Method for recycling lead oxide-containing waste material

Patent metadata

Field	Value
Publication number	US-9828653-B2
Application number	US-201414906366-A
Country	US
Kind code	B2
Filing date	May 27, 2014
Priority date	Feb 21, 2014
Publication date	Nov 28, 2017
Grant date	Nov 28, 2017

Abstract

Provided is a method for recycling a lead oxide-containing waste material, comprising: (1) contacting the lead oxide-containing waste material with a desulphurizer under desulphurization reaction conditions, and performing a solid-liquid separation on the mixture after contacting to obtain a filtrate and a filtration residue; (2) performing a conversion reaction on the above-mentioned filtration residue at a temperature of 350-750° C. so as to convert the lead-containing components in the filtration residue into lead oxide; (3) contacting the product obtained from step (2) with an alkaline solution so as to dissolve the PbO therein, and then performing a solid-liquid separation to obtain a PbO-alkaline solution; and (4) crystallizing the PbO-alkaline solution from step (3) to obtain PbO crystals and an alkaline filtrate. The method can reduce the energy consumption.

First claim

The invention claimed is:

1. A method for recovering lead oxide from lead oxide-containing wastes, comprising the following steps:
(1) controlling a lead oxide-containing waste to contact with a desulfurizing agent to desulfurize through wet ball milling, and carrying out solid-liquid separation for a mixture obtained from the contact, to obtain filtrate and filter residue;
(2) controlling the filter residue to have a conversion reaction at 350-750° C. temperature, to convert lead-containing components in the filter residue into PbO;
(3) controlling a product obtained in step (2) to contact with alkaline solution A, to dissolve the PbO in the product, and then carrying out solid-liquid separation to obtain PbO-alkaline solution;
(4) controlling the PbO-alkaline solution obtained in step (3) to crystallize, to obtain PbO crystals and alkaline filtrate;
wherein the contact in step (3) is carried out in presence of a dissolution promoter, which is selected from the group consisting of ethylene diamine, sodium acetate, sodium tartrate, EDTA, glycerol, butanediol, pentanol, sorbitol, xylitol, histidine, arginine, and glycocoll; and the dosage of the dissolution promoter is 0.2-20 wt % of the alkaline solution A.

2. The method according to claim 1 , wherein the conversion reaction in step (2) is carried out in the presence of a promoter, which is added in step (1) and/or step (2).

3. The method according to claim 2 , wherein the promoter is selected from the group consisting of lead powder, barium powder, aluminum powder, sodium powder, lithium powder, potassium powder, magnesium powder, naphthalene, camphor, urea, nickel powder, tin powder, stibium powder, zinc powder, carbon powder, active carbon containing 0.5-95 wt % PbO, and a mixture of above-mentioned substances with β-lead peroxide mixed at any mix ratio.

4. The method according to claim 3 , wherein the dosage of the promoter is 0.05-30 wt % of the filter residue obtained in step (1).

5. The method according to claim 1 , further comprising: cooling a product obtained in step (2) to 100-300° C. during a period of 0.5-30 min before performing step (3).

6. The method according to claim 5 , wherein the cooling is carried out in a manner of liquid mist cooling.

7. The method according to claim 1 , wherein the alkaline solution A used in step (3) is either or both of sodium hydroxide solution and potassium hydroxide solution, the concentration of the alkaline solution A is 12-60 wt %, and the dosage of the alkaline solution A ensures that the concentration of a product obtained in step (2) used in the contact in step (3) is 30-120 g/L, the contact temperature in step (3) is 45-135° C., and the contact time in step (3) is 0.5-100 min.

8. The method according to claim 1 , wherein in step (4), a crystallization process is carried out in stages, including: a first stage of crystallization at 60-135° C. and a second stage of crystallization at −5° C. to 60° C., wherein, the duration of the first stage of crystallization is 1-60 min, the duration of the second stage of crystallization is 3-600 min.

9. The method according to claim 1 , further comprising:
(5) treating the PbO crystals obtained in step (4) by ball milling for crystal transformation, to obtain PbO in α-structure.

10. The method according to claim 9 , wherein the conditions of ball milling for crystal transformation include: based on 1,000 g lead oxide, the mass of the balls is 5-500 g, the number of the balls is 5-100, the ball milling time is 0.1-200 min, and the temperature is 5-550° C.

11. The method according to claim 1 , further comprising: substituting a product obtained in step (2) with the PbO crystal obtained in step (4) and repeating step (3) and step (4) cyclically.

12. The method according to claim 1 , wherein the contact between the lead oxide-containing waste and the desulfurizing agent is implemented through a wet ball milling and mixing process.

13. The method according to claim 1 , wherein in step (1), the desulfurizing agent is NaOH and/or KOH solution, and the concentration of the NaOH and/or KOH solution is 4-23 wt %.

14. The method according to claim 5 , wherein cooling a product obtained in step (2) to 100-150° C. during a period of 1-10 min, before performing step (3).

15. The method according to claim 6 , wherein a coolant of the cooling is one or more of water, methanol, ethanol, and acetone.

16. The method according to claim 6 , wherein the size of mist droplets is 2-50 μm.

17. The method according to claim 5 , further comprising: substituting a product obtained in step (2) with the PbO crystal obtained in step (4) and repeating step (3) and step (4) cyclically.

18. The method according to claim 9 , further comprising: substituting a product obtained in step (2) with the PbO crystal obtained in step (4) and repeating step (3) and step (4) cyclically.

Assignees

• Chilwee Power Co Ltd
• Univ Beijing Chem Tech
• Chilwee Power Co Ltd & Beijing Univ Of Chemical Technology

Inventors

• Pan Junqing
• Liu Xiaowei
• Sun Yanzhi
• Ma Yongquan
• Niu Yinjian
• Chen Tixian
• Zhang Xuan
• Cai Xiaoxiang
• Song Shuang
• Zhou Mingming
• Zhou Longrui
• Cao Guoqing
• Yang Xinxin
• Wang Jianglin
• Wu Xin

Classifications

• C22B7/006

  Wet processes · CPC title

• Y02P10/234

  Cross-Sectional Technologies · mapped topic

• C22B13/045 Primary

  Recovery from waste materials · CPC title

• Y02P10/20

  Recycling · CPC title

• C01D5/00

  Sulfates or sulfites of sodium, potassium or alkali metals in general {(sulfites in general C01B17/62)} · CPC title