FIELD: chemistry.
SUBSTANCE: invention relates to an improved method for ammonolysis of chlorohydrocarbons by reacting chlorohydrocarbons and ammonia to obtain a solution of aminochlorohydrates and ammonium chloride, neutralising that solution and separating amines. Before the neutralisation step, the solution of aminochlorohydrates and ammonium chloride undergoes at least four-step cooling: at the first step to temperature 20-25°C and holding at that temperature for about 30 minutes, followed by slow cooling at a rate of 4-5°C/h to temperature 10°C at the second step and holding at that temperature for 2 hours while stirring, further cooling at a rate of 10°C/h to temperature minus 10°C at the third step and holding for 1 hour and cooling at the fourth step to temperature minus 25°C and holding for 1 hour. Further, the solution of aminochlorohydrates is separated from the crystallised ammonium chloride by filtration and taken to the neutralisation step, and ammonium chloride is purified. At the purification step, ammonium chloride is washed with hydrochloric acid with weight ratio of HCl of 20-36% and weight ratio of ammonium chloride to acid equal to 1:2, followed by holding the mixture until formation of layers, separating ammonium chloride from hydrochloric acid and drying until all moisture is removed.
EFFECT: method reduces the amount of sodium chloride formed at the step for neutralising products of ammonolysis of chlorohydrocarbons, reduces the amount of waste water, increases energy efficiency of the process, and also increases output of amines and enables to obtain an additional commercial product in form of ammonium chloride.
6 cl, 5 ex
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Authors
Dates
2012-08-20—Published
2010-12-29—Filed