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Method for preparing tetrabasic lead sulfate with small grain size with sol-gel method

A tetrabasic lead sulfate, sol-gel technology, applied in lead sulfate, lead-acid battery electrodes, structural parts, etc., can solve problems such as the decrease in specific capacity, and achieve the effects of preventing agglomeration, high product purity, and uniform dispersion.

Active Publication Date: 2016-09-21
BOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current commercial tetrabasic lead sulfate (4BS) has a large grain size and interlocking interconnections, so that a part of 4BS cannot be converted into α-PbO during the formation process. 2 , as an additive will lead to a decrease in specific capacity

Method used

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  • Method for preparing tetrabasic lead sulfate with small grain size with sol-gel method
  • Method for preparing tetrabasic lead sulfate with small grain size with sol-gel method
  • Method for preparing tetrabasic lead sulfate with small grain size with sol-gel method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1.1. Weigh 6.5g of lead acetate and 7.68g of citric acid complexing agent (molar ratio 1:2), dissolve them in 100mL of distilled water under the condition of stirring in a water bath at 90°C, add 0.58g of sulfuric acid solution with a mass concentration of 51%, After the fumed silica dispersant of 0.28g, lead oxide / lead sulfate sol is obtained;

[0033] 1.2. Continue to stir the lead oxide / lead sulfate sol obtained in step 1.1 in a water bath at 90°C, and evaporate to dryness to obtain lead oxide / lead sulfate xerogel;

[0034] 1.3. The lead oxide / lead sulfate xerogel obtained in step 1.2 was pre-sintered at 150°C for 3.5 hours at a low temperature and sintered at a high temperature at 500°C for 5 hours in an air atmosphere to obtain tetrabasic lead sulfate powder;

[0035] 1.4. After grinding the powder obtained in step 1.3, pass through a 200-mesh sieve to obtain tetrabasic lead sulfate (4BS). The grain size of the tetrabasic lead sulfate is 500 nm-1 μm.

[0036] The...

Embodiment 2

[0042] 1.1. Weigh 6.5g of lead acetate and 17.53g of EDTA complexing agent (molar ratio 1:3), dissolve them in 100mL of distilled water under the condition of stirring in a water bath at 80°C, add 0.20g of sulfuric acid solution with a mass concentration of 60%, 0.13 After the fumed silica dispersant of g, continue to stir, obtain plumbous oxide / lead sulfate sol;

[0043] 1.2. Continue to evaporate the lead oxide / lead sulfate sol obtained in step 1.1 under the condition of stirring in an 80°C water bath to obtain lead oxide / lead sulfate xerogel;

[0044] 1.3. The lead oxide / lead sulfate xerogel obtained in step 1.2 was pre-sintered at 200°C for 2 hours at a low temperature and sintered at a high temperature at 400°C for 6 hours in an air atmosphere to obtain tetrabasic lead sulfate powder;

[0045] 1.4. After grinding the powder obtained in step 1.3, pass through a 200-mesh sieve to obtain tetrabasic lead sulfate (4BS).

Embodiment 3

[0047] 1.1. Weigh 6.5g of lead acetate and 3.84g of citric acid complexing agent (molar ratio 1:1), dissolve them in 100mL of distilled water under the condition of stirring in a water bath at 85°C, add 0.58g of sulfuric acid solution with a mass concentration of 15%, After the aluminum oxide dispersant of 0.39g, obtain plumbous oxide / lead sulfate sol;

[0048] 1.2. Continue to stir the lead oxide / lead sulfate sol obtained in step 1.1 in a water bath at 85°C, and evaporate to dryness to obtain lead oxide / lead sulfate xerogel;

[0049] 1.3. The lead oxide / lead sulfate xerogel obtained in step 1.2 was pre-sintered at 550°C for 1.5 hours at a low temperature and sintered at a high temperature at 300°C for 7 hours in an air atmosphere to obtain tetrabasic lead sulfate powder;

[0050] 1.4. After grinding the powder obtained in step 1.3, pass through a 200-mesh sieve to obtain tetrabasic lead sulfate (4BS).

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Abstract

The invention relates to a method for preparing tetrabasic lead sulfate with small grain size with a sol-gel method. The method comprises the following steps: under a water-bath stirring condition, taking lead acetate and a complexing agent to be dissolved in distilled water, and then adding a sulfuric acid solution and a dispersing agent to obtain a lead oxide / lead sulfate sol; continuously stirring the lead oxide / lead sulfate sol in water bath, after drying by distillation, carrying out low-temperature presintering and high-temperature sintering respectively in an air atmosphere so as to obtain tetrabasic lead sulfate powder, grinding, and sieving to obtain the tetrabasic lead sulfate with small grain size. The method has the advantages that the preparation process, condition and equipment are relatively simple, and the synthetic tetrabasic lead sulfate with small grain size has excellent performance as a positive active substance additive, and the specific capacity can be improved while the cycle life of a positive active substance is prolonged.

Description

technical field [0001] The invention relates to a method for preparing tetrabasic lead sulfate (4BS) with small grain size by a sol-gel method. Background technique [0002] Tetrabasic lead sulfate (4BS) is one of the components of the positive electrode active material during the curing process. During the chemical formation process, it can be converted into α-PbO with a relatively coarse grain size. 2 . α-PbO 2 It can be used as the active material skeleton to ensure the smooth progress of charging and discharging, and improve the cycle life of the positive electrode active material of the lead-acid battery. In order to increase the proportion of 4BS in the positive electrode active material, it is common practice to add a part of 4BS as a seed crystal during the process of mixing with lead paste to promote the formation of 4BS during the curing process. The grain size of the current commercial tetrabasic lead sulfate (4BS) is large and interconnected, so that a part of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/62H01M4/20C01G21/20
CPCC01G21/20H01M4/20H01M4/62Y02E60/10
Inventor 郎笑石蔡克迪李兰杨喜宝王莉丽张帆
Owner BOHAI UNIV
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