1. Electrochemical preparation of cuprous oxid powder: Part II. Process conditions
- Author
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W. C. Cooper and J. Ji
- Subjects
Electrolysis ,General Chemical Engineering ,Inorganic chemistry ,Sodium chromate ,Oxide ,chemistry.chemical_element ,Electrolyte ,Electrochemistry ,Copper ,Chloride ,law.invention ,chemistry.chemical_compound ,chemistry ,law ,Materials Chemistry ,medicine ,Electrolytic process ,medicine.drug - Abstract
Practical electrosynthesis of cuprous oxide powder was carried out on a laboratory scale in a cell specially constructed both with and without a diaphragm under the various operating conditions guided by the authors' previous research. The electrolysis was appraised in terms of the quality of the cuprous oxide product, the electrodissolution of the copper anode, and the SEM microstructure of the cuprous oxide powder. In a cell having a diaphragm, of which nylon fabric is the best, the optimal electrolysis operating conditions are: 250gl−1 NaCl, 0.1–1.0gl−1 NaOH, 500–1500Am−2, 80°C, perforated titanium sheet as the cathode, and around 3% cell volume of electrolyte circulation per minute. Under these conditions a product containing more than 97% cuprous oxide can easily be produced with very stable electrolysis and quite uniform dissolution of the copper anode. To eliminate the use of a diaphragm in the cell, the addition of sodium chromate, sodium dichromate, or calcium gluconate is effective in a sense, depending upon the requirements of the cuprous oxide product. For a product in which more than 95% cuprous oxide and no copper powder are required but a slightly higher content of chloride is allowable, sodium chromate and dichromate can be proposed for use with the former around 0.03–0.05gl−1 and the latter around 0.020–0.025gl−1, although the copper anode will not be perfectly evenly dissolved. For a product in which more than 97% cuprous oxide is demanded and a very small amount of copper powder is tolerated, calcium gluconate would be acceptable at around 4.5gl−1 with quite even dissolution of the copper anode. As to the auxiliary additives, hydrazine hydrate has a negative effect on the quality of the cuprous oxide product. Sucrose can cause a small increase in the chloride content but can make the particles of cuprous oxide more compact thereby increasing sharply its apparent density. Hydroxylamine hydrochloride is the best auxiliary additive which has a positive effect on the purity of the cuprous oxide product but produces no obvious change in the microstructure on the cuprous oxide particles. Even though most work has been concentrated on the electrolytic process, the subsequent processes are equally important: 65–70°C, distilled water for washing, benzotriazole in ethanol solution for stabilization of the cuprous oxide, and 100°C at a vacuum of less than 20mm Hg for drying seem to be satisfactory. A vacuum drying temperature of 55–60°C may be more appropriate to ensure against any oxidation of the product.
- Published
- 1990
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