Patent GB-1156725-A (GB)
Title: Process for the Encapsulation of Dispersible Materials
IPC: B01J13/08
Filed: 1966-07-12
Abstract: 1,156,725. Coated flexible sheet materials. CIBA Ltd. 12 July, 1966 [2 Aug., 1965], No. 31304/66. Heading B2E. [Also in Divisions B8, C1 and D2]  Microcapsules containing solids, gases or liquid's are formed by finely dispersing the core material in a liquid by means of a "tenside" i.e. a surface active agent, the tenside then being caused to form a shell about each material particle by modifying the dispersion conditions e.g. by adjustment of pH; heating, addition of reactants or catalysts. The cores may be hydrophobic or hydrophilic, the dispersing. liquid being varied correspondingly. Use of tensides eliminates the necessity for maintaining dispersion of core material by agitation during encapsulation.  Suitable tensides are surface-active crosslinkable aminoplasts, preferably etherified methyloilmelamines or corresponding meithylolureas. Tenside forming processes are detailed, an example of which is given below: A mixture of 120 parts of polyethyleneglycol of molecular weight 1540 and 120 parts of a butanolic solution of about 75% dry content of a dimethylolurea - n - butyl ether is heated for 45 minutes at 100‹C under vacuum to produce 224 parts of the tenside. 16 parts of n - butanol pane recovered. The tensides may be dispersed in water, aliphatic and aromatic hydrocarbons and halogenated hydrocarbons such as benzene, toluene, chlorobenzene, tetra and decahydronaphthalene, trichlorethylene and carbon tetrachloride. Shell producing pH adjusting additions include, acetic, formic, citric acids, aluminium sulphate, titanium oxychloride and ammonium salts forming acids in the presence of formaldehyde. Also oxidants capable of oxidizing formaldehyde to formic acid. The process may be used to encapsulate dyestuffs to form coating for copy paper (red fat dyestuff dissolved in tricresylphosphate; dilute alkyl resin lacquer pigmented with channel black; - azo pigment), lubrieating oil and fabric waterproofing agents. In one example of this last, paraffin oil is encapsulated using a tenside based on melamine and the capsule 'mass mixed with an aqueous dispersion of a copolymer formed from acrylic acid isobutyl ester, acrylonitrile and acrylic acid. Also added to the mixture are ammonia and a paraffin wax emulsion in the tenside already used. There results a viscid readily brushable mass which is applied to cotton fabric and hardened at 150‹C to form a water repellant air permeable coating. In another example a solution of monoammionium phosphate is encapsulated and incorporated in a mixture similar to that just described. The process may be used to form a foil like agglomerate of capsules acting as cement which joins two surfaces separated by the foil. In this process, the material used in forming the tenside in the example given above is encapsulated by using a solution of that tenside in water. A butanolic solution of a dimeithylolurea-n-butyl is emulsified in the tenside solution, the emulsion diluted with water and formic acid added. After heating for 30 minutes at 95‹C and cooling to 20‹C the whole is neutralized with ammionia poured out in a thin layer and dried under vacuum to form a flexible foil with a capsule structure. If the foil is heated for 15 minutes at 150‹C., it is cured right through. In other uses, a melamine coated paraffin wax is formed. A curing catalyst is produced by encapsulating ammonium chloride using a melamine as tenside.