Tetraethoxysilane → Tetraethoxysilane

1.01 g tetraethylorthosilicate, 2.0 g deionized water, and 0.41 g germanium ethoxide were mixed together in a tared 23 mL Teflon liner. Then 0.42 g of 1,4,8,11-tetramethyl-1,4,8,11-tetraazacyclotetradecane (Strem Chemicals) was dissolved in the mixture. The Teflon container was then capped, sealed, and placed within an 23-mL steel Parr autoclave. The autoclave was allowed to remain at room temperature for 2 days during which time the TEOS and germanium ethoxide were allowed to hydrolyze. The Teflon cup was then removed from the autoclave and 0.13 g 50% HF was added and mixed to create a white viscous gel. The ethanol (formed from the hydrolysis of the TEOS and germanium oxide) and water were allowed to evaporate within a vented hood with flowing air over the course of 3-4 days. Sufficient water was added and mixed into the gel to bring the molar ratio H2O/(Si+Ge) to 7. The liner was then capped and placed within a Parr Steel autoclave reactor. The autoclave was then fixed in a rotating spit within an oven heated at 160° C. for 10 days. The solid products were recovered from the cooled reactor by vacuum filtration and washed with copious quantities of water.

1. customsealed
2. customThe Teflon cup was then removed from the autoclave and 0.13 g 50% HF
3. additionwas added
4. additionmixed

ORD-Eintrag

ord-8d44390428f44ba6a6ed232acbbc61e3

Quelldatensatz

uspto-grants-2011_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07906101B2