I bought ultra pure silicon dioxide (Silica) from lobe chemie. many trials have been carried out to functionalize the silica surface with (3-aminopropyl) triethoxysilane. I tried to operate the reaction in methanol, toluene and even in water. Preactivation with sulfuric acid and hydrogen peroxide mixture was also conducted. unfortunately, all these trials were failed. any suggestions?
Md. Abdur Rahman
, good point! What about rehydroxylation of SiO2 by refluxing in HCl?C.f. Supporting information:
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In my personal experience, functionalization of Silica gel with (3-aminopropyl)triethoxysilane is relatively easy to achieve. I suspect your problem may exist in the silica which you bought from lobe chemie. Ultra pure spherical silica with specific particle size, pore diameter and surface area is very important in the functionalization of SiO₂. I suggest you buy spherical silica from Diaso or Fuji in japan. Then preactive in hydrochloric acid for 24 hours, operate the reaction in toluene.
I do not see the advantage to buy a powder. A simple Stober-Synthesis using TEOS in EtOH and ammonia solution (step by step growing (adding TEOS in EtOH) to the desired particle size) and then adding of (3-aminopropyl)triethoxysilane should solve your problem.
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