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相转移催化剂双子型磷钨酸季铵盐的制备、表征及催化油酸裂解制备壬二酸 |
Preparation and characterization of phase transfer catalyst gemini phosphotungstic acid quaternary ammonium salt and its catalytic cracking of oleic acid to prepare azelaic acid |
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DOI: |
中文关键词: 磷钨酸季铵盐 双子型表面活性剂 季铵盐 油酸 壬二酸 |
英文关键词:phosphotungstic acid quaternary ammonium salt gemini surfactant quaternary ammonium salt oleic acid azelaic acid |
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中文摘要: |
以溴代十八烷烃和四甲基乙二胺合成双子型表面活性剂,并与磷钨酸采用共沉淀的方法制备双子型磷钨酸季铵盐\[C42H90N2\]HPW12O40。利用1H NMR、13C NMR、FT-IR、XRD、XPS对催化剂进行了表征,并采用该催化剂催化油酸氧化裂解制备壬二酸。结果表明:双子型磷钨酸季铵盐不仅保留了均相催化剂高效传质的优点,而且还具有非均相催化剂易于回收的优势,在回收率方面优于单子型磷钨酸季铵盐。在油酸质量1 g、m(氧化剂)/m(油酸)2.5、稳定剂(锡酸钠)用量为氧化剂(30%H2O2)质量的0.5%、催化剂用量为油酸质量的8%、反应温度90 ℃、反应时间4 h条件下,壬二酸产率为85.1%,壬酸产率为90.8%,在此条件下催化剂重复使用4次,壬二酸产率在82%以上。 |
英文摘要: |
A gemini surfactant was synthesized with bromooctadecane and tetramethylethylenediamine, and the gemini phosphotungstic acid quaternary ammonium salt \[C42H90N2\]HPW12O40 was prepared by co-precipitation with phosphotungstic acid. The catalyst was characterized by 1H NMR, 13C NMR, FT-IR, XRD and XPS, and it was used for oxidative cracking of oleic acid to prepare azelaic acid. The results showed that gemini phosphotungstic acid quaternary ammonium salt not only retained the advantages of high efficiency mass transfer of homogeneous catalyst, but also had the advantage of easy recovery of non-heterogeneous catalyst, and was also superior to monoton phosphotungstic acid quaternary ammonium salt in terms of recovery rate. Under the conditions of the mass of oleic acid 1 g, mass ratio of oxidant to oleic acid 2.5, stabilizer (sodium stannate) dosage 0.5% of the oxidant (30% H2O2) mass, catalyst dosage 8% of oleic acid mass, reaction temperature 90 ℃ and reaction time 4 h, the yields of azelaic acid and pelargonic acid were 85.1% and 90.8% respectively. When the catalyst was reused for four times, the yields of azelaic acid were still above 82%. |
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