阅读说明：本技术 一种红丹的制备方法 (Preparation method of red lead ) 是由 代少振 项晨 于 2020-12-09 设计创作，主要内容包括：本发明涉及一种红丹的制备方法,其特征在于,包括如下步骤：步骤1：对淋酸铅泥进行脱硫,并进行固液分离得到包含脱硫铅泥；步骤2,将脱硫铅泥转入固化室,将其中的游离铅转变成氧化铅；步骤3,将固化得到的固化铅泥转入球磨机高温氧化研磨制备红丹。本发明制备红丹的方法,工艺简单、成本低、效率高。(The invention relates to a preparation method of red lead, which is characterized by comprising the following steps: step 1: desulfurizing the acid leaching lead mud, and performing solid-liquid separation to obtain desulfurized lead mud; step 2, transferring the desulfurized lead mud into a curing chamber, and converting free lead in the desulfurized lead mud into lead oxide; and 3, transferring the solidified lead mud obtained by solidification into a ball mill for high-temperature oxidation grinding to prepare the red lead. The method for preparing the red lead has the advantages of simple process, low cost and high efficiency.)

1. The preparation method of the red lead is characterized by comprising the following steps: step 1: desulfurizing the acid leaching lead mud, and performing solid-liquid separation to obtain desulfurized lead mud; step 2, transferring the desulfurized lead mud into a curing chamber, and converting free lead in the desulfurized lead mud into lead oxide; and 3, transferring the solidified lead mud obtained by solidification into a ball mill for high-temperature oxidation grinding to prepare the red lead.

2. The method for preparing red lead according to claim 1, wherein carbon dioxide is also obtained in the step 3, and the carbon dioxide is used for desulfurizing the waste lead plaster in the step 1.

3. The method for preparing red lead according to claim 2, wherein the carbon dioxide is used for desulfurizing the leached lead mud in step 1 by combining with the ammonia water obtained by reacting the desulfurized mother liquor obtained in step 1 with an alkali salt.

4. The method for preparing red lead according to claims 1-3, wherein step 1 is preceded by a step of pressure filtration of the acid leaching lead slime.

5. The method of claim 1-3, wherein the curing temperature in step 2 is 70-80 ℃.

6. The method for preparing red lead according to claims 1-3, wherein in step 3, the temperature of the ball mill is raised to 310-.

Technical Field

The invention relates to the field of lead-acid storage batteries.

Background

The red lead is an important raw material for manufacturing lead-acid storage batteries, and is widely applied to positive active materials of valve-regulated lead-acid storage batteries, traction batteries, fixed batteries, electric vehicle lead-acid storage batteries and submarine batteries. The main functions of red lead in lead-acid batteries are as follows: 1. shortening the curing time of the green polar plate and improving the curing quality of the polar plate; 2. the formation time is shortened; 3. the initial capacity of the storage battery is improved. At present, red lead is usually required to be added in the preparation method of the positive electrode material of the lead-acid storage battery, and at present, a user usually needs to additionally purchase red lead or additionally use a smelting furnace to prepare the red lead and add the red lead in the paste mixing process, so that the production cost is greatly improved.

Disclosure of Invention

In order to solve the technical problems, the invention provides a method for preparing red lead, which is characterized by comprising the following steps: step 1: desulfurizing the acid leaching lead mud, and performing solid-liquid separation to obtain desulfurized lead mud; step 2, transferring the desulfurized lead mud into a curing chamber, and converting free lead in the desulfurized lead mud into lead oxide; and 3, transferring the solidified lead mud obtained by solidification into a ball mill for high-temperature oxidation grinding to prepare the red lead.

Further, carbon dioxide is also obtained in the step 3, and the carbon dioxide is used for desulfurizing the waste lead plaster in the step 1.

Further, the carbon dioxide is combined with ammonia water obtained after the reaction of the desulfurization mother liquor obtained in the step 1 and alkali salt, and is used for desulfurizing the leached lead mud in the step 1.

Further, before the step 1, a step of performing pressure filtration on the acid leaching lead mud is also included.

Further, the curing temperature in step 2 is 70-80 ℃.

Further, in the step 3, the temperature of the ball mill is raised to 310-.

The method for preparing the red lead has the advantages of simple process, low cost and high efficiency.

Drawings

FIG. 1 is a flow chart of the preparation of red lead according to the present invention.

Detailed Description

The invention is further described below with reference to the specific drawings.

As shown in FIG. 1, the method for preparing red lead according to the present invention is as follows:

(1) positive electrode acid-leaching lead mud filter pressing

Pumping the positive electrode acid leaching lead mud into a filter press for filter pressing to separate out lead mud and dilute sulfuric acid, returning the dilute sulfuric acid to the acid leaching process to adjust the density, continuing to leach acid, and conveying the filter cake lead mud into a desulfurization reaction kettle for later use.

(2) Acid leaching lead mud lead sulfate detection

And detecting the content of lead sulfate in the filter cake lead sulfate leaching mud after filter pressing.

(3) Acid leaching lead mud desulfurization

Putting the metered lead mud into a desulfurization reaction kettle, adding ammonia water with the molar ratio of 2-5:1 to lead sulfate in the lead mud, controlling the mass concentration of the ammonia water to be 5-10%, introducing carbon dioxide gas under the condition of stirring and shearing after the addition is finished, reacting for 1-3h at normal temperature, and after the reaction is finished, performing filter pressing separation to obtain the desulfurized lead mud and a desulfurization mother solution. The reaction equation is as follows: PbSO4+2NH3+ CO2+ H2O → PbCO3+ (NH4)2SO4

(4) Purification of desulfurized mother liquor

Adding 0.1-0.5% of PAC into the desulfurization mother liquor, stirring and mixing for 15-30 min, then continuously adding 0.1-0.5% of PAM, stirring and mixing for 15-30 min, performing filter pressing separation to obtain purified desulfurization mother liquor and a small amount of lead-containing filter residues, and smelting the lead-containing filter residues to prepare crude lead.

(5) Regeneration of purified and desulfurized mother liquor

Adding a mixture of the sulfuric acid radical and the purified desulfurization mother liquor in a molar ratio of 1-1.05: 1, stirring and reacting for 0.5-1 h at normal temperature, and filtering and separating by a ceramic membrane filter to obtain high-purity superfine barium sulfate solid and dilute ammonia solution after the reaction is finished. The reaction equation is as follows:

(NH4)2SO4+Ba(OH)2→BaSO4+NH3.H2O

(6) barium sulfate and ammonia water treatment

And washing barium sulfate with a small amount of pure water to neutral, drying the barium sulfate to be used as a battery additive for recycling, and circularly using dilute ammonia water for desulfurization of the acid leaching lead mud.

(7) Method for preparing red lead from desulfurized lead mud

And putting the desulfurized lead slime and the positive plate into a positive plate curing room together for curing and drying treatment at the temperature of 60-70 ℃ to convert free lead in the desulfurized lead slime into lead oxide. And after the solidification and drying are finished, transferring the lead slime into a ball mill, heating to 310-450 ℃ for reaction for 2-3h, converting lead carbonate in the lead slime into lead oxide, collecting and recycling the byproduct carbon dioxide for desulfurization and conversion of the acid leaching lead slime, then continuously heating to 460-480 ℃ and blowing air, carrying out grinding and oxidation reaction for 3-5h, and obtaining the battery-grade red lead after the reaction is finished. The reactions that occur are as follows: curing and drying: pb + O2 → PbO; and (3) decomposing lead carbonate: PbCO3 → PbO + CO 2; preparing red lead: 6PbO + O2 → 2Pb3O 4.

The method utilizes the waste acid leaching lead mud to prepare the red lead, fully utilizes the waste acid leaching lead mud, and fully utilizes the existing storage battery production equipment such as a curing chamber, a ball mill and the like, and also utilizes the curing temperature of a polar plate of the curing chamber of 60-70 ℃ to convert free lead in the desulfurized lead mud into lead oxide by firstly entering the curing chamber and then entering the ball mill, thereby saving the energy consumption in the oxidation process of the free lead, fully utilizing the space utilization rate of the curing chamber to reduce the production cost and facilitating the rapid oxidation of the free lead. The ball mill does not need to additionally use high-temperature smelting equipment to carry out high-temperature smelting on the desulfurized lead slime.

The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.