Ethanol → Tetraethoxysilane

Participants

Reaction Steps

The preparation of triethoxysilane was carried out in a reactor having working capacity of 9 L, which was equipped with an electric heating control device of reaction capacity, and an impeller stirrer having 4 wings to control rotational speed to 300-1500 rpm. 3.3 kg of metal silicon was ground in a solvent environment of 6.6 kg of THERMINOL® 66 using Planetary Mill until the particle size is 30-100 μm. In the pulverizing process, 0.2 kg of CuCl catalyst was put into the suspension. In the state of continuous operation of the stirrer at 850 rpm, contact mass was heated to temperature of 242+2° C., the feed of ethanol as anhydrous alcohol to the reactor was started at 600 ml/hr using dosing pump (Digital dosing pump), GRUNDFOS® DME 60-10 AR. Samples were taken when liquid product was generated in the reactor, then every 30 minutes. As a result of analysis of the samples in Gas chromathograph, Agilent® GC7890A, synthesis reaction was started 10 minutes after alcohol was poured, and reaction rate increased for initial 60 minutes. The synthesis reaction rate of triethoxysilane decreased after 180 minutes, and completely slowed down 260 minutes after alcohol was fed. Herein, 1635 g of triethoxysilane and 105 g of tetraethoxysilane were obtained. The selectivity of triethoxysilane was 94%.

Provenance & Evidence