The method of obtaining oxide hexaferrite
(57) Abstract:The invention relates to a method for producing oxide hexaferrite liquid-phase oxidation of hexaferrite environment, trifluorotrichloroethane, and the oxidation of hexaferrite carried out in the presence of heated metal surface with a temperature below 170°C with simultaneous removal of heat from the reaction zone. The invention can be used in organofluorine chemistry to obtain oxide hexaferrite, which is an intermediate for obtaining surfactants, oils, solvents, etc. the Technical result - obtaining conversion hexaferrite, close to 100% when entering the downloaded HEXAFLUOROPROPYLENE about 75-85%. table 2. The inventive object is to organofluorine chemistry. Oxide of hexaferrite (EGFP) are used for obtaining surfactants, parfocality oils, solvents, perfluorinated alkylvinyl esters, etc. (L. F. Sokolov, P. I. Shafts, S. C. Sokolov. // USP, 1984. So LIII. Vol. 7. C. 1222-1246).A method of obtaining EGFP oxidation of hexaferrite (HFP) an alkaline solution of hydrogen peroxide (Eleuterio H. S. // J. Macromol. Sci., Chem., 1972, v. The paragraph does not exceed 45%.Output EGFP does not exceed 50% and in another way - oxidation HFP hipogalactiei alkali and alkaline earth metals in aqueous solution at atmospheric pressure and room temperature (Izv. An SSSR, Ser. chem., 1979, S. 2812. A. J. Zapevalov, and others).Closest to the claimed is a method for EGFP oxidation HFP oxygen in inert solvent (U.S. Pat. USA 3536733, 1970). The process is carried out in a stainless steel autoclave with stirring at a temperature of 430 K, a pressure of 2.8 MPa in the environment of Halocarbon 113. Conversion of HFP reaches 70%, and the output EGFP on unreacted HFP - 70%,
Further processing EGFP raw involves dividing EGFP and HFP, which have practically the same boiling point - 29oC. Commonly used methods of extractive distillation and the photochemical synthesized or chlorination lead to a significant complication of technology, the increase of the expenditure ratio and the cost of the target product.Therefore, the main task for the authors of the present invention was to obtain the highest possible conversion of HFP with acceptable yield and reaction time.To solve the task oxide using submersible heated metal surface with a temperature not lower than 170oC, which in these conditions generates active centers, as the initiator of the chain oxidation process. Unlike the closest analogue that allows you to get the HFP conversion close to 100%, and the output EGFP reaches 87%.Table 1 shows the mapping of the data closest analogue and the proposed method. As can be seen from table 1, the inventive method is characterized by higher than in the nearest analogue output EGFP and conversion of HFP. close to 100%, which allows to exclude from the process flowsheet stage of purification of the target product from the source of raw materials.The applicant asserts that the proposed facility meets the criteria of the invention "inventive step", because in the patent and scientific and technical documentation are not found together claimed funds in the solution method of obtaining EGFP known to specialists in this field.Examples of industrial application of the claimed method.Example 1. In a reactor of 10 l load 8 kg halon 113 and 4 kg of HFP. Heat the reaction mixture to 150oC. with Nitrogen to create a pressure of 3 MPa. Include mixing. Using a submersible heat exchanger remove heat of reaction and maintain temp nl/hour. These settings support for 100 minutes Off the oxygen supply. Poured the reaction mixture. 4 kg loaded HFP get 330-350 g EGFP.Example 2. In a reactor of 10 l load 8 kg halon 113 and 4 kg of HFP. Heat the reaction mixture to 150oC. Nitrogen creates a pressure of 3 MPa. Include mixing. Include oxygen with a flow rate of 400 to 450 nl/h. The reactor is mounted submerged in the reaction mixture an electric fuel element in a metal casing, the surface of which is supported at a temperature of 175oC. the Heat of reaction away with coolant, which is supplied to the jacket of the reactor. These settings support for 100 minutes Off the oxygen supply. Poured the reaction mixture. 4 kg loaded HFP get 330-350 g EGFP.The main options of the industrial implementation are shown in table 2, including the option # 1. The Complainant submits that all the intervals of variation of parameters are workable.This shows that the applied method allows in industrial conditions to obtain the oxide of hexaferrite with the release of 75-85% on the downloaded HEXAFLUOROPROPYLENE when conversion hexaferrite, b is on in the environment, trifluorotrichloroethane, characterized in that the oxidation hexaferrite carried out in the presence of heated metal surface with a temperature below 170°C with simultaneous removal of heat from the reaction zone.
SUBSTANCE: invention relates to a method for synthesis of 3,4-epoxycarane of formula I
with simultaneous production of 3-caren-5-one of formula II
and 3-carene-2,5-dione of formula III
, involving the following: 3-carene is treated with diluted hydrogen peroxide in acetonitrile in conditions for catalytic action of manganese sulphate in the presence of sodium bicarbonate and salicylic acid with subsequent extraction of the reaction mixture with methylene chloride, vacuum distillation of crude epoxy and release of 3,4-epoxycarane with 88% purity and 45% output. 3-caren-5-one II and 3-carene-2,5-dione III are separated through chromatograph on an inverted C-18 phase with output of 13% and 7% respectively.
EFFECT: design of a method for synthesis of intermediate compounds for a range of medical, industrial and perfume preparations.
1 cl, 4 ex
SUBSTANCE: invention relates to chemistry of terpene compounds, specifically to production of 2,3-epoxypinane of formula I The method involves the following: turpentine containing 75.6% α-pinene is treated with diluted hydrogen peroxide in acetonitrile under conditions of catalytic action of manganese sulphate in the presence of sodium bicarbonate and salicylic acid. The reaction mixture is extracted with methylene chloride and the reaction mass undergoes vacuum distillation to extract 2,3-epoxypinane with 90% purity with output of 26% and a fraction rich in unreacted α-pinene (62%), which is re-epoxydated.
EFFECT: simple, cheap and efficient method of producing 2,3-epoxypinane for preparation of several medical, industrial and perfume preparations.
1 cl, 3 ex
SUBSTANCE: invention relates to chemical engineering and specifically to a method of producing hexafluoropropylene oxide (HFPO), which is a semi-product for synthesis of a wide range of compounds. According to the invention, HFPO is obtained via liquid-phase oxidation of hexafluoropropylene with oxygen at high temperature and pressure in a medium of a fluorine-containing solvent - perfluoropolyoxamethylene acetyl fluorides of general formula CF3O(CF2O)nCF2COF, where n=1-4, in the presence of a catalyst of a fluorine-containing organic peroxide compound (FOPC). The FOPC is separated from the hexafluoropropylene oxidation products and used in amount of 0.005-0.05 wt % with respect to "active" oxygen. Perfluoropolyoxamethylene acetyl fluorides are separated from hexafluoropropylene oxidation products by distillation and used in a mixture with polyfluorochloroalkane - freon-328, freon-113, freon-123a with content thereof of 0-30 wt %.
EFFECT: high rate, selectivity and explosion safety of the process of producing HFPO by stabilising concentration of the catalyst used, as well as reducing environmental impact by cutting use of freon-113.
3 cl, 3 tbl, 6 ex
SUBSTANCE: proposed method includes the catalytic oxidation of cis-cyclooctene by molecular oxygen in the liquid phase at atmospheric pressure and at the temperature of 100-130°C. Oxidation is carried out using a catalytic system comprising an organic or inorganic molybdenum compound and a phthalimide compound (N-hydroxyphthalimide, 4-methyl-N-hydroxyphthalimide, 4-phenyl-N-hydroxyphthalimide) in the amount of 0.2-0.4 wt %, at the ratio of the components of the catalytic system (molybdenum compound: phthalimide compound) 1:1÷10.
EFFECT: increasing the selectivity of production and reducing the number of by-products.
SUBSTANCE: invention relates to safe operation of chemical processing equipment during a chemical process. The method for safe operation of chemical processing equipment for oxidising olefins involves measuring the rate of pressure rise after deliberate restricted inflammation of at least one substance within the olefin oxidation process. A plurality of values of the rate of pressure rise corresponding to the set of the proposed process conditions is obtained. A specific value is selected from the plurality of values of the rate of pressure rise, which corresponds to a specific set of process conditions and ensures a safe olefin oxidation process. The olefin oxidation process is carried out in the specific chemical processing equipment using a specific set of process conditions which correspond to the selected rate of pressure rise.
EFFECT: safe operation of chemical processing equipment during olefin oxidation process.
6 cl, 2 dwg, 1 tbl
SUBSTANCE: claimed invention suggests method of ethylene oxide production, including: a. cracking ethane-containing initial material in cracking zone under conditions of cracking for obtaining olefins, including, at least, ethylene and hydrogen, b. conversion of initial oxygenate in zone of conversion of oxygenates into olefins (OTO) to obtain olefins, including, at least, ethylene; c. supply of, at least, part of ethylene, obtained at stage (a) and/or (b), into zone of ethylene oxidation together with initial oxygen-containing material, and oxidation of ethylene to obtain, at least, ethylene oxide and carbon dioxide; and in which, at least, part of initial oxygenate is obtained by supply of carbon dioxide, obtained at stage (c), and initial hydrogen-containing material, into zone for synthesis of oxygenates and synthesis of oxygenates, where initial hydrogen-containing material includes hydrogen, obtained at stage (a). In other aspect claimed invention suggests integrated system for ethylene oxide production.
EFFECT: elaboration of process for obtaining ethylene oxide and optionally monoethylene oxide by integration of processes of cracking ethane and OTO, making it possible to reduce carbon dioxide emissions and quantity of synthesis-gas, required for synthesis of oxygenates.
15 cl, 1 dwg, 6 tbl, 1 ex