Page 83 - 《精细化工》2023年第1期

第 40 卷第 1 期 精 细 化 工 Vol.40, No.1
20 23 年 1 月 FINE CHEMICALS Jan. 2023

功能材料
P(NVP-DVB)的改性及其检测水中双酚 A 的应用

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张金颐，崔 阳，何 柳，张有来，孟祥太，张舜光
（天津理工大学 化学化工学院，天津 300384）

摘要：为提高水中双酚 A（BPA）检测的准确性，采用两步法制备胺功能化聚(N-乙烯吡咯烷酮-二乙烯苯)
〔P(NVP-DVB)〕吸附剂。采用 SEM、FTIR、BET、TGA 和水接触角测试对两步反应中的样品进行表征，并将
胺功能化 P(NVP-DVB)用于水中 BPA 检测。通过优化实验得到氯甲基化反应的最佳条件为：以多聚甲醛
〔(CH 2 O) n 〕和盐酸为氯化试剂，ZnCl 2 为催化剂，n(HCl)∶n〔(CH 2 O) n 〕∶n(ZnCl 2 )=1∶1∶1，反应温度为 80 ℃，
氯化时间为 3 h，在该条件下制得中间体〔P(NVP-DVB-CH 2 Cl)〕氯含量可达 11.14%；以苯胺为胺化试剂对
2
P(NVP-DVB-CH 2 Cl)进行接枝改性制得的 P(NVP-DVB-苯胺)，其平均孔径为 8.59 nm，比表面积为 590.36 m /g，
热失重率为 70.66%，其对水中 BPA 的回收效果最好，回收率为 99.65%，相对标准偏差为 1.96%，其在模拟水
样和实际水样中应用效果均较好，且回收率比商业吸附剂提高了近 32%。
关键词：P(NVP-DVB)；氯甲基化；胺功能化；双酚 A；固相萃取；回收率；功能材料
中图分类号：TQ424；O625.6 文献标识码：A 文章编号：1003-5214 (2023) 01-0075-12

Modification of P(NVP-DVB) and its application in the
detection of BPA in aqueous solution

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ZHANG Jinyi, CUI Yang, HE Liu, ZHANG Youlai, MENG Xiangtai, ZHANG Shunguang
（School of Chemistry and Chemical Engineering, Tianjin University of Technology, Tianjin 300384, China）

Abstract: To improve the accuracy of bisphenol A (BPA) detection in aqueous solution, a two-step method
was used to prepare amine functionalized poly(N-vinylpyrrolidone-divinylbenzene)[P(NVP-DVB)]
adsorbent. The samples were characterized by SEM, FTIR, BET, TGA and water contact angle test in the
two-step reaction and the amine functionalized P(NVP-DVB) was applied to the detection of BPA in
aqueous solution. The optimal conditions for the chloromethylation reaction were obtained through
optimization experiments: paraformaldehyde [(CH 2O) n] and hydrochloric acid as chlorination reagents and
ZnCl 2 as catalyst, intermediate P(NVP-DVB-CH 2Cl) had a chlorine content up to 11.14% under the
condition of n(HCl)∶n[(CH 2O) n ]∶n(ZnCl 2 )=1∶1∶1, reaction temperature of 80 ℃, chlorination time of
3 h. Aniline as amination reagent was grafted to P(NVP-DVB-CH 2Cl) intermediate to obtain
P(NVP-DVB-aniline). The average pore size of P(NVP-DVB-aniline) was 8.59 nm, the specific surface
2
area was 590.36 m /g, and the thermal mass loss rate was 70.66%. The recovery effect of BPA in aqueous
solution was highest for the P(NVP-DVB-aniline), and the recovery rate was 99.65%, and the relative
standard deviation was 1.96%, and the apply effect was better in both simulated and actual aqueous samples, and
the recovery rate was nearly 32% higher than that of commercial adsorbent.
Key words: P(NVP-DVB); chloromethylation; amine functionalization; bisphenol A; solid phase extraction;
recovery rate; functional materials

[1]
双酚 A（BPA）广泛存在于工业废水、供水管 严重污染 。从当前研究现状来看，过量的 BPA 会
[2]
内层涂料及垃圾填埋场渗透液中，使生活用水受到 给人体带来癌症与肥胖等相关的疾病 。目前，色

收稿日期：2022-05-07; 定用日期：2022-08-04; DOI: 10.13550/j.jxhg.20220443
基金项目：天津市自然科学基金项目（18JCYBJC28500）；天津市教委科研计划项目（2018KJ138）
作者简介： 张金颐（1996—），女，硕士生，E-mail：zhangjinyi@stud.tjut.edu.cn。联系人：张舜光（1981—），男，讲师，E-mail：zsg@tjut.edu.cn。