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公开(公告)号：US06465682B2
公开(公告)日：2002-10-15
申请号：US09954559
申请日：2001-09-17
IPC分类号： C07C6724
CPC分类号： C07C67/26 , B01J8/10 , B01J19/002 , B01J2208/00176 , B01J2208/00212 , B01J2208/00362 , B01J2208/00867 , B01J2219/00063 , B01J2219/002 , B01J2219/00213 , B01J2219/00225 , B01J2219/00272 , C07C69/54
摘要： In a production process for a hydroxyalkyl ester, comprising the step of carrying out a reaction between a carboxylic acid and an alkylene in the presence of a catalyst, the present invention is to provide: a production process which can stop the reaction economically and sufficiently safely. In a production process which comprises the step of carrying out the reaction between a carboxylic acid and an alkylene in a reactor 1 in the presence of a catalyst so as to produce a hydroxyalkyl ester, the reaction is stopped by introducing a reaction terminating liquid 21 into the reactor 1, wherein the reaction terminating liquid comprises water in a ratio of not less than 50 weight %, and has a low temperature of −5 to 45° C.
摘要翻译： 在羟基烷基酯的制备方法中，包括在催化剂存在下进行羧酸和亚烷基之间的反应的步骤，本发明提供：能够经济地，充分地安全地停止反应的生产方法 。 在包括在催化剂存在下在反应器1中进行羧酸和亚烷基之间的反应以产生羟烷基酯的步骤的生产方法中，通过将反应终止液体21引入到 反应器1，其中反应终止液体包含比例不小于50重量％的水，并且具有-5至45℃的低温。
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公开(公告)号：US06610879B2
公开(公告)日：2003-08-26
申请号：US09901011
申请日：2001-07-10
IPC分类号： C07C6952
摘要： When carrying out a liquid-phase reaction by using a heterogeneous catalyst, the separation of the heterogeneous catalyst and the reaction liquid is carried out certainly and effectively. A reaction method involves carrying out a reaction in liquid phase by using a heterogeneous catalyst particle 30 in a reactor 10, and comprises the steps of: (a) allowing a reaction liquid 40 supplied into the reactor 10 from such as a supplying inlet 12 to react in the presence of the heterogeneous catalyst particle 30, and (b) passing the resultant reaction liquid 40 containing the heterogeneous catalyst particle 30 through a line screen 20 having an opening width where the heterogeneous catalyst particle 30 is not allowed to pass substantially, and then extracting the reaction liquid 40 separated from the heterogeneous catalyst particle 30 from the reactor 10 by way of such as an extracting outlet 14.
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公开(公告)号：US06414182B1
公开(公告)日：2002-07-02
申请号：US09620546
申请日：2000-07-22
申请人： Yasuhiro Shingai , Tokumasa Ishida , Fumio Shibusawa , Tetsuya Kajihara , Yukihiro Yoneda , Hajime Matsumoto , Masatoshi Ueoka
发明人： Yasuhiro Shingai , Tokumasa Ishida , Fumio Shibusawa , Tetsuya Kajihara , Yukihiro Yoneda , Hajime Matsumoto , Masatoshi Ueoka
IPC分类号： C07C6728
摘要： The present invention provide a production process for a hydroxyalkyl ester which comprises the step of carrying out a reaction between a carboxylic acid and an alkylene oxide in the presence of a catalyst, wherein the production process sufficiently enhances the conversion or selectivity in the reaction. The production process is characterized in that the reaction is carried out in a reaction liquid under conditions where a relationship a
摘要翻译： 本发明提供一种羟烷基酯的制备方法，其包括在催化剂存在下，在羧酸和烯化氧之间进行反应的步骤，其中所述制备方法足以提高反应中的转化率或选择性。 其制造方法的特征在于，反应在反应液中，在反应液中保持a
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公开(公告)号：US06534625B2
公开(公告)日：2003-03-18
申请号：US09965699
申请日：2001-09-26
IPC分类号： C08F600
CPC分类号： C07C67/26 , C07C29/106 , C07C67/48 , C07C69/54 , C07C31/202
摘要： The present invention provides a process for producing a hydroxyalkyl (meth)acrylate which comprises the step of carrying out a reaction between (meth)acrylic acid and an alkylene oxide, wherein the process provides enablement for economically and efficiently recovering and recycling the unreacted residue of the alkylene oxide. The process for producing a hydroxyalkyl (meth)acrylate comprises the steps of, carrying out a reaction between (meth)acrylic acid and an alkylene oxide; stripping the unreacted residue of the alkylene oxide from the resultant reaction liquid; and causing a solvent to absorb the stripped alkylene oxide; wherein: water is used as the absorbing solvent; and an absorbing liquid resultant from the absorption of the unreacted residue of the alkylene oxide is used for production of an alkylene glycol.
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公开(公告)号：US06458988B1
公开(公告)日：2002-10-01
申请号：US09664953
申请日：2000-09-16
IPC分类号： C07C6726
摘要： A production process for a hydroxyalkyl(meth)acrylate, which comprises the steps of carrying out a reaction between (meth)acrylic acid and an alkylene oxide and stripping the unreacted residue of the alkylene oxide from the resultant reaction liquid, wherein: (1) the stripping step is performed by use of an inert gas, and the concentration of oxygen in the inert gas is adjusted in the range of 0.1 to 5 mol %; (2) the concentration of the unreacted residue of the (meth)acrylic acid in the resultant reaction liquid is suppressed to not higher than 10 weight %; (3) the difference in operational pressure between the stripping step and the absorption step of causing a solvent to absorb the stripped alkylene oxide is suppressed to not more than 1,000 hPa; (4) the reaction liquid resultant from the reaction is directly supplied to the stripping step without being heated; (5) a part of the liquid left behind in the stripping step is heated and then supplied to the stripping step again; (6) a hydroxyalkyl (meth)acrylate solution is used as the absorbing solvent; (7) a part of the liquid resultant from the absorption step is cooled and then supplied to the absorption step again; or (8) a part or the whole of the absorbing liquid which is on the way of the absorption step is extracted and then cooled and then supplied to the absorption step again.
摘要翻译： （甲基）丙烯酸羟烷基酯的制备方法，其包括以下步骤：从所得反应液体中进行（甲基）丙烯酸和烯化氧之间的反应并从所述环氧烷脱除未反应的残留物，其中：（1） 通过使用惰性气体进行汽提工序，将惰性气体中的氧浓度调整为0.1〜5摩尔％的范围; （2）将所得反应液中的（甲基）丙烯酸的未反应残渣的浓度抑制在10重量％以下。 （3）使汽提步骤和使溶剂吸附汽提的环氧烷的吸收步骤之间的操作压力差被抑制在不超过1,000hPa; （4）将反应产生的反应液直接供给到汽提步骤而不加热; （5）在汽提步骤中留下的一部分液体被加热，然后再次供给到汽提步骤; （6）使用（甲基）丙烯酸羟烷基酯溶液作为吸收溶剂; （7）从吸收步骤得到的液体的一部分被冷却，然后再次供给到吸收步骤; 或者（8）吸收步骤中的吸收液体的一部分或全部被提取，然后冷却，然后再次供给到吸收步骤。
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公开(公告)号：US06465681B2
公开(公告)日：2002-10-15
申请号：US10021061
申请日：2001-12-19
申请人： Masahiro Uemura , Tokumasa Ishida , Yukihiro Yoneda , Tetsuya Kajihara , Yasuhiro Shingai , Tadayoshi Kawashima
发明人： Masahiro Uemura , Tokumasa Ishida , Yukihiro Yoneda , Tetsuya Kajihara , Yasuhiro Shingai , Tadayoshi Kawashima
IPC分类号： C07C6726
摘要： The present invention provides: a production process for a hydroxyalkyl(meth)acrylate, which can raise productivity together with avoiding danger of explosion, and further can suppress side-formation of impurities such as a diester or a monoester wherein the impurities have a bad influence on product quality. When the time from the start of adding an alkylene oxide (AO) till the end of supplying the entirety of the AO is defined as T (hour), the amount of more than 50% of the entirety of the AO is supplied before T/2 (hour) has passed since the start of adding the AO. In addition, when the total amount of an AO as supplied and the time from the start of adding the AO till the end of supplying the entirety of the AO are defined as W (mol) and T (hour) respectively, the supply of the AO is started at a supplying speed V0 (mol/hour) that is faster than the average supplying speed V (=W/T) (mol/hour), and thereafter the supplying speed of the AO is decreased at least once, and then the supply of the entirety of the AO is completed for T (hour) from the start of adding the AO.
摘要翻译： 本发明提供：（甲基）丙烯酸羟烷基酯的制造方法，其能够提高生产率，同时避免爆炸的危险，并且还可以抑制杂质如杂质影响不良的杂质的副产物 对产品质量。 当从添加烯化氧（AO）开始直到提供AO全部结束时的时间定义为T（小时）时，超过全部AO的50％的量在T / 从加入AO开始，已经过了2（小时）。 此外，当供应的AO的总量和从AO的添加开始到提供AO的全部的时间分别被定义为W（mol）和T（小时）时， AO以比平均供给速度V（= W / T）（mol /小时）快）的供给速度V0（mol /小时）开始，此后AO的供给速度至少减少一次，然后 从添加AO开始，T（小时）完成AO的整体供应。
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7.发明授权Process for preserving resin catalyst for addition reaction of alkylene oxide and utilization of this process 失效用于保护用于环氧烷加成反应的树脂催化剂的方法和该方法的利用公开(公告)号：US06858761B2
公开(公告)日：2005-02-22
申请号：US10100766
申请日：2002-03-18
IPC分类号： B01J33/00 , B01J31/08 , C07B61/00 , C07C51/353 , C07C59/42 , C08G65/26 , C08G65/30 , C07C29/10 , B01J20/24 , C07C67/26
CPC分类号： C08G65/2615 , C08G65/2642 , C08G65/30 , Y02P20/584
摘要： The present invention provides a process and its utilization in a process comprising the step of carrying out an addition reaction of an alkylene oxide to an addition-receiving substance in the presence of a resin catalyst, thereby producing the addition reaction product, when the resin catalyst as used for the reaction is persevered so as to recycle it after it is recovered, the unreacted alkylene oxide remaining in the resin catalyst can be prevented from polymerizing and solidifying during the preservation, and the resin catalyst accordingly can be preserved stably for a long time. The resin catalyst as recovered after it is used for the reaction may be preserved under any of the following conditions: 1) at a low temperature of not higher than 40° C.; 2) in the presence of a carboxylic acid; 3) in the presence of a liquid having an alkylene oxide concentration of not more than 2 weight %; and 4) in the coexistence of a carboxylic acid and a liquid having an alkylene oxide concentration of not more than 2 weight %. The present catalyst is recycled for the above addition reaction.
摘要翻译： 本发明提供了一种方法及其在一种方法中的应用，该方法包括在树脂催化剂存在下进行环氧烷与加成物质的加成反应的步骤，由此生成加成反应产物，当树脂催化剂 如反应所用的那样被持续以便在回收之后再循环，可以防止保留在树脂催化剂中的未反应的烯化氧在保存期间聚合和固化，因此可以长时间稳定地保存树脂催化剂 。 用于反应后回收的树脂催化剂可以在以下任一条件下保存：1）在不高于40℃的低温下; 2）在羧酸存在下; 3）在具有不大于2重量％的环氧烷浓度的液体的存在下; 和4）在羧酸和烯化氧浓度不大于2重量％的液体的共存下。 将本催化剂再循环用于上述加成反应。
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8.发明授权公开(公告)号：US06596129B1
公开(公告)日：2003-07-22
申请号：US09702588
申请日：2000-10-31
IPC分类号： B01D500
CPC分类号： B01D3/14 , B01D5/0036 , B01D5/006 , Y10S203/22
摘要： The present invention provides: a process can be preventive of a polymerization in a distillation apparatus when distilling a solution containing easily polymerizable substances such as (meth)acrylic acid and (meth)acrylic acid ester. In the distillation process for an easily polymerizable substance-containing solution which includes the step of distilling an easily polymerizable substance-containing solution by a distillation column equipped with a condenser for condensation at a vapor outlet of the distillation column, at least one condenser for polymerization inhibition is further placed in series on a vapor outlet side of the condenser for condensation, and the easily polymerizable substance which is contained in vapor from an upstream condenser is condensed by a downstream condenser.
摘要翻译： 本发明提供：当蒸馏含有易于聚合的物质如（甲基）丙烯酸和（甲基）丙烯酸酯的溶液时，可以防止蒸馏装置中聚合的方法。 在一种易于聚合的含物溶液的蒸馏方法中，该方法包括通过在蒸馏塔的蒸汽出口处装有冷凝器的蒸馏塔将容易聚合的含有物质的溶液蒸馏的步骤，至少一个聚合用冷凝器 抑制作用进一步串联在冷凝器的蒸汽出口侧，用于冷凝，并且来自上游冷凝器的蒸气中容纳的容易聚合物质通过下游冷凝器冷凝。
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公开(公告)号：US06660881B2
公开(公告)日：2003-12-09
申请号：US09928574
申请日：2001-08-12
申请人： Hajime Matsumoto , Tetsuya Kajihara , Yasuhiro Shingai , Masatoshi Ueoka , Yukihiro Yoneda , Masahiro Uemura , Sei Nakahara , Fumio Munechika
发明人： Hajime Matsumoto , Tetsuya Kajihara , Yasuhiro Shingai , Masatoshi Ueoka , Yukihiro Yoneda , Masahiro Uemura , Sei Nakahara , Fumio Munechika
IPC分类号： C07C6954
摘要： The present invention provides a process for producing a (meth)acrylic ester which enables to obtain a (meth)acrylic ester in an excellent reaction yield. The process for producing a (meth)acrylic ester uses an alcohol and an acid as raw materials and an ion-exchange resin as a catalyst, and the process is characterized by comprising a dehydration step and an esterification step, wherein the esterification reaction step follows the dehydration step in which water impregnated in the ion-exchange resin is removed by using as a dehydrating solvent at least one member selected from the group consisting of the alcohol, the acid, and the resulting ester.
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公开(公告)号：US06452040B2
公开(公告)日：2002-09-17
申请号：US09779205
申请日：2001-02-08
IPC分类号： C07C6726
摘要： The present invention provides a production process for a hydroxyalkyl (meth)acrylate which process enables to maintain the oxygen concentration of a gas phase portion of a reactor within a specific low concentration range in any stage of before adding raw materials, during the reaction, and after the reaction. The production process comprises the step of carrying out a reaction between (meth)acrylic acid and an alkylene oxide in the presence of a catalyst in order to produce the hydroxyalkyl (meth)acrylate, wherein an inert gas and/or a mixed gas of oxygen and an inert gas with a beforehand adjusted oxygen concentration of 0.1 to 14 vol % is used to maintain the oxygen concentration of a gas phase portion of a reactor in the range of 0.1 to 14 vol % (1) before adding the alkylene oxide or (2) during the above reaction or (3) between the completion of the above reaction and the charge for the next reaction. In addition, another production process comprises the step of carrying out a reaction between (meth)acrylic acid and an alkylene oxide in the presence of a catalyst in order to produce the hydroxyalkyl (meth)acrylate, wherein the oxygen concentration of a gas phase portion of a reactor is maintained in the range of 0.1 to 14 vol % throughout the production steps.
摘要翻译： 本发明提供一种（甲基）丙烯酸羟烷基酯的制备方法，该方法能够在反应期间在添加原料之前的任何阶段将反应器的气相部分的氧浓度保持在特定的低浓度范围内，以及 反应后。 该制备方法包括在催化剂存在下进行（甲基）丙烯酸和烯化氧之间的反应以制备（甲基）丙烯酸羟烷基酯的步骤，其中惰性气体和/或氧气的混合气体 使用事先调节氧浓度为0.1〜14体积％的惰性气体，在加入环氧烷之前将反应器的气相部分的氧浓度维持在0.1〜14体积％（1）的范围内，或（ 2）在上述反应期间或（3）完成上述反应和下一反应的电荷之间。 此外，另一种制备方法包括在催化剂存在下进行（甲基）丙烯酸和烯化氧之间的反应以制备（甲基）丙烯酸羟烷基酯的步骤，其中气相部分的氧浓度 的反应器在整个生产步骤中保持在0.1至14体积％的范围内。
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