Prepn. of glycerol di:chlorohydrin(s) - from allyl chloride aq. emulsion and chlorine, continuously in tubular reactor under adiabatic conditions

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.