1-(4-甲基苯基)乙醇的合成工艺研究

Synthesis process of 1-(4-methyl phenyl)ethanol

采用乙酰氯为酰化剂、三氯化铝催化甲苯的傅-克酰基化反应制备4-甲基苯乙酮,然后采用固定床将其在CuO-NiO-MnO2/SiO2铜基催化剂上连续催化加氢制备1-(4-甲基苯基)乙醇。研究结果表明,以二氯甲烷作溶剂,n(AlCl3)∶n(甲苯)∶n(乙酰氯)=1.1∶1∶1.1时,反应时间1h,反应温度0℃,甲苯的转化率达100%,4-甲基苯乙酮的收率为99.5%,纯度可达99.2%。然后在铜基催化剂CuO-NiO-MnO2/SiO2的催化下,氢气压力2.0MPa,反应温度100℃,n(H2)∶n(4-甲基苯乙酮)=30∶1,液空速为0.30h-1的条件下,4-甲基苯乙酮加氢制备1-(4-甲基苯基)乙醇,4-甲基苯乙酮的转化率为100%,1-(4-甲基苯基)乙醇的收率为97.6%。

Using acetyl chloride as acylating agent,4-methyl acetophenone was prepared by toluene on catalyst of aluminium trichloride through Friedel-Crafts acylation,then 4-methyl acetophenone was hydrogenated to 1-（4-methyl phenyl）ethanol continuously on nano CuO-NiO-MnO2/SiO2 catalyst in a fixed bed.Research results showed that,the conversion of toluene and yield of 4-methyl acetophenone reached 100% and 99.5%respectively,while the purity of products was 99.2% under the conditions of dichloromethane as solvent,n（AlCl3）∶n（toluene）∶n（acetyl chloride）=1.1∶1∶1.1,reaction time 1h,reaction temperature 0 ℃.Then 4-methyl acetophenone was hydrogenated to 1-（4-methyl phenyl）ethanol on nano CuO-NiO-MnO2/SiO2 catalyst,the conversion of 4-methyl acetophenone and yield of 1-（4-methyl phenyl）ethanol approached 100%and 97.6%respectively under the conditions of H2 pressure 2.0MPa,reaction temperature 100℃,n（H2）∶ n（4-methyl acetophenone）= 30∶ 1,liquid hourly space velocity 0.30h-1.