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1. 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。

2. 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。

3. 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。

4. 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。

5. 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.

6. 发明申请

US20090118530A1 Industrial Process for Production of Aromatic Carbonate 审中-公开
标题翻译：工业生产芳香族碳酸酯的工艺
公开(公告)号：US20090118530A1
公开(公告)日：2009-05-07
申请号：US11991473
申请日：2006-12-07
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 , C07C68/06
CPC分类号： C07C68/065 , C07C68/06 , Y02P20/127 , C07C69/96
摘要： It is an object of the present invention to provide a specific process that enables an aromatic 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 an aromatic monohydroxy compound. When producing an aromatic carbonate from a cyclic carbonate and an aromatic monohydroxy compound, the above object can be attained by carrying out a step of: (I) producing a dialkyl carbonate and a diol using a reactive distillation column having a specified structure, and (II) producing the an aromatic carbonate using a first reactive distillation column having a specified structure.
摘要翻译：本发明的一个目的是提供一种特别的方法，其能够使制造高品质高性能芳族聚碳酸酯所需的芳族碳酸酯在工业上大量（例如不小于1吨/小时）稳定地生产来自环状碳酸酯和芳族单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）。当从环状碳酸酯和芳族单羟基化合物制备芳族碳酸酯时，可以通过以下步骤来实现上述目的：（I）使用具有特定结构的反应性蒸馏塔制备碳酸二烷基酯和二醇，和（ II）使用具有特定结构的第一反应蒸馏塔生产芳族碳酸酯。

7. 发明申请

US20090030223A1 PROCESS FOR INDUSTRIALLY PRODUCING DIALKYL CARBONATE AND DIOL WITH HIGH YIELD 审中-公开
标题翻译：工业生产碳酸二乙酯和高铝合金的工艺
公开(公告)号：US20090030223A1
公开(公告)日：2009-01-29
申请号：US11991248
申请日：2006-12-06
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 , C07C31/20 , B01D3/14
CPC分类号： B01D3/009 , B01D3/32 , C07C68/065 , Y02P20/127 , C07C69/96
摘要： It is an object of the present invention to provide a solution by providing 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 are provided a specific continuous multi-stage distillation column having a specified structure, and a production process using this continuous multi-stage distillation column, in 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：本发明的目的是通过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体方法来提供溶液，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，稳定地选择性高，生产稳定，连续地将原料进料到其中存在催化剂的连续多级蒸馏塔中并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生产方法，其中可以以工业规模生产碳酸二烷基酯和二醇不小于2吨/小时，不低于1.3吨/小时，选择性不低于1000小时，选择性不低于95％，优选不低于97％，更优选不低于99％优选为3000小时以上，更优选为5000小时以上。

8. 发明申请

US20080041712A1 Industrial Process For Production Of High-Purity Diphenyl Carbonate 有权
标题翻译：高纯度碳酸二苯酯生产工艺
公开(公告)号：US20080041712A1
公开(公告)日：2008-02-21
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： B01D3/14 , C07C33/00
CPC分类号： B01D3/143 , B01D3/009 , 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 a high-purity diphenyl 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 from a reaction mixture containing a catalyst and reaction by-products that has been obtained through transesterification reaction and the like using a dialkyl carbonate and a phenol as a starting material. 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 to a high-purity diphenyl carbonate that can be used as a raw material of a high-quality and high-performance polycarbonate. 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：本发明的目的是提供一种具体方法，其能够将高纯度碳酸二苯酯用作高质量和高性能聚碳酸酯的原料，以在较长时间内稳定地制备，从含有催化剂的反应混合物和通过酯交换反应等获得的反应副产物使用碳酸二烷基酯和苯酚作为起始原料的工业规模不低于1吨/小时。虽然已经有关于通过反应蒸馏法生产含有芳族碳酸酯的反应混合物的方法的各种建议，但是这些方法都已经在小规模和操作时间短的实验室水平上，并且没有公开具体方法或能够从这种反应混合物到能够用作高质量和高性能聚碳酸酯的原料的高纯度碳酸二苯酯在工业规模上批量生产的装置。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。

9. 发明授权

US08044167B2 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：US08044167B2
公开(公告)日：2011-10-25
申请号：US12508331
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： C07G64/00
CPC分类号： C08G64/307 , B01D3/009 , B01D3/146 , C07C68/06 , C07C68/08 , Y02P20/127 , Y02P20/582 , C07C69/96
摘要： An aromatic polycarbonate that is obtained by transesterification between a high-purity diphenyl carbonate and an aromatic dihydroxy compound. 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. Moreover, it is particularly preferable if a reactive distillation column and the three distillation columns, each of which has a specified structure, and the three distillation columns are each operated under specified distillation conditions.
摘要翻译：通过高纯度碳酸二苯酯和芳族二羟基化合物之间的酯交换获得的芳族聚碳酸酯。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。此外，特别优选的是，反应性蒸馏塔和具有特定结构的三个蒸馏塔和三个蒸馏塔各自在规定的蒸馏条件下运行。

10. 发明授权

US07622601B2 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：US07622601B2
公开(公告)日：2009-11-24
申请号：US11660902
申请日：2005-10-12
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： C08G64/307 , B01D3/009 , B01D3/146 , C07C68/06 , C07C68/08 , Y02P20/127 , Y02P20/582 , C07C69/96
摘要： 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. Moreover, it is particularly preferable if a reactive distillation column and the three distillation columns, each of which has a specified structure, and the three distillation columns are each operated under specified distillation conditions.
摘要翻译：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。此外，特别优选的是，反应性蒸馏塔和具有特定结构的三个蒸馏塔和三个蒸馏塔各自在规定的蒸馏条件下运行。

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