The method of receiving diperchlorate

 

(57) Abstract:

Using diperchlorate (hcfc22) is the refrigerants that do not Deplete the ozone layer, and a raw material for producing Voropayev the synthesis Conditions for the fluorination of chloroform hydrogen fluoride in the presence of petaluridae antimony at high temperature and pressure conditions in the two reactors by bubbling gaseous hydrogen fluoride in the first reactor and recycling unreacted while hydrogen fluoride in the second reactor delegacia leaving the second reactor synthesis gas and returning phlegmy in the second reactor, and the reaction gases from the first reactor at a temperature of 38 to -30° C and autogenous pressure, separate pagkalipas connections gases then served in the second reactor, there serves chloroform in an amount necessary to bind unreacted in the first reactor hydrogen fluoride increases the efficiency of the process while maintaining a high degree of conversion of hydrogen fluoride 3 table

 

Same patents:

FIELD: industrial organic synthesis.

SUBSTANCE: invention relates to preparation of alkylaromatic intermediates including perfluorinated carbon atom utilized in production of agrochemically important active compounds. Intermediates simultaneously containing aniline function are obtained from homocyclic arylcarbamoyl fluoride including at least one perhalogenated carbon atom preferably bearing at least two halogen atoms capable of being replaced by fluorine atoms when in liquid-phase contact with hydrofluoric acid and water. During this reaction, molar ratio of hydrofluoric acid to arylcarbamoyl fluoride is maintained equal to 4, preferably to 5 and not higher than 11. Water is added to reaction mixture (at 10 to 90°C) when only one exchangeable halogen atom remains unreplaced. Arylcarbamoyl fluoride is obtained in situ by adding corresponding isocyanate to liquid hydrofluoric acid at temperature not exceeding 10°C. Process is carried out continuously in two reactors, the first one serving for halogen exchange reaction and the second for addition of water. Temperature 40°C is maintained until only one exchangeable halogen atom remains unreplaced.

EFFECT: increased yield and improved quality of desired product and economical characteristics.

9 cl, 4 ex

FIELD: organic chemistry, in particular difluorochloromethane useful as cooling agent, propellant, blowing agent, as well as in fluoromonomers production.

SUBSTANCE: chloroform is treated with hydrogen fluoride in presence of catalyst predissolved in chloroform with concentration of 20-30 mol.% and chlorine, at temperature of 60-110°C and pressure of 7013 atm. As catalyst mixture of antimony pentachloride, fluorotetrachloride and trichloride in ratio of 1:(0.03-0.15):(0.03-0.15), respectively is used. Process is carried out under continuous controlling reaction mass electrical resistance which is maintained in limits of 600-1600 Om. Chlorine is introduced in amount of 0.01-0.3 mass % with respect to chloroform. Method of present invention makes it possible to control synthesis parameters in dependence of reaction mass electrical resistance.

EFFECT: increased process selectivity; new catalyst.

5 cl, 4 ex

FIELD: organic chemistry.

SUBSTANCE: claimed method includes interaction of mixture C3-C6-hydrofluoroalkane/hydrogen fluoride in absence of catalyst with at least one chloro-containing or cloro- and fluoro-containing organic compound reactive towards hydrogen fluoride in liquid phase. Hydrofluoroalkane is obtained by interaction of at least one chloro-containing or cloro- and fluoro-containing precursor with hydrogen fluoride in the first step. In one of the next steps at least part of products from the first step is made to react with hydrogen fluoride, wherein one step includes separation method. Also disclosed are azeotrope or pseudo-azeotrope composition applicable for 1,1,1,3,3-pentafluorobutane purification. Claimed composition contains as main components 1.5-27.5 mol.% of 1,1,1,3,3-pentafluorobutane and 72.5-98.5 mol.% of hydrogen fluoride.

EFFECT: method with optimized parameters.

16 cl, 4 dwg, 1 tbl, 5 ex

FIELD: chemical industry; method of production of the fluorine-containing compounds.

SUBSTANCE: the invention is pertaining to the chemical industry, in particular, to the improved method of production of fluorine-containing compounds from the halogen-containing, compounds, preferably, from chlorine-containing compounds due to an exchange of halogen for fluorine at presence of the HF-additional compound of the mono- or bicyclic amine with at least two atoms of nitrogen. At that at least one atom of nitrogen is built in the cyclic system as the fluorating agent; or at presence of anhydrous hydrogen fluoride - as the fluorating agent and the indicated HF-additional compound of the mono- or bicyclic amine as the catalyst. At usage of the applicable solvents the reaction mixtures can be divided into two phases and thus to simplify the reprocessing of the products. The invention also is pertaining to the HF-additional compounds of 1.5-diazabicyclo[4.3.0]non-5-en and N,N-dialkylaminopiridin, where alkyl represents C1-C4alkyl and where the molar ratio of HF to amine makes 1:1, and to HF- additional compounds 1.8- diazabicyclo[5.4.0]undecyl-7-ene, where the molar ratio of HF to amine compounds more than 1:1.

EFFECT: the invention ensures at usage of the applicable solvents to divide the reaction mixture into two phases and thus to simplify reprocessing of the products.

17 cl, 13 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to an improved solid-phase method for synthesis of radioisotope indicators, in particular, for synthesis of compounds labeled with 18F that can be used as radioactive indicators for positron- emission tomography (PET). In particular, invention relates to a method for synthesis of indicator labeled with 18F that involves treatment of a precursor fixed on resin if the formula (I): SOLID CARRIER-LINKER-X-INDICATOR wherein X means a group promoting to nucleophilic substitution by a definite center of a fixed INDICATOR with 18F- ion for preparing a labeled indicator of the formula (II): 18F-INDICATOR; to compound of the formula (Ib):

and compound of the formula (Ih): ;

to radiopharmaceutical set of reagents for preparing indicator labeled with 18F for using in PET; to a cartridge for radiopharmaceutical set of reagents for preparing indicator labeled with 18F for using in positron-emission tomography.

EFFECT: improved method of synthesis.

13 cl, 1 sch, 3 ex

FIELD: isomerization and disproportionation catalysts.

SUBSTANCE: invention relates to crystalline α-chromium oxide, chromium-containing catalytic compositions, methods for preparation thereof, and to a process of fluorine distribution in hydrocarbon and/or halogenated hydrocarbon in presence of indicated catalytic compositions. Claimed crystalline α-chromium oxide, wherein about 0.05 to about 6 atomic % chromium in the lattice of α-chromium oxide is substituted by trivalent cobalt (Co+3) atoms is via coprecipitation of solid substance by introducing ammonium hydroxide, this method being supplemented by introducing an excess of ammonium nitrate into precipitated mixture before dehydration step and calcination step at 375 to 1000°C in presence of oxygen. Chromium-containing catalytic compositions containing crystalline cobalt-substituted α-chromium oxide as chromium-containing component optionally treated with fluorination agent are also claimed. Composition preparation procedure comprises: (a) coprecipitation of solid substance by introducing ammonium hydroxide into aqueous solution of soluble cobalt salt and soluble trivalent chromium salt, wherein solution contains at least three moles nitrate per mole chromium and has concentration of cobalt from about 0.05 to about 6 mol % based on total content of cobalt and chromium in solution, followed by introducing into solution at least three moles ammonium per mole chromium; (b) collecting coprecipitated solid substance obtained in step (a); (c) drying collected solid substance; and (d) calcination of dried solid substance at 375 to 1000°C in presence of oxygen.

EFFECT: increased activity of catalytic composition in above-indicated processes.

15 cl, 8 dwg, 13 ex

FIELD: isomerization and disproportionation catalysts.

SUBSTANCE: invention relates to crystalline α-chromium oxide, chromium-containing catalytic compositions, method for preparation thereof, and to a process of fluorine distribution in hydrocarbon and/or halogenated hydrocarbon in presence of indicated catalytic compositions. In claimed α-chromium oxide, about 0.05 to about 2 atomic % chromium in the lattice of α-chromium oxide is substituted by nickel atoms and, optionally, further chromium atoms in the lattice are substituted by trivalent cobalt atoms, the total amount of nickel and trivalent cobalt atoms in the α-chromium oxide lattice not exceeding 6 atomic %. Claimed α-chromium oxide is prepared via coprecipitation of solid substance by introducing ammonium hydroxide, this method being supplemented by introducing an excess of ammonium nitrate into precipitated mixture before dehydration step and calcination step at 375 to 1000°C in presence of oxygen. Chromium-containing catalytic compositions containing crystalline nickel-substituted α-chromium oxide as chromium-containing component optionally treated with fluorination agent are also claimed. Composition preparation procedure comprises: (a) coprecipitation of solid substance by introducing ammonium hydroxide into aqueous solution of soluble bivalent nickel salt, soluble trivalent chromium salt, and optionally soluble bi- or trivalent cobalt salt, wherein solution contains at least three moles nitrate per mole chromium and has concentration of nickel from about 0.05 to about 2 mol % based on total content of nickel, chromium, and cobalt (if present) in solution and total concentration of nickel and cobalt (if present) not higher than 6 mol % on the same basis; (b) collecting coprecipitated solid substance obtained in step (a); (c) drying collected solid substance; and (d) calcination of dried solid substance at 375 to 1000°C in presence of oxygen.

EFFECT: increased activity of catalytic composition in above-indicated processes.

15 cl, 8 dwg, 13 ex

FIELD: organic chemistry.

SUBSTANCE: claimed method includes interaction of octachlorocyclopentene with hydrogen fluoride or hexachlorocyclopentene and simultaneous interaction of formed octachlorocyclopentene with hydrogen fluoride. Process is carried out at elevated temperature (60-180°C) and pressure up to 25 kgf/cm2 in presence of catalyst of general formula SbFnCl5-n, wherein n = 1 or 2 (including fractional numbers), obtained in situ in reactor by feeding of gaseous hydrogen fluoride through layer of SbCl5.

EFFECT: high active catalyst, decreased equipment corrosion, increased product yield.

1 cl, 3 ex

FIELD: organic chemistry.

SUBSTANCE: claimed method includes fluorination of cyclic fluorine- and/or chlorine-containing product of general formula C5FxC8-x, wherein x = 0-8, mixture obtained by chlorofluorination of hexachlorocyclopentadiene with potassium chloride in dimethylformamide as solvent at 130-150°C. Fluorination is carried out in presence of water in amount of 0.9 % or less based on mass of raw materials. Dimethylformamide is filtered from salts and fed in fluorination.

EFFECT: simplified method of increased yield.

1 cl, 3 tbl, 16 ex

FIELD: industrial organic synthesis and catalysts.

SUBSTANCE: invention relates to catalysts that can be used in reactions of gas-phase fluorination of halogenated hydrocarbons and provides catalyst for fluorination of halogenated hydrocarbons with hydrogen fluoride gas, which catalyst contains chromium(III) oxide and aluminum compound, the content of latter being 2-15 wt % as calculated for Al2O3. Mixed chromium(III) and aluminum oxides have specific surface 130-300 m2/g, pore volume at least 0.3 cm3/g, and monomodal pore size distribution within the range 70 to 300 Å. Catalyst preparation and activation methods are also described. Fluorination of halogenated hydrocarbons in presence of proposed catalyst is effected at 260-380°C, pressure 0.1-0.5 MPa, and molar ratio of HF to halogenated hydrocarbon between 4:1 and 40:1.

EFFECT: increased activity and selectivity of catalyst.

11 cl, 3 dwg, 2 tbl, 8 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for preparing fluoro-organic compounds. Method involves the gas-phase catalytic hydrofluorination of trifluoroethylene at increased temperature in the presence of the chrome-magnesium-fluoride catalyst comprising 8-24 wt.-% of trivalent chrome fluoride uniformly distributed in magnesium fluoride with the dispersity index from 0.125 to 0.315 mm. The process is carried out at temperature 140-190C and time contact for 4.5 s. Method provides the high yield of 1,1,1,2-tetrafluoroethane with selectivity index up to 99.9%.

EFFECT: improved preparing method.

2 tbl, 7 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for purifying octafluoropropane. Method is carried out by interaction of crude octafluoropropane comprising impurities with the impurity-decomposing agent at increased temperature and then with adsorbent that are able to remove indicated impurities up to the content less 0.0001 wt.-% from indicated crude octafluoropropane. The impurity-decomposing agent comprises ferric (III) oxide and compound of alkaline-earth metal in the amount from 5 to 40 wt.-% of ferric oxide and from 60 to 95 wt.-% of compound of alkaline-earth metal as measured for the complete mass of the impurity-decomposing agent. Ferric (III) oxide represents γ-form of iron hydroxyoxide and/or γ-form of ferric (III) oxide. Impurities represent at least one compound taken among the group consisting of chloropentafluoroethane, hexafluoropropene, chlorotrifluoromethane, dichlorodifluoromethane and chlorodifluoromethane. Adsorbent represents at least one substance taken among the group consisting of activated coal, molecular sieves and carbon molecular sieves. Crude octafluoropropane comprises indicated impurities in the amount from 10 to 10 000 mole fr. by mass. Invention proposes gas, etching gas and purifying gas comprising octafluoropropane with purity degree 99.9999 wt.-% and above and containing chlorine compound in the concentration less 0.0001 wt.-%. Invention provides enhancing purity of octafluoropropane.

EFFECT: improved purifying method.

13 cl, 11 tbl, 12 ex

FIELD: chemical technology.

SUBSTANCE: invention relates to processing liquid fluorocarbon raw to valuable fluorine-containing gaseous products and to quenching probe method used (abrupt cooling). Method for treatment of fluorocarbon raw involves generation of high temperature in the zone of arc between at least one cathode and at least one anode, generation of high temperature in the zone by electric arc and gaseous thermal plasma with tail torch. Chemical active thermal mixture with tail torch of thermal plasma is formed from fluorocarbon raw that comprises at least one fluorocarbon compound. Fluorocarbon compound dissociates and forms at least one fluorocarbon precursor or its chemically active species having less carbon atoms as compared with fluorocarbon compound. Then chemically active thermal mixture is cooled to form fluorocarbon from the precursor or chemically active species of fluorocarbon product. Preferably, raw has a liquid form and represents fluorocarbon by-side products comprising two or more fluorocarbon compounds being one of them represents the main product containing less five carbon atom usually. Preferably, raw is added to the tail torch of plasma and plasma is fed to the high temperature zone. The self-cleansing quenching probe comprises external cylindrical component assembled on reactor and having the central channel for cooling hot gas or chemically active thermal mixture. The internal cylindrical component is installed with a gap inside of the external component and used for cooling hot gas or chemically active thermal mixture that pass through peripheral gap between components. Method provides reducing exploitation consumptions, possibility for regulating parameters of the process and the composition of feeding mixture and the yield of end products.

EFFECT: improved method for processing.

20 cl, 5 tbl, 3 dwg, 7 ex

FIELD: organic chemistry.

SUBSTANCE: claimed method includes interaction of mixture C3-C6-hydrofluoroalkane/hydrogen fluoride in absence of catalyst with at least one chloro-containing or cloro- and fluoro-containing organic compound reactive towards hydrogen fluoride in liquid phase. Hydrofluoroalkane is obtained by interaction of at least one chloro-containing or cloro- and fluoro-containing precursor with hydrogen fluoride in the first step. In one of the next steps at least part of products from the first step is made to react with hydrogen fluoride, wherein one step includes separation method. Also disclosed are azeotrope or pseudo-azeotrope composition applicable for 1,1,1,3,3-pentafluorobutane purification. Claimed composition contains as main components 1.5-27.5 mol.% of 1,1,1,3,3-pentafluorobutane and 72.5-98.5 mol.% of hydrogen fluoride.

EFFECT: method with optimized parameters.

16 cl, 4 dwg, 1 tbl, 5 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a new mixture of perfluoro-, α-chloroperfluoro- and α,ω-dichloroperfluoroalkanes of the formula: X(CF2)nY (wherein X = Y means F, Cl; X means F; Y means Cl; n = 12, 14, 16) used as powder-accelerators for plastic ski, and to a method for preparing these mixtures. Method for preparing mixtures of perfluoro-, α-chloroperfluoro- and α,ω-dichloroperfluoroalkanes involves interaction of perfluoro- and ω-chloroperfluorocarboxylic acids with potassium alkali at temperature below 60°C and then with potassium persulfate at 90-95°C. As the parent acid method involves using mixtures of perfluoroenanthic acid and ω-chloroperfluoroenanthic acid, perfluoroenanthic acid and ω-chloroperfluoropelargonic acid, perfluoropelargonic acid and ω-chloroperfluoroenanthic, perfluoropelargonic, ω-chloroperfluoropelargonic, ω-chloroperfluoroenanthic and ω-chloroperfluoropelargonic acids taken in the mole ratio = 1:1. Process is carried out in the mole ratio of acids mixture and potassium persulfate = 1:0.6. The developed method provides preparing new mixtures of powder-accelerators for plastic ski based on domestic raw.

EFFECT: improved preparing method, valuable properties of mixtures.

4 cl, 4 tbl, 9 ex

FIELD: chemical technology.

SUBSTANCE: invention relates to a method for isolation of 1-fluoro-1,1-dichloroethane, 1,1-difluoro-1-chloroethane, 1,1,1-trifluoroethane and hydrogen chloride from reaction mixture prepared by synthesis of vinylidene chloride and hydrogen fluoride. Process involves separating for layers and rectified separation. Gaseous mixture synthesis consisting of 1-fluoro-1,1-dichloroethane, 1,1-difluoro-1-chloroethane, 1,1,1-trifluoroethane, hydrogen fluoride and hydrogen chloride is absorbed with liquid mixture of substances prepared after separating for layers. The liquid mixture of substances comprises hydrogen fluoride, 1-fluoro-1,1-dichloroethane and 1,1-difluoro-1-chloroethane. Gaseous substances are fed for rectified separation and distillate obtained after rectifying that comprises hydrogen chloride and 1,1,1-trifluoroethane is fed for rectified separation and 1,1,1-trifluoroethane is recovered inversely for rectification in the amount determined by temperature and pressure values of the distillate condensation process. Vat product containing hydrogen fluoride, 1-fluoro-1,1-dichloroethane and 1,1-difluoro-1-chloroethane is fed for separating for layers and then prepared hydrogen fluoride with impurities of organofluoric compounds is recovered for absorption as liquid spraying. Mixture enriched with 1-fluoro-1,1-dichloroethane, 1,1-difluoro-1-chloroethane and containing hydrogen fluoride is fed for rectification wherein hydrogen fluoride as a component of mixture with 1,1-difluoro-1-chloroethane that is similar by the content of components to azeotropic mixture is separated and recovered its for repeated separating for layers and rectification. After repeated separation hydrogen fluoride is recovered for the synthesis. Mixture of 1-fluoro-1,1-dichloroethane and 1,1-difluoro-1-chloroethane is fed for rectified separation. Method provides increasing yield of commercial products as result of evolving gases synthesis of vinylidene chloride and hydrogen fluoride, simplifying the process and prevents accumulation of by-side products in the process.

EFFECT: improved method for isolation.

2 cl, 1 dwg, 4 ex

FIELD: chemical industry; methods and devices for reprocessing of the trifluotomethanesulfofluoride into the salt of the triluoromethanesulfo acid.

SUBSTANCE: the invention is pertaining to the improved method of production of the, which is the source product for the synthesis the trifluoromethanesulfofluoride derivatives of the triluoromethanesulfo acid, which are used in the thin organic synthesis, in production of the drugs, fungicides, extractants, catalysts, and also to the device for the method realization. The technical result of the invention is intensification of the process, the increase of productivity, the decrease of the losses of the trifluoromethanesulfofluoride at its reprocessing into the salt of the triluoromethanesulfo acid. The solution of the problem provides for feeding of the trifluoromethanesulfofluoride in its gaseous state into the mixture of the hydroxide (or oxide) the alkali-earth or the alkali metal with the water at the constant control of the pH value of the water mixture and the stopping delivery of the trifluoromethanesulfofluoride at рН=7. At that the trifluoromethanesulfofluoride is fed in the descending loop of the circulation of the water mixture at the volumetric ratio of the water mixture to the gas of not less than 6 and under the constant control of the contents of the trifluoromethanesulfofluoride in the effluent gases; feeding of the trifluoromethanesulfofluoride is terminated if its concentration in the effluent gases exceeds 0.5 % of their volume.

EFFECT: the invention ensures intensification of the process of reprocessing of the trifluoromethanesulfofluoride into the salt of the triluoromethanesulfo acid, the increased productivity, the decreased losses of the trifluoromethanesulfofluoride at its reprocessing into the salt of the triluoromethanesulfo acid.

3 cl, 4 ex, 1 dwg

FIELD: chemistry of organophosphorus compounds, chemical technology.

SUBSTANCE: invention describes a method for synthesis of monohydroperfluoroalkanes, bis-(perfluoroalkyl)phosphinates and perfluoroalkylphosphonates. Method involves treatment of at least one perfluoroalkylphosphorane with at least one base wherein base(s) are chosen from group consisting of alkali-earth metal hydroxides, metalloorganic compound in useful solvent or at least one organic base and an acid in useful reaction medium. Also, invention describes novel perfluoroalkylphosphonates and bis-(perfluoroalkyl)phosphinates, using novel perfluoroalkylphosphonates and bis-(perfluoroalyl)phosphinates as ionic liquids, catalysts of phase transfer or surfactants.

EFFECT: improved method of synthesis.

18 cl, 19 ex

FIELD: chemistry.

SUBSTANCE: invention relates to the method for producing the pentafluorethane which includes the interaction of mixture containing the fluoric hydrogen and at least one generic substance, chosen from halogenethanes with the formula CX3-CHX2 and halogenethenes with the formula CX2=CX2, where each X is chosen independently from the group consisting of F and Cl (providing not more than four of X are F), in presence of the fluorination catalyst in the reaction zone, with producing the mixture of HF, HCl, pentafluorethane, insufficiently fluorinated halogenated hydrocarbon intermediate compounds and less than 0.2 mole percent of chlorinepentafluorethane taken from the total halogenated hydrocarbons in the mixture. The fluorination catalyst contains the crystalline cobalt-substituted chromium alpha-oxide (i), where about 0.05 to 6 atom percents of chromium atoms in the crystal lattice of the chromium alpha-oxide are substituted to the trivalent cobalt (ii) and/or fluorinated crystalline oxide (i). The obtained mixture is separated at stage (a) with extraction of CF3CHF2 as a product.

EFFECT: high catalyst activity; reduced residue.

2 cl, 3 tbl, 19 ex

FIELD: chemistry.

SUBSTANCE: invention relates to the systems and methods of C3 saturated and non-saturated fluorocarbon production. Production process of the mixed product containing one or more from CF3CF=CF2, CF3CH=CF2 and CF3CCl=CF2, and one or more from CF3CHFCF3, CF3CH2CF3 and CF3CHClCF3, includes preparation of the base mixture, which contains hydrogen and one or both from CF3CCl2CF3 and CF3CClFCF3, and contact of the base mixture with a catalyst, which contains Pd and Cu with weight ratio Cu to Pd from 3:1 to 28:1 in the reactor, the configuration of which ensures reaction of saturated halogenate fluorocarbon with the catalyst.

EFFECT: development of the systems saturated and non-saturated fluorocarbon production.

26 cl, 36 tbl, 15 ex

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