南京师范大学学报(工程技术版)
南京師範大學學報(工程技術版)
남경사범대학학보(공정기술판)
JOURNAL OF NANJING NORMAL UNIVERSITY(ENGINEERING AND TECHNOLOGY)
2013年
2期
75-80
,共6页
α-蒎烯%环氧化%过氧乙酸%相转移催化剂%2,3-环氧蒎烷
α-蒎烯%環氧化%過氧乙痠%相轉移催化劑%2,3-環氧蒎烷
α-파희%배양화%과양을산%상전이최화제%2,3-배양파완
α-pinene%epoxidation%CH3 CO3 H%phase transfer catalyst%2,3-epoxy pinane
采用自制高浓度过氧乙酸(88%)作为环氧化剂,以苄基三乙基氯化铵( TEBA )为相转移催化剂(PTC),催化氧化α-蒎烯环合成2,3-环氧蒎烷.考察比较了催化剂种类、用量,环氧化剂种类、用量,缚酸剂种类、用量,溶剂种类,反应时间和反应温度对反应结果的影响.其适宜的工艺条件为:α-蒎烯1 mol,TEBA 1.0 mmol,碳酸钠0.8 mol,以二氯甲烷为溶剂,15℃下滴加过氧乙酸3 mol,滴加结束后再机械搅拌2 h.实验表明,该方法大大提高了催化效率,α-蒎烯的转化率接近100%,2,3-环氧蒎烷的选择性在97%以上.
採用自製高濃度過氧乙痠(88%)作為環氧化劑,以芐基三乙基氯化銨( TEBA )為相轉移催化劑(PTC),催化氧化α-蒎烯環閤成2,3-環氧蒎烷.攷察比較瞭催化劑種類、用量,環氧化劑種類、用量,縳痠劑種類、用量,溶劑種類,反應時間和反應溫度對反應結果的影響.其適宜的工藝條件為:α-蒎烯1 mol,TEBA 1.0 mmol,碳痠鈉0.8 mol,以二氯甲烷為溶劑,15℃下滴加過氧乙痠3 mol,滴加結束後再機械攪拌2 h.實驗錶明,該方法大大提高瞭催化效率,α-蒎烯的轉化率接近100%,2,3-環氧蒎烷的選擇性在97%以上.
채용자제고농도과양을산(88%)작위배양화제,이변기삼을기록화안( TEBA )위상전이최화제(PTC),최화양화α-파희배합성2,3-배양파완.고찰비교료최화제충류、용량,배양화제충류、용량,박산제충류、용량,용제충류,반응시간화반응온도대반응결과적영향.기괄의적공예조건위:α-파희1 mol,TEBA 1.0 mmol,탄산납0.8 mol,이이록갑완위용제,15℃하적가과양을산3 mol,적가결속후재궤계교반2 h.실험표명,해방법대대제고료최화효솔,α-파희적전화솔접근100%,2,3-배양파완적선택성재97%이상.
2,3-epoxy pinane is synethesized from α-pinene in the presence of homemade high concentration(88%) per-acetic acid( CH3 CO3 H) by using benzyl triethyl ammonium chloride( TEBA) as phase transfer catalyst( PTC) . The effects of kinds of PTC, TEBA amount, kinds of epoxidizing agent, epoxidizing agent amount, kinds of acid accpetor, acid acceptor amount,kinds of solvent,reaction time and reaction temperature are investigated. The results show that the opti-mum conditions are as follows:the amount of α-pinene is 1 mol,TEBA for 1. 0 mmol,sodium carbonate for 0. 8 mol and the doses of methylene chloride as solvent is 30 mL,then 3 mol homemade high concentration CH3 CO3 H is added drop-wise at 15 ℃,and mechanical agitation has been kept for 2 h after CH3 CO3 H drips off. The experimental results show that when homemade high concentration CH3 CO3 H is used as the oxidant,benzyl triethyl ammonium chloride( TEBA) as phase transfer catalyst,the efficiency of the catalyst is greatly improved,the conversion ofα-pinene is close to 100% and 2,3-epoxy pinane's yield is more than 97%.