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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

Inactive Publication Date: 2002-07-17
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Throughout the above-mentioned domestic and foreign related research, the research on the selective synthesis of different crystal forms of lead dioxide and lead tetraoxide nanocrystals has not been reported at home and abroad.

Method used

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  • Process for synthesizing alpha, beta type lead dioxide and leadleaden oxide naon crystal
  • Process for synthesizing alpha, beta type lead dioxide and leadleaden oxide naon crystal
  • Process for synthesizing alpha, beta type lead dioxide and leadleaden oxide naon crystal

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Weigh 5g of analytically pure lead nitrate and dissolve it in 10mL of water, add solid sodium hydroxide to adjust the pH of the solution to 9.0, add 50mL 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, and the filtrate was treated with 0.01mol·L -1 Potassium chromate solution was tested, and no yellow lead chromate precipitate was observed, indicating that the reaction was carried out completely. Such as figure 1 Shown, product is identified as β-lead dioxide through X-ray powder diffraction; Carry out morphology analysis to β-lead dioxide nanocrystal with 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 the synthesized...

Embodiment 2

[0032] Weigh 3g of analytically pure lead hydroxide in 10mL of water, add 10% sodium hydroxide solution, adjust the pH of the solution to 13.0, add 40mL of 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 obtained precipitate was filtered, washed and dried to obtain brown α-lead dioxide powder, and the filtrate was treated with 0.01mol·L -1 Potassium chromate solution was tested, and no yellow lead chromate precipitate was observed, indicating that the reaction was carried out completely. The obtained α-lead dioxide was pyrolyzed at 410° C. for 6 hours according to the method in Example 1 to prepare trilead tetraoxide nanocrystals.

Embodiment 3

[0034] Weigh 5g of analytically pure lead oxide into 10mL of water, add solid sodium hydroxide, adjust the pH of the solution to 10.0, add 50mL 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 obtained precipitate was filtered, washed and dried to obtain brown β-lead dioxide powder, and the filtrate was treated with 0.01mol·L -1 Potassium chromate solution was tested, and no yellow lead chromate precipitate was observed, indicating that the reaction was carried out completely. The obtained β-lead dioxide was pyrolyzed at 430° C. for 4 hours according to the method in Example 1 to prepare trilead tetraoxide nanocrystals.

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Abstract

The method for synthesizing alpha and beta type lead dioxide nano crystal and lead tetraoxide nano crystal includes the following steps: adding lead salt or lead oxide into water to prepare solution, adding sodium hydroxide, regulating pH value of solutino to 9-14, making said solution produce liquid-phase reaction with oxidants of chlorine gas, etc., under the condition of 30-60 deg.C can obtain alpha type lead dioxide nano crystal, under the condition of 60-200 deg.C can obtain beta type lead dioxide nano crystal, then pyrolyzing the obtained lead dioxide nano crystal at 410-430 deg.C and can obtain lead tetraoxide nano crystal.

Description

technical field [0001] The invention relates to a preparation method of nanometer oxides, in particular to a method for synthesizing alpha and beta type lead dioxide nanocrystals and trilead tetraoxide nanocrystals. Background technique [0002] Lead dioxide is a strong oxidizer that can be ignited when ground with sulfur or red phosphorus, so it is used in the manufacture of matches. It is also one of the basic components of lead-acid battery plates. There are two crystal forms of lead dioxide, the α type belongs to the orthorhombic crystal system, the β type belongs to the tetragonal crystal system, and the α-lead dioxide is not as good as the β-lead dioxide in terms of conductivity and corrosion resistance. Energy Journal (Journal of Powder Sources) magazine 1998, volume 73, pages 152-161 and 2000, volume 88, pages 232-236 reported the differences in the properties of different crystal forms of lead dioxide. At present, the electrolytic method is mainly used to prepare ...

Claims

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Application Information

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IPC IPC(8): C01G21/08C01G21/10
Inventor 庄京李亚栋
Owner TSINGHUA UNIV
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