Polycondensation of epoxy alcohols with polyhdric alcohols and thermal condensation to form polyethercyclicpolyols
AssigneeShell Oil Company
InventorsHarry Frank, George C. Blytas, Anne H. Zuzich
Life of this patent
Estimating the term…
Abstract
Polyethercyclicpolyols are prepared by thermally condensing a polyol having at least three hydroxyl groups of which at least two of the hydroxyl groups are vicinal, precursors of the polyol, cyclic derivatives of the polyol, or mixtures thereof, and controlling process conditions to avoid substantial undesirable degeneration. Lower molecular weight polyethercyclicpolyols are polycondensed with epoxy alcohols to form higher molecular weight polyethercyclicpolyols.
Claims31
A method for preparing polyethercyclicpolyol by copolymerization and thermal condensation, comprising:
- (a) heating a reaction mixture comprising a reactant selected from the group consisting of (1) a polyol having at least three hydroxyl groups of which at least two of the hydroxyl groups are vicinal, (2) precursors of the polyol, (3) cyclic derivatives of the polyol, and (4) mixtures thereof, said heating initiating the thermal condensation;
- (b) removing water formed during the thermal condensation;
- (c) continuing the thermal condensation until at least 1.05 moles of water per mole of reactant are removed, wherein the condensation goes to completion without incurring substantial undesirable degeneration;
- and
- (d) prior to the condensation going to completion, admixing an epoxy alcohol with the reaction mixture.
A method for preparing polyethercyclicpolyol by copolymerization and thermal condensation, comprising:
- (a) heating a reaction mixture comprising a reactant selected from the group consisting of (1) a polyol having at least three hydroxyl groups of which at least two of the hydroxyl groups are vicinal, (2) precursors of the polyol, (3) cyclic derivatives of the polyol, and (4) mixtures thereof, said heating initiating the thermal condensation;
- (b) removing water formed during the thermal condensation;
- (c) continuing the thermal condensation which is initially endothermic, until the condensation becomes essentially thermally balanced, and prior to the reaction becoming exothermic which would lead to substantial undesirable degeneration;
- and
- (d) prior to the condensation becoming essentially thermally balanced, admixing an epoxy alcohol with the reaction mixture.
A method for preparing polyethercyclicpolyol by copolymerization and thermal condensation, comprising:
- (a) heating a reaction mixture comprising a reactant selected from the group consisting of (1) a polyol having at least three hydroxyl groups of which at least two of the hydroxyl groups are vicinal, (2) precursors of the polyol, (3) cyclic derivatives of the polyol, and (4) mixtures thereof, said heating initiating the thermal condensation;
- (b) removing water formed during the thermal condensation;
- (c) continuing the thermal condensation to completion while controlling the temperature and pressure of the reaction within 250.degree.-295.degree. C. and 40 mm-80 mm of mercury to avoid substantial undesirable degeneration and to maximize molecular weight;
- and
- (d) prior to the thermal condensation going to completion, admixing an epoxy alcohol with the reaction mixture.
A method for preparing polyethercyclicpolyol by copolymerization and thermal condensation, comprising:
- (a) heating a reaction mixture comprising a reactant selected from the group consisting of (1) a polyol having at least three hydroxyl groups of which at least two of the hydroxyl groups are vicinal, (2) precursors of the polyol, (3) cyclic derivatives of the polyol, and (4) mixtures thereof, said heating initiating the thermal condensation;
- (b) removing water formed during the thermal condensation;
- (c) continuing the thermal condensation while adding additional reactant in such a manner that the reaction proceeds to completion at a rate faster than the additional reactant is being incorporated, thereby maximizing molecular weight of the polyethercyclicpolyol;
- and
- (d) prior to the thermal condensation going to completion, admixing an epoxy alcohol with the reaction mixture.
A method for preparing polyethercyclicpolyol by copolymerization and thermal condensation, comprising:
- (a) heating a reaction mixture comprising a basic catalyst and a reactant selected from the group consisting of (1) a polyol having at least three hydroxyl groups of which at least two of the hydroxyl groups are vicinal, (2) precursors of the polyol, (3) cyclic derivatives of the polyol, and (4) mixtures thereof, said heating initiating the thermal condensation;
- (b) removing water formed during the thermal condensation;
- (c) continuing the thermal condensation to completion while controlling the pH of the reaction mixture within a starting pH of 5.0-13.5 and a final pH of 5.0-9.5 by addition of the basic catalyst;
- and
- (d) prior to the condensation going to completion, admixing an epoxy alcohol with the reaction mixture.
A method for preparing polyethercyclicpolyol by thermal condensation, comprising:
- (a) heating a reaction mixture comprising a reactant selected from the group consisting of (1) a polyol having at least three hydroxyl groups of which at least two of the hydroxyl groups are vicinal, (2) precursors of the polyol, (3) cyclic derivatives of the polyol, and (4) mixtures thereof, said heating initiating the thermal condensation;
- (b) removing water formed during the thermal condensation;
- (c) continuing the thermal condensation and adding a final quantity of additional reactant to the reaction mixture when the thermal condensation is within at least 90% of completion, thereby buffering the condensation and preventing undesirable degeneration;
- and
- (d) prior to the condensation going to completion, admixing an epoxy alcohol with the reaction mixture.
Dependencies are inferred from the claim text.