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采用半连续种子乳液聚合方法合成了自交联丙烯酸酯类反应性微凝胶乳液,研究了聚合工艺条件对聚合反应稳定性的影响。结果表明,当增大乳化剂SDS/OP-10的用量或加快预乳化单体的滴加速度时,聚合反应稳定性增加;随着引发剂过硫酸钾(KPS)、交联剂三羟甲基丙烷三丙烯酸酯(TMPTMA)和单体用量的增加,微凝胶颗粒分子间的交联反应增强,聚合反应稳定性下降。加入功能性单体甲基丙烯酸(MAA)和丙烯酸(AA)都能使聚合反应的稳定性增强,随着MAA用量的增加,聚合反应稳定性呈先增强后下降的趋势。当所加入的SDS/OP-10质量分数为3%~4%、KPS为0.4%~0.6%、TMPTMA为1%~3%、MAA不超过3%及单体为30%~40%,预乳化单体滴加速率为20~30 mL/h时,聚合过程的稳定性最好。由傅里叶变换红外光谱分析可知,通过优化聚合条件,得到了含有官能性环氧基和羧基的丙烯酸酯类反应性微凝胶乳液。
The semi-continuous seed emulsion polymerization was used to synthesize self-crosslinking acrylate microemulsion. The effects of polymerization conditions on the stability of the polymerization reaction were studied. The results showed that when the dosage of emulsifier SDS / OP-10 was increased or the dropping rate of pre-emulsified monomer was increased, the stability of polymerization increased. With the increase of initiator KPS, Propane triacrylate (TMPTMA) and the amount of monomer increases, the cross-linking reaction between microgel particles increases, and the stability of the polymerization decreases. The stability of polymerization reaction can be enhanced by adding MAA and AA. With the increase of MAA dosage, the stability of polymerization reaction firstly increases and then decreases. When the content of SDS / OP-10 is 3% ~ 4%, KPS is 0.4% ~ 0.6%, TMPTMA is 1% ~ 3%, MAA is less than 3% and monomer is 30% ~ 40% Monomer dropping rate of 20 ~ 30 mL / h, the best stability of the polymerization process. From Fourier transform infrared spectroscopy analysis, it can be seen that by optimizing the polymerization conditions, an acrylic reactive microgels emulsion containing functional epoxy groups and carboxyl groups was obtained.