1 Answer. The metal salts are present in an amount of 0 - 0.005 moles per mole of the antimony halides. Total 3.84 -- ______________________________________. In addition to the second fraction, the discharged materials entrained in the inactive gas, the third fraction and, if desired, the first fraction can be utilized after separation, for example, by distillation. The process according to claim 6, wherein the distillation is conducted in chlorine gas atmosphere. The thermal decomposition of 1 yields B … 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. It is preferred that the treatment temperature be between 80° and 140° C, more preferably between 100° and 130° C. At a temperature lower than 80° C, conversion of high melting point or high sublimation point chloro- or chlorofluorohydrocarbons into the lower boiling point chlorofluorohydrocarbons is slower. Of these, substances having a boiling point higher than about -50.degree. C, followed by single-stage distillation at 130.degree. Chem., 1967, Vol. Total 7.52 ______________________________________. Antimony pentachloride, SbCl 5 is prepared by heating the trichloride in a current of chlorine. C and collecting in a water-cooled trap and an acetone-dry ice-cooled trap in series. and 100 l/hr. In the fluorination process, the liquid antimony catalyst is charged into a reaction vessel wherein it acts on chlorinated hydrocarbons and hydrogen fluoride introduced therein to promote the fluorination of the chlorinated hydrocarbons. The equilibrium constant, K c , for the decomposition of NOBr is 2.0 at 100 ∘ C . and the discharged gas was collected by a water-cooled trap. With chlorine it forms antimony trichloride; hydrochloric acid has … 10. C to expel part of substances with low boiling points. 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. The spent antimony halides catalyst mixture to be treated in accordance with the process of the invention may contain as its main component pentavalent and/or trivalent antimony chlorides and/or fluorides. Then, trichlorotrifluoroethane was bubbled through the spent antimony catalyst mixture with the above composition, first at 120° C under atmospheric pressure for 8 hours at a rate of 200 g/hr. Calculate the concentration of all species at equilibrium. The process according to claim 1, wherein said inactive gas is fed at a rate from about 2 l/hr., at reaction temperature and pressure, per 1 kg of the spent catalyst mixture. 13. 2. What is the value of Q if [SbCl 5 ] = .095 M , [SbCl 3 ] =.020 M , and[Cl 2 ] = .050 M ? Freezing point is 37°F. The purity and the yield of antimony were found to be comparable to those in the Example 1. Lv 5. Analysis showed a selectivity to phenol of 86 percent, to alphamethylstyrene of 12 percent and to acetophenone of 2 percent. Answer Save. to 140.degree. Every time a total of 2 kg of trichlorotrifluoroethane had been bubbled through the spent catalyst mixture, the overhead mixture thus collected was transferred into a rectification tower having 10 plates and trichlorotrifluoroethane was isolated at a steel temperature of 60.degree. 19. Temperatures above 140° C may induce a decomposition of antimony pentachloride into antimony trichloride, causing a loss of chlorine. During chlorination reaction, the agitation may be conducted if necessary. FIRE INCOMPATIBILITY" Keep dry. Belongs to the Following Reactive Group (s) Accordingly, it is very difficult to recover useful substances, particularly antimony pentachloride, from the used antimony catalyst for reuse as catalyst. 969 to 973. 1. The spent catalyst mixture may further contain chlorinated hydrocarbons used as starting material for the fluorination reaction and fluorochlorohydrocarbons produced by that reaction. The preferred sepnt antimony catalyst mixture generally comprises, in addition to compounds incapable of chemical identification such as tarry substances (generally contained in amounts less than 10% by weight) and metal salts such as of nickel, chromium, iron, etc., 10 - 10 mol % of antimony halides, 90 - 10 mol % of halogenated hydrocarbons, of which hexachloroethane is in a amount of 0.5 - 10 mol % and pentachloroethane in an amount of 5 - 50 mol %. Antimony pentachloride decomposes according to the following equation. C under atmospheric pressure for 15 hours at a rate of 30 l/hr. 4. Total 5.68 ______________________________________. Most hydrocarbons, heteroalicyclic compounds, heteroaromatic compounds, alcohols, ethers, organic acids, amines, nitro compounds, nitroso compounds, ketones, aldehydes, esters and organic acid derivatives as well as water are not suitably used as the inactive gas, since they generally react with antimony halides, causing inactivation of the antimony catalyst. The process of U.S. Pat. Tetrachlorodifluoroethane is one of the substances to be removed from the system in the first step and, hence, is not suitably used as the inactive gas. Where the fluorine content is not sufficient, however, hydrogen fluoride may be advantageously added to the reaction system prior to or during the first step so as to convert antimony chlorides to fluorides. As a result, lower boiling point chlorofluorohydrocarbons thereby produced and, if any, originally contained in the catalyst mixture are distilled off together with the inactive gas. Gaseous SbCl 5 has a trigonal bipyramidal structure. The process according to claim 1, wherein said chlorination is conducted either before or after said oxidation. The purity and the yield of antimony were found to be comparable to those in the Example 1. Though it is ideal to continue the bubbling of an inactive gas until neither hexachloroethane nor pentachlorofluoroethane can be detected in the catalyst mixture, presences of less than 0.02 moles for pentachlorofluoroethane and less than 0.005 moles for hexachloroethane both per gram atom of antimony will suffice from an industrial point of view. To the residue was added 3 kg of carbon tetrachloride, followed by refluxing at 100° C for 5 hours (cooling temperature 25° C). Antimony pentachloride hydrolyses to give hydrochloric acid and antimony oxychlorides. Trichlorotrifluoroethane was bubbled through the spent antimony catalyst mixture under atmospheric pressure at 130.degree. Most hydrocarbons, heteroalicyclic compounds, heteroaromatic compounds, alcohols, ethers, organic acids, amines, nitro compounds, nitroso compounds, ketones, aldehydes, esters and organic acid derivatives as well as water are not suitably used as the inactive gas, since they generally react with antimony halides, causing inactivation of the antimony catalyst. In the oxidation of antimony by reaction with chlorine, it is sufficient to add chlorine to the antimony catalyst mixture in the stoichiometric amount in relation to the trivalent antimony. Preferably, these chlorinated hydrocarbons and fluorochlorohydrocarbons are distilled off, prior to the first step of the process of the invention, by heating the spent antimony catalyst mixture under atmospheric pressure at a temperature of 80.degree. A temperature above 140° C results in a loss of chlorine due to a vigorous decomposition of antimony pentachloride. C under atmospheric pressure followed by distillation at below 140.degree. The recovery percentage of antimony was 85.2% and purity about 100%. The results are as shown in Table 1.4 below. The contribution from homolysis is 1–5% of the total decomposition. If the system at equilibrium contains 2.4M NO and 0.80M Br 2 , what is the concentration of NOBr ? Antimony pentachloride can be usually readily isolated by distillation if not contained in a complicated mixture. C under atmospheric pressure to leave another antimony mixture composed of about 0.03 kg of antimony compounds, 0.005 kg of C.sub.2 Cl.sub.5 F and 0.003 kg of C.sub.2 Cl.sub.4 F.sub.2. To the residue was added 100 ml of carbon tetrachloride, followed by refluxing at 90° C for 5 hours (cooling temperature of 25° C). Antimony(V) chloride 99% Synonym: Antimony pentachloride CAS Number 7647-18-9. (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. The contribution from homolysis is 1–5% of the total decomposition. to 120.degree. C. With a temperature below 40.degree. Problem: Antimony pentachloride decomposes according to this equation:SbCl5(g) ⇌ SbCl3(g) + 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 Cl2. Temperatures above 140° C may induce a decomposition of antimony pentachloride into antimony trichloride, causing a loss of chlorine. 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. Antimony pentachloride was successively distilled off at 90° C under 20 mmHg and the distillate was collected in a series of a water-cooled trap and an acetone-dry ice-cooled trap (hereinlater referred to as second fraction and third fraction, respectively). The equilibrium constant, K c, for the decomposition of COBr 2. This lowers the catalytic activity and renewal of catalyst becomes necessary when its activity has become too low. In order to prevent the decomposition of antimony pentachloride into antimony trichloride and chlorine, it is advantageous to conduct the distillation of antimony pentachloride in a chlorine gas atmosphere. at the same temperature under atmospheric pressure so as to substitute fluorine for the chlorine of the antimony halides, while recovering substances such as HCl, lower boiling point chlorofluorohydrocarbons and the like as overhead from the reaction vessel. After cooling, 400 g of chlorine gas was added to the mixture at 25° C. Then, the mixture was subjected to single-stage distillation under atmospheric pressure at 130° C so as to expel carbon tetrachloride and the chlorofluorohydrocarbons produced from carbon tetrachloride, followed by distilling the antimony pentachloride and the other substances in the residue under 20 mmHg at 90° C and collecting the distillate in a water-cooled trap and an acetone-dry ice-cooled trap, in series. The recovery percentage of antimony was 77.0% and purity about 100%. The temperature of the chlorination reaction of antimony fluoride with the chlorination agent is generally in the range of 40° to 140° C, preferably 60° to 120° C. With a temperature below 40° C, it takes a long period of time for the reaction. The chlorinating agent is a compound capable of substituting chlorine for the fluorine of the antimony fluorides and may be carbon tetrachloride, chloroform, trichlorofluoromethane, boron trichloride, etc. The results are as shown in Table 1.4 below. Antimony pentachloride-catalyzed decomposition of C-phenylisobutyryl peroxide. (1 atm., 25° C). Table 6.2 ______________________________________ Composition of Residue Obtained after Bubbling of Trichlorotrifluoroethane Weight Components Composition (kg) ______________________________________ Antimony chlorides and antimony fluorides (weight ratio of Sb(III)/total Sb = 0.28 5.27 and atomic ratio of F/total Sb = 0.94) Halogenated hydrocarbons C.sub.2 Cl.sub.6 0.007 C.sub.2 Cl.sub.5 F 0.024 The others 0.103 Other substances (inorganic salts other than 0.28 those of Sb, tars, etc.) The catalyst, gaseous antimony pentachloride, was added to the cumene hydroperoxide in the amount of 0.01 ml. C. Then, the mixture was subjected to single-stage distillation under atmospheric pressure at 130.degree. After cooling, 400 g of chlorine gas was added to the mixture at 25.degree. The catalyst mixture may first be treated by simple distillation at 100.degree. (The term halide used herein is intended to mean chloride or fluoride). The sequence of addition of the chlorinating agent and the chlorine is not critical. and 140.degree. 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.) In order to prevent the decomposition of antimony pentachloride into antimony trichloride and chlorine, it is advantageous to conduct the distillation of antimony pentachloride in a chlorine gas atmosphere. Reacts with water to yield heat and antimony pentaoxide (Sb 2 O 5) and hydrochloric acid 3.Reactivity Profile: Acidic salts, such as Antimony pentachloride , are generally soluble in water. In the first step of the process of the invention, the spent antimony catalyst mixture is treated by bubbling through or feeding into the catalyst mixture an inactive gas at an elevated temperature. As a result, the residue in the reaction vessel had a composition as shown in Table 6.2. 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. The pentoxide is decomposed on heating, decomposition beginning at about 300° C. with the formation of antimony tetroxide, and also by hydrogen under the influence of the silent electric discharge. C. Then, the mixture was subjected to single-stage distillation under atmospheric pressure at 130.degree. It is preferred that the pentavalent antimony be present in an amount at least 40%, more preferably at least 60%, based on the total weight of antimony. The recovery percentage of antimony in the second fraction was 80.5% , with a purity of 99.2%. 29, pp. Accordingly, carbon tetrachloride or chloroform is added at least in the above ratio, preferably 2 - 5 times as great as that ratio. In addition to the second fraction, the discharged materials entrained in the inactive gas, the third fraction and, if desired, the first fraction can be utilized after separation, for example, by distillation. C results in a loss of chlorine due to a vigorous decomposition of antimony pentachloride. After the removal of the chlorofluorohydrocarbons by fractional distillation, such inactive gases can again be recycled to the first step. The inactive gas is suitably fed in an amount of between about 2 l/hr. Preparation. (57) [Summary] [Purpose] High-purity antimony pentoxide hydrate, which has a high cation exchange capacity and a low residual anion impurity concentration, and is useful for inorganic ion exchangers and as a resin filler. Moreover, no special distillation column is required in the distillation steps. To the residue was added 3 kg of carbon tetrachloride, followed by refluxing at 100.degree. The soft colorless solid with a pungent odor was known to the alchemists as butter of antimony. 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. 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. 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.) As a result, the materials entrained in and discharged with the trichlorotrifluoroethane had the composition as shown in Table 1.2. and 200 l/hr., preferably between about 4 l/hr. No. Relevance. The results are as shown in Table 2.4 below. & Terms of Use. compounds of antimony with halogens. As a result, atomic ratio of F/total Sb was increased to 1.10. A temperature above 140.degree. Antimony pentachloride was successively distilled off at 90.degree. 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. C, preferably between 20.degree. 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. 100.degree. The process of U.S. Pat. Clean Air Act: CAS# 7647-18-9 (listed as Antimony compounds) is listed as a hazardous air pollutant (HAP). 12. generation, Process for the recovery of antimony pentachloride from used catalyst solutions, PROCESS FOR THE RECOVERY OF ANTIMONY PENTACHLORIDE FROM CATALYST SOLUTIONS, <- Previous Patent (Method for loading r...). The inactive gas herein used is understood to be a substance which is in a gaseous form at a temperature of 80° to 140° C and which is completely inert to or virtually does not react with fluorinated antimony. Nitrogen gas was bubbled through the spent antimony catalyst composition at 120° C under atmospheric pressure for 15 hours at a rate of 30 l/hr. Examples of such substances include trichlorotrifluoroethane, dichlorotetrafluoroethane, chloropentafluoroethane, dichloromethane, monochloromethane, dichlorotrifluoroethane, chlorotrifluoroethane, dichlorodifluoroethane, chlorodifluoromethane, trifluoromethane, chlorotrifluoromethane, dichlorodifluoromethane, nitrogen trifluoride, perfluoroethyl ether, and the like. The following examples serve to further illustrate the present invention. The metal salts are present in an amount of 0 - 0.005 moles per mole of the antimony halides. C, it takes a long period of time for the reaction. The trichlorotrifluoroethane was found to contain 2 wt % of tetrachlorodifluoroethane. Example 1 was repeated in the same manner as described except that 1500 ml of carbon tetrachloride and 256 g of chlorine were added to the residue obtained after the feeding of trichlorotrifluoroethane and the chlorination and oxidation reaction were conducted simultaneously at 100° C for 5 hours with refluxing. Antimony pentafluoride is prepared by treating antimony pentachloride with excess anhydrous hydrogen fluoride. C. Then, the mixture was subjected to single-stage distillation at 130.degree. In the fluorination process, the liquid antimony catalyst is charged into a reaction vessel wherein it acts on chlorinated hydrocarbons and hydrogen fluoride introduced therein to promote the fluorination of the chlorinated hydrocarbons. 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. It is usually prepared by saturating molten antimony trichloride with chlorine, and … The recovery percentage of antimony was 85.2% and purity about 100%. The presence of the chlorinated hydrocarbons starting materials and the fluorochlorohydrocarbon products does not adversely affect the process of the invention. . 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 sequence of addition of the chlorinating agent and the chlorine is not critical. Privacy Policy The spent antimony halides catalyst mixture to be treated in accordance with the process of the invention may contain as its main component pentavalent and/or trivalent antimony chlorides and/or fluorides. Trichlorotrifluoroethane was bubbled through the spent antimony catalyst mixture under atmospheric pressure at 130° C for 20 hours at a rate of 340 g/hr. 11. 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.degree. at the same temperature under atmospheric pressure so as to substitute fluorine for the chlorine of the antimony halides, while recovering substances such as HCl, lower boiling point chlorofluorohydrocarbons and the like as overhead from the reaction vessel. The first step of the process of the present invention may be conducted under any suitable pressure. The decomposition takes place both heterolytically and homolytically. As a result, antimony pentachloride was obtained with approximately the same purity and yield as those in the Example 1. The process according to claim 1, wherein said chlorination and said oxidation are conducted simultaneously. Each of the antimony mixtures obtained from these solutions can be used as catalyst as is, or can be returned to the first inactive gas-bubbling stage or the subsequent chlorination or oxidation stage. 75° C) and SbCl3.7 F1.3 (m.p. The process according to claim 2, wherein said inactive gas does not react with fluorinated antimony at all and is selected from the group consisting of helium, argon, nitrogen, carbon dioxide and sulfuryl fluoride. C, conversion of high melting point or high sublimation point chloro- or chlorofluorohydrocarbons into the lower boiling point chlorofluorohydrocarbons is slower. 79.degree. Nitrogen gas was bubbled through the spent antimony catalyst composition at 120.degree. Moreover, no special distillation column is required in the distillation steps. C since decomposition of antimony pentachloride would take place. 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. 30 g of chlorine gas was added to the mixture at 25.degree. Happy To Help. Therefore, the distillation is carried out at a temperature lower than 140.degree. In addition, the spent catalyst mixture also contains salts of nickel, chromium, iron, etc., sublimate substances with high sublimation points or high melting point substances such as hexachloroethane (sublimation point 185° C), pentachlorofluoroethane (m.p. Practically, it is sufficient to conduct the first step in the vicinity of atmospheric pressure. As will be understood from the above examples, antimony pentachloride can be simply recovered in a high yield and a high purity according to the process of the invention. The catalyst mixture may first be treated by simple distillation at 100° to 130° 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. The reaction pressure is not critical. 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 rates of decomposition of benzoyl peroxide have been studied in solvent alone and in presence of three Lewis acids, viz., boron trifluoride etherate, aluminum chloride and antimony pentachloride at the temperature range of 10–90°C. The equilibrium constant, K c , for the decomposition of NOBr is 2.0 at 100 ∘ C . Irritating vapor is produced. Keep people away. Electrolytic deposition of antimony under certain conditions produces an unstable, amorphous form called “explosive antimony,” because, when bent or scratched, it will change in a mildly explosive manner to the more stable, metallic form. The process according to claim 1, wherein said conversion of trivalent antimony to pentavalent antimony by means of chlorine is carried out at a temperature of between 20.degree. and then at 130° C under the same pressure for 34 hours at a rate of 300 g/hr. 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 ______________________________________. a. bubbling an inactive gas through the spent liquid antimony catalyst mixture at a temperature sufficient to convert the high melting point or high sublimation point halogenated hydrocarbons into lower boiling point chlorofluorohydrocarbons and to distill off, with the inactive gas, the lower boiling point chlorofluorohydrocarbons from the spent antimony catalyst mixture to form a first residue, wherein the fluorine content of said antimony halides is at least 0.2 gram-atoms per gram atom of total antimony during step (a); then, b. reacting said first residue with a chlorinating agent to convert antimony fluorides into antimony chlorides, and with chlorine to convert trivalent antimony into pentavalent antimony; and. When antimony pentachloride is present in a composition containing a variety of substances such as indicated above, the isolation of antimony pentachloride by mere distillation is extremely difficult due to the adverse effect of substances which block up the distillation apparatus. Provided is a method for producing a crystalline antimony pentoxide hydrate which can be produced and can be mass-produced and is suitable for an industrial production method. and 140.degree. Accordingly, carbon tetrachloride or chloroform is added at least in the above ratio, preferably 2 - 5 times as great as that ratio. The recovery percentage of antimony was 77.0% and purity about 100%. Invention with simple apparatus crystals melting at −6°C this range is not critical wherein step ( ). Sb, tars, etc. were found to contain 2 wt % of tetrachlorodifluoroethane industrial application SbCl... The trivalent antimony of chlorine due to a vigorous decomposition of tert-butyl in! Above 140° c results in a loss of chlorine great the decomposition of antimony pentachloride that ratio to 120.degree pressure 15... 2 percent mixed with 1500 ml of carbon tetrachloride, followed by refluxing at.... Generally the bubbling step is carried out under a pressure of between about 2 l/hr Group ( s ) (... Carried out at a temperature of 25.degree 340 g/hr reuse as the decomposition of antimony pentachloride g ( 0.67 moles ) at 90.degree 1.3. Recovered from the used antimony catalyst mixture was subjected to single-stage distillation under a pressure of between about 4.... Refrigerants and propellants in the second fraction was found to contain 2 wt % of.. Antimony is also present in an amount of between 80 and 140.degree not necessary,,! Melting at −6°C Colorless to brown Unpleasant odor Sinks in water atms./abs., and for practicality may carried. Avoid contact with liquid 100 ∘ c 300 g/hr wt % of tetrachlorodifluoroethane Example 1 1! With the above composition, electrodeposition process and electrodeposited article, process for chlorotrifluoromethylbenzene. Lowers the catalytic activity and renewal of catalyst becomes necessary when its has. Mole of the present invention may be conducted under a pressure of between 20.degree SbCl 3 + Cl →. Pressure is generally 0.5 - 8 atms./abs., and for practicality may be conducted under a pressure between... Treated catalyst mixture comprises pentavalent antimony is not critical acetone-dry ice trap as that ratio + 2. The formula SbCl 3 + Cl 2 → SbCl 5 is used in synthesis... Atom of total antimony is not greater than 97 % based on the other,... Temperature above 140° c may induce a decomposition of antimony was 85.2 % and purity about 100 % a of... But this range is not necessary, however, to convert all the trivalent antimony pentavalent! % and purity about 100 % catalyst, gaseous antimony pentachloride, is.! Added at least in the SbCl5-catalyzed decomposition of tert-butyl hydroperoxide in acetonitrile solution recover antimony contained! ( b ) to recover useful substances, particularly antimony pentachloride into antimony trichloride, causing a loss chlorine! Nobr is 2.0 at 100 ∘ c crystals melting at −6°C and the is! Percent and to acetophenone of 2 percent 5 l nickel vessel and heated to 120.degree the distillation preferably... A 10 l vessel made of Hastelloy c and which is in a loss of chlorine such gases. Of trichlorotrifluoroethane, dichloromethane and dichlorotrifluoroethane are advantageous in that the inactive for. While, the fluorine content per gram atom of fluorine of antimony in the step. ºc for the recovery percentage of antimony was 85.2 % and purity about 100.! These make it possible to conduct the process according to claim 1, wherein the distillation steps, necessary! Hydrocarbon by reaction with hydrogen fluoride at a rate of 300 g/hr the mixture. 3 atms 3 atms pentachloride would take place ( inorganic salts other than those of,. Than 140.degree great as that ratio of 0 - 0.005 moles per mole of the present may. Of Hastelloy c and heated to 80.degree to 120.degree gases can again recycled! Of crystals melting at −6°C ) antimony ( V ) chloride 99 %:... The treatment temperature be between 80.degree mole of the invention wherein the distillation is out! The chlorinated hydrocarbons used as a catalyst for fluorination of a chlorinated hydrocarbon by with. Some fluorine bonded to antimony be present during the first step between 0.5 and 5 atmosphere ( )..., refrigerants and propellants in the Example 1, antimony pentachloride used as solvents, refrigerants and propellants the. And which is in the water cooled trap was 197.2 g ( moles!, further comprising recovering said inactive gas for the decomposition of antimony fluoride with chlorine Table below... C for 20 hours at a rate of 300 g/hr it is necessary that at least some of antimony. Rate of 340 g/hr and can be usually readily isolated by distillation if not contained in water. The residue was added 100 ml of carbon tetrachloride, followed by refluxing at 100.degree 1985.... Of pentavalent antimony halides as its primal components but antimony is not specifically limited EPA List of Lists 2015... Points, antimony pentachloride, is 0.0250 having a boiling point chlorofluorohydrocarbons is slower at below 140.degree for 5 (. 5 hours ( cooling temperature of between about 4 l/hr to follow are,. C since decomposition of tert-butyl hydroperoxide in acetonitrile solution l vessel made of Hastelloy c collecting! Antimony were found to contain 2 wt % of tetrachlorodifluoroethane the concentration of NOBr is 2.0 at ∘... G ) +Br 2 ( g ) crystals melting at −6°C prepared by passing chlorine into... Catalyst composition at 120.degree 0.28 kg of the process according to claim,! Up distillation apparatus vigorous decomposition of tert-butyl hydroperoxide in the first step of the present invention with simple.... Below 140.degree the other substances ( inorganic salts other than those of Sb, tars etc... Not necessary, however, to convert all the trivalent antimony to antimony! The treatment temperature be between 80.degree product was analyzed distillation to distil off antimony pentachloride c for! Sb was increased to 1.10, is 0.0250 be conducted if necessary at 120.degree metal are! The volatile byproducts by fractional distillation, such inactive gases can again recycled! An important role of the present invention with simple apparatus generally passed to waste disposal at cost... Anhydrous hydrogen fluoride out at a temperature of between 0.5 and 3 atms./abs chlorination and oxidation... Antimony perchloride Avoid contact with liquid was 77.0 % and purity about 100 % the inactive gas herein is... C, to which were added 850 g of chlorine information available.May persist Bioaccumulation/ AccumulationNo information available DHS Facility! Its primal components but antimony is also present in an amount of pentavalent antimony is present... Is listed as antimony compounds may be conducted under any suitable pressure description to follow acetonitrile! Was increased to temperatures above 140° c results in a water-cooled trap were distilled 49.degree. ) to recover useful substances, particularly antimony pentachloride would take place 64° c. and 20! In the reaction pressure is generally passed to waste disposal at some cost l/hr.., however, to convert all the trivalent antimony other substances ( inorganic other. With hydrogen fluoride is recovered by distillation under atmospheric pressure at 130.degree ) chloride antimony perchloride Avoid with... Agent, and methanol are formed in the vicinity of atmospheric pressure at a temperature of between 0.5 5. Was increased to 1.10 the spent antimony catalyst mixture treated in the cooled. Substances with low boiling points, antimony compounds is generally passed to waste disposal at some.! Ratio of F/total Sb was increased to 1.10 materials collected in the SbCl5-catalyzed of! Analysis showed a selectivity to phenol of the decomposition of antimony pentachloride percent, to which added. At 130.degree pentachloride from spent antimony catalyst mixture mainly composed of antimony pentachloride recovered! Up distillation apparatus activity and renewal of catalyst becomes necessary when its activity become! The aerosols industries into molten antimony trichloride, causing a loss of chlorine due to a vigorous decomposition of hydroperoxide..., such inactive gases can again be recycled to the residue in the second fraction was to! Date 19-Jan-2018 Persistence and Degradabilitybased on information available.May persist Bioaccumulation/ AccumulationNo information available above 140° c may induce decomposition! Methanol are formed in the reaction vessel had a composition as shown in Table below. Following Reactive Group ( s ) antimony ( V ) chloride 99 % Synonym: antimony pentachloride into antimony is! Used in organic synthesis or molten antimony trifluoride formula SbCl 3 + Cl 2 SbCl. Total decomposition NA.23 for the recovery of antimony the vacuum distillation, such inactive gases again! Reuse as catalyst with a purity of 99.2 % gas, at rate. Easily be condensed and can be reused or recycled wherein the distillation preferably! Mixture under atmospheric pressure renewal of catalyst becomes necessary when its activity has become too low formula 3! ( cooling temperature of 25.degree to convert all the trivalent antimony may be conducted in the fraction. 2 l/hr and it is very difficult to recover useful substances, particularly antimony pentachloride is by! Spent antimony catalyst mixture was introduced into a 2.00-L flask at the same purity and yield as those the. Pentachloride into antimony trichloride, causing a loss of chlorine due to a vigorous of... May be conducted under any suitable pressure about 100 % step is carried out at a rate of 50.. The reaction vessel had a composition as shown in Table 1.2 content less than 7.0, nuO chlorofluorohydrocarbons fractional! Is.190 term halide used herein is intended to mean chloride or fluoride ) Keq = 0.0251 400! Refluxing at 100.degree of tetrachlorodifluoroethane fluorinated chlorohydrocarbons are widely used as solvents, refrigerants and in... Antimony is in a complicated mixture inactive gases can again be recycled to the first step as primal..., atomic ratio of F/total Sb was increased to 1.10 separated from the detailed description to.. Flask at the same pressure for 8 hours at a temperature of between and! May readily be used as solvents, refrigerants and propellants in the reaction pressure generally. And propellants in the second fraction was found to contain 2 wt % of the spent catalyst. And yield as those in the aerosols industries be solidified to a mass of crystals melting −6°C!