- A process for the preparation of the fluoro method
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The invention relates to a method of preparing fluoroalcohol of which the structure formula is F3C(CF2)nCH2OH, wherein n is an integer of 2-8. The method includes following steps: (I) mixing fluorocarboxylic acid and isopropyl alcohol and performing a temperature-increasing reflux reaction; (II) when the reaction is finished, distilling the reaction liquid to remove generated water and isopropyl alcohol, and cooling the rest reaction liquid to room temperature; (III) pouring the reaction liquid into distillated water, regulating the pH value to 6.5-7 by an alkali liquid, allowing the reaction liquid to stand to layer the reaction liquid to obtain an organic layer; (IV) removing water from the organic layer to obtain fluorocarboxylic isopropyl ester; (V) adding the fluorocarboxylic isopropyl ester and a solvent into a high-pressure reaction kettle with addition of a hydrogenation catalyst and a co-catalyst, sealing the reaction kettle, increasing the temperature and filling hydrogen to a high pressure for performing a reaction for 20-60 h; (VI) when the reaction is finished, cooling the reaction kettle to room temperature, discharging hydrogen to obtain a reaction mixed liquid; (VII) performing rectification to the reaction mixed liquid to separate the solvent, cooling the rest liquid and pouring the rest liquid into distillated water and regulating the pH value to 6.5-7 by an acid liquid; and (VIII) allowing the mixed liquid to stand to layer the mixed liquid to obtain an organic layer, removing water from the organic layer and distilling the organic layer to obtain the corresponding fluoroalcohol.
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Paragraph 0030
(2017/06/29)
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- METHOD FOR PRODUCING PERFLUOROALCOHOL AND DEUTERATED PERFLUOROALCOHOL
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PROBLEM TO BE SOLVED: To provide a method for efficiently synthesizing a perfluoroalcohol at a low coat. SOLUTION: This method for producing the perfluoroalcohol expressed by general formula (I) (Rf is a perfluoroalkyl; and YA and YB are each independently hydrogen or deuterium) comprises reducing a perfluorocarboxylic acid expressed by general formula (II) in water and/or heavy water in the presence of a transition metal catalyst by using a hydrogen donor.
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Page/Page column 6
(2008/06/13)
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- Aggregation Behavior of Mixed Fluorocarbon and Hydrocarbon Molecules in Aqueous Organic Solvents. Nonideality and Ideality of Mixing
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The emission spectra of naphthalene labeled hydrocarbons (NpHCn) and fluorocarbons (NpFCn) and anthracene labeled hydrocarbons (AnHCn) and fluorocarbons (AnFCn) in aqueous organic mixed solvents were investigated.The fluorescence spectrum of NpHC16 in dimethyl sulfoxide-water (DMSO-H2O) is dominated by excimer emission due to formation of aggregates.Addition of a fluorocarbon compound with chain length of seven perfluoromethylenes results in a reduction in the excimer emission and an enhancement of monomer emission, suggesting formation of coaggregates.In contrast, addition of a perfluorocarbon compound with chain length of 12 perfluoromethylenes results in no change in the fluorescence spectrum of NpHC16.Similarly, NpFC7 and NpFC12 in DMSO-H2) also exhibit excimer emission exclusively.Fluorescence studies show that hydrocarbon compounds coaggregate with NpFC7 but do not coaggregate with NpFC12.Selective excitation of the naphthalene moiety in the mixture solution of NpHC16 with AnFC7 or in the mixture solution of NpFC7 with AnHC12 exclusively leads to the emission of the anthracene moiety, suggesting that efficient energy transfer between the naphthalene and the anthracene chromophores occurs.On the other hand, for the mixture of NpHC16 with AnFC12 or NpFC12 with AnHC12, no energy tranfer was detected.All these observations indicate that fluorcarbon compounds with short chains can mix with hydrocarbon compounds ideally, while those with long chains behave nonideally.The mixed critical aggregation concentrations of NpHC16 with NpFC7 and with NpFC12 are measured as a function of overall composition of the mixtures, which give insight into yje magnitude of the nonideality of the mixings.
- Tung, Chen-Ho,Ji, Hai-Feng
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p. 8311 - 8316
(2007/10/02)
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- Hydrophobic Effects on Photochemical and Photophysical Processes: Evidence for Aggregation of Perfluorocarbon in Aqueous-Organic Solvents
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The emission spectra and photodimerization of fluorinated alkyl 2-naphthoates (NpFCn) and 9-anthrylmethyl perfluoroalkanoates (AnFCn) in aqueous-organic binary solvents have been investigated.The fluorescence spectra of NpFCn in dimethyl sulfoxide-water (DMSO-H2O) are dominated by excimer emission.Addition of long chain fluorocarbon compounds to the solution results in a reduction in the excimer emission and an enhancement of monomer emission.Selective excitation of the naphthalene moiety in the mixture solution of NpFCn and AnFCn leads to strong emission from AnFCn.Photoirradiation of NpFCn yields a 'cubane-like' photodimer with a relatively high quantum yield.All these observations suggest that hydrophobic interactions force molecules with long fluorocarbon chains to form aggregates in aqueous-organic binary solvents.
- Tung, Chen-Ho,Ji, Hai-Feng
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p. 2761 - 2766
(2007/10/03)
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- AMINE(POLYFLUOROALKOXYACYL)IMIDE SURFACTANTS
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Twenty-one examples (10a-d, 11a-l and 12a-e) of a new class of surfactants, the amine(polyfluoroalkoxyacyl)imides, were prepared by the reaction of esters containing polyfluoroalkoxy groups with tertiary alkylaminimides and hydroxyalkylaminimides.Included are five examples of difunctional aminacylimides that contain the hydrophilic portion of the molecule in the middle.These new surfactants are among the most potent known in their ability to form aqueous solutions with very low surface tensions and can be used to prepare stable emulsions of perfluorodecalin in water.Two new esters (ethyl perfluorooctyloxyacetate, 7, and ethyl 1H,1H-perfluorooctyloxyacetate, 9) used as intermediates to the surfactants were prepared by the alkylation of perfluoro- and 1H,1H-perfluorooctanol salts with ethyl bromoacetate.Other esters used in the preparation of the surfactants were derived from oligomers of hexafluoropropene oxide.
- Haywood, Lisa,McKee, Sean,Middleton, W. J.
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p. 419 - 431
(2007/10/02)
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