Synthesis of SiCl4 via the Chloride Salt-Catalyzed Reaction of Orthosilicates with SOCl2

This paper details a method to chlorinate tetraalkyl orthosilicates in the presence of a catalyst using SOCl2 as the chloride source/deoxygenating agent. Several inexpensive catalysts were screened, and it was found that soluble chloride salts performed better than Lewis base catalysts. The optimize...

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Bibliographic Details
Published inIndustrial & engineering chemistry research Vol. 56; no. 40; pp. 11652 - 11655
Main Authors Roberts, John M, Placke, Jessica L, Eldred, Donald V, Katsoulis, Dimitris E
Format Journal Article
LanguageEnglish
Published American Chemical Society 11.10.2017
Subjects
catalysts
chlorides
Lewis bases
process design
reaction mechanisms
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ISSN0888-5885
1520-5045
1520-5045
DOI10.1021/acs.iecr.7b03301

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Summary:This paper details a method to chlorinate tetraalkyl orthosilicates in the presence of a catalyst using SOCl2 as the chloride source/deoxygenating agent. Several inexpensive catalysts were screened, and it was found that soluble chloride salts performed better than Lewis base catalysts. The optimized reaction employed a widely used and commercially available soluble chloride salt catalyst (e.g., NBu4Cl, 0.4 equiv), 16 equiv of SOCl2, and afforded quantitative yield of SiCl4 after 3 h. As the bulk of the orthosilicate substrate increased, the yield of SiCl4 decreased. A reaction mechanism has been proposed.
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ISSN:0888-5885
1520-5045
1520-5045
DOI:10.1021/acs.iecr.7b03301