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Method for preparing tetrabasic lead sulfate

A tetrabasic lead sulfate and sulfuric acid technology, applied in lead sulfate and other directions, can solve the problems of uneven particle size, low impurity content, and high equipment requirements, and achieve uniform and controllable particle size, high purity, and simple and controllable process. Effect

Active Publication Date: 2016-01-27
SHENZHEN CENT POWER TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims at the technical problems of high equipment requirements, low yield and product purity and uneven particle size existing in various methods for preparing tetrabasic lead sulfate in the prior art, and provides a method starting from lead acetate. Novel process for preparing tetrabasic lead sulfate with high purity, low impurity content and uniform particle size from starting materials

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  • Method for preparing tetrabasic lead sulfate
  • Method for preparing tetrabasic lead sulfate
  • Method for preparing tetrabasic lead sulfate

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Embodiment 1

[0055] A lead acetate solution is obtained by leaching waste lead plaster with acetic acid, and the obtained lead acetate solution is adjusted to a pH of about 5 through ammonia water or sodium hydroxide, and filtered through a filter membrane to obtain a lead acetate solution from which impurities are removed. The concentration of the impurity-removing lead acetate solution was determined to be 0.7924mol / L, and the dosage of sodium hydroxide was determined according to the molar ratio of sodium hydroxide / lead acetate of 2.5:1. Heat 100 mL of impurity-removing lead acetate solution to 90° C., add 20.64 g of 40 wt % sodium hydroxide solution preheated to 90° C., stir and react for 30 minutes to obtain lead oxide, and its XRD pattern is as follows: image 3 shown. The obtained lead oxide and 20wt% sulfuric acid solution and deionized water are mixed according to the mass ratio of 1:0.4484:4~10, stirred and reacted at 80°C for 1 hour, the obtained mixture is filtered, and the fil...

Embodiment 2

[0057] A lead acetate solution is obtained by leaching waste lead plaster with acetic acid, and the obtained lead acetate solution is adjusted to a pH of about 5 through ammonia water or sodium hydroxide, and filtered through a filter membrane to obtain a lead acetate solution from which impurities are removed. The concentration of the impurity-removing lead acetate solution was determined to be 0.8107mol / L, and the dosage of sodium hydroxide was determined according to the molar ratio of sodium hydroxide / lead acetate of 2.5:1. Heat 100 mL of impurity-removing lead acetate solution to 90° C., add 21.12 g of 40 wt % sodium hydroxide solution preheated to 90° C., and stir for 30 minutes to obtain lead oxide. The obtained lead oxide and 20wt% sulfuric acid solution and deionized water are mixed according to the mass ratio of 1:0.4484:4~10, stirred and reacted at 80°C for 1 hour, the obtained mixture is filtered, and the filter residue is transferred to a tube furnace at 650°C. Si...

Embodiment 3

[0059] A lead acetate solution is obtained by leaching waste lead plaster with acetic acid, and the obtained lead acetate solution is adjusted to a pH of about 5 through ammonia water or sodium hydroxide, and filtered through a filter membrane to obtain a lead acetate solution from which impurities are removed. The concentration of the impurity-removing lead acetate solution was determined to be 0.8107mol / L, and the dosage of sodium hydroxide was determined according to the molar ratio of sodium hydroxide / lead acetate of 2.5:1. Heat 100 mL of impurity-removing lead acetate solution to 90° C., add 21.12 g of 40 wt % sodium hydroxide solution preheated to 90° C., and stir for 30 minutes to obtain lead oxide. The obtained lead oxide and 20wt% sulfuric acid solution and deionized water are mixed according to the mass ratio of 1:0.4484:4~10, stirred and reacted at 80°C for 1 hour, the obtained mixture is filtered, and the filter residue is transferred to a tube furnace at 450 Sinte...

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Abstract

The invention provides a method for preparing tetrabasic lead sulfate. The method comprises the following steps: S10. impurities are removed from a lead acetate stock solution, so as to obtain a lead acetate solution; S20. the lead acetate solution is mixed with an alkaline solution under a heated condition, and lead oxide is obtained after filtering; S30. the lead oxide is mixed with sulfuric acid, filtering is carried out after reaction, and ball milling is carried out after sintering to obtain the tetrabasic lead sulfate. The method provided by the invention has the advantages of simple and controllable processes, high product purity (above 99 percent), and uniform and controllable particle sizes; moreover, according to the method, the lead acetate serves as the initiator to prepare the high-purity tetrabasic lead sulfate, and multiple batches of measurements of the tetrabasic lead sulfate show that the contents of iron element and barium element, which are the impurities significantly affecting the battery performance, are below 20 ppm and below 2 ppm respectively.

Description

technical field [0001] The invention relates to the field of lead-acid batteries, in particular to a method for preparing tetrabasic lead sulfate. Background technique [0002] Tetrabasic lead sulfate (4PbO·PbSO 4 , referred to as 4BS) as a positive electrode additive, which is added to the positive plate as a seed crystal, promotes the formation of the active material skeleton during the battery production and curing process, shortens the curing time, optimizes the crystal structure and distribution of the plate, and prolongs the battery cycle. life. It is widely used and relatively expensive. [0003] At present, there are many methods for preparing 4BS. The common preparation methods use lead oxide and lead powder or lead-containing waste in the battery production process as raw materials, and adopt methods such as hydrothermal synthesis, ball milling, and sintering. The 4BS prepared by the hydrothermal synthesis method is rod-shaped and has a large particle size. As a...

Claims

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Application Information

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IPC IPC(8): C01G21/20
Inventor 李名扬张衍夫杨家宽喻文昊胡金丰胡雨辰张伟董金鑫梁莎吴旭胡敬平
Owner SHENZHEN CENT POWER TECH
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