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Water-Soluble, Film-Forming Inorganic Compounds, Fireproof and Fire

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Water-Soluble, Film-Forming Inorganic Compounds, Fireproof and Fire Europaisches Patentamt ® European Patent Office ® Publication number: 0 346 162 Office europeen des brevets A2 ® EUROPEAN PATENT APPLICATION (3) Application number: 89305928.7 ® int. ci .4; C 04 B 41/50 C 04 B 12/00, C 04 B 28/00, @ Date of filing: 12.06.89 C 09 J 1/00, B 32 B 7/12 @ Priority: 10.06.88 JP 144397/88 @ Inventor: Kokuta, Naota 10.06.88 JP 144398/88 364-1 Emisu Shikama-ku 10.06.88 JP 144399/88 Himeji Hyogo (JP) Kokuta, Kenji @ Date of publication of application : 13.12.89 Bulletin 89/50 20-6 Honson 5-chome Chigasaki Kanagawa (JP) @ Designated Contracting States: DE FR GB IT Kokuta, Katsuhiro 20-6 Honson 5-chome © Applicant: KOHMIX CO., LTD. Chigasaki Kanagawa (JP) Honson 5-chome 20-6, Chigasaki Kokuta, Hiroshi Kanagawa (JP) 20-6 Honson 5-chome Chigasaki Kanagawa (JP) @ Representative: Lamb, John Baxter et al MARKS & CLERK 57/60 Lincoln's Inn Fields London WC2A3LS (GB) @ Water-soluble, film-forming inorganic compounds, fireproof and fire-resistance composites and fire-resistance, flexible, sheet composite covering materials formed by the use of the compounds, and fire-resistance-covering process. (g) This invention is concerned with water-soluble film-forming inorganic compounds having a specific gravity of 1.1 or more and capable of being formed into a film at ordinary temperature or by heating, said compound being formed by a reaction of a metal, a mineral acid compound capable of hydrating accompa- nied by the dissociation of boric acid or hydrofluoric acid, and an alkali metal, wherein in water or a solution of said mineral acid compound, said metal in solid state reacts with a concentrated solution of said alkali metal, and then said mineral acid compound takes part in the reaction, while reaction temperature is controlled within a temperature range of 50° C to 100°C. The invention also relates to fireproof and heat-resist- ance layered composites made of metal, wood, and the like with the above-mentioned water-soluble film-forming inorganic compound as adhesive or coating, or in combination with other fastening means. Bundesdruokerei Berlin EP 0 346162 A2 Description Water-soluble, film-forming inorganic compounds, fireproof and fire-resistance composites and fire-resistance, flexible, sheet composite covering materials formed by the use of the compounds, and fire-resistance-covering process. 5 BACKGROUND OF THE INVENTION Field of the Inention Film-forming inorganic compounds capable of being formed to be flexible according to the prsent invention 10 have extensive industrial uses, for example, as coatings for papers, fibers, cloths, and the like; for the purpose of preventing firing, increasing heat resistance, raising melting point as applied to a glass cloths, and preventing ignition, flaming and fuming as in wood impregnated with the compounds; and as rust inhibiting coatings and refractory adhesives to ceramics; and so on. Besides the present invention relates to fireproof and fire-resistance composites and refractory flexible 15 sheet composite covering materials for use in the interior as of very tall buildings, and for the purposes as of heat-resistance and heat-insulation and sound-insulation in motor vehicles, ships, and the like, and also relates to fire-resistance-covering process using these composite materials. Description of the Prior Art 20 Sodium silicate used so far as inorganic adhesive or coating material has disadvantages: for example, it is hygroscopic, gets carbonized with turning white, gets solidified with occurrence of cracks, and tends to peel. A fluoride can be added to improve water-proofness, and this is not always sufficiently effective. Silica sol and silica alkoxide are commercially available. They themselves have no film-forming property, and so modified by addition of an organic compound into film-forming substance but failed to become high 25 temperature resistant and refractory. Teflon, a synthesis product of freon and organic compound, has good heat resistance compared with general synthetic resins but is not qualified as refractory. There have been proposed in U. S. patents Nos. 4,117,088, 4,029,747 4,117,099 and Japanese unexamined patent publication No. 51-132196 methods of preparing water-soluble inorganic complexes by reaction of a metal with ammonia, or sulfuric or phosphoric acid or their salts with an alkaline metal, and the products have 30 not any film-forming property. "Hardening phenomenon" has been in the first place generally described as beginning upon reaching supersaturation of a solute, and thus occurring through gel bonding into a crystalline structure. In the above-mentioned U. S. patents, to a water-soluble inorganic complex was added such as silica sol, sodium silicate, pozzolan or fly ash for the realization of much supersaturation of a metallic component such as Si, 35 resulting in getting little film forming property, that is, in failure to form flexible coating film. Aqueous solutions as of sodium silcofluoride, sodium silicoborate can be dried to get merely powdered, with failure to form coating. Likewise glass, for example, as a compound of silicic acid, boric acid and alkali metal, may be adaptive for preparing water soluble coating. As described above, Teflon which is a fluorine-containing compound cannot be processed into high 40 molecular coating film by the use of inorganic compounds and nothing else. It therefore is an object of the present invention to provide a water-soluble film-forming inorganic compound having high molecular weight, without needing solvent, and being capable of being formed into flexible coating film. For providing such film-forming property as usual organic coatings have, it may be necessary to change into 45 high molecular compound. Fire-proof and flame-proof characteristics comes from becoming heat-resistant film- forming material capable of blocking supply of oxygen. Further the fire- and flame-proof coating film suitable for metal plates fibrous products is required in combination to be a flexible heat-resistant coating film. On the other hand, from the viewpoint of low expenditure involving wide-spread uses, without needing solvent, and polymerization associated with a high productivity are required. 50 The present invention has solved all the above-mentioned problems. SUMMARY OF THE INVENTION Water-soluble film-forming compounds according to the invention can be produced only by the reaction of a metal, a mineral or submineral acid compound (referred collectively to as mineral acid compounds hereinafter) 55 able to hydrate, then accompanied by dissociation of boric or hydrofluoric acid, and a alkali metal. For example, the reaction product of Si, F and Na, which probably is sodium silicofluoride, has so low solubility as incapable of be aqueous solution of 2.45% or more in solid content even at 100 °C. Another reaction product of Si, B and Na, probably sodium silicoboride, is similar. Contrast to these, the aqueous solutions according to the invention, if they has solid contents 45% or more, were analysed with detection only of Si, F and Na, or Si, B 60 and Na, and this have demonstrated that they were not known compounds. According to the above-mentioned U. S. Patent, for example, reaction among silicon, sodium hydroxide and sulfuric acid can occur when sodium hydroxide flakes are dropped and placed in contact with metallic silicon, which is found at the bottom of a reaction vessel, and at this localized area. When metallic silicon lumps were 2 EP 0 346 162 A2 Bxcessively laid over the bottom of the reaction vessel, and the reaction vessel was filled to a half ot it with a diluted solution of boric acid, the feeding sodium hydroxide flakes at a time by spreading in so much amount as the silicon surface was covered, however, was observed to be not cause localized reaction because, if this was ocal reaction involving sodium hydroxide flakes, reaction would occur overall the botom of the vessel at a time, but actually partial consumption occurred intermittently, and so that the reaction or consumption of 5 rJissoved components at the bottom was allowed in accordance with the solubility. Likewise, with 1 m/m aluminum wire as a metal, irrespective of sodium hydroxide flakes were scattered, reaction accompanied by the appearance of white cloud not can be observed only in the vicinity of the flakes and as if it had crept but also along the aluminum wire. Besides, when metallic silicon was wrapped in a iron mesh and suspended 5 cm or longer above the bottom of the reaction vessel, sodium hydroxide flakes were w supplied to the bottom not to be placed into direct contact with silicon, and thus reaction commenced accompanied by production of bubbles in the same was as in the direct contact. From the above-described, the present invention is demonstrated to be distinguishable from the localized reaction of flakes described in the above-mentioned U. S. Patents, and this is explainable as follows: dissolution of flakes settled to the bottom of the reaction vessel achieves to equilibrium point at a certain 15 solubility, that is, consumption of them by the reaction or change in solubility of them owing to convection contributes to additional dissolution. Water-soluble film-forming inorganic compounds according to the invention can be produced by reaction Detween a solid metal and a concentrated alkali metal solution, in which hydrated boric acid and hydrofluoric acid takes part, the reaction proceeding exothermic reaction or under heating. With borax and sodium fluoride, 20 Dwing to their lower solubilities than that of the acid, the reaction is not directly activated and can be controlled. In summer, frequently the reaction must be regulated so as not to cause boiling by cooling or by addition of at least one selected from the group of hafnium compounds or zircon, zirconias and zirconia-byproduct zirca, (these zirconium compounds are referred collectively to as zircons hereinafter) in 0.5 to 100% of the mineral acid compounds.
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