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Pd(OH)2/C催化剂是制备六硝基六氮杂异伍兹烷(HNIW,C L-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AC RO S O rganics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(O H)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%。
The Pd (OH) 2 / C catalyst is the key material for preparing hexanitrohexaazaisowurtzitane (HNIW, C L-20). Three kinds of commercial activated carbons were selected as carriers. Several hexa-benzylhexaazaisowurtzitane (HBIW) hydrogenolyzed debenzylation Pd (OH) 2 / C catalysts were prepared by impregnation method. The effects of surface properties, pore size distribution, catalyst preparation temperature, alkali species and palladium loading on the catalytic activity of Pd (OH) 2 / C catalysts were investigated. Catalytic activity and N2 adsorption, temperature programmed desorption (TPD), powder X-ray diffraction (XRD) and transmission electron microscopy (TEM) showed that the surface properties, pore size distribution, reaction temperature and palladium loading of activated carbon significantly affect the catalytic activity of Pd ) 2 / C catalyst, and the specific surface area of activated carbon and the type of base used in the catalyst preparation are not the key factors affecting the performance of Pd (OH) 2 / C catalyst. Pretreated with 30% nitric acid, ACRO SO rganics company granular activated carbon as a carrier, sodium carbonate as a source of alkali, at a reaction temperature of 5 ° C, the 9% Pd (OH) 2 / C catalyst has the best catalytic active. When the amount of palladium in the catalyst was 0.3% (mass fraction) of the substrate HBIW, the yield of hydrogenolysis-deacetylated product reached 93%.