以Ni-B为催化剂合成5-氨基苯并咪唑酮

摘要

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。

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	马洪庆
	孟舒献
	冯亚青
	方硕

关键词： 5-氨基苯并咪唑酮； Ni-B催化剂； 5-硝基苯并咪唑酮

Abstract：

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.

Keywords： 5-amino benzimidazolone-2； Ni-B catalyst； 5-nitro benzimidazolone-2

Received 2013-12-12;

Fund:

国家自然基金(21076147)。

Corresponding Authors: 孟舒献, E-mail: msxmail@tju.edu.cn。 Email: msxmail@tju.edu.cn

About author: 马洪庆(1987-),女,硕士研究生,现从事油漆中间体方面的研究。

引用本文:

马洪庆, 孟舒献, 冯亚青, 方硕.以Ni-B为催化剂合成5-氨基苯并咪唑酮[J]. 化学工业与工程, 2016,33(1): 40-44

Ma Hongqing, Meng Shuxian, Feng Yaqing, Fang Shuo.Preparation of 5-Amino Benzimidazolone-2 with Ni-B Catalyst[J]. Chemcial Industry and Engineering, 2016,33(1): 40-44

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