摘要 |
Prepn. of glycerol dichlorohydrins comprises reacting allyl chloride (I) and Cl2 in aq. medium. An aq. emulsion of (I) in a wt. ratio of H2O: (I) of >=25:1 is prepd. by feeding H2O and (I) into a static mixer. The emulsion is continuously fed to the inlet of an elongate tubular reactor. Gaseous Cl2 is continuously fed to the reactor at the inlet and opt. also at >=1 other places. The total molar amt. of Cl2 is molar amt. of (I). Reaction is under adiabatic conditions at 10-50 degrees C at the inlet. Residence time is >=15 secs. and the linear velocity of the mixt. is >=0.5m./sec. High yields are obtainable on a commercial scale. The process is simple. Pref. >=30% of the Cl2 is fed to the inlet of the reactor, and the Cl2 opt. contains =10 vol.% inert gas. The wt. ratio of H2O: (I) is pref. 25-45:1, esp. 35-36:1, and 0.1-1 (esp. 0.2-0.5) wt.% emulsifiers, etc. are opt. added. The velocity of the mixt. in the reactor is pref. 0.5-2 m/sec. and the residence time is 15-45 secs. The product effluent contains 3-5wt.% glycerol dichlorohydrins. Temp. at the inlet is pref. 25 degrees C and there is pref. an over-press of =1 atmos. w.r.t. press. generated by passage of the mixt. |