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The purification of Methyltris(methyl ethyl ketoxime) silane mainly involves physical separation, chemical neutralization, and refining processes. The commonly used methods include:
During the reaction, by controlling conditions such as temperature and stirring speed, methyltris(methyl ethyl ketoxime) silane and unreacted substances separate into two phases.
Upper phase: Crude product (containing silane and unreacted materials)
Lower phase: Precipitate of methyl ethyl ketoxime hydrochloride
After separation, the crude product is subjected to neutralization and evaporation treatments.
Neutralization reaction: The crude product is reacted with ammonia gas, converting methyl ethyl ketoxime hydrochloride into ammonium chloride precipitate. Solid impurities are removed by filtration.
Filtration separation: The neutralized liquid is processed with a thin-film evaporator to remove solvents and unreacted substances, yielding high-purity silane.
Ultrasonic extraction: Utilizes ultrasonic energy to enhance solubility differences between silane and impurities, achieving rapid separation.
Liquid–liquid extraction: By adjusting the density difference between the extractant (e.g., n-hexane) and the reaction mixture, silane can be selectively extracted.
Using cation-modified polyethersulfone membranes with quaternary ammonium groups to adsorb and remove hydrolysis products such as methyltrihydroxysilane, thereby improving silane purity.
Through repeated evaporation and condensation steps, residual solvents and trace impurities are gradually removed. For example, solvents are first evaporated under high pressure, followed by vacuum distillation, ultimately obtaining high-purity silane.