Method of forming polyhedral oligomeric silsesquioxane compounds
View Patent ↗A mixture of at least two polyhedral oligomeric silsesquioxane (POSS) compounds is formed in the presence of rhenium on cerium(IV) oxide. The POSS compounds are formed utilizing a method that includes the step of combining (a) a trihalosilane, (b) hydrogen gas, and (c) the rhenium on cerium(IV) oxide, in a reactor at a temperature of from 250° C. to 600° C. to form the mixture. The trihalosilane has the formula RSiX 3 wherein R is an alkyl group having from 1 to 4 carbon atoms, an aryl group, and wherein X is a halo atom. This method allows for the efficient, predictable, and accurate production of the POSS compounds with a minimized need for use of expensive separation techniques. In addition, this method produces the POSS compounds in commercially useful quantities as major reaction products thereby avoiding the need to run multiple reactions.
1. A method of forming a mixture comprising at least two polyhedral oligomeric silsesquioxane (POSS) compounds in the presence of rhenium on cerium(IV) oxide, said method comprising the step of combining (a) a trihalosilane, (b) hydrogen gas, and (c) the rhenium on cerium(IV) oxide in a reactor at a temperature of from 250° C. to 600° C. to form the mixture, wherein the (a) trihalosilane has the formula RSiX 3 , R is an alkyl group having from 1 to 4 carbon atoms or an aryl group, and X is a halo atom.
2. A method as set forth in claim 1 wherein each of the at least two POSS compounds is fully condensed.
3. A method as set forth in claim 1 wherein each of the at least two POSS compounds independently has the formula (RSiO 1.5 ) n wherein R is an alkyl group having from 1 to 4 carbon atoms and n is 6, 8, 10, or 12.
4. A method as set forth in claim 1 wherein at least one POSS compound has the formula (RSiO 1.5 ) n wherein R is an alkyl group having from 1 to 4 carbon atoms and n is 6, 8, 10, or 12.
5. A method as set forth in claim 1 wherein at least one POSS compound has the formula (RSiO 1.5 ) n wherein R is a methyl group and n is 6, 8, 10, or 12.
6. A method as set forth in claim 1 wherein the mixture consists essentially of three POSS compounds wherein each POSS compound independently has the formula (RSiO 1.5 ) n wherein R is an alkyl group having from 1 to 4 carbon atoms and wherein n is 6 for a first POSS compound, 8 for a second POSS compound, and 10 for a third POSS compound.
7. A method as set forth in claim 1 wherein the trihalosilane is further defined as CH 3 SiCl 3 .
8. A method as set forth in claim 1 further comprising the step of separating one of the POSS compounds from the mixture via sublimation.
9. A method as set forth in claim 1 further comprising the step of reactivating the rhenium on cerium(IV) oxide after the mixture is formed.
10. A method as set forth in claim 9 wherein the step of reactivating occurs in a second reactor.
11. A method as set forth in claim 1 further comprising the step of adding an additional amount of the rhenium on cerium(IV) oxide to the reactor after the step of combining.
12. A method as set forth in claim 1 wherein the process is further defined as continuous and the reactor is further defined as a fluidized bed reactor.
13. A method as set forth in claim 1 wherein the reactor is operated at a pressure that exceeds atmospheric pressure.
14. A method as set forth in claim 1 further comprising the step of removing the POSS compounds from the reactor.
15. A method as set forth in claim 1 wherein the mixture comprises at least three polyhedral oligomeric silsesquioxane (POSS) compounds, wherein the (a) trihalosilane is further defined as CH 3 SiCl 3 , wherein each POSS compound independently has the formula (CH 3 SiO 1.5 ) n , and wherein n is 6 for a first POSS compound, 8 for a second POSS compound, and 10 for a third POSS compound.
16. A method as set forth in claim 15 wherein the mixture consists essentially of the first, second, and third POSS compounds.
17. A method as set forth in claim 15 further comprising the step of separating one of the POSS compounds from the mixture via sublimation.
18. A method as set forth in claim 15 further comprising the step of reactivating the rhenium on cerium(IV) oxide after the mixture is formed.
19. A method as set forth in claim 18 wherein the step of reactivating occurs in a second reactor.
20. A method as set forth in claim 15 further comprising the step of adding an additional amount of the rhenium on cerium(IV) oxide to the reactor after the step of combining.
21. A method as set forth in claim 15 wherein the process is further defined as continuous and the reactor is further defined as a fluidized bed reactor.