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United States Patent (19) 11) 4,351,741 Vogt (45) "Sep

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United States Patent (19) 11) 4,351,741 Vogt (45) United States Patent (19) 11) 4,351,741 Vogt (45) "Sep. 28, 1982 54 METHOD OF PREPARING ANTIMONY Theoretical Chemistry, Longmans, Green & Co., Ltd., PENTOXDE, COLLOIDS THEREOF AND vol IX, p. 439 (1949). THEIR PREPARATION Primary Examiner-Richard D. Lovering , 75) Inventor: John W. Vogt, Chagrin Falls, Ohio Attorney, Agent, or Firm-Maky, Renner, Otto & Boisselle (73) Assignee: The Harshaw Chemical Company, Cleveland, Ohio 57 ABSTRACT A method of preparing antimony pentoxide from solids *) Notice: The portion of the term of this patent containing antimony sulfides is described. The method subsequent to Jun. 20, 1995, has been comprises the steps of disclaimed. (a) leaching the antimony values from the solids with (21) Appl. No.: 9,032 an aqueous potassium hydroxide solution to form an antimony-containing solution and a gangue, 22 Filed: Feb. 5, 1979 (b) oxidizing the antimony present in the leaching 51) Int. Cl. ....................... B01J 13/00; C01G30/00 solution to a pentavalent antimony, (c) recovering the oxidized solution, and (52) U.S. C. ............................. 252/313 R; 106/18.25; (d) adding an inorganic acid to the solution to reduce. 106/18.28; 252/609; 252/610; 423/87; 423/617 the pH of the solution to about 5-7 whereby anti 58 Field of Search .............. 252/313 R; 423/87, 617 mony pentoxide is precipitated from the solution. (56) References Cited The gangue may be separated from the leach solu U.S. PATENT DOCUMENTS tion either prior to or after the oxidizing step. 3,860,523 1/1975 Petrow et al. .............. 252/313 RX In a preferred embodiment, the oxidation of the solution 4,026,819 5/1977 Langere et al.................. 252/313 R is conducted in the presence of a catalyst which com 4,096,232 6/1978 Vogt ............................... 423/617X prises a water-soluble copper salt, a quinone, a hydro quinone or mixtures of one or more of these. OTHER PUBLICATIONS Mellor; A Comprehensive Treatise on Inorganic and 16 Claims, No Drawings 4,351,741 1 2 and thereafter deionizing the potassium antimonate by METHOD OF PREPARING ANTIMONY passing the solution through a hydrogen form cation PENTOXIDE, COLLOEDS THEREOF AND THEIR exchange resin. PREPARATION Another method for forming sols of antimony pen toxide is described in U.S. Pat. No. 3,657,179. This BACKGROUND OF THE INVENTION patent describes the reaction of antimony trichloride Attempts have been made to incorporate metallic with nitric acid to form a dispersion in a polar organic oxides such as antimony oxide into organic polymers, solvent, and stabilizing the dispersion with an alpha both natural and synthetic, to improve their properties. hydroxy carboxylic acid. Such dispersions contain from For example, these oxides have been used to improve 10 about 0.01 to 5% water by weight. the resistance to burning, particularly when employed Another process for preparing colloidal dispersions in conjunction with organic halogen compounds and of antimony pentoxide is described in U.S. Pat. No. other halogen-containing materials. While the exact 3,994,825, and the process involves mixing particles of mechanism which results in the flame-retardant proper antimony trioxide with an aliphatic polyhydroxy alco ties is not fully understood, it is believed that an anti 15 hol having vicinal hydroxyl groups and contacting said mony oxide halogen compound may be formed in situ particles with hydrogen peroxide to convert the anti which interferes with oxidizing reactions and therefore mony trioxide to hydrous antimony pentoxide. Reac inhibits burning. tion preferably is accomplished at a temperature of A variety of techniques have been employed to intro between 50 and 105 C. The colloidal sol which results duce the antimony oxide into organic polymers. For 20 is a stable dispersion containing antimony pentoxide example, oxide particles prepared by milling have been with a reported average size of from about 50 Ang suspended in spinning solutions, molding solutions, or stroms to about 200 Angstroms. polymer melts in attempts to incorporate the oxide in More recently, an improved method for preparing the resulting film, fiber or molded body. The use of this colloidal aqueous sols of antimony pentoxide from a technique generally results in delustering of the poly 25 water insoluble metal antimonate was described in U.S. mer due to the scattering of light by the large oxide particles, and the large particles also have relatively low Pat. No. 4,110,247. The method involves passing a chemical reactivity and a low efficiency as a flame slurry of a water-insoluble metal antimonate through a proofing agent. In the case of fibers, the diameter of the fluidized bed containing a cation exchange resin oxide particles may approach the diameter of the fibers 30 whereby the metal antimonate is converted to a colloi themselves thereby weakening the bond between the dal antimony pentoxide. organic polymer and the oxide. SUMMARY OF THE INVENTION Antimony oxides also have been applied as surface coatings along with a resinous binder. These coating The present invention provides a method of prepar techniques, however, also result in delustering and pro 35 ing antimony pentoxide and colloidal aqueous sols of duce fabrics which have a stiff, harsh hand, poor flexi antimony pentoxide from antimony sulfide bearing bility and low tear strength. solids, particularly naturally occurring ores and ore Additional attempts have been made in the art to concentrates. The method of the invention comprises avoid some of the deficiencies of the above procedures the steps of by using aggregates of oxides prepared as gels, as pre 40 (a) leaching the antimony values from the solids with cipitated powders, and as aggregates prepared by oxi an aqueous potassium hydroxide solution to form an dizing the corresponding metallic halides. The use of antimony-containing solution and a gangue, aggregates, however, has resulted in non-uniformity of (b) oxidizing the antimony present in the leaching properties resulting from the difficulties of preparing solution to a pentavalent antimony, uniform aggregates and homogenously distributing the 45 (c) recovering the oxidized solution, and aggregates throughout the polymer. (d) adding an inorganic acid to the solution to reduce More recently, it has been discovered that antimony the pH of the solution to about 5-7 whereby antimony oxide prepared as sols of colloidal particles of antimony pentoxide is precipitated from the solution. The gangue oxide dispersed in various liquid media is useful. For may be removed from the leach solution either before example, U.S. Pat. No. 3,676,362 describes sols com 50 or after the oxidizing step. The antimony pentoxide posed of substantially discrete colloidal particles of recovered as a precipitate in the method of the inven antimony oxide having an average particle size in the tion either can be dried to a powder which is easily range of about 2 to about 50 millimicrons dispersed in a reduced by milling to useful particle sizes for dispersion polar, organic liquid. Such sols can be mixed with a in plastics and other materials, or the antimony pentox solution of a polymer in a polar organic liquid, and the 55 ide precipitate can be dispersed in water to form stable mixture processed in a conventional manner for making antimony pentoxide colloids containing up to about 30 fibers and films. These sols are prepared by reacting a to 40% solids. metal halide with water and ammonia in a polar organic DESCRIPTION OF THE PREFERRED liquid. The water converts the halide to antimony oxide EMBODIMENTS in colloidal dispersion and an ammonium salt precipi 60 tates. The present invention relates to a method of prepar U.S. Pat. No. 3,860,523 describes the preparation of ing antimony pentoxide and antimony pentoxide colloi colloidal antimony oxide sol, preferably in the Sb2O5 dal sols from naturally occurring ores which contain form with an average particle diameter of about 2 to 100 antimony sulfide. The method of the invention com millimicrons. The sol is prepared by first preparing 65 prises leaching the antimony from the antimony sulfide water-soluble potassium antimonate by reacting anti bearing ores utilizing an alkaline solution prepared from mony trioxide with potassium hydroxide and hydrogen potassium hydroxide, oxidizing the antimony present in peroxide in the ratio of 1 mole to 2.1 moles to 2 moles, the leach solution to a pentavalent antimony, and pre 4,351,741 3 4. cipitating antimony pentoxide from the oxidized solu salt, a quinone, a hydroquinone, or mixtures of one or tion by the addition of an inorganic acid to the solution more of these materials. In addition to the above named to reduce the pH to from about 5 to 7. The antimony materials, the catalysts also may contain ferrous ions. pentoxide prepared in this manner appears to have For example, the effectiveness of copper ions appears to unique properties such as the facile reduction of the be improved by the presence of a small amount of fer dried powder to fine particle size antimony pentoxide. rous ions. Copper salts which are useful include copper Also, it has been discovered that the antimony pentox sulfate, copper chloride, etc. The catalyst also may be a ide powder obtained in this manner exhibits excellent quinone which may be defined as a cyclic unsaturated dispersability in thermoplastics such as polypropylene. ketone having two carbonyl groups directly attached to Moreover, aqueous colloids can be prepared from the O a six-membered ring containing two double bonds (No antimony pentoxide prepared in accordance with the menclature of Organic Compounds, John H. Fletcher et method of the invention which exhibit improved stabil al., editors, American Chemical Society, Washington, ity, even when the colloids contain up to about 30 to D.C., 1974, page 225).
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