Patent GB-995351-A (GB)
Title: Particulate cleaning agent and method of preparation thereof
IPC: C08J3/14
Filed: 1961-10-30
Abstract: Abrasive melamine- or melamine-urea-formaldehyde resins consist of rounded particles, or friable agglomerates thereof. The particles have major diameters of 1 to 20 m . Slurries of the particles in pure neutral water have an acid pH.  The particles may have a core of an insoluble substance whose hardness is at least 2 on Moh's scale.  The diameter of the core is 0.5 to 15 m . The molar ratio of formaldehyde to melamine and urea, if any, is 2 : 1 to 4 : 1 and the weight ratio urea to melamine is not more than 4 : 1. The particulate resins are prepared by (1) dissolving in water a melamine- or melamine-urea-formaldehyde condensate and adding to the solution 0 to 90%, by weight of the condensate, of a particulate insoluble substance of hardness at least 2 on Moh's scale and of particle diameter 0.5 to 15 m ; (2) acidifying the solution at a temperature of at least 25 DEG C.; and (3) removing water from the friable gel. The weight ratio of water to condensate and particulate insoluble substance in stages (1) and (2) is 1 : 1 to 1 : 8. If the acid used is an inorganic acid it is added in an amount equivalent to a number of moles of HCl which is 0.2 to 0.5 times the total number of moles of melamine and urea. If the acid is an organic acid or a Bronsted acid it is added in an amount equivalent to a total number of moles of acetic acid which is 0.35 to 1 times the total number of moles of melamine and urea. Mixtures of acids may be used. The friable gel may be dispersed in water and filtered to remove soluble impurities. The gel may be heat cured. The acidification may be carried out using one or more of e.g. hydrochloric, nitric, sulphuric, phosphoric, hydrobromic, hydriodic, perchloric, acetic, formic, citric, tartaric, lactic, maleic, malonic and gluconic acids and ammonium chloride and sulphate.  Thickening agents, e.g. Irish moss, gum arabic, sodium carboxymethylcellulose and hydroxyethylcellulose, binders, e.g. colloidal magnesium aluminium silicate, and soluble inorganic salts, e.g. NaCl, Na2SO4, KCl, NaNO3, NaF, Cu2Cl2 and cobaltous nitrate may be added to the solution in stage (1). The insoluble substance may be silica, sand, ground glass, quartz, pumice, alumina, silicon carbide, ilmanite, haematite and titanium dioxide.  The particulate resins may be mixed with humectants, e.g. glycerine and sorbitol; sudsers, e.g. sodium lauryl sulphate, sodium coconut monoglyceride sulphonate and the condensation product of dodecyl alcohol with 1 to 6 moles of ethylene oxide; binders, e.g. sodium carboxymethyl cellulose, hydroxyethylcellulose and very high moleculecular weight polyethylene oxides; and sources of fluoride ions, e.g. NaF, KF, NH4F, LiF, FeF2, indium fluoride, palladium fluoride, Na2SiF6, Na2ZnF6, NaBF4, fluorotitanates, SnF2, SnClF, Sn2ClF3, KSnF3 and mono-, di- and tri-ethanol-ammonium fluorides to give dentifrices.  If the fluoride does not provide stannous ions a source thereof, e.g. SnCl2, Sn(NO3)2 may be added. Flavouring and colouring agents and sweetening agents such as saccharin may also be added. The resins may also be used as abrasives in, for example, powdered scouring cleansers, hand soaps, metal polishes, automobile cleaners and scouring pads. Examples are given of the preparation of the particulate resins and of their use in a toothpaste. Specifications 810,345, 848,235, 865,272 and 939,230 are referred to.ALSO:Dentifrices comprise 20 to 50% by weight of rounded particles or friable agglomerates thereof (see Division C3) comprising (A) melamine-formaldehyde resin, wherein the molar ratio of formaldehyde to melamine is 2 : 1 to 4 : 1 or (B) melamine-formaldehyde resin and urea-formaldehyde resin, the weight of urea being up to four times that of the melamine, wherein the molar ratio of formaldehyde to total urea and melamine is 2 : 1 to 4 : 1; the particles having major diameters of 1 to 20m  and imparting an acid pH to a slurry of the particles in pure neutral water.  The particles may have a core of a particulate insoluble substance of hardness at least 2 on Moh's scale and of particle diameter 0,5 to 15m .  The insoluble substance may be silica, sand, ground, glass, quartz, pumice, alumina, silicon carbide, ilmenite, haematite or titanium dioxide.  The dentifrices may also contain humectants, e.g. glycerine and sorbitol; sudsers, e.g. sodium lauryl sulphate, sodium coconut monoglyceride sulphonate and the condensation product of dodecyl alcohol with 1 to 6 moles of ethylene oxide; binders, e.g. sodium carboxymethyl cellulose, hydroxyethyl cellulose and very high molecular weight polyethylene oxides; sources of fluoride ions, e.g. NaF, KF, NH4F, LiF, FeF2, indium fluoride, palladium fluoride, Na2SiF6, Na2ZrF6, NaBF4, fluorotitanates, SnF2, SnClF, Sn2ClF3, KSnF3, and mono-, di- and triethanol - ammonium fluorides; flavourings; colorants and sweetening agents, e.g. saccharin.  If the source of fluoride ions does not provide stannous ions a source thereof, e.g. SnCl2, or Sn(NO3)2, may be added.  Specifications 810,345, 848,235, 865,272 and 939,230 are referred to.