Elementorganic monomers : technology, properties, by NA

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Raw stock is sent to the apparatus in tanks 1 installed in the drafting device (one is shown in the figure). Then it is sent by nitrogen flow to the batch boxes: trifluoromonochloropropane to batch box 2, trichlorosilane to batch box 3, ethyl bromide to batch box 4, and dibutyl ether (dehydrated with burnt calcium chloride and filtered) to batch box 5. Before the synthesis begins, working mixtures I and II are prepared in apparatus 6. Mixture I consists of trichlorosilane and ethyl bromide, and mixture II consists of trichlorosilane, dibutyl ether, trifluoromonochloropropane and ethyl bromide.

This seems to be due to copper shielding the surface of silicon. A similar situation is observed in the direct synthesis of ethylchlorosilanes. For the direct synthesis of phenylchlorosilanes, copper content in contact mass should be significantly bigger than for the synthesis of methyland ethylchlorosilanes. Good yields of phenylchlorosilanes are attained if catalysed by silver (10% of silicon), but owing to its high cost and scarcity, industrial preference is given to copper. However, the catalytic activity of contact mass is determined not only by copper concentration.

After nitrogen blowing, the process is continued by adding dibutyl ether, switching on the agitator and heating the reactive mixture up to 35 °C with hot water sent into the jacket of the apparatus. After that, all mixture I necessary to start the reaction self-flows into the reactor from batch box 8. When the mixture is added, the temperature of the reactive mixture rises to 80-105 °C. After the temperature stops rising, the jacket is filled with water, and the temperature in the reactor is reduced down to 25-26 °C.

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