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filingDate 1945-10-30-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationDate 1948-06-23-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber GB-603810-A
titleOfInvention Hydrolysis of acetone auto-condensation products
abstract Acetone and isophorone are made from acetone auto-condensation products which do not contain more than 10 per cent of isophorone or lower-boiling compounds, by heating such products with an aqueous solution containing .5 to 25 per cent of an alkali metal hydroxide at a temperature of 130-235 DEG C. The hydroxide is preferably sodium or potassium hydroxide, or may be lithium, rubidium or caesium hydroxides or mixtures thereof. The preferred concentration of hydroxide is 1-10 per cent, and the preferred temperature range 170-220 DEG C. and higher ketones of the general formula C3nH4n+2O, which may be used separately or together, and may be prepared by autocondensation of acetone with alkaline catalyst (see Specification 583,863), acids (e.g. hydrochloric and sulphuric), by vapour phase methods as described in Specification 525,142, or by catalysts such as alkaline earth hydroxides, sodium alcoholate, calcium carbide, sodium amide. The process may be batchwise or continuous, and the reactor may be fitted with a fractionating column, whereby an azeotropic mixture of acetone and water may be withdrawn. In examples: (1) acetone was heated under pressure with aqueous potassium hydroxide, and the organic products obtained were fed to a continuous distillation column under pressure together with more potassium hydroxide solution to reconvert the diacetone alcohol and mesityl oxide formed to acetone. The organic products were then fractionally distilled, and the fraction of higher boiling point than isophorone was heated under pressure with potassium hydroxide, which treatment effected an increase in the proportion of acetone and isophorone of about 13 per cent. In a further example: (2) a fraction of the high-boiling ketones boiling between 123-142 DEG C. at 10 mm. pressure was heated under pressure with potassium hydroxide solution, the treatment causing about 31.5 per cent hydrolysis to acetone and isophorone.
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