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1. 发明授权

US4830846A Separation process for anhydrous HCl and HBr by thermal cleavage 失效
标题翻译：通过热裂解分离无水HCl和HBr的方法
公开(公告)号：US4830846A
公开(公告)日：1989-05-16
申请号：US150184
申请日：1988-01-29
申请人： Herbert C. Jackson, Jr. , Robert A. DeVries , Hughie R. Frick
发明人： Herbert C. Jackson, Jr. , Robert A. DeVries , Hughie R. Frick
IPC分类号： C01B7/07 , C01B7/09
CPC分类号： C01B7/0706 , C01B7/093
摘要： A method for the separation of anhydrous HCl and HBr from mixtures of the two acids comprising treating the mixture with a hindered pyridine to form a mixture of hindered pyridine salts of the acids, and heating the mixture of salts to a temperature at which thermal cleavage of at least the hydrochloride salt is induced. The hindered pyridines are defined as aromatic compounds having one or more nitrogen atoms in an aromatic ring, or a polymer with pendant aromatic moieties having one or more nitrogens in an aromatic ring, having an appropriate degree of steric hindrance such that the salt formed by the nitrogen atom of the aromatic compound and a strong protic base will undergo dissociation to the aromatic compound and the protic acid at a temperature below the decomposition temperature of the aromatic compound. The formation of salts and their cleavage can be done as either a one-step or two-step process. The separation process is based on the fact that the HCl salts are less stable to heat than the HBr salts, and thus will cleave at a faster rate at any given temperature. It is possible to carry out the thermal cleavage at a temperature sufficient to induce cleavage of only the HCl salts, of both simultaneously, or at two separate sequential temperatures, to cleave only the HCl salts first and then the remaining HBr salts.
摘要翻译：一种从两种酸的混合物中分离无水HCl和HBr的方法，包括用受阻吡啶处理混合物以形成酸的受阻吡啶盐的混合物，并将盐的混合物加热至热裂解至少引起盐酸盐。受阻吡啶被定义为在芳香环中具有一个或多个氮原子的芳族化合物，或具有在芳香环中具有一个或多个氮的侧面芳族部分的聚合物，具有适当的空间位阻程度，使得由芳族化合物的氮原子和强质子碱将在低于芳族化合物的分解温度的温度下解离成芳族化合物和质子酸。盐的形成及其裂解可以作为一步法或两步法进行。分离过程基于HCl盐比HBr盐不太稳定的事实，因此在任何给定温度下以更快的速率裂解。可以在足以诱发仅同时或两个独立的连续温度的HCl盐的裂解的温度下进行热裂解，以首先仅切割HCl盐，然后仅剩下其余的HBr盐。

2. 发明授权

US5138081A Process for purifying vinylically-unsaturated organosilicon compounds 失效
标题翻译：乙烯基不饱和有机硅化合物的纯化方法
公开(公告)号：US5138081A
公开(公告)日：1992-08-11
申请号：US694521
申请日：1991-04-30
申请人： Robert A. DeVries , Mary L. Ash , Hughie R. Frick, deceased
发明人： Robert A. DeVries , Mary L. Ash , Hughie R. Frick, deceased
IPC分类号： C07F7/08 , C07F7/18 , C07F7/20
CPC分类号： C07F7/1896 , C07F7/0889 , C07F7/089 , C07F7/1892 , C07F7/20
摘要： A process for purifying an impure vinylically-unsaturated organosilicon product compound prepared by reaction between a vinylically-unsaturated organosilicon precursor and a halogenated organic compound in the presence of a homogeneous zerovalent palladium catalyst complex, the catalyst complex including an organophosphine or organoarsine ligand, in the presence of a hydrogen halide acceptor in an essentially anhydrous diluent, comprising treating a mixture containing the impure vinylically-unsaturated organosilicon product compound with a peroxide for a time sufficient to oxidize organophosphine or organoarsine impurities present in a mixture being treated. The peroxide can be selected from aqueous hydrogen peroxide or organic peroxides. The thus-treated mixture can be further treated by chromatography over silica gel or alumina. In optional embodiments, chromatography over silica gel or alumina can precede treatment with the peroxide.
摘要翻译：一种在均相的零价钯催化剂络合物（包括有机膦或有机砷配体）的催化剂络合物的存在下，通过在乙烯基不饱和有机硅前体和卤代有机化合物之间的反应制备的不纯的乙烯基不饱和有机硅产物化合物的方法，在基本上无水的稀释剂中存在卤化氢受体，包括用过氧化物处理含有不纯的乙烯基不饱和有机硅产物化合物的混合物足以氧化存在于待处理的混合物中的有机膦或有机砷杂质。过氧化物可以选自过氧化氢水溶液或有机过氧化物。这样处理的混合物可以通过硅胶或氧化铝上的色谱进一步处理。在任选的实施方案中，硅胶或氧化铝上的色谱可以在用过氧化物处理之前进行。

3. 发明授权

US3931325A Perfluorocyclohexene-1,4-dione 失效
标题翻译：全氟环己烯-1,4-二酮
公开(公告)号：US3931325A
公开(公告)日：1976-01-06
申请号：US448135
申请日：1974-03-04
申请人： Harold E. Doorenbos , Hughie R. Frick
发明人： Harold E. Doorenbos , Hughie R. Frick
IPC分类号： C07C45/63 , C07C49/463 , C08G65/00 , C07C49/48
CPC分类号： C08G65/007 , C07C45/63 , C07C49/463
摘要： Two new organic compounds are disclosed, perfluorocyclohexane-1,4-dione and perfluorocyclohexene-1,4-dione, which are obtained concurrently or alternatively by reacting fluoranil with substantially pure anhydrous cobalt trifluoride. These compounds are clear, colorless liquids which are useful as monomers in the synthesis of thermally stable elastomeric polymers. Also disclosed is the dihydrate of said perfluorocyclohexane-1,4-dione, namely, octafluoro-1,1,4,4-cyclohexanetetraol. Another aspect of this invention is a series of polyethers formed by reacting said perfluorocyclohexane-1,4-dione with cesium fluoride and a cyclic or noncyclic aliphatic perhaloalkene having from 2 to 12 carbon atoms and a fluorine atom on at least each of the carbon atoms connected by the double bond, said polymer having as a repeating unit ##SPC1##WhereinR is a divalent radical selected from the group consisting of ##EQU1## WHEREIN X is a halogen selected from the group consisting of fluorine, chlorine, bromine, iodine, or any stable combination thereof within the same molecule;n is an integer of from 1 to 4;y is an integer of from 0 to 10; andZ is an integer of from 0 to (10-y).When of sufficiently high molecular weight or when lightly cross-linked, these polymers are elastomers having high thermal stability.
摘要翻译：公开了两种新的有机化合物，全氟环己烷-1,4-二酮和全氟环己烯-1,4-二酮，它们同时或通过使荧蒽与基本上纯的无水三氟化碳反应得到。这些化合物是透明无色液体，它们可用作合成热稳定弹性聚合物的单体。还公开了所述全氟环己烷-1,4-二酮的二水合物，即八氟-1,1,4,4-环己烷四醇。本发明的另一方面是通过使全氟环己烷-1,4-二酮与氟化铯和具有2至12个碳原子的环状或非环状脂肪族全卤代烯烃和至少每个碳原子上的氟原子反应而形成的一系列聚醚所述聚合物具有作为重复单元的所述聚合物，其中R是选自以下的二价基团：-C = C-和-C = C-ANGLE || CnX2n X2y + 1CyCzX2z + 1 WHEREIN X是卤素选自氟，氯，溴，碘或其相同分子内的任何稳定的组合; N是1到4的整数; Y是0到10的整数; 和Z是从0到（10-Y）的整数。

4. 发明授权

US5264646A Process for preparing vinylically-unsaturated compounds 失效
标题翻译：制备乙烯基不饱和化合物的方法
公开(公告)号：US5264646A
公开(公告)日：1993-11-23
申请号：US677023
申请日：1991-03-28
申请人： Robert A. DeVries , Gregory F. Schmidt , Hughie R.* Frick , Bonnie Frick
发明人： Robert A. DeVries , Gregory F. Schmidt , Hughie R.* Frick , Bonnie Frick
IPC分类号： C07B37/04 , C07B63/02 , C07F7/08 , C07F7/18 , C07F7/20 , C07C1/30
CPC分类号： C07F7/0889 , C07B37/04 , C07B63/02 , C07F7/0849 , C07F7/1892 , C07F7/1896 , C07F7/20
摘要： A process for preparing a vinylically-unsaturated product compound comprises reacting a halogenated organic compound with a hydrolytically-stable, vinylically-unsaturated precursor compound in the presence of (a) a homogeneous zerovalent palladium catalyst complex, (b) an organic hydrogen halide acceptor and (c) a diluent, wherein the diluent is water or an aqueous solution containing up to 95% by volume of an organic solvent. The halogenated organic compound is selected from aryl halides, benzyl halides or vinylic halides. The hydrolytically-stable, vinylically-unsaturated precursor compound is selected from organosilicon compounds, hydrocarbon compounds or compounds containing at least one of an oxygen atom, a nitrogen atom, a sulfur atom, a phosphorus atom or a combination thereof.
摘要翻译：制备乙烯基不饱和产物化合物的方法包括在（a）均相的零价钯催化剂络合物，（b）有机卤化氢受体和（b）有机卤化氢受体的存在下使卤代有机化合物与水解稳定的乙烯基不饱和前体化合物反应，（c）稀释剂，其中稀释剂是水或含有至多95％（体积）有机溶剂的水溶液。卤代有机化合物选自芳基卤化物，苄基卤化物或乙烯基卤化物。水解稳定的乙烯基不饱和前体化合物选自有机硅化合物，烃化合物或含有氧原子，氮原子，硫原子，磷原子或其组合中的至少一个的化合物。

5. 发明授权

US5243068A Process for preparing vinylically-unsaturated compounds (II) 失效
标题翻译：制备乙烯基不饱和化合物（II）的方法
公开(公告)号：US5243068A
公开(公告)日：1993-09-07
申请号：US877580
申请日：1992-05-01
申请人： Robert A. DeVries , Hughie R. Frick, deceased
发明人： Robert A. DeVries , Hughie R. Frick, deceased
IPC分类号： C07F7/08 , C07F7/20
CPC分类号： C07F7/20 , C07F7/0849 , C07F7/0889
摘要： A process for preparing a vinylically-unsaturated product compound comprises reacting a halogenated organic compound with a hydrolytically-stable, vinylically-unsaturated precursor compound in the presence of (a) a homogeneous zerovalent palladium catalyst complex, (b) an inorganic hydrogen halide acceptor and (c) a diluent, wherein the diluent is water or an aqueous solution containing up to 95% by volume of an organic solvent. The halogenated organic compound is selected from aryl halides, benzyl halides or vinylic halides. The hydrolytically-stable, vinylically-unsaturated precursor compound is selected from hydrocarbon compounds or compounds containing at least one of an oxygen atom, a nitrogen atom, a sulfur atom, a phosphorus atom or a combination thereof.
摘要翻译：一种制备乙烯基不饱和产物化合物的方法包括在（a）均匀的零价钯催化剂络合物，（b）无机卤化氢受体和（b）无机卤化氢受体的存在下使卤代有机化合物与水解稳定的乙烯基不饱和前体化合物反应，（c）稀释剂，其中稀释剂是水或含有至多95％（体积）有机溶剂的水溶液。卤代有机化合物选自芳基卤化物，苄基卤化物或乙烯基卤化物。水解稳定的乙烯基不饱和前体化合物选自烃化合物或含有氧原子，氮原子，硫原子，磷原子或其组合中的至少一种的化合物。

6. 发明授权

US5136069A Process for preparing vinylically-unsaturated compounds (II) 失效
标题翻译：制备乙烯基不饱和化合物（II）的方法
公开(公告)号：US5136069A
公开(公告)日：1992-08-04
申请号：US676622
申请日：1991-03-28
申请人： Robert A. DeVries , Hughie R. Frick, deceased
发明人： Robert A. DeVries , Hughie R. Frick, deceased
IPC分类号： C07F7/08 , C07F7/20
CPC分类号： C07F7/0889 , C07F7/0849 , C07F7/20
摘要： A process for preparing a vinylically-unsaturated product compound comprises reacting a halogenated organic compound with a hydrolytically-stable, vinylically-unsaturated precursor compound in the presence of (a) a homogeneous zerovalent palladium catalyst complex, (b) an inorganic hydrogen halide acceptor and (c) diluent, wherein the diluent is water or an aqueous solution containing up to 95% by volume of an organic solvent. The halogenated organic compound is selected from aryl halides, benzyl halides or vinylic halides. The hydrolytically-stable, vinylically-unsaturated precursor compound is selected from hydrocarbon compounds or compounds containing at least one of an oxygen atom, a nitrogen atom, a sulfur atom, a phosphorus atom, silicon atom or a combination thereof.
摘要翻译：一种制备乙烯基不饱和产物化合物的方法包括在（a）均匀的零价钯催化剂络合物，（b）无机卤化氢受体和（b）无机卤化氢受体的存在下使卤代有机化合物与水解稳定的乙烯基不饱和前体化合物反应，（c）稀释剂，其中稀释剂是水或含有至多95％（体积）有机溶剂的水溶液。卤代有机化合物选自芳基卤化物，苄基卤化物或乙烯基卤化物。水解稳定的乙烯基不饱和前体化合物选自含有氧原子，氮原子，硫原子，磷原子，硅原子或其组合中的至少一种的烃化合物或化合物。

7. 发明授权

US3996200A Perfluorinated para-diketone polymers 失效
标题翻译：全氟化对二酮聚合物
公开(公告)号：US3996200A
公开(公告)日：1976-12-07
申请号：US612390
申请日：1975-09-11
申请人： Harold E. Doorenbos , Hughie R. Frick
发明人： Harold E. Doorenbos , Hughie R. Frick
IPC分类号： C08G65/00 , C08G16/00
CPC分类号： C08G65/007
摘要： Two new organic compounds are disclosed, perfluorocyclohexane-1,4-dione and perfluorocyclohexene-1,4-dione, which are obtained concurrently or alternatively by reacting fluoranil with substantially pure anhydrous cobalt trifluoride. These compounds are clear, colorless liquids which are useful as monomers in the synthesis of thermally stable elastomeric polymers. Also disclosed is the dihydrate of said perfluorocyclohexane-1,4-dione, namely, octafluoro-1,1,4,4-cyclohexanetetraol. Another aspect of this invention is a series of polyethers formed by reacting said perfluorocyclohexane-1,4-dione with cesium fluoride and a cyclic or noncyclic aliphatic perhaloalkene having from 2 to 12 carbon atoms and a fluorine atom on at least each of the carbon atoms connected by the double bond, said polymer having as a repeating unit ##STR1## wherein R is a divalent radical selected from the group consisting of ##STR2## wherein X is a halogen selected from the group consisting of fluorine, chlorine, bromine, iodine, or any stable combination thereof within the same molecule;n is an integer of from 1 to 4;y is an integer of from 0 to 10; andz is an integer of from 0 to (10-y).When of sufficiently high molecular weight or when lightly cross-linked, these polymers are elastomers having high thermal stability.
摘要翻译：公开了两种新的有机化合物，全氟环己烷-1,4-二酮和全氟环己烯-1,4-二酮，它们同时或通过使荧蒽与基本上纯的无水三氟化碳反应得到。这些化合物是透明无色液体，它们可用作合成热稳定弹性聚合物的单体。还公开了所述全氟环己烷-1,4-二酮的二水合物，即八氟-1,1,4,4-环己烷四醇。本发明的另一方面是通过使全氟环己烷-1,4-二酮与氟化铯和具有2至12个碳原子的环状或非环状脂肪族全卤代烯烃和至少每个碳原子上的氟原子反应而形成的一系列聚醚所述聚合物具有作为重复单元的重复单元，其中R是选自下列的二价基团：其中X是选自氟，氯，溴，碘的卤素，或其相同分子内的任何稳定的组合; N是1到4的整数; Y是0到10的整数; 和Z是从0到（10-Y）的整数。

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