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

A lead dioxide, nanocrystalline technology, applied in lead dioxide, lead oxide, lead dan and other directions, to achieve the effect of less by-products, lower production costs, and solve environmental pollution problems

Inactive Publication Date: 2004-10-20
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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

[0031] Weigh 5 g of analytically pure lead nitrate and dissolve it in 10 mL of water, add solid sodium hydroxide, adjust the pH of the solution to 9.0, add 50 mL of sodium hypochlorite solution (available chlorine content > 5.5%) after the solution is completely dissolved, and stir well. After reacting at 60 °C for 6 h, the obtained precipitate was filtered, washed and dried to obtain a brown powder. The filtrate used 0.01 mol·L -1 The potassium chromate solution was tested, and no yellow lead chromate precipitate was observed, indicating that the reaction was very complete. like 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 microscopy (TEM), from figure 2 It can be seen that the shape of the rod is rod-like, the diameter of the rod is between 10 and 20 nm, the length is 400 nm, and the aspect ratio is more than 20. The synthesized β-lead dioxid...

Embodiment 2

[0033] Weigh 3 g of analytically pure lead hydroxide in 10 mL of water, add sodium hydroxide solution with a concentration of 10%, adjust the pH of the solution to 13.0, add 40 mL of sodium hypochlorite solution (available chlorine content > 5.5%) after the solution is completely dissolved, and stir well. After reacting at 30°C for 24h, the obtained precipitate was filtered, washed and dried to obtain brown α-lead dioxide powder. The filtrate was 0.01mol·L -1 The potassium chromate solution was tested, and no yellow lead chromate precipitate was observed, indicating that the reaction was very complete. The obtained α-lead dioxide was pyrolyzed at 410° C. for 6 hours according to the method in Example 1 to prepare lead tetroxide nanocrystals.

Embodiment 3

[0035] 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 solution is completely dissolved, and stir well. After reacting at 120 °C for 2 h, the obtained precipitate was filtered, washed and dried to obtain brown β-lead dioxide powder. The filtrate was 0.01 mol·L -1 The potassium chromate solution was tested, and no yellow lead chromate precipitate was observed, indicating that the reaction was very complete. The obtained β-lead dioxide was pyrolyzed at 430° C. for 4 hours according to the method in Example 1 to prepare lead tetroxide 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 α and β type lead dioxide nanocrystals and lead tetroxide nanocrystals. Background technique [0002] Lead dioxide is a strong oxidant that can catch fire when ground with sulfur or red phosphorus, so it is used in matchmaking. It is also one of the basic components of lead-acid battery plates. There are two crystal forms of lead dioxide, α-type belongs to orthorhombic system, β-type belongs to tetragonal system, and α-lead dioxide is inferior to β-lead dioxide in terms of electrical conductivity and corrosion resistance. The Journal of Powder Sources, 1998, Vol. 73, pp. 152-161, and 2000, Vol. 88, pp. 232-236, reported the differences in the properties of lead dioxide with different crystal forms. At present, lead dioxide is mainly prepared by electrolysis, and this method was reported on pages 2279-2288, Vol. The preparation of lead dioxid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G21/08C01G21/10
Inventor 庄京李亚栋
Owner TSINGHUA UNIV
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