55 results about "Antimony pentachloride" patented technology

A process for making 2-chloro-1,1,1,2-tetrafluoropropane. The process has the step of contacting 2-chloro-3,3,3-trifluoropropene with hydrogen fluoride in the presence of a catalyst having about 25 to about 99.9 mole percent antimony pentachloride and about 0.1 to about 75 mole percent of a metal of a Lewis acid under conditions sufficient to form the 2-chloro-1,1,1,2-tetrafluoropropane. There is a second process for making 2-chloro-1,1,1,2-tetrafluoropropane. The process has the step of hydrofluorinating about 75 to about 99.9 mole percent 2-chloro-3,3,3-trifluoropropene and about 0.1 to about 25 mole percent of one or more other hydrocarbons having at least one chlorine atom in the presence of a catalyst of fluorinated antimony pentachloride under conditions sufficient to form the 2-chloro-1,1,1,2-tetrafluoropropane. There is yet another process for hydrofluorinating 2-chloro-3,3,3-trifluoropropene to 2-chloro-1,1,1,2-tetrafluoropropane. The process has the step of contacting the 2-chloro-3,3,3-trifluoropropene with hydrogen fluoride in the presence of a vapor phase catalyst under conditions sufficient to form the 2-chloro-1,1,1,2-tetrafluoropropane.

The invention discloses a preparation method of trifluoroacetic acid low in synthesis cost. The preparation method comprises the steps of (1) preparing 1,1-difluoro tetrachloroethane from 1,1-difluoroethane or chloride thereof through ultraviolet catalysis and a chlorine reaction; (2) implementing catalytic oxidation on the 1,1-difluoro tetrachloroethane to obtain 1,1-difluoro-1-chloroacetyl chloride, wherein in the catalytic oxidation, mol ratio of the 1,1-difluoro tetrachloroethane to an oxidizing agent is 1: (2-4), dosage of the catalyst is 0.5-5% of the total weight of an reactant, and reaction temperature is 50-70 DEG C; (3) carrying out hydrogen fluoride (HF) fluoridation on the 1,1-difluoro-1-chloroacetyl chloride under the catalyst to obtain trifluoroacetyl fluoride, wherein mol ratio of the 1,1-difluoro-1-chloroacetyl chloride to the HF is 1: (2-3), reaction temperature is 40-60 DEG C, and the catalyst is either antimony or antimony pentachloride; and (4) hydrolyzing the prepared trifluoroacetyl fluoride to obtain trifluoroacetic acid.

The invention discloses a producing process for synthesizing 1, 1, 1, 2-tetrafluoroethane by a liquid phase-gas phase method, comprising three steps: firstly, using trichloroethylene and hydrogen fluoride to synthesize 1, 1, 1-trifluoro-2- chloroethane by the liquid phase method under the action of a catalyst antimony pentachloride; sencondly, extracting and separating 1, 1, 1-trifluoro-2- chloroethane, hydrogen fluoride azeotrope, i.e. separating the mixed gas and the liquid phase coarse product obtained in the first step in a separating tower from a phase to another phase, separating the hydrogen chloride from the top of the tower, extracting the 1, 1, 1-trifluoro-2- chloroethane, hydrogen fluoride azeotrope from the tower, circulating a tower kettle with high-boiling to a liquid phase fluorinated reaction kettle; and thirdly, carrying out a gas phase fluorinated reaction on the 1, 1, 1-trifluoro-2- chloroethane obtained through the chromatography by a laminator and the hydrogen fluoride through a gasifier in the gas phase fluorinated reactor. The process has advantages of high conversion rate of the trichloroethylene, good selectivity, long service life of the catalyst, high yield, simple separating operation, low consumption and the like.

A method of recovering metallic elemental antimony from waste fluorination catalyst antimony pentachloride belongs to the waste catalyst recovery technical field, and comprises the following steps of extraction and reduction, wherein, the extraction comprises the steps of using extractant to extract waste fluorination catalyst antimony pentachloride so as to obtain inorganic phase extract containing antimony ions; the reduction comprises the steps of using reducing agent to reduce the inorganic phase extract containing antimony ions to obtain mud containing antimony powder, washing, filtering and drying the mud to obtain metallic antimony. The present invention has the advantages that: the treatment process is simple and easy to implement; the influence on the environment can be decreased; the antimony powder obtained by using the method can be used to react with chlorine to generate antimony pentachloride for recycling.

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.

This invention discloses metal antimony purifying method and its mechanism. The method is to fill the industrial antimony in the chlorination tower; lead chlorine in the middle of the tower, heat at the 1/3 lower part of the tower to decompose antimony pentachloride; chloride and the superfluous mental blocks in the tower react to create antimony trichloride. The antimony trichloride in the storage tank automatically flows to re-boiling equipment and steam to go into rectification 1; through reflux control valve adjust flow amount of antimony trichloride and reflux amount, and the antimony trichloride goes into the re-boiler of rectification 2; the lower output mouth of the rectification tower arch is connected by the channel with the material interface of the storage tank that has two outputting mouths connected with the computation tank of reductive tank and re-boiler of sub-grade rectification system by the tube. The upper outputting mouth is connected with the residue tank by the pipeline; orderly connect the multi-grade rectification tower and continuously bring in the superfluous hydrogen and revert it and get 99.999%, 99.9999% and 99.99999% metal antimonies.

The invention relates to a norbornene-perfluoromethyl vinyl ether binary copolymer catalyst and a binary copolymerization method. The preparation method of the catalyst is characterized by comprising the following steps: in a container of dry inert gas atmosphere, dissolving antimony pentachloride and ligand in a first solvent; dropwise adding tetra-isopropoxy titanium at 200-300rpm, and then continuously stirring for 30-50 minutes at 30-50 DEG C to obtain an antimony-titanium complex catalyst; adding a norbornene monomer and a perfluoromethyl vinyl ether monomer in a molar ratio of 1:1 into an autoclave after repeated vacuumizing and nitrogen charge; adding a second solvent and dissolving; adding the antimony-titanium complex catalyst, and reacting for 1-6 hours at 30-120 DEG C and under the pressure of 0.1-8MPa; pouring the reaction product into an ethanol solution containing 4-5wt% of hydrochloric acid; washing the obtained precipitate with ethanol to neutrality; and performing vacuum drying to obtain a norbornene-perfluoromethyl vinyl ether binary copolymer.

The invention discloses a method for preparing sodium pyroantimonate by using waste antimony pentachloride as a raw material. The method comprises the following steps of A, an extraction step, wherein a waste antimony pentachloride catalyst is extracted by using industrial water to obtain an organic phase and an inorganic phase, the inorganic phase is separated to obtain an antimony ion containing water solution, and the volume ratio of the waste catalyst to the industrial water is 1:0.5-1:2; B, an oxidation step, wherein the antimony ion containing water solution is oxidized by using hydrogen peroxide to obtain antimony oxidation liquid, and the hydrogen peroxide water using amount is 1-2 times of the theoretic using amount; and C, a neutralization step, wherein neutralization reaction on the antimony oxidation liquid is carried out by using sodium hydroxide water solution, a pH value of the reaction liquid is regulated to be between 7 and 13, and after the reaction is carried out for 10-300 minutes at 50-90 DEG C, cooling, filtering, washing and drying are performed to obtain sodium pyroantimonate. The method has the advantages of simple process, low material consumption, low cost, good quality of the product and environmental friendliness; the extraction ratio of antimony is more than 99.2 percent, and the highest is 99.85 percent; and the total yield of antimony is more than 98 percent, and the highest is 99.65 percent.

The invention discloses a low temperature synthesis method for graphite fluoride. The method includes: reacting graphite with antimony pentachloride at 300-400DEG C for 7h to prepare an antimony pentachloride graphite intercalation compound; and introducing a fluorine-nitrogen mixed gas into the reactor to carry out reaction for 5-10h, with the fluorine accounting for 12%-15% of the total volume of the fluorine-nitrogen mixed gas. The graphite fluoride synthesis reaction temperature is far below its decomposition temperature, thus avoiding the potential danger of explosion. Graphite fluoride can form in ordinary fluorination equipment, the reaction temperature control range is large and is easy to control. The production cost is low, and the output rate is high.

The invention discloses a method for preparing 4.4-dichlorodiphenyl sulfone by using sulfur trioxide, which comprises the following steps: dripping sulfur trioxide into chlorobenzene to perform a sulfonation reaction; after the sulfonation reaction is finished, adding dimethyl sulfoxide serving as a catalyst, heating, introducing nitrogen, dripping thionyl chloride to perform an acid halogenation reaction and absorbing sulfur dioxide and hydrogen chloride generated in an acid halogenation reaction process by using alkaline liquor; and after acid halogenation reaction is finished, adding antimony pentachloride serving as a catalyst, introducing nitrogen, and dripping chlorobenzene at room temperature to perform a Friedel-Crafts reaction to produce coarse 4.4-dichlorodiphenyl sulfone. Therefore, the method can effectively lower reaction temperature and reaction time, thereby saving production cost; in addition, nitrogen is introduced into the reaction solution in the whole reaction process, so the production of byproducts is reduced effectively. The 4.4-dichlorodiphenyl sulfone yield of the method may reach 98 percent.

The invention provides an antimony pentachloride waste liquid treatment system. The antimony pentachloride waste liquid treatment system mainly comprises a primary reaction kettle and a secondary reaction kettle, wherein the primary reaction kettle is sequentially connected to a vacuum filtration machine, a first-stage filtrate tank, a first pipeline pump and the secondary reaction kettle; the secondary reaction kettle is sequentially connected to a filter press, a secondary-stage filtrate tank, a second pipeline pump and a wastewater treatment system; the primary reaction kettle is sequentially connected to a graphene condenser, a liquid distribution tank and a first-stage falling film absorption tower, and the liquid distribution tank is respectively connected to a dilute acid storage tank and a chloroform storage tank; the first-stage falling film absorption tower is sequentially connected to a fourth pipeline pump, the first-stage falling film absorption tower, a secondary-stage falling film absorption tower and a third pipeline pump; the secondary reaction kettle, the first-stage filtrate tank and the secondary-stage falling film absorption tower are connected to a vacuum buffer tank which is connected to a vacuum pump. The antimony pentachloride waste liquid treatment system can be used for recovering antimony oxide in waste liquid very well and collecting acid gas and chloroform generated in a reaction process and is complete in treatment and good in effect.

A method for producing difluoromethane, including the catalytic reaction of dichloromethane with hydrogen fluoride in the liquid phase, in the presence of chlorine, and in the presence of an ionic liquid catalyst consisting of the product of the reaction of antimony pentachloride with an organic salt having the general formula X+A, where A is a halide anion or hexafluoroantimonate, and X+ is a quaternary ammonium cation, quarternary phosphonium or ternary sulfonium. Further, equipment suitable for implementing said method.

The invention discloses a method for increasing a proportion of paradichlorobenzene in a benzene chlorination product. The method comprises the steps: adding a combined catalyst in benzene, introducing chlorine under a stirring condition, to obtain the chlorination product with high paradichlorobenzene content, wherein the temperature of the whole process is controlled to be 50-80 DEG C, and the amount of the introduced chlorine is controlled to ensure that the conversion rate of the benzene is more than 99 percent and the conversion rate of chlorobenzene is more than 93 percent, and in addition, the combined catalyst comprises a main catalyst and a co-catalyst, the main catalyst is one of iron powder, ferric trichloride, aluminum trichloride, antimony trichloride, antimony pentachloride or tin tetrachloride, the co-catalyst is a dibenzo thiazepine organic matter, and the weight ratio of the main catalyst to the co-catalyst is 1:1. According to the method, the proportion of the paradichlorobenzene in the product is effectively increased, the ratio of the paradichlorobenzene to orthodichlorobenzene can reach 4.8, the content of the orthodichlorobenzene is less than 0.4 percent, and the content of phenyl polychloride is less than 1 percent.

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 invention discloses preprocessing equipment for an antimony pentachloride waste catalyst and a processing method thereof. The technical problem that the processing on the antimony pentachloride waste catalyst is lacked in the prior art is mainly solved. The preprocessing equipment for the antimony pentachloride waste catalyst disclosed by the invention comprises a reactor, wherein the reactoris connected with a rectifying tower; the rectifying tower is connected with a catalyst processing tank; the catalyst processing tank is connected with a gas-liquid separation tank; the gas-liquid separation tank is connected with a washing unit; the washing unit is connected with an alkali washing unit; the alkali washing unit is connected with a burning device. According to the preprocessing equipment disclosed by the invention, the problem is solved preferably, and the preprocessing equipment can be used for preprocessing the antimony pentachloride waste catalyst.

The preparation of chlorinated hydrocarbons, such as pentachloropropanes, such as 1,1,1,2,3-pentachloropropane, from tetrachloropropanes, such as 1,1,1,3-tetrachloropropane, in the presence of a polyvalent antimony compound that includes a pentavalent antimony compound, such as antimony pentachloride, is described. Also described are methods for preparing optionally chlorinated alkenes, such as, tetrachloropropenes, from chlorinated alkanes, such as pentachloropropanes, in the presence of polyvalent antimony compound that includes a pentavalent antimony compound, as well as methods for recovering polyvalent antimony compounds from such processes.

The invention discloses a preparation method of 1, 3-dichloro-1, 1-difluoropropane, and belongs to the technical field of fluorine-containing chemicals. Under the action of a lewis acid catalyst, in the presence or absence of a solvent, 1, 1, 1, 3-tetrachloropropane reacts with antimony trifluoride to generate 1, 3-dichloro-1, 1-difluoropropane, and the lewis acid catalyst is niobium pentachloride, tantalum pentachloride or antimony pentachloride. According to the preparation method of the 1, 3-dichloro-1, 1-difluoropropane, the raw materials are easy to obtain, the conversion rate is high, the 1, 3-dichloro-1, 1-difluoropropane can be prepared with high selectivity, and the selectivity can reach 90% under better conditions.

The invention discloses a synthesis method of polydifluorodichloroethylene, belonging to the technical field of synthesis. The method comprises the following steps: by using trichloromethane as a raw material, introducing fluorine gas for fluorination, carrying out fluorination again under the actions of added magnesium fluoride and anhydrous hydrofluoric acid, putting the reaction product in a reaction kettle, simultaneously adding trifluoroacetic acid and antimony pentachloride, introducing hexafluoropropylene gas, reacting to obtain difluorodichloroethylene, taking out the difluorodichloroethylene, putting the difluorodichloroethylene into an enamel polymerization still, and carrying out polymerization reaction by using potassium permanganate as a catalyst, potassium persulfate as an initiator and sodium fluosilicate as an activator, thereby obtaining the polydifluorodichloroethylene. The method has the advantage of simple synthesis steps. The obtained product has low linear expansion coefficient (lowered by 25.8% or above), and is easy for formation and secondary processing. The product has the advantages of favorable mechanical properties and favorable resilience, and the strength is enhanced by 50% or above.

The invention discloses a method for recovering diantimony trioxide from a monochlorodifluoromethane reaction residual liquid. The method comprises the following steps: 1, extracting: extracting wasteantimony pentachloride in a monochlorodifluoromethane reaction residual liquid in a hydrolysis kettle by using an extracting agent to obtain an antimony ion-containing aqueous solution, carrying outsteam stripping on the antimony ion-containing aqueous solution by using nitrogen with a flow rate of 100 L/min for 6 hours, and absorbing the steam stripping substance by using an alkaline solution;2, reducing: reducing the antimony ion-containing aqueous solution by using a reducing agent to obtain an aqueous solution containing trivalent antimony ions; 3, hydrolyzing: hydrolyzing the aqueous solution containing the trivalent antimony ions by using water to obtain a turbid liquid containing diantimony trioxide solid; and 4, carrying out suction filtration on the hydrolyzed turbid liquid containing the diantimony trioxide solid, and drying to obtain diantimony trioxide with a content of 99.9% and a particle size of more than 400 meshes and a hydrolysis mother liquor.

The invented compound contains effective dose of antimony halide and medicinal carrier and/or excipient. The described antimony halide includes antimonous chloride, antimonous bromide, antimonous triiodide, antimonous fluoride, antimonous pentafluoride and antimony pentachloride, the active component in the described compound is one of the above-mentioned antimony halide or their combination. Said invention relates to adoption of antimony halide, special SbCl3 to cure various leukemia and malignant lymphoma.