摘要
采用逐级优化的单因素实验考察钛硅-1分子筛(TS-1)催化丙酮氨氧化合成丙酮肟的反应条件.结果表明:催化剂用量、氨酮摩尔比、氧酮摩尔比、氨水及双氧水滴加时间、氨水及双氧水滴加组合模式、叔丁醇与水体积比及反应温度等因素对反应效果影响较显著.适宜的反应条件为:每mol丙酮催化剂用量4g以上,氨酮摩尔比2.0以上,氧酮摩尔比1.0~1.4,氨水及双氧水滴加时间不小于1h,且同时滴加完毕,后续反应时间不小于1h,V(叔丁醇)/V(水)=2.3,反应温度70℃.在此优化反应条件下,丙酮转化率可达95%,丙酮肟选择性为98%.
The reaction conditions of acetone ammoxidation with NH3 and H2O2 as ammoxidation agents over titanium silicalite-1 (TS-1) toward acetone oxime were investigated by single factor experiments. Results showed that the catalyst amount, n( NH3 )/n( acetone) , n( H2O2 )/n(acetone), the addition time of NH3· H2O and H2O2, the ways to introduce NH3· H2O and H2O2, V(tert-butyl alcohol)/V( H2O) , and the reaction temperature have a remarkable influence on the reaction. The conversion of the acetone and the selectivity to acetone oxime can reach 95% and 98% under the optimized operation conditions as follows: m( catalyst ) /n ( acetone ) was larger than 4 g/mol, n ( NH3 )/n (acetone) was above 2. 0, n(H2O2)/ n(acetone) was at 1.0 - 1.4, the addition time of NH3 ·H2O and H2O2 was larger than 1 h, and the dropwise of NH3.H2O and H2O2 at one time, and the following reaction time longer than 1 h, the V(tert-butyl alcohol)/V( H2O) at about 2. 3, and the reaction temperature at about 70 ℃.
出处
《南京工业大学学报(自然科学版)》
CAS
北大核心
2009年第4期74-78,共5页
Journal of Nanjing Tech University(Natural Science Edition)
基金
国家自然科学基金资助项目(20636020)
国家高技术研究发展计划(863计划)资助项目(2007AA06A402)
关键词
反应条件
丙酮
氨氧化
TS-1
reaction conditions
acetone
ammoxidation
TS-1