In situ hydrolysis of alkoxy silanes containing orthotitanate catalysts

Claim 1

A METHOD FOR THE MANUFACTURE OF ANORGANOSILOXANE LAMINATE WHICH COMPRISES (1) CONTACTING A FIBROUS SHEET MATERIAL WITH A MIXTURE OF (A) A SILANE OF THE FORMULA RNSI(OR'')4-N IN WHICH R IS SELECTED FROM THE GROUP CONSISTIG OF PHENYL AND MONOVALENT ALIPHATIC HYDROCARBON RADICALS WITH LESS THAN 4 CARBON ATOMS AND R'' IS AN ALKYL GROUP OF LESS THAN 4 CARBON ATOMS WITH N HAVING AN AVERAGE VALUE OF FROM .9 TO 1.9, AND (B) A HYDROLYSIS CATALYST SELECTED FROM THE GROUP CONSISTING OF ORTHOTITANATES HAVING THE GENEAL FORMULA TI(OR")4 AND PARTIAL CONDENSATES THEREOF, IN WHICH R" IS SELECTED FROM THE GROUP CONSISTING OFHYDROGEN, HYDROCARBON GROUPS CONTAINING 1-30 CARBON ATOMS AND APPROPRIATELY SUBSTITUTED HYDROCARBONS IN WHICH ANY ATOMS OTHER THAN CARBON AND HYDROGENARE SELECTED FROM THE GROUP CONSISTING OF NITROGEN AND OXYGEN ATOMS, SAID CATALYST BEING PRESENT IN AN AMOUNT FROM .0002 TO .06 MOL OF TI PER MOL OF SI, AND (2) THEN CONTACTING THE MATERIAL WITH WATER WHEREBY THE SILANE IS AT LEAST PARTIALLY HYDROLYZED, SAID SILANE (A) BEING EMPLOYED IN SUCH AMOUNT THAT THERE IS A PICK-UP BY THE MATERIAL OF AT LEAST 1.5 PERCENT BY WEIGHT RESIDUAL ORGANOSILOXANE BASED ON THE WEIGHT OF THE MATERIAL, (3) PRE-CURING THE IMPREGNATED SHEET OF MATERIAL TO AN EXTENT SUCH THAT IT IS SUFFICIENTLY THERMOPLASTIC TO BE LAMINATED WITH OTHER SHEETS OF IMPREGNATGED MATERIAL, (4) ASSEMBLING MULTIPLE PLIES OF THE SHEETS OF MATERIAL SO IMPREGNATED AND PRE-CURED TO FORM A LAMINATE, (5) SUBJECTING THE ASSEMBLY TO SUFFICIENT HEAT AND PRESSURE TO BOND AND CONSOLIDATE THE PLIES, AND (6) AFTER-CURING THE RESULTING LAMINATE AT GRADUALLY INCREASING TEMPERATURES.

Claim 2

A METHOD FOR THE MANUFACTURE OF ANORGANOSILOXANE LAMINATE WHICH COMPRISES (1) CONTACTING A FIBROUS SHEET MATERIAL WITH A MIXTURE OF (A) A SILANE OF THE FORMULA RNSI(OR'')4-N IN WHICH R IS SELECTED FROM THE GROUP CONSISTIG OF PHENYL AND MONOVALENT ALIPHATIC HYDROCARBON RADICALS WITH LESS THAN 4 CARBON ATOMS AND R'' IS AN ALKYL GROUP OF LESS THAN 4 CARBON ATOMS WITH N HAVING AN AVERAGE VALUE OF FROM .9 TO 1.9, AND (B) A HYDROLYSIS CATALYST SELECTED FROM THE GROUP CONSISTING OF ORTHOTITANATES HAVING THE GENEAL FORMULA TI(OR")4 AND PARTIAL CONDENSATES THEREOF, IN WHICH R" IS SELECTED FROM THE GROUP CONSISTING OFHYDROGEN, HYDROCARBON GROUPS CONTAINING 1-30 CARBON ATOMS AND APPROPRIATELY SUBSTITUTED HYDROCARBONS IN WHICH ANY ATOMS OTHER THAN CARBON AND HYDROGENARE SELECTED FROM THE GROUP CONSISTING OF NITROGEN AND OXYGEN ATOMS, SAID CATALYST BEING PRESENT IN AN AMOUNT FROM .0002 TO .06 MOL OF TI PER MOL OF SI, AND (2) THEN CONTACTING THE MATERIAL WITH WATER WHEREBY THE SILANE IS AT LEAST PARTIALLY HYDROLYZED, SAID SILANE (A) BEING EMPLOYED IN SUCH AMOUNT THAT THERE IS A PICK-UP BY THE MATERIAL OF AT LEAST 1.5 PERCENT BY WEIGHT RESIDUAL ORGANOSILOXANE BASED ON THE WEIGHT OF THE MATERIAL, (3) PRE-CURING THE IMPREGNATED SHEET OF MATERIAL TO AN EXTENT SUCH THAT IT IS SUFFICIENTLY THERMOPLASTIC TO BE LAMINATED WITH OTHER SHEETS OF IMPREGNATGED MATERIAL, (4) ASSEMBLING MULTIPLE PLIES OF THE SHEETS OF MATERIAL SO IMPREGNATED AND PRE-CURED TO FORM A LAMINATE, (5) SUBJECTING THE ASSEMBLY TO SUFFICIENT HEAT AND PRESSURE TO BOND AND CONSOLIDATE THE PLIES, AND (6) AFTER-CURING THE RESULTING LAMINATE AT GRADUALLY INCREASING TEMPERATURES.