Process for the production of a bodied silicone resin without the use of a catalyst

Claim 2

A process for the production of a bodied silicone resin without the use of a catalyst comprising (a) adding a organohalosilane to a homogeneous hydrolysis mixture where there is present per part or organohalosilane from at least 1.7 to 10 parts of water and from at least 0.2 to 5 parts of acetone and from 0 to about 1 mole of an aliphatic monohydric alcohol having from 1 to 8 carbon atoms, per mole of halogen attached to the silicone of the organohalosilane to produce a silicone resin hydrolyzate (b) separating the acid/water layer from the silicone resin hydrolyzate; (c) adding to the silicone resin hydrolyzate at least 5% by weight of water based on the silicone resin hydrolyzate; (d) heating the silicone resin hydrolyzate gradually for a period of time of 1 to 8 hours to at least 130° C; and (e) removing the water and acetone from the silicone resin hydrolyzate to leave the silicone resin; wherein said organohalosilane is selected from the group consisting of (1) organotrihalosilane (2) a mixture of organotrihalosilane and diorganodihalosilane, (3) a reaction product of an aliphatic monohydric alcohol having from 1 to 8 carbon atoms and a member selected from the class consisting of organotrihalosilane and a mixture of organotrihalosilane and diorganodihalosilane, which reaction product can have substituted an average of up to one alkoxy radical per halogen radical, (4) a mixture of the reaction product of (3) and a member selected from organotrihalosilane and diorganodihalosilane, and wherein the organo groups of said organohalosilane and the silicone resin are selected from the class consisting of monovalent hydrocarbon radicals, and halogenated monovalent hydrocarbon radicals.

Claim 3

The process of claim 1 wherein the amount of water added in step (c) is 10% to 100% by weight of the silicone resin hydrolyzate.

Claim 4

The process of claim 2 wherein in step (d) the silicone resin hydrolyzate is heated in the range of 140° C to 160° C.

Claim 5

The process of claim 3 wherein after step (d) and in conjunction with step (e) further comprising (f) adding to said silicone resin hydrolyzate from 10% to 100% by weight of water based on said hydrolyzate and from 0.05 to 0.3 parts of water-immiscible organic solvent per part by weight of said hydrolyzate and heating the mixture at the reflux temperature of said water-immiscible organic solvent until all water is removed and the said silicone resin has an acid content that does not exceed 5 parts per million.

Claim 6

The process of claim 4 wherein step (f) is repeated until the acid content of said silicone resin is less than 5 parts per million.

Claim 7

The process of claim 3 wherein step (c) and (d) are repeated until the silicone resin has an acid content that does not exceed 5 parts per million and until all water and acetone are removed from the silicone resin to yield the said silicone resin at 100% solids.

Claim 8

A silicone resin produced by the process of claim 1 having a silanol content of 2% to 4% by weight.

Claim 9

A silicone paint containing the silicone resin of claim 1.

Claim 10

A silicone molding and encapsulating composition containing the silicone resin of claim 1.

Claim 11

The silicone resin of claim 1 wherein said resin containing 10 mole percent of monomethylsiloxy units, 20 mole percent of monophenylsiloxy units, 40 mole percent of dimethylsiloxy units and 30 mole of diphenylsiloxy units.

Claim 12

The process of claim 4 wherein the water-immiscible organic solvents are selected from the class consisting of xylene, toluene and aliphatic solvents.

Claim 13

An encapsulating film composed of a silicone resin having a viscosity in the range of 40,000 to 100,000 centipoise which is produced by a process comprising (a) adding an organohalosilane to a homogeneous hydrolysis mixture where there is present per part of organohalosilane from at least 1.7 to 10 parts of water and from at least 0.2 to 5 parts of acetone and from 0 to about 1 mole of an aliphatic monohydric alcohol having from 1 to 8 carbon atoms per mole of halogen attached to the silicone of the organohalosilane to produce a silicone resin hydrolyzate; (b) separating the acid/water layer from the silicone resin hydrolyzate; (c) adding to the silicone resin hydrolyzate at least 5% by weight of water based on the silicone resin hydrolyzate; (d) heating the silicone resin hydrolyzate gradually for a period of time of 1 to 8 hours to at least 130° C; and (e) removing the water and acetone from the silicone resin hydrolyzate to leave the silicone resin wherein organohalosilane is selected from the group consisting of (1) organotrihalosilane; (2) a mixture of organotrihalosilane and diorganodihalosilane; (3) a reaction product of an aliphatic monohydric alcohol having from 1 to 8 carbon atoms and a member selected from the class consisting of organotrihalosilane, and a mixture of organotrihalosilane and diorganodihalosilane, which reaction product can have substituted an average of up to one alkoxy radical per halogen radical; (4) a mixture of the reaction product of (3) and a member selected from organotrihalosilane and diorganodihalosilane, and wherein the organo groups of said organohalosilane and the silicone resin are selected from the class consisting of monovalent hydrocarbon radicals, and halogenated monovalent hydrocarbon radicals.

Claim 14

An encapsulating film composed of a silicone resin having a viscosity in the range of 40,000 to 100,000 centipoise which is produced by a process comprising (a) adding an organohalosilane to a homogeneous hydrolysis mixture where there is present per part of organohalosilane from at least 1.7 to 10 parts of water and from at least 0.2 to 5 parts of acetone and from 0 to about 1 mole of an aliphatic monohydric alcohol having from 1 to 8 carbon atoms per mole of halogen attached to the silicone of the organohalosilane to produce a silicone resin hydrolyzate; (b) separating the acid/water layer from the silicone resin hydrolyzate; (c) adding to the silicone resin hydrolyzate at least 5% by weight of water based on the silicone resin hydrolyzate; (d) heating the silicone resin hydrolyzate gradually for a period of time of 1 to 8 hours to at least 130° C; and (e) removing the water and acetone from the silicone resin hydrolyzate to leave the silicone resin wherein organohalosilane is selected from the group consisting of (1) organotrihalosilane; (2) a mixture of organotrihalosilane and diorganodihalosilane; (3) a reaction product of an aliphatic monohydric alcohol having from 1 to 8 carbon atoms and a member selected from the class consisting of organotrihalosilane, and a mixture of organotrihalosilane and diorganodihalosilane, which reaction product can have substituted an average of up to one alkoxy radical per halogen radical; (4) a mixture of the reaction product of (3) and a member selected from organotrihalosilane and diorganodihalosilane, and wherein the organo groups of said organohalosilane and the silicone resin are selected from the class consisting of monovalent hydrocarbon radicals, and halogenated monovalent hydrocarbon radicals.

Claim 15

The encapsulating film of claim 12 which is cured by the addition of 0.05% to 1% by weight based on the silicone resin of metal salt of a carboxylic acid, the metal being selected from the class consisting of lead to manganese in the periodic table, and heating the film above 200° C.