摘要
针对SAPO-11的一维十元环直孔道结构,设计了具有特殊分子结构的长链烷烃3-乙基-十一烷。以3-戊酮和溴辛烷与镁反应生成的格氏试剂为原料,经加成、水解、脱水、催化加氢反应生成3-乙基-十一烷,红外和质谱分析确定合成产物正确。影响醇脱水反应的主要因素为温度和硫酸含量,适宜的脱水反应条件为温度50℃、时间90 min、硫酸质量分数60%,硫酸与3-乙基-3-十一醇的体积比1:1;影响烯烃加氢的主要因素为反应压力和催化剂用量,适宜的加氢反应条件为常温、时间120 min、0.6 MPa,催化剂与原料的质量比3%。在所确定的合成条件下,3-乙基-十一烷的总收率达到了71.24%,纯度达到了97.20%,能满足作为探针分子的纯度要求。
In allusion to the molecular sieve of SAPO-11 with unidimensional 10-rings pore channel,3-ethylicundecane was selected as probe molecule for its special molecular structure.3-ethylicundecane was prepared from3-pentanone and Grignard reagent via addition reaction,hydrolyzation,dehydration,catalytic hydrogenation.After analysed by FTIR and MS,the results showed that the factors effect on dehydration were temperature and H2SO4 content.The best condition for dehydration were as follows: temperature:50 ℃,time:90min,H2SO4 mass fraction:60%,volume ratio of H2SO4 and 3-ethylicundecane was 1:1.The factors effect on olefin hydrogenation were reaction pressure and catalyst,and the reaction conditions were normal temperature,120 min,0.6 MPa,mass ratio of material and catalyst was 3%.Under the experimental condition mentioned above,the total yield and the purity of 3-ethylicundecane was 71.24% and 97.20%,reaches the purity as probe moleculars.
出处
《化工生产与技术》
CAS
2011年第5期30-33,8-9,共4页
Chemical Production and Technology
