The maximum amount of pentavalent antimony is not specifically limited. 3,760,059, there is disclosed a process wherein a spent antimony catalyst mixture is mixed with trichloroethylene and heated to reduce all of the antimony compounds contained in the catalyst mixture into antimony trichloride, and the antimony trichloride is then crystallized in organic solution and separated, followed by coversion to antimony pentachloride by oxidation. The process according to claim 1, wherein said spent antimony halides catalyst mixture has been used in the fluorination of chlorinated hydrocarbons having 1 or 2 carbons with hydrogen fluoride. It is necessary that at least some fluorine bonded to antimony be present in the first step. Answer Save. and 100 l/hr. This material contains Antimony(V)-Pentachloride (listed as Antimony), 99%, (CAS# 7647-18-9) which is subject to the reporting requirements of Section 313 of SARA Title III and 40 CFR Part 373. C, preferably between 20.degree. and the discharged gas was collected by a water-cooled trap. The spent catalyst mixture may further contain chlorinated hydrocarbons used as starting material for the fluorination reaction and fluorochlorohydrocarbons produced by that reaction. 6 years ago. Total 5.58 -- ______________________________________. The discharged gas was collected by an acetone-dry ice trap. C to remove low boiling point substances under atmospheric pressure, thereby obtaining 7.52 kg of a spent antimony catalyst mixture having the composition shown in Table 6.1. 4. MDL number MFCD00011213. Happy To Help. With chlorine it forms antimony trichloride; hydrochloric acid has … Trichlorotrifluoroethane was bubbled through the spent antimony catalyst mixture under atmospheric pressure at 130.degree. The thermal decomposition of 1 yields B … C under reduced pressure. 79.degree. 29, pp. C. The distillation is preferably conducted under a pressure of between 20 and 130 mmHg. To the residue was added 3 kg of carbon tetrachloride, followed by refluxing at 100° C for 5 hours (cooling temperature 25° C). 79° C) have a tendency to block up distillation apparatus. Of these, substances having a boiling point higher than about -50° C (minus) are preferred, since they can easily be condensed and can be reused or recycled. The discharged antimony halides can be trapped by suitable means and, after removal of certain organic compounds contained therein, can be again introduced into the system or readily used as catalyst. The resultant catalyst mixture was then heated to 120° C to remove low boiling point substances under atmospheric pressure, thereby obtaining 7.52 kg of a spent antimony catalyst mixture having the composition shown in Table 6.1. C under the same pressure for 34 hours at a rate of 300 g/hr. During the course of employment over a long period of time, however, various impurities or other substances are accumulated in the liquid catalyst, including small amounts of impurities introduced with the chlorinated hydrocarbons such as chlorohydrocarbons, water and the like; small amounts of high boiling point or high sublimating point chloro- or chloro-fluoro-hydrocarbons secondarily produced during the contact reaction; and inorganic metal salts such as of nickel, chromium iron, and the like, the metals being mainly derived from the materials of the reaction vessel. 19. and the discharged gas was collected by a water-cooled trap. Also, it is necessary that at least some of pentavalent antimony be present during the first step. With a content of bound fluorine smaller than the above defined range, the sublimate substances with high sublimation points and high melting point substances can not be satisfactorily converted to low boiling point substances, or it takes along period of conversion time because of lower conversion rate. From 11.5 kg of a spent antimony catalyst mixture, as shown in Table 2.1, obtained by heating in a 10 l vessel made of Hastelloy C (product of Haynes Stellite Co.) under normal pressure at 130° C to remove substances with low boiling points, antimony pentachloride was recovered. C at atmospheric pressure to distil off the remaining chlorinating agent and the substances converted from the chlorination agent, and also chlorine, as the case may be. Clean Air Act: CAS# 7647-18-9 (listed as Antimony compounds) is listed as a hazardous air pollutant (HAP). Presence of a small amount of trivalent antimony is desirable, since the trivalent antimony serves as a promoter for conversion of undesirable compounds such as hexachloroethane into the lower boiling point compounds. The decomposition of antimony pentachloride (SbCl 5) isdescribed by the equation: SbCl 5 (g) ↔ SbCl 3 (g) + Cl 2 (g) At 448°C, the equilibrium constant for this reaction is.0251. (EPA List of Lists, 2015) DHS Chemical Facility Anti-Terrorism Standards (CFATS) The thus recovered trichlorotrifluoroethane was reused as the inactive gas for the bubbling step. The process according to claim 1, wherein said chlorination and said oxidation are conducted simultaneously. C under atmospheric pressure so as to expel carbon tetrachloride and the chlorinated hydrocarbons produced from carbon tetrachloride, thereby obtaining a distillate (hereinlater referred to as "first fraction"). Examples of the former inactive substances include helium, argon, nitrogen, carbon dioxide, sulfuryl fluoride (SO.sub.2 F.sub.2), and the like. Antimony pentachloride can be usually readily isolated by distillation if not contained in a complicated mixture. Such an antimony catalyst is generally in the form of liquid and contains partly-fluorinated antimony and trivalent antimony. Example 1 was further repeated in the same manner and conditions as described, but the oxidation by the reaction with chlorine was conducted prior to the chlorination with carbon tetrachloride. This material contains Antimony(V)-Pentachloride (listed as Antimony), 99%, (CAS# 7647-18-9) which is subject to the reporting requirements of Section 313 of SARA Title III and 40 CFR Part 373. As a result, the materials entrained in and discharged with the trichlorotrifluoroethane had the composition as shown in Table 1.2. As to the amount of the chlorinating agent, one mol of carbon tetrachloride or chloroform serves to substitute about 2 gram atoms of fluorine bonded to antimony with chlorine. Purification of the third fraction was also effected by distilling off CCl.sub.4, CCl.sub.3 F, C.sub.2 Cl.sub.4 F.sub.2 and C.sub.2 Cl.sub.3 F.sub.3 contained therein at 50.degree. C since decomposition of antimony pentachloride would take place. 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. Table 1.1 ______________________________________ Composition of Spent Antimony Catalyst Mixture Weight Molar Compositon Composition Components (kg) (mol) ______________________________________ Antimony chlorides and antimony fluorides (weight ratio of Sb(III)/total Sb = 0.207 3.81 13.8 and atomic ratio of F/total Sb = 0.57) C.sub.2 -halogenated hydrocarbons C.sub.2 Cl.sub.6 0.14 0.58 C.sub.2 Cl.sub.5 F 0.67 3.03 others 0.77 3.87 Other substances (inorganic salts other than 0.19 -- those of Sb, tars, etc.) This lowers the catalytic activity and renewal of catalyst becomes necessary when its activity has become too low. The equilibrium constant, K c , for the decomposition of NOBr is 2.0 at 100 ∘ C . The first step plays an important role of the process of the present invention. C. The antimony catalyst mixture remaining after the first step is mixed with a chlorinating agent to convert the antimony fluorides into antimony chlorides, and with elemental chlorine to convert trivalent antimony to pentavalent antimony. The recovery percentage of antimony in the second fraction was 80.5% , with a purity of 99.2%. Lv 5. The process according to claim 1, wherein antimony pentachloride is recovered by distillation at 100.degree. C) and the like (which also tend to block up distillation apparatus), or small amounts of the starting materials for the fluorination reaction and the reaction products. Then, trichlorotrifluoroethane was bubbled through the spent antimony catalyst mixture with the above composition, first at 120.degree. The discharged gas was recovered by a water cooled trap. The amount of the antimony pentachloride collected in the water-cooled trap was 5.41 kg (18.2 moles). C), pentachlorofluoroethane (m.p. 9.83 kg of a used antimony catalyst mixture consisting of 6.02 kg (21.1 moles) antimony halides (weight ratio of Sb (III)/total Sb = 0.22, atomic ratio of F/total Sb = 0.10), 3.53 kg of halogenated hydrocarbons (CCl4, CCl3 F, C2 Cl6, C2 Cl5 F, etc.) The spent antimony catalyst mixture comprises pentavalent antimony halides as its primal components but antimony is also present in the form of trivalent compounds. Liquid Colorless to brown Unpleasant odor Sinks in water remove substances with low points... Not adversely affect the process of the process according to claim 1, wherein antimony pentachloride was obtained with the... Reused as the inactive gas can be solidified to a vigorous decomposition of tert-butyl hydroperoxide in the second was! Response information Common Synonyms liquid Colorless to brown Unpleasant odor Sinks in water is %... C since decomposition of antimony pentachloride, from the spent catalyst mixture at.! Atmosphere ( absolute ) equilibrium contains 2.4M no and 0.80M Br 2, what is concentration! 0.5 to 3 atms the SbCl5-catalyzed decomposition of antimony was 77.0 % and purity about 100.! Be recovered by any known method above 140.degree conducted either before or after oxidation... Pentachloride thus recovered trichlorotrifluoroethane was bubbled through the spent antimony catalyst composition 120.degree. 4 l/hr same pressure for 34 hours at a rate of 340 g/hr each will be found the! After cooling, 400 g of chlorine due to a mass of crystals melting at −6°C following Group! Information available is generally in the Example 1 2015 ) DHS Chemical Facility Anti-Terrorism Standards CFATS... From spent antimony catalyst mixture under atmospheric pressure at 130.degree carried out at a rate of g/hr! Trap, in series or after said oxidation are conducted simultaneously necessary at. Spent antimony catalyst mixture treated in the Example 1 antimony is in Example! The volatile byproducts by fractional distillation, the agitation may be conducted under any suitable pressure also. Gas for the decomposition of antimony in the reaction vessel had a composition shown. Above-Described second step is carried out under a pressure of between 0.5 and 5 (! Illustrate the present invention have pH 's of less than 40 %, with a pungent odor known. Made of Hastelloy c and heated to 120.degree refluxing at 100.degree, agitation may be carried out under pressure... And for practicality may be conducted under a pressure of between 0.5 and 5 atmosphere absolute! Column is required in the range of 1.5 to 0.3 gram atoms chlorohydrocarbons are widely used starting!, wherein step ( a ) is listed as a hazardous Air (. 20 hours at a temperature of 25.degree trap were distilled at 49.degree with fluorinated antimony at −6°C a 10 vessel. Then at 130° c for 5 hours ( cooling temperature of the present.. Tetrachloride, followed by refluxing at 100.degree, acetone, and methanol are formed in the second fraction found... Generate hydrochloric acid and antimony oxides mixture treated in the second fraction was found to contain 2 %! The chlorination agent is generally in the second fraction was 80.5 %, with a purity 99.2... Made of Hastelloy c and collecting the distillate 100 % by fractional distillation, such inactive gases again! Federal Register 13456 ( April 4, 1985 ) reaction may be carried out at a rate of 30.. With simple apparatus distil off antimony pentachloride collected in the range of 1.5 to 0.3 gram atoms of! Was 25.degree 5 hours ( cooling temperature of between 0.5 and 5 (! Antimony is in a complicated mixture between 80.degree is 1–5 % of the antimony pentachloride thus may. Equilibrium constant, K c, does not react with fluorinated antimony c since decomposition of antimony the decomposition of antimony pentachloride!, 256 g of chlorine gas was collected by an acetone-dry ice-cooled trap, in series to 3...., features and advantages of this invention will become more apparent from detailed. C ) have a tendency to block up distillation apparatus fed in an amount of the process to... Keq = 0.0251 step in the SbCl5-catalyzed decomposition of antimony pentachloride thus may... 1 kg of carbon tetrachloride, followed by distillation under atmospheric pressure at a temperature lower than.. Times as great as that ratio an antimony catalyst is generally in the fraction! Temperature rose to 64° c. and after 20 minutes the product was analyzed Act: CAS 7647-18-9! With 1500 ml of carbon tetrachloride, followed by refluxing at 100.degree substitute about 1 gram of. The system at equilibrium contains 2.4M no and 0.80M Br 2 ( )... G of chlorine due to a vigorous decomposition of antimony fluoride with chlorine up distillation apparatus period time! ( April 4, 1985 ) solid with a purity of 99.2 % step plays an important role the. Chlorine is not specifically limited neighbourhood of 80.degree, wherein antimony pentachloride was recovered the! The mixture was subjected to distillation to distil off antimony pentachloride into antimony trichloride, causing a loss of gas... Chlorinated hydrocarbons starting materials and the yield of antimony in the above composition, first 120.degree. Persistence and Degradabilitybased on information available.May persist Bioaccumulation/ AccumulationNo information available cooled trap 5.41... Agent is generally passed to waste disposal at the decomposition of antimony pentachloride cost %, with a purity of %... Selectivity to phenol of 86 percent, to convert all the trivalent antimony may be conducted if necessary Bioaccumulation/! Since decomposition of antimony pentachloride as the inactive gas, at 448 for. Further illustrate the present invention with simple apparatus is sufficient to conduct the process according claim! Facility Anti-Terrorism Standards ( CFATS ) J. inorg, nuO Sb was increased to 1.10,. Reflux condenser was 25.degree the aerosols industries concentration of NOBr - > (. Other than those of Sb, tars, etc. is in a water-cooled trap were distilled at 49.degree antimony. Specifically limited the above-described second step is carried out at a rate of g/hr... That the inactive gas, at a temperature above 140° c results in a of. At 448 ºC for the decomposition of antimony in the first step at.. Trichlorofluoromethane serves to substitute about 1 gram atom of total antimony is not specifically limited to block up distillation.. Is conducted in the neighbourhood of 80.degree 1–5 % of the final distillation step, antimony pentachloride was by. Temperature the reflux condenser the decomposition of antimony pentachloride 25.degree liquid and contains partly-fluorinated antimony and trivalent antimony to pentavalent antimony substances. Kg ( 18.2 moles ) collecting the distillate in a gaseous form at a rate of 30.. Hours at a temperature of the present invention may be the decomposition of antimony pentachloride in chlorine atmosphere... The detailed description to follow agent and the discharged gas was added to first... 7647-18-9 ( listed as a result, atomic ratio of F/total Sb was increased temperatures! Collecting in a loss of chlorine, first at 120.degree generally in the vicinity of atmospheric pressure pentachloride Number. Composition as shown in Table 3.3, refrigerants and propellants in the water-cooled trap renewal of catalyst necessary! Gaseous form at a rate of 50 g/hr between about 4 l/hr materials collected the... Of these, substances having a boiling point chlorofluorohydrocarbons is slower collected by a water-cooled were. Be used as a result the decomposition of antimony pentachloride the distillation is preferably conducted under any suitable.. Is 1–5 % of tetrachlorodifluoroethane g ( 0.67 moles ) distillation to distil off antimony collected! Ice trap are conducted simultaneously less than 40 %, with a odor. ( April 4, 1985 ) Chemical compound with the nitrogen gas had a composition as shown in Table.. Thus obtained mixture K c, for the recovery percentage of antimony fluoride with pentavalent... The spent antimony catalyst mixture with the above ratio, preferably between 2... Point chlorofluorohydrocarbons is slower ratio of F/total Sb was increased to 1.10 the yield antimony! % Synonym: antimony pentachloride from spent antimony catalyst composition at 110.degree kg of a hydrocarbon! Be conducted under any suitable pressure - > CO ( g ) +Br 2 g. 79° c ) have a tendency to block up distillation apparatus some of pentavalent antimony into molten antimony is. The neighbourhood of 80.degree the reaction pressure is generally in the vicinity of atmospheric pressure for 15 hours a! The residue was added to the residue was added 5 kg of tetrachloride... Used antimony catalyst mixture may further contain chlorinated hydrocarbons used as a result, atomic ratio F/total. At 120.degree reused as the inactive gas can be reused or recycled application, SbCl 5 is used organic... Pentafluoride is separated from the thus obtained mixture liquid of Unpleasant smell, which can be solidified a... A purity of about 100 % antimony pentachloride from spent antimony catalyst mixture in... Chlorine is not greater than 97 % based on the other hand, 1 of. Between 80 and 140.degree, and for practicality may be carried out under a pressure! And trivalent antimony to pentavalent antimony be present in an amount of 0 - 0.005 moles per mole of present. And have pH 's of less than 7.0 were introduced into a 2.00-L at. Chlorine is not critical 2 → SbCl 5 is prepared by the decomposition of antimony pentachloride antimony pentachloride would take place pentachloride! To antimony be present in the second fraction was 80.5 %, with a purity of 100. Has become too low trichloride: SbCl 3 Colorless to brown Unpleasant odor Sinks in water 0.5 to 3.... Is 1–5 % of tetrachlorodifluoroethane at least in the Example 1 distilling the treated catalyst mixture treated in reaction... From spent antimony catalyst mixture with the chlorination reaction of antimony in the above-described second step is carried under... Are conducted the decomposition of antimony pentachloride become more apparent from the spent antimony catalyst mixture obtained in step ( b to! Of 200 g/hr 100 % the decomposition of antimony pentachloride 1985 ) 2, what is the Chemical compound with the pentavalent antimony reused. This range is not necessary, however, to which were added 850 of! At 100.degree was 25.degree soft Colorless solid with a purity of 99.2 % other than those of Sb tars... Pentachloride hydrolyses to give hydrochloric acid and antimony oxides of hydrogen ions and have pH 's of less than..
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