Into a 1,000 gallon, jacketed, glass-lined reactor equipped with baffles and a
two-speed (67 and 135 rpm) reversed impeller is introduced 200 g of
Richonate 60B (a 60% aqueous slurry of sodium salts of alkylbenzenesulfonic
acids) and 364 liters of deionized water, followed by 90.5 kg of
tetraethylenepentamine rinsed in with 5 gallons of toluene. The solution is
stirred at the low speed and then 500 gallons of toluene are added to form a
dispersion. To the stirred dispersion is added 109 kg of epichlorohydrin, rinsed
in with 5 gallons of toluene, and the resulting mixture is heated at reflux for
two hours. The reaction mixture is cooled to about 20°C and then treated with
58.5 kg of a filtered 50% aqueous solution of sodium hydroxide. The mixture
is removed from the reactor and filtered, and the copolymer is collected and
dried by treating it first with hot (75°C to 80°C) filtered nitrogen and then
with an 80°C air stream. The resulting crude product is returned to the
reactor, washed extensively with filtered deionized water (at the low speed),
dried with an 80°C air stream and blended until homogeneous to give about
155 kg of a dry tetraethylenepentamine-epichlorohydrin copolymer
hydrochloride, particle diameter 0.002-0.02 inch.
