伯仲胺基团修饰Fe_(3)O_(4)磁性材料的制备和性能表征  

Preparation and performance characterization of primary secondary amine-modified Fe_(3)O_(4)magnetic materials

作　　者：周书威 傅红[2] 杨方 ZHOU Shuwei;FU Hong;YANG Fang(Fuzhou Customs Technical Center,Fuzhou 350001,China;College of Biological Science and Engineering,Fuzhou University,Fuzhou 350108,China)

机构地区：[1]福州海关技术中心,福州350001 [2]福州大学生物科学与工程学院,福州350108

出　　处：《复合材料学报》2024年第4期1977-1986,共10页Acta Materiae Compositae Sinica

基　　金：国家重点研发专项(2017YFF0211304);福建省自然基金项目(2020J01098)。

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Fe_(3)O_(4)得到磁性吸附材料。经响应面试验优化得到KH792对酸化Fe_(3)O_(4)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Fe_(3)O_(4)对没食子酸吸附量为22.8 mg/g,比市售Fe_(3)O_(4)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Fe_(3)O_(4)表面羟基通过Fe−O−Si键结合,酸化提高了Fe_(3)O_(4)表面羟基含量,因此也增强了KH792对Fe_(3)O_(4)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。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 Fe_(3)O_(4)with N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane(KH792)as an amination reagent.The optimal modification condition of KH792 for acidified Fe_(3)O_(4)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 Fe_(3)O_(4)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 Fe_(3)O_(4).Additionally,the modified Fe_(3)O_(4)exhibits excellent performances of rapid solidliquid 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 Fe_(3)O_(4)surface hydroxyl group's by Fe−O−Si bonding,and acidification improves the number of hydroxyl groups on Fe_(3)O_(4)surface,thus improving the KH792 modification for Fe_(3)O_(4).The magnetic products prepared in this work can be used for the purification of organic acids in complex sample matrices.

关 键 词：N-β-(氨乙基)-γ-氨丙基三甲氧基硅烷 酸化Fe_(3)O_(4) 直接修饰法 磁性吸附材料 修饰机制 

分 类 号：TB331[一般工业技术—材料科学与工程]