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化工学报  2014 

H4SiW12O40/SiO2催化正丁醛自缩合反应

DOI: 10.3969/j.issn.0438-1157.2014.06.022, PP. 2106-2112

Keywords: 正丁醛,催化剂,羟醛缩合,合成,辛烯醛,多相反应

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Abstract:

正丁醛自缩合合成辛烯醛是工业生产辛醇的重要步骤之一。首先考察了3种杂多酸H3PW12O40、H4SiW12O40和H3PMo12O40对正丁醛自缩合反应的催化性能,发现H4SiW12O40的催化性能最好。其次,利用浸渍法制备了负载型H4SiW12O40催化剂,考察了载体和制备条件对催化剂性能的影响,确定以SiO2为载体,H4SiW12O40负载量为50%(质量分数),在150℃焙烧2h的制备条件。探讨了反应条件对催化剂性能的影响,确定了适宜反应条件:催化剂与正丁醛的质量比为0.15,反应温度120℃,反应时间6h。在此条件下,正丁醛的转化率为90.4%,辛烯醛的选择性为89.2%。通过对催化剂进行ICP-AES分析和XRD表征,发现活性组分流失是造成催化剂稳定性差的主要原因。为减缓H4SiW12O40的流失,以[emim]BF4离子液体为模板剂,采用溶胶-凝胶法制备了H4SiW12O40/SiO2催化剂,实验结果表明,催化剂稳定性有一定程度的提高。

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