US4196278A — Method for the controlled polymerization of polyp…

Claim 1

Independent Claim 87 words

A process for preparation of polyphenylene oxide polymer having a predetermined molecular weight, said process comprising the steps of: (a) adding oxygen to a reaction mixture comprising a main charge of a phenolic monomer, an oxidative coupling catalyst and a solvent; and (b) while continuing the addition of oxygen to the reaction mixture of step (a), adding to said reaction mixture an additional amount of phenolic monomer at a rate that is sufficient to control polymerization and producing a polyphenylene oxide polymer of a predetermined molecular weight.

Claim 2

Dependent Claim 87 words

A process for preparation of polyphenylene oxide polymer having a predetermined molecular weight, said process comprising the steps of: (a) adding oxygen to a reaction mixture comprising a main charge of a phenolic monomer, an oxidative coupling catalyst and a solvent; and (b) while continuing the addition of oxygen to the reaction mixture of step (a), adding to said reaction mixture an additional amount of phenolic monomer at a rate that is sufficient to control polymerization and producing a polyphenylene oxide polymer of a predetermined molecular weight.

Claim 3

Dependent Claim 109 words

A process as defined in claim 1 wherein the phenolic monomer has the formula: ##STR5## wherein X is a substituent selected from the group consisting of hydrogen, chlorine, bromine and iodine, Q is a monovalent substituent selected from the group consisting of hydrocarbon radicals, halohydrocarbon radicals having at least two carbon atoms between the halogen atom and the phenol nucleus; hydrocarbonoxy radicals and halohydrocarbonoxy radicals having at least two carbon atoms between the halogen atom and the phenol nucleus; Q' and Q" are the same as Q and in addition may be halogen, with the proviso that Q, Q' and Q" are all free of a tertiary alpha-carbon atom.

Claim 4

Dependent Claim 15 words

A process as defined in claim 1 wherein the catalyst is a complex copper-amine catalyst.

Claim 5

Dependent Claim 79 words

A process as defined in claim 1 wherein the catalyst is a complex manganese catalyst of the formula (L) x Mn wherein L is hydroxyoxime ligand of the formula: ##STR6## wherein R a , R b , R c and R d are independently selected from the group consisting of hydrogen, acyclic and cyclic hydrocarbon radicals, and n is a positive integer equal to 0 to 1, and x is a positive number at least equal to about 10.

Claim 6

Dependent Claim 24 words

A process as defined in claim 3 wherein the complex copper-amine catalyst is based on a copper compound and a primary or secondary amine.

Claim 7

Dependent Claim 14 words

A process as defined in claim 5 wherein the amine is a dialkyl amine.

Claim 8

Dependent Claim 63 words

A process as defined in claim 3 wherein the catalyst comprises (a) a copper compound (b) a diamine of the formula: R.sup.1 HN--R.sup.2 --NHR.sup.1 wherein each R 1 is independently isopropyl, a C 4-8 tertiary alkyl or a cycloalkyl group having no hydrogens on the alpha-carbon atom and R 2 is C 2-4 alkylene or C 3-7 cycloalkylene; and (c) a tertiary amine.

Claim 9

Dependent Claim 19 words

A process as defined in claim 3 wherein the copper-amine catalyst is derived from cuprous oxide, butyldimethylamine and N,N'-di-tert-butylethylenediamine.

Claim 10

Dependent Claim 19 words

A process as defined in claim 3 wherein the copperamine catalyst is derived from cuprous oxide, butyldimethylamine and N,N'-di-tert-butylethylenediamine.

Claim 11

Dependent Claim 88 words

A process for the preparation of poly(2,6-dimethyl-1,4-phenylene oxide) polymer having a predetermined molecular weight, said process comprising the steps of: (a) adding oxygen to a reaction mixture comprising a main charge of a phenolic monomer, an oxidative coupling catalyst and a solvent; and (b) while continuing the addition of oxygen to the reaction mixture of step (a), adding to said reaction mixture an additional amount of phenolic monomer at a rate that is sufficient to control polymerization and producing a poly(2,6-dimethyl-1,4-phenylene oxide polymer of a predetermined molecular weight.

Claim 12

Dependent Claim 88 words

A process for the preparation of poly(2,6-dimethyl-1,4-phenylene oxide) polymer having a predetermined molecular weight, said process comprising the steps of: (a) adding oxygen to a reaction mixture comprising a main charge of a phenolic monomer, an oxidative coupling catalyst and a solvent; and (b) while continuing the addition of oxygen to the reaction mixture of step (a), adding to said reaction mixture an additional amount of phenolic monomer at a rate that is sufficient to control polymerization and producing a poly(2,6-dimethyl-1,4-phenylene oxide polymer of a predetermined molecular weight.

Claim 13

Dependent Claim 21 words

A process as defined in claim 10 wherein the catalyst is a manganese catalyst derived from manganese chloride and benzoin oxime.

Claim 14

Dependent Claim 116 words

A process for preparation of polyphenylene oxide polymer, having a predetermined molecular weight, said process comprising the steps of: (a) adding oxygen to a reaction mixture comprising a main charge of from 85 to 99.9% by weight of the total amount of monomer adding during the reaction of an oxidative coupling catalyst and a solvent; and (b) while continuing the addition of oxygen to the reaction mixture of step (a), adding to said reaction mixture at a rate of 0.2 to 15% by weight of the main phenolic monomer charge per hour of reaction time an additional amount of phenolic monomer, and controlling the polymerization and producing a polyphenylene oxide polymer of a predetermined molecular weight.

Claim 15

Dependent Claim 116 words

A process for preparation of polyphenylene oxide polymer, having a predetermined molecular weight, said process comprising the steps of: (a) adding oxygen to a reaction mixture comprising a main charge of from 85 to 99.9% by weight of the total amount of monomer adding during the reaction of an oxidative coupling catalyst and a solvent; and (b) while continuing the addition of oxygen to the reaction mixture of step (a), adding to said reaction mixture at a rate of 0.2 to 15% by weight of the main phenolic monomer charge per hour of reaction time an additional amount of phenolic monomer, and controlling the polymerization and producing a polyphenylene oxide polymer of a predetermined molecular weight.

Claim 16

Dependent Claim 109 words

A process as defined in claim 12 wherein the phenolic monomer has the formula: ##STR7## wherein X is a substituent selected from the group consisting of hydrogen, chlorine, bromine and iodine, Q is a monovalent substituent selected from the group consisting of hydrocarbon radicals, halohydrocarbon radicals having at least two carbon atoms between the halogen atom and the phenol nucleus; hydrocarbonozy radicals and halohydrocarbonoxy radicals having at least two carbon atoms between the halogen atom and the phenol nucleus; Q' and Q" are the same as Q and in addition may be halogen, with the proviso that Q, Q' and Q" are all free of a tertiary alpha-carbon atom.

Claim 17

Dependent Claim 15 words

A process as defined in claim 12 wherein the catalyst is a complex copper-amine catalyst.

Claim 18

Dependent Claim 80 words

A process as defined in claim 12 wherein the catalyst is a complex manganese catalyst of the formula (L) x Mn wherein L is a hydroxyoxime ligand of the formula: ##STR8## wherein R a , R b , R c and R d are independently selected from the group consisting of hydrogen, acyclic and cyclic hydrocarbon radicals, and n is a positive integer equal to 0 to 1, and x is a positive number at least equal to about 10.

Claim 19

Dependent Claim 24 words

A process as defined in claim 14 wherein the complex copper-amine catalyst is based on a copper compound and a primary or secondary amine.

Claim 20

Dependent Claim 14 words

A process as defined in claim 16 wherein the amine is a dialkyl amine.

Claim 21

Dependent Claim 63 words

A process as defined in claim 14 wherein the catalyst comprises (a) a copper compound (b) a diamine of the formula: R.sup.1 HN--R.sup.2 --NHR.sup.1 wherein each R 1 is independently isopropyl, a C 4-8 tertiary alkyl or a cycloalkyl group having no hydrogens on the alpha-carbon atom and R 2 is C 2-4 alkylene or C 3-7 cycloalkylene; and (c) a tertiary amine.

Claim 22

Dependent Claim 19 words

A process as defined in claim 14 wherein the copper-amine catalyst is based on cupric chloride and di-n-butyl amine.

Claim 23

Dependent Claim 19 words

A process as defined in claim 14 wherein the copper-amine catalyst is based on cuprous oxide, butyldimethylamine and N,N'-di-tert-butylethylenediamine.

Claim 24

Dependent Claim 120 words

A process for the preparation of poly(2,6-dimethyl-1,4-phenylene oxide) polymer, having a predetermined molecular weight, said process comprising the steps of: (a) adding oxygen to a reaction mixture comprising a main charge of from 85 to 99.9% by weight of the total amount of monomer added during the reaction of a phenolic monomer, an oxidative coupling catalyst and a solvent; and (b) while continuing the addition of oxygen to the reaction mixture of step (a), adding to said reaction mixture at a rate of 0.2 to 15% by weight of the main phenolic monomer charge per hour of reaction time an additional amount of phenolic monomer, and controlling the polymerization and producing a poly(2,6-dimethyl-1,4-phenylene oxide polymer of a predetermined molecular weight.

Claim 25

Dependent Claim 120 words

A process for the preparation of poly(2,6-dimethyl-1,4-phenylene oxide) polymer, having a predetermined molecular weight, said process comprising the steps of: (a) adding oxygen to a reaction mixture comprising a main charge of from 85 to 99.9% by weight of the total amount of monomer added during the reaction of a phenolic monomer, an oxidative coupling catalyst and a solvent; and (b) while continuing the addition of oxygen to the reaction mixture of step (a), adding to said reaction mixture at a rate of 0.2 to 15% by weight of the main phenolic monomer charge per hour of reaction time an additional amount of phenolic monomer, and controlling the polymerization and producing a poly(2,6-dimethyl-1,4-phenylene oxide polymer of a predetermined molecular weight.

Claim 26

Dependent Claim 22 words

A process as defined in claim 21 wherein the catalyst is a complex manganese catalyst based on manganese chloride and benzoin oxime.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1983-04-01	1983-10-01	1984-04-01	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1987-04-01	1987-10-01	1988-04-01	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1991-04-01	1991-10-01	1992-04-01	$7700.00	Window Closed / Lapsed

Method for the controlled polymerization of polyphenylene oxide polymers

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