氧化亚铜制备及其工艺优化研究

发布时间：2018-01-04 23:01

  本文关键词：氧化亚铜制备及其工艺优化研究　出处：《电子科技大学》2016年硕士论文　论文类型：学位论文

  更多相关文章： 氧化亚铜 电解法 亚硫酸钠 印制电路蚀刻废液 循环利用

【摘要】：氧化亚铜在塑料、涂料、陶瓷、玻璃、工业催化以及农业等领域有广泛的用途,因此是一种重要的无机化工原料。现有制备技术能够制备出合格的氧化亚铜粉末,但是都存在一定的局限性,比如产业化前景不明朗、适用范围窄、难以制备高纯度、均匀分散的氧化亚铜粉末。工业氧化亚铜HG2961-2010标准发布实施后,氧化亚铜产品的质量要求也相应提高。原有的氧化亚铜制备技术已经不能适应新的工业标准,因此迫切需要新的优化技术来提升产品质量。这其中提高氧化亚铜含量、降低杂质含量是最关键的因素。因此,在氧化亚铜制备技术中将重点研究如何提高产品纯度,降低杂质含量,改善粉末团聚,减少有毒化学试剂使用,最终能够实现工业化生产。本文采用电解法制备氧化亚铜,采用化学分析、扫描电子显微镜、X射线衍射等测试手段对样品进行了表征,研究了氯化钠浓度、氢氧化钠浓度、反应温度、葡萄糖酸钙浓度以及阳极电流密度对氧化亚铜含量及杂质含量的影响,确定了最佳反应条件:氯化钠浓度为4.30 mol/L,氢氧化钠浓度为0.025 mol/L,反应温度为80℃,电流密度为1000 A/m2,葡萄糖酸钙浓度为0.0002 mol/L。葡萄糖酸钙替代重铬酸钠作为添加剂制备氧化亚铜,既可以得到高纯度氧化亚铜,而且对环境没有污染,符合绿色化学的要求。采用亚硫酸钠还原硫酸铜制备氧化亚铜,采用化学分析、扫描电子显微镜、X射线衍射仪等测试手段对样品进行了表征,研究了铜离子浓度、铜离子与亚硫酸钠用量比、反应温度、反应时间以及反应pH对氧化亚铜含量及杂质含量的影响,确定了最佳反应条件:温度为100℃,反应pH为4.5,铜离子浓度为1.25 mol/L,亚硫酸钠与硫酸铜用量比=1.9:1,反应时间为2小时。通过亚硫酸钠还原氯化铜制备氧化亚铜的正交实验结果,确定了制备氧化亚铜的最佳实验条件:氯离子浓度为6.35 mol/L,反应时间2小时,铜离子浓度2.50 mol/L,反应pH为8.5。通过以印制电路蚀刻废液为原料制备氧化亚铜的正交实验结果,确定了制备氧化亚铜的最佳实验条件:还原反应温度为55℃,反应时间5小时,保温温度70℃。与国内国外主要氧化亚铜生产商的产品做了比较,发现亚硫酸钠还原硫酸铜法、亚硫酸钠还原氯化铜法制备的氧化亚铜已经达到了国际先进水平,尤其是以印制电路蚀刻废液作为铜离子来源,降低了生产成本,是一种低成本、高质量的氧化亚铜制备方法。
[Abstract]:Cuprous oxide is widely used in plastics, coatings, ceramics, glass, industrial catalysis and agriculture. Therefore, it is an important inorganic chemical raw material. The existing preparation technology can prepare qualified cuprous oxide powder, but there are some limitations, such as the prospect of industrialization is not clear, the scope of application is narrow. It is difficult to prepare copper oxide powder with high purity and uniform dispersion. The industrial copper oxide HG2961-2010 standard has been issued and implemented. The quality requirements of cuprous oxide products have been improved accordingly. The original preparation technology of cuprous oxide can not meet the new industrial standards. Therefore, new optimization technology is urgently needed to improve the quality of the product, in which the increase of cuprous oxide content and the reduction of impurity content are the most important factors. In the preparation technology of cuprous oxide, emphasis will be placed on how to improve product purity, reduce impurity content, improve powder agglomeration and reduce the use of toxic chemical reagents. In this paper, copper oxide was prepared by electrolysis. The samples were characterized by chemical analysis, scanning electron microscopy and X-ray diffraction, and the concentration of sodium chloride was studied. The effects of sodium hydroxide concentration, reaction temperature, calcium gluconate concentration and anode current density on the content of cuprous oxide and impurity were investigated. The optimum reaction conditions were determined as follows: sodium chloride concentration was 4.30 mol/L. The concentration of sodium hydroxide is 0.025 mol / L, the reaction temperature is 80 鈩，

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