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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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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：US07241915B2
公开(公告)日：2007-07-10
申请号：US10361973
申请日：2003-02-11
申请人： Tokumasa Ishida , Yasuhiro Shingai
发明人： Tokumasa Ishida , Yasuhiro Shingai
IPC分类号： C07C67/27 , C07C69/533
摘要： The present invention provides a process for inhibition of polymerization of a (meth)acrylate ester, which has an extremely higher effect of inhibition of polymerization than in cases where conventional polymerization inhibitors are used. In the process for inhibition of polymerization of a (meth)acrylate ester; an N-oxyl compound and at least one member selected from the group consisting of manganese salt compounds, copper salt compounds, 2,2,6,6-tetramethylpiperidine compounds, and nitroso compounds are used together as polymerization inhibitors, and further an acid is used.
摘要翻译： 本发明提供了抑制聚合反应的方法，该方法与使用常规的聚合抑制剂的情况相比，具有极高的聚合抑制效果。 在抑制（甲基）丙烯酸酯的聚合过程中， N-氧基化合物和选自锰盐化合物，铜盐化合物，2,2,6,6-四甲基哌啶化合物和亚硝基化合物中的至少一种作为聚合抑制剂，另外酸是 用过的。
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公开(公告)号：US06706208B2
公开(公告)日：2004-03-16
申请号：US09728179
申请日：2000-12-01
IPC分类号： C09K300
摘要： To sufficiently stabilize a hydroxyalkyl (meth)acrylate in spite of its easily polymerizable property, a hydroxyalkyl saturated-carboxylate and/or alkylene glycol as well as a phenol compound is added thereto.
摘要翻译： 为了充分稳定（甲基）丙烯酸羟烷基酯，尽管其易于聚合的性质，但是向其中加入饱和羧酸羟烷基酯和/或亚烷基二醇以及酚化合物。
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公开(公告)号：US06552218B2
公开(公告)日：2003-04-22
申请号：US09944087
申请日：2001-09-04
IPC分类号： C07C6726
摘要： The present invention provides a process for producing a hydroxyalkyl (meth)acrylate which enables to control sufficiently the formation of a diester at the time of a reaction and/or at the time of distillation. In the process for producing the hydroxyalkyl (meth)acrylate which comprises the step of carrying out a reaction between (meth)acrylic acid and an alkylene oxide in the existence of a catalyst, (1) the reaction between (meth)acrylic acid and the alkylene oxide, or (2) distillation of the resultant hydroxyalkyl (meth)acrylate is performed in the coexistence of a liquid having the relative dielectric constant of not less than 20 at 25° C.
摘要翻译： 本发明提供了一种制备羟基烷基（甲基）丙烯酸酯的方法，其能够充分控制在反应时和/或蒸馏时二酯的形成。在制备（甲基）丙烯酸羟烷基酯的方法中， 其包括在催化剂存在下进行（甲基）丙烯酸和烯化氧反应的步骤，（1）（甲基）丙烯酸与环氧烷之间的反应，或（2）所得物 羟基烷基（甲基）丙烯酸酯在25℃下相对介电常数不小于20的液体共存时进行。
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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：US07045651B2
公开(公告)日：2006-05-16
申请号：US10435992
申请日：2003-05-12
申请人： Tokumasa Ishida , Masahiro Uemura
发明人： Tokumasa Ishida , Masahiro Uemura
IPC分类号： C07C67/26
摘要： The present invention provides a novel production process for a hydroxyalkyl (meth)acrylate, in which it is possible that: in a batch reaction system, the amount of the hydroxyalkyl (meth)acrylate (which is the objective product) as produced is kept nearly on the same level as conventional and further, at the same time, there is suppressed the side production of the alkylene oxide's diaddition product (dialkylene glycol mono(meth)acrylate) that lowers the purity of the product to thus give a bad influence upon its quality. The present invention production process comprises the step of carrying out a batch reaction between (meth)acrylic acid and an alkylene oxide in the presence of a catalyst in order to produce the hydroxyalkyl (meth)acrylate; with the production process being characterized by arranging that the reaction should be initiated in a state of a catalyst concentration of more than 1, wherein the catalyst concentration is defined as the amount of the catalyst as used relative to the integrated amount of the (meth)acrylic acid as supplied and is assumed to be 1 in terms of the amount of the entire catalyst to be used relative to the amount of the entire (meth)acrylic acid to be supplied.
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公开(公告)号：US20080154060A1
公开(公告)日：2008-06-26
申请号：US11659370
申请日：2005-08-05
IPC分类号： C07C59/42
摘要： Processes for producing a hydroxyalkyl(meth)acrylate which comprise reacting (meth)acrylic acid with an alkylene oxide in the presence of a catalyst. A first process is characterized in that the amount of the acid ingredient is kept, on calculation, at 0.010 or more in terms of molar ratio to the catalyst present in the liquid reaction mixture and that the liquid reaction mixture from which the hydroxyalkyl(meth)acrylate has been distilled off is used in the subsequent reaction. A second process is characterized in that a dialkylene glycol mono(meth)acylate is supplied to the reaction system to cause the dialkyleneglycol mono(meth)acylate to coexist in the liquid reaction mixture.
摘要翻译： 制备（甲基）丙烯酸羟烷基酯的方法，其包括在催化剂存在下使（甲基）丙烯酸与烯化氧反应。 第一种方法的特征在于，根据计算，按照与液体反应混合物中存在的催化剂的摩尔比计算酸成分的量为0.010以上，并且其中（甲基）丙烯酸羟烷基酯的液体反应混合物， 蒸馏出的丙烯酸酯用于随后的反应。 第二种方法的特征在于向反应体系中加入单（甲基）丙烯酸二亚烷基二醇酯，以使液体反应混合物中的二烷基二醇单（甲基）酰化物共存。
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公开(公告)号：US08203018B2
公开(公告)日：2012-06-19
申请号：US11659370
申请日：2005-08-05
摘要： Processes for producing a hydroxyalkyl(meth)acrylate which comprise reacting (meth)acrylic acid with an alkylene oxide in the presence of a catalyst. A first process is characterized in that the amount of the acid ingredient is kept, on calculation, at 0.010 or more in terms of molar ratio to the catalyst present in the liquid reaction mixture and that the liquid reaction mixture from which the hydroxyalkyl(meth)acrylate has been distilled off is used in the subsequent reaction. A second process is characterized in that a dialkylene glycol mono(meth)acylate is supplied to the reaction system to cause the dialkyleneglycol mono(meth)acylate to coexist in the liquid reaction mixture.
摘要翻译： 制备（甲基）丙烯酸羟烷基酯的方法，其包括在催化剂存在下使（甲基）丙烯酸与烯化氧反应。 第一种方法的特征在于，根据计算，按照与液体反应混合物中存在的催化剂的摩尔比计算酸成分的量为0.010以上，并且其中（甲基）丙烯酸羟烷基酯的液体反应混合物， 蒸馏出的丙烯酸酯用于随后的反应。 第二种方法的特征在于向反应体系中加入单（甲基）丙烯酸二亚烷基二醇酯，以使液体反应混合物中的二烷基二醇单（甲基）酰化物共存。
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