Method of producing organosilicon composition with in situ produced cure inhibitor

Claim 1

A method of preparing a storage stable, one part, heat curable organosilicon composition consisting essentially of (A) mixing (1) an organosilicon polymer having an average of from one to three groups per silicon atom selected from the group consisting of monovalent hydrocarbon radicals, aliphatic-unsaturation-free monovalent halohydrocarbon radicals, and cyanoalkyl radicals, there being an average per molecule of (1) of at least two monovalent hydrocarbon radicals containing aliphatic unsaturation, the remaining valences of the silicon atoms of said organosilicon polymer being satisfied by divalent radicals selected from the group consisting of divalent oxygen atoms, divalent hydrocarbon radicals, divalent hydrocarbon ether radicals, and divalent haloarylene radicals, said divalent radicals linking silicon atoms; (2) a platinum catalyst in an amount of at least 0.1 part by weight of platinum per one million parts by weight of the combined weights of organosilicon polymer (1) and organosilicon compound (5); (3) an acetylenic alcohol, liquid at the reaction conditions of step (B) and distillable at temperatures of less than 120° C. at a pressure of 133 pascal, in an amount sufficient to provide at least one mole of acetylenic radical for each 3 moles of silicon-bond hydrogen atoms in siloxane compound (4); (4) a siloxane compound having at least 3 silicon-bonded hydrogen atoms with no more than one silicon-bonded hydrogen atom per silicon atom, the organic groups on the silicon atoms being monovalent hydrocarbon radicals having no aliphatic unsaturation, the siloxane compound being a linear, branched, or cyclic molecule containing from 3 to 100 siloxane units, then (B) heating to a temperature which is between 100° and 150° C. and which is also above the temperature at which an olefinic siloxane compound formed by the reaction of the acetylenic alcohol (3) and the siloxane compound (4) is no longer an inhibitor for the reaction in a closed container for a time sufficient to allow the reaction to produce the olefinic siloxane compound, (C) cooling to below 50° C., (D) reducing pressure over the reaction mixture to an amount sufficient to remove any unreacted acetylenic alcohol (3), then (E) admixing (5) an organosilicon compound containing silicon-bonded hydrogen atoms, there being in addition an average of up to 2 monovalent organic radicals per silicon atom selected from the group consisting of monovalent hydrocarbon radicals free of aliphatic unsaturation, monovalent halohydrocarbon radicals free of aliphatic unsaturation, and cyanoalkyl radicals, the remaining valences of the silicon atoms being satisfied by divalent radicals selected from the group consisting of divalent oxygen atoms, divalent hydrocarbon radicals free of aliphatic unsaturation, divalent hydrocarbon ether radicals, and divalent haloarylene radicals, said divalent radicals linking silicon atoms, there being an average of at least two silicon-bonded hydrogen atoms per molecule of organosilicon compound (5), the sum of the average number of aliphatic unsaturated monovalent radicals per molecule of organosilicon polymer (1) and the average number of silicon-bonded hydrogen atoms per molecule of organosilicon compound (5) being at least 4, the organosilicon composition further restricted in that the amount of organosilicon polymer (1) is sufficient to control the reaction exotherm.

Claim 2

A method of preparing a storage stable, one part, heat curable organosilicon composition consisting essentially of (A) mixing (1) an organosilicon polymer having an average of from one to three groups per silicon atom selected from the group consisting of monovalent hydrocarbon radicals, aliphatic-unsaturation-free monovalent halohydrocarbon radicals, and cyanoalkyl radicals, there being an average per molecule of (1) of at least two monovalent hydrocarbon radicals containing aliphatic unsaturation, the remaining valences of the silicon atoms of said organosilicon polymer being satisfied by divalent radicals selected from the group consisting of divalent oxygen atoms, divalent hydrocarbon radicals, divalent hydrocarbon ether radicals, and divalent haloarylene radicals, said divalent radicals linking silicon atoms; (2) a platinum catalyst in an amount of at least 0.1 part by weight of platinum per one million parts by weight of the combined weights of organosilicon polymer (1) and organosilicon compound (5); (3) an acetylenic alcohol, liquid at the reaction conditions of step (B) and distillable at temperatures of less than 120° C. at a pressure of 133 pascal, in an amount sufficient to provide at least one mole of acetylenic radical for each 3 moles of silicon-bond hydrogen atoms in siloxane compound (4); (4) a siloxane compound having at least 3 silicon-bonded hydrogen atoms with no more than one silicon-bonded hydrogen atom per silicon atom, the organic groups on the silicon atoms being monovalent hydrocarbon radicals having no aliphatic unsaturation, the siloxane compound being a linear, branched, or cyclic molecule containing from 3 to 100 siloxane units, then (B) heating to a temperature which is between 100° and 150° C. and which is also above the temperature at which an olefinic siloxane compound formed by the reaction of the acetylenic alcohol (3) and the siloxane compound (4) is no longer an inhibitor for the reaction in a closed container for a time sufficient to allow the reaction to produce the olefinic siloxane compound, (C) cooling to below 50° C., (D) reducing pressure over the reaction mixture to an amount sufficient to remove any unreacted acetylenic alcohol (3), then (E) admixing (5) an organosilicon compound containing silicon-bonded hydrogen atoms, there being in addition an average of up to 2 monovalent organic radicals per silicon atom selected from the group consisting of monovalent hydrocarbon radicals free of aliphatic unsaturation, monovalent halohydrocarbon radicals free of aliphatic unsaturation, and cyanoalkyl radicals, the remaining valences of the silicon atoms being satisfied by divalent radicals selected from the group consisting of divalent oxygen atoms, divalent hydrocarbon radicals free of aliphatic unsaturation, divalent hydrocarbon ether radicals, and divalent haloarylene radicals, said divalent radicals linking silicon atoms, there being an average of at least two silicon-bonded hydrogen atoms per molecule of organosilicon compound (5), the sum of the average number of aliphatic unsaturated monovalent radicals per molecule of organosilicon polymer (1) and the average number of silicon-bonded hydrogen atoms per molecule of organosilicon compound (5) being at least 4, the organosilicon composition further restricted in that the amount of organosilicon polymer (1) is sufficient to control the reaction exotherm.

Claim 6

A method of preparing a storage stable, one part, heat curable organosilicon composition consisting essentially of (A) mixing (1) an organosilicon polymer having an average of from one to three groups per silicon atom selected from the group consisting of monovalent hydrocarbon radicals, aliphatic-unsaturation-free monovalent halohydrocarbon radicals, and cyanoalkyl radicals, there being an average per molecule of (1) of at least two monovalent hydrocarbon radicals containing aliphatic unsaturation, the remaining valences of the silicon atoms of said organosilicon polymer being satisfied by divalent radicals selected from the group consisting of divalent oxygen atoms, divalent hydrocarbon radicals, divalent hydrocarbon ether radicals, and divalent haloarylene radicals, said divalent radicals linking silicon atoms; (2) a platinum catalyst in an amount of at least 0.1 parts by weight of platinum per one million parts by weight of the combined weights of organosilicon polymer (1) and organosilicon compound (5); (3) an acetylenic alcohol, liquid at the reaction conditions of step (B) and distillable at temperatures of less than 120° C. at a pressure of 133 pascal, in an amount sufficient to provide at least one mole of acetylenic radical for each 3 moles of silicon-bond hydrogen atoms in siloxane compound (4); (4) a siloxane having at least 3 silicon-bonded hydrogen atoms with no more than one silicon-bonded hydrogen atom per silicon atom, the organic groups on the silicon atoms being monovalent hydrocarbon radicals having no aliphatic unsaturation, the siloxane compound being a linear, branched, or cyclic molecule containing from 3 to 100 siloxane units, then (B) heating to a temperature which is between 100° and 150° C. and which is also above the temperature at which an olefinic siloxane compound formed by the reaction of the acetylenic alcohol (3) and the siloxane compound (4) is no longer an inhibitor for the reaction in a closed container for a time sufficient to allow the reaction to produce the olefinic siloxane compound, (D) reducing pressure over the reaction mixture in the mixer to an amount sufficient to remove any unreacted acetylenic alcohol (3), then (C) cooling to below 50° C., then (E) admixing (5) an organosilicon compound containing silicon-bonded hydrogen atoms, there being in addition an average of up to 2 monovalent organic radicals per silicon atom selected from the group consisting of monovalent hydrocarbon radicals free of aliphatic unsaturation, monovalent halohydrocarbon radicals free of aliphatic unsaturation, and cyanoalkyl radicals, the remaining valences of the silicon atoms being satisfied by divalent radicals selected from the group consisting of divalent oxygen atoms, divalent hydrocarbon radicals free of aliphatic unsaturation, divalent hydrocarbon ether radicals, and divalent haloarylene radicals, said divalent radicals linking silicon atoms, there being an average of at least two silicon-bonded hydrogen atoms per molecule of organosilicon compound (5), the sum of the average number of aliphatic unsaturated monovalent radicals per molecule of organosilicon polymer (1) and the average number of silicon-bonded hydrogen atoms per molecule of organosilicon compound (5) being at least 4, the organosilicon composition further restricted in that the amount of organosilicon polymer (1) is sufficient to control the reaction exotherm.

Claim 7

A method of preparing a storage stable, one part, heat curable organosilicon composition consisting essentially of (A) mixing (1) an organosilicon polymer having an average of from one to three groups per silicon atom selected from the group consisting of monovalent hydrocarbon radicals, aliphatic-unsaturation-free monovalent halohydrocarbon radicals, and cyanoalkyl radicals, there being an average per molecule of (1) of at least two monovalent hydrocarbon radicals containing aliphatic unsaturation, the remaining valences of the silicon atoms of said organosilicon polymer being satisfied by divalent radicals selected from the group consisting of divalent oxygen atoms, divalent hydrocarbon radicals, divalent hydrocarbon ether radicals, and divalent haloarylene radicals, said divalent radicals linking silicon atoms; (2) a platinum catalyst in an amount of at least 0.1 parts by weight of platinum per one million parts by weight of the combined weights of organosilicon polymer (1) and organosilicon compound (5); (3) an acetylenic alcohol, liquid at the reaction conditions of step (B) and distillable at temperatures of less than 120° C. at a pressure of 133 pascal, in an amount sufficient to provide at least one mole of acetylenic radical for each 3 moles of silicon-bond hydrogen atoms in siloxane compound (4); (4) a siloxane having at least 3 silicon-bonded hydrogen atoms with no more than one silicon-bonded hydrogen atom per silicon atom, the organic groups on the silicon atoms being monovalent hydrocarbon radicals having no aliphatic unsaturation, the siloxane compound being a linear, branched, or cyclic molecule containing from 3 to 100 siloxane units, then (B) heating to a temperature which is between 100° and 150° C. and which is also above the temperature at which an olefinic siloxane compound formed by the reaction of the acetylenic alcohol (3) and the siloxane compound (4) is no longer an inhibitor for the reaction in a closed container for a time sufficient to allow the reaction to produce the olefinic siloxane compound, (D) reducing pressure over the reaction mixture in the mixer to an amount sufficient to remove any unreacted acetylenic alcohol (3), then (C) cooling to below 50° C., then (E) admixing (5) an organosilicon compound containing silicon-bonded hydrogen atoms, there being in addition an average of up to 2 monovalent organic radicals per silicon atom selected from the group consisting of monovalent hydrocarbon radicals free of aliphatic unsaturation, monovalent halohydrocarbon radicals free of aliphatic unsaturation, and cyanoalkyl radicals, the remaining valences of the silicon atoms being satisfied by divalent radicals selected from the group consisting of divalent oxygen atoms, divalent hydrocarbon radicals free of aliphatic unsaturation, divalent hydrocarbon ether radicals, and divalent haloarylene radicals, said divalent radicals linking silicon atoms, there being an average of at least two silicon-bonded hydrogen atoms per molecule of organosilicon compound (5), the sum of the average number of aliphatic unsaturated monovalent radicals per molecule of organosilicon polymer (1) and the average number of silicon-bonded hydrogen atoms per molecule of organosilicon compound (5) being at least 4, the organosilicon composition further restricted in that the amount of organosilicon polymer (1) is sufficient to control the reaction exotherm.