目的:优化Cu-Co-P非晶合金的化学镀工艺,研究其对硼氢化钠水解制氢的催化性能。方法以铁片为基体,研究化学镀Cu-Co-P非晶合金的制备工艺,探讨镀液成分对沉积速率、镀液稳定性及镀层质量的影响,并根据研究结果筛选出化学镀Cu-Co-P的优化配方。采用该配方对氧化铝(γ-Al2 O3)基体施镀,制备出负载型Cu-Co-P/γ-Al2 O3非晶合金催化剂,对其组成、形貌和结构等进行表征。利用硼氢化钠水解制氢实验,评价制备的负载型Cu-Co-P多元合金催化剂的催化性能。结果根据优化配方制备出的负载型非晶合金Cu-Co-P/γ-Al2 O3催化剂的比表面积为233 m2/g,相对组成为57.85%Cu+39.69%Co钴+2.46%P(均为质量分数)。45℃条件下,在20 mL含1 g硼氢化钠和1 g氢氧化钠的溶液中,硼氢化钠水解制氢的速率为1295 mL/( g·min)。结论化学镀Cu-Co-P的优化配方组成为:硫酸钴20 g/L,硫酸铜0.7 g/L,次亚磷酸钠40 g/L,柠檬酸钠20 g/L,EDTA-2Na 10 g/L,氟化铵25 g/L。工艺参数为:温度(85±1)℃,pH=9。
ABSTRACT:Objective To optimize the preparation process of Cu-Co-P amorphous alloy and to study its catalytic performance for hydrogen generation in the hydrolysis of sodium borohydride. Methods The amorphous alloy Cu-Co-P was prepared on iron sheets by electroless deposition method. The effects of bath composition on deposition rate, bath stability and coating quality were investi-gated. The optimized formulation was screened out based on the research results. The supported amorphous alloy catalysts Cu-Co-P/γ-Al2 O3 were synthesized according to the optimized formulation. The composition, surface morphology and phase structure of the deposited Cu-Co-P/γ-Al2 O3 catalyst were characterized. The catalytic properties of the prepared multiple amorphous alloy cata-lysts Cu-Co-P were investigated using the hydrolysis reaction of sodium borohydride solution. Results The BET surface area of the obtained supported Cu-Co-P/γ-Al2 O3 amorphous alloy catalyst was 233 m2/g, and it contained 57. 85wt% Cu, 39. 69wt% Co and 2. 46wt% P. A hydrogen generation rate of 1295 mL/(g·min) was achieved at 45 ℃ by hydrolysis of NaBH4 solution containing 1 g NaBH4 and 1 g NaOH. Conclusion The optimized electroless plating formulation of Cu-Co-P was 20 g/L cobalt sulfate hepta-hydrate, 0. 7 g/L copper sulfate pentahydrate, 40 g/L sodium hypophosphite monohydrate, 20 g/L trisodium citrate dehydrate, 10 g/L ethylenediamine tetraacetic acid disodium salt and 25 g/L ammonium fluoride. The process was controlled at (85±1) ℃ and pH=9.
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