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将杉木粉热解、再用发烟硫酸磺化为杉木炭磺酸,FT-IR、XPS等分析表明,磺化反应成功地将磺酸基团键合到杉木炭骨架上。杉木炭磺酸对乙酰乙酸乙酯和取代酚的Pechmann缩合反应表现了较好的催化活性,催化合成了取代4-甲基香豆素。考察了催化剂的用量等反应条件对Pechmann缩合反应收率的影响,并比较研究了杉木炭磺酸与其他磺酸树脂的催化活性。结果表明,无溶剂条件下,杉木炭磺酸对7-羟基-4-甲基香豆素的合成具有很好的催化性能。在反应温度105℃、n(乙酰乙酸乙酯)∶n(间苯二酚)=1∶1和反应时间2.5h条件下,杉木炭磺酸添加量n(-SO3H+)为取代酚的0.1(mol)%时,产率高达92.9%,选择性为97.8%(HPLC)。
The pyrolysis of Chinese fir powder and the sulfonation of oleum to Cunninghamia lanceolata were also studied. The results of FT-IR and XPS indicated that sulfonation successfully bonded the sulfonic acid groups to the CAC frame. The CZC exhibited good catalytic activity for Pechmann condensation of ethyl acetoacetate and substituted phenol and the catalytic synthesis of substituted 4-methylcoumarin. The effects of reaction conditions such as the amount of catalyst on the yield of Pechmann condensation reaction were investigated. The catalytic activity of Chinese fir sulfonic acid with other sulfonic acid resins was also studied. The results show that the Chinese fir carbon acid sulfonic acid has good catalytic performance for the synthesis of 7-hydroxy-4-methylcoumarin without solvent. Under the conditions of reaction temperature of 105 ℃, n (ethyl acetoacetate): n (resorcinol) = 1: 1 and reaction time of 2.5h, the amount of Chinese fir carbon acid added n (-SO3H +) was 0.1 mol)%, the yield is as high as 92.9% and the selectivity is 97.8% (HPLC).