# US 8,771,620 B2 · Method for recycling lead from waste glass containing lead

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- Number: US 8,771,620 B2
- Document ID: US8771620B2
- Status: Granted
- Kind: B2
- Application number: 13/814,477
- Filed: 2010-10-27
- Published: 2013-05-23
- Granted: 2014-07-08
- Earliest claimed: 2010-08-09
- Assignees: Shenzhen Gem High-Tech Co., Ltd
- Applicants: Kaihua Xu; Miaomiao Guo; Xianda He; Xiaokui Liang
- Inventors: Kaihua Xu; Miaomiao Guo; Xianda He; Xiaokui Liang
- Web page: https://patentgrep.com/patent/US8771620B2

## CPC

- C22B 13/045: {Recovery from waste materials}
- Y02P 10/20: Recycling
- C22B: PRODUCTION AND REFINING OF METALS (electrolytic C25); PRETREATMENT OF RAW MATERIALS
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

Disclosed is a method for recycling lead from waste glass containing lead, which comprises the following steps: mechanical crushing waste glass containing lead, ball milling and screening to obtain glass powder containing lead; alkaline roasting the glass powder containing lead to obtain a roasted material; mixing polycarboxylic acid complexant and nitric acid to produce leaching agent, and then placing the roasted material into the leaching agent to obtain leachate; regulating pH value of the leachate to solidify metal ion to obtain precipitate, separating and removing impurities, rinsing and drying to obtain chemical product containing lead. The method avoids environment pollution caused by waste glass containing lead.

## Claims

### Claim 1

A method for treating waste glass containing lead, comprising:
(1) providing glass containing lead, mechanically crushing, ball milling and sieving the glass containing lead to obtain glass containing lead powders;
(2) roasting the glass containing lead powders with alkaline liquor to obtain a roasted material;
(3) providing polycarboxylic acid complexing agent and nitric acid, mixing the polycarboxylic acid complexing agent and nitric acid to produce leaching agent, immersing the roasted material in the leaching agent to obtain leachate;
(4) regulating pH value of the leachate, precipitating metal ion to obtain precipitates, separating the precipitates and liquid from the leachate for removing impurities, rinsing and drying the precipitates to obtain chemical product containing lead.

### Claim 2 (depends on 1)

The method as claimed in claim 1, wherein, roasting temperature in said step (2) is in the range of 500° C. to 700° C.

### Claim 3 (depends on 2)

The method as claimed in claim 2, wherein, roasting temperature in said step (2) is 600° C.

### Claim 4 (depends on 1)

The method as claimed in claim 1, wherein, said polycarboxylic acid complexing agent in step (3) is acetic acid or edetic acid.

### Claim 5 (depends on 4)

The method as claimed in claim 4, wherein, said polycarboxylic acid complexing agent in step (3) is acetic acid, mixed with nitric acid according to the volume ratio of 3:1 to 9.

### Claim 6 (depends on 1)

The method as claimed in claim 1, wherein, immersing time temperature in said step (3) is in the range of 60° C. to 100° C.

### Claim 7 (depends on 6)

The method as claimed in claim 6, wherein, immersing time temperature in said step (3) is 80° C.

### Claim 8 (depends on 1)

The method as claimed in claim 1, wherein, said step (4) comprises: (a1) regulating pH value of the leachate to 1-3, adding precipitator SO42− into the leachate, precipitating Pb2+ and Ba2+ to obtain PbSO4 and BaSO4 precipitates; (a2) adding CO32− into the leachate containing the PbSO4 and BaSO4 precipitates as obtained in step (a1), transforming said PbSO4 precipitate into PbCO3 precipitate, (a3) adding HNO3 solution into the leachate containing the PbCO3 and BaSO4 precipitates as obtained in step (a2), reacting PbCO3 with HNO3 to obtain a solution containing Pb(NO3)2 and BaSO4 precipitate; (a4) filtrating the solution containing Pb(NO3)2 and BaSO4 precipitate as obtained in step (a3), separating solid BaSO4 precipitate and liquid Pb(NO3)2 solution for removing impurities; (a5) taking filtrate liquid Pb(NO3)2 solution as obtained in step (a4) and adding said precipitator SO42− again to precipitate Pb2+ to obtain PbSO4 precipitate; (a6) adding strongly alkaline liquor into the solution containing the PbSO4 precipitate as obtained in step (a5) to regulate pH value to 8-10 to produce 3PbO.PbSO4.H2O, rinsing, and drying the obtained 3PbO.PbSO4.H2O.

### Claim 9 (depends on 1)

The method as claimed in claim 1, wherein, said step (4) comprises: (b1) regulating the pH value of said leachate to 11-12; precipitating Pb2+ to obtain Pb(OH)2 precipitate; (b2) filtrating the leachate containing the Pb(OH)2 precipitate as obtained in step (b1), separating solid which is containing Pb(OH)2 precipitate and liquid for removing impurities; (b3) taking solid dregs which is containing Pb(OH)2 precipitate as obtained in step (b2), adding HNO3 solution into the solid dregs which is containing Pb(OH)2 precipitate to regulate pH value to 0.5-1, reacting Pb(OH)2 with HNO3 to obtain a solution containing Pb(NO3)2; (b4) adding SO42− into the solution containing Pb(NO3)2 as obtained in step (b3) to precipitate Pb2+ to obtain PbSO4; (b5) adding strongly alkaline liquor into the solution containing the PbSO4 precipitate as obtained in step (b4) to regulate pH value to 8-10 to produce 3PbO.PbSO4.H2O, rinsing and drying the obtained 3PbO.PbSO4. H2O.

### Claim 10 (depends on 9)

The method as claimed in claim 9, wherein, said step of regulating pH value of said leachate to 11-12 is carried out as follows: adding solid NaOH to regulate pH value of said leachate to 6, then adding 10 mol/L NaOH solution to regulate pH value of said leachate to 11-12.

### Claim 11 (depends on 2)

The method as claimed in claim 2, wherein, said polycarboxylic acid complexing agent in step (3) is acetic acid or edetic acid.

### Claim 12 (depends on 3)

The method as claimed in claim 3, wherein, said polycarboxylic acid complexing agent in step (3) is acetic acid or edetic acid.

### Claim 13 (depends on 2)

The method as claimed in claim 2, wherein, immersing temperature in said step (3) is in the range of 60° C. to 100° C.

### Claim 14 (depends on 3)

The method as claimed in claim 3, wherein, immersing temperature in said step (3) is in the range of 60° C. to 100° C.

### Claim 15 (depends on 2)

The method as claimed in claim 2, wherein, said step (4) comprises: (a1) regulating pH value of the leachate to 1-3, adding precipitator SO42− into the leachate, precipitating Pb2+ and Ba2+ to obtain PbSO4 and BaSO4 precipitates; (a2) adding CO32− into the leachate containing the PbSO4 and BaSO4 precipitates as obtained in step (a1), transforming said PbSO4 precipitate into PbCO3 precipitate, (a3) adding HNO3 solution into the leachate containing the PbCO3 and BaSO4 precipitates as obtained in step (a2), reacting PbCO3 with HNO3 to obtain a solution containing Pb(NO3)2 and BaSO4 precipitate; (a4) filtrating the solution containing Pb(NO3)2 and BaSO4 precipitate as obtained in step (a3), separating solid BaSO4 precipitate and liquid Pb(NO3)2 solution for removing impurities; (a5) taking filtrate liquid Pb(NO3)2 solution as obtained in step (a4) and adding said precipitator SO42− again to precipitate Pb2+ to obtain PbSO4 precipitate; (a6) adding strongly alkaline liquor into the solution containing the PbSO4 precipitate as obtained in step (a5) to regulate pH value to 8-10 to produce 3PbO.PbSO4.H2O, rinsing, and drying the obtained 3PbO.PbSO4. H2O.

### Claim 16 (depends on 3)

The method as claimed in claim 3, wherein, said step (4) comprises: (a1) regulating pH value of the leachate to 1-3, adding precipitator SO42− into the leachate, precipitating Pb2+ and Ba2+ to obtain PbSO4 and BaSO4 precipitates; (a2) adding CO32− into the leachate containing the PbSO4 and BaSO4 precipitates as obtained in step (a1), transforming said PbSO4 precipitate into PbCO3 precipitate, (a3) adding HNO3 solution into the leachate containing the PbCO3 and BaSO4 precipitates as obtained in step (a2), reacting PbCO3 with HNO3 to obtain a solution containing Pb(NO3)2 and BaSO4 precipitate; (a4) filtrating the solution containing Pb(NO3)2 and BaSO4 precipitate as obtained in step (a3), separating solid BaSO4 precipitate and liquid Pb(NO3)2 solution for removing impurities; (a5) taking filtrate liquid Pb(NO3)2 solution as obtained in step (a4) and adding said precipitator SO42− again to precipitate Pb2+ to obtain PbSO4 precipitate; (a6) adding strongly alkaline liquor into the solution containing the PbSO4 precipitate as obtained in step (a5) to regulate pH value to 8-10 to produce 3PbO.PbSO4.H2O, rinsing, and drying the obtained 3PbO.PbSO4.H2O.

### Claim 17 (depends on 2)

The method as claimed in claim 2, wherein, said step (4) comprises: (b1) regulating the pH value of said leachate to 11-12; precipitating Pb2+ to obtain Pb(OH)2 precipitate; (b2) filtrating the leachate containing the Pb(OH)2 precipitate as obtained in step (b1), separating solid which is containing Pb(OH)2 precipitate and liquid for removing impurities; (b3) taking solid dregs which is containing Pb(OH)2 precipitate as obtained in step (b2), adding HNO3 solution into the solid dregs which is containing Pb(OH)2 precipitate to regulate pH value to 0.5-1, reacting Pb(OH)2 with HNO3 to obtain a solution containing Pb(NO3)2; (b4) adding SO42− into the solution containing Pb(NO3)2 as obtained in step (b3) to precipitate Pb2+ to obtain PbSO4; (b5) adding strongly alkaline liquor into the solution containing the PbSO4 precipitate as obtained in step (b4) to regulate pH value to 8-10 to produce 3PbO.PbSO4.H2O, rinsing and drying the obtained 3PbO.PbSO4. H2O.

### Claim 18 (depends on 3)

The method as claimed in claim 3, wherein, said step (4) comprises: (b1) regulating the pH value of said leachate to 11-12; precipitating Pb2+ to obtain Pb(OH)2 precipitate; (b2) filtrating the leachate containing the Pb(OH)2 precipitate as obtained in step (b1), separating solid which is containing Pb(OH)2 precipitate and liquid for removing impurities; (b3) taking solid dregs which is containing Pb(OH)2 precipitate as obtained in step (b2), adding HNO3 solution into the solid dregs which is containing Pb(OH)2 precipitate to regulate pH value to 0.5-1, reacting Pb(OH)2 with HNO3 to obtain a solution containing Pb(NO3)2; (b4) adding SO42− into the solution containing Pb(NO3)2 as obtained in step (b3) to precipitate Pb2+ to obtain PbSO4; (b5) adding strongly alkaline liquor into the solution containing the PbSO4 precipitate as obtained in step (b4) to regulate pH value to 8-10 to produce 3PbO.PbSO4.H2O, rinsing and drying the obtained 3PbO.PbSO4. H2O.