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纳米氧化铜直接沉淀法制备工艺及表面改性研究
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摘要
本文简要介绍了纳米氧化铜的性质、用途、国内外研究现状以及制备方法,重点进行了纳米氧化铜粉体制备和表面改性的过程理论分析,并做了相应的试验研究。论文首先对直接沉淀法制备纳米粉体的几个基本过程进行了理论分析论述;然后通过对沉淀反应过程中影响纳米氧化铜收率和产品粒径的主要因素进行单因素、正交试验研究,得到各影响因素的主次顺序以及直接沉淀法制备纳米氧化铜的优惠工艺条件组合;再对沉淀法制得的纳米氧化铜粉体进行表面改性试验研究,通过对影响硬脂酸钠和十二烷基苯磺酸钠两种表面活性剂改性效果的主要因素进行单因素试验研究,得到各因素较适宜的取值范围。
     结果表明:
     (1)以硝酸铜为原料、氢氧化钠-碳酸钠混合溶液为沉淀剂,采用直接沉淀法,通过反应沉淀、过滤、洗涤、干燥、焙烧,制备纳米氧化铜的工艺技术是可行的。通过单因素、正交试验分析,综合考虑产品粒径和制备过程铜收率,得到沉淀反应过程适宜的工艺条件组合是:反应温度25℃,沉淀剂浓度0.5 mol/L,反应时间20 min,沉淀剂用量1.5:1;适宜的焙烧条件是:400℃下焙烧2小时;此时铜收率可达97%以上,产品粒径可达14nm。
     (2)以硬脂酸钠为改性剂对纳米氧化铜粉体进行表面改性处理,各工艺条件较适宜的取值范围为:改性剂用量6~8%;改性时间20~30min;改性温度55~65℃;pH值7.5~8.0。以十二烷基苯磺酸钠为改性剂对纳米氧化铜粉体进行表面改性处理,各工艺条件较适宜的取值范围为:改性剂用量6~10%;改性时间20~30min;改性温度25~35℃;pH值7.5~8.0。
The properties, applications, present research situations at home and abroad as well as preparation methods of nano-copper oxide were briefly introduced in this thesis. Theoretical analysis and corresponding experiments on preparation process and surface modification of nano-copper oxide had been carried out. Firstly, the basic processes of nanometer particles based on direct precipitation preparation were theoretically analyzed. Secondly, through single-factor and multi-factor orthogonal design experiments of the primary factors that influence yield rate and particle size of nano-copper oxide in the precipitation process, the order of the influencing factors and the suitable process conditions for nano-copper oxide prepared with direct precipitation process were obtained. Then, the surface modification experiments on the prepared nano-copper oxide were carried out. Through single-factor experiments of main factors influencing modified results of sodium stearate and lauryl benzene sulfonic acid sodium, the suitable value range of influencing factors was obtained.
     The experimental results show:
     (1) Using cupric nitrate as the raw material, sodium hydroxide and sodium carbonate mixed solution as the precipitate agent, the process technology to prepare nano-copper oxide is feasible. By direct precipitation, filtration, wash, drying and roasting, through single-factor and multi-factor orthogonal test analysis, considering both product particle size and copper receiving rate, the suitable technology conditions for precipitation process are: reaction temperature 25℃, precipitate agent concentration 0.5 mol/L, reaction time 20 min, precipitate agent amount 1.5:1. The suitable roasting condition is roasting at 400℃for 2 hours. Based on these conditions, the nano-copper oxide copper receiving rate can be above 97%, and the particle size can be 14nm.
     (2) Taking sodium stearate as the modification agent' to make surface modification on nano-copper oxide, the suitable value range of each factor is: modification agent amount 6-8%, modification time 20-30 min, modification temperature 55-65℃, pH value 7.5-8.0. Taking lauryl benzene sulfonic acid sodium as the modification agent to make surface modification on nano-copper oxide, the suitable value range of each factor is: modification agent amount 6-10%, modification time 20-30 min, modification temperature 25-35℃, pH value 7.5-8.0.
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