一步催化硝化法制备DNBP

Synthesis of DNBP by One-step Catalytic Nitration

提出了以甲基磺酸作催化剂在硝酸中一步硝化邻仲丁基苯酚制取邻仲丁基-4,6-二硝基苯酚(DNBP)的新工艺。通过单因素实验确定最佳的合成工艺条件如下:n(邻仲丁基苯酚)∶n(硝酸)=1∶3.0、ω(硝酸)=50%、甲基磺酸用量为10%(以邻仲丁基苯酚质量计)、反应时间为4 h、反应温度为45℃,此时DNBP产率达86.8%、纯度高于98.5%。利用红外光谱和质谱对产物进行结构分析,表明该产品为目的产物。

A one-step new process of the preparation of 2-see-butyl-4, 6-dinitrophenol （DNBP） with 2-sechutylphenol and nitric acid as raw materials and methane sulfonic acid as catalyst is proposed in this paper. By single-factor experiments, the optimum synthetic conditions are achieved as follows： n（2-sec-hutylphenol） ： n （nitric acid）=1 ： 3.0,to（nitric acid） = 50 %, catalyst amount is 10 % of mass of 2-sec-hutylphenol, reaction time is 4 h and temperature is 45℃ ,and the yield of DNBP is 86.8% and its purity is above 98. 5%. The structure of the product is identified by IR and MS. Analytic results demonstrate the product prepared is the desired one.