- Method for preparing polyfluorobenzonitrile through catalytic fluorination of polychlorobenzonitrile
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The invention discloses a method for preparing polyfluorobenzonitrile through catalytic fluorination of polychlorobenzonitrile, and belongs to the field of preparation of fine chemical industry intermediates. The preparation method comprises the following steps: carrying out a heating activation reaction on a fluoride salt, an organic solvent and electron-withdrawing substituted phenylborate; andadding polychlorobenzonitrile, heating to 80-120 DEG C, rectifying while reacting, then supplementing polychlorobenzonitrile and potassium fluoride, and rectifying while reacting to obtain polyfluorobenzonitrile. According to the invention, the reaction system is high in catalytic activity, the technical problems of low conversion rate/medium selectivity and the like of the single nitrile compounds with low activity during fluoridation reactions are solved, the mode simultaneously performing reacting and product distilling in the reaction process promotes the continuous forward proceeding of the reaction so as to improve the reaction yield, and the method is suitable for industrial production.
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Paragraph 0027; 0030-0031; 0042-0048; 0051-0054; 0057-0060
(2020/04/22)
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- Production method of high-purity pentachlorobenzene nitrile
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The invention relates to a method for producing high-purity pentachloro benzonitrile. The method comprises the following steps: a, preparing graphene oxide; b, preparing a modified activated carbon catalyst; c, activating the modified activated carbon catalyst; d, pre-vaporizing cyanobenzene; e, performing a chlorination reaction; and f, performing trapping. According to the method, optimization selection is performed on the catalyst, the catalyst is modified, and the modified activated carbon catalyst is fully catalyzed; meanwhile, an improved compound bed process is adopted; and through improvement of the catalyst and the production process, the temperature required for the chlorination reaction is greatly reduced, the product content (more than or equal to 99.6%) is improved, and service life of the catalyst is prolonged to 720 h.
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Paragraph 0031-0048
(2019/07/31)
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- Organochlorine formation in magnesium electrowinning cells
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The formation of organochlorines during the electrolytic production of magnesium was investigated using a laboratory-scale electrolytic cell having a graphite anode, a liquid aluminium alloy cathode, and a molten chloride electrolyte. The cell was operated at current densities ranging from 3000 to 10,000 A m-2 and at temperatures ranging from 660°C to 750°C. Organochlorines were adsorbed from the cell off-gases onto silica gel, extracted with hexane, and determined by gas chromatography. All compounds identified were fully chlorinated aliphatic and aromatic compounds, the major components being hexachlorobutadiene, hexachlorobenzene, hexachloroethylene, and octachlorostyrene. The total amount of organochlorines per tonne of magnesium produced decreased with electrolysis time and with current density and increased with operating temperature; it was also dependent on the type of graphite employed. The output of organochlorines Varied from 5 to 20 g t-1 of magnesium.
- Deutscher,Cathro
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p. 147 - 155
(2007/10/03)
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- Aprotic diazotization in the presence of cuprous cyanide
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In a procedure of extreme simplicity and rapidity a mixture of an aromatic primary amine, copper (I) cyanide and an alkyl nitrite in dimethyl sulphoxide yielded fair to moderate yields of the corresponding nitriles. Side processes observed were reduction (NH2&[H), nitration (NH2←NO2) and hydroxylation (NH2&[OH). In the case of polyhaloanilines halogen dance products could be detected.
- Giumanini, Angelo G.,Verardo, Giancarlo,Geatti, Paola,Strazzolini, Paolo
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p. 7137 - 7148
(2007/10/03)
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