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    Monitoring column breakthrough in a process for removing fluorosurfactant from aqueous fluoropolymer dispersions
    1.
    发明授权
    Monitoring column breakthrough in a process for removing fluorosurfactant from aqueous fluoropolymer dispersions 失效
    在从含氟聚合物水分散体中除去含氟表面活性剂的过程中监测柱的突破

    公开(公告)号：US07671111B2

    公开(公告)日：2010-03-02

    申请号：US11351125

    申请日：2006-02-09

    申请人： Charles Joseph Noelke ,  Steven H. Swearingen ,  David William Johnson

    发明人： Charles Joseph Noelke ,  Steven H. Swearingen ,  David William Johnson

    IPC分类号： C08L1/00

    CPC分类号： C08F6/16 ,  B01J41/05 ,  B01J41/07 ,  C02F2001/422 ,  C02F2101/36 ,  C08J3/03 ,  C08J2327/12 ,  C08L27/12

    摘要： A process for reducing the fluorosurfactant content of a stabilized fluorosurfactant-containing aqueous fluoropolymer dispersion by passing dispersion through a first fixed bed of anion exchange resin to reduce fluorosurfactant content. The first fixed bed has a working zone which moves though the column as the ion exchange resin is saturated. The process includes monitoring a property of the dispersion as the dispersion exits the fixed bed to determine break though of the working zone indicating saturation of the fixed bed. The property being monitored is selected from the group consisting of pH and conductivity.

    摘要翻译： 通过使分散体通过阴离子交换树脂的第一固定床来降低含氟表面活性剂的含水氟聚合物分散体的含氟表面活性剂含量以降低含氟表面活性剂含量的方法。 第一固定床具有当离子交换树脂饱和时通过柱移动的工作区。 该方法包括当分散体离开固定床时监测分散体的性质，以确定指示固定床饱和的工作区的断裂。 被监测的性质选自pH和电导率。

    Processes for the purification and use of 2,2-dichloro-1,1,1,3,3,3-hexafluoropropane and azeotropes thereof with HF
    3.
    发明授权
    Processes for the purification and use of 2,2-dichloro-1,1,1,3,3,3-hexafluoropropane and azeotropes thereof with HF 有权

    公开(公告)号：US06211135B1

    公开(公告)日：2001-04-03

    申请号：US09283448

    申请日：1999-04-01

    申请人： Ralph Newton Miller ,  V. N. Mallikarjuna Rao ,  Steven H. Swearingen

    发明人： Ralph Newton Miller ,  V. N. Mallikarjuna Rao ,  Steven H. Swearingen

    IPC分类号： C11D344

    CPC分类号： C07C19/10 ,  C01B7/195 ,  C01B7/196 ,  C07C17/23 ,  C07C17/38 ,  Y02P20/582 ,  C07C19/08

    摘要： A process is disclosed for the separation of a mixture of HF and CF3CCl2CF3. The process involves placing the mixture in a separation zone at a temperature of from about 0° C. to about 100° C. and at a pressure sufficient to maintain the mixture in the liquid phase, whereby an organic-enriched phase comprising less than 69 mole percent HF is formed as the bottom layer and an HF-enriched phase comprising more than 90 mole percent HF is formed as the top layer. The organic-enriched phase can be withdrawn from the bottom of the separation zone and subjected to distillation in a distillation column to recover essentially pure CF3CCl2CF3. The distillate comprising HF and CF3CCl2CF3 can be removed from the top of the distillation column, while essentially pure CF3CCl2CF3 can be recovered from the bottom of the distillation column. Also, the HF-enriched phase can be withdrawn from the top of the separation zone and subjected to distillation in a distillation column. The distillate comprising HF and CF3CCl2CF3 can be removed from the top of the distillation column while essentially pure HF can be recovered from the bottom of the distillation column. If desired, the two distillates can be recycled to the separation zone. Also disclosed are compositions of hydrogen fluoride in combination with an effective amount of CF3CCl2CF3 to form an azeotrope or azeotrope-like composition with hydrogen fluoride. Included are compositions containing from about 13.8 to 31.3 mole percent CF3CCl2CF3. Also disclosed is a process for producing 1,1,1,3,3,3-hexafluoropropane from a mixture comprising HF and CF3CCl2CF3. This process is characterized by preparing essentially pure CF3CCl2CF3 as indicated above, and reacting the CF3CCl2CF3 with hydrogen. Another process for producing 1,1,1,3,3,3-hexafluoropropane disclosed herein is characterized by contacting an azeotrope of CF3CCl2CF3 as indicated above with hydrogen and reacting the CF3CCl2CF3 with hydrogen in the presence of HF.

    Process for preparing fluorocarboxylic acids
    4.
    发明授权
    Process for preparing fluorocarboxylic acids 有权
    制备氟代羧酸的方法

    公开(公告)号：US07253315B2

    公开(公告)日：2007-08-07

    申请号：US11088370

    申请日：2005-03-24

    申请人： Ta-Wei Fu ,  Steven H. Swearingen ,  Takuya Ichida ,  Shigeyuki Yoshii

    发明人： Ta-Wei Fu ,  Steven H. Swearingen ,  Takuya Ichida ,  Shigeyuki Yoshii

    IPC分类号： C07C53/15 ,  C07C51/58

    CPC分类号： C07C51/04 ,  C07C51/48 ,  C07C59/135 ,  C07C53/21

    摘要： A fluorocarboxylic acid preparation process which includes hydrolyzing fluorocarboxylic acid fluoride in the presence of an aqueous sulfuric acid solution to form a reaction product containing a fluorocarboxylic acid and hydrogen fluoride (present as hydrofluoric acid); and removing at least some of the hydrogen fluoride from the reaction product by washing the reaction production with aqueous sulfuric acid solution. The hydrolyzing and washing are carried out at a temperature at which the fluorocarboxylic acid is a liquid.

    摘要翻译： 一种氟代羧酸制备方法，其包括在硫酸水溶液存在下水解氟代羧酸，形成含有氟代羧酸和氟化氢（以氢氟酸形式存在）的反应产物; 并通过用硫酸水溶液洗涤反应生成，从反应产物中除去至少一些氟化氢。 水解和洗涤在氟代羧酸是液体的温度下进行。

    Process for preparing fluorocarboxylic acids
    5.
    发明授权
    Process for preparing fluorocarboxylic acids 有权
    制备氟代羧酸的方法

    公开(公告)号：US07126016B2

    公开(公告)日：2006-10-24

    申请号：US11088465

    申请日：2005-03-24

    申请人： Ta-Wei Fu ,  Steven H. Swearingen ,  Takuya Ichida ,  Shuji Itatani

    发明人： Ta-Wei Fu ,  Steven H. Swearingen ,  Takuya Ichida ,  Shuji Itatani

    IPC分类号： C07C51/00

    CPC分类号： C07C51/48 ,  C07C51/02 ,  C07C59/135 ,  C07C53/21

    摘要： A fluorocarboxylic acid preparation process continuously carries out acidification reaction treatment and washing treatment, and includes subjecting a fluorocarboxylate-containing aqueous solution to acidification reaction treatment in the presence of sulfuric acid so as to form a sulfate-containing fluorocarboxylic acid phase; and subjecting the fluorocarboxylic acid phase to washing treatment using an aqueous sulfuric acid solution.

    摘要翻译： 氟代羧酸制备方法连续进行酸化反应处理和洗涤处理，包括在含硫酸盐存在下使含氟羧酸酯的水溶液进行酸化反应处理以形成含硫酸盐的氟代羧酸相; 并使用硫酸水溶液对氟代羧酸相进行洗涤处理。

    Process for the manufacture of 1,1,1,3,3-pentafluoropropene, 2-chloro-pentafluoropropene and compositions comprising saturated derivatives thereof
    6.
    发明授权
    Process for the manufacture of 1,1,1,3,3-pentafluoropropene, 2-chloro-pentafluoropropene and compositions comprising saturated derivatives thereof 失效
    用于制备1,1,1,3,3-五氟丙烯，2-氯 - 五氟丙烯的方法和包含其饱和衍生物的组合物

    公开(公告)号：US06548720B2

    公开(公告)日：2003-04-15

    申请号：US10061002

    申请日：2002-01-30

    申请人： William H. Manogue ,  V. N. Mallikarjuna Rao ,  Allen Capron Sievert ,  Steven H. Swearingen

    发明人： William H. Manogue ,  V. N. Mallikarjuna Rao ,  Allen Capron Sievert ,  Steven H. Swearingen

    IPC分类号： C07C1700

    CPC分类号： C07C19/08 ,  B01J23/868 ,  B01J27/12 ,  B01J27/132 ,  B01J37/0009 ,  B01J37/06 ,  C07C17/00 ,  C07C17/087 ,  C07C17/21 ,  C07C17/23 ,  C07C17/354 ,  C07C17/38 ,  C07C43/12 ,  Y02P20/582 ,  C07C21/18

    摘要： A process is disclosed for producing the pentfluropropenes of the formula CF3CX═CF2, where X is H or Cl. The process involves hydrodehalogenating CF3CCl2CF3 with hydrogen at an elevated temperature in the vapor phase over a catalyst comprising an elemental metal, metal oxide, metal halide and/or metal oxyhalide (the metal being copper, nickel, chromium and the halogen of said halides and said oxyhalides being fluorine and/or chlorine. Processes for producing the hydrofluorocarbons CF3CH2CHF2, CF3CHFCF3 and CF3CH2CF3 are also disclosed which involve (a) hydrodehalogenating CF3CCl2CF3 with the hydrogen as indicated above to produce a product comprising CF3CCl═CF2, CF3CH═CF2, HCl and HF; and (b) either reacting the CF3CCl═CF2 and/or CF3CH═CF2 produced in (a) in the vapor phase with hydrogen to produce CF3CH2CHF2, reacting CF3CCl═CF2 produced in (a) with HF to produce CF3CHFCF3, or reacting the CF3CH═CF2produced in (a) with HF to produce CF3CH2CF3. Azeotrope compositions of CF3CHFCH3 with HF, and a process for recovering HF from a product mixture comprising HF and CF3CHFCF3 are also disclosed. Also disclosed are compositions and a process for producing compositions comprising (c1) CF3CHFCF3, CF3CH2CF3 or CHF2CH2CF3 and (c2) at least one saturated halogenated hydrocarbon and/or ether having the formula: CnH2n+2−a−bClaFbOc wherein n is an integer from 1 to 4, a is an integer from 0 to 2n+1, b is an integer from 1 to 2n+2−a, and c is 0 or 1, provided that when c is 1 then n is an integer from 2 to 4, and provided that component (c2) does not include the selected component (c1) compound, wherein the molar ratio of component (c2) to component (c1) is between about 1:99 and a molar ratio of HF to component (c1) in an azeotrope or azeotrope-like composition of component (c1) with HF. The process involves (A) combining (i) the azeotropic composition with (ii) the fluorination precursor to component (c2); and (B) reacting a sufficient amount of the HF from the azeotrope or azeotrope-like composition(i) with precursor component (ii) to provide a composition containing components (c1) and (c2) in the desired ratio. The compositions include at least two (c1) compounds, at least one of which is an ether.

    摘要翻译： 公开了制备式CF 3 C X = CF 2的五氟丙烯的方法，其中X是H或Cl。 该方法包括在气相中在升高的温度下在含有元素金属，金属氧化物，金属卤化物和/或金属卤氧化物（金属为铜，镍，铬和所述卤化物的卤素和所述卤化物的催化剂）的催化剂中用氢气脱氢CF 3 CCl 2 CF 3 还公开了用于制备氢氟烃CF 3 CH 2 CHF 2，CF 3 CHFCF 3和CF 3 CH 2 CF 3的方法，其涉及（a）如上所述用氢气将CF 3 CCl 2 CF 3加氢脱卤以产生包含CF 3 CCl = CF 2，CF 3 CH = CF 2，HCl和HF的产物 将（a）中产生的CF 3 CCl = CF 2和/或CF 3 CH = CF 2与氢气反应以产生CF 3 CH 2 CHF 2，使（a）中制备的CF 3 CCl = CF 2与HF反应产生CF 3 CHFCF 3，或使 CF3CH = CF2，在HF中产生CF 3 CH 2 CF 3，CF 3 CHFCH 3与HF的共沸组合物，以及从含有HF和CF 3 CHFCF 3的产物混合物中回收HF的方法也被公开 。 还公开了组合物和制备组合物的方法，其包含（c1）CF 3 CHFCF 3，CF 3 CH 2 CF 3或CHF 2 CH 2 CF 3和（c2）至少一种具有下式的饱和卤代烃和/或醚：CnH2n + 2-a-bClaFbOc其中n是 如图1〜图4所示，a为0〜2n + 1的整数，b为1〜2n + 2-a的整数，c为0或1，条件是当c为1时，n为2〜4的整数 ，并且条件是组分（c2）不包括选择

    Producing CF.sub.3 CH.sub.2 CF.sub.3 and/or CF.sub.3 CH=CF.sub.2 by the conversion of .alpha.-hydroperfluoroisobutyric acid compounds
    7.
    发明授权
    Producing CF.sub.3 CH.sub.2 CF.sub.3 and/or CF.sub.3 CH=CF.sub.2 by the conversion of .alpha.-hydroperfluoroisobutyric acid compounds 失效
    通过α-氢全氟异丁酸化合物的转化生成CF 3 CH 2 CF 3和/或CF 3 CH = CF 2

    公开(公告)号：US5910615A

    公开(公告)日：1999-06-08

    申请号：US930809

    申请日：1997-10-08

    申请人： Scott C. Jackson ,  Paul Raphael Resnick ,  Steven H. Swearingen

    发明人： Scott C. Jackson ,  Paul Raphael Resnick ,  Steven H. Swearingen

    IPC分类号： C07C17/00 ,  C07C17/361 ,  C07C17/363 ,  C07C19/08

    CPC分类号： C07C17/00 ,  C07C17/361 ,  C07C17/363

    摘要： A process is disclosed for producing 1,1,1,3,3,3-hexafluoropropane and/or 1,1, 1,3,3-pentafluoropropene from (CF.sub.3).sub.2 CHCOOH and/or its water soluble salts. The process involves providing a mixture containing water and such carboxy compound(s) which has a pH of less than about 4, and reacting the mixture at a temperature of at least about 75.degree. C. Certain ether compounds may be included in the mixture along with (CF.sub.3).sub.2 CHCOOH and/or its water soluble salts. The reaction of the carboxy (and optionally ether) compound(s) with water may be employed in connection with a process for producing tetrafluoroethylene and/or hexafluoropropylene by pyrolysis, where by-product perfluoroisobutylene is reacted with water (and optionally an alkanol) to produce (CF.sub.3).sub.2 CHCOOH (and optionally one or more ether compounds).

    摘要翻译： PCT No.PCT / US96 / 05219 Sec。 371日期1997年10月8日第 102（e）日期1997年10月8日PCT 1996年4月15日PCT PCT。 出版物WO96 / 32364 日期1996年10月17日公开了从（CF 3）2 CHCOOH和/或其水溶性盐制备1,1,1,3,3,3-六氟丙烷和/或1,1,1,3,3-五氟丙烯的方法 。 该方法包括提供含有水的混合物和pH小于约4的羧基化合物，并在至少约75℃的温度下使该混合物反应。某些醚化合物可以包含在混合物中 与（CF 3）2 CHCOOH和/或其水溶性盐。 羧基（和任选的醚）化合物与水的反应可以用于通过热解制备四氟乙烯和/或六氟丙烯的方法，其中副产物全氟异丁烯与水（和任选的烷醇）反应到 产生（CF 3）2 CHCOOH（和任选的一种或多种醚化合物）。

    Production CF.sub.3 CH.sub.2 CF.sub.3 and/or CF.sub.3 CH.dbd.CF.sub.2 by the conversion of fluorinated ethers
    9.
    发明授权
    Production CF.sub.3 CH.sub.2 CF.sub.3 and/or CF.sub.3 CH.dbd.CF.sub.2 by the conversion of fluorinated ethers 失效
    通过氟化醚的转化制备CF 3 CH 2 CF 3和/或CF 3 CH = CF 2

    公开(公告)号：US5420368A

    公开(公告)日：1995-05-30

    申请号：US267988

    申请日：1994-06-29

    申请人： Scott C. Jackson ,  Paul R. Resnick ,  Steven H. Swearingen

    发明人： Scott C. Jackson ,  Paul R. Resnick ,  Steven H. Swearingen

    IPC分类号： C07C17/00 ,  C07C17/361 ,  C07C17/395 ,  C07C19/08 ,  C07C21/18

    CPC分类号： C07C21/18 ,  C07C17/00 ,  C07C17/361 ,  C07C17/395 ,  C07C19/08

    摘要： A process is disclosed for producing CF.sub.3 CH.sub.2 CF.sub.3 and/or CF.sub.3 CH.dbd.CF.sub.2 from at least one ether compound selected from the group consisting of compounds having the formula (CF.sub.3).sub.2 CHCF.sub.2 OR and compounds having the formula (CF.sub.3).sub.2 C.dbd.CFOR (wherein R is an alkyl group of the formula C.sub.n H.sub.2n+1 and n is an integer from 1 to 6) by contacting the ether compound(s) with water at an elevated temperature of at least about 75.degree. C. The reaction of ether compound(s) with water may be employed in connection with a process for producing tetrafluoroethylene and/or hexafluoropropylene by pyrolysis, where by-product perfluoroisobutylene is reacted with an alkanol to produce the ether compound (s).

    摘要翻译： 公开了从至少一种选自具有式（CF 3）2 CHCF 2 OR的化合物和具有式（CF 3）2 C = CFOR的化合物）的醚化合物制备CF 3 CH 2 CF 3和/或CF 3 CH = CF 2的方法，其中R是烷基 通式C n H 2n + 1的基团，n是1至6的整数），其中醚化合物与水在至少约75℃的升高的温度下接触。醚化合物与水的反应可以 与通过热解生产四氟乙烯和/或六氟丙烯的方法有关，其中副产物全氟异丁烯与烷醇反应以产生醚化合物。

    Processes for the purification and use of 2-chloro-1,1,1,2,3,3,3-heptafluoropropane and zeotropes thereof with HF
    10.
    发明授权
    Processes for the purification and use of 2-chloro-1,1,1,2,3,3,3-heptafluoropropane and zeotropes thereof with HF 有权

    公开(公告)号：US06677493B1

    公开(公告)日：2004-01-13

    申请号：US09283449

    申请日：1999-04-01

    申请人： Ralph Newton Miller ,  V. N. Mallikarjuna Rao ,  Steven H. Swearingen

    发明人： Ralph Newton Miller ,  V. N. Mallikarjuna Rao ,  Steven H. Swearingen

    IPC分类号： C07C1908

    CPC分类号： C07C21/18 ,  C01B7/195 ,  C07C17/206 ,  C07C17/23 ,  C07C17/38 ,  C07C19/08 ,  C07C19/10 ,  Y02P20/582

    摘要： A process is disclosed for the separation of a mixture of HF and CF3CClFCF3. The process involves placing the mixture in a separation zone at a temperature of from about −30° C. to about 100° C. and at a pressure sufficient to maintain the mixture in the liquid phase, whereby an organic-enriched phase comprising less than 50 mole percent HF is formed as the bottom layer and an HF-enriched phase comprising more than 90 mole percent HF is formed as the top layer. The organic-enriched phase can be withdrawn from the bottom of the separation zone and subjected to distillation in a distillation column to recover essentially pure CF3CClFCF3. The distillate comprising HF and CF3CClFCF3 can be removed from the top of the distillation column while essentially pure CF3CClFCF3 can be recovered from the bottom of the distillation column. The HF-enriched phase can be withdrawn from the top of the separation zone and subjected to distillation in a distillation column. The distillate comprising HF and CF3CClFCF3 can be removed from the top of the distillation column while essentially pure HF can be recovered from the bottom of the distillation column. If desired, the two distillates can be recycled to the separation zone. Also disclosed are compositions of hydrogen fluoride in combination with an effective amount of CF3CClFCF3 to form an azeotrope or azeotrope-like composition with hydrogen fluoride. Included are compositions containing from about 38.4 to 47.9 mole percent CF3CClFCF3. Also disclosed are processes for producing 1,1,1,2,3,3,3-heptafluoro-propane. One process uses a mixture comprising HF and CF3CClFCF3 and is characterized by preparing essentially pure CF3CClFCF3 as indicated above, and reacting the CF3CClFCF3 with hydrogen. Another process uses an azeotropic composition as described above, and reacts the CF3CClFCF3 with hydrogen in the presence of HF. Also disclosed is a process for producing hexafluoropropene. This process is characterized by preparing essentially pure CF3CClFCF3 as indicated above, and dehalogenating the CF3CClFCF3.