摘要
以对氯苯甲醇为原料,过氧化氢为氧化剂,铜盐为催化剂,通过催化氧化绿色合成对氯苯甲醛。考察了铜盐种类及用量、过氧化氢用量及滴加时长、反应温度对对氯苯甲醛收率的影响。得到了制备对氯苯甲醛的最佳条件为:Cu(CH_(3)COO)_(2)·H_(2)O催化剂,n[Cu(CH_(3)COO)_(2)·H_(2)O]∶n(对氯苯甲醇)∶n(过氧化氢)=1.0∶100∶300,水作溶剂,反应温度96℃,反应时间2 h。在该条件下,对氯苯甲醇转化率为93.1%,对氯苯甲醛选择性和收率分别为97.7%和91.0%。将含催化剂水相进行循环利用,发现循环4次后,对氯苯甲醛收率仍可达85%以上。
A green synthesis method of p-chlorobenzaldehyde was achieved from p-chlorobenzyl alcohol using hydrogen peroxide and copper salts as oxidant and catalyst,respectively.The effects of type and amount of copper salt,amount and dropping time of hydrogen peroxide,and reaction temperature on the yield of p-chlorobenzaldehyde were investigated.The optimum reaction conditions for the synthesis of p-chlorobenzaldehyde were obtained as follows:Cu(CH_(3)COO)_(2)·H_(2)O as catalyst,n[Cu(CH_(3)COO)_(2)·H_(2)O]∶n(p-chlorobenzyl alcohol)∶n(hydrogen peroxide)=1.0∶100∶300,water as solvent,reaction temperature of 96℃ and reaction time of 2 h.Under the above-mentioned conditions,the conversion rate of p-chlorobenzyl alcohol was 93.1%,the selectivity and yield of p-chlorobenzaldehyde were 97.7% and 91.0%,respectively.The catalyst-containing water phase was recycled,and the yield could still reach above 85% after being recycled for 4 times.
作者
杨丰科
袁世申
张永富
牛鹏程
茹雨晴
高巍伟
YANG Fengke;YUAN Shishen;ZHANG Yongfu;NIU Pengcheng;RU Yuqing;GAO Weiwei(College of Chemical Engineering,Qingdao University of Science&Technology,Qingdao 266042,Shandong,China)
出处
《精细化工》
EI
CAS
CSCD
北大核心
2022年第3期644-648,共5页
Fine Chemicals
基金
山东省自然科学青年基金(ZR2020QB168)。
关键词
对氯苯甲醇
过氧化氢
催化氧化
绿色合成
对氯苯甲醛
精细化工中间体
p-chlorobenzyl alcohol
hydrogen peroxide
catalytic oxidation
green synthesis
p-chlorobenzaldehyde
fine chemical intermediates
