公开(公告)号：US5948213A

公开(公告)日：1999-09-07

申请号：US118800

申请日：1998-07-17

申请人： Ralph Newton Miller ,  V. N. Mallikarjuna Rao ,  Allen Capron Sievert

发明人： Ralph Newton Miller ,  V. N. Mallikarjuna Rao ,  Allen Capron Sievert

IPC分类号： C07C17/10 ,  C07C17/20 ,  C07C17/23 ,  C07C17/38 ,  C07C19/08 ,  C07C19/10 ,  B01D3/00

CPC分类号： C07C19/10 ,  C07C17/10 ,  C07C17/206 ,  C07C17/23 ,  C07C17/38 ,  C07C19/08 ,  Y02P20/582

摘要： A process is disclosed for producing 1,1,2,2,3,3,4,4-octafluorobutane. The process involves (a) reacting a mixture comprising 2,2,3,3-tetrafluorobutane and chlorine to form a mixture of chloro-compounds wherein compounds of the formula C.sub.4 H.sub.x Cl.sub.6-x F.sub.4 (where x is 0 or 1) comprise at least about 50 mole % of the mixture of chloro-compounds; (b) contacting certain chloro-compounds from (a) and hydrogen fluoride with a fluorination catalyst to form a mixture of fluoro-compounds; and (c) contacting certain fluoro-compounds from (b) and hydrogen with a hydrogenolysis catalyst to produce CHF.sub.2 CF.sub.2 CF.sub.2 CHF.sub.2. Sufficient chloro-compounds formed in (a) and sufficient fluoro-compounds formed in (b) are recycled to provide a selectivity to CHF.sub.2 CF.sub.2 CF.sub.2 CHF.sub.2 of at least about 75% based upon the moles of CH.sub.3 CF.sub.2 CF.sub.2 CH.sub.3 reacted in (a).Also disclosed is a process for the purification of at least one compound selected from the group consisting of CCl.sub.2 F(CF.sub.2).sub.2 CCl.sub.3, CCl.sub.2 F(CF.sub.2).sub.2 CCl.sub.2 F, CCl.sub.2 F(CF.sub.2).sub.2 CClF.sub.2, CClF.sub.2 (CF.sub.2).sub.2 CClF.sub.2, CClF.sub.2 (CF.sub.2).sub.2 CF.sub.3, CHCl.sub.2 (CF.sub.2).sub.2 CCl.sub.2 F, CHClF(CF.sub.2).sub.2 CCl.sub.3, CHCl.sub.2 (CF.sub.2).sub.2 CClF.sub.2, CHClF(CF.sub.2).sub.2 CCl.sub.2 F, CHF.sub.2 (CF.sub.2).sub.2 CCl.sub.3, CHClF(CF.sub.2).sub.2 CClF.sub.2, CHF.sub.2 (CF.sub.2).sub.2 CCl.sub.2 F, CHCl.sub.2 (CF.sub.2).sub.2 CF.sub.3, CHClF(CF.sub.2).sub.2 CF.sub.3, CHF.sub.2 (CF.sub.2).sub.2 CClF.sub.2, CHF.sub.2 CF.sub.2 CF.sub.2 CHF.sub.2, CHF.sub.2 CF.sub.2 CF.sub.2 CH.sub.2 F, CHF.sub.2 CF.sub.2 CF.sub.2 CF.sub.3 and CH.sub.2 FCF.sub.2 CF.sub.2 CF.sub.3 from a mixture of HF and said at least one compound. The purification process involves (a) subjecting the mixture of HF and said compound(s) to a distillation step in which a first distillate is removed; (b) subjecting said first distillate to an additional distillation as described herein; and (c) recovering said compound(s) essentially free of HF as bottoms from either the distillation of (a) or the distillation of (b).New compounds CCl.sub.2 FCF.sub.2 CF.sub.2 CClF.sub.2, CCl.sub.3 CF.sub.2 CF.sub.2 CCl.sub.2 F, CHCl.sub.2 CF.sub.2 CF.sub.2 CCl.sub.3, CHCl.sub.2 CF.sub.2 CF.sub.2 CCl.sub.2 F, CHClFCF.sub.2 CF.sub.2 CCl.sub.3, CHCl.sub.2 CF.sub.2 CF.sub.2 CClF.sub.2, CHClFCF.sub.2 CF.sub.2 CCl.sub.2 F, CHF.sub.2 CF.sub.2 CF.sub.2 CCl.sub.3, CHF.sub.2 CF.sub.2 CF.sub.2 CCl.sub.2 F, CHClFCF.sub.2 CF.sub.2 CF.sub.3, CH.sub.3 CF.sub.2 CF.sub.2 CH.sub.2 Cl and CH.sub.2 ClCF.sub.2 CF.sub.2 CCl.sub.3 are also disclosed, as are compositions which comprise hydrogen fluoride in combination with an effective amount of CHF.sub.2 CF.sub.2 CF.sub.2 CHF.sub.2 to form an azeotrope or azeotrope-like composition with hydrogen fluoride.

公开(公告)号：US5817893A

公开(公告)日：1998-10-06

申请号：US868349

申请日：1997-06-03

申请人： Ralph Newton Miller ,  V. N. Mallikarjuna Rao ,  Allen Capron Sievert

发明人： Ralph Newton Miller ,  V. N. Mallikarjuna Rao ,  Allen Capron Sievert

IPC分类号： C07C17/10 ,  C07C17/20 ,  C07C17/23 ,  C07C17/38 ,  C07C19/08 ,  C07C19/10

CPC分类号： C07C19/10 ,  C07C17/10 ,  C07C17/206 ,  C07C17/23 ,  C07C17/38 ,  C07C19/08 ,  Y02P20/582

摘要： A process is disclosed for producing 1,12,2,3,3,4,4-octafluorobutane. The process involves chlorination of 2,2,3,3-tetrafluorobutane to form a mixture of chloro-compounds wherein compounds of the formula C.sub.4 H.sub.4 Cl.sub.6-x F.sub.4 (where x is 0 or 1) comprise at least 50 mole % of the mixture of chloro-compounds, followed by hydrofluorination, then hydrogenolysis, and sufficient recycle to provide a selectivity to CHF.sub.2 CF.sub.2 CF.sub.2 CHF.sub.2 of at least about 75% based upon the moles of CH.sub.3 CF.sub.2 CF.sub.2 CH.sub.3 reacted. Also disclosed is a multi-distillation process for the purification of CHF.sub.2 CF.sub.2 CF.sub.2 CHF.sub.2 from a mixture of HF and the compound(s). Also disclosed are certain new halogenated butanes containing fluorine, and a composition which contains HF in combination with an effective amount of CHF.sub.2 CF.sub.2 CF.sub.2 CHF.sub.2 to form an azeotrope or azeotrope-like composition with hydrogen fluoride.

摘要翻译： 公开了一种制备1,12,2,3,3,4,4-八氟丁烷的方法。 该方法包括氯化2,2,3,3-四氟丁烷以形成氯化合物的混合物，其中式C4H4Cl6-xF4（其中x为0或1）的化合物包含至少50摩尔％的氯 - 化合物，然后进行氢氟化，然后氢解，并充分循环以提供基于所反应的CH 3 CF 2 CF 2 CH 3的摩尔数至少约75％的CHF 2 CF 2 CF 2 CHF 2的选择性。 还公开了从HF和化合物的混合物中纯化CHF 2 CF 2 CF 2 CHF 2的多蒸馏方法。 还公开了含氟的一些新的卤化丁烷，以及含有HF与有效量的CHF 2 CF 2 CF 2 CHF 2组合以与氟化氢形成共沸物或类共沸组合物的组合物。

公开(公告)号：US06376727B1

公开(公告)日：2002-04-23

申请号：US09367900

申请日：1999-08-19

申请人： V. N. Mallikarjuna Rao ,  Allen Capron Sievert

发明人： V. N. Mallikarjuna Rao ,  Allen Capron Sievert

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： Disclosed are azeotropic compositions comprising CF3CHFCF3 and HF. 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 1-4, a is an integer from 0-2n+1, b is an integer from 1-2n+2a, and c is 0 or 1, provided that when c is 1 then n is an integer from 2-4, 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 (1) 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 (1) with the 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： 公开了包含CF 3 CHFCF 3和HF的共沸组合物。 还公开了组合物和制备包含（c1）CF 3 CHFCF 3，CF 3 CH 2 CF 3或CHF 2 CH 2 CF 3的组合物和（c2）至少一种具有下式的饱和卤代烃和或醚的组合物和方法：C n H 2n + 2-a-b Cl a F b O c其中n是整数 从1-4开始，a是0-2n + 1的整数，b是1-2n + 2a的整数，c是0或1，条件是当c为1时，n为2-4的整数， （c2）与成分（c1）的摩尔比为约1:99，HF与成分（c1）的摩尔比在下述式（c2）中，式（c2） 组分（c1）与HF的共沸物或类共沸组合物。 该方法包括（A）将（1）共沸组合物与（ii）氟化前体与组分（c2）组合; 和（B）使足够量的来自共沸物或类共沸组合物（1）的HF与前体组分（ii）反应，以提供含有所需比例的组分（c1）和（c2）的组合物。 组合物包括至少两种（c1）化合物，其中至少一种是醚。

公开(公告)号：US06224781B1

公开(公告)日：2001-05-01

申请号：US09137343

申请日：1998-08-20

申请人： Barry A. Mahler ,  V. N. Mallikarjuna Rao ,  Allen Capron Sievert ,  Munirpallam A. Subramanian ,  Edwin James Warwas

发明人： Barry A. Mahler ,  V. N. Mallikarjuna Rao ,  Allen Capron Sievert ,  Munirpallam A. Subramanian ,  Edwin James Warwas

IPC分类号： A62D100

CPC分类号： A62D1/0057 ,  A62D1/00

摘要： A process is disclosed for producing compositions including (a) a compound selected from the group consisting of CHF2CF3, CHF2CHF2, CH2FCF3, CH3CF3, CH3CHF2, CH2FCF2CHF2 and CHF2CF2CF2CHF2 and (b) 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 (b) does not include the selected component (a) compound, wherein the molar ratio of component (b) to component (a) is between about 1:99 and a molar ratio of HF to component (a) in an azeotrope or azeotrope-like composition of component (a) with HF. This process involves (A) combining (i) the azeotrope or azeotrope-like composition with (ii) at least one fluorination precursor compound wherein the precursor component (ii) is the fluorination precursor to component (b); 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 (a) and (b) in said ratio.

摘要翻译： 公开了用于制备组合物的方法，其包括（a）选自CHF 2 CF 3，CHF 2 CHF 2，CH 2 FFC 3，CH 3 CF 3，CH 3 CHF 2，CH 2 F 2 CHF 2和CHF 2 CF 2 CF 2 CHF 2的化合物和（b）至少一种具有下式的饱和卤代烃和/或醚： 其中n为1〜4的整数，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 组分（b）与组分（a）的摩尔比为约1:99，摩尔比为2〜4的整数，并且组分（b）不包括所选择的组分（a）化合物，其中组分 HF与组分（a）在组分（a）的共沸物或类共沸组合物中与HF混合。 该方法包括：（i）将共沸物或类共沸组合物与（ii）至少一种氟化前体化合物组合（其中前体组分（ii）为组分（b）的氟化前体）; 和（B）使来自共沸物或类共沸组合物（i）的足够量的HF与前体组分（ii）反应，以提供含有所述比例的组分（a）和（b）的组合物。

公开(公告)号：US06143938A

公开(公告)日：2000-11-07

申请号：US429271

申请日：1999-10-29

申请人： Allen Capron Sievert ,  V. N. Mallikarjuna Rao

发明人： Allen Capron Sievert ,  V. N. Mallikarjuna Rao

IPC分类号： C07C17/04 ,  C07C17/20 ,  C07C17/395 ,  C07C19/08 ,  C07C17/38

CPC分类号： C07C19/08 ,  C07C17/04 ,  C07C17/206 ,  C07C17/395

摘要： A process is disclosed for recovering at least one perhalocycloalkane selected from the group consisting of octafluorocyclobutane, hexafluoro-bis(trifluoromethyl)cyclobutane (1,2 and 1,3; cis and trans), 1,2-dichloro-1,2,3,3,4,4-hexafluorocyclobutane (cis and trans), 1,1,2,2-tetrachloro-3,3,4,4-tetrafluorocyclobutane, 1-chloro-1,2,2,3,3,4-hexafluoro-4-(trifluoromethyl)-cyclobutane, heptafluoro(trifluoromethyl)cyclobutane and chloroheptafluoro-cyclobutane from a mixture comprising (a) the perhalocycloalkane, (b) olefinic impurity and optionally (c) saturated fluorine-containing impurity selected from the group consisting of hydrochlorofluorocarbons, hydrofluorocarbons and mixtures thereof. The process involves (1) contacting the mixture with chlorine under conditions suitable for chlorinating the olefinic impurity, thereby converting the olefinic impurity to a saturated impurity containing at least one chlorine substituent and reducing the hydrogen content of the saturated fluorine-containing impurity (if present), and (2) separating said at least one perhalocycloalkane from the products produced during the chlorination of (1).Also disclosed is a process for producing n-decafluorobutane. The process involves contacting a mixture comprising octafluorocyclobutane (i.e., C-318) and 1,1,1,2,3,4,4,4-octafluorobutene-2 (FC-1318my) with chlorine under conditions suitable for converting the FC-1318my to 2,3-dichloro-1,1,1,2,3,4,4,4-octa-fluorobutane (i.e., CFC-318mbb); separating the C-318 from the CFC-318mbb; and reacting the CFC-318mbb with HF.

摘要翻译： 公开了一种用于回收至少一种选自八氟环丁烷，六氟 - 双（三氟甲基）环丁烷（1,2和1,3;顺式和反式）的全卤烷烃的方法，1,2-二氯-1,2,3 ，3,4,4-六氟环丁烷（顺式和反式），1,1,2,2-四氯-3,3,4,4-四氟环丁烷，1-氯-1,2,2,3,3,4-四氟环丁烷 六氟代-4-（三氟甲基） - 环丁烷，七氟（三氟甲基）环丁烷和氯三氟环丁烷，其包含（a）全卤代环烷烃，（b）烯属杂质和任选的（c）饱和含氟杂质， 氢氯氟烃，氢氟碳化合物及其混合物。 该方法包括（1）在适于氯化烯烃杂质的条件下使混合物与氯接触，从而将烯烃杂质转化为含有至少一个氯取代基的饱和杂质并降低饱和含氟杂质的氢含量（如果存在 ）和（2）从（1）的氯化期间产生的产物中分离出所述至少一种全卤烷烃。 还公开了制备正九氟丁烷的方法。 该方法包括使包含八氟环丁烷（即C-318）和1,1,1,2,3,4,4,4-八氟丁烯-2（FC-1318my）的混合物与氯在适于转化FC- 1318my至2,3-二氯-1,1,1,2,3,4,4,4-八氟丁烷（即CFC-318mbb）; 将C-318与CFC-318mbb分离; 并使CFC-318mbb与HF反应。

公开(公告)号：US6107267A

公开(公告)日：2000-08-22

申请号：US137342

申请日：1998-08-20

申请人： V. N. Mallikarjuna Rao ,  Allen Capron Sievert ,  Munirpallam A. Subramanian

发明人： V. N. Mallikarjuna Rao ,  Allen Capron Sievert ,  Munirpallam A. Subramanian

IPC分类号： B01D3/36 ,  C11D7/30 ,  C11D7/50

CPC分类号： C11D7/5036 ,  B01D3/36 ,  C11D7/30

摘要： A process is disclosed for recovering HF from a product mixture including HF and CF.sub.3 CF.sub.2 CHF.sub.2. The process involves (1) distilling the product mixture to remove all products which have a lower boiling point than the lowest boiling azeotrope containing HF and CF.sub.3 CF.sub.2 CHF.sub.2 ; and (2) distilling the azeotrope to recover HF as an azeotropic composition containing HF and CF.sub.3 CF.sub.2 CHF.sub.2. Also disclosed are compositions of hydrogen fluoride in combination with an effective amount of CF.sub.3 CF.sub.2 CHF.sub.2 to form an azeotrope or azeotrope-like composition with hydrogen fluoride, (e.g., compositions containing from about 57.1 to 67.2 mole percent CF.sub.3 CF.sub.2 CHF.sub.2).A process for producing certain compositions comprising(a) CF.sub.3 CF.sub.2 CHF.sub.2 and (b) at least one saturated halogenated hydrocarbon and/or ether having the formula:C.sub.n H.sub.2n+2-a-b Cl.sub.a F.sub.b O.sub.cwherein 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 (b) does not include CF.sub.3 CF.sub.2 CF.sub.2) is also disclosed. This process involves (A) combining (i) an azeotropic composition of CF.sub.3 CF.sub.2 CHF.sub.2 and HF with (ii) at least one fluorination precursor compound wherein the precursor component (ii) is the fluorination precursor to component (b); and (B) reacting a sufficient amount of the HF from the azeotropic composition (i) with precursor component (ii), to provide a composition containing components (a) and (b) in the desired ratio. In addition, certain compositions are disclosed which include (a) CF.sub.3 CF.sub.2 CHF.sub.2 and (b) at least two saturated halogenated hydrocarbons and/or ethers having the formula:C.sub.n H.sub.2n+2-a-b Cl.sub.a F.sub.b O.sub.cwherein the molar ratio of said at least one compound to HFC-227ca is between about 1:99 and about 43:57 and c is 1 for at least one of the component (b) compounds.

摘要翻译： 公开了从包含HF和CF 3 CF 2 CHF 2的产物混合物中回收HF的方法。 该方法包括（1）蒸馏产物混合物以除去所有具有比含有HF和CF 3 CF 2 CHF 2的最低沸点共沸物沸点低的产物; 和（2）蒸馏共沸物以回收HF作为含有HF和CF 3 CF 2 CHF 2的共沸组合物。 还公开了氟化氢与有效量的CF 3 CF 2 CHF 2组合以与氟化氢形成共沸物或类共沸组合物的组合物（例如，含有约57.1至67.2摩尔％CF 3 CF 2 CHF 2的组合物）。 一种制备某些组合物的方法，其包含（a）CF 3 CF 2 CHF 2和（b）至少一种具有下式的饱和卤代烃和/或醚：n为1至4的整数，a为从 0〜2n + 1，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（（b）成分 也不包括CF 3 CF 2 CF 2）。 该方法包括：（i）将CF 3 CF 2 CHF 2和HF的共沸组合物与（ii）至少一种氟化前体化合物组合（其中前体组分（ii）是组分（b）的氟化前体）; 和（B）使足够量的来自共沸组合物（i）的HF与前体组分（ii）反应，从而以所需的比例提供含有组分（a）和（b）的组合物。 此外，公开了某些组合物，其包括（a）CF 3 CF 2 CHF 2和（b）至少两种具有下式的饱和卤代烃和/或醚：CnH2n + 2-a-bClaFbOc，其中所述至少一种化合物与HFC- 对于至少一种组分（b）化合物，227ca为约1:99至约43:57，c为1。

公开(公告)号：US06281395B1

公开(公告)日：2001-08-28

申请号：US09283451

申请日：1999-04-01

申请人： Mario Joseph Nappa ,  V. N. Mallikarjuna Rao ,  Allen Capron Sievert

发明人： Mario Joseph Nappa ,  V. N. Mallikarjuna Rao ,  Allen Capron Sievert

IPC分类号： C07C1708

CPC分类号： C07C17/087 ,  B01J23/26 ,  C07C17/21 ,  C07C19/08 ,  C07C21/18

摘要： A process is disclosed for the manufacture of CF3CHFCF3 containing less than 0.01 ppm (CF3)2C═CF2. The process involves (a) contacting hexafluoropropene in the vapor phase at a temperature of less than about 260° C. with hydrogen fluoride in the presence of a selected fluorination catalyst or produce a product containing less than 10 parts (CF3)2C═CF2 per million parts of CF3CHFCF3; and (b) treating the product of (a) as necessary to remove excess (CF3)2C═CF2. Suitable catalysts include: (i) an activated carbon treated to contain from about 0.1 to about 10 weight % added alkali or alkaline earth metals, (ii) three dimensional matrix porous carbonaceous materials, (iii) supported metal catalysts comprising trivalent chromium, and (iv) unsupported chrome oxide prepared by the pyrolysis of (NH4)2Cr2O7.

摘要翻译： 公开了用于制造含有小于0.01ppm（CF 3）2 C = CF 2的CF 3 CHFCF 3的方法。 该方法包括（a）在选择的氟化催化剂存在下，在小于约260℃的温度下，使氟化氢在气相中接触六氟丙烯，或者产生含有小于10份（CF 3）2 C = CF 2的产物 百万份CF3CHFCF3; 和（b）根据需要处理（a）的产物以除去过量（CF 3）2 C = CF 2。 合适的催化剂包括：（i）经处理以包含约0.1至约10重量％的加入的碱金属或碱土金属的活性炭，（ii）三维基体多孔碳质材料，（iii）包含三价铬的载体金属催化剂和（ iv）通过（NH 4）2 Cl 2 O 7的热解制备的无载体的氧化铬。

公开(公告)号：US6147267A

公开(公告)日：2000-11-14

申请号：US429272

申请日：1999-10-29

申请人： Allen Capron Sievert ,  V. N. Mallikarjuna Rao

发明人： Allen Capron Sievert ,  V. N. Mallikarjuna Rao

IPC分类号： C07C17/23 ,  C07C17/395 ,  C07C19/08 ,  C07C19/10 ,  C07C19/12 ,  C07C17/38

CPC分类号： C07C19/12 ,  C07C17/23 ,  C07C17/395 ,  C07C19/08 ,  C07C19/10

摘要： A process is disclosed for recovering at least one perfluorocycloalkane selected from the group consisting of octafluorocyclobutane, hexafluoro-bis(trifluoromethyl)cyclobutane (1,2 and 1,3; cis and trans), and heptafluoro(trifluoromethyl)cyclobutane from a mixture comprising (a) the perfluorocycloalkane, (b) olefinic impurity and, optionally, (c) saturated chlorine-containing impurity selected from the group consisting of chlorocarbons, hydrochlorocarbons, hydrochlorofluorocarbons, chlorofluorocarbons and mixtures thereof. The process involves (1) contacting the mixture with hydrogen in the presence of a hydrogenation catalyst under conditions suitable for converting at least a portion of the olefinic impurity to a saturated impurity containing at least one fluorine substituent less than the olefin impurity and reducing the chlorine content of at least a portion of the saturated chlorine-containing impurity (if present), and (2) separating said at least one perfluorocycloalkane from the products produced during the hydrogenation of (1).

摘要翻译： 公开了一种从包含（氟代丁烷，六氟 - 双（三氟甲基）环丁烷（1,2和1,3;顺式和反式）和七氟（三氟甲基）环丁烷的混合物中回收至少一种选自八氟环丁烷，六氟（三氟甲基）环丁烷的全氟环烷烃的方法，该混合物包括 a）全氟环烷烃，（b）烯烃杂质和任选的（c）选自氯代烃，氢氯氟烃，氢氯氟烃，氯氟烃及其混合物的饱和含氯杂质。 该方法包括（1）在氢化催化剂存在下，在适于将至少一部分烯属杂质转化成含有至少一个氟烯取代基的烯属杂质的饱和杂质的条件下，使该混合物与氢接触并还原氯 至少部分饱和含氯杂质（如果存在）的含量，和（2）从（1）的氢化期间产生的产物中分离出所述至少一种全氟环烷烃。

公开(公告)号：US6018083A

公开(公告)日：2000-01-25

申请号：US283450

申请日：1999-04-01

申请人： William H. Manogue ,  Mario Joseph Nappa ,  Allen Capron Sievert ,  V. N. Mallikarjuna Rao

发明人： William H. Manogue ,  Mario Joseph Nappa ,  Allen Capron Sievert ,  V. N. Mallikarjuna Rao

IPC分类号： C07C17/00 ,  C07C17/04 ,  C07C17/21 ,  C07C17/23 ,  C07C19/08 ,  C07C21/18 ,  C07C17/25 ,  C07C17/08

CPC分类号： C07C21/18 ,  C07C17/00 ,  C07C17/04 ,  C07C17/21 ,  C07C17/23 ,  C07C19/08

摘要： A process is disclosed for the separation of a mixture of HF and CF.sub.3 CClFCF.sub.3. The process involves placing the mixture in a separation zone at a temperature of from about -30.degree. C. to about 100.degree. 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 CF.sub.3 CClFCF.sub.3. The distillate comprising HF and CF.sub.3 CClFCF.sub.3 can be removed from the top of the distillation column while essentially pure CF.sub.3 CClFCF.sub.3 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 CF.sub.3 CClFCF.sub.3 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 CF.sub.3 CClFCF.sub.3 to form an azeotrope or azeotrope-like composition with hydrogen fluoride. Included are compositions containing from about 38.4 to 47.9 mole percent CF.sub.3 CClFCF.sub.3.Also disclosed are processes for producing 1,1,1,2,3,3,3-heptafluoropropane. One process uses a mixture comprising HF and CF.sub.3 CClFCF.sub.3 and is characterized by preparing essentially pure CF.sub.3 CClFCF.sub.3 as indicated above, and reacting the CF.sub.3 CClFCF.sub.3 with hydrogen. Another process uses an azeotropic composition as described above, and reacts the CF.sub.3 CClFCF.sub.3 with hydrogen in the presence of HF.Also disclosed is a process for producing hexafluoropropene. This process is characterized by preparing essentially pure CF.sub.3 CClFCF.sub.3 as indicated above, and dehalogenating the CF.sub.3 CClFCF.sub.3.

公开(公告)号：US06683226B2

公开(公告)日：2004-01-27

申请号：US10367317

申请日：2003-02-14

申请人： Allen Capron Sievert ,  V. N. Mallikarjuna Rao

发明人： Allen Capron Sievert ,  V. N. Mallikarjuna Rao

IPC分类号： C07C1723

CPC分类号： C07C21/18 ,  C07C17/00 ,  C07C17/206 ,  C07C17/23 ,  C07C19/10 ,  Y02P20/582

摘要： A process for the manufacture of CF3CF═CF2 is disclosed. The process involves contacting 2,3-dichloro-1,1,1,2,3,3-hexafluoropropane with at least 0.1 mole of hydrogen in a reaction vessel of titanium, nickel or iron or their alloys, which is either empty or packed with particles or formed shapes of titanium, nickel or iron or their alloys, at a temperature within the range of from about 350° C. to about 600° C. and for a time sufficient to produce hexafluoropropene. Also disclosed are compositions which comprise hydrogen fluoride in combination with an effective amount of CClF2CClFCF3 to form an azeotrope or azeotrope-like composition with hydrogen fluoride. The compositions contain from about 8.7 to 33.6 mole percent CClF2CClFCF3.

摘要翻译： 公开了制备CF 3 CF = CF 2的方法。 该方法包括在钛，镍或铁或其合金的反应容器中将2,3-二氯-1,1,1,2,3,3-六氟丙烷与至少0.1摩尔的氢气接触，其为空或包装 具有钛，镍或铁或其合金的颗粒或形成形状，在约350℃至约600℃的温度下，并持续足以产生六氟丙烯的时间。 还公开了包含氟化氢与有效量的CClF 2 CClFCF 3组合以与氟化氢形成共沸物或类共沸组合物的组合物。 组合物含有约8.7至33.6摩尔％CClF 2 CClFCF 3。