P(NVP-DVB)的改性及其检测水中双酚A的应用

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

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〔(CH2O)n〕和盐酸为氯化试剂，ZnCl2为催化剂，n(HCl):n〔(CH2O)n〕:n(催化剂)=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-CH2Cl)〕氯含量可达11.14%；以苯胺为胺化试剂对P(NVP-DVB-CH2Cl)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 m2/g，苯胺的热失重率为81.11%，其对水中BPA的回收效果最好，回收率为99.65%，相对标准偏差（RSD）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近20%。

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)〕 adsorbents. The samples were characterized by SEM, FTIR, BET, TGA, and water contact angle test.in the two-step reaction and the amine functionalized N-vinylpyrrolidone-divinylbenzene was applied to the detection of BPA in aqueous solution. The optimal conditions for the chloromethylation reaction were obtained through optimization experiments: we used paraformaldehyde 〔(CH2O)n〕and hydrochloric acid as the chlorination reagents and finally synthesized intermediates 〔P(NVP-DVB-CH2Cl)〕with chlorine content up to 11.14% under the condition of n(HCl): n〔(CH2O)n〕: n(catalyst)=1:1:1, here we used ZnCl2 as the catalyst, the reaction temperature is 80℃, the chlorination time is 3 h; aniline as amination reagent was grafted to P(NVP-DVB-CH2Cl) intermediates to obtain P(NVP-DVB-aniline), the average pore size was 8.59 nm,the specific surface area was 590.36 m2/g, and the thermal weight loss rate of aniline was 81.11%. The recovery effect rate 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 20 percentage points higher than that of commercial adsorbents, and the adsorption effect of BPA in aqueous solution was better.