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1. 发明授权

US07714047B2 Process for producing aqueous fluoropolymer dispension and aqueous fluoropolymer dispersion 有权
标题翻译：生产含氟聚合物含水量和含氟聚合物含水分散体的方法
公开(公告)号：US07714047B2
公开(公告)日：2010-05-11
申请号：US12476172
申请日：2009-06-01
申请人： Nobuhiko Tsuda , Chie Sawauchi , Yasuhiko Sawada , Tetsuo Shimizu
发明人： Nobuhiko Tsuda , Chie Sawauchi , Yasuhiko Sawada , Tetsuo Shimizu
IPC分类号： C08K5/41
CPC分类号： C08F6/20 , C08F6/16 , C08F14/18 , C08F14/26 , C08F214/26 , C08L27/12 , C08F2/16
摘要： The present invention provides a method of producing a fluoropolymer aqueous dispersion by which the fluorine-containing emulsifier contained in the fluoropolymer aqueous dispersion as obtained after polymerization can be efficiently removed as well as a fluoropolymer aqueous dispersion low in fluorine-containing emulsifier concentration. The present invention is a method of producing a fluoropolymer aqueous dispersion which comprises carrying out a concentration treatment comprising a concentration operation of a pretreatment fluoropolymer aqueous dispersion, wherein the pretreatment fluoropolymer aqueous dispersion is obtained by carrying out a polymerization in an aqueous medium in the presence of a fluorine-containing surfactant (A), the fluorine-containing surfactant (A) is a fluorine-containing surfactant having an octanol/water partition coefficient of 1.5 to 3.5.
摘要翻译：本发明提供一种含氟聚合物水性分散体的制造方法，其中可以有效地除去聚合后得到的含氟聚合物水分散体中所含的含氟乳化剂以及含氟乳化剂浓度低的含氟聚合物水分散体。本发明是一种含氟聚合物水性分散体的制造方法，其特征在于，进行包含预处理含氟聚合物水分散液的浓缩操作的浓缩处理，其中，所述预处理含氟聚合物水分散体是通过在水性介质中进行聚合而得到的含氟表面活性剂（A）的含氟表面活性剂（A）为辛醇/水分配系数为1.5〜3.5的含氟表面活性剂。

2. 发明申请

US20070155891A1 Water base dispersion of fluorinated polymer and process for producing the same 审中-公开
标题翻译：氟化聚合物的水基分散体及其制备方法
公开(公告)号：US20070155891A1
公开(公告)日：2007-07-05
申请号：US10582107
申请日：2004-12-09
申请人： Nobuhiko Tsuda , Chie Sawauchi , Yasuhiko Sawada , Tetsuo Shimizu
发明人： Nobuhiko Tsuda , Chie Sawauchi , Yasuhiko Sawada , Tetsuo Shimizu
IPC分类号： C08L27/12
CPC分类号： C08J3/03 , C08F6/16 , C08F14/26 , C08F214/26 , C08J2327/12 , C08L27/18 , C08L71/02 , C08L27/12 , C08F2/20 , C08L2666/14
摘要： The object of the present invention is a fluoropolymer aqueous dispersion showing only a moderate viscosity increase upon temperature rise and having a low fluorine-containing anionic surfactant concentration as well as a method of producing such fluoropolymer aqueous dispersion. The present invention provides a fluoropolymer aqueous dispersion comprising a particle comprising a fluoropolymer dispersed in an aqueous medium in the presence of a nonionic surfactant, wherein a supernatant for assaying as obtained by subjecting the fluoropolymer aqueous dispersion to 30 minutes of centrifugation at 25° C. and at a gravitational acceleration of 1677 G, when subjected to high-performance liquid chromatography [HPLC] under the conditions of a flow rate of 1.0 ml/minute and a column temperature of 40° C. using an acetonitrile/0.05 M aqueous solution of phosphoric acid (60/40% by volume) mixture as a developing solution, followed by detection at an absorption wavelength at which the nonionic surfactant can be identified, shows a ratio (A1/A0), which is the ratio between the total area (A0) under the detected line and the area (A1) under the detected line over a retention time period shorter than 16 minutes, of not lower than 0.4 and the supernatant for assaying has a fluorine-containing anionic surfactant content of not higher than 100 ppm.
摘要翻译：本发明的目的是提供一种含氟聚合物水性分散体，其含氟聚合物水性分散体的制造方法，仅在温度上升时适度粘度上升，含氟阴离子表面活性剂浓度低的方法。本发明提供一种含氟聚合物水分散体，其包含在非离子表面活性剂存在下分散在含水介质中的含氟聚合物的颗粒，其中通过在25℃下使含氟聚合物水分散体离心30分钟获得的上清液并且在1677G的重力加速度下，在流速为1.0ml /分钟，柱温为40℃的条件下进行高效液相色谱[HPLC]，使用乙腈/0.0M的磷酸（60/40体积％）混合物作为显影液，然后在可以鉴定非离子表面活性剂的吸收波长处进行检测，显示出比例（A≤0.1/ 0 ），其是在检测到的线下的总面积（A ^{0 ）与所检测到的线之间的面积（A ^{1 < 保留时间短于16分钟，不低于 0.4，测定用上清液的含氟阴离子表面活性剂含量不高于100ppm。}}

3. 发明授权

US07696268B2 Process for producing aqueous fluoropolymer dispersion and aqueous fluoropolymer dispersion 有权
标题翻译：制备含氟聚合物含水分散体和含氟聚合物水分散体的方法
公开(公告)号：US07696268B2
公开(公告)日：2010-04-13
申请号：US10577424
申请日：2004-10-29
申请人： Nobuhiko Tsuda , Chie Sawauchi , Yasuhiko Sawada , Tetsuo Shimizu
发明人： Nobuhiko Tsuda , Chie Sawauchi , Yasuhiko Sawada , Tetsuo Shimizu
IPC分类号： C08K5/42
CPC分类号： C08F6/20 , C08F6/16 , C08F14/18 , C08F14/26 , C08F214/26 , C08L27/12 , C08F2/16
摘要： The present invention provides a method of producing a fluoropolymer aqueous dispersion by which the fluorine-containing emulsifier contained in the fluoropolymer aqueous dispersion as obtained after polymerization can be efficiently removed as well as a fluoropolymer aqueous dispersion low in fluorine-containing emulsifier concentration. The present invention is a method of producing a fluoropolymer aqueous dispersion which comprises carrying out a concentration treatment comprising a concentration operation of a pretreatment fluoropolymer aqueous dispersion, wherein the pretreatment fluoropolymer aqueous dispersion is obtained by carrying out a polymerization in an aqueous medium in the presence of a fluorine-containing surfactant (A), the fluorine-containing surfactant (A) is a fluorine-containing surfactant having an octanol/water partition coefficient of 1.5 to 3.5.
摘要翻译：本发明提供一种含氟聚合物水性分散体的制造方法，其中可以有效地除去聚合后得到的含氟聚合物水分散体中所含的含氟乳化剂以及含氟乳化剂浓度低的含氟聚合物水分散体。本发明是一种含氟聚合物水性分散体的制造方法，其特征在于，进行包含预处理含氟聚合物水分散液的浓缩操作的浓缩处理，其中，所述预处理含氟聚合物水分散体是通过在水性介质中进行聚合而得到的含氟表面活性剂（A）的含氟表面活性剂（A）为辛醇/水分配系数为1.5〜3.5的含氟表面活性剂。

4. 发明申请

US20090239994A1 PROCESS FOR PRODUCING AQUEOUS FLUOROPOLYMER DISPERSION AND AQUEOUS FLUOROPOLYMER DISPERSION 有权
标题翻译：生产水性氟聚合物分散体和水性氟聚合物分散体的方法
公开(公告)号：US20090239994A1
公开(公告)日：2009-09-24
申请号：US12476172
申请日：2009-06-01
申请人： Nobuhiko Tsuda , Chie Sawauchi , Yasuhiko Sawada , Tetsuo Shimizu
发明人： Nobuhiko Tsuda , Chie Sawauchi , Yasuhiko Sawada , Tetsuo Shimizu
IPC分类号： C08L27/18
CPC分类号： C08F6/20 , C08F6/16 , C08F14/18 , C08F14/26 , C08F214/26 , C08L27/12 , C08F2/16
摘要： The present invention provides a method of producing a fluoropolymer aqueous dispersion by which the fluorine-containing emulsifier contained in the fluoropolymer aqueous dispersion as obtained after polymerization can be efficiently removed as well as a fluoropolymer aqueous dispersion low in fluorine-containing emulsifier concentration. The present invention is a method of producing a fluoropolymer aqueous dispersion which comprises carrying out a concentration treatment comprising a concentration operation of a pretreatment fluoropolymer aqueous dispersion, wherein the pretreatment fluoropolymer aqueous dispersion is obtained by carrying out a polymerization in an aqueous medium in the presence of a fluorine-containing surfactant (A), the fluorine-containing surfactant (A) is a fluorine-containing surfactant having an octanol/water partition coefficient of 1.5 to 3.5.
摘要翻译：本发明提供一种含氟聚合物水性分散体的制造方法，其中可以有效地除去聚合后得到的含氟聚合物水分散体中所含的含氟乳化剂以及含氟乳化剂浓度低的含氟聚合物水分散体。本发明是一种含氟聚合物水性分散体的制造方法，其特征在于，进行包含预处理含氟聚合物水分散液的浓缩操作的浓缩处理，其中，所述预处理含氟聚合物水分散体是通过在水性介质中进行聚合而得到的含氟表面活性剂（A）的含氟表面活性剂（A）为辛醇/水分配系数为1.5〜3.5的含氟表面活性剂。

5. 发明申请

US20070135558A1 Process for producing aqueous fluoropolymer dispersion and aqueous fluoropolymer dispersion 有权
标题翻译：制备含氟聚合物含水分散体和含氟聚合物含水分散体的方法
公开(公告)号：US20070135558A1
公开(公告)日：2007-06-14
申请号：US10577424
申请日：2004-10-29
申请人： Nobuhiko Tsuda , Chie Sawauchi , Yasuhiko Sawada , Tetsuo Shimizu
发明人： Nobuhiko Tsuda , Chie Sawauchi , Yasuhiko Sawada , Tetsuo Shimizu
IPC分类号： D06M15/277
CPC分类号： C08F6/20 , C08F6/16 , C08F14/18 , C08F14/26 , C08F214/26 , C08L27/12 , C08F2/16
摘要： The present invention provides a method of producing a fluoropolymer aqueous dispersion by which the fluorine-containing emulsifier contained in the fluoropolymer aqueous dispersion as obtained after polymerization can be efficiently removed as well as a fluoropolymer aqueous dispersion low in fluorine-containing emulsifier concentration. The present invention is a method of producing a fluoropolymer aqueous dispersion which comprises carrying out a concentration treatment comprising a concentration operation of a pretreatment fluoropolymer aqueous dispersion, wherein the pretreatment fluoropolymer aqueous dispersion is obtained by carrying out a polymerization in an aqueous medium in the presence of a fluorine-containing surfactant (A), the fluorine-containing surfactant (A) is a fluorine-containing surfactant having an octanol/water partition coefficient of 1.5 to 3.5.
摘要翻译：本发明提供一种含氟聚合物水性分散体的制造方法，其中可以有效地除去聚合后得到的含氟聚合物水分散体中所含的含氟乳化剂以及含氟乳化剂浓度低的含氟聚合物水分散体。本发明是一种含氟聚合物水性分散体的制造方法，其特征在于，进行包含预处理含氟聚合物水分散液的浓缩操作的浓缩处理，其中，所述预处理含氟聚合物水分散体是通过在水性介质中进行聚合而得到的含氟表面活性剂（A）的含氟表面活性剂（A）为辛醇/水分配系数为1.5〜3.5的含氟表面活性剂。

6. 发明申请

US20080114118A1 Method For Producing Fluorine-Containing Elastomer Polymer 审中-公开
标题翻译：生产含氟弹性体聚合物的方法
公开(公告)号：US20080114118A1
公开(公告)日：2008-05-15
申请号：US11547637
申请日：2005-04-05
申请人： Nobuhiko Tsuda , Yoshiki Tanaka , Shigeru Morita , Yasuhiko Sawada , Tetsuo Shimizu
发明人： Nobuhiko Tsuda , Yoshiki Tanaka , Shigeru Morita , Yasuhiko Sawada , Tetsuo Shimizu
IPC分类号： C08L27/12 , C08F16/24
CPC分类号： C08F14/18 , C08F2/16
摘要： Disclosed is a method for producing a fluorine-containing elastomer polymer which is excellent in productivity and crosslinkability. Specifically disclosed is a method for producing a fluorine-containing elastomer polymer wherein a fluorine-containing monomer is polymerized in an aqueous solvent in the presence of an emulsifying agent containing a fluorine-containing vinyl group and a chain transfer agent. This method for producing a fluorine-containing elastomer polymer is characterized in that the emulsifying agent containing a fluorine-containing vinyl group is composed of a compound having a radically polymerizable unsaturated bond and a hydrophilic group in a molecule.
摘要翻译：公开了一种生产性和交联性优异的含氟弹性体聚合物的制造方法。具体公开了一种含氟弹性体聚合物的制造方法，其中含氟单体在含有含氟乙烯基和链转移剂的乳化剂存在下，在含水溶剂中聚合。该含氟弹性体聚合物的制造方法的特征在于，含有含氟乙烯基的乳化剂由分子内具有自由基聚合性不饱和键和亲水性基团的化合物构成。

7. 发明授权

US09096701B2 Aqueous tetrafluoroethylene polymer dispersion, process for producing the same, tetrafluoroethylene polymer powder, and molded tetrafluoroethylene polymer 有权
标题翻译：四氟乙烯聚合物水分散体，其制备方法，四氟乙烯聚合物粉末和四氟乙烯聚合物
公开(公告)号：US09096701B2
公开(公告)日：2015-08-04
申请号：US13599986
申请日：2012-08-30
申请人： Nobuhiko Tsuda , Yoshinori Nanba , Yasuhiko Sawada , Tetsuo Shimizu
发明人： Nobuhiko Tsuda , Yoshinori Nanba , Yasuhiko Sawada , Tetsuo Shimizu
IPC分类号： C08F214/26 , C08F14/26
CPC分类号： C08F214/26 , C08F14/26 , C08F2/16
摘要： The present invention provides a tetrafluoroethylene polymer aqueous dispersion obtained by carrying out a TFE polymerization in an aqueous medium in the presence of a fluorovinyl group-containing emulsifier, wherein the TFE polymer aqueous dispersion contains a particle comprising a TFE polymer dispersed in the aqueous medium, the fluorovinyl group-containing emulsifier comprises a fluorovinyl group-containing compound, and the TFE polymer aqueous dispersion has a fluorine-containing surfactant content of not higher than 1000 ppm by mass.
摘要翻译：本发明提供一种四氟乙烯聚合物水分散体，其通过在含氟乙烯基的乳化剂的存在下在水性介质中进行TFE聚合而得到，其中TFE聚合物水分散体含有包含分散在水性介质中的TFE聚合物的颗粒，含有氟乙烯基的乳化剂含有含氟乙烯基的化合物，TFE聚合物水性分散体的含氟表面活性剂含量不高于1000质量ppm。

8. 发明申请

US20060223924A1 Method for producing fluorine-containing ploymer, aqueous dispersion of fluorine-containing polymer,2-acyloxycarboxylic acid derivative , and surface active agent 有权
标题翻译：含氟聚合物的制造方法，含氟聚合物的水分散体，2-酰氧基羧酸衍生物，表面活性剂
公开(公告)号：US20060223924A1
公开(公告)日：2006-10-05
申请号：US10564642
申请日：2004-07-16
申请人： Nobuhiko Tsuda , Yoshihiro Yamamoto , Yoshinori Nanba , Yasuhiko Sawada , Tetsuo Shimizu
发明人： Nobuhiko Tsuda , Yoshihiro Yamamoto , Yoshinori Nanba , Yasuhiko Sawada , Tetsuo Shimizu
IPC分类号： C08K5/09 , C07C69/66
CPC分类号： C08F20/22 , C07C69/63 , C08F14/18 , C08K5/10 , C08F2/10
摘要： The present invention provides a method of producing a fluoropolymer, wherein polymerization using a carboxylate ester bond-containing carboxylic acid derivative as a surfactant in an aqueous medium to give the fluoropolymer is conducted, the above carboxylate ester bond-containing carboxylic acid derivative has a carboxylate ester bond and —COOM (M representing H, NH4, Li, Na or K), the above carboxylate ester bond may optionally be substituted by fluorine atom.
摘要翻译：本发明提供一种含氟聚合物的制造方法，其中在水性介质中使用含羧酸酯键的羧酸衍生物作为表面活性剂进行聚合，得到含氟聚合物，上述含羧酸酯键的羧酸衍生物具有羧酸盐酯键和-COOM（M代表H，NH 4，Li，Na或K），上述羧酸酯键可任选被氟原子取代。

9. 发明授权

US07754796B2 Method for producing fluorine-containing polymer, aqueous dispersion of fluorine-containing polymer, 2-acyloxycarboxylic acid derivative, and surface active agent. 有权
标题翻译：含氟聚合物的制造方法，含氟聚合物的水分散体，2-酰氧基羧酸衍生物和表面活性剂。
公开(公告)号：US07754796B2
公开(公告)日：2010-07-13
申请号：US12494208
申请日：2009-06-29
申请人： Nobuhiko Tsuda , Yoshihiro Yamamoto , Yoshinori Nanba , Yasuhiko Sawada , Tetsuo Shimizu
发明人： Nobuhiko Tsuda , Yoshihiro Yamamoto , Yoshinori Nanba , Yasuhiko Sawada , Tetsuo Shimizu
IPC分类号： C08K5/09 , C08K5/10 , C08F2/26 , C08F14/18 , C08G73/24
CPC分类号： C08F20/22 , C07C69/63 , C08F14/18 , C08K5/10 , C08F2/10
摘要： The present invention provides a method of producing a fluoropolymer, wherein polymerization using a carboxylate ester bond-containing carboxylic acid derivative as a surfactant in an aqueous medium to give the fluoropolymer is conducted, the above carboxylate ester bond-containing carboxylic acid derivative has a carboxylate ester bond and —COOM (M representing H, NH4, Li, Na or K), the above carboxylate ester bond may optionally be substituted by fluorine atom.
摘要翻译：本发明提供一种含氟聚合物的制造方法，其中在水性介质中使用含羧酸酯键的羧酸衍生物作为表面活性剂进行聚合，得到含氟聚合物，上述含羧酸酯键的羧酸衍生物具有羧酸盐酯键和-COOM（M代表H，NH4，Li，Na或K），上述羧酸酯键可以任选被氟原子取代。

10. 发明申请

US20070142513A1 Surfactant, method of producing a fluoropolymer, fluoropolymer aqueous dispersion 审中-公开
标题翻译：表面活性剂，含氟聚合物的制造方法，含氟聚合物水性分散体
公开(公告)号：US20070142513A1
公开(公告)日：2007-06-21
申请号：US11312570
申请日：2005-12-21
申请人： Nobuhiko Tsuda , Yoshinori Nanba , Yasuhiko Sawada , Tetsuo Shimizu
发明人： Nobuhiko Tsuda , Yoshinori Nanba , Yasuhiko Sawada , Tetsuo Shimizu
IPC分类号： C08K5/42
CPC分类号： C08K5/42
摘要： The present invention provides a surfactant making it possible to obtain particles comprising a fluoropolymer at a size smaller in diameter in an aqueous dispersion obtained by polymerization in the presence of the same. The present invention is a surfactant comprising a fluorine-containing-sulfobutanedioic-acid-ester derivative represented by the general formula (i): Y—Rf1—(CH2)m—OCOCH(SO3M)-CH2COO—(CH2)n—Rf2—Y (i) wherein Y represents hydrogen atom or fluorine atom; when Y is hydrogen atom, one of Rf1 and Rf2 is —(CF2CF2)3— and the other is —(CF2CF2)2— or —(CF2CF2)3— and, when Y is fluorine atom, Rf1 and Rf2 are the same or different and each is a divalent hydrocarbon group containing 1 to 4 carbon atoms and containing at least one fluorine atom; m and n are the same or different and each represents an integer of 1 to 3; and M represents NH4, Li, Na, K or H.
摘要翻译：本发明提供了一种表面活性剂，其可以获得包含通过在其存在下通过聚合获得的水分散体中的直径小的含氟聚合物的颗粒。本发明是包含由通式（i）表示的含氟磺基丁二酸 - 酯衍生物的表面活性剂：＆lt;线内配方说明=“在线式”末端=“铅”→> Y - （CH 2） - （O 3 M）-CH 2 - （CH 2）＆lt;＆lt;＆lt; COO-（CH 2）＆gt;＆lt; 2＆lt; 2＆lt; 2＆gt; -Y（i）其中Y代表氢原子或氟原子; 当Y是氢原子时，Rf 1和Rf 2之一是 - （CF 2 CH 2 CH 2）（CF 2）2 - 或 - （CF 2）2 - - - （CF 2）2 - R 2和R 2可以相同或不同，并且当Y是氟原子时，R f'1和R f'2 < 各自是含有1至4个碳原子并含有至少一个氟原子的二价烃基; m和n相同或不同，各自表示1〜3的整数。 M表示NH 4，Li，Na，K或H.

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