Pd(OH)2/C催化剂是制备六硝基六氮杂异伍兹烷(HNIW,CL-20)的关键材料.选择三种市售的活性炭为载体,采用浸渍沉积法制备了几种六苄基六氮杂异伍兹烷(HBIW)氢解脱苄Pd(OH)2/C催化剂.考察了载体活性炭的表面性质、孔径分布、催化剂制备温度、碱的种类及钯负载量对Pd(OH)2/C催化剂的催化活性的影响.催化活性和N2吸附、程序升温脱附(TPD)、粉末X射线衍射(XRD)和透射电镜(TEM)的特性表明,活性炭的表面性质、孔径分布、反应温度和钯负载量显著影响Pd(OH)2/C催化剂的催化活性,而活性炭的比表面积和催化剂制备过程中所用碱的种类不是影响Pd(OH)2/C催化剂性能的关键因素.用30%硝酸预处理ACROS Organics公司产的颗粒状活性炭为载体,碳酸钠为碱源,在反应温度5℃下,制得的9%Pd(OH)2/C催化剂有最佳的催化活性.催化剂中钯用量为底物HBIW的0.3%(质量分数)时,氢解脱苄乙酰化产物收率达93%.
Pd(OH)2/C catalyst is a key material for the preparation of hexanitrohexaazaisowurtzitane (HNIW,CL-20). Several Pd(OH) 2/C catalysts for the hydrogenolytic debenzylation of hexabenzylhexaazaisowurtzitane (HBIW) were prepared through soaking-deposition method with three types of commercial activated carbons as carriers. Effects of the surface properties and pore size distributions of activated carbons, the preparation temperature of catalyst, the kinds of base and the loading amount of palla- dium on the catalytic activity of Pd( OH )2/C catalyst were investigated. The catalytic activity and the characteristics of N2 adsorp- tion, temperature programmed desorption (TPD) , powder X-ray diffraction (XRD) and transmission electron microscope (TEM) show that the catalytic activity of Pd(OH )2/C catalyst is strongly influenced by the surface property and pore size distribution of activated carbon, reaction temperature and the loading amount of palladium, whereas the specific surface area of activated carbon and the kinds of base used in preparation process of catalyst are not key factors affecting the properties of Pd (OH)2/C catalyst. Using disodium carbonate as base source and 30% nitric acid pretreated granular activated carbon ( produced by ACROS Organics Company) as carrier, the 9% Pd( OH ) 2 IC catalyst prepared under the reaction temperature of 5℃, has the best catalytic activity. When the amount of palladium used in catalyst is 0.3% (wt/wt) of HBIW substrate, the product yield of hydrogenolytic debenzy- lation-acetylation reaction of HBIW reaches 93%