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Ultrafine lead oxide prepared from desulfurated lead plaster by means of three-stage process and method thereof

A technology for desulfurization lead paste and lead oxide, applied in lead oxide, recycling technology, regeneration of useful parts, etc., can solve the problems of complex process, high citric acid, high price, low smoke and dust rate, low lead volatilization, etc. The effect of high vertical yield

Inactive Publication Date: 2013-10-30
湖北金洋冶金股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN101573461A adopts citric acid and sodium citrate mixed solution to process lead plaster to prepare superfine lead oxide, consumes more citric acid at the same time, the price is higher, and it is difficult to recover sodium sulfate
The process is relatively complicated, and at the same time, volatile agents such as nitric acid and ammonia water are used in the reaction

Method used

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  • Ultrafine lead oxide prepared from desulfurated lead plaster by means of three-stage process and method thereof
  • Ultrafine lead oxide prepared from desulfurated lead plaster by means of three-stage process and method thereof
  • Ultrafine lead oxide prepared from desulfurated lead plaster by means of three-stage process and method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Preparation of desulfurized lead paste

[0032] After the waste lead-acid batteries are deacidified, they are crushed, sorted, and sieved to obtain the waste lead plaster; the pretreated waste lead plaster is added to the solution with a desulfurizing agent, and the commonly used desulfurizing agents are sodium carbonate, sodium bicarbonate, and ammonium carbonate. After the desulfurization is completed, solid-liquid separation is carried out.

[0033] (2) Preparation of lead acetate solution

[0034] Add the desulfurized lead paste of (1) into the acetic acid solution, the feeding ratio of the desulfurized lead paste and acetic acid is 1:2.5 in the molar ratio of the lead in the desulfurized lead paste to the acetic acid, and at the same time add the reducing agent hydrogen peroxide, the PbO in the desulfurized lead paste 2React with hydrogen peroxide at a molar ratio of 1:1.5, react for 0.5 h and then filter and separate to obtain lead acetate solution. The poss...

Embodiment 2

[0049] Difference with embodiment 1 is: leaching agent is nitric acid, and the molar ratio of the lead in the desulfurization lead paste and nitric acid is that the molar ratio of the lead in the desulfurization lead paste and nitric acid is 1:2.5, add reducing agent hydrogen peroxide simultaneously, the lead in the desulfurization lead paste PbO 2 React with hydrogen peroxide at a molar ratio of 1:1.5, react for 0.5 h and then filter and separate to obtain lead nitrate solution. The possible reaction equation between desulfurization lead paste and nitric acid solution may be:

[0050] PbCO2 3 +2HNO 3 →Pb(NO 3 ) 2 +H 2 O + CO 2 (9)

[0051] PbO+2HNO 3 →Pb(NO 3 ) 2 +H 2 O (10)

[0052] PbO 2 +2HNO 3 +H 2 o 2 →Pb(NO 3 ) 2 +2H 2 O+O 2 (11)

[0053] Pb 3 (CO 3 ) 2 (OH) 2 +6HNO 3 →3Pb(NO 3 ) 2 +4H 2 O+2CO 2 (12)

[0054] Pb 10 O(CO 3 ) 6 (OH) 6 +20HNO 3 →10Pb(NO 3 ) 2 +13H 2 O+6CO 2 (13)

[0055] NaPb 2 (CO 3 ) 2 OH+5HNO 3 →2Pb(NO ...

Embodiment 3

[0061] The difference from Example 1 is that the calcination temperature is 450°C, and the red ultrafine lead oxide compound product is finally obtained, XRD sees Figure 6 , see SEM Figure 7 , Figure 8 , The raw material utilization rate is 98.0%, and the yield is 99.2%. Others are the same as in Example 1, and the main process parameters are shown in Table 1.

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Abstract

The invention discloses ultrafine lead oxide prepared from desulfurated lead plaster by means of three-stage process and a method for preparing the ultrafine lead oxide. The method comprises the following steps of: carrying out a desulfurization and lead plaster acid leaching process by causing the desulfurated lead plaster to react with acid, simultaneously adding a reducing agent, and carrying out solid-liquid separation after the reaction is ended to obtain a plumbic acid containing solution; carrying out a lead carbonate preparation process by causing the plumbic acid containing solution to react with sodium carbonate, carrying out solid-liquid separation, washing and drying to obtain the lead carbonate; carrying out a roasting process by preparing the ultrafine lead carbonate by roasting the lead carbonate, wherein the ultrafine lead oxide can be PbO, Pb3O4, or the mixture of the PbO and the Pb3O4, the mean particle granularity of the ultrafine lead oxide is less than 2 mu m, and the nanocrystalline grain size is less than 500nm. Compared with the prior art, the preparation method of the ultrafine lead oxide disclosed by the invention has the following beneficial effects: the active material of the ultrafine lead oxide powder compound for the production of a storage battery enterprise can be directly prepared, lead volatilize quantity is small, the ash rate is low, the direct lead yield is high, the energy consumption is low, pollutants of sulfur dioxide and the like are not generated, and the like.

Description

technical field [0001] The invention relates to the field of recycling of waste lead-acid batteries, in particular to reclaiming waste lead paste which pollutes the environment from waste lead batteries through wet leaching and low-temperature roasting processes to directly prepare superfine lead powder, which belongs to the technical field of recycled lead production. Background technique [0002] Lead has a wide range of uses, and its annual output ranks fourth among nonferrous metals after aluminum, copper, and zinc. With the increase of the number of automobiles, the lead-acid battery industry has developed rapidly, and the amount of waste lead-acid batteries produced every year is constantly increasing. Lead-acid battery is the battery with the largest output and widest application among all kinds of batteries in the world, and its lead consumption accounts for 82% of the total lead consumption in the world. In order to save limited mineral resources and avoid environm...

Claims

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Application Information

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IPC IPC(8): C22B7/00H01M6/52C01G21/02
CPCY02E60/12Y02P10/20Y02W30/84
Inventor 杨家宽朱新锋李富元周锋刘建文江姝杨丹妮李磊张伟孙晓娟王琴
Owner 湖北金洋冶金股份有限公司
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