乙二胺-N-丙基改性硅胶的可控键合制备及其在银杏酸脱除中的应用研究

doi:10.3976/j.issn.1002-4026.20230063

山东科学 ›› 2024, Vol. 37 ›› Issue (1): 51-58.doi: 10.3976/j.issn.1002-4026.20230063

乙二胺-N-丙基改性硅胶的可控键合制备及其在银杏酸脱除中的应用研究

潘翔宇(), 靳钊(), 关彤, 陈贝怡

青岛科技大学高分子科学与工程学院,山东青岛 266045

收稿日期:2023-04-14 出版日期:2024-02-20 发布日期:2024-01-26
通信作者: 靳钊 E-mail:1342478509@qq.com;jinzhao@qust.edu.cn
作者简介:潘翔宇(1998—),男,硕士研究生,研究方向为功能化色谱填料的研究。E-mail:1342478509@qq.com

Controllable bonding preparation of ethylenediamine-N-propyl modified silica gel and its application in ginkgolic acid removal

PAN Xiangyu(), JIN Zhao(), GUAN Tong, CHEN Beiyi

School of Polymer Science and Engineering, Qingdao University of Science and Technology, Qingdao 266045, China

Received:2023-04-14 Online:2024-02-20 Published:2024-01-26
Contact: JIN Zhao E-mail:1342478509@qq.com;jinzhao@qust.edu.cn

摘要/Abstract

摘要：

优化了乙二胺-N-丙基键合硅胶(PSA)键合量可控的制备工艺,考察了PSA制备的批次重复性,并进行PSA制备的中试放大实验。采用红外光谱、元素分析及电位滴定法对所制备的PSA进行性能评价,结果表明:在3 460 cm^-1处出现了N—H伸缩振动峰,在2 960 cm^-1和2 860 cm^-1处出现了—CH的不对称和对称伸缩振动峰,708 cm^-1处出现了—NH₂的变形振动吸收峰,表明乙二胺-N-丙基成功接枝到硅胶表面;随着制备体系中硅烷化试剂比例的增加,碳、氮和氢元素的含量以及电位滴定法得到的离子交换容量均呈现上升趋势,说明乙二胺-N-丙基官能团的键合量逐渐增加。将制备的PSA填充成分离纯化小柱,考察了不同键合量PSA对银杏叶提取物中银杏酸的脱除效率,结果表明:PSA对银杏酸有强吸附能力,可应用于银杏叶提取物中银杏酸的脱除,2^#、3^#、4^#和5^#PSA分离纯化柱的最大上样体积分别为21、22、23、24 mL,且脱除效率随乙二胺-N-丙基键合量的增加而升高。

关键词: 乙二胺-N-丙基改性硅胶, 键合量, 银杏酸脱除

Abstract:

In this paper, the preparation process of N-propylethylenediamine bonded silica gel (PSA) with controllable bonding amount was optimized; the batch repeatability of PSA preparation was examined; and the pilot scale-up experiment of PSA preparation was conducted. The properties of the PSA were investigated by infrared spectroscopy, elemental analysis, and potentiometric titration. The results showed that N—H stretching vibration peaks appeared at 3 460 cm^-1, asymmetric and symmetric stretching vibration peaks of —CH appeared at 2 960 cm^-1 and 2 860 cm^-1, and deformation vibration absorption peaks of —NH₂appeared at 708 cm^-1, indicating that N-propylethylenediamine was successfully grafted onto the surface of silica gel.Furthermore, with the increasing proportion of silane reagent in the preparation system, the content of carbon, nitrogen, and hydrogen elements and the ion exchange capacity obtained by potentiometric titration showed an upward trend, indicating that the bonding amount of ethylenediamine-N-propyl functional group gradually increased. Moreover, the prepared PSA packing component was separated from the purification column, and the removal efficiency of ginkgolic acid from the extract of ginkgo biloba leaves using PSA with different bonding amounts was investigated. The results showed that PSA had a strong adsorption capacity for ginkgolic acid and could be used to remove ginkgolic acid from the extract of ginkgo biloba leaves, the maximum sample loading volumes for PSA separation and purification columns 2^#, 3^#, 4^#, and 5^# are 21, 22, 23, 24 mL, respectively. In addition, the removal efficiency was found to increase with the increasing amount of ethylenediamine-N-propyl bonding.

Key words: ethylenediamine-N-propyl modified silica gel, bonding quantity, ginkgo acid removal

中图分类号:

O658

潘翔宇, 靳钊, 关彤, 陈贝怡. 乙二胺-N-丙基改性硅胶的可控键合制备及其在银杏酸脱除中的应用研究[J]. 山东科学, 2024, 37(1): 51-58.

PAN Xiangyu, JIN Zhao, GUAN Tong, CHEN Beiyi. Controllable bonding preparation of ethylenediamine-N-propyl modified silica gel and its application in ginkgolic acid removal[J]. Shandong Science, 2024, 37(1): 51-58.

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PSA编号	离子交换容量/(mmol·g^-1)	相对标准偏差(RSD)/%
批次1	2.31	0.7
批次2	2.29
批次3	2.34
商品化	1.94

PSA编号	元素质量分数/%
PSA编号	N	C	H
批次1	2.83	6.48	1.65
批次2	2.79	6.37	1.71
批次3	3.31	7.46	2.03
安捷伦	2.73	6.47	1.77

乙二胺-N-丙基改性硅胶的可控键合制备及其在银杏酸脱除中的应用研究

Controllable bonding preparation of ethylenediamine-N-propyl modified silica gel and its application in ginkgolic acid removal

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