CAJ | 학술논문

制备了氯甲基化聚苯乙烯-二乙烯苯接枝磷钨杂多酸季铵盐催化剂,用红外光谱和电感耦合等离子体原子发射光谱对催化剂进行了表征.无溶剂下以H2O2(w(H2O2)=34.5%)和3-环己烯甲酸-3'-环己烯甲酯(简称A)为原料,催化合成3,4-环氧基环己基甲酸-3',4'-环氧基环己基甲酯(简称AOO),探讨了催化剂用量、n(A):n(H2O2)、反应时间、反应温度等因素对反应的影响.获得了适宜的合成条件为(以60mmol A计):反应温度65 ℃,反应时间100 min,催化剂用量5.0 g,n(A):n(H2O2)=1∶3.该条件下A的平均转化率达99%以上,AOO的平均产率达78.9%.催化剂平均回收率在93%以上.
제비료록갑기화취분을희-이을희분접지린오잡다산계안염최화제,용홍외광보화전감우합등리자체원자발사광보대최화제진행료표정.무용제하이H2O2(w(H2O2)=34.5%)화3-배기희갑산-3'-배기희갑지(간칭A)위원료,최화합성3,4-배양기배기기갑산-3',4'-배양기배기기갑지(간칭AOO),탐토료최화제용량、n(A):n(H2O2)、반응시간、반응온도등인소대반응적영향.획득료괄의적합성조건위(이60mmol A계):반응온도65 ℃,반응시간100 min,최화제용량5.0 g,n(A):n(H2O2)=1∶3.해조건하A적평균전화솔체99%이상,AOO적평균산솔체78.9%.최화제평균회수솔재93%이상.
Chloromethylated polystyrene divinylbenzene grafted quaternary ammonium salt of phosphor-tungstic heteropoly acid had been prepared as a catalyst. The catalyst had been characterized by IR spectrum and inductively coupled plasma atomic emission spectrometry. 3,4-Epoxycyclohexylmethyl-3',4'-Epoxycyclohexane Carboxylate (AOO) had been synthesized by epoxidation of 3-Cyclohexenylmethyl 3'-Cyclohexenecarboxylate (A) with hydrogen peroxide (w (H2O2 ) = 34.5 % ) as oxidant under organic solvent-free condition. The main influence factors in the reaction, such as mole ration of A to H2O2 , reaction time, temperature, amounts of catalyst and so on, had been studied. The appropriate reaction condition are as fallows(based on 60 mmol the condition, average conversion of A is more than 99% and average yield of AOO is 78.9%. The average recovery of catalyst is over 93%.