N,N-Dimethylaniline → Benzenamine, N,N-dimethyl-, sulfate (1:1)

The SO2 -lean and dimethyl aniline-enriched effluent gas from absorber section 5 of tower 6 which contains about 0.15 percent by volume SO2 and about 800-900 p.p.m. of gaseous dimethyl aniline, passes upwardly sequentially through sulfurous acid scrubbing section 9 and sulfuric acid scrubbing section 10. A tail gas containing 0.05 percent by volume SO2 and virtually free of gaseous dimethyl aniline is withdrawn from sulfuric acid scrubbing section 10 through line 18. Substantially pure SO2 gas bled off the upper SO2 gas-containing space in liquefied SO2 surge tank 59 and aqueous ammonium sulfate solution withdrawn from the lower portion of regenerator section 33 of tower 31 are separately supplied into scrubbing section 9 through lines 19 and 20 respectively. The SO2 gas is supplied into the lower portion of scrubber section 9 below the lowermost tray therein through line 19 at a volumetric velocity or flow rate of 30 SCFM (dry) and at a temperature of 80°F. The liquid aqueous ammonium sulfate solution is pumped into the upper portion of scrubbing section 9 above the uppermost tray therein through line 20 at a temperature of 80 F. and a flow rate of 26 g.p.m. and at flow rates of ammonium sulfate and water contained therein of 13.0 lbs/minute and 208 lbs/minute respectively. The uprising SO2 gas in scrubbing section 9 is dissolved in and reacts with the water of the downwardly flowing aqueous ammonium sulfate to form in scrubbing section 9 a dilute sulfurous acid-and ammonium sulfate-containing aqueous solution. A major portion, i.e. more than 50 percent, of the gaseous dimethyl aniline present in the gas is removed from the gas in scrubbing section 9 by reaction with the sulfurous acid in the presence of the ammonium sulfate to form dimethyl aniline sulfite. The aqueous sulfurous acid-and ammonium sulfate-containing scrubbing solution also containing the thus-formed dimethyl aniline sulfite is withdrawn from the lowermost tray in scrubber section 9 through line 62 at a temperature of 80°F. and passed at a flow rate of 34.8 g.p.m. and at flow rates of SO2, SO4 and dimethyl aniline contained therein of 5.0 lbs/minute, 0.6 lb/minute and 8.6 lbs/minute respectively to collection tank 63. The uprising effluent gas leaving scrubbing section 9 contains, by volume, about 60 to 80 p.p.m. of residual gaseous dimethyl aniline and about 0.07-0.10 percent SO2, and the gas enters and passes upwardly within sulfuric acid scrubbing section 10. Dilute liquid aqueous sulfuric acid solution of 10 percent sulfuric acid concentration is supplied at a flow rate of 0.4 g.p.m. and at ambient temperature into the sulfuric acid scrubbing section 10 above the uppermost tray therein. Substantially all of the residual dimethyl aniline is removed from the gas in scrubbing section 10 by reaction with the sulfuric acid of the dilute sulfuric acid solution to form dimethyl aniline sulfate. Dilute liquid aqueous sulfuric acid solution containing the thus-formed dimethyl aniline sulfate is removed from the lowermost tray in scrubbing section 10 at a temperature of 80°F. and passed through line 64 at a flow rate of 16.4 g.p.m. and at flow rates of dimethyl aniline, H2So4 and water contained therein of 41 lbs/minute, 15.6 lbs/minute and 141.2 lbs/minute respectively to recycle tank 65. A major portion of the dilute aqueous sulfuric acid solution containing the dimethyl aniline sulfate in tank 65 is withdrawn from a lower portion of tank 65 and pumped at a temperature of 80°F. and at a flow rate of 16 g.p.m. as recycle scrubbing solution through line 68 and introduced into scrubber section 10 above the uppermost tray therein. A minor or relatively small portion of the dilute sulfuric acid solution containing dimethyl aniline sulfate is withdrawn from an upper portion of recycle tank 65 through line 66 at a temperature of 80°F. and passed through line 66 at a flow rate of 0.4 g.p.m. to collection tank 63.