反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
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 24.4% by weight of tert-butyl hydroperoxide and 12.7% by weight of potassium hydroxide in water. 33.6 kg/h of a solution of 70% by weight of tert-butyl hydroperoxide in water, 27.2 kg/h of a solution of 45% by weight of potassium hydroxide in water, 38.0 kg/h of water and 18.4 kg/h of isobutyroyl chloride are then fed to the first reactor. Cooling with cooling water keeps the internal temperature in the first reactor at 11° C. and in the second reactor at 12° C. The reaction mixture withdrawn from the second reactor is mixed with 8.0 kg/h of isododecane and the organic phase is removed.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 47 mbar. 33.4 kg/h of a 75% by weight solution of tert-butyl peroxyisobutyrate in isododecane are obtained (92.8% based on isobutyroyl chloride). The space-time yield is 2.69 kg/l·h.
WORKUP
后处理
- customThe reaction is effected in a reactor
- customBefore the start of the reaction
- customat 11° C.
- customat 12° C
- customThe reaction mixture withdrawn from the second reactor
- additionis mixed with 8.0 kg/h of isododecane
- customthe organic phase is removed
- 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
- dry with materialwith a 1% by weight solution of sodium hydrogencarbonate in water, and then dried
- customby stripping in a packed column at 20° C.