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出 处:《精细化工》2014年第11期1324-1328,1375,共6页Fine Chemicals
摘 要:以工业品甲基丙烯酰氧乙基三甲基氯化铵(DMC)为原料,过硫酸铵(APS)为引发剂,乙二胺四乙酸四钠(Na4EDTA)为络合剂,采用一次性加入引发剂、两步升温引发的水溶液聚合方法合成聚甲基丙烯酰氧乙基三甲基氯化铵(PDMC)。用正交实验优化反应条件,得到的最佳工艺条件为:w(DMC)=72.5%,m(APS)∶m(DMC)和m(Na4EDTA)∶m(DMC)分别为0.20∶100和0.018∶100。在聚合反应引发温度T1为35℃下反应3 h后,再在聚合反应熟化温度T2为50℃下完成反应3 h。在最佳工艺条件下,得到的PDMC胶体产物的特征黏度为10.38d L/g,单体转化率为98.40%。用FTIR和1HNMR对产物的结构进行了表征。该文所得结果为合成工艺的进一步优化和系列化相对分子质量PDMC产物的合成研究奠定了基础。Using industrial monomer solution of methacrylatoethyltrimethyl ammonium chloride(DMC) as raw material, ammonium persulphate(APS) as initiator and tetrasodium EDTA(Na4EDTA) as chelating agent, the preparation of poly(methacrylatoethyltrimethyl ammonium chloride) (PDMC) was researched, based on the method of adding initiator all at once, two-step increasing of temperature for aqueous polymerization. The optimal process conditions were w(DMC)=72.5%, m(APS):m(DMC)=0.20:100, m(Na4EDTA):m(DMC)=0.018:100, and polymerization carried out at 35℃ and then 50℃, each for 3h via the orthogonal experimental method. The intrinsic viscosity of PDMC product and monomer conversion rate under optimal process conditions reached 10.38 dL/g-1 and 98.40% respectively. Structure of the product was characterized via FTIR and 1HNMR spectra.Thepreparation of PDMC products with serial molecular weight.
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