Method for synthesizing silane coupler
A technology of silane coupling agent and monohalogenated alkane, which is applied in the field of synthesis of organosilicon monomers, can solve problems such as difficult separation, high price, and dangerous operation, and achieve simple separation and purification process, easy operation, and reduced side reactions Effect
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Embodiment 1
[0026] Embodiment 1: the synthesis of cyclohexyltriethoxysilane
[0027] Tetraethoxysilane, chlorocyclohexane and iodine are dried with anhydrous calcium chloride and set aside; the magnesium powder is soaked with acetone to remove oil stains, poured out the acetone, and then soaked with 1-2% hydrochloric acid for 5- After 10 minutes, filter out the magnesium, wash with ethanol once more, dry quickly, and set aside.
[0028] Add 416 (2mol) tetraethoxysilane, 24g (1.2mol) magnesium and 2g (0.01mol) iodine into a 1000ml three-necked flask, stir (about 100r / min) and heat up under nitrogen protection. When the temperature reached 151±1°C, 118.5 g (1.0 mol) of chlorocyclohexane was added dropwise, and the addition was completed in about 1.5 hours. Subsequently, the reaction was continued at 150±1° C. for 2 h, and then the reaction was terminated. The generated magnesium salt was filtered off, and the filtrate was poured into a distillation flask to evaporate tetraethoxysilane and...
Embodiment 2
[0029] Embodiment 2: the synthesis of cyclohexyltriethoxysilane
[0030] The method pretreatment raw material by the embodiment 1, standby.
[0031] Add 312g (1.5mol) of tetraethoxysilane, 28.8g (1.2mol) of magnesium and 0.2g (0.001mol) of iodine into a 1000ml three-necked flask. Stir (approximately 100r / min) and heat up under nitrogen protection. When the temperature reached 180±1°C, 118.5 g (1.0 mol) of chlorocyclohexane began to be added dropwise, and the addition was completed in about 1.5 hours. Subsequently, the reaction was continued at 120±1° C. for 5 h, and then the reaction was terminated. The generated magnesium salt was filtered off, and the filtrate was poured into a distillation flask to evaporate tetraethoxysilane and iodine to obtain a crude product of cyclohexyltriethoxysilane. Then, the crude product was purified by rectification to obtain a colorless and transparent cyclohexyltriethoxysilane (boiling point: 253°C) with a yield of 97% and a purity of 99.5%...
Embodiment 3
[0032] Embodiment 3: the synthesis of cyclopentyltriethoxysilane
[0033] The method pretreatment raw material by the embodiment 1, standby.
[0034] Add 312g (1.5mol) of tetraethoxysilane, 26.4g (1.1mol) of magnesium and 0.2g (0.001mol) of iodine into a 1000ml three-necked flask. Stir (approximately 100r / min) and heat up under nitrogen protection. When the temperature reached 165±1°C, 105 g (1.0 mol) of chlorocyclopentane was added dropwise, and the addition was completed in about 1.5 hours. , about 1.5h dropwise completed. Subsequently, the reaction was continued at 130±1° C. for 3.5 h, and then the reaction was terminated. The generated magnesium salt was filtered off, and the filtrate was poured into a distillation flask to evaporate tetraethoxysilane and iodine to obtain a crude product of cyclohexyltriethoxysilane. Then, the crude product was purified by rectification to obtain a colorless and transparent cyclohexyltriethoxysilane (boiling point: 230°C) with a yield ...
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