反应详情

The reaction is effected in a reactor arrangement of a first reactor of type E with a downstream reactor of type C. Before the start of the reaction, the first reactor is filled with a solution of 23.1% by weight of tert-amyl hydroperoxide, 9.9% by weight of potassium hydroxide and 8.3% by weight of sodium hydroxide in water. 20.2 kg/h of a solution of 88% by weight of tert-amyl hydroperoxide in water, 15.8 kg/h of a solution of 45% by weight of potassium hydroxide in water, 12.2 kg/h of a solution of 50% by weight of sodium hydroxide in water, 24.4 kg/h of water and 18.0 kg/h of pivaloyl chloride are then fed to the first reactor. Cooling with cooling water keeps the internal temperature in the first reactor at 18° C. and in the second reactor at 10° C. The reaction mixture withdrawn from the second reactor is mixed with 8.8 kg/h of isododecane and the organic phase is removed. The organic phase is washed successively with an 8% by weight solution of sodium hydroxide in water, with a solution of 10% by weight of sodium sulphite in water comprising acetic acid and with a 1% by weight solution of sodium hydrogencarbonate in water, and then dried by stripping in a packed column at 20° C. and 45 mbar. 35.0 kg/h of a 75% by weight solution of tert-amyl peroxypivalate in isododecane are obtained (93.5% based on pivaloyl chloride). The space-time yield is 2.82 kg/l·h.

1. customThe reaction is effected in a reactor
2. customBefore the start of the reaction
3. customat 18° C.
4. customat 10° C
5. customThe reaction mixture withdrawn from the second reactor
6. additionis mixed with 8.8 kg/h of isododecane
7. customthe organic phase is removed
8. washThe organic phase is washed successively with an 8% by weight solution of sodium hydroxide in water, with a solution of 10% by weight of sodium sulphite in water
9. dry with materialwith a 1% by weight solution of sodium hydrogencarbonate in water, and then dried
10. customby stripping in a packed column at 20° C.