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    • 1. 发明专利
    • DE1467630A1
    • 1969-07-17
    • DE1467630
    • 1963-05-28
    • MONSANTO CO
    • EUGENE FEIERSTEIN HAROLDYU SHEN CHUNGROY VERSEN ROBERT
    • C01B25/41C11D20060101C11D3/02C11D3/06C11D3/34C11D11/00
    • 1,053,384. Alkali metal polyphosphate hydrates. MONSANTO CO. June 5, 1963 [June 6, 1962], No. 22373/63. Heading C1A. [Also in Division C5] A hydrated alkali metal polyphosphate in solid porous condition is produced by foaming an aqueous slurry containing an alkali metal polyphosphate, preferably in amount of at least 10% by weight of the slurry, and at least 10%, preferably at least 25% and at most 50%, of its weight of water, heating the slurry whilst it is in a foamed condition, preferably at a temperature of at least 50‹ C., especially in the range 50‹ to 135‹ C., thereby to form hydrated alkali metal polyphosphate therein, and converting the foamed slurry to solid condition. The slurry may contain a foaming agent, e.g. synthetic anionic, non-ionic and ampholytic active detergent materials, examples of which are listed. The slurry may also contain a hydratable inorganic salt to absorb any excess water. The foaming may, in part, be effected by generating steam from the free water in the slurry or by injection of a gas into the slurry.
    • 2. 发明专利
    • DE1567661A1
    • 1972-04-13
    • DE1567661
    • 1963-04-18
    • MONSANTO CO
    • YU SHEN CHUNG
    • C01B25/445C01B25/38
    • Alkali metal polyphosphates are obtained by heating a mixture of an alkali metal salt of a volatile acid and a water-soluble material selected from ammonium phosphate salts and mixed ammonium-alkali metal phosphate salts at above 200 DEG C., the overall ratio of alkali metal to phosphorus being between 0.75 and 3. The alkali metal salt is one which decomposes at below 600 DEG C. in a concentrated phosphoric acid medium, and the metal may be sodium, potassium, lithium, rubidium or caesium. The volatile acid is one which may be removed, or its degradation products removed, by distillation from a concentrated phosphoric acid medium at below 600 DEG C. at atmospheric pressure, e.g. hydrofluoric, hydrochloric, hydrobromic, hydriodic, nitric, nitrous, carbonic, oxalic and formic acids. The ammonium phosphate salts, of water solubility at least 5% at 25 DEG C., may be mono-, di- and triammonium orthophosphates, ammonium pyrophosphates, trimetaphosphates, tetrameta phosphates, tripolyphosphates, the ammonium salts of polymeric phosphoric acids with more than four phosphorus atoms per molecule, and mixtures thereof, and polyammonium polyphosphates formed by reaction of NH3, H2O and P2O5. The mixed ammonium-alkali metal phosphates may be monosodium monoammonium orthophosphate, disodium diammonium orthophosphate and monopotassium tetra-ammonium tripolyphosphate. At least half the alkali metal requirement is preferably in the form of the volatile acid salt. The ratio of ammonium ion to metal is at least 1, except when the metal carbonate, bicarbonate, formate or oxalate is utilized when it may be as low as 0.7. Preferably alkaline earth metal cations are absent. Alkali metal trimetaphosphate is obtained when the ratio of alkali metal to phosphorus is 1, tripolyphosphate when the ratio is 1.67 and pyrophosphate when the ratio is 2. With intermediate ratios mixtures are obtained. Ratios between 0.75 and 1 give "ultraphosphates," and between 2 and 3 mixtures of pyrophosphate and orthophosphate are obtained. When the ratio is above 2, the more alkaline reacting alkali metal salts are utilized, e.g. sodium carbonate, potassium carbonate, sodium oxalate and formate. The mixture is prepared by blending crystals of the reactants in e.g. a ribbon mixer, or by mixing solutions and drying, or, less desirably, by mixing the molten reactants. The mixture is heated in e.g. an externally heated stainless steel drum, to a temperature at least 50 DEG C. higher than that at which it initially melts, but preferably to below the melting point of the polyphosphate being prepared, and maintained at this temperature for at least 5 minutes. The reaction temperature is generally above 300 DEG C. Preferably the temperature of the mixture is raised over a period of at least 10 minutes through at least 150 DEG C. after the first gaseous decomposition products are evolved, which usually occurs about 110 DEG C. The end of the reaction is indicated when the reaction mixture becomes solid, e.g. between 350 DEG C. and 625 DEG C. The product is cooled to ambient temperature. Alternatively the reaction mixture may be quenched while still molten. In examples the specified alkali metal salts are sodium chloride, sodium carbonate, sodium nitrate, potassium chloride, potassium carbonate, potassium chlorate and mixtures thereof.
    • 3. 发明专利
    • DE1567670A1
    • 1972-04-13
    • DE1567670
    • 1964-03-18
    • MONSANTO CO
    • YU SHEN CHUNG
    • C01B25/38C01B25/39C01B25/41C01B25/42C01B25/445C01B25/45C01B37/04C02F5/08C11D3/06
    • A detergent composition contains as builder an effervescent composition comprising an amorphous alkali metal condensed phosphate, free alkali metal carbonate and free condensed phosphoric acid, which has an alkali metal to phosphorus molar ratio of from 0.5 to 5 and the ability to sequester in aqueous solution at least 1 g. of calcium per 100 g. of the said composition. The term "alkali metal" includes ammonium. Specified surface active compounds included in the detergent composition are alkali metal salts of organic sulphates or sulphonates, polyethylene oxide condensates with fatty acids, phenols, alcohols, amides or amines and amphoteric compounds such as sodium-N-methyl laurate and N-COCO- beta-amino propionate. In an example detergent tablets are prepared from a builder of the invention, sodium metasilicate, sodium dodecyl benzene sulphonate, sodium sulphate and sodium carboxymethyl cellulose.ALSO:An effervescent composition comprising an amorphous alkali metal condensed phosphate, free alkali metal carbonate and free condensed phosphoric acid has an alkali metal to phosphorus molar ratio of from 0.5 to 5 and the ability to sequester in an aqueous solution at least 1 g. of calcium per 100 g. of said composition. The term "alkali metal" includes ammonium. The amorphous condensed phosphates used may be those obtained as intermediate products in the process of Specification 1,066,233. The composition itself may be prepared by applying the first stage of said process, employing as the alkali metal source an alkali metal carbonate and mixing the reactants in such a manner that complete reaction does not occur, e.g. by carrying out the reaction at 20 DEG to 50 DEG C. and/or without complete mixing of the reactants. In one method a stream of a liquid condensed phosphoric acid is slowly added to an agitated bed of the carbonate to produce an encapsulated material comprising free acid coated with a conglomerate mass of condensed phosphate and free carbonate. Materials such as alkali metal or alkaline earth metal hydroxides, sulphates, phosphates, other condensed phosphates, or silicates may be incorporated in the composition either by mixing with the reactants or with the final product. In examples, effervescent materials are prepared from condensed phosphoric acid and soda ash, which may contain sodium tripolyphosphate with or without sodium sulphate. The compositions are used as water softeners or in detergent compositions (see Division C5).