续生产碳酸二烷基酯和二醇的方法。该方法包括以环状碳酸酯和脂肪族一元醇为起始原料，连续将原料连续供入连续多级蒸馏塔中，其中存在催化剂，在塔内同时进行反应和蒸馏从气体形式的塔的上部排出含有生成的碳酸二烷基酯的低沸点反应混合物，并以液体形式连续地从塔的下部抽出含有二醇的高沸点反应混合物。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。

8. 发明授权

US08049028B2 Industrial process for separating out dialkyl carbonate 有权
标题翻译：用于分离碳酸二烷基酯的工业方法
公开(公告)号：US08049028B2
公开(公告)日：2011-11-01
申请号：US11991073
申请日：2006-12-15
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 , B01D3/009 , B01D3/32 , C07C68/08 , Y02P20/127 , Y02P20/582 , C07C69/96
摘要： It is an object of the present invention to provide a specific apparatus and process for using a single distillation column on a low boiling point reaction mixture containing a large amount of a dialkyl carbonate and an aliphatic monohydric alcohol produced through a reactive distillation process of taking a cyclic carbonate and the aliphatic monohydric alcohol as starting materials, continuously feeding the starting materials into a continuous multi-stage distillation column in which a homogeneous catalyst is present, and carrying out reaction and distillation simultaneously in the column, so as to separate the low boiling point reaction mixture by distillation into a column top component BT having the aliphatic monohydric alcohol as a main component thereof and a column bottom component BB having the dialkyl carbonate as a main component thereof stably for a prolonged period of time industrially.
摘要翻译：本发明的目的是提供一种在含有大量碳酸二烷基酯和通过反应蒸馏方法生产的脂族一元醇的低沸点反应混合物上使用单一蒸馏塔的具体装置和方法，环状碳酸酯和脂肪族一元醇作为起始原料，将起始原料连续进料到其中存在均相催化剂的连续多级蒸馏塔中，并在塔中同时进行反应和蒸馏，以分离低沸点通过蒸馏将具有脂肪族一元醇作为主要成分的塔顶成分BT和以碳酸二烷基酯为主要成分的塔底成分BB在工业上稳定地延长时间。

9. 发明授权

US07812189B2 Industrial process for production of high-purity diphenyl carbonate 有权
标题翻译：生产高纯度碳酸二苯酯的工业方法
公开(公告)号：US07812189B2
公开(公告)日：2010-10-12
申请号：US11660362
申请日：2005-08-24
申请人： Shinsuke Fukuoka , Hiroshi Hachiya , Kazuhiko Matsuzaki , Hironori Miyaji
发明人： Shinsuke Fukuoka , Hiroshi Hachiya , Kazuhiko Matsuzaki , Hironori Miyaji
IPC分类号： C07C69/96
CPC分类号： B01D3/143 , B01D3/009 , C07C68/06 , C07C68/08 , Y02P20/127 , C07C69/96
摘要： According to the present invention, there are provided a high boiling point material separating column A and a diphenyl carbonate purifying column B each comprising a continuous multi-stage distillation column having specified structures, and there is provided a specific process that enables a high-purity diphenyl carbonate which is 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 from a reaction mixture containing the diphenyl carbonate using an apparatus in which these two continuous multi-stage distillation columns are connected together.
摘要翻译：根据本发明，提供了一种分离塔A和碳酸二苯酯精制塔B的高沸点物质，它们均包含具有特定结构的连续多级蒸馏塔，并且提供了能够获得高纯度碳酸二苯酯作为高质量，高性能的聚碳酸酯的原料，以不低于1吨/小时的工业规模从含有碳酸二苯酯的反应混合物中长时间稳定地制备而成，其使用这两个连续多级蒸馏塔连接在一起的装置。

10. 发明申请

US20090270656A1 Industrial Process for Producing High-Purity Diol 审中-公开
标题翻译：生产高纯度二醇的工业方法
公开(公告)号：US20090270656A1
公开(公告)日：2009-10-29
申请号：US11991387
申请日：2007-01-26
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： C07C31/20 , C07C29/80 , B01J10/00
CPC分类号： C07C68/065 , B01D3/009 , B01D3/146 , B01D3/32 , C07C29/128 , C07C29/80 , Y02P20/127 , C07C69/96 , C07C31/202
摘要： It is an object of the present invention to provide a specific apparatus and process for industrially producing a high-purity diol by taking a cyclic carbonate and an aliphatic monohydric alcohol as starting materials. Moreover, it is an object to thus provide a specific industrial apparatus and industrial production process that are inexpensive and, for example, enable the high-purity diol to be produced in an amount of not less than 1 ton/hr, preferably not less than 2 tons/hr, more preferably not less than 3 tons/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). According to the present invention, the above objects can be attained by using a continuous multi-stage distillation column A, a continuous multi-stage distillation column C, and a continuous multi-stage distillation column E, which have a specified structure, and withdrawing a liquid component from the side cut outlet, which is installed at the bottom of a chimney tray having a specified structure installed in an enrichment section of the continuous multi-stage distillation column E.
摘要翻译：本发明的目的是提供一种通过以环状碳酸酯和脂族一元醇为起始原料工业生产高纯度二醇的具体装置和方法。此外，其目的是提供廉价的特定的工业设备和工业生产方法，例如使得能够以不低于1吨/小时的量生产高纯度二醇，优选不低于 2吨/小时，更优选不小于3吨/小时，稳定地长时间（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）。根据本发明，上述目的可以通过使用具有特定结构的连续多级蒸馏塔A，连续多级蒸馏塔C和连续多级蒸馏塔E来实现，来自侧切口的液体成分安装在连续多级蒸馏塔E的富集部分中的具有特定结构的烟囱式塔盘的底部。

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