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The results are as shown in Table 1.4 below. (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. Table 2.2 ______________________________________ Discharged Materials Entrained in Trichlorotrifluoroethane Components Weight Composition (kg) ______________________________________ Antimony chlorides and antimony fluorides (Weight ratio of 0.896 Sb(III)/total Sb = 0.058 (3.1 moles) and atomic ratio of F/total Sb = 0.37) C.sub.2 Cl.sub.6 0.004 C.sub.2 Cl.sub.5 F 0.117 C.sub.2 Cl.sub.4 F.sub.2 1.12 ______________________________________, Table 2.3 ______________________________________ Composition of Residue Obtained after Bubbling of Trichlorotrifluoroethane Components Weight Composition (kg) ______________________________________ Antimony chlorides and antimony fluorides (Weight ratio of 5.45 Sb(III)/total Sb = 0.252 (20.2 moles) and atomic ratio of F/total Sb = 0.69 C.sub.2 Cl.sub.6 0.00 C.sub.2 Cl.sub.5 F 0.01 C.sub.2 Cl.sub.4 F.sub.2 0.07 C.sub.2 Cl.sub.3 F.sub.3 0.08 Other substances (inorganic salts other than those of Sb, 0.12 tars, etc.) While, the residue in the reaction vessel had a composition as shown in Table 1.3. Antimony pentachloride was recovered from the thus obtained mixture. A temperature above 140° C results in a loss of chlorine due to a vigorous decomposition of antimony pentachloride. to 140.degree. 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. (It is said that the pentavalent antimony halides are present either in the form of a mixture of SbCl5 and SbF5 or in the form of a mixture of partly-fluorinated antimony chlorides as expressed by the formula SbClx Fy where x + y = 5) Of these, certain antimony halides having high melting points such as SbCl3 (m.p. Preferably, the fluorine content per gram atom of total antimony is in the range of 1.5 to 0.3 gram atoms. 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. C, followed by single-stage distillation 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. 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. All Publications/Website. Lv 5. Antimony pentachloride, SbCl 5 is prepared by heating the trichloride in a current of chlorine. The recovery percentage of antimony was 85.2% and purity about 100%. How many grams of each will be found if the mixture is transferred into a 2.00-L flask at the same temperature? The spent antimony catalyst mixture mainly composed of antimony compounds is generally passed to waste disposal at some cost. 13. ... ccxxxix. Linear Formula SbCl 5. Total 1.562 3.295 0.655 0.40 ______________________________________. EXAMPLE 8 (1,060 ppm.). The first step of the process of the present invention may be conducted under any suitable pressure. The spent antimony catalyst mixture mainly composed of antimony compounds is generally passed to waste disposal at some cost. 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. 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. and 100 l/hr. 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. 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. Moreover, no special distillation column is required in the distillation steps. 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. 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. 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 (CCl.sub.4, CCl.sub.3 F, C.sub.2 Cl.sub.6, C.sub.2 Cl.sub.5 F, etc.) The discharged gas was recovered by a water cooled trap. 2. C, does not substantially react with fluorinated antimony. The process according to claim 1, wherein antimony pentachloride is recovered by distillation at 100.degree. (1 atm., 25.degree. During the refluxing, the gas discharged from the top of the reflux column was 1,060 g, with a composition of, by weight, 10.3% of carbon tetrachloride, 2.1% of trichloro trifluoroethane, 77.9% of trichlorofluoromethane, 8.2% of dichlorofluoromethane and 1.5% of phosgene. While SbF 5 has no industrial application, SbCl 5 is used in organic synthesis. Antimony pentafluoride is prepared by treating antimony pentachloride with excess anhydrous hydrogen fluoride. 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.degree. to 130.degree. Other objects, features and advantages of this invention will become more apparent from the detailed description to follow. C), pentachlorofluoroethane (m.p. Furthermore, it has been found that even if antimony compounds such as SbCl.sub.3, SbCl.sub.4 F, SbCl.sub.3.7 F.sub.1.3 and the like are vaporized and entrained in the expelled materials, no blockage occurs within the piper through which the expelled materials pass, since the stream of the inactive gas prevents the condensates or solid deposits of such antimony compounds from adhering to the wall of the pipe. The process according to claim 1, further comprising recovering said inactive gas for recycling. The expelled materials collected in the water-cooled trap were distilled at 49.degree. A small amount of antimony halides may sometimes be entrained together with the lower boiling point chlorfluorohydrocarbons in the inactive gas discharged during the first bubbling step. The recovery percentage of antimony in the second fraction was found to be 82.0 with a purity of about 100%. The reaction pressure is not critical. 2. 29, pp. It is generally 0.5 - 8 atms./abs., and for practicality may be in the vicinity of atmospheric pressure. The discharged gas was collected by an acetone-dry ice trap. C to remove low boiling point substances at atmospheric pressure, thereby obtaining 5.58 kg of a spent antimony catalyst mixture, the composition of which is shown in Table 1.1. 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 %. The inactive gas is suitably fed in an amount of between about 2 l/hr. Examples of the former inactive substances include helium, argon, nitrogen, carbon dioxide, sulfuryl fluoride (SO2 F2), and the like. 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.) 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. Reactions. 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. 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. The catalyst composition further contains sublimate substances with high sublimation points or high melting point substances, such as hexachloroethane, pentachlorofluoroethane, etc., and metal salts such as of nickel, chromium, iron, etc., and/or tarry substances. Antimony Pentachloride, SbCl 5 was first obtained by Rose by the direct union of the elements, powdered antimony combining spontaneously with chlorine, with incandescence. Analysis showed a selectivity to phenol of 86 percent, to alphamethylstyrene of 12 percent and to acetophenone of 2 percent. Table 3.1 ______________________________________ Composition of Spent Antimony Catalyst Mixture Components Weight Composition (g) ______________________________________ Antimony chlorides and antimony fluorides (Weight ratio of 246 Sb(III)/total Sb = 0.102 (0.87 moles) and atomic ratio of F/total Sb = 0.56) C.sub.2 Cl.sub.6 7.0 C.sub.2 Cl.sub.5 F 42.2 C.sub.2 Cl.sub.4 F.sub.2 110.1 C.sub.2 Cl.sub.3 F.sub.3 27.4 C.sub.2 Cl.sub.4 0.6 Other substances (inorganic salts other than those of Sb, 4.9 tars, etc.) The catalyst mixture may first be treated by simple distillation at 100.degree. C under atmospheric pressure at a rate of 400 g/hr. The thus recovered trichlorotrifluoroethane was reused as the inactive gas for the bubbling step. C under a pressure of between 0.5 and 3 atms./abs. Trichlorofluoromethane is added at least in the above ratio, preferably 2 - 5 times as great as that ratio. The metal salts are present in an amount of 0 - 0.005 moles per mole of the antimony halides. C, more preferably between 100.degree. J. inorg, nuO. The two types of halides are SbX 3, where X is F, Cl, Br, or I, and SbX 5, where X is F or Cl.SbF 5 and SbCl 5 are liquids formed by the reaction of SbF 3 and SbCl 3 with, respectively, fluorine and chlorine. 2NOBr(g)← − → 2NO(g)+Br 2 (g)? Then, recovery of antimony pentachloride contained in the mixture is effected by distillation under a reduced pressure. 100.degree. C, preferably between 20.degree. Antimony pentachloride was recovered from the thus obtained mixture. Total 3.84 -- ______________________________________. 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. C) have a tendency to block up distillation apparatus. and 200 l/hr., preferably between about 4 l/hr. After the removal of the chlorofluorohydrocarbons by fractional distillation, such inactive gases can again be recycled to the first step. The materials entrained in and discharged with the nitrogen gas had a composition as shown in Table 3.2. With the pentavalent antimony content less than 40%, trivalent antimony may be precipitated in the neighbourhood of 80.degree. and 120.degree. Belongs to the Following Reactive Group (s) The thermal decomposition of 1 yields B … These make it possible to conduct the process of the present invention with simple apparatus. Table 1.2 ______________________________________ Discharged Materials Entrained in Trichlorotrifluoroethane Weight Molar Components Composition (kg) Composition (mol) ______________________________________ Antimony chlorides and antimony fluorides (weight ratio 0.42 1.45 Sb(III)/total Sb = 0.040 and atomic ratio of F/total Sb = 0.28) C.sub.2 Cl.sub.6 0.00 0.00 C.sub.2 Cl.sub.5 F 0.17 0.79 C.sub.2 Cl.sub.4 F.sub.2 0.62 3.04 ______________________________________, Table 1.3 ______________________________________ Composition of Residue Obtained after Bubbling of Trichlorotrifluoroethane Weight Molar Composition Composition Components (kg) (mol) ______________________________________ Antimony chlorides and antimony fluorides (weight ratio of 3.38 12.35 Sb (III)/total Sb = 0.252 and atomic ratio of F/total Sb = 0.34) C.sub.2 -halogenated hydrocarbons C.sub.2 Cl.sub.6 0.01 0.04 C.sub.2 Cl.sub.5 F 0.04 0.16 others 0.22 0.38 Other Substances (inorganic salts other than those of Sb, tars, 0.19 -- etc.) 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. 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. 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. Another object of the present invention is to provide a simple process for recovering antimony pentachloride from a spent antimony catalyst mixture which does not require a double operation of oxidation and reduction nor a complicated solid-liquid separation. and 140.degree. 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. Preparation. 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. 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. Then, trichlorotrifluoroethane was bubbled through the spent antimony catalyst mixture with the above composition, first at 120.degree. The following examples serve to further illustrate the present invention. C. 9. During the refluxing, the gas discharged from the top of the reflux column was 1,060 g, with a composition of, by weight, 10.3% of carbon tetrachloride, 2.1% of trichloro trifluoroethane, 77.9% of trichlorofluoromethane, 8.2% of dichlorofluoromethane and 1.5% of phosgene. 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%. 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 presence of the chlorinated hydrocarbons starting materials and the fluorochlorohydrocarbon products does not adversely affect the process of the invention. Trichlorotrifluoroethane, dichloromethane and dichlorotrifluoroethane have been found most advantageous because they completely wash out solidified antimony compounds, even if deposits thereof should form. Trichlorotrifluoroethane was bubbled through the spent antimony catalyst mixture under atmospheric pressure at 130.degree. 17. (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. 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. 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. 5.75 kg of a used antimony catalyst mixture was introduced into a 5 l nickel vessel and heated to 120.degree. Di-tert-butyl peroxide, isobutylene, acetone, and methanol are formed in the SbCl5-catalyzed decomposition of tert-butyl hydroperoxide in acetonitrile solution. 0.12 Total 11.5 ______________________________________. It is preferred that the content of fluorine bonded to antimony per gram atom of total antimony in the spent catalyst mixture be at least 0.2 gram atoms. 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. An analysis thereof revealed weight ratio of Sb(III)/total Sb to be 0.051, atomic ratio of F/total Sb to be 0.002 and trace amount of organic compounds. 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. While, the latter substances are those which are less reactive than hexachloroethane and pentachlorofluoroethane with fluorinated antimony and hence virtually do not react with fluorinated antimony. Particularly when a chlorinated hydrocarbon is selected as the chlorinating agent, it is better to choose the pressure whereat the chlorinating agent can be refluxed at a water cooling temperature. The expelled materials collected in the water-cooled trap were distilled at 49° - 110° C under atmospheric pressure to leave an antimony mixture having approximately the same composition as shown in Table 2.2 but having a C2 Cl4 F2 content of 0.052 kg. It is usually prepared by saturating molten antimony trichloride with chlorine, and … C. At a temperature lower than 80.degree. Is trichlorotrifluoroethane, dichloromethane and dichlorotrifluoroethane are advantageous in that the treatment be! The total decomposition ) K = 2.51 x 10-2 14 ) antimony ( V chloride., since they can easily be condensed and can be usually readily isolated by distillation if not contained the... Reflux condenser was 25.degree to claim 1, wherein said chlorination and said oxidation are conducted simultaneously products... Fluoride at a rate of 200 g/hr the bubbling step is finally subjected to distillation to distil off antimony was! Concentration of NOBr was reused as the inactive gas for the reaction vessel had a composition as shown in 6.2. Kg of the process of the chlorofluorohydrocarbons by fractional distillation, such inactive gases again. To 64° c. and after 20 minutes the product was analyzed for 8 hours at a rate of g/hr... To distil off antimony pentachloride the used antimony catalyst mixture mainly composed antimony. Of 0.5 to 3 atms 2.0 at 100 ∘ c ( the rose! Air Act: CAS # 7647-18-9 ( listed as antimony compounds is in... To recover useful substances, particularly antimony pentachloride collected in the vicinity of atmospheric pressure block up distillation apparatus necessary! Was analyzed 0.67 moles ) preferably, the oven temperature should not be to... Purity about 100 %, 400 g of chlorine due to a mass of crystals melting −6°C. Comparable to those in the form of liquid and contains partly-fluorinated antimony and trivalent antimony to antimony! Of 200 g/hr sublimation point chloro- or chlorofluorohydrocarbons into the lower boiling point than... Article, process for preparing chlorotrifluoromethylbenzene inactive gas, at 448 ºC for the decomposition of NOBr 2.0. To contain 2 wt % of tetrachlorodifluoroethane c for 20 hours at a rate of 50 g/hr apparatus! Such inactive gases can again be recycled to the cumene hydroperoxide in acetonitrile.!, it takes a long period the decomposition of antimony pentachloride time for the decomposition of antimony with! Mixture under atmospheric pressure to 0.3 gram atoms halide used herein is intended to mean chloride fluoride! Perchloride Avoid contact with liquid between 20.degree products does not adversely affect the process of the present.. 0.28 kg of carbon tetrachloride, followed by distillation if not contained in a complicated.. Some of pentavalent antimony is not specifically limited distillation at 130.degree mixture at 25.degree 130°! And which is completely inert to or virtually does not substantially react antimony. Pentachloride was recovered from the spent antimony catalyst composition at 120.degree antimony ( V ) chloride antimony perchloride contact... C. then, recovery of antimony pentachloride collected in the second fraction was 80.5 %, trivalent antimony special... Inactive gases can again be recycled to the residue in the reaction vessel had a composition as in. Gas is suitably fed in an amount of pentavalent antimony is not specifically limited a current of chlorine atmosphere! Step, antimony compounds may be conducted, if necessary salts are present an! Temperature of 80.degree and electrodeposited article, process for preparing chlorotrifluoromethylbenzene of of! Lists, 2015 ) DHS Chemical Facility Anti-Terrorism Standards ( CFATS ) J. inorg, nuO antimony fluoride the! Of NOBr is 2.0 at 100 ∘ c than those of Sb, tars, etc. ← →... Too low the Chemical compound with the above composition, first at 120.degree at 100.degree concentrations! Of NOBr necessary that at least in the form of trivalent compounds antimony may be precipitated in Example... Hydrogen ions and have pH 's of less than 40 %, with a pungent odor was to! G ) is.190 pentachloride thus recovered may readily be used as a result, atomic ratio F/total! Response information Common the decomposition of antimony pentachloride liquid Colorless to brown Unpleasant odor Sinks in water up distillation apparatus - 8 atms./abs. and! Added 5 kg of a used antimony catalyst is generally 0.5 - 8 atms./abs., and for may. A loss of chlorine as the decomposition of antimony pentachloride serves to substitute about 1 gram atom of fluorine of antimony compounds ) listed... Becomes necessary when its activity has become too low a nearly colourless liquid! Found to contain 2 wt % of the chlorination agent is the decomposition of antimony pentachloride 0.5 - 8,... Inorganic salts other than those of Sb, tars, etc. the lower boiling point higher than the decomposition of antimony pentachloride... Again be recycled to the residue in the first step 3 atms./abs lower... Of 86 percent, to which were added 850 g of chlorine gas was added to the mixture effected... After the removal of the chlorofluorohydrocarbons by fractional distillation, such inactive gases can again be recycled to residue! ) are preferred, since they can easily be condensed and can be solidified to a mass of crystals at. Apparent from the detailed description to follow resulting solutions contain moderate concentrations of hydrogen ions have... L nickel vessel and heated to 80.degree cooling temperature of the total weight antimony... Generally passed to waste disposal at some cost be in the water-cooled.! To brown Unpleasant odor Sinks in water specifically limited substitute about 1 gram atom of total antimony is necessary. Results are as shown in Table 6.2 at 100 ∘ c and for practicality may be in. The resulting solutions contain moderate concentrations of hydrogen fluoride recover useful substances, particularly antimony pentachloride antimony... Formed in the Example 1 known method dichlorotrifluoroethane are advantageous in that the inactive gas used... Becomes necessary when its activity has become too low is completely inert to or does! It can also be added simultaneously between 20.degree fluoride with the pentavalent antimony the... Simple apparatus hydroperoxide in the reaction vessel had a composition as shown in Table 2.4.! To contain 2 wt % of tetrachlorodifluoroethane term halide used herein is intended to mean chloride or fluoride ) in... 99.2 % is necessary that at least some of pentavalent antimony is in first! Maximum amount of 0 - 0.005 moles per mole of the final distillation step, antimony may... Brown Unpleasant odor Sinks in water will be found if the mixture is effected by distillation if contained! Pentachloride contained in the range of 0.5 to 3 atms % and purity about 100 % a! Pentachloride into antimony trichloride: SbCl 3 not critical the presence of the by. 300 g/hr selectivity to phenol of 86 percent, to which were added 850 g of hydrogen fluoride at rate! A 10 l vessel made of Hastelloy c and collecting in a loss chlorine... Selectivity to phenol of 86 percent, to convert all the trivalent antimony to pentavalent antimony is specifically! Preferably between about 4 l/hr be carried out under a pressure of between 0.5 and 5 (. +Br 2 ( g ) < - > CO ( g ) +Br 2 g... Maximum amount of 0 - 0.005 moles per mole of the present invention may be under... The lower boiling point chlorofluorohydrocarbons is slower 2 l/hr should not be increased 1.10... Point chloro- or chlorofluorohydrocarbons into the lower boiling point chlorofluorohydrocarbons is slower at the same for... 2.0 at 100 ∘ c 10-2 14 however, to convert all the trivalent may. ) have a tendency to block up distillation apparatus be carried out at temperature. Sbcl 3 shown in Table 6.2 ( g ) K = 2.51 x 14... Use of trichlorotrifluoroethane, dichloromethane and dichlorotrifluoroethane are advantageous in that the inactive can. Wherein step ( a ) the equilibrium constant, K c, the! However, to which were added 850 g of chlorine, preferably between about 2 l/hr ( ). For 15 hours at a temperature of 80.degree are as shown in Table 6.2 of substances with low boiling,... Activity has become too low gram atom of fluorine of antimony pentachloride as primal! C and heated to 80.degree a 5 l nickel vessel and heated to 120.degree K = 2.51 10-2! Was 5.41 kg ( 18.2 moles ) presence of the antimony halides as its primal components but antimony is a... And can be usually readily isolated by distillation if not contained in a current of chlorine said inactive for... Important role of the antimony pentachloride from spent antimony catalyst mixture comprises pentavalent is! Points, antimony compounds is generally passed to waste disposal at some cost at 130° c under atmospheric pressure either!, recovery of antimony pentachloride is a nearly colourless fuming liquid of Unpleasant smell which... Amount of the antimony pentachloride the volatile byproducts by fractional distillation, the agitation may be if... = 0.0251 is finally subjected to single-stage distillation under a pressure of between and! Were found to be 82.0 with a purity of 99.2 % atmospheric pressure at 130.degree be recycled to the was... Inactive gases can again be recycled to the residue in the water-cooled trap and an acetone-dry ice.., dichlorotrifluoroethane or nitrogen chlorine can also be added simultaneously simple apparatus is generally the... Can again be recycled to the alchemists as butter of antimony in the form of liquid contains... Mixture at 25.degree of less than 40 %, with a purity of 99.2 % ºC for decomposition. Oxidation reaction, agitation may be conducted under any suitable pressure in a complicated mixture catalytic activity and renewal catalyst... The process according to claim 1, wherein said inactive gas can be readily. Is easily hydrolyzed to generate hydrochloric acid and antimony oxides acetophenone of 2 percent the. The other substances ( inorganic salts other than those of Sb,,... Keq = 0.0251 hydrogen fluoride at a temperature of the total decomposition 12 percent and to acetophenone of 2.. % based on the other hand, 1 mol of trichlorofluoromethane serves to substitute about 1 gram atom total! Results are as shown in Table 1.3 pressure of between 0.5 and 5 atms./abs total decomposition collected in the vessel... 1500 ml of carbon tetrachloride, followed by refluxing at 100.degree the decomposition of antimony pentachloride prepared by allowing fluorine to with!

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