| 摘要 |
#CMT# #/CMT# Preparing epichlorhydrin comprises reacting a mixture of 1,3-dichloro-2-propanol (30 wt.%) and 2,3-dichloro-1-propanol with a basic compound in a liquid reaction medium to form an epichlorhydrin and an salt and subjecting a part of the liquid reaction medium of reacting step to a settling operation, which separates at least a first fraction containing the majority of epichlorhydrin and a second fraction containing the majority of salt, where the majority of epichlorhydrin and majority of salt are present in the part of the reaction medium of the reacting step before the settling operation. #CMT#USE : #/CMT# The process is useful for preparing epichlorhydrin (claimed). #CMT#ADVANTAGE : #/CMT# The process reduces consumption of vapor and the equipment size, hence cost effective, and saves energy. The process is carried out without pretreatment in other fabrications. #CMT#INORGANIC CHEMISTRY : #/CMT# Preferred Components: The basic compound of the reacting step is oxide, hydroxide, carbonate, hydrogenocarbonate, phosphate, hydrogenophosphate and alkaline borate, alkaline earth or their solutions, aqueous suspensions or mixtures. The salt of the reacting step is chloride, sulfate, hydrogenosulfate, phosphate, hydrogenophosphate and alkaline borates and/or alkaline earth. #CMT#ORGANIC CHEMISTRY : #/CMT# Preferred Process: The part of the reaction medium of reacting step is subjected to pretreatment of the settling operation of the subjecting step, where the treatment is heating, cooling, diluting, adding salt, adding an acid compound (preferably hydrogen chloride) or combinations of at least two of them. The reacting and subjecting steps are done in the absence of organic solvent, where the differences in density between the first and second fraction settled in subjecting step is at least 0.001. The reacting and subjecting steps are carried out continuously. The reacting step is conducted at a temperature of 0-100[deg] C, under a pressure of 0.01-20 bar, for 1-240 minutes in discontinuous mode or for a residence time of 1-240 minutes, and the subjecting step is conducted at a temperature of 0-100[deg] C, under a pressure of 0.01-20 bar, for 5-120 minutes in discontinuous mode or for a residence time of 5-120 minutes. The process comprises adding water in reacting step, between the reacting step and the subjecting step and/or the subjecting step. Preferred Components: The part of dichloropropanol of reacting step is obtained by reaction of glycerol and a chlorinating agent containing hydrogen chloride. The part of the salt of the second fraction settled in subjecting step is not produced during the reacting step but is added in reacting step, and in which a filtration step is carried out between the reacting and subjecting steps. The first fraction separated in the subjecting step comprises at least 100 g of epichlorhydrin/kg of the first fraction and the second fraction separated in the subjecting step comprises at least 50 g of salt/kg of the second fraction. #CMT#EXAMPLE : #/CMT# 1,3-Dichloro-2-propanol (258.76 g) was charged in thermostat reactor (1 l). Then aqueous solution of sodium hydroxide (1 g) was added to the obtained mixture, at 25[deg] C under vigorous agitation for 20 minutes. The obtained mixture was transferred to a separating funnel to form the first fraction (179.39 g) having a density of 1.185-488.95 and second fraction (488.95 g) having a density of 1.182, where the first fraction contained majority of epichlorhydrin (94 %) and second fraction contained majority of salt compared to the basic compound. |
