- Preparation method of fluorine-containing dicarboxylic acid
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The invention discloses a preparation method of fluorine-containing dicarboxylic acid, which comprises: by using fluorine-containing cycloolefin as a raw material, performing oxidation with an oxidantunder the actions of a solvent and a catalyst to generate the corresponding fluorine-containing dicarboxylic acid. According to the method, a mixed solvent composed of the organic solvent and water is used as a solvent system of an oxidation reaction, the fluorine-containing cycloolefin is oxidized into corresponding fluorine-containing dicarboxylic acid by using the oxidant under the action of the catalyst, and the method has the characteristics of simple operation, stable process, safety, short reaction time, high yield and high product quality, and is suitable for large-scale production.
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Paragraph 0045-0047
(2020/07/12)
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- Preparation method of fluorine-containing carboxylic acid
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The invention discloses a preparation method of fluorine-containing carboxylic acid. The method comprises the following steps: reacting fluorine-containing carboxylate used as a raw material with an acylating chlorination reagent to obtain a corresponding mixture of fluorine-containing acyl chloride and fluorine-containing anhydride, and hydrolyzing and drying the mixture of fluorine-containing acyl chloride and fluorine-containing anhydride to obtain high-purity fluorine-containing carboxylic acid. The method provided by the invention is suitable for post-treatment of fluorine-containing carboxylic acid prepared by a fluorine-containing olefin (monoolefine, diene, cycloolefin and the like) oxidation method, replaces the traditional strong acid acidification and ether continuous extractionprocess, and is simpler, more convenient and more applicable; and the method can also be used for recovering and purifying a fluorine-containing carboxylate emulsifier. The purity of the fluorine-containing carboxylic acid prepared by the method can reach 98% or above.
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- Production process of fluorine-containing carboxylic acid
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The invention discloses a production process of fluorine-containing carboxylic acid. The method comprises the following steps: by taking fluorine-containing olefin as a raw material, carrying out an oxidation reaction to obtain fluorine-containing carboxylate, reacting the fluorine-containing carboxylate with an acylating chlorination reagent to obtain a corresponding mixture of fluorine-containing acyl chloride and fluorine-containing acid anhydride, and hydrolyzing and drying the mixture of fluorine-containing acyl chloride and fluorine-containing acid anhydride to prepare the high-purity fluorine-containing carboxylic acid. The method provided by the invention is suitable for post-treatment of fluorine-containing carboxylic acid prepared by a fluorine-containing olefin (monoolefine, diene, cycloolefin and the like) oxidation method, replaces the traditional strong acid acidification and ether continuous extraction process, and is simpler, more convenient and more applicable; the purity of the fluorine-containing carboxylic acid prepared by the method can reach 98% or above.
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Paragraph 0032-0034
(2020/07/13)
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- METHODS OF MAKING POLYFUNCTIONAL POLYFLUORINATED COMPOUNDS
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A method of making a polyfunctional polyfluorinated compound includes combining first components that include a polyfluorinated cyclic compound having 4 to 7 ring carbon atoms and at least one of osmium tetroxide, ruthenium tetroxide or a precursor thereof and forming a polyfluorinated dicarboxylic acid. Two of the ring carbon atoms of the polyfluorinated cyclic compound form a double bond or an epoxide. The precursor reacts with an oxidant to form ruthenium tetroxide. Methods also include converting the polyfluorinated dicarboxylic acid to a polyfluorinated dicarboxylic acid halide and converting the polyfluorinated dicarboxylic acid halide to other polyfunctional polyfluorinated compounds.
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Page/Page column 21-23
(2019/07/13)
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- Method for synthesizing tetrafluoroallene
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The invention relates to a method for synthesizing tetrafluoroallene and belongs to the field of organic chemical synthesis. The method for synthesizing tetrafluoroallene is characterized in that hexafluoroglutaric acid is produced through a reaction of dichlorohexafluorocyclopentene under the action of an oxidizing agent. Tetrafluoroallene is produced by heating a mixture of hexafluoroglutaric acid and a sodium hydroxide solution. Raw materials are convenient to obtain; a product is simple to separate and purify, industrial production is easy, and few three industrial wastes are produced.
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Paragraph 0010; 0023-0025; 0028-0030
(2018/04/21)
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- DEFLUORINATION OF HEXADECAFLUOROBICYCLODEC-1-ENE: A FACILE SYNTHESIS OF PERFLUOROAROMATICS
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Depending mainly on the polarity of the aprotic solvent used, defluorination of hexadecafluorobicyclodec-1(6)-ene (1) with activated zinc gave tetradecafluorobicyclodec-1(2),6(7)-diene (2), perfluorotetraline (3), decafluoro-1,2-dihydronaphthalene (4) and perfluoronaphthalene (5).In methanol, 2,7-dimethoxy-dodecafluorobicyclodec-1(2),6(7)-diene (6) was formed.These products were characterized by elemental analysis, IR, UV, 1H NMR and 19F NMR.An electron transfer and then a radical intermediate seem to be involved in such defluorination reactions.
- Hu, Chang-Ming,Long, Fei,Xu, Ze-Qi
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- POLYFLUORO-COMPOUNDS BASED ON THE CYCLOHEPTANE RING SYSTEM. PART 2. THE 1H,3H- and 1H,4H-DODECAFLUOROCYCLOHEPTANES, DERIVED UNDECAFLUOROCYCLOHEPTENES AND DECAFLUOROCYCLOHEPTA-1,4- and 1,3-DIENE
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From the mixture obtained by reaction of cycloheptane with cobalt(III) fluoride at 180-190 deg C, the cis- and trans-1H,3H- and 1H,4H-dodecafluorocycloheptanes were isolated.Each 1H,3H-compound was dehydrofluorinated by aqueous potash to 3H- and 4H-undecafluorocyclohept-1-ene, and thence decafluorocyclohepta-1,4- and 1,3-diene.The 1H,4H-isomers each gave 4H- and 5H-undecafluorocyclohept-1-ene and thence the two dienes on dehydrofluorination.The dichloro-adduct of the 5H-ene was reduced by lithium aluminium hydride, and the three possible 1H,2H,5H-undecafluorocycloheptanes were isolated.Likewise, the 4H-ene gave the 4 possible 1H,2H,4H-undecafluorides.All were identified by further fluorination with cobalt(III) fluoride at 160 deg C, to appropriate dodecafluorocycloheptanes.
- Khalil, Abd E. M. M.,Stephens, Robert,Tatlow, John Colin
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- POLYFLUOROCYCLOALKENES. PART XVI . SOME ADDITION REACTIONS OF 1-TRIFLUOROMETHYLNONAFLUOROCYCLOHEX-1-ENE
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Reactions with alcohols and base repleaced the vinylic fluorine of 1-trifluoromethylnonafluorocyclohex-1-ene (I) by methoxy and ethoxy groups.Fluorination with cobaltic fluoride gave, from the former, a number of saturated polyfluoro-ethers.Oxidation of the alkoxy-cycloalkenes gave hexafluoroglutaric acid.Cycloalkene I gave with ammonia an imino-enamine, which was hydrolysed by dilute acid to a keto-enamine.I was defluorinated by heated iron to octafluorotoluene.
- Carter, Paul A.,Patrick, Colin R.,Tatlow, John Colin
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p. 407 - 412
(2007/10/02)
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