Method for comprehensive recovery of silver-containing lead slag

Patent metadata

Field	Value
Publication number	US-11345975-B2
Application number	US-201716073805-A
Country	US
Kind code	B2
Filing date	Nov 21, 2017
Priority date	Nov 5, 2016
Publication date	May 31, 2022
Grant date	May 31, 2022

Abstract

The main steps are as follows: purification, de-leading, recovery and filtration, dissolving lead, hot filtration, cooling filtration, washing and hot decomposition, silver is recycled as silver powder, lead was recovered in the form of red lead, yellow lead and chlorinated lead respectively. Compared to existing technologies, the invention adopts a wet process, the amount of waste gas and dust produced in the process of fire treatment is reduced; silver powder, red (yellow) lead and chloride lead were obtained, it can be sold as final product with high value-added features. The tail liquid produced by the process returns to the corresponding process respectively, and the tailless liquid is discharged. The pyrolysis flue gas returns to the lead removal process, flue gas treatment process is reduced, lead smoke pollution is avoided. This method has the characteristics of simple technics and pollution-free process.

First claim

What is claimed is:

1. A comprehensive recovery method of silver lead slag, comprising steps of:
(1) Purification: adding silver lead slag into ammonia-ammonium chloride solution, keeping warm and stirring the ammonia-ammonium chloride solution with the added silver lead slag, and after filtration, obtaining a residue removal and an impurity removal solution;
(2) De-leading: adding ammonium bicarbonate into the impurity removal solution obtained in step (1), and obtaining by filtration a de-lead residue and a de-lead solution;
(3) Recovery and filtration: adding into methanol the de-lead solution obtained in step (2) to initiate a silver reduction, wherein methanol:silver is 1:4˜1:6 in molar ratio, and wherein after filtration, a silver powder and a reduced liquid are obtained, wherein the reduced liquid after filtration is returned to step (1) for use in the Purification;
(4) Dissolving lead: adding the residue removal obtained in step (1) into a sodium chloride-hydrochloric acid solution, and adding a lead powder to the sodium chloride-hydrochloric acid solution to perform lead dissolution to, after that, obtain lead pulp;
(5) Hot filtration: hot filtrating the lead pulp obtained in step (4) to obtain lead-soluble slag, wherein the lead-soluble slag is recovered by tri-chlorination;
(6) Cooling filtration: cooling down to room temperature the lead-soluble slag obtained in step (5) to obtain lead chloride and a coolant, wherein the coolant is returned to step (4) for use in the lead dissolution;
(7) Washing: washing the de-lead residue obtained in step (2) by ammonium hydroxide until no silver is present in washing liquid to obtain lead carbonate, wherein the washing liquid is returned to step (1) for use in the Purification; and
(8) Hot decomposition: performing hot decomposition of the lead carbonate which is obtained in step (7), wherein a red lead product is obtained when a temperature of the hot decomposition is 450° C.˜500° C. and a time of the hot decomposition is 1˜2.5 h, and wherein a yellow lead product is obtained when temperature of the hot decomposition is 550° C.˜650° C. and a time of the hot decomposition is 1˜2.5 h, and wherein smoke generated during the hot decomposition is returned to step (2) for use in the De-leading.

2. A comprehensive recovery method of silver lead slag in claim 1 , wherein in step (1)
a mass percentage concentration of ammonia in the ammonia-ammonium chloride solution is 5%˜15%, ammonium chloride is 200˜400 g/L, a solid mass ratio between ammonia-ammonium chloride solution and silver-lead slag solution is 5:1˜30:1, reaction temperature is 30° C.˜60° C., and reaction time is 2-5 hours.

3. A comprehensive recovery method of silver lead slag in claim 1 , wherein the ammonium bicarbonate added in step (2) is a room temperature saturated solution, and wherein the addition of the ammonium bicarbonate into the obtained impurity removal solution is continued until the addition no longer causes precipitation.

4. A comprehensive recovery method of silver lead slag in claim 1 , wherein in step (4) a solubility of sodium chloride is 200 g/L˜300 g/L, and PH in solution is 0˜0.5.

5. A comprehensive recovery method of silver lead slag in claim 1 , wherein in step (4), a liquid-solid ratio between sodium chloride-hydrochloric acid solution and the residue removal is 20:1˜30:1, reaction temperature is 65° C.˜95° C., reaction time is 1-3 hours, 1 the reaction process always controls the pH of the reaction solution from 0˜1, and the amount of lead powder added is 0.5 g/L-3 g/L.

Assignees

• Univ Beijing Technology

Inventors

• Pan De'An
• Wu Yufeng
• Li Liquan

Classifications

• C22B13/045

  Recovery from waste materials · CPC title

• C22B7/008

  by an alkaline or ammoniacal leaching · CPC title

• C22B11/042 Primary

  Recovery of noble metals from waste materials · CPC title

• C22B7/006

  Wet processes · CPC title

• C22B7/04 Primary

  Working-up slag · CPC title