41 results about "Antimony pentafluoride" patented technology

A method for the preparation of 1,2,2,2-tetrafluoroethyl difluoromethyl ether (CF₃CHFOCHF₂, Desflurane) is provided, which comprises reacting CF₃CHClOCHF₂ (isoflurane) and hydrogen fluoride in the presence of antimony pentafluoride such that desflurane is formed.

The invention discloses a low-temperature process for producing graphite fluoride comprising, immersing graphite with hydrochloric acid and hydroperoxide to obtain expanded graphite, reacting with fluorine gas of a finite concentration and Sb in sealed container to obtain antimony pentafluoride, placing the expanded graphite and antimony pentafluoride into sealed container to obtain intercalation graphite, placing intercalation graphite into confined reaction stove, letting in fluorine gas for reaction. The process according to the invention increases the utilization ratio of the fluorine gas.

The invention discloses a method for preparing graphite fluoride at low temperature. The method comprises the following steps: using ferric fluoride as a catalyst, and performing reaction of crystalline flake graphite and bromine trifluoride at low temperature to generate a graphite intercalation compound; then, performing reaction of potassium manganese hexafluoride and antimony pentafluoride to generate fluorine; and performing reaction of the fluorine generated and the graphite intercalation compound to form the graphite fluoride with high fluorine content. Through purifying treatment by a solvent, the prepared graphite fluoride is high in purity.

The invention discloses a detection method of purity of antimony pentafluoride products. The detection method comprises the following steps of: (i) preparing a sample, including sampling, solidifying and hydrolyzing; (ii) quantifying trivalent antimony, namely utilizing an oxidation-reduction titration method to measure the trivalent antimony; (iii) detecting total content of antimony, namely using an inductively coupled plasma emission spectrometer, selecting 206.836nm as an analytical line used for measuring, and detecting the content of total antimony elements in hydrolysate; (iv) calculating the content of pentavalent antimony, namely subtracting the content of the trivalent antimony from the total content of the antimony elements to obtain the content of the pentavalent antimony; andthrough calculating, obtaining the purity of the antimony pentafluoride products. The detection method is simple and convenient and feasible and is convenient for operation, the measurement accuracy is high, and the method is particularly suitable for detecting the purity of the antimony pentafluoride products prepared by fluoride and simple substance antimony as raw materials.

The invention discloses a method for preparing HCFC-244bb. According to the method, 2-chloro-3, 3, 3-trifluoropropene is used as raw materials. The method comprises the following steps that, a metal halide and an ionic liquid are used as a catalyst, and fluorination is conducted on 2-chloro-3, 3, 3-trifluoropropene and a hydrogen fluoride solution, so that HCFC-244bb is prepared, wherein the metalhalide is antimony pentafluoride or antimony pentachloride or tantalum pentafluoride or tantalum pentachloride or niobium pentafluoride or niobium pentachloride, the general formula of ionic liquid is X+A-, X+ is positive ions of C1-C8 alkyl substitution type double-alkyl imidazole, pyridine and quaternary ammonium salt, A- is negative ions of tetrafluroborate negative ions or hexafluorophosphatenegative ions, the molar ratio between the metal halide and the ionic liquid is 1-3:1, the molar ratio between hydrogen fluoride and 2-chloro-3, 3, 3-trifluoropropene ranges is 1.1-10:1, and the reaction temperature ranges from 20 DEG C to 70 DEG C. The method for preparing HCFC-244bb has the advantages that the reaction temperature is low, the conversion rate is high, the selectivity is high, and chlorine is not needed in the reaction process. The method is used for preparation of HCFC-244bb.

The invention discloses a dehydrofluorination catalyst aiming at solving the problems of low activity of the catalsyt and low selectivity to Z-type fluoroolefin. The precursor of the catalyst consistsof 30-80 percent of trivalent chromium compound, 10-35 percent of metal halide and 10-35 percent of fluoride of ammonium by mass percent, wherein the trivalent chromium compound is chromic oxide or chromium hydroxide, the metal halide is stannic chloride, titanium tetrachloride, tantalum chloride, antimony pentachloride, tin tetrafluoride, titanium tetrafluoride, tantalic fluoride or antimony pentafluoride, and the fluoride of ammonium is ammonium fluoride or ammonium bifluoride. The catalyst is prepared by the following method: evenly mixing the trivalent chromium compound, the metal halideand the fluoride of ammonium by mass percent, pressing and shaping the mixture, and then baking and activating by hydrogen fluoride. The dehydrofluorination catalyst has high activity and selectivityto the Z-type fluoroolefin and is mainly used for preparing corresponding Z-type fluoroolefin by dehydrofluorination using hydrofluorocarbon as the material under the condition of gaseous phase reaction.

The present invention provides a 1,1,1,3,3,3-hexafluoropropane production method, which comprises carrying out a reaction of 1,1,1,3,3,3-hexachloropropane and hydrofluoric acid under the effect of a catalyst to prepare the 1,1,1,3,3,3-hexafluoropropane, wherein the catalyst contains antimony pentafluoride and tin tetrafluoride. With the preparation method of the present invention, the 1,1,1,3,3,3-hexachloropropane conversion rate can be improved, and the prepared 1,1,1,3,3,3-hexafluoropropane of the present invention can be used as the refrigerant and the fire extinguishing agent.

The invention relates to antimony pentafluoride rectification equipment, which includes a distilling condenser and a recovery condenser. A liquid antimony pentafluoride crude product is subjected to heating gasification in a heating area of the distilling condenser, then undergoes at least twice condensation in a first condensation area and a second condensation area so as to form tail gas, so that the antimony pentafluoride in the gas phase can condense more fully, and the yield of the antimony pentafluoride product can be enhanced. The antimony pentafluoride primary product obtained by twice condensation in the first condensation area and the second condensation area then passes through a reflux inlet and a reflux outlet to undergo repeated cycling rectification in the distilling condenser and the recovery condenser, so that the antimony pentafluoride can be separated from other impurities more thoroughly, and the finally obtained antimony pentafluoride product can have higher purity. At the same time, the insides of the distilling condenser and the recovery condenser always maintain a negative pressure state, the temperature needed by heating gasification is lowered, and the corrosion degree of antimony pentafluoride on the rectification equipment is reduced, thereby reducing the generation of impurities and enhancing the product purity.

The invention discloses a preparation method of antimony pentafluoride. The method comprises the following steps: 1) crushing a metallic antimony block, and adding to a reactor; 2) vacuumizing the reactor to form negative pressure, and heating to 120 DEG C to remove moisture in the reactor and a material; 3) introducing nitrogen to the reactor, so as to pressurize to constant pressure; 4) slowly introducing fluorine, reacting to generate antimony pentafluoride vapor, beginning to warm in the reaction, and emptying for a plurality of times until the pressure of a buffer tank does not ascend again; 5) preparing an antimony pentafluoride product from the antimony pentafluoride vapor in a condensation reflux mode. The invention simultaneously discloses the reactor for preparing antimony pentafluoride. In the reactor, metallic antimony directly reacts with fluorine, so as to generate antimony pentafluoride, so that the product quality is improved and the process is simplified, and the reactor is convenient to operate. Condensation reflux liquid takes away a part of reaction heat, so as to well control the internal temperature of the reactor; meanwhile, continuous reaction is also ensured; chemical corrosion inside the reactor is reduced. Thus, the service life of the reactor is prolonged.

The invention relates to a method for purifying graphite by co-heating hexafluoromanganate and antimony pentafluoride generating fluorine gas, which comprises the following steps of: vacuumizing a fluorine gas reactor, and removing air in the reactor; taking materials of antimony pentafluoride and hexafluoromanganate according to the mass ratio of 2-3:1 and adding into a reactor for reaction to generate fluorine gas; arranging a plurality of groups of graphite products in a graphitization furnace according to required spacing, sequentially filling a heat preservation material and a resistor material, heating the graphitization furnace to furnace center temperature of 1,800-1,900 DEG C after the furnace loading is finished, and introducing nitrogen into the furnace core to remove the air inthe furnace center; when the temperature is raised to 1,900-2,000 DEG C, the chlorine is stopped, and the chlorine is converted to be introduced; when the temperature is raised to 2,300-2,500 DEG C,the fluorine gas generated by the reaction is communicated into the graphitization furnace. The method for purifying graphite by co-heating hexafluoromanganate and antimony pentafluoride generating fluorine gas uses hexafluoromanganate and antimony pentafluoride to produce fluorine gas instead of freon used in the purification process in the prior art, so that the problem that the adverse effect on the environment in the use process of the freon is avoided while the purification effect is good.

The invention relates to the technical field of chemical synthesis, and in particular discloses a preparation method of 2-fluorine-3-chlorine-5-trifluoromethylpyridine. The preparation method of the 2-fluorine-3-chlorine-5-trifluoromethylpyridine is characterized by comprising the following steps: taking 2-chlorine-5-trichloromethylpyridine as a raw material, taking tungsten hexachloride as a catalyst, heating and introducing chlorine to perform chlorination reaction, thereby obtaining 2,3-dichloro-5-trichloromethylpyridine; putting the 2,3-dichloro-5-trichloromethylpyridine into a fluorination kettle, adding antimony pentafluoride and anhydrous hydrogen fluoride, stirring and heating to perform reaction, cooling after reaction, washing with water, layering, feeding to a rectification kettle, and performing reduced-pressure rectification, thereby preparing the 2-fluorine-3-chlorine-5-trifluoromethylpyridine. The process is reliable, the raw materials are sufficient in the market and easily available, and the preparation method of the 2-fluorine-3-chlorine-5-trifluoromethylpyridine is low in production cost, simple in operation, high in yield and favorable for large-scale production.

The invention discloses a preparation method of lithium oxalyldifluoroborate, and belongs to the technical field of lithium ion battery electrolyte preparation. The preparation method comprises the following steps: 1) mixing lithium tetrafluoroborate, lithium oxalate, an organic solvent and an auxiliary agent, and carrying out a reaction on the obtained mixed solution to obtain a reaction solutioncontaining LiODFB, wherein the auxiliary agent is niobium pentachloride, niobium pentafluoride or antimony pentafluoride; 2) filtering the reaction solution containing LiODFB, and concentrating the filtrate to obtain a lithium oxalyldifluoroborate crude product; and 3) recrystallizing the lithium oxalyldifluoroborate crude product, and conducting drying to obtain lithium oxalyldifluoroborate. Thepreparation method provided by the invention has the advantages of high conversion rate, high product purity and high yield, and no corrosive gas is generated in the reaction process.

The invention discloses a high-strength anti-aging underground communication pipe and a preparation method thereof.The high-strength anti-aging underground communication pipe is prepared from, by mass, 180-220 parts of polypropylene, 20-24 parts of corn starch, 16-20 parts of PPG-n castorate, 14-18 parts of polyvinyl alcohol, 20-24 parts of dimethyl phthalate, 16-20 parts of cobalt acetylacetonate, 14-18 parts of butyl carbitol acet, 16-20 parts of graphite fiber, 14-18 parts of paraffin oil, 20-24 parts of polymethyl acrylate, 16-20 parts of zirconium oxide, 16-20 parts of boron carbide, 14-18 parts of zinc oxide, 20-24 parts of montmorillonoid, 16-20 parts of 1,4-dyhydroxyl sulfanilic acid, 14-18 parts of antimony pentafluoride, 20-24 parts of sodium antimonite, 16-20 parts of furan resin, 14-18 parts of Pulullan, 20-24 parts of sorbitol, 14-18 parts of tetramethrin, 20-24 parts of stearoylbenzoylmethane and 16-20 parts of aluminum dihydrogen phosphate.

The invention discloses a hydrogen fluoride detection reagent and a preparing method thereof and belongs to the technical field of gas detection. The reagent comprises, by weight, 5 to 12 parts of lanthanum trichloride, 2 to 8 parts of antimony pentafluoride, 2 to 8 parts of potassium nitrate, 3 to 6 parts of triethanolamine oleate, 2 to 7 parts of n-butyl alcohol, 3 to 8 parts of sodium sulfate, 4 to 10 parts of aluminum chloride, and 12 to 18 parts of deionized water. The preparing method includes the steps of 1, preparing premixed liquid; 2, acquiring clarified mixed liquid; and 3, allowing vacuum standing for 12 to 48 hours and performing sealing to obtain the hydrogen fluoride detection reagent. The hydrogen fluoride detection reagent is of high response speed and high accuracy, the problem that the prior art is poor in precision is effectively solved, and the content of hydrogen fluoride can be detected effectively and quickly.

Preparation of 3,5-bis-(trifluoromethyl)-benzoyl chlorides (I) involves converting a 3,5-dimethyl-benzoic acid (V) into the acid chloride (IV), subjecting the side-chains to radical chlorination, fluorinating with anhydrous hydrogen fluoride and/or antimony pentafluoride to give a 3,5-bis-(trifluoromethyl)-benzoyl fluoride and reacting with silicon tetrachloride in presence of another Lewis acid. Preparation of 3,5-bis-(trifluoromethyl)-benzoyl chlorides of formula (I) involves: (1) converting a 3,5-dimethyl-benzoic acid of formula (V) into the corresponding acid chloride of formula (IV); (2) subjecting the side-chains to complete radical chlorination to give a 3,5-bis-(trichloromethyl)-benzoyl chloride of formula (III); (3) fluorinating with anhydrous hydrogen fluoride and/or antimony pentafluoride to give a 3,5-bis-(trifluoromethyl)-benzoyl fluoride of formula (II); and (4) reacting with silicon tetrachloride in presence of another Lewis acid. [Image] X : H, F or Cl. Independent claims are included for the intermediates (III; X = F or Cl) and (IV; X = F or Cl) as new compounds.

The invention discloses a PE anti-static and anti-radiation electric mine pipe fitting, which is made of a base pipe and a functional layer, and the functional layer includes the following components in terms of mass percentage: polyethylene 15‑50wt.%, corn Starch 15-50wt.%, cobalt acetylacetonate 20-55wt.%, potassium titanate whisker reinforcement 0.1-2.0wt.%, antimony pentafluoride 0.05-1.0wt.%, furan resin 0.1-1wt.%. An antistatic coating is arranged between the base pipe and the functional layer, and the antistatic coating is composed of ethyl silicate paint. The antistatic coating composed of the ethyl silicate system of the present invention has good electrical conductivity, and its effects of removing static electricity and anti-radiation are very stable and extremely good.