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利用丙烯酸二甲氨基乙酯和1,4-二溴丁烷的季铵化反应,合成了一种具有β位季铵结构的可水解交联剂(LC)。将LC单独使用,或和N,N-亚甲基双丙烯酰胺(Bis)联合使用,同时与丙烯酰胺(AM)和2-丙烯酰胺-2-甲基丙磺酸(AMPS)经反相细乳液聚合制得具有延时溶胀特性的交联聚丙烯酰胺(PAM)微球。DLS测试结果表明:微球粒径为300~500 nm,粒径分布窄。通过透光率变化表征了微球的溶胀动力学,结果表明:在中性和75℃下,LC水解速率比中性的丙烯酸酯交联剂快4倍左右,并且其水解速率随p H的降低而变慢,弱酸性条件可抑制LC水解,p H=8.9时,溶胀时间为2 d,p H=5.0时,溶胀时间延长至40 d。通过调节LC质量分数(2%~5%)、Bis质量分数(0~0.05%)、水质p H值(5.0~8.9)和温度(75~100℃)使微球溶胀时间在2~40 d范围内可调。
A quaternary ammonium β -position hydrolyzable crosslinker (LC) was synthesized by the quaternization of dimethylaminoethyl acrylate and 1,4-dibromobutane. LC was used alone or in combination with N, N-methylene bisacrylamide (Bis), while the reverse phase thinning with acrylamide (AM) and 2- acrylamido-2-methylpropanesulfonic acid (AMPS) Crosslinked polyacrylamide (PAM) microspheres with delayed swelling properties were prepared by emulsion polymerization. DLS test results show that: microspheres particle size of 300 ~ 500 nm, particle size distribution is narrow. The swelling kinetics of the microspheres was characterized by the change of light transmittance. The results showed that the LC hydrolysis rate was about 4 times faster than that of the neutral acrylate cross-linking agent at neutral and 75 ℃, Lower and slower, mild acidic conditions can inhibit LC hydrolysis, p H = 8.9, the swelling time of 2 d, p H = 5.0, the swelling time was extended to 40 d. The swelling time of microspheres was controlled within 2 ~ 40 d by adjusting the mass fraction of LC from 2% to 5%, the mass fraction of Bis from 0 to 0.05%, the pH of water from 5.0 to 8.9 and the temperature from 75 to 100 ℃. Adjustable range.