Hydrochloric Acid → HCID 18959084, compound

Participants

Reaction Steps

Before the start of the reaction, the loop reactor is filled with a solution of 25.8% by weight of tert-butyl hydroperoxide and 16.4% by weight of potassium hydroxide. Initially 24.6 kg/h of a solution of 70% by weight of tert-butyl hydroperoxide in water, 24.0 kg/h of a solution of 45% by weight of potassium hydroxide in water, 17.4 kg/h of water and 24.0 kg/h of 2-ethylhexanoyl chloride are then fed to the loop reactor. Cooling with cooling water keeps the internal temperature at 35° C. in the loop reactor and at 27° C. in the stirred cell reactor. The partial neutralization is effected with 5.4 kg/h of 31% by weight hydrochloric acid with addition of 6.0 kg/h of water at a temperature of 18° C. The organic phase is extracted with 26.0 kg/h of a 15% by weight aqueous solution of potassium hydroxide. This affords 29.2 kg/h of aqueous extract comprising 10.8% by weight of tert-butyl hydroperoxide and 13.4% by weight of potassium hydroxide, which are feeded into the loop reactor. From the time at which the aqueous extract is recycled into the loop reactor, the metered addition of the feedstocks is changed to 20.0 kg/h of a solution of 70% by weight of tert-butyl hydroperoxide in water, 15.4 kg/h of a solution of 45% by weight of potassium hydroxide in water and 1.4 kg/h of water. After the extraction, the organic phase is washed with 36.0 kg/h of a solution of 1% by weight of sodium sulphite and 0.2% by weight of sulphuric acid, and dried by stripping at 33° C. and 40 mbar. 31.6 kg/h of tert-butyl peroxy-2-ethylhexanoate are obtained with a purity of 99.3% (98.5% yield based on 2-ethylhexanoyl chloride).

Provenance & Evidence