Patent GB-917831-A (GB)
Title: A process for treating reinforcing silica
IPC: C09C1/30
Filed: 1961-06-15
Abstract: Reinforcing, hydrophobic silica, suitable for use as a filler in rubber and as a flatting agent in paints, may be prepared by contacting in an organic medium, silica, an organosilicon compound, and a third compound which is an amino compound, a carboxylic acid salt, a quaternary ammonium hydroxide or a phosphoric acid salt.  The silica used (100 parts) has a surface area of at least 50 square metres gm-1.  The organosilicon compound (1,8 parts) contains in each molecule an average of from 0,1 to 2 hydroxy and/or alkoxyl radicals per silicon atom and 1 to 3 silicon bonded organic radicals selected from substituted monovalent hydrocarbon radicals containing less than 13 carbon atoms (preferably perfluoralkylethyl radicals) and monovalent hydrocarbon radicals.  Not more than 3 silicon atoms have attached thereto as the only organic radicals, 2 monovalent aliphatic hydrocarbon radicals per silicon atom, any remaining silicon valencies being satisfied by siloxane oxygen atoms.  The third compound (at least 0,01 parts) may be (i) an amino compound (having a basic dissociation constant in dilute aqueous solution of at least 10-7 at 25 DEG C.) or (ii) a quaternary p  ammonium hydroxide or (iii) a salt of phosphoric acid and a basic amino compound or (iv) a carboxylic acid salt of a substance selected from a basic amino compound, a quaternary ammonium hydroxide, or a metal ranging from lead to manganese inclusive in the electromotive series of metals. The organic solvents which may be employed include, hydrocarbons, halogenohydrocarbons, alcohols, ethers, esters, nitriles and amides. It is preferred to disperse the silica with the organosilicon compound and the third compound in the organic solvent, and agitate until a minimum viscosity is attained.  The solvent can be removed, preferably by evaporation, whereupon if the silica is to be used as a rubber filler, it is heated to about 150 DEG C. to remove any excess compounds of the third type.  The silica thus produced, when incorporated as a filler into silicone rubber improves the physical properties of the rubber; it may also be used for thermal insulation and as a flatting agent for paint.  According to examples (1) phenyldimethylethoxy silane and phenylmethyldimethoxy silane were added to separate portions of fume silica and n-hexylamine in the solvent toluene.  The samples were then agitated from 1 to 4 days until an essentially minium viscosity was reached, when the toluene was evaporated off and the remaining fillers were heated at 150 DEG C. for 4 hours; (4) 3,3,3-trifluoropropylmethyldimethoxy silane was added to fume silica and n-hexylamine in the solvent aceto-nitrile and treated as in (1) above; (6) includes references to lead naphthenate, cobalt octoate, dibutyl tin-dibenzoate and dibutyl tin dilaurate; (7) refers to the use of triethylamine, ethylenediamine, n-methylbutylamine, benzylamine and piperazine; (8) refers to n-hexylamine octoate, di-2-ethylhexylamine acetate, trimethylamine stearate, triphenylsilpropylamine formate, ethylene diamine di-hexoate, ammonium stearate, 1,2-aminopropane phenylphosphate, eicosylamine phosphate, benzyltrimethylammonium hydroxide and phenyltrimethylammonium 2-ethylhexoate.  Specification 684,296 and 716,536 are referred to.ALSO:Reinforcing, hydrophobic silica suitable for use as a filler in silicone rubbers is prepared by contacting in an organic medium, fume silica, an organosilicon compound and a third compound which is an amino compound, a carboxylic acid salt, a quaternary ammonium hydroxide or a phosphoric acid salt (see Group III). Examples refer to mixtures of the above prepared fillers with conventional rubber forming silicones and dichlorobenzoyl peroxide. Specifications 684,296 and 716,536 are referred to.