文章摘要
王娣,李步卫,安华良,赵新强,王延吉.MIL-100(Fe)催化正戊醛自缩合反应性能[J].精细化工,2019,36(1):
MIL-100(Fe)催化正戊醛自缩合反应性能
MIL-100 (Fe) Catalyzed Self-Condensation of n-Valeraldehyde
投稿时间:2018-03-20  修订日期:2018-08-10
DOI:
中文关键词: 正戊醛  羟醛缩合  2-丙基-2-庚烯醛  MIL-100(Fe)  反应网络  催化技术
英文关键词: n-valeraldehyde  aldol condensation  2-propyl-2-heptenal  MIL-100(Fe)  reaction network  catalysis technology
基金项目:
作者单位E-mail
王娣 河北工业大学 WangDi3698521@163.com 
李步卫 河北工业大学  
安华良 河北工业大学  
赵新强 河北工业大学  
王延吉 河北工业大学  
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中文摘要:
      摘要:以硝酸铁和苯三甲酸为原料,采用水热法制备了金属有机骨架材料MIL-100(Fe)催化剂,采用XRD、SEM、BET对其结构进行了表征。评价了MIL-100(Fe)催化正戊醛自缩合合成2-丙基-2-庚烯醛的反应性能。根据GC-MS分析结果,推测了该反应体系中的副产物以及可能发生的副反应。通过条件优化实验,得到适宜的反应条件为:催化剂质量分数为15%(以正戊醛的质量为基准,下同)、反应温度为130 ℃、反应时间为8 h。在此条件下,正戊醛转化率为73.5%,2-丙基-2-庚烯醛收率和选择性分别为63.2%和86.0%。MIL-100(Fe)催化剂重复使用4次后,催化活性没有明显下降,通过XRD、FTIR分析证明其催化剂结构未发生坍塌。建立了MIL-100( Fe)催化正戊醛自缩合反应网络。
英文摘要:
      Abstract: Metal-organic frameworks MIL-100(Fe) catalyst was prepared by hydrothermal method using ferric nitrate and benzene tricarboxylic acid as raw materials. Its structure was characterized by XRD, SEM and BET. The catalytic performance of MIL-100(Fe) for n-valeraldehyde self-condensation to 2-propyl-2-heptenal was evaluated. The components existing in the reaction system were identified by GC-MS analysis. The effect of reaction conditions on 2-propyl-2-heptenal synthesis was investigated and the suitable reaction conditions were determined as follows: a weight percentage of MIL-100(Fe)=15% (benchmarked against the quality of n-valeraldehyde, the following is the same), reaction temperature of 130 ℃, and reaction time of 8 h. Under the above conditions, the conversion of n-valeraldehyde was 73.5%, and the yield and selectivity of 2-propyl-2-heptenal were 63.2% and 86.0%, respectively. The MIL-100(Fe) catalyst could be reused for four times without a significant loss in its catalytic activity. XRD, FTIR analysis showed that the catalyst structure did not collapse. Lastly a possible reaction network of n-valeraldehyde self-condensation catalyzed by MIL-100(Fe) was established based on speculation of the side-reactions.
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