- Method for preparing perfluoroalkyl ethanol
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The invention discloses a method for preparing perfluoroalkyl ethanol. The method comprises the following steps: enabling perfluoroalkyl ethyl iodide, a mixed solvent and water to react, and separating and purifying the obtained mixture containing perfluoroalkyl ethanol, by-product olefins, solvent salt and water, thereby obtaining the perfluoroalkyl ethanol product, wherein the separation and purification comprise the following steps: (1) adding a mixture containing perfluoroalkyl ethanol, by-product olefins, solvent salt and water into a rectifying tower for performing reduced pressure distillation, controlling the vacuum degree to be -0.91 to -0.96MPa so as to obtain distillate containing perfluoroalkyl ethanol, by-product olefins and water and bottom liquid, performing strong base treatment on the bottom liquid, and filtering to obtain the recycled mixed solvent; and (2) performing azeotropic distillation on the distillate, thereby obtaining the mixed solution of the by-product olefins and water and the product perfluoroalkyl ethanol. The method disclosed by the invention has the advantages of simplicity in process, greening, environment friendliness, convenience, high efficiency and low cost.
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Paragraph 0026-0032
(2017/11/29)
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- Synthesis of 2-(perfluoroalkyl)ethyl potassium sulfates based on perfluorinated Grignard reagents
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The first example of nucleophilic substitution with perfluoroalkyl Grignard reagents on the sp3 carbon centre is described. Thus, a series of organometals RF-MgBr, prepared from perfluorinated alkyl iodides RF-I with RF = C4F9, C 6F13, C8F17, C10F 21 and C12F25, reacted with 1,3,2-dioxathiolane-2,2-dioxide to afford the corresponding 2-(perfluoroalkyl) ethyl magnesium sulfates, which were isolated after metathesis to the corresponding potassium salts. In the model reaction, perfluorohexylmagnesium iodide was reacted with methyl triflate yielding polyfluorinated alkane. The attempts to extend the reaction to 1,3,2-dioxathiane-2,2-dioxide were unsuccessful due to its inferior reactivity and only reduced polyfluoroalkane and the product of coupling were detected in the reaction mixture. Polyfluorinated sulfates are easily hydrolyzed with hydrochloric or triflic acid to the corresponding alcohols, which is an alternative to standard transformation of perfluoroalkyl iodides to 2-(perfluoroalkyl)ethanols. Quantum-chemical calculations of the PES of the reaction with both sulfur-containing heterocycles found that the failure of the reaction with 1,3,2-dioxathiane-2,2-dioxide is caused by higher activation energy of the process.
- Paterová, Jana,Skalicky, Martin,Rybá?ková, Markéta,Kví?alová, Magdalena,Cva?ka, Josef,Kví?ala, Jaroslav
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experimental part
p. 1338 - 1343
(2011/02/22)
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- PROCESS FOR PRODUCING FLUORINATED (METH)ACRYLIC ESTER
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A mixture of fluoroalkyl iodides of the formula C2F5(CF2CF2)nI ( n is an integer of ≥0) wherein the sum of such fluoroalkyl iodides of n=3 and n=4 contained is ≥85 mol% is provided. This mixture is subjected to an ethylene addition step and an esterification step, and C2F5(CF2CF2)nCH=CH2 and C2F5(CF2CF2)nCH2CH2OH are removed. Thus, there can be obtained a mixture of fluorine-containing (meth)acrylic esters of the formula C2F5(CF2CF2)nCH2CH2OCOCR1=CH2 (wherein R1 represents a hydrogen atom or a methyl group, and n is an integer of ≥0) wherein the content of impurities (namely, olefins of the formula C2F5(CF2CF2)nCH=CH2 and alcohols of the formula C2F5(CF2CF2)nCH2CH2OH) is low.
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Page/Page column 9
(2010/11/25)
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- PROCESS FOR PRODUCING FLUORINATED ACRYLIC ESTER
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A mixture of fluoroalkyl alcohols represented by C 2 F 5 (CF 2 CF 2 ) n CH 2 CH 2 OH wherein "n" is an integer equal to or more than 0 wherein the sum of the fluoroalkyl alcohols of n=3 and n=4 contained is 85 mol% or more is prepared and reacted with an acrylic acid compound followed by removing unreacted C 2 F 5 (CF 2 CF 2 ) n CH 2 CH 2 OH, to give a mixture of fluorine-containing acrylic esters wherein the content of impurities (that is, olefins represented by C 2 F 5 (CF 2 CF 2 ) n CH=CH 2 and the alcohols represented by C 2 F 5 (CF 2 CF 2 ) n CH 2 CH 2 OH) is low.
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Page/Page column 7
(2008/06/13)
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- PROCESS FOR PRODUCING FLUORINATED ACRYLIC ESTER
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A mixture of fluorine-containing acrylic esters represented by CF3(CF2)nCH2CH2OCOCR1=CH2 wherein R1 is a hydrogen atom, a methyl group or a halogen atom and "n" is an integer of at least zero is subjected to distillation under such conditions that the esters are not polymerized, so as to give a mixture of the esters with a less content of impurities (that is, olefins represented by CF3(CF2)nCH=CH2 and alcohols represented by CF3(CF2)nCH2CH2OH) at a high yield.
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Page/Page column 7-8
(2008/06/13)
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- Purification of fluorinated alcohols
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A process for reducing the level of perfluoroalkanoic acids, perfluoroalkanoic esters, and perfluoroalkyliodides in fluorinated alcohols comprising heating a fluorinated alcohol, or mixtures thereof, containing said acids, esters, or iodides to a temperature of at least 175° C. in the presence of water and a base additive is disclosed.
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Page/Page column 4-5
(2008/06/13)
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- Catalysts for the preparation of fluorinated alcohols and process for the preparation of fluorinated alcohols
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The present invention provides a catalyst for preparing a fluorine-containing alcohol compound, the catalyst having at least one component selected from elements in Group 1B, Group 2B, Group 6A, Group 7A and Group 8 of the periodic table, ions of these elements, oxides containing these elements, hydroxides containing these elements and salts containing these elements, said component being supported on at least one complex oxide selected from Si—Al complex oxides, Al—P complex oxides and Si—Al—P complex oxides; and a method for preparing a fluorine-containing alcohol compound, the method comprising reacting a halogenated fluorine compound with water in the presence of the catalyst. According to the present invention, a fluorine-containing alcohol compound can be prepared at a relatively low reaction temperature and in a high yield.
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Page column 8-9
(2008/06/13)
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