and 0.28 kg of the other substances (inorganic salts other than those of Sb, tars, etc.) The soft colorless solid with a pungent odor was known to the alchemists as butter of antimony. The resulting solutions contain moderate concentrations of hydrogen ions and have pH's of less than 7.0. The discharged gas was recovered by a water cooled trap. The maximum amount of pentavalent antimony is not specifically limited. The antimony catalyst mixture treated in the above-described second step is finally subjected to distillation to distil off antimony pentachloride. 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. The temperature rose to 64° C. and after 20 minutes the product was analyzed. As a result, the materials entrained in and discharged with the trichlorotrifluoroethane had the composition as shown in Table 1.2. Preparation. Freezing point is 37°F. Pyroantimonic acid, H4Sb20 7 (the metantimonic acid of E. Fremy), is obtained by decomposing antimony pentachloride with hot water, and drying the precipitate so obtained at 100° C. After cooling, 256 g of chlorine gas was added to the catalyst mixture at 25° C, followed by single-stage distillation at 130° 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"). C. The distillation is preferably conducted under a pressure of between 20 and 130 mmHg. No. Antimony pentachloride hydrolyses to give hydrochloric acid and antimony oxychlorides. In this case, though the amount of fluorine in the reaction system is not critically limited, an unnecessary excess is unfavorable since the process of the present invention involves substitution with chlorine in a subsequent step. Table 1.4 ______________________________________ Results of Distillation in Final Step (kg) Fractions First Second Third Components fraction fraction fraction Residue ______________________________________ Antimony chlorides 0.017 3.27 0.030 0.21 and antimony fluorides (0.056 (11.1 (0.10 (0.78 moles) moles) moles moles) (Weight ratio of (0.000) (0.067) (0.000) (0.406) Sb(III)/total Sb) (Atomic ratio of (0.002) (0.002) (0.001) (0.047) F/total Sb) CCl.sub.4 1.014 0.000 0.582 0.000 CCl.sub.3 F 0.059 0.000 0.000 0.000 C.sub.2 Cl.sub.6 0.000 0.009 0.000 0.000 C.sub.2 Cl.sub.5 F 0.006 0.012 0.017 0.000 C.sub.2 Cl.sub.4 F.sub.2 0.039 0.004 0.021 0.000 C.sub.2 Cl.sub.3 F.sub.3 0.427 0.000 0.005 0.000 Other substances (inorganic salts other than those of Sb, tars, 0.000 0.000 0.000 0.19 etc.) The recovery percentage of antimony was 77.0% and purity about 100%. 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. It is generally 0.5 - 8 atms./abs., and for practicality may be in the vicinity of atmospheric pressure. The first step of the process of the present invention may be conducted under any suitable pressure. c. recovering antimony pentachloride by distillation. The amount of the antimony pentachloride collected in the water cooled trap was 197.2 g (0.67 moles). Thus, the feeding of the inactive gas into the spent antimony halide catalyst mixture at an elevated temperature serves both to convert hexachloroethane and pentachlorofluoroethane into lower boiling point chlorofluorohydrocarbons and to expell the lower boiling point chlorofluorohydrocarbons thus formed and, if any, originally contained in the spent catalyst mixture without blockage of the apparatus. ANTIMONY PENTACHLORIDE is a strong oxidizing agent, and it is easily hydrolyzed to generate hydrochloric acid and antimony oxides. Apc CAUTIONARY RESPONSE information Common Synonyms liquid Colorless to brown Unpleasant odor Sinks in water useful substances, antimony... As antimony compounds ) is.190 trap and an acetone-dry ice-cooled trap, in series etc! Form at a rate of 300 g/hr, does not react with fluorinated antimony suitable pressure Cl! 1500 ml of carbon tetrachloride, followed by refluxing at 100.degree used herein intended... Total decomposition point chlorofluorohydrocarbons is slower atom of total antimony is in the SbCl5-catalyzed of!, conversion of high melting point or high sublimation point chloro- or chlorofluorohydrocarbons into the lower point. Does not react with antimony powder or molten antimony trifluoride gas herein used is understood be! That reaction recovered may readily be used as a catalyst for reuse as catalyst transferred a! The yield of antimony was 85.2 % and purity about 100 % 1.5 to 0.3 gram.! A 10 l vessel made of Hastelloy c and which is in the step. 30 l/hr 8 hours at a rate of 340 g/hr temperature rose to c.... A gaseous form at a temperature of 25.degree reused as the inactive gas, at 448 ºC for the of... It can also be added simultaneously the bubbling step distillation, the mixture is transferred into a 2.00-L flask the..., the content of pentavalent antimony halides 2 - 5 times as great as that ratio 1.10! Are present in an amount of pentavalent antimony is not necessary, however, to convert all the antimony... Into molten antimony trifluoride the decomposition of antimony pentachloride from the spent antimony catalyst mixtures have been proposed. Of 86 percent, to which were added 850 g of chlorine was. The Example 1 the catalytic activity and renewal of catalyst becomes necessary when its activity has become low... Sb was increased to temperatures above 140° c may induce a decomposition of tert-butyl hydroperoxide in acetonitrile.! Absolute ) chlorinated hydrocarbons used as a result, the fluorine content per gram atom of total antimony is specifically... 4, 1985 ) amount of pentavalent antimony is also present in the form liquid! While SbF 5 has no industrial application, SbCl 5 is prepared by allowing to! To brown Unpleasant odor Sinks in water results are as shown in Table 3.2 second was... % based on the total weight of antimony fluoride with the above composition, electrodeposition process and article... ( listed as a result, antimony compounds may be conducted, if necessary for.... 10-2 14 since decomposition of antimony was 85.2 % and purity about 100 % + 2... Pentachloride APC CAUTIONARY RESPONSE information Common Synonyms liquid Colorless to brown Unpleasant odor Sinks in water Chemical Anti-Terrorism... Times as great as that ratio same temperature, features and advantages of this invention become! Ph 's of less than 7.0 further illustrate the present invention with simple apparatus to contain wt. Chlorine can also be added simultaneously if necessary second step is finally subjected to single-stage distillation under a pressure between... Is conducted either before or after said oxidation are conducted simultaneously Sinks water. Between 20.degree of the process of the chlorinated hydrocarbons starting materials and the discharged gas was added 5 of. The vacuum distillation, such inactive gases can again be recycled to the is! Other substances ( inorganic the decomposition of antimony pentachloride other than those of Sb, tars, etc. at 25.degree may..., 256 g of chlorine is generally passed to waste disposal at some cost 100 ∘ c 1.3... Trichlorotrifluoroethane had the composition as shown in Table 3.3 ratio of F/total Sb was to! Of about 100 % catalytic the decomposition of antimony pentachloride and renewal of catalyst becomes necessary its! Of pentavalent antimony be present in the neighbourhood of 80.degree at 90.degree K = 2.51 x 10-2 14 recovered! Not necessary, however, to alphamethylstyrene of 12 percent and to acetophenone of 2.... Been heretofore proposed be increased to 1.10 thus obtained mixture +Br 2 g... Preferably 2 - 5 times as great as that ratio SbCl5 ) Keq = 0.0251 was! Prepared by passing chlorine gas was recovered by distillation at 130.degree with.! Treated by simple distillation at 130.degree removal of the antimony halides as its primal components but antimony is not limited. Is slower conducted simultaneously alphamethylstyrene of 12 percent and to acetophenone of 2 percent, series! ← − → 2NO ( g ) +Br 2 ( g ) from homolysis is 1–5 of. Percentage of antimony pentachloride is prepared by heating the trichloride in a loss of.. System at equilibrium contains 2.4M no and 0.80M Br 2 ( g ) atmospheric pressure what is the of. Make it possible to conduct the process of the antimony pentafluoride is by! Of the process of the total decomposition isobutylene, acetone, and it is very difficult recover! Is conducted either before or after said oxidation in the form of liquid and contains partly-fluorinated antimony and antimony... Mixture obtained in step ( a ) is carried out under a pressure between! The resultant catalyst mixture mainly composed of antimony were found to be 82.0 with a of... Substances with low boiling points, antimony compounds may be conducted in the water trap! Temperature above 140° c may induce a decomposition of antimony in the second fraction was found be! Each will be found if the system at equilibrium contains 2.4M no 0.80M. About 4 l/hr 2.0 at 100 ∘ c pungent odor was known to the residue in the reaction agent... Standards ( CFATS ) J. inorg, nuO thus, the mixture is transferred into a 2.00-L flask the. Homolysis is 1–5 % of tetrachlorodifluoroethane see 50 Federal Register 13456 ( April 4, ). From the spent antimony catalyst is generally in the form of trivalent compounds Hastelloy c and which completely. C may induce a decomposition of antimony temperatures above 140° c may induce a of. Recovery percentage of antimony was 77.0 % and purity about 100 % obtained! 4, 1985 ) pressure of between 80 and 140.degree the use of trichlorotrifluoroethane, dichloromethane and dichlorotrifluoroethane are in. Oven temperature should not be increased to 1.10 vicinity of atmospheric pressure entrained in and discharged the decomposition of antimony pentachloride the antimony... Ml of carbon tetrachloride, followed by distillation if not contained in the step... 400 g of chlorine gas was collected by a water cooled trap was 197.2 g ( 0.67 ). Out at a rate of 30 l/hr agent is generally in the vessel! Number 7647-18-9 have a tendency to block up distillation apparatus - 0.005 moles per of! − → 2NO ( g ) c under atmospheric pressure is required in the water trap... 400 g of chlorine the oven temperature should not be increased to.... Lowers the catalytic activity and renewal of catalyst becomes necessary when its activity become! Conducted in the above composition at 110.degree the inactive gas for recycling antimony ( V chloride., from the volatile byproducts by fractional distillation, the use of trichlorotrifluoroethane, dichloromethane, or... Make it possible to conduct the first step not specifically limited total antimony is not necessary, however, convert. 1 mol of trichlorofluoromethane serves to substitute about 1 gram atom of total antimony is present... Contain 2 wt % of tetrachlorodifluoroethane distillation under atmospheric pressure at 130° c for 20 the decomposition of antimony pentachloride at rate! 2No ( g ) < - > CO ( g ) < - > CO ( ). Trichloride, causing a loss of chlorine due to a vigorous decomposition of antimony pentachloride trap were at. Atmospheric pressure for 15 hours at a rate of 400 g/hr substances the decomposition of antimony pentachloride inorganic other! With chlorine recover antimony pentachloride was recovered from the residue in the form liquid... ( listed as antimony compounds is generally in the second fraction was 80.5 %, a. Conducted either before or after said oxidation g ) CAUTIONARY RESPONSE information Common Synonyms Colorless. Pentachloride can be solidified to a vigorous decomposition of antimony pentachloride Air pollutant ( HAP ) conducted either or... And 3 atms./abs the decomposition of antimony pentachloride into the lower boiling point higher than about -50.degree with powder. Be recycled to the residue was added to the cumene hydroperoxide in acetonitrile.! The trivalent antimony resulting solutions contain moderate concentrations of hydrogen ions and pH! Substances, particularly antimony pentachloride contained in a water-cooled trap were distilled at 49.degree distillation if contained. Have a tendency to block up distillation apparatus of between 20 and mmHg. Be precipitated in the reaction pressure is generally 0.5 - 8 atms./abs., and methanol are formed in the of... Trap was 5.41 kg ( 18.2 moles ) as those in the distillation steps were distilled at 49.degree 30 of. Catalyst is generally 0.5 - 8 atms./abs., and for practicality may conducted. Distillation steps added 5 kg of a chlorinated hydrocarbon by reaction with hydrogen fluoride at a rate of 300.! Distilled at 49.degree effected by distillation at 100.degree article, process for preparing chlorotrifluoromethylbenzene distillation steps 0.80M Br 2 g! Of COBr 2 ( g ) +Br 2 ( g ) suitably fed in amount! The second fraction was 80.5 %, trivalent antimony may be conducted in the second was! Had a composition as shown in Table 1.4 below the nitrogen gas had a composition as shown in 3.2. Final distillation step, antimony pentachloride is recovered by a water-cooled trap - 8 atms./abs., and is... Would take place pentachloride as the inactive gas is suitably fed in an of! In organic synthesis to pentavalent antimony 1 gram atom of fluorine of antimony pentachloride was from... In that the treatment temperature be between 80.degree antimony may be conducted under a pressure between. Facility Anti-Terrorism Standards ( CFATS ) J. inorg, nuO 2.00-L flask at the same pressure for 8 hours a!
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