Thermoset water-in-oil emulsions
AssigneeAshland Oil, Inc.
InventorsRobert H. Leitheiser, Casimir C. Peloza
Life of this patent
Estimating the term…
Abstract
Pumpable or pourable thermosetting water-in-oil emulsions comprising water as the continuous phase and a mixture containing an unsaturated polyester and copolymerizable solvent such as styrene as the continuous phase, wherein polyesters of a molecular weight of about 1800 or more and a peroxide-cobalt-tertiary amine curing system are employed.
Claims33
A method for producing shapeable water-in-resin composition which is polymerizable to a thermoset cellular solid product which comprises forming a pumpable water-in-oil emulsion, comprising water emulsified in an oil phase, by agitating:
- water;
- peroxide catalyst;
- cobalt salt promoter;
- tertiary aromatic amine promoter;
- said cobalt salt promoter and tertiary aromatic amine promoter being present in the oil phase in an amount in the range of about 0.1 to 5% by weight of the oil phase;
- unsaturated polyester which has a mean molecular weight in the range of 1800 to 100,000, said polyester including reaction product of polycarboxylic acid, at least a portion of which is .alpha.,.beta. ethylenically unsaturated, and polyhydric alcohol;
- and ethylenically unsaturated solvent which is copolymerizeable with said polyester;
- the weight ratio of polyester and solvent to water being in the range of 1:10 to 10:1;
- and the weight ratio of polyester to solvent being in the range of 10:1 to 1:10.
A method for producing shapeable water-in-resin composition which is polymerizeable to a thermoset cellular solid product which comprises forming a pumpable water-in-oil emulsion having water emulsified in an oil phase, said emulsion including:
- peroxide catalyst;
- cobalt salt promoter;
- tertiary aromatic amine promoter;
- said cobalt salt promoter and tertiary aromatic amine promoter being present in the oil phase in an amount in the range of about 0.1 to 5% by weight of the oil phase;
- unsaturated polyester which has a mean molecular weight in the range of 1800 to 100,000 and includes reaction product of (A) dicarboxylic acid, at least a portion of which is .alpha.,.beta.-ethylenically unsaturated acid and, as saturated acid, phthalic, isophthalic or terephthalic acid, and (B) dihydric alcohol;
- and ethylenically unsaturated solvent which is copolymerizeable with said polyester;
- the weight ratio of polyester and copolymerizeable solvent to water being in the range of 1:10 to 10:1;
- and the weight ratio of polyester to copolymerizeable solvent being in the range of 10:1 to 1:10.
A method for producing shapeable water-in-resin composition which is polymerizable to a thermoset cellular solid product which comprises:
- forming a pumpable water-in-oil emulsion having water emulsified in an oil phase, by bringing together under vigorous agitation water and an oil phase, said emulsion including peroxide catalyst in an effective amount in the range of 0.001 to 10% by weight of the copolymerizeable solvent referred to below;
- cobalt salt promoter;
- tertiary aromatic amine promoter;
- said cobalt salt promoter and tertiary aromatic amine promoter being present in said oil phase in an amount in the range of about 0.1 to 5% by weight of the oil phase, said amount being sufficient to accelerate catalysis by the peroxide catalyst;
- unsaturated polyester which has a mean molecular weight in the range of 1800 to 100,000 as calculated from the formula:
- MW = 2(56,100)/R.sub.n
- wherein MW is mean molecular weight and R.sub.n is reactivity number, being the sum of the acid value and the hydroxyl value attained in an esterification reaction which forms the polyester, said polyester including the esterification reaction product of (A) dicarboxylic acid, at least a portion of which is .alpha.,.beta.-ethylenically unsaturated acid and, as saturated acid, phthalic, isophthalic, or terephthalic acid in an amount up to 5 moles per mole of unsaturated acid, which is sufficient to impart appreciable compressive strength, tensile strength, and impact resistance to the thermoset product;
- and (B) dihydric alcohol;
- and styrene as copolymerizeable solvent for said polyester;
- the weight ratio of polyester and copolymerizeable solvent to water being in the range of 1:4 to 2:1;
- and the weight ratio of polyester to copolymerizeable solvent being in the range of 1:2 to 2:1.
A method for producing thermoset cellular solid material which comprises forming a pumpable water-in-oil emulsion, comprising water emulsified in an oil phase, by agitating:
- water;
- peroxide catalyst;
- cobalt salt promoter;
- tertiary aromatic amine promoter;
- said cobalt salt promoter and tertiary aromatic amine promoter being present in the oil phase in amount in the range of about 0.1 to 5% by weight of the oil phase;
- unsaturated polyester which has a mean molecular weight in the range of 1800 to 100,000, said polyester including reaction product of polycarboxylic acid, at least a portion of which is .alpha.,.beta.-ethylenically unsaturated, and polyhydric alcohol;
- and ethylenically unsaturated solvent which is copolymerizeable with said polyester;
- the weight ratio of polyester and solvent to water being in the range of 1:10 to 10:1;
- the weight ratio of polyester to copolymerizable solvent being in the range of 10:1 to 1:10;
- and polymerizing said water-in-oil emulsion for forming the cellular solid material.
A method for producing thermoset cellular solid material which comprises forming a pumpable water-in-oil emulsion having water emulsified in oil phase, said emulsion including peroxide catalyst;
- cobalt salt promoter;
- tertiary aromatic amine promoter;
- said cobalt salt promoter and tertiary aromatic amine promoter being present in the oil phase in an amount in the range of about 0.1 to 5% by weight of the oil phase;
- unsaturated polyester which has a molecular weight in the range of 1800 to 100,000 and includes reaction product of (A) polycarboxylic acid, at least a portion of which is .alpha.,.beta.-ethylenically unsaturated acid and (B) polyhydric alcohol;
- and ethylenically unsaturated solvent which is copolymerizable with said polyester;
- the weight ratio of polyester and solvent to water being in the range of 1:10 to 10:1;
- and the weight ratio of polyester to solvent being in the range of 10:1 to 1:10;
- and polymerizing the water-in-oil emulsion without breaking said emulsion for forming the cellular solid material.
A method for producing thermoset cellular solid material which comprises forming a pumpable water-in-oil emulsion having water emulsified in an oil phase by adding water while vigorously agitating the oil phase, said emulsion including:
- peroxide catalyst;
- cobalt salt promoter;
- tertiary aromatic amine promoter;
- said cobalt salt promoter and tertiary aromatic amine promoter being present in the oil phase in an amount in the range of about 0.1 to 5% by weight of the oil phase;
- unsaturated polyester which has a mean molecular weight in the range of 1800 to 100,000 and includes a reaction product of (A) dicarboxylic acid, at least a portion of which is .alpha.,.beta.-ethylenically unsaturated acid and, as saturated acid, phthalic, isophthalic, or terephthalic acid, and (B) dihydric alcohol;
- and ethylenically unsaturated solvent which is copolymerizable with said polyester;
- the weight ratio of polyester and copolymerizable solvent to water being in the range of 1:4 to 2:1;
- and the weight ratio of polyester to copolymerizable solvent being in the range of 1:2 to 2:1;
- and polymerizing the water-in-oil emulsion without breaking said emulsion for forming the cellular solid material.
A method for producing shapeable water-in-oil resin composition which is polymerizable to a thermoset cellular solid product which comprises forming a pumpable water-in-oil emulsion having water emulsified in an oil phase, by bringing together under vigorous agitation water and an oil phase, said emulsion including:
- water;
- peroxide catalyst in an effecive amount in the range of 0.001 to 10% by weight of the copolymerizable solvent referred to below;
- cobalt salt promoter and tertiary aromatic amine promoter being present in said oil phase in an amount in the range of about 0.1 to 5% by weight of the oil phase, said amount being sufficient to accelerate catalysis of the peroxide catalyst;
- unsaturated polyester which has a mean molecular weight in the range of 1800 to 100,000 as calculated from the formula:
- MW = 2(56,100)/R.sub.n
- wherein MW is mean molecular weight and R.sub.n is reactivity number, being the sum of the acid value and the hydroxyl value attained in an esterification reaction which forms the polyester, said polyester including the esterification reaction product of (A) dicarboxylic acid, at least a portion of which is .alpha.,.beta.-ethylenically unsaturated acid and, as saturated acid, phthalic, isophtalic, or terephthalic acid, in an amount up to 5 moles per mole of unsaturated acid, which is sufficient to impart appreciable compressive strength, tensile strength and impact resistance to the thermoset product;
- and (B) dihydric alcohol;
- and styrene as copolymerizable solvent for said polyester;
- the weight ratio of polyester and copolymerizable solvent to water being in the range of 1:4 to 2:1;
- and the weight ratio of polyester to copolymerizable solvent being in the range of 1:2 to 2:1;
- and polymerizing the water-in-oil emulsion without breaking said emulsion for forming the cellular solid material.
Dependencies are inferred from the claim text.