A kind of preparation method of naphthyl alkoxysilane monomer
A technology of naphthylalkoxysilane and alkoxysilane, which is applied in the field of preparation of naphthylalkoxysilane monomers, can solve problems such as environmental pollution and a large number of high-cost solvents, reduce solvent consumption, and facilitate cleaning The effect of production and steaming cost
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Embodiment 1
[0021] Synthesis and Purification of Naphthyltrimethoxysilane
[0022] 1) Synthesis of naphthyltrimethoxysilane: add 8.2g (0.36mol) sodium flakes, 100ml tetramethoxy Heat the silane to 70°C; keep the temperature at 70°C, add 25ml of 1-bromonaphthalene to the constant pressure dropping funnel, and slowly drop it into the four-neck bottle, control the dropping speed, after dropping, raise the temperature to 80°C for 2 hours ; Cool down to 50°C. 8.3ml of tetrachlorosilane was added dropwise, stirred and refluxed, and the reaction temperature was controlled not to exceed 80°C. The reddish-brown crude product was filtered by suction. The reddish-brown crude product was distilled to remove the remaining tetramethoxysilane under normal pressure, then distilled under reduced pressure, and the fraction at 130-135°C was collected at 5 mmHg to obtain 25 g of the crude product of naphthyltrimethoxysilane.
[0023] 2) Purification of naphthyltrimethoxysilane: Add 20 g of the crude produ...
Embodiment 2
[0025] Synthesis and Purification of Naphthylmethyldimethoxysilane
[0026] 1) Synthesis of naphthylmethyldimethoxysilane: Add 8.2g of sodium flakes and 100ml of methyltrimethoxysilane to a four-neck flask equipped with a mechanical stirrer, a thermometer, a constant pressure dropping funnel and a spherical condenser And heat to 75°C; keep the temperature at 75°C, add 25ml of 1-bromonaphthalene into the constant pressure dropping funnel, and slowly drop it into the four-necked bottle, control the dropping speed, after the drop, raise the temperature to 80°C for 1 hour ; Cool down to 50°C. 8.3ml of tetrachlorosilane was added dropwise, stirred and refluxed, and the reaction temperature was controlled not to exceed 80°C. The reddish-brown crude product was filtered by suction. Then filter the mixed solution obtained after the reaction, and distill the resulting solution under normal pressure to remove the remaining methyltrimethoxysilane, distill under reduced pressure, collec...
Embodiment 3
[0029] Synthesis and Purification of Naphthyltriethoxysilane
[0030] 1) Synthesis of naphthyltriethoxysilane: Add 8.2g of sodium flakes and 100ml of tetraethoxysilane to a 1L four-neck flask equipped with a mechanical stirrer, a thermometer, a constant pressure dropping funnel and a spherical condenser and heat to 70°C; keep the temperature at 70°C, add 25ml of 1-bromonaphthalene into the constant pressure dropping funnel, and slowly drop it into the four-neck bottle, control the dropping speed, after the drop, raise the temperature to 70°C for 2 hours; 8.3ml of tetrachlorosilane was added dropwise, stirred and refluxed, and the reaction temperature was controlled not to exceed 80°C. Then filter the mixed liquid obtained after the reaction, and distill the resulting liquid under normal pressure to remove the remaining tetraethoxysilane, distill under reduced pressure, collect 150-135 ° C fractions at 5 mmHg to obtain naphthyl triethoxysilane The crude product is 30g.
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