伯仲胺基团修饰Fe3O4磁性材料的制备和性能表征

Preparation and performance characterization of primary secondary amine-modified Fe3O4 magnetic materials

  • 摘要: 食品中的有机酸等内源性物质会干扰其中痕量残留物的检测,为消除此影响,以N-β-(氨乙基)-γ-氨丙基三甲氧基硅烷(KH792)为氨基化试剂,直接修饰酸化后的Fe3O4得到磁性吸附材料。经响应面试验优化得到KH792对酸化Fe3O4的最佳修饰条件为温度 82.5℃、pH=4.9,KH792添加量 1.8 mL,在最佳条件下,KH792直接修饰的酸化Fe3O4对没食子酸吸附量为22.8 mg/g,比市售Fe3O4提高了188%,且具备快速固液分离的能力、良好的稳定性及分散性。通过BET、Zeta电位、FTIR和XPS对直接修饰的产物性能进行了表征,结果表明,KH792与Fe3O4表面羟基通过Fe—O—Si键结合,酸化提高了Fe3O4表面羟基含量,因此也增强了KH792对Fe3O4的修饰效果,本文制备的磁性产物可用于净化复杂样品基质中的有机酸。

     

    Abstract: Endogenous substances, such as organic acids in food, can interfere with the detection of trace residues. To eliminate this effect, the magnetic adsorbent material was obtained by directly modifying acidified Fe3O4 with N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane (KH792) as an amination reagent. The optimal modification condition of KH792 for acidified Fe3O4 was optimized by response surface methodology, which was 82.5℃, pH=4.9, and KH792 addition of 1.8 mL. Under these optimal conditions, the acidified Fe3O4 directly modified by KH792 has an adsorption capacity of 22.8 mg/g and shows a 188% increase in the adsorption capacity of the gallic acid compared to commercially available Fe3O4. Additionally, the modified Fe3O4 exhibits excellent performances of rapid solid-liquid separation, good stability, and dispersibility. The properties of the directly modified products were characterized by BET, Zeta potential, FTIR, and XPS. The results show that KH792 bonds on Fe3O4 surface hydroxyl group's by Fe—O—Si bonding, and acidification improves the number of hydroxyl groups on Fe3O4 surface, thus improving the KH792 modification for Fe3O4. The magnetic products prepared in this work can be used for the purification of organic acids in complex sample matrices.

     

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