阅读说明：本技术 一种废旧铅膏回收方法 (Waste lead plaster recovery method ) 是由 代少振 项晨 于 2020-10-09 设计创作，主要内容包括：本发明涉及一种废旧铅膏回收方法,其特征在于,包括如下步骤：步骤1：废铅膏与硫酸反应得到硫酸铅铅膏；步骤2,硫酸铅与碳酸氨反应,固液分离后得到碳酸铅与硫酸氨溶液；步骤3,硫酸氨溶液加入氧化钙反应,固液分离得到硫酸钙与氨水溶液,碳酸铅高温熔炼后得到粗铅与二氧化碳气体；步骤4,硫酸钙高温熔炼后得到氧化钙、二氧化硫与二氧化碳气体,二氧化硫用于制备硫酸返回步骤1中与废铅膏反应,所述氧化钙用于返回加入步骤3中的硫酸氨溶液制备氨水,所述二氧化碳与所述氨水吸收制备碳酸氨溶液用于步骤2中制得碳酸铅。本发明的废旧铅膏回收方法,回收形成循环系统、效率高。(The invention relates to a waste lead plaster recovery method, which is characterized by comprising the following steps: step 1: reacting the waste lead plaster with sulfuric acid to obtain lead sulfate lead plaster; step 2, reacting lead sulfate with ammonium carbonate, and carrying out solid-liquid separation to obtain a solution of lead carbonate and ammonium sulfate; step 3, adding calcium oxide into the ammonium sulfate solution for reaction, performing solid-liquid separation to obtain calcium sulfate and an ammonia water solution, and smelting lead carbonate at high temperature to obtain lead bullion and carbon dioxide gas; and 4, calcium sulfate is smelted at a high temperature to obtain calcium oxide, sulfur dioxide and carbon dioxide gas, the sulfur dioxide is used for preparing sulfuric acid and returns to the step 1 to react with the waste lead paste, the calcium oxide is used for returning and adding the ammonium sulfate solution in the step 3 to prepare ammonia water, and the carbon dioxide and the ammonia water are absorbed to prepare an ammonia carbonate solution which is used for preparing lead carbonate in the step 2. The waste lead plaster recovery method provided by the invention has the advantages that the waste lead plaster is recovered to form a circulating system, and the efficiency is high.)

1. A waste lead plaster recovery method is characterized by comprising the following steps: step 1: reacting the waste lead plaster with sulfuric acid to obtain lead sulfate lead plaster; step 2, reacting lead sulfate with ammonium carbonate, and carrying out solid-liquid separation to obtain a solution of lead carbonate and ammonium sulfate; step 3, adding calcium oxide into the ammonium sulfate solution for reaction, performing solid-liquid separation to obtain calcium sulfate and an ammonia water solution, and smelting lead carbonate at high temperature to obtain lead bullion and carbon dioxide gas; and 4, calcium sulfate is smelted at a high temperature to obtain calcium oxide, sulfur dioxide and carbon dioxide gas, the sulfur dioxide is used for preparing sulfuric acid and returns to the step 1 to react with the waste lead paste, the calcium oxide is used for returning and adding the ammonium sulfate solution in the step 3 to prepare ammonia water, and the carbon dioxide and the ammonia water are absorbed to prepare an ammonia carbonate solution which is used for preparing lead carbonate in the step 2.

2. The waste lead plaster recovery method according to claim 1, wherein in the step 1, the waste lead plaster is conveyed into a reaction kettle to be mixed with 10% -30% of waste sulfuric acid for shearing reaction for 1-3h, and the reaction temperature is 70-100 ℃, so that the lead sulfate lead plaster is obtained.

3. The method for recycling the waste lead plaster according to the claim 1, wherein in the step 2, the lead sulfate and the ammonium carbonate are mixed and subjected to a shearing reaction at normal temperature for 1-2h, and a solution of the lead carbonate and the ammonium sulfate is obtained after solid-liquid separation.

4. The waste lead plaster recovery method according to claim 1, wherein in the step 3, calcium oxide is added into the ammonium sulfate solution, mixed at normal temperature, ground and sheared for 1-3 hours, and the calcium sulfate and the ammonia water solution are obtained through solid-liquid separation.

5. The method for recycling waste lead plaster as claimed in claim 1, wherein in the step 3, the lead carbonate and the coal powder are mixed and smelted at the temperature of 700-900 ℃ to obtain crude lead and carbon dioxide gas, and the crude lead and the carbon dioxide gas are absorbed by ammonia water after surface cooling to prepare the ammonia carbonate solution.

6. The method for recycling waste diachylon as claimed in claim 1, wherein in the step 4, the calcium sulfate and the coal powder are mixed and calcined at the temperature of 600-800 ℃ to obtain calcium oxide, sulfur dioxide and carbon dioxide gas, and the sulfur dioxide is absorbed by hydrogen peroxide to prepare sulfuric acid.

7. The method for recycling waste lead plaster as claimed in claim 1, wherein the carbon dioxide for preparing the ammonia carbonate solution by reacting with the ammonia water comprises carbon dioxide obtained by smelting calcium sulfate and carbon dioxide obtained by smelting lead carbonate.

Technical Field

The invention relates to the technical field of waste treatment.

Background

The waste lead plaster mainly comprises the following components: the lead sulfate content is about 50% -60%, the lead dioxide content is about 20% -30%, the lead oxide content is about 5% -15%, and the metallic lead content is about 1% -2%. Because the melting point and the decomposition temperature of the lead sulfate are high, the property is stable, the chemical conversion reaction is difficult to occur, and lead dioxide (generally regarded as the anhydride of the original high lead acid or higher lead acid) has strong oxidizing property and is insoluble in oxidizing acid and alkali, the recycling treatment of the waste lead plaster becomes the key point for recycling the waste lead-acid storage battery.

Disclosure of Invention

In order to solve the technical problem, the invention provides a waste lead plaster recovery method, which is characterized by comprising the following steps: step 1: reacting the waste lead plaster with sulfuric acid to obtain lead sulfate lead plaster; step 2, reacting lead sulfate with ammonium carbonate, and carrying out solid-liquid separation to obtain a solution of lead carbonate and ammonium sulfate; step 3, adding calcium oxide into the ammonium sulfate solution for reaction, performing solid-liquid separation to obtain calcium sulfate and an ammonia water solution, and smelting lead carbonate at high temperature to obtain lead bullion and carbon dioxide gas; and 4, calcium sulfate is smelted at a high temperature to obtain calcium oxide, sulfur dioxide and carbon dioxide gas, the sulfur dioxide is used for preparing sulfuric acid and returns to the step 1 to react with the waste lead paste, the calcium oxide is used for returning and adding the ammonium sulfate solution in the step 3 to prepare ammonia water, and the carbon dioxide and the ammonia water are absorbed to prepare an ammonia carbonate solution which is used for preparing lead carbonate in the step 2.

Further, in the step 1, the waste lead plaster is conveyed into a reaction kettle to be mixed with 10% -30% of waste sulfuric acid and subjected to shearing reaction for 1-3 hours at the reaction temperature of 70-100 ℃, so that the lead sulfate lead plaster is obtained.

Further, in the step 2, the lead sulfate and the ammonium carbonate are mixed and subjected to a shearing reaction at normal temperature for 1-2 hours, and a solution of the lead carbonate and the ammonium sulfate is obtained after solid-liquid separation.

Further, in the step 3, adding calcium oxide into the ammonium sulfate solution, mixing, grinding and shearing at normal temperature for 1-3h, and performing solid-liquid separation to obtain calcium sulfate and an ammonia water solution.

Further, in the step 3, the lead carbonate and the coal powder are mixed and smelted at the temperature of 700-900 ℃ to obtain crude lead and carbon dioxide gas, and the crude lead and the carbon dioxide gas are absorbed by ammonia water after surface cooling to prepare an ammonia carbonate solution.

Further, in the step 4, the calcium sulfate and the coal powder are mixed and calcined at the temperature of 600-.

Further, in the step 1, the carbon dioxide which reacts with the ammonia water to prepare the ammonia carbonate solution includes carbon dioxide obtained by melting calcium sulfate and carbon dioxide obtained by melting lead carbonate.

The waste lead plaster recovery method provided by the invention has the advantages that the waste lead plaster is recovered to form a circulating system, and the efficiency is high.

Drawings

FIG. 1 is a flow chart of the waste lead plaster recovery process of the present invention.

Detailed Description

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

As shown in fig. 1

Step 1: lead sulfate preparation

And conveying the waste lead plaster into a reaction kettle, mixing and shearing the waste lead plaster with 10-30% of waste sulfuric acid for 1-3 hours at the reaction temperature of 70-100 ℃ to obtain the lead sulfate lead plaster. The reaction formula is as follows:

PbO+H2SO4→PbSO4+H2O

PbO2+Pb+2H2SO4→2PbSO4+2H2O

2PbO2+2H2SO4→2PbSO4+2H2O+O2

step 2: preparation of lead carbonate

And (3) mixing the lead sulfate prepared in the step (1) with ammonia carbonate, carrying out shearing reaction for 1-2h at normal temperature, and carrying out solid-liquid separation to obtain a solution of lead carbonate and ammonia sulfate. The reaction formula is as follows:

PbSO4+(NH4)2CO3→PbCO3+(NH4)2SO4

and step 3: preparation of ammonia water from ammonia sulfate and smelting of lead carbonate

And (3) adding the ammonium sulfate solution prepared in the step (2) into calcium oxide, mixing, grinding and shearing at normal temperature for 1-3h, and carrying out solid-liquid separation to obtain calcium sulfate and an ammonia water solution. The reaction formula is as follows:

(NH4)2SO4+CaO+H2O→CaSO4+2NH3.H2O

mixing the lead carbonate and the coal powder in the step 2, smelting at the temperature of 700-900 ℃ to obtain crude lead and carbon dioxide gas,

the reaction formula is as follows:

2PbCO3+C→2Pb+3CO2

and (4) cooling the surface of the carbon dioxide, and absorbing the cooled carbon dioxide with ammonia water to prepare an ammonia carbonate solution.

And 4, step 4: calcination of calcium sulfate

Mixing calcium sulfate and coal powder, calcining at the temperature of 600-800 ℃, calcining to obtain calcium oxide, sulfur dioxide and carbon dioxide gas, wherein the calcium oxide is used for preparing ammonia water, the sulfur dioxide is absorbed by hydrogen peroxide to prepare sulfuric acid for recycling, the carbon dioxide and the ammonia water are absorbed to prepare ammonia carbonate solution for recycling, and the carbon dioxide can comprise carbon dioxide formed by mixing and calcining calcium sulfate and coal powder, and lead carbonate and coal powder, and are mixed and smelted to obtain carbon dioxide.

The reaction equation is as follows: 2CaSO4+ C → 2CaO + CO2+2SO2

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.