Patent GB-619356-A (GB)
Title: Improvements in or relating to anion exchange resins
IPC: B01J41/12
Filed: 1946-12-04
Abstract: A chlorinated paraffin wax and an alkylene polyamine containing at least one nitrogen atom for each two carbon atoms it contains are reacted at between 110 DEG  and 160 DEG  C. for at least 6 hours to give an anion exchange or acid absorbing resin.  The wax preferably contains between 40 and 55 per cent of chlorine, the weight of alkylene polyamine is preferably at least twice the weight of the wax and the initial reaction temperature is preferably between 110 DEG and 140 DEG  C., although it may be allowed to rise at a later stage. The reaction mixture may contain diluents or solvents such as benzene, toluene, trichlorethylene, ethylene dichloride, water, ethanol, amyl alcohol and diethyl carbitol or excess polyamine may act as diluent.  The reaction is normally carried out at atmospheric pressure, but superatmospheric pressure, as up to 15 to 16 lbs. sq. in., may be used.  Alkylene polyamines specified are ethylene diamine, diethylene triamine, triethylene tetramine, tetraethylene pentamine, piperazine, tetramethylene diamine and polyvinylamine.  A mixture of alkylene polyamines may be made by heating together ethylene dichloride with an excess of aqueous ammonia under pressure, neutralizing the liberated acid, distilling off ammonia and most of the water, extracting the amines with an organic solvent which is then distilled off.  Also ethyleneimine may be polymerized to provide suitable polyamines.  In examples: (1) aqueous alkylene polyamines obtained by reacting ethylene dichloride and aqueous ammonia were boiled at 125 DEG  C., under reflux with chlorinated paraffin wax for 24 hours, the mixture being partly diluted with water after 6 hours; (2) ethylene diamine monohydrate was reacted for 30 hours with chlorinated paraffin wax; (3) an alkylene polyamine mixture was reacted for 36 hours with chlorinated paraffin wax, the temperature being first 125 DEG  C., and later 140 DEG  C.ALSO:A chlorinated paraffin wax and an alkylene polyamine containing at least one nitrogen atom for each two carbon atoms it contains are reacted at between 110 DEG  and 160 DEG  C. for at least 6 hours to give an anion exchange or acid absorbing resin.  The wax preferably contains between 40 and 55 per cent of chlorine, the weight of alkylene polyamine is preferably at least twice the weight of the wax and the initial reaction temperature is preferably between 110 DEG  and 140 DEG  C., although it may be allowed to rise at a later stage.  The reaction mixture may contain diluents or solvents such as benzene, toluene, trichlorethylene, ethylene dichloride, water, ethanol, amyl alcohol and diethyl carbitol or excess polyamine may act as diluent. The reaction is normally carried out at atmospheric pressure, but superatmospheric pressure, as up to 15 to 16 lbs. sq. in., may be used.  Alkylene polyamines specified are ethylene diamine, diethylene triamine, triethylene tetramine, tetraethylene pentamine, piperazine, tetramethylene diamine and polyvinylamine.  A mixture of alkylene polyamines may be made by heating together ethylene dichloride with an excess of aqueous ammonia under pressure, neutralising the liberated acid, distilling off ammonia and most of the water, extracting the amines with an organic solvent which is then distilled off.  Also ethyleneimine may be polymerised to provide suitable polyamines.  In examples: (1) aqueous alkylene polyamines obtained by reacting ethylene dichloride and aqueous ammonia were boiled at 125 DEG  C., under reflux with chlorinated paraffin wax for 24 hours, the mixture being partly diluted with water after 6 hours; (2) ethylene-diamine monohydrate was reacted for 30 hours with chlorinated paraffin wax; (3) an alkylene polyamine mixture was reacted for 36 hours with chlorinated paraffin wax, the temperature being first 125 DEG  C., and later 140 DEG  C.