Process for synthesizing alpha, beta type lead dioxide and leadleaden oxide naon crystal
A technology of lead dioxide and nanocrystals, applied in the direction of lead dioxide, lead oxide, lead red, etc., to achieve the effects of less by-products, lower production costs, and solve environmental pollution problems
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[0029] Example 1:
[0030] Weigh 5 g of analytically pure lead nitrate and dissolve it in 10 mL of water, add solid sodium hydroxide to adjust the pH of the solution to 9.0, add 50 mL of sodium hypochlorite solution (available chlorine content>5.5%) after the dissolution is complete, and stir evenly. After reacting at 60°C for 6 hours, the resulting precipitate was filtered, washed, and dried to obtain a brown powder. The filtrate used 0.01mol·L -1 The potassium chromate solution was tested, and the formation of yellow lead chromate precipitate was not observed, indicating that the reaction proceeded completely. Such as figure 1 As shown, the product was identified as β-lead dioxide by X-ray powder diffraction; the morphology of β-lead dioxide nanocrystals was analyzed by transmission electron microscope (TEM), from figure 2 It can be seen that its morphology is rod-shaped, the diameter of the rod is between 10-20nm, the length is 400nm, and the aspect ratio is more than 20. Put...
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[0031] Example 2:
[0032] Weigh 3g of analytically pure lead hydroxide into 10mL of water, add 10% sodium hydroxide solution, adjust the pH of the solution to 13.0, and add 40mL sodium hypochlorite solution (available chlorine content>5.5%) after the dissolution is complete, and stir evenly. After reacting at 30°C for 24 hours, the resulting precipitate is filtered, washed, and dried to obtain brown α-lead dioxide powder. The filtrate is 0.01 mol·L -1 The potassium chromate solution was tested, and the formation of yellow lead chromate precipitate was not observed, indicating that the reaction proceeded completely. The obtained α-lead dioxide was pyrolyzed at 410° C. for 6 h according to the method in Example 1, to prepare nanocrystals of lead tetroxide.
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[0033] Example 3:
[0034] Weigh 5 g of analytically pure lead oxide in 10 mL of water, add solid sodium hydroxide to adjust the pH of the solution to 10.0, add 50 mL of sodium hypochlorite solution (available chlorine content>5.5%) after the dissolution is complete, and stir evenly. After reacting at 120°C for 2 hours, the resulting precipitate is filtered, washed, and dried to obtain brown β-lead dioxide powder. The filtrate is 0.01 mol·L -1 The potassium chromate solution was tested, and the formation of yellow lead chromate precipitate was not observed, indicating that the reaction proceeded completely. The obtained β-lead dioxide was pyrolyzed at 430° C. for 4 hours according to the method in Example 1, to prepare nanocrystals of lead tetroxide.
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