摘要
采用新型催化剂活性铬 ( )络合物和叔胺作为共催化剂 ,催化丙烯酸 ( AA)和环氧氯丙烷 ( ECH)的开环酯化反应 ,合成丙烯酸 2羟 3氯丙酯。研究了反应温度和时间、催化剂种类与用量对合成的影响 ,得到了合成丙烯酸 2羟 3氯丙酯的最佳合成条件。即将 1 0 0份的 AA(含 0 .0 2 %的氢醌 )、1 0 5份的 ECH,和分别占反应物总重量 0 .2 9%和 0 .2 5%的环烷酸铬 ( )和 N,N二甲基苯胺混合 ,在 90℃反应 3 h,然后减压蒸馏除去过量的 ECH,在 3 99.8Pa下收集 95~ 98℃的馏分 ,即得标题物 ,收率 98%。用 IR表征了其结构。
A novel catalystactive Chromium(Ⅲ) complex and tertamine were used to catalyzed the ringopening esterifying reaction of epichlorohydrin(ECH) and acrylic acid(AA) to give 2hydroxylchloropropyl acrylate in high yield. Reacting temperature and time, kind and amount of catalyst influencing on the synthesis were researched. The optimal condition of the synthesis of 2hydroxyl3chloropropyl acrylate was gained. Thus, 100 parts AA(contg. 0.02% hydroquinone), 105 parts ECH, 0.29% by wt. chromium(Ⅲ) naphthenate, 0.25% by wt. N,Ndimethylaniline were mixed. The mixture was reacted at 90 ℃ for 3 h, then removed the excessed ECH in vacuo, under 399.8 Pa at 95~98 ℃ to give the title compound in 98% yield. The main structure was analyzed by Infrared Spectroscopy.
出处
《精细石油化工》
CAS
CSCD
北大核心
1999年第4期43-46,共4页
Speciality Petrochemicals
关键词
铬
络合物
丙烯酸
合成
羟氯丙酯
催化剂
催化
chromium(Ⅲ) complex
-2-hydroxyl-3-chloropropyl acrylate
synthesis