Reacción #950798

Ecuación de reacción

epichlorohydrin

ethylene glycol

Epichlorohydrin

ethylene glycol

BF3 ethylene glycol

→

polyepichlorohydrin

Epichlorohydrin

Disolventes

water

water

Condiciones de reacción

Tratamiento posterior

1. 1
   Otrofitted with a mechanical stirrer, funnel, condenser
2. 2
   workup.ADDITIONwas added into the reaction mixture
3. 3
   OtroThe organic phase in the flask was then separated from the aqueous phase
4. 4
   Otrothe organic phase was dried at 40° C. under vacuum for one day
5. 5
   workup.ADDITIONby adding the epichlorohydrin to the bulk ethylene glycol containing the catalyst over a period of time in order

Procedimiento

Epichlorohydrin (ECH) was polymerized in bulk in the presence of ethylene glycol as an initiator and a BF3 /ethylene glycol complex as a catalyst. The reaction was conducted in a 2-liter, three-necked flask fitted with a mechanical stirrer, funnel, condenser and thermometer. The reaction was conducted while maintaining the flask in a water bath at 20° C. Epichlorohydrin was slowly added to ethylene glycol containing a complex of BF3 /ethylene glycol at rate of 15 to 40 grams per hour. Following the addition of epichlorohydrin, the reaction mass was held in the water bath at 20° C. for an additional 4 hours. At the end of the reaction period, 300 mL of dionized water was added into the reaction mixture with stirring to inactivate the catalyst. The organic phase in the flask was then separated from the aqueous phase and the organic phase was dried at 40° C. under vacuum for one day. The polymerization temperature was controlled by adding the epichlorohydrin to the bulk ethylene glycol containing the catalyst over a period of time in order to obtain a linear polyepichlorohydrin (PECH) diol having a relatively narrow molecular weight distribution with a polydispersity below about 1.5. The molecular weight of the PECH diol was determined by gel permeation chromatography (GPC). The weight ratios of ECH to glycol, the rate of ECH addition and the temperature of the reaction were varied to demonstrate the effect of these variables on the molecular weight of the resulting PECH. The results are listed in Table 1 below.

Fuente