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Preparation of nanometer cuprous oxide by microwave assisted reduction under atmospheric pressure

2019-04-16
Cuprous oxide is a copper inorganic salt with higher added value than copper sulfate, and is widely used in the coating industry, glass industry, agriculture and other fields. In recent years, with the ultra-fine and high purity of cuprous oxide, its application value has been greatly improved. The particle size of Cu2O prepared by the preparation method of several kinds of Cu2O particles in the country is usually in the range of several micrometers to several tens of micrometers, and the dispersibility is poor. In this study, nano-sized cuprous oxide was prepared by microwave-assisted sodium sulfite reduction under normal pressure. Several factors affecting the yield of cuprous oxide were investigated. The surface morphology and particle size distribution of Cu2O were characterized.


 
 
    First, reagents and instruments
 
    Reagents: self-produced copper sulfate, sodium sulfite, self-dispensing agent.
 
    Instruments: NN-S3440WF household modified microwave oven, electronic constant speed mixer, electric thermostatic water bath, XL30W scanning electron microscope, LS800 laser particle size tester.
 
    Second, the principle of testing
 
    Copper sulfate and sodium sulfite were separately prepared into a solution of a certain concentration, and mechanical impurities in the solution were removed by filtration. The copper sulfate and sodium sulfite solutions to which the dispersing agent was adjusted and adjusted in pH were separately charged into the dosing bottle. After the reaction was started, the two solutions were cocurrently added to the Erlenmeyer flask in the microwave oven through a Y-shaped tube. After the reaction was completed, the Erlenmeyer flask was taken out, clarified, filtered, and repeatedly washed with alcohol until the sulfate was qualified. The product is kept in an anhydrous alcohol medium to prevent oxidation. Its reaction formula is issued:
 
2CuSO4+3Na2SO3→Cu2O+3Na2SO4+2SO2(g)
It can be seen from Table 1 that when the microwave power is 140W, the color of the solution after the reaction is light green, indicating that there is still a part of unreacted copper ions in the solution after the reaction, and the yield of copper is low; when the microwave power is 530 W, the reaction process A large amount of SO2 gas is generated, the operating environment is deteriorated, and a large amount of green-white powder is present in the cup wall and U-shaped tube, indicating that high-power microwave radiation causes the solution to reach a boiling state, and the solution is largely volatilized, which not only causes large copper loss, but also production equipment. The corrosion is severe; when the microwave power is 320W, the solution after the reaction is colorless, and the product is mud red. Therefore, the microwave radiation power is preferably 320W.