Silicone pressure-sensitive adhesive process and product with improved lap-shear stability-II

Claim 1

A method of making a silicone pressure-sensitive adhesive composition having improved lap shear stability which consists essentially of the steps of: (I) mixing (A) from 40 to 70 inclusive parts by weight of at least one benzene-soluble resin copolymer containing silicon-bonded hydroxyl radicals and consisting essentially of R 3 SiO 1/2 units and SiO 4/2 units in a mole ratio of from 0.6 to 0.9 R 3 SiO 1/2 units for each SiO 4/2 unit present, (B) from 30 to 60 parts by weight of at least one polydiorganosiloxane consisting essentially of ARSiO units terminated with endblocking TRASiO 1/2 units, each said polydiorganosiloxane having a viscosity of from 100 centipoise to 30,000,000 centipoise at 25° C., and each T is R-- or X--, (C) a sufficient amount of at least one organosilicon endblocking agent capable of generating an endblocking triorganosilyl unit of the formula ZR 2 Si-- to provide a 1:0.8 to 1:3 mole ratio of total silicon-bonded hydroxyl and X radicals present in said (A) and (B) to total endblocking triorganosilyl units provided by all endblocking agent present, said agent being selected from the group consisting of ZR 2 SiNH 2 and (ZR 2 Si) 2 NH, (D) from 0.1 to 10 moles of water per mole of ═NH provided by said (C), (E) from 0.001 to 10 parts by weight per 100 parts by weight of (A) and (B) of at least one ammonia scavenger compound selected from the group consisting of HOC m H 2m+1 , HOC x H 2x (OC x H 2x ) y (O) v H, C w H 2w+1 (OC x H 2x ) y OC w H 2w+1 , C w H 2w+1 C(O) OC n H 2n+1 and HC(O)OC n H 2n+1 , and (F) when necessary, an effective amount of an organic solvent which is inert with respect to (A) through (E), inclusive, to reduce the viscosity of a mixture of (A), (B), and (C), (II) condensing (A), (B) and (C) at a temperature of from 80° C. to 160° C. and at the same time at least periodically removing any condensation by-products from the mixture at least until a substantial amount of the endblocking triorganosilyl units have reacted with the silicon-bonded hydroxyl radicals and X radicals of said (A) and (B), and (III) stripping substantially any remaining condensation by-products, (D) and (E) from the mixture after the condensation reaction of step II is substantially complete, wherein each R is a monovalent organic radical selected from the group consisting of hydrocarbon radicals of from 1 to 6 inclusive carbon atoms, each X radical is selected from the group consisting of HO--, H-- and R'O-- radicals, each R' is an alkyl radical of from 1 to 4 inclusive carbon atoms, m has a value of from 2 to 4, n has a value of from 1 to 6, v is 0 or 1, w has a value of from 1 to 3, x has a value of from 2 to 6, y has a value of from 0 to 3, each A radical is selected from the group consisting of R-- and halohydrocarbon radicals of from 1 to 6 inclusive carbon atoms, each Z radical is A-- or QR"--, each R" is a divalent alkylene radical of from 1 to 6 inclusive carbon atoms, each Q is an organofunctional monovalent radical selected from the group consisting of RCOE'--, RE'OC--, NC--, R'E'--, HO--, G 2 N--, HO(R"O) n --where E' is --O --, --NH-- or --S--, and each G is R'-- or H--,

Claim 2

A method of making a silicone pressure-sensitive adhesive composition having improved lap shear stability which consists essentially of the steps of: (I) mixing (A) from 40 to 70 inclusive parts by weight of at least one benzene-soluble resin copolymer containing silicon-bonded hydroxyl radicals and consisting essentially of R 3 SiO 1/2 units and SiO 4/2 units in a mole ratio of from 0.6 to 0.9 R 3 SiO 1/2 units for each SiO 4/2 unit present, (B) from 30 to 60 parts by weight of at least one polydiorganosiloxane consisting essentially of ARSiO units terminated with endblocking TRASiO 1/2 units, each said polydiorganosiloxane having a viscosity of from 100 centipoise to 30,000,000 centipoise at 25° C., and each T is R-- or X--, (C) a sufficient amount of at least one organosilicon endblocking agent capable of generating an endblocking triorganosilyl unit of the formula ZR 2 Si-- to provide a 1:0.8 to 1:3 mole ratio of total silicon-bonded hydroxyl and X radicals present in said (A) and (B) to total endblocking triorganosilyl units provided by all endblocking agent present, said agent being selected from the group consisting of ZR 2 SiNH 2 and (ZR 2 Si) 2 NH, (D) from 0.1 to 10 moles of water per mole of ═NH provided by said (C), (E) from 0.001 to 10 parts by weight per 100 parts by weight of (A) and (B) of at least one ammonia scavenger compound selected from the group consisting of HOC m H 2m+1 , HOC x H 2x (OC x H 2x ) y (O) v H, C w H 2w+1 (OC x H 2x ) y OC w H 2w+1 , C w H 2w+1 C(O) OC n H 2n+1 and HC(O)OC n H 2n+1 , and (F) when necessary, an effective amount of an organic solvent which is inert with respect to (A) through (E), inclusive, to reduce the viscosity of a mixture of (A), (B), and (C), (II) condensing (A), (B) and (C) at a temperature of from 80° C. to 160° C. and at the same time at least periodically removing any condensation by-products from the mixture at least until a substantial amount of the endblocking triorganosilyl units have reacted with the silicon-bonded hydroxyl radicals and X radicals of said (A) and (B), and (III) stripping substantially any remaining condensation by-products, (D) and (E) from the mixture after the condensation reaction of step II is substantially complete, wherein each R is a monovalent organic radical selected from the group consisting of hydrocarbon radicals of from 1 to 6 inclusive carbon atoms, each X radical is selected from the group consisting of HO--, H-- and R'O-- radicals, each R' is an alkyl radical of from 1 to 4 inclusive carbon atoms, m has a value of from 2 to 4, n has a value of from 1 to 6, v is 0 or 1, w has a value of from 1 to 3, x has a value of from 2 to 6, y has a value of from 0 to 3, each A radical is selected from the group consisting of R-- and halohydrocarbon radicals of from 1 to 6 inclusive carbon atoms, each Z radical is A-- or QR"--, each R" is a divalent alkylene radical of from 1 to 6 inclusive carbon atoms, each Q is an organofunctional monovalent radical selected from the group consisting of RCOE'--, RE'OC--, NC--, R'E'--, HO--, G 2 N--, HO(R"O) n --where E' is --O --, --NH-- or --S--, and each G is R'-- or H--,