Patent GB-573308-A (GB)
Title: Improvements in and relating to the preparation, treatment and application of resins
IPC: C08G75/16
Filed: 1941-10-23
Abstract: Resins for lacquers and adhesives are made by heating in aqueous media (a) an alkali or alkaline earth disulphide, (b) ethylene dichloride, b ,b 1 - dichloroethyl sulphide, b ,b 1 - dichlorethyl disulphide or a ,a 1-dichloromethyl ether, and (c) glycerol a ,g -dichlorohydrin, the molar proportion of (b) and (c) being between 5 and 50 per cent and 50 and 95 per cent respectively. Rubber-like resins are similarly made from the disulphide, (a) ethylene dichloride, b ,b 1 - di - chloroethyl sulphide, b ,b 1-dichlorethyl disulphide, b 1,b -dichloroethyl sulphone or a ,a 1-dichloromethyl ether, and (b) glycerol a ,g -dichlorohydrin or b ,b 1-dichloroethyl sulphoxide, the molar proportions of (a) and (b) being between 5 and 75 per cent and 25 and 95 per cent, respectively.  Plastic or syrupy resins are similarly made from the disulphide, (a) ethylene dichloride, b ,b 1-dichloroethyl sulphide, b ,b 1-dichlorethyl disulphide, b ,b 1-dichloroethyl sulphone, b ,b 1-dichloroethyl sulphoxide, a ,a 1-dichloromethyl ether, glycerol a ,g -dichlorohydrin, a ,g -dichloroacetone or trichloroethyl phosphate, and (b) b -hydroxy g -chloropropyl monochloracetate, b  - chloroethyl monochloroacetate, ethylene bismonochloroacetate, diethylene bismonochloracetate, thiodiethylene bismonochloracetate, glycerol trimonochloracetate, mannitol bismonochloracetate, b ,b 1 - dichlorethylether, trichloroethyl phosphate and a ,g -dichloroacetone, the molar proportions of (a) and (b) being between 5 and 60 per cent and 40 and 95 per cent, respectively.  Hard resins are similarly made from the disulphide and two different substances from the group ethylene dichloride, b ,b 1-dichlorethyl sulphide, b ,b 1-dichloroethyl disulphide, b ,b 1-dichloroethyl sulphone and a ,a 1-dichloromethyl ether, the molar proportions being between 5 and 95 per cent.  Dispersing agents, e.g. zinc oxide or magnesium hydroxide and water-dispersible colloids may be added to the disulphide solution prior to reaction.  The halogen compound mixture may be emulsified with sodium oleate before reaction.  An emulsifying agent may also be added to the ingredients for or during the preparation of the aqueous disulphide solution.  The resin may be heated after formation in the resulting aqueous liquid.  The resins may be purified by washing with a non-solvent, e.g. benzene or ethanol or a partial solvent, e.g. acetone or dioxan.  Adhesives, lacquers, or putties may be made by dissolving the resin in cyclohexanone, with or without diluents, e.g. acetone, dioxan or chlorinated bodies.  The resins may be compounded with rubber, stearic acid, fillers, e.g. zinc oxide and gas black and softening agents, e.g. tetramethylthiuram disulphide and mercaptobenzthiazole disulphide and vulcanized.  The products may be coated on to fabrics, e.g. in the form of aqueous dispersions and thereafter calendered and vulcanized. In a typical example, crystalline sodium sulphide, sulphur and sodium oleate are dissolved in water and the mixture heated to form sodium disulphide.  A mixture of ethylene dichloride and glycerol a ,g -dichlorohydrin emulsified with aqueous sodium oleate is added and the mixture heated under reflux.  The liquid is decanted, the resin coagulated with hydrochloric acid, comminuted and washed with dilute aqueous caustic soda, water and finally refluxed with acetone.  The product is tough, hard, and elastic and soluble in cyclohexanone. Specifications 302,270, [Class 2 (iii)], 446,173, 450,218 and 452,441 and U.S.A. Specifications 1,890,191 and 2,026,875 are referred to.