超细镍基催化剂用于1-硝基蒽醌加氢制备1-氨基蒽醌

Preparation of 1-aminoanthraquinone by catalytically hydrogenating 1-nitroanthraquinone with ultrafine nickel-based catalyst

采用溶胶-凝胶法制备了超细镍基催化剂,用BET、TPR、XRD、HRTEM对成型后的催化剂进行物化性能表征,比表面积为363m2/g,孔容为0.38cm3/g,活性组分NiO在催化剂中高度分散,并且在催化剂表面无明显的堆积现象,粒径尺寸不大于10nm。用该催化剂在连续流动固定床小型反应装置上进行1-硝基蒽醌加氢制备1-胺基蒽醌反应,在温度为120℃,液时空速2.0h-1,氢气/1-硝基蒽醌(干品)物质的量比为40,压力3.0MPa条件下,加氢产品纯度达到98.38%,具有优良的加氢性能。该催化剂经过30d的加氢实验后,催化剂活性依然良好,性能未见下降,表明该超细镍基催化剂具有良好的稳定性与使用寿命。

The ultrafine nickel-based catalyst was prepared by the sol-gel process and characterized with BET, TPR, XRD, HRTEM techniques. Specific surface area of the catalyst was 363mg/g, and pore volume was 0.38cm3/g, with double holes structural characteristics. The nickel in the catalyst was highly dispersed, and parti- cle size was less than 10nm. The catalyst activity was evaluated in the continuous flow fixed bed reactor for the syn- thesis of 1-aminoanthraquinone from the hydrogenation of 1-nitroanthaquinone. Under the following operating condi- tions： reaction temperature 120℃, liquid space velocity 2. 0h-1 , mol ratio of hydrogen and 1-nitroanthaquinone 40 and hydrogen pressure 3.0MPa, the purity of prepared 1-aminoanthraquinone was 98.38%. The experements results show that the catatyst has excellent hydrogenation reaction activity. After 30 days of the hydrogenation experiment, the catalytic activity was still excellent. It is indicated that the nickel-based catalyst has good stability and lifetime.