聚苯胺/石墨烯涂覆型阴离子交换固定相的制备及表征

doi:10.3724/SP.J.1123.2019.08034

色谱 ›› 2020, Vol. 38 ›› Issue (4): 458-463.DOI: 10.3724/SP.J.1123.2019.08034

聚苯胺/石墨烯涂覆型阴离子交换固定相的制备及表征

刘军伟¹^,^*(), 孙言¹, 于文浩¹, 王超威¹, 李振兴¹, 孙雨安¹, 张书胜², 朱岩³^,^*()

1. 郑州轻工业大学应用化学系,河南郑州 450002
2. 郑州大学现代分析与基因测序中心,河南郑州 450001
3. 浙江大学化学系,浙江杭州 310028

收稿日期:2019-08-27 出版日期:2020-04-08 发布日期:2020-12-10
通讯作者: 刘军伟,朱岩
基金资助:
郑州轻工业大学博士基金项目(2017BSJJ037)

Preparation and characterization of polyaniline/graphene-coated anion-exchange chromatographic stationary phase

LIU Junwei¹^,^*(), SUN Yan¹, YU Wenhao¹, WANG Chaowei¹, LI Zhenxing¹, SUN Yu’an¹, ZHANG Shusheng², ZHU Yan³^,^*()

1. Department of Applied Chemistry, Zhengzhou University of Light Industry, Zhengzhou 450002, China
2. Center of Advanced Analysis and Gene Sequencing, Zhengzhou University, Zhengzhou 450001, China
3. Department of Chemistry, Zhejiang University, Hangzhou 310028, China

Received:2019-08-27 Online:2020-04-08 Published:2020-12-10
Contact: LIU Junwei, ZHU Yan
Supported by:
Doctoral Fund of Zhengzhou University of Light Industry(2017BSJJ037)

摘要/Abstract

摘要：

该文以聚苯胺/石墨烯复合材料为涂覆材料,制备了一种涂覆型阴离子交换固定相。首先以苯胺和石墨烯为原料制备聚苯胺/石墨烯复合材料,并通过物理吸附涂覆在聚苯乙烯-二乙烯苯微球表面;然后以聚苯胺中的氮原子为反应位点,通过季铵化制备一系列具有不同交换容量的涂覆型阴离子交换固定相。通过扫描电镜(SEM)、傅里叶红外光谱(FT-IR)和元素分析(EA)对该涂覆型阴离子交换固定相进行表征,结果表明聚苯胺/石墨烯成功地涂覆在微球表面且发生了季铵化。通过分离常规阴离子和有机酸,对自制阴离子交换色谱柱的色谱性能进行评价。结果显示,8次季铵化的聚苯胺/石墨烯涂覆聚苯乙烯-二乙烯苯阴离子交换色谱柱对常规阴离子和有机酸呈现良好的分离效果。

关键词: 聚苯胺/石墨烯, 聚苯乙烯-二乙烯苯, 季铵化, 阴离子交换, 固定相

Abstract:

A polyaniline/graphene (PANI/G) composite was selected as the coating material to prepare a coated anion-exchange chromatographic stationary phase. First, aniline and graphene were used to prepare the PANI/G composite, which was coated onto the surface of poly(styrene-divinylbenzene) (PS-DVB) microspheres by physical absorption. Then, a series of anion-exchange stationary phases with different exchange capacities were obtained by quaternization using the nitrogen atom of polyaniline as the reactive site. The stationary phase was characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), and elemental analysis (EA). The results revealed that PANI/G was successfully coated onto the surface of PS-DVB and quaternized. The efficiency of the self-fabricated chromatographic column was evaluated by separating conventional anions and organic acids. The PANI/G-coated PS-DVB anion-exchange chromatographic column that was quaternized eight times showed good separation performance for conventional anions and organic acids.

Key words: polyaniline/graphene (PANI/G), poly(styrene-divinylbenzene) (PS-DVB), quaternization, anion-exchange, stationary phase

中图分类号:

O658

刘军伟, 孙言, 于文浩, 王超威, 李振兴, 孙雨安, 张书胜, 朱岩. 聚苯胺/石墨烯涂覆型阴离子交换固定相的制备及表征[J]. 色谱, 2020, 38(4): 458-463.

LIU Junwei, SUN Yan, YU Wenhao, WANG Chaowei, LI Zhenxing, SUN Yu’an, ZHANG Shusheng, ZHU Yan. Preparation and characterization of polyaniline/graphene-coated anion-exchange chromatographic stationary phase[J]. Chinese Journal of Chromatography, 2020, 38(4): 458-463.

图/表 4

图1 (a, b)PS-DVB微球和(c)聚苯胺/石墨烯涂覆PS-DVB微球的扫描电镜图

Fig. 1 Scanning electron micrographs of (a, b) PS-DVB microspheres and (c) PANI/G coated PS-DVB microspheres PS-DVB: poly(styrene-divinylbenzene); PANI/G: polyaniline/graphene.

图2 (a)PS-DVB、(b)聚苯胺/石墨烯涂覆型PS-DVB及其 (c)2次、(d)4次、(e)6次和(f)8次季铵化聚苯胺/石墨烯涂覆PS-DVB的红外光谱图

Fig. 2 FT-IR spectra of (a) PS-DVB, (b) PANI/G coated PS-DVB, and PANI/G coated PS-DVB quaternized (c) twice, (d) quartic, (e) sextic, and (f) eight times

图3 8次季铵化聚苯胺/石墨烯涂覆型固定相对6种常规阴离子的分离

Fig. 3 Separation of six conventional anions by PANI/G coated stationary phase quaternized eight-times Mobile phase: 4.5 mmol/L Na2CO3+0.8mmol/L NaHCO3; flow rate: 1.0 mL/min; injection volume: 25 μL. Peak Nos.: 1. F- (0.2 mmol/L); 2. Cl- (0.2 mmol/L); 3. N O 2 - (0.2 mmol/L); 4. Br- (0.2 mmol/L); 5. N O 3 - (0.2 mmol/L); 6. S O 4 2 - (0.2 mmol/L).

图4 8次季铵化聚苯胺/石墨烯涂覆型固定相对4种有机酸的分离

Fig. 4 Separation of four organic acids by PANI/G coated stationary phase quaternized eight times Mobile phase: 4.5 mmol/L Na2CO3+0.8mmol/L NaHCO3; flow rate: 1.0 mL/min; injection volume: 25 μL. Peak Nos.: 1. acetic acid (2.0 mmol/L); 2. formic acid (2.0 mmol/L); 3. propionic acid (5.0 mmol/L); 4. butyric acid (1.0 mmol/L).

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聚苯胺/石墨烯涂覆型阴离子交换固定相的制备及表征

Preparation and characterization of polyaniline/graphene-coated anion-exchange chromatographic stationary phase

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