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氧化亞銅制備及其工藝優(yōu)化研究

發(fā)布時(shí)間:2018-01-04 23:01

  本文關(guān)鍵詞:氧化亞銅制備及其工藝優(yōu)化研究 出處:《電子科技大學(xué)》2016年碩士論文 論文類(lèi)型:學(xué)位論文


  更多相關(guān)文章: 氧化亞銅 電解法 亞硫酸鈉 印制電路蝕刻廢液 循環(huán)利用


【摘要】:氧化亞銅在塑料、涂料、陶瓷、玻璃、工業(yè)催化以及農(nóng)業(yè)等領(lǐng)域有廣泛的用途,因此是一種重要的無(wú)機(jī)化工原料,F(xiàn)有制備技術(shù)能夠制備出合格的氧化亞銅粉末,但是都存在一定的局限性,比如產(chǎn)業(yè)化前景不明朗、適用范圍窄、難以制備高純度、均勻分散的氧化亞銅粉末。工業(yè)氧化亞銅HG2961-2010標(biāo)準(zhǔn)發(fā)布實(shí)施后,氧化亞銅產(chǎn)品的質(zhì)量要求也相應(yīng)提高。原有的氧化亞銅制備技術(shù)已經(jīng)不能適應(yīng)新的工業(yè)標(biāo)準(zhǔn),因此迫切需要新的優(yōu)化技術(shù)來(lái)提升產(chǎn)品質(zhì)量。這其中提高氧化亞銅含量、降低雜質(zhì)含量是最關(guān)鍵的因素。因此,在氧化亞銅制備技術(shù)中將重點(diǎn)研究如何提高產(chǎn)品純度,降低雜質(zhì)含量,改善粉末團(tuán)聚,減少有毒化學(xué)試劑使用,最終能夠?qū)崿F(xiàn)工業(yè)化生產(chǎn)。本文采用電解法制備氧化亞銅,采用化學(xué)分析、掃描電子顯微鏡、X射線衍射等測(cè)試手段對(duì)樣品進(jìn)行了表征,研究了氯化鈉濃度、氫氧化鈉濃度、反應(yīng)溫度、葡萄糖酸鈣濃度以及陽(yáng)極電流密度對(duì)氧化亞銅含量及雜質(zhì)含量的影響,確定了最佳反應(yīng)條件:氯化鈉濃度為4.30 mol/L,氫氧化鈉濃度為0.025 mol/L,反應(yīng)溫度為80℃,電流密度為1000 A/m2,葡萄糖酸鈣濃度為0.0002 mol/L。葡萄糖酸鈣替代重鉻酸鈉作為添加劑制備氧化亞銅,既可以得到高純度氧化亞銅,而且對(duì)環(huán)境沒(méi)有污染,符合綠色化學(xué)的要求。采用亞硫酸鈉還原硫酸銅制備氧化亞銅,采用化學(xué)分析、掃描電子顯微鏡、X射線衍射儀等測(cè)試手段對(duì)樣品進(jìn)行了表征,研究了銅離子濃度、銅離子與亞硫酸鈉用量比、反應(yīng)溫度、反應(yīng)時(shí)間以及反應(yīng)pH對(duì)氧化亞銅含量及雜質(zhì)含量的影響,確定了最佳反應(yīng)條件:溫度為100℃,反應(yīng)pH為4.5,銅離子濃度為1.25 mol/L,亞硫酸鈉與硫酸銅用量比=1.9:1,反應(yīng)時(shí)間為2小時(shí)。通過(guò)亞硫酸鈉還原氯化銅制備氧化亞銅的正交實(shí)驗(yàn)結(jié)果,確定了制備氧化亞銅的最佳實(shí)驗(yàn)條件:氯離子濃度為6.35 mol/L,反應(yīng)時(shí)間2小時(shí),銅離子濃度2.50 mol/L,反應(yīng)pH為8.5。通過(guò)以印制電路蝕刻廢液為原料制備氧化亞銅的正交實(shí)驗(yàn)結(jié)果,確定了制備氧化亞銅的最佳實(shí)驗(yàn)條件:還原反應(yīng)溫度為55℃,反應(yīng)時(shí)間5小時(shí),保溫溫度70℃。與國(guó)內(nèi)國(guó)外主要氧化亞銅生產(chǎn)商的產(chǎn)品做了比較,發(fā)現(xiàn)亞硫酸鈉還原硫酸銅法、亞硫酸鈉還原氯化銅法制備的氧化亞銅已經(jīng)達(dá)到了國(guó)際先進(jìn)水平,尤其是以印制電路蝕刻廢液作為銅離子來(lái)源,降低了生產(chǎn)成本,是一種低成本、高質(zhì)量的氧化亞銅制備方法。
[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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