Method for whole component microwave fast digestion and precious metal extraction from ionic liquid of waste circuit board

Patent metadata

Field	Value
Publication number	US-11661639-B2
Application number	US-202217743385-A
Country	US
Kind code	B2
Filing date	May 12, 2022
Priority date	Jan 23, 2020
Publication date	May 30, 2023
Grant date	May 30, 2023

Abstract

The invention discloses Method for whole component microwave fast digestion and precious metal extraction from ionic liquid of waste circuit board, and belongs to the field of hydrometallurgy. Based on the theory that microwaves can directly penetrate through a leaching medium to directly heat a circuit board, microwave-assisted leaching can reinforce mass transfer and heat transfer in the traditional leaching process, the leaching time is greatly shortened, and the leaching efficiency is improved. Before leaching, a waste circuit board does not need to be smashed, and environmental protection is achieved while energy is saved. The temperature rising process and reaction time of the reaction can be controlled, the whole process is conducted under the airtight condition, heat loss in the leaching process is avoided, the valuable leaching rate is high, the selectivity is high, and efficient leaching of valuable metal can be achieved. Precious metal leachate is extracted through imidazolium ionic liquid, the selectivity of the imidazolium ionic liquid to gold is high, and the co-extraction phenomenon of gold, nickel, copper and other ions is avoided. The method for extracting the precious metal leachate through ionic liquid is a green and clean recycling method, and the overall recycling rate of gold, nickel and copper can reach 99% or above.

First claim

We claim:

1. A method for whole component microwave fast digestion and precious metal extraction from ionic liquid of waste circuit board, the method comprising the following steps:
(1) pretreatment of waste circuit boards: cut waste circuit boards into pieces to obtain the waste circuit boards to be leached;
(2) configuration of precious metal leaching solution for waste circuit boards: add pure water, thiourea, sulfuric acid, and sodium peroxide to a beaker, and stir until all are dissolved to obtain a leaching solution; a concentration of the leaching solution is: thiourea 1.5-4 mol/L, sulfuric acid 0.5-2 mol/L, sodium peroxide 1-3 mol/L;
(3) microwave-assisted leaching of waste circuit boards: put the pretreatment circuit boards in a digestion tank, and pour the leaching solution into the digestion tank at the same time, heating time of a microwave digestion instrument is set to 1-1.5 h, heating temperature of the microwave digestion instrument is set to 180-200° C. with 20 min insulation, cooling time of the microwave digestion instrument is set to 15-30 min, cool down to 60° C. to obtain precious metal leachate and resin-containing waste residue;
(4) conduct filtration and, after filtration, place the precious metal leachate in step (3) in an extraction tank, add imidazole ionic liquid [BMIM][NTF2] according to a volume ratio of the imidazole ionic liquid to the precious metal leachate of 1:1 to 1:5, and fully stir for 5 to 15 minutes to make a first oil phase and a first liquid phase thoroughly mixed to obtain a first mixed phase; the first mixed phase is centrifuged and separated to obtain an organic phase and a raffinate;
(5) add an oxalic acid solution to the organic phase obtained in step (4) according to a volume ratio of the organic phase to the oxalic acid solution of 1:1 to 1:10, a concentration of the oxalic acid solution is 1-3 mol/L, and back extraction is performed; stir for 5-15 minutes to make a second oil phase and a second liquid phase fully mixed to obtain a second mixed phase; after centrifuging and separating the second mixed phase, a back extraction raffinate and a pure ionic liquid are obtained;
(6) the back extraction raffinate in step (5) is filtered to obtain first tail liquid and crude gold powder;
(7) precious metal separation of raffinate: add sodium hydroxide to the raffinate obtained in step (4), adjust the pH to 6.7-7.0, conduct hydrolyzation, precipitation and filtration to obtain copper hydroxide precipitation and copper removal solution; add solids sodium hydroxide to the copper removal solution, adjust the pH to 9.5-10.0, conduct hydrolyzation, precipitation and filtration to obtain nickel hydroxide precipitate and second tail liquid.

2. A method for whole component microwave fast digestion and precious metal extraction from ionic liquid of waste circuit board according to claim 1 , wherein the pure ionic liquid obtained in step (5) is recycled to step (4) to repeat step (4).

3. A method for whole component microwave fast digestion and precious metal extraction from ionic liquid of waste circuit board according to claim 1 , wherein the first tail liquid obtained in step (6) undergoes evaporation and crystallization to recover sodium chloride.

4. A method for whole component microwave fast digestion and precious metal extraction from ionic liquid of waste circuit board according to claim 1 , wherein sulfuric acid, thiourea, and sodium peroxide are added to the second tail liquid obtained in step (7) to make the sulfuric acid, thiourea, and sodium peroxide in the second tail liquid meet the concentration standard of the leaching solution in step (2), repeat until the sulfate reaches saturation, then, the second tail liquid does not return to the leaching process.

Assignees

• Univ Beijing Technology

Inventors

• Wu Yufeng
• Yan Jiewen
• Li Bin

Classifications

• C22B15/0089

  by chemical methods · CPC title

• C22B7/007 Primary

  by acid leaching · CPC title

• C22B23/0461 Primary

  by chemical methods · CPC title

• C22B11/046

  from manufactured products, e.g. from printed circuit boards, from photographic films, paper or baths · CPC title

• C22B23/043

  Sulfurated acids or salts thereof · CPC title