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Process for Preparing Colloidal Solution of Antimony Pentoxide

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Process for Preparing Colloidal Solution of Antimony Pentoxide Europaisches Patentamt European Patent Office (jj) Publication number: 0134 708 B1 Office europeen des brevets ® EUROPEAN PATENT SPECIFICATION (§) Date of publication of patent specification: 18.10.89 @ Int. CI.4: C 01 G 30/00, B 01 J 13/00, ~ C 09 K 21/00 (n) Application number: 84305426.3 (22) Date of filing: 09.08.84 (H) Process for preparing colloidal solution of antimony pentoxide. (30) Priority: 16.08.83 JP 149358/83 (73) Proprietor: NISSAN CHEMICAL INDUSTRIES LTD. 3-7-1, Kanda Nishiki-cho (§) Date of publication of application: Chiyoda-ku Tokyo (JP) 20.03.85 Bulletin 85/12 Inventor: Watanabe, Yoshitane @ Publication of the grant of the patent: 3-5-1-91 1,Hirai 18.10.89 Bulletin 89/42 Edogawa-ku Tokyo (JP) Inventor: Suzuki, Keitaro c/o Nissan Kagaku Yatsu-Ryo (§) Designated Contracting States: 5-32-9, Yatsu Narashino-shi BEDE FRGB Chiba-ken (JP) Inventor: Teranishi, Masayuki 7-27-13, Takanedai (3) References cited: Funabashi-shi Chiba-ken (JP) EP-A-0025 246 DE-A-2 622 608 DE-A-2715 737 @ Representative: Wood, Anthony Charles et al GB-A-2126205 Urquhart-Dykes & Lord 91 Wimpole Street CD US-A-4348301 London W1M8AH (GB) oo o ^- CO Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition shall CL be filed in a written reasoned statement. It shall not be deemed to have been filed until the opposition fee has been LU paid. (Art. 99(1) European patent convention). Courier Press, Leamington Spa, England. 1 EP 0 134 708 B1 2 Description monate to an acid treatment under the conditions as prescribed hereinlater to form a gel, and then Background of the invention peptizing the gel by use of an organic base. This invention relates to a process for preparing According to this invention, there is provided a a colloidal solution of antimony pentoxide. More 5 process for preparing an antimony pentoxide sol, particularly, it relates to a novel process for which comprises dispersing an alkali antimonate preparing a colloidal solution of antimony pen- in water, reacting the alkali antimonate with a toxide by obtaining an antimony pentoxide gel monovalent or divalent inorganic acid added in a from an alkali antimonate and an inorganic acid, stoichiometrical amount of 0.7 times to 5 times and then peptizing the gel by use of a base. io the amount of the alkali antimonate to form an The colloidal solution of antimony pentoxide antimony pentoxide gel, followed by separation (hereinafter referred to as "antimony pentoxide and water washing of the gel, dispersing said gel sol") is used as a flame retardant or the like for in water, and peptizing the thus dispersed gel by plastics, fibers, etc. Conventional processes for adding an organic amine or guanidine hydroxide preparing the antimony pentoxide sol are roughly 15 in such a manner that the stoichiometrical classified into an ion exchange method and a amount of base/Sb205 ranges from 0.03 to 1. Y hydrogen peroxide method. As the former ion exchange method, there may be mentioned a Brief description of the drawing method in which potassium antimonate is Figs. 1, 2 and 3 each show an electricon deionized (U.S. Patent 3,860,523), or a method in 20 microscopic photograph of antimony pentoxide which sodium antimonate is deionized (U.S. sol obtained in Examples 1, 3 and 6, respectively; Patent 4,110,247). The antimony pentoxide sols Fig. 4, a photograph of antimony pentoxide sol obtainable by this method have good dispersibil- prepared by an ion exchange method; and Fig. 5, ity as they are comprised of particles almost by a hydrogen peroxide method. Magnification: spherical in shape, and are characteristic in that 25 200,000 each. they can further be made higher in concentration. However, it is difficult according to this ion Description of the preferred embodiments exchange method to effect ion exchange when Alkali antimonate which is a starting material the concentration of antimony pentoxide exceeds used in this invention is represented by the 10%, Moreover, this method has a drawback that 30 general formula: it requires complicated operations such that sub- sequent operations for separation and regenera- M20 • Sb2Os • XH20, tion of ion exchange resins must be carried out. The latter hydrogen peroxide method is a method in which M represents an alkali metal such as in which antimony trioxide is oxidized by use of 35 sodium and potassium, and X=0 to 6. Sodium is hydrogen peroxide at a high temperature (see, preferred as the alkali metal. Particularly pre- USP 4,022,710; Japanese Unexamined Patent ferred is a hydrate of sodium antimonate Publication No. 21298/1977; U.S. Patents, 4,028,226 and 4,026,819). This method shows Na20 • Sb2Os • 6H20 (NaSb(OH)6; high productivity because it is possible to obtain 40 antimony pentoxide sols comprising about 30% 63 to 64% by weight of Sb205, 12 to 13% by antimony pentocide directly, but inadvantageous weight of Na20 and 23 to 24% by weight of H20). in that the viscosity increases when antimony The acid usable in this invention for the step of pentoxide exceeds 30%. Moreover, this method forming the antimony pentoxide gel by the reac- has drawbacks that colloidal particles of the sols 45 tion of an alkali antimonate with an acid includes are irregular in shape so that there is obtained monovalent or divalent inorganic acids such as only poor dispersibility and, because of strong hydrochloric acid, nitric acid, sulfuric acid and surface activity, poor compatibility with resin sulfamic acid. Phosphoric acid, which has acid emulsions and the like. strength almost equal to antimonic acid GB— A— 2126205 discloses a finding that a so (HSb(OH)6), is unavailable for obtaining the anti- hydrated metal oxide or hydroxide can be pep- mony pentoxide gels. Acids of weaker acid tized in water by adding a quaternary ammonium strength, such as formic acid, exalic acid, etc., are hydroxide. A preferred metal oxide is hydrous also unavailable for obtaining the desired anti- antimony (V) oxide. The extent of peptization can mony pentoxide gels. be sufficient for creation of a sol. 55 In the reaction of an alkali antimonate with the above acid in this invention, it is possible to use Summary of the invention the alkali antimonate in concentration of 2 to 35% In order to eliminate the above-mentioned by weight in terms of anhydrous antimony pen- drawbacks in the conventional processes for pre- toxide (Sb2Os) in the reaction mixture. In case the paring antimony pentoxide sols, the present 60 concentration is less than 2% by weight, the inventors have made intensive studies on the amount of antimony pentoxide gels produced preparation of antimony pentoxide sol composi- becomes too small to be desirable from economi- tion. As a result, they have found a novel process cal viewpoint. In case it is in excess of 35% by in which the desired antimony pentoxide sol is weight, the solid portion in the reaction mixture obtained by first subjecting a starting alkali anti- 65 reaches 50% or more and the reaction becomes 2 3 EP 0134 708 B1 4 heterogeneous. Preferable concentration ranges After dispersing the wet cake of the antimony from 6 to 25% by weight as the anhydrous pentoxide gels in water, antimony pentoxide sols antimony pentoxide. can be obtained by peptizing the gels under the In the reaction of alkali antimonate with the conditions prescribed below. above acid according to this invention, concen- 5 By the way, the antimony pentoxide gels can tration of the acid may be selected such that the not be peptized under the conditions prescribed stoichiometrical amount of acid/alkali antimonate below, if they are turned to a dry gel. ranges from 0.7 to 5, preferably, from 1 to 3. In The base usable in the step of peptizing the case the stoichiometrical amount is less than 0.7, antimony pentoxide gels according to this inven- it is impossible to obtain the desired antimony 10 tion may include amines such as triethanolamine, pentoxide gels even if reaction temperature and tripropanolamine, diethanolamine, mono- concentration of alkali antimonate are elevated. In ethanoiamine, N-ethylaminoethanolamine, etc; case it exceeds 5, the antimony pentoxide gels quaternary ammonium hydroxides such as tet- formed are peptized at the stage of water wash- raethanolammonium hydroxide, monomethyl- ing, whereby sols are washed away into a filtrate, 15 triethanolammonium hydroxide; and organic and thus the productivity becomes inferior. bases such as guanidine hydroxide, etc. Bases In the reaction of alkali antimonate with the such as sodium hydroxide, potassium hydroxide above acid according to this invention, reaction and ammonia are not suitable as the base since temperature may range from room temperature they, which are incorporated into the structure of to 100°C, and the reaction time available may 20 the antimony pentoxide, can only be peptized in range from 1 hourto 15 hours. In order to obtain part (see Comparative Examples). Addition of any antimony pentoxide sols of good shape, it is of these bases is effective in that the antimony preferred to employ the reaction temperature not pentoxide gels formed by the reaction are pep- higher than 50°C and the reaction time not longer tized, and, in addition, plays an important role in than 10 hours. When the reaction temperature is 25 that fine particles thereof are dehydrated and higher than 50°C and the reaction time exceeds 1 5 condensated to become colloidal particles of anti- hours, particles of the resultant antimony pentox- mony pentoxide nearly spherical in shape and 10 ide sols tends to become irregular in shape.
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