水热辅助sol-gel法制备冠醚改性硅胶及在DGT技术中的应用  

Hydrothermal assisted sol-gel process derived crown ether-modified silica and its application on DGT technique

作　　者：李大武 尤楠 LI Da-wu;YOU Nan(Department of Trace Examination,National Police University of China,Shenyang 110035,China;Key Laboratory of Impression Evidence Examination and Identification Technology,Ministry of Public Security, Shenyang 110035,China;College of Petrochemical Engineering,Liaoning Shihua University,Fushun 113001,China)

机构地区：[1]中国刑事警察学院痕迹检验技术系,辽宁沈阳110035 [2]痕迹检验鉴定技术公安部重点实验室,辽宁沈阳110035 [3]辽宁石油化工大学石化学院,辽宁抚顺113001

出　　处：《化学研究与应用》2021年第10期1877-1882,共6页Chemical Research and Application

基　　金：国家自然科学基金项目(21477082)资助;上海市刑事科学技术研究院现场物证重点实验室开放课题项目(2016XCW2K03)资助;痕迹检验鉴定技术公安部重点实验室(中国刑事警察学院)(2021002)资助。

摘　　要：本文采用水热辅助溶胶-凝胶法制备了一种高容量的冠醚改性硅胶,实验采用傅立叶红外光谱、扫描电镜、热重和氮气吸附等方法对其进行表征,并应用薄膜扩散梯度(DGT)技术,采集水环境中有效态Ca^(2+)离子。结果表明,水热辅助溶胶-凝胶法能够显著提高冠醚改性硅胶的吸附容量,与溶胶-凝胶法相比,吸附容量提高了1.5倍;基于该方法所制备的冠醚改性硅胶的DGT装置对Ca^(2+)离子的累积过程完全符合DGT技术的理论方程;应用结果表明,水热辅助溶胶-凝胶法制备的冠醚改性硅胶更适合作为DGT的结合相用于采集环境中的Ca^(2+)离子。Calcium(Ca^(2+))ion is one of key elements for the plant nutrition.An understanding of Ca^(2+) concentration in soil solutions may be useful for improving agricultural practices.A specific sorbent for binding Ca^(2+)ions,the crown ether-modified silica with high capacity,was prepared using a hydrothermal-assisted sol-gel method,characterized by Fourier transmission infrared spectrum,scanning electron microscopy and nitrogen adsorption,and applied to diffusive gradients in thin-films(DGT)technique for sampling available Ca^(2+).The results showed that the prepared sorbents with high adsorption capacity was 1.5 times as much as that of the sorbents from sol-gel method which was improved significantly by hydrothermal-assisted process due to high the reaction efficiency.The experiment values of the Ca^(2+) uptake by diffusive gradients in thin-films(DGT)technique based on the crown ether-modified silica derived from hydrothermal-assisted sol-gel method agreed well the theoretical calculated values from DGT equation.The application results indicated that the crown ether-modified silica derived from hydrothermal-assisted sol-gel method was more suitable as the DGT binding agent.

关 键 词：冠醚 硅胶 钙 薄膜扩散梯度 

分 类 号：O655[理学—分析化学]