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在氧气气氛中,硝酸氧化脱羧3,4-亚甲二氧基苯乙醇酸(DMA)后生成的NO很快氧化为NO2,与水作用后生成HNO3和HNO2可以继续参与反应,从而实现了氧气部分替代硝酸氧化脱羧合成洋茉莉醛的过程。在此过程中,NO2起到了O2传送带的作用,而HNO2则是反应真正的氧化剂。在低温、低浓度硝酸和亚硝酸钠引发剂存在条件下,考察了反应温度、硝酸浓度、硫酸浓度和反应时间等参数的影响。当n(HNO3)/n(DMA)=0.45且反应温度为331.2 K时,反应65 m in后氧气替代硝酸率达到32.9%,DMA转化率为97.0%,反应选择性为97.0%。根据实验结果,提出了进一步提高氧气替代硝酸率,从而实现O2作为氧化剂、HNO3作为催化剂的绿色过程的设想。
In the oxygen atmosphere, NO generated after oxidative decarboxylation of 3,4-methylenedioxyphenylglycolic acid (DMA) by nitric acid is quickly oxidized to NO2, and HNO3 and HNO2 are formed after the interaction with water to continue the reaction, thereby achieving oxygen Partial replacement of nitric acid oxidative decarboxylation of jasmonic acid into the process. In this process, NO2 plays the role of O2 conveyor belt, and HNO2 is the real oxidant. Under the condition of low temperature, low concentration nitric acid and sodium nitrite initiator, the effects of reaction temperature, nitric acid concentration, sulfuric acid concentration and reaction time were investigated. When n (HNO3) / n (DMA) = 0.45 and the reaction temperature was 331.2 K, the oxygen substitution rate of nitric acid reached 32.9% after 65 mins reaction, the conversion of DMA was 97.0% and the selectivity of reaction was 97.0%. According to the experimental results, the idea of further increasing the oxygen substitution rate of nitric acid, thus realizing the green process of O2 as an oxidant and HNO3 as a catalyst, is proposed.