以Ni-B为催化剂合成5-氨基苯并咪唑酮

研究了5-硝基苯并咪唑酮与氢气在高压釜中反应合成5-氨基苯并咪唑酮的工艺路线,该反应属于液相催化加氢还原反应。对自制的非晶态Ni-B催化剂用SEM, XRD 和 BET等测试方法进行了表征,并将其用于催化合成5-氨基苯并咪唑酮。XRD 测试表明Ni-B催化剂为非晶态合金催化剂,BET测试非晶态Ni-B催化剂的比表面积和孔容,通过计算,该催化剂的比表面积为51 m²/g,总孔容为0.0524 cm³/g。并对反应温度、催化剂的用量和催化剂回收利用进行了研究。确定最适条件为:催化剂用量为5.5%~6.6%,(相对于5-硝基苯并咪唑酮的质量),反应温度180 ℃,反应压力2.0 MPa,反应时间8 h,溶剂无水乙醇100 mL,产物产率为92.4%,质量分数在99%以上。

Preparation of 5-Amino Benzimidazolone-2 with Ni-B Catalyst

5-Amino benzimidazolone-2 was prepared by 5-nitro benzimidazolone-2 and hydrogen in autoclave. And this reaction is classified to catalytic hydrogenation reduction. In this research, the Ni-B catalyst was characterized by SEM, XRD and BET, and its catalytic performance for the synthesis of 5-amino benzimidazolone-2 was investigated. XRD shows that Ni-B catalyst is amorphous alloy. And BET shows the specific surface area and pore volume of Ni-B catalyst. By calculating, the specific surface area is 51 m²/g, total entrance is 0.0524 cm³/g. The reaction temperature, the amount of catalyst and catalyst recycling were also studied. At last, the study has shown the optimum reaction conditions: the amount of catalyst is 5.5%~6.6%,the reaction temperature is 180 ℃, the reaction pressure is 2.0 MPa, the reaction time is 8 h, the amount of absolute ethanol is 100 mL as reaction medium. And the yield and purity of the product was up to 92.4% and 99%, respectively.