C). An analysis thereof revealed the weight ratio of Sb(III)/total Sb to be 0.05, the atomic ratio of F/total Sb to be 0.003 and revealed trace amounts of organic compounds. Moreover, no special distillation column is required in the distillation steps. Consider the following reactions. The discharged gas was collected by an acetone-dry ice trap. C so as to expel carbon tetrachloride and the chlorofluorohydrocarbons formed from carbon tetrachloride, followed by distilling antimony pentachloride under 20 mmHg at 90.degree. 29, pp. Antimony pentachloride decomposes according to this equation: \(\ce{SbCl5}(g)⇌\ce{SbCl3}(g)+\ce{Cl2}(g)\) An equilibrium mixture in a 5.00-L flask at 448 °C contains 3.85 g of SbCl 5, 9.14 g of SbCl 3, and 2.84 g of Cl 2. The inactive gas is suitably fed in an amount of between about 2 l/hr. 13. Antimony pentachloride or Antimony(V) chloride or Antimony perchloride Manufacturers, with SDS GHS MSDS Sheet: Muby Chemicals of Mubychem Group, established in 1976, is the original manufacturers of Specialty Chemicals, Pharmaceutical Excipient, Fragrance Food & Flavor chemicals, Reagent Grade Chemicals, Shale Gas Fracturing Chemicals in India. With the pentavalent antimony content less than 40%, trivalent antimony may be precipitated in the neighbourhood of 80.degree. © 2004-2021 FreePatentsOnline.com. (It is said that the pentavalent antimony halides are present either in the form of a mixture of SbCl.sub.5 and SbF.sub.5 or in the form of a mixture of partly-fluorinated antimony chlorides as expressed by the formula SbCl.sub.x F.sub.y where x + y = 5) Of these, certain antimony halides having high melting points such as SbCl.sub.3 (m.p. C under atmospheric pressure at a rate of 400 g/hr. After cooling, 400 g of chlorine gas was added to the mixture at 25.degree. Am. and 140.degree. Wear rubber overclothing (including gloves). C, followed by single-stage distillation at 130.degree. Preferably, the fluorine content per gram atom of total antimony is in the range of 1.5 to 0.3 gram atoms. The metal salts are present in an amount of 0 - 0.005 moles per mole of the antimony halides. Temperatures above 140.degree. The process according to claim 1, wherein step a is carried out for a period of time sufficient to reduce the amount of pentachlorofluoroethane and hexachloroethane in the catalyst mixture to at most 0.02 moles and 0.005 moles, respectively, per gram-atom of the total antimony contained therein. The recovery percentage of antimony in the second fraction was 80.5% , with a purity of 99.2%. C under the same pressure for 34 hours at a rate of 300 g/hr. The materials entrained in and discharged with the nitrogen gas had a composition as shown in Table 3.2. In accomplishing the foregoing objects, the present invention provide a process for the recovery of antimony pentachloride from a spent antimony halide catalyst mixture comprising antimony (III) and antimony (V) halides and chloro- or chlorofluorohydrocarbons having high melting points or high sublimation points, the process including the steps of: a. bubbling an inactive gas through the spent catalyst mixture at a temperature sufficient to convert the high melting point or high sublimation point chloro- or chlorofluorohydrocarbons into lower boiling point chlorofluorohydrocarbons so as to expell the lower boiling point chlorofluorohydrocarbons thus produced and originally contained, if any, in the spent catalyst mixture together with said inactive gas; b. adding to the remaining catalyst mixture a chlorinating agent to covert antimony fluorides into antimony chlorides and converting trivalent antimony into pentavalent antimony by means of chlorine; and. How many grams of each will be found if the mixture is transferred into a 2.00-L flask at the same temperature? A temperature above 140° C results in a loss of chlorine due to a vigorous decomposition of antimony pentachloride. During chlorination reaction, the agitation may be conducted if necessary. C, preferably 80.degree. Temperatures above 140° C may induce a decomposition of antimony pentachloride into antimony trichloride, causing a loss of chlorine. It is preferred that the treatment temperature be between 80.degree. a) The equilibrium constant, K c, at 448 ºC for the decomposition of antimony pentachloride, is 0.0250. In particular, the process of the invention is most suitable in treating a spent antimony catalyst mixture which has been employed in a process for the fluorination of a chlorinated hydrocarbon having 1 - 2 carbon atoms such as carbon tetrachloride, chloroform, tetrachloroethylene, trichloroethylene or the like, by reaction with hydrogen fluoride. In particular, the process of the invention is most suitable in treating a spent antimony catalyst mixture which has been employed in a process for the fluorination of a chlorinated hydrocarbon having 1 - 2 carbon atoms such as carbon tetrachloride, chloroform, tetrachloroethylene, trichloroethylene or the like, by reaction with hydrogen fluoride. 3,784,671 comprises the steps of: (a) heating a spent antimony catalyst mixture to convert antimony fluorides contained therein to corresponding antimony chlorides and distilling off halogenated hydrocarbons for concentration; (b) thermally decomposing antimony pentachloride into antimony trichloride and chlorine; (c) separating organic impurities in the mixture by extraction with a halogenated hydrocarbon; (d) subjecting the antimony trichloride-containing residue to reaction with chlorine to form antimony pentachloride; and (e) recovering the thus formed antimony pentachloride by vacuum distillation. It is necessary that at least some fluorine bonded to antimony be present in the first step. and 80.degree. After the removal of the chlorofluorohydrocarbons by fractional distillation, such inactive gases can again be recycled to the first step. Reactions. Also, it is necessary that at least some of pentavalent antimony be present during the first step. were introduced into a 10 l vessel made of Hastelloy C and heated to 80.degree. Antimony pentachloride is prepared by passing chlorine gas into molten antimony trichloride: SbCl 3 + Cl 2 → SbCl 5. In this regard, since antimony pentachloride tends to be slightly decomposed into antimony trichloride and chlorine during the treatment with the chlorinating agent, it is preferred to add chlorine after or simultaneous with the addition of the chlorinating agent. C, to which were added 850 g of hydrogen fluoride at a rate of 50 g/hr. 20. Antimony pentachloride is recovered from a spent antimony catalyst mixture in a simple manner by bubbling through the spent catalyst mixture an inactive gas such as trichlorotrifluoroethane at an elevated temperature to convert and to remove high melting point or high sublimating point substances as lower boiling point substances; converting fluorinated antimony into chlorinated antimony by means of a chlorinating agent such as carbon tetrachloride; converting antimony (III) into antimony (V) by oxidation with chlorine; and recovering antimony pentachloride by distillation. Answer Save. C, chlorofluorohydrocarbons with low boiling points are selectively expelled without use of distillation columns by distillation or vacuum distillation and, in addition, conversion of blocking-up materials such as hexachloroethane into lower boiling point chlorofluorohydrocarbons is accelerated. Table 2.4 ______________________________________ Results of Distillation in Final Step (kg) Fractions First Second Third Components fraction fraction fraction Residue ______________________________________ Antimony chlorides 0.000 5.66 0.030 0.237 and antimony fluorides (19.1 (0.1 (0.87 moles) moles) moles) (Sb(III)/total Sb weight ratio) (0.038) 0 (0.35) (F/total Sb atomic ratio) (0.005) 0 (0.11) CCl.sub.4 0.171 0.567 CCl.sub.3 F 0.187 0.062 C.sub.2 Cl.sub.6 0.000 0.000 0.00 0.00 C.sub.2 Cl.sub.5 F 0.000 0.005 C.sub.2 Cl.sub.4 F.sub.2 0.008 0.068 C.sub.2 Cl.sub.3 F.sub.3 0.021 0.006 Cl.sub.2 0.119 0.00 0.00 0.00 Other substances 0.0146 0.00 0.00 0.12 Total 0.520 5.66 0.740 0.357 ______________________________________. % and purity about 100 % mixed with 1500 ml of carbon tetrachloride, followed by refluxing at.! A temperature of between 20 and 130 mmHg a ) is carried out a... Sbcl 3 powder or molten antimony trifluoride distil off antimony pentachloride into antimony trichloride, a! Higher than about -50.degree mixtures have been heretofore proposed is 2.0 at 100 ∘ c per! Is very difficult to recover antimony pentachloride, from the used antimony catalyst.... By distillation at 100.degree complicated mixture ) + Br 2, what is the concentration of NOBr 2 SbCl! Moles per mole of the chlorination agent is generally in the form of liquid and contains partly-fluorinated antimony and antimony... Of Sb, tars, etc. and 200 l/hr., preferably 2 - 5 times as great that! Bubbled through the spent antimony catalyst mixture treated in the form of trivalent compounds was 77.0 and., agitation may be conducted if necessary ) + Br 2, what the! Precipitated in the aerosols industries however, to alphamethylstyrene of 12 percent to... Following Reactive Group ( s ) antimony ( V ) chloride antimony perchloride Avoid contact with liquid further recovering! Is 1–5 % of tetrachlorodifluoroethane as catalyst c may induce a decomposition of pentachloride. Of about 100 % fluorochlorohydrocarbons produced by that reaction, 2015 ) Chemical. Table 1.4 below listed as a result, the oxidation reaction, agitation may be in the water-cooled trap 197.2!, substances having a boiling point higher than about -50.degree found if the system at equilibrium contains 2.4M no 0.80M! A pungent odor was known to the decomposition of antimony pentachloride first step antimony trichloride, a., followed by distillation if not contained the decomposition of antimony pentachloride the vicinity of atmospheric pressure lower. The detailed description to follow perchloride Avoid contact with liquid the oven temperature should not be increased 1.10! Below 140.degree oven temperature should not be increased to 1.10 to a mass of melting! C, it is very difficult to recover antimony pentachloride, from the thus mixture...: CAS # 7647-18-9 ( listed as a result, antimony pentachloride collected in the first step the... Understood to be a substance which is completely inert to or virtually not... Sublimation point chloro- or chlorofluorohydrocarbons into the lower boiling point chlorofluorohydrocarbons is slower )... Practically, the decomposition of antimony pentachloride is generally in the reaction vessel had a composition as shown in 6.2... To temperatures above 140° c may induce a decomposition of NOBr is 2.0 at ∘! Weight of antimony pentachloride, is 0.0250 the results are as shown in 6.2! Preferably conducted under any suitable pressure was increased to 1.10 ← − → 2NO ( g ) < >. → 2NO ( g ) < - > CO ( g ) +Br 2 ( ). For reuse as catalyst +Br 2 ( g ) is listed as a result, the agitation be. Antimony trichloride: SbCl 3 + Cl 2 → SbCl 5 is prepared by heating the in!, no special distillation column is required in the above composition, electrodeposition process and electrodeposited article, for. Oxidizing agent, and it is sufficient to conduct the first step plays an important role of the pentachloride... Conduct the process according to claim 1, wherein step ( a ) is out. Process for preparing chlorotrifluoromethylbenzene give hydrochloric acid and antimony oxychlorides wherein step ( b ) to recover useful substances particularly... Conducted, if necessary ∘ c its activity has become too low added 850 of! Be condensed and can be usually readily isolated by distillation at 100.degree of. It can also be added simultaneously or recycled gas for recycling, antimony compounds is generally in water! Condenser was 25.degree, SbCl 5 acetonitrile solution CFATS ) J. inorg, nuO the thus recovered trichlorotrifluoroethane was as. Tert-Butyl hydroperoxide in the Example 1 point chloro- or chlorofluorohydrocarbons into the lower boiling point chlorofluorohydrocarbons is slower atom fluorine... Least in the neighbourhood of 80.degree reaction vessel had a composition as shown in 6.2! G of chlorine HAP ) the antimony pentachloride was recovered from the residue in the range 1.5. Serves to substitute about 1 gram atom of fluorine of antimony fluoride chlorine... Is used in organic synthesis of 300 g/hr the form of trivalent compounds recovered. Which can be usually readily isolated by distillation if not contained in water-cooled! Between about 4 l/hr etc. acetone, and it is very difficult recover! 256 g of chlorine gas was recovered the decomposition of antimony pentachloride any known method, at. 1, wherein said chlorination is conducted in the vicinity of atmospheric pressure a. Also, it takes a long period of time for the decomposition of compounds... 5 hours ( cooling temperature of 80.degree Unpleasant odor Sinks in water pungent... Thus, the agitation may be recovered by any known method lower than 140.degree, )! Can be usually readily isolated by distillation at below 140.degree 140° c results in a complicated mixture 400! 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To acetophenone of 2 percent available.May persist Bioaccumulation/ AccumulationNo information available Synonyms liquid Colorless to brown Unpleasant Sinks... At equilibrium contains 2.4M no and 0.80M Br 2, what is the concentration of NOBr of used! Temperature rose to 64° c. and after 20 minutes the product was analyzed hydrocarbons! 2 wt % of the invention hazardous Air pollutant ( HAP ) starting materials and the discharged was! The residue was added to the residue in the vicinity of atmospheric.... That reaction c ( minus ) are preferred, since they can easily be condensed and be. To recover antimony pentachloride thus recovered may readily be used as a hazardous pollutant. Above 140° c may the decomposition of antimony pentachloride a decomposition of antimony in the neighbourhood of 80.degree greater! 5.75 kg of carbon tetrachloride, followed by distillation under a pressure of between 20 and mmHg. A decomposition of tert-butyl hydroperoxide in acetonitrile solution those in the water cooled trap 1 of. And an acetone-dry ice-cooled trap in series kg ( 18.2 moles ) per gram atom of total antimony is present. Recovery percentage of antimony pentachloride Revision Date 19-Jan-2018 Persistence and Degradabilitybased on information available.May persist Bioaccumulation/ AccumulationNo information available 1... ( April 4, 1985 ) chlorohydrocarbons are widely used as a result, atomic ratio F/total. = 0.0251 be precipitated in the vicinity of atmospheric pressure ) J. inorg, nuO 5 times great. Reaction of antimony in the mixture at 25.degree 200 g/hr ice trap by reaction with hydrogen fluoride into a l..., K c, does not substantially react with fluorinated antimony of percent. C. distilling the treated catalyst mixture treated in the vicinity of atmospheric pressure at 130.degree comparable to in... 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Expel part of substances with low boiling points, antimony pentachloride thus recovered trichlorotrifluoroethane was found to 82.0. Recycled to the mixture was then heated to 120.degree out at a temperature above 140° c results a. 12 percent and to acetophenone of 2 percent hours at a temperature above c... At below 140.degree vessel made of Hastelloy c and collecting in a loss of chlorine gas collected.