Patent GB-859709-A (GB)
Title: Process for the manufacture of stable aqueous resin emulsions of the oil-in-water type
IPC: D06P1/56
Filed: 1958-03-05
Abstract: A solution in an alcohol of 3-7 carbon atoms having at least a limited miscibility with water, of an aminoplast etherified with the same alcohol is extracted with a liquid which does not dissolve the etherified aminoplast but which removes the alcohol from it, and the alcohol-free etherified aminoplast is then emulsified in water with the aid of an emulsifying agent.  The aminoplast is formed from formaldehyde and urea, melamine, thiourea, guanidine, dicyandiamide, biuret, or formo-, aceto or benzoguanamine.  Suitable alcohols are propanol, n-butanol, amyl, hexyl, or benzyl alcohol or cyclohexanol. The preferred extracting agent is water.  Benzine, or a mixture of benzine and water may be used.  Extraction may be counter-current and continuous or may be effected in successive stages e.g. in a Werner-Pfleider mixer.  Using water the extract is desirably saturated with alcohol which may then be recovered.  The final stages of the extraction may be at raised temperature.  The extracted resin may be dissolved e.g. in a hydrocarbon, halogenated hydrocarbon, higher alcohol ether, ketone or ester to facilitate emulsification. High boiling esters which are plasticizers may be used.  Such a solvent may be added to the resin before or during an extraction with water.  Suitable emulsifying agents are soaps, sulphoricinoleates; fatty alcohol sulphonates; salts or quaternary compounds of high molecular weight amines; ethylene oxide condensates of compounds containing reactive hydrogen such as fatty acids, fatty acid amides of at least 8 carbon atoms, oleyl amine, mercaptans, octadecyl-, oleyl or hydroabietyl alcohol, isohexyl-, octyl-, dodecyl or octadecyl phenol; reaction products of polyisocyanates with such ethylene oxide condensates (Specification 822,504); proteins or their condensates with alkylene oxides or with fatty acids.  The suspensions may be mixed with aqueous dispersions of homo- or co-polymers, matting or hydrophobic agents, methylol compounds of urea or melamine, plasticizers, watersoluble thickeners or aqueous emulsions of hydrocarbons.  In Examples (1) a butanol solution of a butylated melamine-formaldehyde condensate is extracted several times with water, and the residual resin heated to 60 DEG C. and emulsified in water with an emulsifier prepared by the action of hexamethylene-, 1, 6-diisocyanate with a compound formed from 1 mol of hydroabetyl alcohol and 200 mols of ethylene oxide.  (2) the residual resin of (1) is dissolved in gasoline and emulsified in water with the aid of a castor-oilethylene oxide adduct.  (3) is similar to (1) the extracted resin being dissolved in dioctyl phthalate before emulsification.  The emulsion is mixed with water, petroleum, or emulsifying agent and a butadiene-styrene copolymer.  (4) A resin solution as in (1) is mixed with dioctylphthate before the extraction with water.  The extraction residue is emulsified as in (1) and the emulsion mixed with an aqueous carbon black dispersion and with the mixed emulsion of Example (3) to give a black textile-printing paste. (5) A cyclohexanol solution of a cyclohexyl ether of a urea-formaldehyde condensate is extracted with water.dissolved in pine oil and emulsified in water (6) A butanol-m-xylene solution of a butylated urea-formaldehyde condensate is extracted with water, the residue dissolved in monochlorbenzene and emulsified in water.  The product is mixed with a cation-active emulsion of a copolymer of n-butyl acrylate and vinyl acetate prepared in presence of a quaternary acrylamide compound.  (7). The extracted resin of Example (3) is mixed with m-xylene and sanga oil and emulsified in water containing casein, urea, thiourea borax and triethanolamine.  (8) A toluene-butanol solution of a butylated benzoguanamine-formaldehyde condensate is extracted with water and the residue emulsified in aqueous trithanolammonium oleate. (9), A butanol solution of a butylated melamine-formaldehyde condensate is extracted with gasoline and the residual resin is dissolved in a mixture of butyl acetate, decahydronaphthalene and dioctyl phthalate, and emulsified. Petroleum may be emulsified into this emulsion.  (10) is similar to the first part of (9). (11) is similar to example (8) using a particular form of extraction apparatus (12) is similar to (1).  (13) A propanol solution of the propyl ether of hexamethylol melamine is extracted with water and the residual resin emulsified.  The emulsions of the invention are suitable as adhesives, as dressing or binding agents for fixing pigments on paper, leather or textiles.ALSO:An apparatus for extracting a solvent from a solution of a resin consists of a vertical tube with inlet and outlet connections at top and bottom to permit water to flow up the tube in countercurrent with the resin solution.  Near the upper end of the tube is a perforated plate subjected to powerful vibrations by an electromagnetic device thus splitting the resin solution into fine particles which collect at the bottom of the tube after removal of the solvent by the water and are removed by an outlet valve.