Ni_2P的水热合成与表征  

Preparation and characterization of nickel phosphide catalysts

作　　者：罗旭东[1] 魏民[1] 鄢景森[2] 王海彦[1] 

机构地区：[1]辽宁石油化工大学环境与化工学院,辽宁抚顺113001 [2]辽宁科技学院药化学院,辽宁本溪117000

出　　处：《应用化工》2016年第11期2098-2101,2106,共5页Applied Chemical Industry

基　　金：辽宁省教育厅科技研究一般项目(L2014507)

摘　　要：以水为溶剂，红磷、硝酸镍为原料，采用水热法制备磷化镍（Ni2 P），并考察了P／Ni摩尔比、表面活性剂种类、反应时间和反应温度对产物晶型、晶粒大小、形貌的影响。利用XRD（ X射线衍射）、BET （ N2吸附）、SEM （扫描电子显微镜）分别对产物的织构与形貌进行了表征。结果表明，反应温度以及表面活性剂的种类都会不同程度地影响产物的相态，温度太低，很难合成Ni2 P；温度太高，容易生成Ni2 P、Ni12 P5的混合物，硬脂酸钠易于合成六方相Ni2 P，而且可显著增大比表面积；P／Ni摩尔比、反应时间也会不同程度地影响产物的结晶度。当添加了适量硬脂酸钠以及P／Ni摩尔比为6时，经过时间12 h、温度120℃，合成了纯净的六方相Ni2 P，形状类似为球形，粒径4～6μm，比表面积为32．734 m2／g。The nickel phosphides were prepared by hydrothermal （ solvothermal ） method, using water as solvent ,nickel nitrate and non-toxic phosphorus as raw material , and investigated the influence on the crystal form ,grain size and morphology of products from different reaction time ,reaction temperature ,P/Ni mole ratio and surfactant .Different product construction and morphology were characterized by XRD （ X-ray diffraction）,BET （N2 physisorption） and SEM（scanning electron microscope）.The results showed that reaction temperature and the kind of surfactant have a certain influence on the phase of products;the reaction temperature was too low to product the hexagonal nickel phosphide （ Ni2 P） and it was higher to product mixture of Ni 2 P and Ni12 P5;Sodium stearate was beneficial to product Ni 2 P and could increase the specific surface area dramatically;the reaction time and the initial P/Ni mole ratio both had influence on the crystallinity of products in different degree .The pure hexagonal nickel phosphide （ Ni2 P） had been successfully prepared at 120 ℃,12 h,the initial P/Ni mole ratio of 6 under the addition of some sodium stearate.Its grain size was 4~6 μm and specific surface area is 32.734 m2/g.

关 键 词：磷化镍(Ni2P) 水热法 表面活性剂 

分 类 号：TQ138.1[化学工程—无机化工]