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US 12,460,052 B2Granted
Poly(diorgano/organohydrogen)siloxane copolymers
AssigneesDow Global Technologies LLC, Dow Silicones Corporation
InventorsMichael Depierro, Xiaoyun Chen, Michael Hausinger
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Abstract
A method for preparing a poly(diorgano/organohydrogen)siloxane copolymer is provided. The method includes use of a vibrational spectroscopy technique.
Claims15
A method for preparing a poly(diorgano/organohydrogen) siloxane copolymer, wherein the method comprises:
- 1) Combining starting materials comprising
- A) a source of siloxane units of formula (R2SiO2/2),
- B) a source of siloxane units of formula (RHSiO2/2),
- where each R is independently selected from the group consisting of a monovalent hydrocarbyl group and a monovalent halogenated hydrocarbyl group, and
- C) an acid catalyst,
- thereby forming a mixture;
- 2) Agitating the mixture at a temperature of 20° C. to 110° C., thereby forming a reaction mixture comprising the poly(diorgano/organohydrogen) siloxane copolymer via equilibration reaction;
- 3) Using a vibrational spectroscopy technique selected from the group consisting of infra-red spectroscopy and Raman spectroscopy to monitor a spectral region including an absorbance band that corresponds to one or both of a concentration of decoupled (RHSiO2/2) and a concentration of coupled (RHSiO2/2) units in the reaction mixture;
- 4) Stopping the equilibration reaction when a target related to the absorbance band is reached.
6 more elements
A method comprising:
- 1) Combining starting materials comprising
- A) a source of siloxane units of formula (R2SiO2/2),
- B) a source of siloxane units of formula (RHSiO2/2),
- where each R is independently selected from the group consisting of a monovalent hydrocarbyl group and a monovalent halogenated hydrocarbyl group, and
- C) an acid catalyst,
- thereby forming a mixture;
- 2) Agitating the mixture at a temperature of 20° C. to 110° C., thereby forming a reaction mixture comprising the poly(diorgano/organohydrogen) siloxane copolymer via equilibration reaction;
- 3) Using a vibrational spectroscopy technique selected from the group consisting of infra-red spectroscopy and Raman spectroscopy to monitor a spectral region including an absorbance band that corresponds to one or both of a concentration of decoupled (RHSiO2/2) and a concentration of coupled (RHSiO2/2) units in the reaction mixture;
- 4) Stopping the equilibration reaction when a target related to the absorbance band is reached, where the target is a rate of change of the absorbance band height or a rate of change of the absorbance band area, and the rate of change has a value of 0% to 10% of its maximum absolute value measurable during the course of the equilibration reaction, thereby preparing a a poly(diorgano/organohydrogen) siloxane copolymer;
- and
- adding the poly(diorgano/organohydrogen) siloxane copolymer as a crosslinker to a curable silicone formulation.
8 more elements
Dependencies are inferred from the claim text.