双官能度引发剂合成及AM聚合

Synthesis of bifunctional initiator and AM polymerization initiating

以2,5-二甲基-2,5-己二醇(DIOL)为原料,质量分数为30%的H2O2为氧化剂,H2SO4为催化剂,在较温和条件下合成双官能度引发剂2,5-二甲基-2,5-二过氧化羟基己烷(DIOOH),考察H2O2与DIOL物质的量比、H2SO4与DIOL物质的量比、反应时间、反应温度因素对DIOOH产率的影响,采用13C-NMR、MS等手段对产物结构进行表征.结果表明,优化的合成工艺条件:H2O2与DIOL物质的量比为7,H2SO4与DIOL物质的量比为6,反应时间为90min,反应温度为30℃,此时DIOOH的产率达到71.6%;用DIOOH引发AM聚合,DIOOH质量浓度为9mg/L时,PAM的特性黏数达到277.6mL/g.

Bifunctional initiator 2,5-dimethyl-2,5-bis(hydroxyl-peroxide)hexane(DIOOH) is synthesized with 2,5-dimethyl-2,5-hexanediol(DIOL) as raw material,30% hydrogen peroxide as oxidant and concentrated sulfuric acid as a catalyst for a more moderate conditions. The four factors such as amount of substance ratio of H2O2 and DIOL,amount of substance ratio of H2SO4 and DIOL,reaction time and reaction temperature are investigated via experiments on yield of DIOOH. The product structure is characterized by method of 13C-NMR and MS. The results show that the optimization of synthesis technology processes are that amount of substance ratio of H2O2 and DIOL is 7,amount of substance ratio of H2SO4 and DIOL is 6,reaction time is 90 minutes and reaction temperature is 30 ℃. Under these conditions,yield of DIOOH is 71.6% and intrinsic viscosity of PAM can reach 277.6 dL/g when DIOOH initiates AM polymerization and mass concentration of DIOOH is 9 mg/L in polymerization system.