Method for preparing lead nitrate and lead oxide by using lead plaster of waste lead accumulator

A technology of waste lead storage battery and lead nitrate, which is applied in the field of producing lead nitrate and lead oxide from lead paste of waste lead storage battery. The effect of high product purity and low raw material consumption

Inactive Publication Date: 2010-10-13
HEFEI UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] It can be seen from the above that the current technology for producing lead nitrate and lead oxide from waste lead battery lead paste has problems such as complex process flow, high raw material consumption, low lead recovery rate, and low product purity.

Method used

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  • Method for preparing lead nitrate and lead oxide by using lead plaster of waste lead accumulator

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Embodiment 1: This embodiment is carried out according to the following steps:

[0031] 1. In the lead paste with a particle size of 74 μm, add the ammonium carbonate solution with a weight percent concentration of 6% in a weight ratio of 1:10, stir and react for 2 hours at a temperature of 95 ° C, filter, and wash the filter cake to nearly neutral. Collect filter cake, filtrate and washing solution for later use.

[0032] 2, in the above-mentioned lead paste desulfurization filter cake, it is 1: 10 to add the dilute nitric acid that the weight percent concentration is 7% and the weight ratio is that 1: 0.1 adds the hydrogen peroxide that the volume percent concentration is 30%, reacts at 60 ℃ After 1 hour, filter, the filter residue is sent to the desulfurization process, and the filtrate is collected for use.

[0033] 3. The filtrate obtained by leaching the nitric acid is evaporated and concentrated to a density of 1.32 g / cm3, adding the 70% concentrated nitric aci...

Embodiment 2

[0035] Embodiment 2: This embodiment is carried out according to the following steps:

[0036] 1. In the lead paste with a particle size of 74 μm, add the ammonium carbonate solution with a weight percent concentration of 5.5% in a weight ratio of 1:11, stir and react for 2.5 hours at a temperature of 80 ° C, filter, and wash the filter cake to nearly neutral. Collect filter cake, filtrate and washing solution for later use.

[0037] 2, in the above-mentioned lead paste desulfurization filter cake, it is 1: 9 to add the dilute nitric acid that the weight percentage concentration is 9% and the weight ratio is that 1: 0.15 adds the hydrogen peroxide that the volume percentage concentration is 29% by weight, reacts at 60 ℃ After 1 hour, filter, the filter residue is sent to the desulfurization process, and the filtrate is collected for use.

[0038] 3. The filtrate obtained by leaching the nitric acid was evaporated and concentrated to a density of 1.40g / cm 3 , adding 68% conc...

Embodiment 3

[0040] Embodiment 3: This embodiment is carried out according to the following steps:

[0041]1. In the lead paste with a particle size of 74 μm, add the ammonium carbonate solution with a weight percent concentration of 4.5% in a weight ratio of 1:12, stir and react for 2.5 hours under a temperature condition of 65 ° C, filter, and wash the filter cake to nearly neutral. Collect filter cake, filtrate and washing solution for later use.

[0042] 2, in the above-mentioned lead paste desulfurization filter cake, it is 1: 8.5 by weight to add the diluted nitric acid that the volume percent concentration is 11% and the weight ratio is that 1: 0.2 adds the hydrogen peroxide that the volume percent concentration is 28%, reacts at 45 ℃ 1.5 hours, filter, the filter residue is sent to the desulfurization process, and the filtrate is collected for use.

[0043] 3. The filtrate obtained by leaching the nitric acid was evaporated and concentrated to a density of 1.43g / cm 3 , under sti...

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Abstract

The invention discloses a method for preparing lead nitrate and lead oxide by using lead plaster of a waste lead accumulator, which comprises the following steps of: mixing the lead plaster with the granularity of less than 100 microns and 4.5 to 6.5 percent ammonium carbonate solution in a weight ratio of 1: 10-12, then reacting the mixture for 2 to 3 hours at the temperature of between 60 and 100 DEG C with stirring, separating and washing the reaction product, and collecting filter cakes; then mixing the filter cakes, 6 to 12 percent diluted nitric acid and 28 to 30 percent hydrogen peroxide in turn in a weight ratio of 1: 8-10 and 1: 0.05-0.2 respectively, reacting the mixture for 1 to 1.5 hours at the temperature of between 40 and 60 DEG C with stirring, separating and washing the reaction product, and collecting filtrate; concentrating the filtrate till the density of the solution is 1.30 to 1.45 g / cm<3>, adding 65 to 70 percent nitric acid into the solution in a volume ratio of 1: 8-10 and mixing the solution, reacting the solution for 1 to 2 hours with stirring, separating and washing the reaction product, and drying and dehydrating the filter cakes to obtain a lead nitrate product; and performing reaction conversion on the lead nitrate and sodium hydroxide solution, and calcining the reaction product to obtain a lead oxide product. The purities of both the lead nitrate and the lead oxide are more than or equal to 99 percent. The process adopts closed cycle and has no three-waste emission.

Description

1. Technical field [0001] The invention relates to the technical fields of the recovery and treatment, resource utilization and preparation of inorganic compounds of lead in waste lead-acid batteries, in particular to a method for recycling and processing lead paste of waste lead-acid batteries and preparing lead nitrate and lead oxide by wet process . 2. Background technology [0002] Lead is one of the metals commonly used by human beings, and its output ranks fourth in non-ferrous metals after aluminum, copper and zinc. According to reports, in 2008, the global production and consumption of refined lead reached 8.6895 million tons and 8.7047 million tons respectively. In 2008, my country's refined lead consumption reached 3.1349 million tons. At present, lead is mainly used in lead-acid batteries. According to incomplete statistics, about 80% to 85% of the lead consumed in the world is used for lead-acid batteries. With the rapid development of modern communication an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00
CPCY02P10/20
Inventor 于少明王玉黄宪法马成兵
Owner HEFEI UNIV OF TECH
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