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1. 发明申请

US20100298595A1 METHOD FOR SEPARATION OF OLEFIN-ALCOHOL AZEOTROPIC MIXTURE 有权
标题翻译：烯烃 - 醇混合物的分离方法
公开(公告)号：US20100298595A1
公开(公告)日：2010-11-25
申请号：US12864475
申请日：2009-01-09
申请人： Yuuki Matsuda , Kazuyoshi Ichihara , Takeomi Hirasaka , Takuya Ichida
发明人： Yuuki Matsuda , Kazuyoshi Ichihara , Takeomi Hirasaka , Takuya Ichida
IPC分类号： C07C67/10 , C07C29/78 , C07C29/80
CPC分类号： C07C17/392 , C07C17/38 , C07C29/78 , C07C67/11 , C07C21/18 , C07C31/12 , C07C69/653
摘要： There is provided a method for separating and collecting at least alcohol with a high purity from an azeotropic mixture of olefin and alcohol.The method conducts the following steps: an azeotropic mixture crystallization step of subjecting an azeotropic mixture of alcohol and olefin represented by the formula: RfCH═CH2 [wherein Rf represents a linear perfluoroalkyl group having 1 to 10 carbon atoms] to a crystallization procedure to separate the mixture into an olefin portion having a higher olefin concentration than that of the original azeotropic mixture and an alcohol portion having a higher alcohol concentration than that of the original azeotropic mixture; and an alcohol purification step of subjecting the separated alcohol portion to either a crystallization procedure or a distillation procedure to separate the alcohol portion into a low-alcohol portion having a lower alcohol concentration than that of the original alcohol portion and a high-alcohol portion having a higher alcohol concentration than that of the original alcohol portion, and thereby collecting alcohol as the high-alcohol portion.
摘要翻译：提供了从烯烃和醇的共沸混合物中分离和收集至少具有高纯度的醇的方法。该方法进行以下步骤：共沸混合物结晶步骤，其对由式R f CH = CH 2 [其中R f表示具有1至10个碳原子的直链全氟烷基]表示的醇和烯烃共沸混合物进行结晶步骤以分离该混合物成为具有比原始共沸混合物更高的烯烃浓度的烯烃部分和具有比原始共沸混合物的醇浓度高的醇部分; 以及醇分离步骤，使分离的醇部分进行结晶过程或蒸馏步骤，以将醇部分分离成具有比原始醇部分低的醇浓度的低醇部分，以及具有比原始醇部分高的醇浓度，从而收集作为高醇部分的醇。

2. 发明授权

US08143440B2 Method for separation of olefin-alcohol azeotropic mixture 有权
标题翻译：分离烯烃 - 醇共沸混合物的方法
公开(公告)号：US08143440B2
公开(公告)日：2012-03-27
申请号：US12864475
申请日：2009-01-09
申请人： Yuuki Matsuda , Kazuyoshi Ichihara , Takeomi Hirasaka , Takuya Ichida
发明人： Yuuki Matsuda , Kazuyoshi Ichihara , Takeomi Hirasaka , Takuya Ichida
IPC分类号： C07C67/10 , C07C31/34
CPC分类号： C07C17/392 , C07C17/38 , C07C29/78 , C07C67/11 , C07C21/18 , C07C31/12 , C07C69/653
摘要： There is provided a method for separating and collecting at least alcohol with a high purity from an azeotropic mixture of olefin and alcohol.The method conducts the following steps: an azeotropic mixture crystallization step of subjecting an azeotropic mixture of alcohol and olefin represented by the formula: RfCH═CH2 [wherein Rf represents a linear perfluoroalkyl group having 1 to 10 carbon atoms] to a crystallization procedure to separate the mixture into an olefin portion having a higher olefin concentration than that of the original azeotropic mixture and an alcohol portion having a higher alcohol concentration than that of the original azeotropic mixture; and an alcohol purification step of subjecting the separated alcohol portion to either a crystallization procedure or a distillation procedure to separate the alcohol portion into a low-alcohol portion having a lower alcohol concentration than that of the original alcohol portion and a high-alcohol portion having a higher alcohol concentration than that of the original alcohol portion, and thereby collecting alcohol as the high-alcohol portion.
摘要翻译：提供了从烯烃和醇的共沸混合物中分离和收集至少具有高纯度的醇的方法。该方法进行以下步骤：共沸混合物结晶步骤，其对由式R f CH = CH 2 [其中R f表示具有1至10个碳原子的直链全氟烷基]表示的醇和烯烃共沸混合物进行结晶步骤以分离该混合物成为具有比原始共沸混合物更高的烯烃浓度的烯烃部分和具有比原始共沸混合物的醇浓度高的醇部分; 以及醇分离步骤，使分离的醇部分进行结晶过程或蒸馏步骤，以将醇部分分离成具有比原始醇部分低的醇浓度的低醇部分，以及具有比原始醇部分高的醇浓度，从而收集作为高醇部分的醇。

3. 发明授权

US07572940B2 Process for producing 2-perfluoroalkylethyl alcohol 有权
标题翻译： 2-全氟烷基乙醇的制备方法
公开(公告)号：US07572940B2
公开(公告)日：2009-08-11
申请号：US12258197
申请日：2008-10-24
申请人： Yuuki Matsuda , Takeomi Hirasaka , Takuya Ichida
发明人： Yuuki Matsuda , Takeomi Hirasaka , Takuya Ichida
IPC分类号： C07C29/09 , C07C29/12
CPC分类号： C07C29/12 , C07C303/24 , C07C305/06 , C07C31/38
摘要： In a first sulfation step, 2-perfluoroalkylethyl iodide is brought into contact with fuming sulfuric acid to obtain a reaction mixture comprising 2-perfluoroalkylethyl sulfate and bis(2-perfluoroalkylethyl)sulfate. Then, in a first hydrolysis step, 2-perfluoroalkylethyl sulfate produced in the first sulfation step is hydrolyzed to obtain a reaction mixture comprising 2-perfluoroalkylethyl alcohol. In a second sulfation step, bis(2-perfluoroalkylethyl)sulfate produced in the first sulfation step is brought into contact with fuming sulfuric acid to obtain a reaction mixture comprising 2-perfluoroalkylethyl sulfate. Then, in a second hydrolysis step, 2-perfluoroalkylethyl sulfate produced in the second sulfation step is hydrolyzed to obtain a reaction mixture comprising 2-perfluoroalkylethyl alcohol. According to such procedures, 2-perfluoroalkylethyl alcohol can be obtained in a high yield.
摘要翻译：在第一次硫酸化步骤中，使2-全氟烷基乙基碘与发烟硫酸接触，得到包含2-全氟烷基乙基硫酸酯和双（2-全氟烷基乙基）硫酸酯的反应混合物。然后，在第一水解步骤中，将在第一硫酸化步骤中生产的2-全氟烷基乙基硫酸酯水解，得到包含2-全氟烷基乙醇的反应混合物。在第二次硫酸化步骤中，将在第一硫酸化步骤中生产的双（2-全氟烷基乙基）硫酸盐与发烟硫酸接触，得到包含2-全氟烷基乙基硫酸酯的反应混合物。然后，在第二水解步骤中，将在第二硫酸化步骤中生产的2-全氟烷基乙基硫酸酯水解，得到包含2-全氟烷基乙醇的反应混合物。根据这样的方法，可以高产率获得2-全氟烷基乙醇。

4. 发明申请

US20090118552A1 PROCESS FOR PRODUCING 2-PERFLUOROALKYLETHYL ALCOHOL 有权
标题翻译：生产2-全氟烷基乙醇的方法
公开(公告)号：US20090118552A1
公开(公告)日：2009-05-07
申请号：US12258197
申请日：2008-10-24
申请人： Yuuki MATSUDA , Takeomi Hirasaka , Takuya Ichida
发明人： Yuuki MATSUDA , Takeomi Hirasaka , Takuya Ichida
IPC分类号： C07C29/09
CPC分类号： C07C29/12 , C07C303/24 , C07C305/06 , C07C31/38
摘要： In a first sulfation step, 2-perfluoroalkylethyl iodide is brought into contact with fuming sulfuric acid to obtain a reaction mixture comprising 2-perfluoroalkylethyl sulfate and bis(2-perfluoroalkylethyl)sulfate. Then, in a first hydrolysis step, 2-perfluoroalkylethyl sulfate produced in the first sulfation step is hydrolyzed to obtain a reaction mixture comprising 2-perfluoroalkylethyl alcohol. In a second sulfation step, bis(2-perfluoroalkylethyl)sulfate produced in the first sulfation step is brought into contact with fuming sulfuric acid to obtain a reaction mixture comprising 2-perfluoroalkylethyl sulfate. Then, in a second hydrolysis step, 2-perfluoroalkylethyl sulfate produced in the second sulfation step is hydrolyzed to obtain a reaction mixture comprising 2-perfluoroalkylethyl alcohol. According to such procedures, 2-perfluoroalkylethyl alcohol can be obtained in a high yield.
摘要翻译：在第一次硫酸化步骤中，使2-全氟烷基乙基碘与发烟硫酸接触，得到包含2-全氟烷基乙基硫酸酯和双（2-全氟烷基乙基）硫酸酯的反应混合物。然后，在第一水解步骤中，将在第一硫酸化步骤中生产的2-全氟烷基乙基硫酸酯水解，得到包含2-全氟烷基乙醇的反应混合物。在第二次硫酸化步骤中，将在第一硫酸化步骤中生产的双（2-全氟烷基乙基）硫酸盐与发烟硫酸接触，得到包含2-全氟烷基乙基硫酸酯的反应混合物。然后，在第二水解步骤中，将在第二硫酸化步骤中生产的2-全氟烷基乙基硫酸酯水解，得到包含2-全氟烷基乙醇的反应混合物。根据这样的方法，可以高产率获得2-全氟烷基乙醇。

5. 发明授权

US08232434B2 Process for producing fluoroalkyl iodide telomer 有权
标题翻译：制备氟烷基碘调聚物的方法
公开(公告)号：US08232434B2
公开(公告)日：2012-07-31
申请号：US12935521
申请日：2009-03-30
申请人： Takeomi Hirasaka , Yoshinori Tanaka
发明人： Takeomi Hirasaka , Yoshinori Tanaka
IPC分类号： C07C17/00 , C07C17/266
CPC分类号： C07C17/278 , C07C17/383
摘要： A novel process for producing a fluoroalkyl iodide telomer is provided, which is able to obtain a fluoroalkyl iodide telomer having a desired chain length, efficiently.A fluoroalkyl iodide represented by the general formula RfI (wherein Rf is a C1-10 fluoroalkyl group) and tetrafluoroethylene are used as a telogen and a taxogen, respectively. These compounds are supplied to a distillation apparatus. In a reaction zone located in an intermediate part of the distillation apparatus, the compounds are subjected to a telomerization reaction in the presence of a metal catalyst with heating to generate a fluoroalkyl iodide telomer represented by the general formula Rf(CF2CF2)nI (wherein Rf is the same as defined above and n is an integer of 1-4). Thereafter, a fraction comprising the fluoroalkyl iodide telomer is separated by distillation.
摘要翻译：提供了一种制备氟代烷基碘调聚物的新方法，其能够有效地获得具有所需链长的氟烷基碘调节物。以通式RfI（其中Rf为C1-10氟代烷基）和四氟乙烯为代表的氟代烷基碘分别用作前体和一种taxogen。将这些化合物供应到蒸馏装置。在位于蒸馏装置的中间部分的反应区中，化合物在金属催化剂的存在下加热进行调聚反应，生成由通式Rf（CF 2 CF 2）n I表示的氟代烷基碘调节物（其中Rf 与上述相同，n为1-4的整数）。此后，通过蒸馏分离包含氟代烷基碘调聚物的馏分。

6. 发明申请

US20080021184A1 Method For Producing Fluorine-Containing (Meth)Acrylic Ester 审中-公开
标题翻译：生产含氟（甲基）丙烯酸酯的方法
公开(公告)号：US20080021184A1
公开(公告)日：2008-01-24
申请号：US11587918
申请日：2005-04-15
申请人： Yoshio Funakoshi , Yoshinori Tanaka , Takeomi Hirasaka
发明人： Yoshio Funakoshi , Yoshinori Tanaka , Takeomi Hirasaka
IPC分类号： C08F118/02
CPC分类号： C07C17/275 , C07C17/278 , C07C17/383 , C07C19/16 , C07C67/11 , C08F214/18 , C08F214/186 , C08F220/14 , C07C21/18 , C07C69/653
摘要： A mixture of fluoroalkyl iodides of the formula C2F5(CF2CF2)nI (“n” is an integer of ≧0) wherein the sum of such fluoroalkyl iodides of n=3 and n=4 contained is ≧85 mol % is provided. This mixture is subjected to an ethylene addition step and an esterification step, and C2F5(CF2CF2)nCH═CH2 and C2F5(CF2CF2)nCH2CH2OH are removed. Thus, there can be obtained a mixture of fluorine-containing (meth)acrylic esters of the formula C2F5(CF2CF2)nCH2CH2OCOCR1═CH2 (wherein R1 represents a hydrogen atom or a methyl group, and “n” is an integer of ≧0) wherein the content of impurities (namely, olefins of the formula C2F5(CF2CF2)nCH═CH2 and alcohols of the formula C2F5(CF2CF2)nCH2CH2OH) is low.
摘要翻译：式C 2氟代烷基碘的混合物（CF 2 CH 2）n 提供了n = 3和n = 4的所述氟代烷基碘的总和为> = 85mol％的（“n”为> = 0的整数）。将该混合物进行乙烯加成步骤和酯化步骤，并且将C 2 F 5 F（CF 2 CF 2）（CH 2）2 CH 2 CH 2 CH 2 CH 2 CH 2 CH 2 CH 2 CH 2 CH 2 C 除去CH 2，CH 2，OH 2 OH。因此，可以得到式C 2 F 5的CF 3（CF 2）CF 3的含氟（甲基）丙烯酸酯的混合物， 2 2 CH 2 CH 2 2 OCOCR 1 -CH 2 /其中R 1表示氢原子或甲基，“n”为> = 0的整数），其中杂质含量（即式C

7. 发明申请

US20070244338A1 Method for Producing Fluorine-Containing Acrylic Ester 审中-公开
标题翻译：生产含氟丙烯酸酯的方法
公开(公告)号：US20070244338A1
公开(公告)日：2007-10-18
申请号：US11587597
申请日：2005-04-15
申请人： Yoshio Funakoshi , Takeomi Hirasaka , Yoshinori Tanaka
发明人： Yoshio Funakoshi , Takeomi Hirasaka , Yoshinori Tanaka
IPC分类号： C07C69/62 , C07C31/34
CPC分类号： C07C67/08 , C07C17/275 , C07C17/278 , C07C17/383 , C07C19/16 , C08F14/18 , C08F220/24 , C07C69/653 , C08F2/02
摘要： A mixture of fluoroalkyl alcohols represented by C2F5(CF2CF2)nCH2CH2OH wherein “n” is an integer equal to or more than 0 wherein the sum of the fluoroalkyl alcohols of n=3 and n=4 contained is 85 mol % or more is prepared and reacted with an acrylic acid compound followed by removing unreacted C2F5(CF2CF2)nCH2CH2OH, to give a mixture of fluorine-containing acrylic esters wherein the content of impurities (that is, olefins represented by C2F5(CF2CF2)nCH═CH2 and the alcohols represented by C2F5(CF2CF2)nCH2CH2OH) is low.
摘要翻译：由C 2 F 5表示的氟烷基醇的混合物（CF 2 CO 2 2）其中“n”是等于或大于0的整数，其中n = 3和n = 4的氟烷基醇的总和含量为85摩尔％以上，并与丙烯酸化合物反应，然后除去未反应的C 2 H 5 F（CF 2 CH 2） 2 N 2 CH 2 CH 2 OH，得到含氟丙烯酸酯的混合物，其中含量为杂质（即，由C 2 F 5表示的烯烃（CF 2 CO 2）n CH 2 CH 2和由C 2 H 5表示的醇（CF 2 CH 2） SUB 2 CH 2 CH 2 CH 2）低。

8. 发明申请

US20110028768A1 PROCESS FOR PRODUCING FLUOROALKYL IODIDE TELOMER 有权
标题翻译：生产氟代碘化物TELOMER的方法
公开(公告)号：US20110028768A1
公开(公告)日：2011-02-03
申请号：US12935521
申请日：2009-03-30
申请人： Takeomi Hirasaka , Yoshinori Tanaka
发明人： Takeomi Hirasaka , Yoshinori Tanaka
IPC分类号： C07C17/383
CPC分类号： C07C17/278 , C07C17/383
摘要： A novel process for producing a fluoroalkyl iodide telomer is provided, which is able to obtain a fluoroalkyl iodide telomer having a desired chain length, efficiently.A fluoroalkyl iodide represented by the general formula RfI (wherein Rf is a C1-10 fluoroalkyl group) and tetrafluoroethylene are used as a telogen and a taxogen, respectively. These compounds are supplied to a distillation apparatus. In a reaction zone located in an intermediate part of the distillation apparatus, the compounds are subjected to a telomerization reaction in the presence of a metal catalyst with heating to generate a fluoroalkyl iodide telomer represented by the general formula Rf(CF2CF2)nI (wherein Rf is the same as defined above and n is an integer of 1-4). Thereafter, a fraction comprising the fluoroalkyl iodide telomer is separated by distillation.
摘要翻译：提供了一种制备氟代烷基碘调聚物的新方法，其能够有效地获得具有所需链长的氟烷基碘调节物。以通式RfI（其中Rf为C1-10氟代烷基）和四氟乙烯为代表的氟代烷基碘分别用作开环素和紫杉醇。将这些化合物供应到蒸馏装置。在位于蒸馏装置的中间部分的反应区中，化合物在金属催化剂的存在下加热进行调聚反应，生成由通式Rf（CF 2 CF 2）n I表示的氟代烷基碘调节物（其中Rf 与上述相同，n为1-4的整数）。此后，通过蒸馏分离包含氟代烷基碘调聚物的馏分。

9. 发明申请

US20070232766A1 Method for Producing Fluorine-Containing Acrylic Ester 审中-公开
标题翻译：生产含氟丙烯酸酯的方法
公开(公告)号：US20070232766A1
公开(公告)日：2007-10-04
申请号：US11587599
申请日：2005-04-15
申请人： Takeomi Hirasaka , Yoshinori Tanaka , Yoshio Funakoshi , Osamu Yamamoto
发明人： Takeomi Hirasaka , Yoshinori Tanaka , Yoshio Funakoshi , Osamu Yamamoto
IPC分类号： C08F120/22 , C08F118/02 , C08F18/20 , C08F2/00 , C08F20/22 , C08F218/00 , C08F220/22 , C08F6/00
CPC分类号： C07C17/383 , C07C67/54 , C07C21/18 , C07C69/653
摘要： A mixture of fluorine-containing acrylic esters represented by CF3(CF2)nCH2CH2OCOCR1═CH2 wherein R1 is a hydrogen atom, a methyl group or a halogen atom and “n” is an integer of at least zero is subjected to distillation under such conditions that the esters are not polymerized, so as to give a mixture of the esters with a less content of impurities (that is, olefins represented by CF3(CF2)nCH═CH2 and alcohols represented by CF3(CF2)nCH2CH2OH) at a high yield.
摘要翻译：由CF 3表示的含氟丙烯酸酯的混合物（CF 2 N 2）2 CH 2 其中R 1是氢原子，甲基或卤素原子，“n”是氢原子， “是至少为零的整数在使酯不聚合的条件下进行蒸馏，从而得到具有较少含量杂质的酯的混合物（即，由CF 3表示的烯烃< （CF 2）2 CH 2 CH 2和由CF 3代表的醇（CF _{> 2 CH 2 CH 2 CH 2 OH）。}

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