Hydrosilylation method
AssigneeDow Global Technologies LLC
InventorsRafael Benavides, David A. Babb, Matthias Schaefer, Patrick Fontanella, William H. Heath, Wenwen Li
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Abstract
Vinyl-functional alcohols are silylated by reaction with a hydrolysable silyl hydride compound. The starting alcohol is heated and then combined with the silyl hydride and catalyst and allowed to heat exothermically. Cooling is applied when the conversion of vinyl groups is between 90-99%. In some embodiments, specified amounts of water are present. The cooling regimen and control of water content reduces certain side reactions, leading to greater yields to desired product.
Claims20
A process for producing a silyl-terminated alcohol by reacting a vinyl-functional alcohol with a hydrolysable silyl hydride in the presence of a platinum catalyst, comprising the steps of:
- a) heating the vinyl-functional alcohol to a temperature of 40 to 65° C. in the presence of 150 to 2000 ppm water based on the weight of the vinyl-functional alcohol, then
- b) adding the platinum catalyst and from 0.8 to 1.1 moles of the hydrolysable silyl hydride per mole of vinyl-functional alcohol to the heated vinyl-functional alcohol to form a reaction mixture;
- then
- c) reacting the reaction mixture under conditions such that at least part of the vinyl-functional alcohol and at least part of the hydrolysable silyl hydride react to form the silyl-terminated alcohol, wherein the temperature of the reaction mixture increases at least partially due to exothermic heat of reaction to above 75° C. but not greater than 100° C., and then
- d) upon conversion of 90 to 99% of the vinyl groups of the vinyl-functional alcohol, cooling the reaction mixture to a temperature of 65° C. or below, whereby after step d) the conversion of vinyl-functional alcohol is at least 90% and the amount of high molecular weight impurities is no greater than 10% of the combined weight of the starting amounts of vinyl-functional alcohol and hydrolysable silyl hydride.
A process for producing a silyl-terminated alcohol by reacting a vinyl-functional alcohol with a hydrolysable silyl hydride in the presence of a platinum catalyst, comprising the steps of:
- a) forming a heated mixture of a vinyl-functional alcohol and 150 to 2000 ppm water based on the weight of the vinyl-functional alcohol, which heated mixture has a temperature of 40 to 80° C., then
- b) adding the platinum catalyst and from 0.8 to 1.1 mole of the hydrolysable silyl hydride per mole of vinyl-functional alcohol to the heated mixture to form a reaction mixture;
- and then
- c) reacting the reaction mixture under conditions including a temperature of 70 to 100° C. such that at least part of the vinyl-functional alcohol and at least part of the hydrolysable silyl hydride react to form the silyl-terminated alcohol, wherein the conversion of vinyl-functional alcohol is at least 90% and the amount of high molecular weight impurities is no greater than 10% of the combined weight of the starting amounts of vinyl-functional alcohol and hydrolysable silyl hydride.
Dependencies are inferred from the claim text.