超支化聚酯阻垢剂的合成  

Synthesis of hyperbranched polyester scale inhibitor

作　　者：王亚杰 秦冬玲 杨刚 WANG Yajie;QIN Dongling;YANG Gang(State Key Laboratory of Materials Chemical Engineering,College of Chemical and Engineering,Nanjing Tech University,Nanjing 211800,China)

机构地区：[1]南京工业大学化工学院材料化学工程国家重点实验室,江苏南京211800

出　　处：《南京工业大学学报（自然科学版）》2021年第4期442-449,共8页Journal of Nanjing Tech University(Natural Science Edition)

基　　金：国家科技支撑计划(2013BAE11B03)。

摘　　要：以绿色化学为指导思想,合成一种不含N、P元素的高性能绿色阻垢剂。以2,2二羟甲基丙酸(DMPA)和三羟甲基丙烷(TMP)为原料,在对甲苯磺酸催化下,采用一锅熔融缩聚法合成第二代端羟基超支化聚酯(HBPE—OH)。为提高HBPE—OH改性程度,首次选用4二甲氨基吡啶(DMAP)作为催化剂,用丁二酸酐(SA)对HBPE—OH进行端基羧酸化改性,得到具有阻垢功能的端羧基超支化聚酯(HBPE—COONa)。采用单因素实验考察了缩聚反应时间、反应温度、催化剂用量及羧酸化改性反应时间、反应温度对阻垢性能的影响。结果表明:缩聚反应最佳条件为反应时间4 h,反应温度140℃,催化剂用量为0.8%;端基羧酸化最佳条件为反应时间3 h,反应温度70℃,羧酸化程度高达95.4%。用傅里叶红外光谱仪(FT IR)和核磁共振波普仪(NMR)对HBPE—OH和HBPE—COONa进行表征,表明阻垢剂结构完整,羧酸化程度较高,并用扫描电子显微镜(SEM)对CaSO_(4)垢样进行表征,验证了阻垢剂晶格畸变机制。With the guidance of green chemistry,a high-performance green scale inhibitor containing no nitrogen and phosphorus elements was synthesized.The second-generation hydroxyl-terminated hyperbranched polyester(HBPE—OH)was synthesized by the one-pot melt polycondensation method under the p-toluenesulfonic acid catalyst,using 2,2-dimethylolpropionic acid(DMPA)and trimethylolpropane(TMP)as the reaction raw materials.To improve the modification of HBPE—OH,4-dimethylaminopyridine(DMAP)was selected as the catalyst for the first time,and succinic anhydride(SA)was used to modify the carboxylic acid end group of HBPE—OH for obtaining scale-protected carboxyl group hyperbranched polyester(HBPE—COONa).The effects of polycondensation reaction time,reaction temperature,catalyst amount,carboxylic acid modification reaction time and reaction temperature on scale inhibition were investigated by single-factor experiments.Results showed that the optimum reaction conditions for the polycondensation were reaction time of 4 h,the reaction temperature of 140℃,the catalyst amount of 0.8%.The best conditions for end-group carboxylation were reaction time of 3 h,reaction temperature of 70℃,and carboxylation of 95.4%.HBPE—OH and HBPE—COONa were characterized by Fourier transform infrared spectroscopy(FT-IR)and nuclear magnetic resonance spectroscopy(NMR),indicating that the scale inhibitor was successfully synthesized.The SEM was used to characterize CaSO_(4) scale samples,and the scale inhibition mechanism was verified.

关 键 词：绿色化学 超支化聚酯 羧酸化 阻垢剂 

分 类 号：TQ317[化学工程—高聚物工业] TQ085