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Method for preparing nano lead product by lead plaster of waste lead-acid storage batteries

A technology of waste lead-acid batteries and lead compounds, which is applied in the field of preparing nano-PbO from PbS and lead acetate crystals, can solve the problems of nano-PbO and PbS that have not yet been seen, and achieve high efficiency, low pollution, and mitigation of environmental hazards.

Active Publication Date: 2012-12-12
STATE GRID HENAN ELECTRIC POWER ELECTRIC POWER SCI RES INST +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent 200880001666.1 proposes to use lead paste to prepare nano-PbO 2 and Pb 3 o 4 method, there is no relevant report on the use of lead paste to prepare nano-PbO and PbS

Method used

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  • Method for preparing nano lead product by lead plaster of waste lead-acid storage batteries
  • Method for preparing nano lead product by lead plaster of waste lead-acid storage batteries

Examples

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Effect test

Embodiment 1

[0020] A method for preparing nano-lead compounds from waste lead-acid storage battery lead paste, specifically as follows:

[0021] ①Take 1g of lead paste, 10g of sodium acetate, 35g of acetic acid and 3mL of 30% H 2 o 2 After the aqueous solution was mixed, it was diluted with 250 mL of deionized water, and then stirred at 20° C. for 6 h. Filter after the reaction, adjust the pH of the filtrate to 7.1, let it stand for 1 hour, and filter again to obtain 0.95 g of lead acetate crystals. 1 H NMR spectrum (see figure 1 ) shows that the purity of lead acetate crystals is higher. SEM spectrogram test (see figure 2 ) shows that its structure is formed by stacking cuboids of different sizes, and the particle size of the cuboids is hundreds of nanometers.

[0022] ②Take 0.1g of lead acetate crystals formed by the reaction and calcinate at 250°C for 2h to obtain 0.06g of powdery product. The product is analyzed by X-ray diffraction test, and the results are shown in image 3 ...

Embodiment 2

[0025] A method for preparing nano-lead compounds from waste lead-acid storage battery lead paste, specifically as follows:

[0026] ①Take 1.5g of lead paste, 16.5g of sodium acetate, 45g of acetic acid and 4.5mL of 30% H 2 o 2 After the aqueous solutions were mixed, they were diluted with 370 mL of deionized water, and then stirred at 25° C. for 8 h. After the reaction was completed, filter, adjust the pH of the filtrate to 7.2, let it stand for 2 hours, and filter again to obtain 1.37 g of lead acetate crystals.

[0027] ②Take 0.2g of lead acetate crystals produced by the reaction and calcinate them at 300°C for 2h to obtain 0.11g of powdered nano-PbO product with a particle size of about 150-250nm.

[0028] ③Mix 1.5mmol (0.488g) of lead acetate crystals formed by the reaction, 2.7mmol (0.203g) of thioacetamide and 3mmol of sodium dodecylsulfonate (0.864g), and then add 45mL of deionized water and 45mL of ethanol After mixing, put it in a polytetrafluoroethylene-lined rea...

Embodiment 3

[0030] A method for preparing nano-lead compounds from waste lead-acid storage battery lead paste, specifically as follows:

[0031] ①Take 2g of lead plaster, 24g of sodium acetate, 50g of acetic acid and 6mL of 30% H 2 o 2 After the aqueous solution was mixed, it was diluted with 500 mL of deionized water, and then stirred and reacted at 30° C. for 10 h. After the reaction was completed, filter, adjust the pH of the filtrate to 7.3, let it stand for 2 hours, and filter again to obtain 1.83 g of lead acetate crystals.

[0032] ② Take 0.3g of lead acetate crystals formed by the reaction and calcinate at 350°C for 3h to obtain 0.17g of powdered nano-PbO product with a particle size of about 150-250nm.

[0033] ③ Mix 2mmol (0.65g) of lead acetate crystals, 4mmol (0.304g) of thiourea, 3mmol (1.092g) of hexadecyltrimethylammonium bromide, 3mmol of OP-10 (about 1.5g), and then add The mixture consisting of 67mL deionized water and 67mL polyethylene glycol, mixed evenly, placed in...

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Abstract

The invention relates to a method for preparing a nano lead product by lead plaster of waste lead-acid storage batteries. The method comprises the following steps of: mixing the lead plaster, sodium acetate, acetic acid and H2O2 according to a ratio, diluting the mixture by de-ionized water, agitating and reacting the diluted mixture at 20-30 DEG C for 6-10 hours, carrying out solid-liquid separation on the mixture after the reaction, adjusting the pH (Potential of Hydrogen) of the mixture to 7.1-7.3, standing the mixture for 1-2 hours, and filtering the mixture to obtain a lead acetate crystal; calcining the lead acetate crystal at 250-350 DEG C for 2-3 hours to obtain nano PbO powder; and mixing the lead acetate crystal, a sulfur source and a surfactant according to a ratio, adding a liquid medium in the mixture, mixing the mixture and the liquid medium uniformly, placing the obtained mixture into a reaction kettle at 120-130 DEG C for 10-15 hours, naturally cooling the mixture to a room temperature, carrying out solid-liquid separation on the mixture, and washing black sediments by water and ethanol to obtain the nano PbS product. The method disclosed by the invention not only provides a raw material and a method for manufacturing the nano lead product, and is good for relieving environmental damages which are possibly caused by a large amount of waste lead-acid storage batteries and realizing high efficiency and low pollution of a lead resource recycling process.

Description

technical field [0001] The invention belongs to the technical field of preparation of nano-lead compounds, and in particular relates to a method for preparing lead acetate from waste lead-acid storage battery lead paste, and then preparing nano-PbO and PbS from lead acetate crystals. Background technique [0002] The excellent optical, electrical and mechanical properties of one-dimensional semiconductor nanomaterials have made them widely researched and applied in nanotransistors, sensors, optoelectronic devices, etc., especially in nanoelectronic integrated circuits, which have great development prospects. As an important member of Group IV-VI semiconductors, nano-PbO can be used to manufacture burning rate catalysts, active materials for chemical power sources, optical glass with high refractive index, and first-class medical raw materials for surface grinders of precision machine tools, etc., with a wide range of uses. However, due to the smaller energy band gap and larg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/54C22B7/00
CPCY02E60/12Y02P10/20Y02W30/84
Inventor 李东梅吴文龙朱莉娜赵光金汪永威
Owner STATE GRID HENAN ELECTRIC POWER ELECTRIC POWER SCI RES INST
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