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    • 4. 发明授权
      US6018083A Process for the production of fluorocarbons 失效
    • Process for the production of fluorocarbons
    • US6018083A
    • 2000-01-25
    • US283450
    • 1999-04-01
    • William H. Manogue , Mario Joseph Nappa , Allen Capron Sievert , V. N. Mallikarjuna Rao
    • William H. Manogue , Mario Joseph Nappa , Allen Capron Sievert , V. N. Mallikarjuna Rao
    • C07C17/00 , C07C17/04 , C07C17/21 , C07C17/23 , C07C19/08 , C07C21/18 , C07C17/25 , C07C17/08
    • C07C21/18 , C07C17/00 , C07C17/04 , C07C17/21 , C07C17/23 , C07C19/08
    • 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 The organic-enriched phase can be withdrawn from the bottom of the separation zone and subjected to distillation in a distillation column to recover essentially pure CF.sub.3 CClFCF.sub.3.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 The HF-enriched phase can be withdrawn from the top of the separation zone and subjected to distillation in a distillation column.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.
    • 基本信息 添加关注 加入工作空间 PDF全文 PDF下载 全文下载 相似专利 双屏查看 权利要求书 说明书全文 Global Dossier Espacenet 法律信息 同族专利 专利引用
    • 5. 发明授权
      US06281395B1 1,1,1,2,3,3,3-heptafluoropropane manufacturing process 有权
    • 1,1,1,2,3,3,3-heptafluoropropane manufacturing process
    • 1,1,1,2,3,3,3-七氟丙烷制造方法
    • US06281395B1
    • 2001-08-28
    • US09283451
    • 1999-04-01
    • Mario Joseph Nappa , V. N. Mallikarjuna Rao , Allen Capron Sievert
    • Mario Joseph Nappa , V. N. Mallikarjuna Rao , Allen Capron Sievert
    • C07C1708
    • C07C17/087 , B01J23/26 , C07C17/21 , C07C19/08 , C07C21/18
    • 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.
    • 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。
    • 基本信息 添加关注 加入工作空间 PDF全文 PDF下载 全文下载 相似专利 双屏查看 权利要求书 说明书全文 Espacenet 法律信息 同族专利 专利引用
    • 6. 发明授权
      US06376727B1 Processes for the manufacture of 1,1,1,3,3-pentafluoropropene, 2-chloro-pentafluoropropene and compositions comprising saturated derivatives thereof 失效
    • Processes for the manufacture of 1,1,1,3,3-pentafluoropropene, 2-chloro-pentafluoropropene and compositions comprising saturated derivatives thereof
    • 用于制造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
    • US06376727B1
    • 2002-04-23
    • US09367900
    • 1999-08-19
    • V. N. Mallikarjuna Rao , Allen Capron Sievert
    • V. N. Mallikarjuna Rao , Allen Capron Sievert
    • C07C1700
    • 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
    • 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.
    • 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。
    • 基本信息 添加关注 加入工作空间 PDF全文 PDF下载 全文下载 相似专利 双屏查看 权利要求书 说明书全文 Espacenet 法律信息 同族专利 专利引用
    • 7. 发明授权
      US06274780B1 Catalysts for halogenated hydrocarbon processing and their preparation and use 失效
    • Catalysts for halogenated hydrocarbon processing and their preparation and use
    • 用于卤代烃加工的催化剂及其制备和用途
    • US06274780B1
    • 2001-08-14
    • US08677062
    • 1996-07-09
    • V. N. Mallikarjuna Rao , Munirpallam A. Subramanian
    • V. N. Mallikarjuna Rao , Munirpallam A. Subramanian
    • C07C1700
    • C07C17/358 , B01J27/12 , B01J27/132 , C07C17/00 , C07C17/206 , C07C17/21 , C07C17/37 , C07C19/08 , C07C19/12 , C07C19/10
    • A process is disclosed for changing the fluorine content of halogenated hydrocarbons containing from 1 to 6 carbon atoms, in the presence of a multiphase catalyst. The process involves producing the catalyst by heating a single phase solid catalyst precursor having the formula (NH3)6Cr2−xMxF6 (where x is in the range of 0.1 to 1 and M is at least one metal selected from the group consisting of Al, Sc, V, Fe, Ga and In) to about 400° or less to produce a multiphase composition wherein a phase containing crystalline M fluoride is homogeneously dispersed with a phase containing chromium fluoride. Also disclosed are multiphase catalyst compositions consisting essentially of chromium fluoride and a crystalline fluoride of at least one metal selected from the above group (provided the atom percent of Cr is at least equal to the atom percent of the crystalline fluoride metals). Phases of the crystalline fluorides are homogeneously dispersed with phases of the chromium fluoride. Preparation of homogeneously dispersed multiphase catalyst compositions consisting essentially of fluorides of chromium and crystalline fluorides of at least one other metal selected from the above group (the atom percent Cr being at least equal to the atom percent of the other metal(s)) is also disclosed.
    • 公开了在多相催化剂存在下改变含有1〜6个碳原子的卤代烃的氟含量的方法。 该方法包括通过加热具有式（NH 3）6 C 2-x M x F 6的单相固体催化剂前体（其中x在0.1至1的范围内，M是至少一种选自Al，Sc ，V，Fe，Ga和In）至约400°以下，以产生多相组合物，其中含有结晶M氟化物的相通过含氟化铬的相均匀分散。 还公开了基本上由氟化铬和选自上述组中的至少一种金属的结晶氟化物组成的多相催化剂组合物（条件是Cr的原子百分数至少等于结晶氟化物金属的原子百分数）。 结晶氟化物的相与氟化铬的相分别均匀分散。 制备均匀分散的多相催化剂组合物，其主要由铬的氟化物和选自上述组中的至少一种其它金属的晶体氟化物（原子百分比Cr至少等于其它金属的原子百分比）组成）也是 披露
    • 基本信息 添加关注 加入工作空间 PDF全文 PDF下载 全文下载 相似专利 双屏查看 权利要求书 说明书全文 Espacenet 法律信息 同族专利 专利引用
    • 8. 发明授权
      US06224781B1 Compositions comprising hydrofluorocarbons and their manufacture 有权
    • Compositions comprising hydrofluorocarbons and their manufacture
    • 包含氢氟碳化合物及其制备的组合物
    • US06224781B1
    • 2001-05-01
    • US09137343
    • 1998-08-20
    • Barry A. Mahler , V. N. Mallikarjuna Rao , Allen Capron Sievert , Munirpallam A. Subramanian , Edwin James Warwas
    • Barry A. Mahler , V. N. Mallikarjuna Rao , Allen Capron Sievert , Munirpallam A. Subramanian , Edwin James Warwas
    • A62D100
    • A62D1/0057 , A62D1/00
    • 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.
    • 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。
    • 基本信息 添加关注 加入工作空间 PDF全文 PDF下载 全文下载 相似专利 双屏查看 权利要求书 说明书全文 Espacenet 法律信息 同族专利 专利引用
    • 9. 发明授权
      US06143938A Process for perhalocycloalkane purification 失效
    • Process for perhalocycloalkane purification
    • 全卤烷烃纯化方法
    • US06143938A
    • 2000-11-07
    • US429271
    • 1999-10-29
    • Allen Capron Sievert , V. N. Mallikarjuna Rao
    • Allen Capron Sievert , V. N. Mallikarjuna Rao
    • C07C17/04 , C07C17/20 , C07C17/395 , C07C19/08 , C07C17/38
    • C07C19/08 , C07C17/04 , C07C17/206 , C07C17/395
    • 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.
    • 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。
    • 基本信息 添加关注 加入工作空间 PDF全文 PDF下载 全文下载 相似专利 双屏查看 权利要求书 说明书全文 Espacenet 法律信息 同族专利 专利引用
    • 10. 发明授权
      US6107267A Compositions comprising CF.sub.3 CF.sub.2 CHF.sub.2 and their manufacture 失效
    • Compositions comprising CF.sub.3 CF.sub.2 CHF.sub.2 and their manufacture
    • 包含CF 3 CF 2 CHF 2的组合物及其制备
    • US6107267A
    • 2000-08-22
    • US137342
    • 1998-08-20
    • V. N. Mallikarjuna Rao , Allen Capron Sievert , Munirpallam A. Subramanian
    • V. N. Mallikarjuna Rao , Allen Capron Sievert , Munirpallam A. Subramanian
    • B01D3/36 , C11D7/30 , C11D7/50
    • C11D7/5036 , B01D3/36 , C11D7/30
    • 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.
    • 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。
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