| Acidic copper chloride etching waste solution is a waste produced during the etching process of printed circuit board.Rich copper resources and hydrochloric acid are found in the waste solution.Direct emissions will cause serious pollution to soil,water resources and endanger human health.The harmless disposal of waste solution is urgent.In this paper,three kinds of fine copper compounds were prepared by chemical treatment of acid copper chloride etching waste solution.The technology preparing copper hydroxide,basic copper carbonate and active copper oxide from acidic copper chloride etching waste liquid was studied,and the optimum synthetic route of each product was determined.The equipment selection,economic benefit estimation and environmental protection analysis of active copper oxide production process were carried out.Meanwhile,fourier infrared spectroscopy?FT-IR?,scanning electron microscopy?SEM?,thermogravimetric analysis?TG?,X-ray diffraction?XRD?and other means were used to characterize the product.The main research results of this paper are as follows:?1?The optimal preparation conditions for preparing copper hydroxide from acidic copper chloride etching waste solution were determined.The p H was 13,the precipitant ratio n?Na OH?:n?HFD?was 9.8:0.2,the assistant was C,the etching solution diluted 1.5times,and drying for 5.5h.XRD and SEM analysis results showed that the copper hydroxide product has single composition and good dispersibility,and the morphology and particle size of the fiber accumulation were between 4?11?m.The results of chemical analysis showed that the recovery rate of copper was?99.9%,and the purity of the product was more than 97.0wt.%,meeting the requirements of copper hydroxide for industrial use.?2?The optimal preparation conditions for preparing basic copper carbonate from acidic copper chloride etching waste solution were determined.The p H was 7,reaction at70?for 1.0h,the etching solution dilution was 1 times,the precipitant ratio n?Na2CO3?:n?Na HCO3?was 1:2,and the precipitant concentration was 3.6mol/L.XRD analysis results showed that the basic copper carbonate product has single composition.The results of chemical analysis showed that the copper content of the product reached 55.52wt.%and Cl-content 130 ppm,which met the requirements of industrial grade basic copper carbonate.?3?The optimal technological conditions for preparing active copper oxide with copper hydroxide as the intermediate were determined.The p H was 11,the reaction temperature was 100?,the reaction time was 70min,the liquid-solid ratio was 13:1,the calcining was temperature 400?,and the calcining time was 40min.XRD and SEM analysis results showed that the copper oxide product has a single composition,bamboo leaf shape,about 2?4?m in length and about 0.2?0.8?m in width,and agglomerated.The results of chemical analysis showed that the purity of the product more than 99.0wt.%and the activity was 17.3s.However,the content of chlorine is 45ppm,which is not in line with the 15ppm required in the industrial active copper oxide standard.?4?The optimal technological conditions for preparing active copper oxide with basic copper carbonate as the intermediate were determined.The reaction temperature95?,the liquid-solid ratio 25:1,the dosage of assistant A was 8.5g,the calcining temperature was 500?,the calcining time was 1.0h.XRD and SEM analysis results showed that the copper oxide product has a single composition,a shape similar to sea urchin,and a diameter of 2?9?m.The results of chemical analysis showed that the product purity reached over 99.0wt.%,the content of chloride ion decreased to below15ppm,and the activity was 14s which met the requirements of industrial active copper oxide standard and could be used in electroplating process.?5?Economic benefit estimation result showed that the preparation of active Cu O with Cu?OH?2·Cu CO3 as the intermediate can produce good economic benefit.The environmental analysis showed that the preparation process was clean and environmental process. |
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