Patent GB-748710-A (GB)
Title: Improved process for the purification of dimethylterephthalate
IPC: C07C69/82
Filed: 1953-06-24
Abstract: A process for the purification of dimethyl terephthalate comprises the steps of melting the crude terephthalate, submitting it to distillation in the presence of a stream of an inert gas, said gas entraining the dimethyl terephthalate as vapour, partially refluxing said vapour and subsequently cooling said gas mixed with terephthalate vapour to return said vapour directly to the solid state, thereby separating it from said gas.  The process may comprise heating the crude terephthalate in a still, entraining the vapours evolved by means of a stream of inert gas, passing the inert gas and entrained vapours through a heated rectifying column comprising a number of bubble plates thereby partly to reflux said vapours and thereafter rapidly cooling said gas and the vapours entrained thereby to a temperature below the melting-point of dimethyl terephthalate in a chamber wherein said terephthalate is thus separated from said gas and collected in the solid state.  In the apparatus in Fig. 1 (see Group III) a stream of inert gas, e.g. nitrogen, is passed into or over the surface of a molten mass of the crude ester in a still.  The mixture of gas and vapour rise through a heated column containing plates or trays, e.g. bubble caps, and part of the terephthalate is refluxed and the remainder entrained by the gas is returned directly to the solid state by passing the mixture into a cooled chamber.  The inert gas is preferably recycled to the still by a pump.  In Fig. 3 (not shown) the variation of the vapour pressure of dimethyl terephthalate with temperature is shown.ALSO:<PICT:0748710/III/1> A process for the purification of dimethyl terephthalate comprises the steps of melting the crude terephthalate, submitting it to distillation in the presence of a stream of an inert gas, said gas entraining the dimethyl terephthalate as vapour, partially refluxing said vapour and subsequently cooling said gas mixed with terephthalate vapour to return said vapour directly to the solid state, thereby separating it from said gas.  The process may comprise heating the crude terephthalate in a still, entraining the vapours evolved by means of a stream of inert gas, passing the inert gas and entrained vapours through a heated rectifying column comprising a number of bubble plates thereby partly to reflux said vapours and thereafter rapidly cooling said gas and the vapours entrained thereby to a temperature below the melting point of dimethyl terephthalate in a chamber wherein said terephthalate is thus separated from said gas and collected in the solid state.  In the apparatus (Fig. 1) a stream of inert gas, e.g. nitrogen; is passed through pipe 12 into or over the surface of a molten mass of the crude ester in vessel 10 provided with heating jacket 11. The mixture of gas and vapour rise through a heated column 14 provided with plates 16 wherein part of the terephthalate is refluxed and the remainder entrained by the gas is returned directly to the solid state by passing the mixture through a heater pipe 17 into a cooled chamber 19.  The inert gas is preferably recycled to the still by a pump 13