Comprehensive Recovery Method Of Pyrolysis Polymetallic Product From Waste Integrated Circuit Board

Abstract

The invention relates to a method for multi-metal products recovery from pyrolytic waste integrated circuit boards. The method mainly comprises the steps of smelting and blending, atomization, acidolysis and filtration, noble metal recycling, copper extraction and back extraction, nickel extraction and back extraction. Compared with the prior art, the method has the advantages that smoke pollution and the smelting slag treatment in the process of preparing a black copper ingot through multi-metal collaborative smelting are reduced, and the problems of low anode efficiency of the black copper electrolysis process are solved. Meanwhile, the high-temperature high-oxygen atomized gas generated in the atomizing process provides a heat source and an oxygen source for subsequent acidolysis, so that the energy consumption is further reduced. The method has the advantages such as short process, remarkable energy conservation and emission reduction.

Claims

1. A method for multi-metal products recovery from pyrolytic waste integrated circuit boards, comprising the following steps: (1) melting and blending: adding multi-metals obtained by pyrolysis of waste integrated circuit boards into a smelting furnace, and adding a covering agent for smelting and blending under 1200-1350° C. with 0.5-1 hour to obtain an alloy solution, wherein the covering agent comprises one of carbon powder or coal powder, and an amount of covering agent added is 5-15% of the mass of multi-metal; (2) atomization: atomize the alloy solution obtained in step (1) to obtain atomized powder and atomized gas; (3) acidolysis and filtration: the atomized powder obtained in step (2) is immersed in an acidolysis solution for acidolysis, the acidolysis solution and acidolysis slag are obtained by filtration, and the acidolysis slag is recovered to obtain rare and precious metals; (4) copper extraction and back extraction: the acidolysis solution obtained in step (3) is subjected to copper extraction and back extraction to obtain copper sulfate and copper raffinate; (5) nickel extraction and back extraction: copper raffinate obtained in step (4) is subjected to nickel extraction and back extraction to obtain nickel sulfate and nickel raffinate, and the nickel raffinate returns to the acidolysis and filtration step as a supplementary solution of the acidolysis solution, wherein during the atomization step, an atomization water pressure is 10-15 MPa, an oxygen pressure is 1-1.2 MPa, and a nozzle aperture is 2˜3 mm, wherein during the acidolysis and filtration step, 150-200 Kg/m.sup.3 sulfuric acid is used as the acidolysis solution, the solution-solid ratio is 10 L:1 Kg-15 L:1 Kg, an atomization gas is stirred with a flow rate of 1-300 L/min per liter of the acidolysis solution, the acidolysis step uses 98% mass percent industrial concentrated sulfuric acid for acidity adjustment, a time of the acidolysis is 1-3 hours, and a pH at the end of the acidolysis reaction is 3-4.

Description

DESCRIPTION OF THE DRAWINGS

[0015] FIG. 1 shows the flow chart of multi-metal products obtained from pyrolytic waste integrated circuit boards

[0016] FIG. 2 shows a flow chart of a method for multi-metal products recovery from pyrolytic waste integrated circuit boards

PREFERRED EMBODIMENTS

[0017] The raw materials of multi-metal products used for comprehensive recovery in the embodiments are all obtained by using the method of CN108160665A.

Embodiment 1

[0018] Follow the steps below to recover:

[0019] (1) Melting and blending: adding multi-metals obtained by pyrolysis of waste integrated circuit boards into a smelting furnace, and adding a covering agent for smelting and blending under 1200° C. with 0.5 hour to obtain an alloy solution; adopts carbon powder or coal powder as the covering agent, and the amount of covering agent added is 5% of the mass of multi-metal.

[0020] (2) Atomization: atomize the alloy solution obtained in step (1) to obtain atomized powder and atomized gas; the atomization water pressure is 10 MPa, the oxygen pressure is 1 MPa, and the nozzle aperture is 2 mm.

[0021] (3) Acidolysis and filtration: the atomized powder obtained in step (2) is immersed in an acidolysis solution for acidolysis, the acidolysis solution and acidolysis slag are obtained by filtration, and the acidolysis slag is preciously recovered to obtain rare and precious metals; during the acidolysis and filtration process, 150 Kg/m.sup.3 sulfuric acid is used as acidolysis solution, the solution-solid ratio is 10 L:1 Kg, the atomization gas is stirred with a flow rate of 1 L/min per liter acidolysis solution, acidolysis process adopts 98% mass percent industrial concentrated sulfuric acid for acidity adjustment, the acidolysis time is 1 hour, the pH at the end of the reaction is 3.

[0022] (4) Copper extraction and back extraction: the acidolysis solution obtained in step (3) is subjected to copper extraction and back extraction to obtain copper sulfate and copper raffinate;

[0023] (5) nickel extraction and back extraction: copper raffinate obtained in step (4) is subjected to nickel extraction and back extraction to obtain nickel sulfate and nickel raffinate, and the nickel raffinate returns to the acidolysis and filtration process as a supplementary solution of acidolysis solution.

[0024] The copper recovery rate is 99.3%, the nickel recovery rate is 99.2%, and the precious metal recovery rate is 98.5%.

Embodiment 2

[0025] Follow the steps below to recover:

[0026] (1) Melting and blending: adding multi-metals obtained by pyrolysis of waste integrated circuit boards into a smelting furnace, and adding a covering agent for smelting and blending under 1350° C. with 1 hour to obtain an alloy solution; adopts carbon powder or coal powder as the covering agent, and the amount of covering agent added is 15% of the mass of multi-metal.

[0027] (2) Atomization: atomize the alloy solution obtained in step (1) to obtain atomized powder and atomized gas; the atomization water pressure is 15 MPa, the oxygen pressure is 1.2 MPa, and the nozzle aperture is 3 mm.

[0028] (3) Acidolysis and filtration: the atomized powder obtained in step (2) is immersed in an acidolysis solution for acidolysis, the acidolysis solution and acidolysis slag are obtained by filtration, and the acidolysis slag is preciously recovered to obtain rare and precious metals; during the acidolysis and filtration process, 150 Kg/m.sup.3 sulfuric acid is used as acidolysis solution, the solution-solid ratio is 15 L:1 Kg, the atomization gas is stirred with a flow rate of 300 L/min per liter acidolysis solution, acidolysis process adopts 98% mass percent industrial concentrated sulfuric acid for acidity adjustment, the acidolysis time is 3 hours, the pH at the end of the reaction is 4.

[0029] (4) Copper extraction and back extraction: the acidolysis solution obtained in step (3) is subjected to copper extraction and back extraction to obtain copper sulfate and copper raffinate;

[0030] (5) nickel extraction and back extraction: copper raffinate obtained in step (4) is subjected to nickel extraction and back extraction to obtain nickel sulfate and nickel raffinate, and the nickel raffinate returns to the acidolysis and filtration process as a supplementary solution of acidolysis solution. The copper recovery rate is 98.9%, the nickel recovery rate is 98.3%, and the precious metal recovery rate is 99.1%.

Embodiment 3

[0031] Follow the steps below to recover:

[0032] (1) Melting and blending: adding multi-metals obtained by pyrolysis of waste integrated circuit boards into a smelting furnace, and adding a covering agent for smelting and blending under 1200° C. with 1 hour to obtain an alloy solution; adopts carbon powder or coal powder as the covering agent, and the amount of covering agent added is 5% of the mass of multi-metal.

[0033] (2) Atomization: atomize the alloy solution obtained in step (1) to obtain atomized powder and atomized gas; the atomization water pressure is 10 MPa, the oxygen pressure is 1.2 MPa, and the nozzle aperture is 2 mm.

[0034] (3) Acidolysis and filtration: the atomized powder obtained in step (2) is immersed in an acidolysis solution for acidolysis, the acidolysis solution and acidolysis slag are obtained by filtration, and the acidolysis slag is preciously recovered to obtain rare and precious metals; during the acidolysis and filtration process, 200 Kg/m.sup.3 sulfuric acid is used as acidolysis solution, the solution-solid ratio is 10 L:1 Kg, the atomization gas is stirred with a flow rate of 10 L/min per liter acidolysis solution, acidolysis process adopts 98% mass percent industrial concentrated sulfuric acid for acidity adjustment, the acidolysis time is 3 hours, the pH at the end of the reaction is 3.

[0035] (4) Copper extraction and back extraction: the acidolysis solution obtained in step (3) is subjected to copper extraction and back extraction to obtain copper sulfate and copper raffinate;

[0036] (5) nickel extraction and back extraction: copper raffinate obtained in step (4) is subjected to nickel extraction and back extraction to obtain nickel sulfate and nickel raffinate, and the nickel raffinate returns to the acidolysis and filtration process as a supplementary solution of acidolysis solution. The copper recovery rate is 99.1%, the nickel recovery rate is 99.3%, and the precious metal recovery rate is 98.8%.

Embodiment 4

[0037] Follow the steps below to recover:

[0038] (1) Melting and blending: adding multi-metals obtained by pyrolysis of waste integrated circuit boards into a smelting furnace, and adding a covering agent for smelting and blending under 1350° C. with 0.5 hour to obtain an alloy solution; adopts carbon powder or coal powder as the covering agent, and the amount of covering agent added is 15% of the mass of multi-metal.

[0039] (2) Atomization: atomize the alloy solution obtained in step (1) to obtain atomized powder and atomized gas; the atomization water pressure is 15 MPa, the oxygen pressure is 1 MPa, and the nozzle aperture is 3 mm.

[0040] (3) Acidolysis and filtration: the atomized powder obtained in step (2) is immersed in an acidolysis solution for acidolysis, the acidolysis solution and acidolysis slag are obtained by filtration, and the acidolysis slag is preciously recovered to obtain rare and precious metals; during the acidolysis and filtration process, 150 Kg/m.sup.3 sulfuric acid is used as acidolysis solution, the solution-solid ratio is 15 L:1 Kg, the atomization gas is stirred with a flow rate of 20 L/min per liter acidolysis solution, acidolysis process adopts 98% mass percent industrial concentrated sulfuric acid for acidity adjustment, the acidolysis time is 1 hour, the pH at the end of the reaction is 4.

[0041] (4) Copper extraction and back extraction: the acidolysis solution obtained in step (3) is subjected to copper extraction and back extraction to obtain copper sulfate and copper raffinate;

[0042] (5) nickel extraction and back extraction: copper raffinate obtained in step (4) is subjected to nickel extraction and back extraction to obtain nickel sulfate and nickel raffinate, and the nickel raffinate returns to the acidolysis and filtration process as a supplementary solution of acidolysis solution. The copper recovery rate is 98.7%, the nickel recovery rate is 99.1%, and the precious metal recovery rate is 99.1%.

Embodiment 5

[0043] Follow the steps below to recover:

[0044] (1) Melting and blending: adding multi-metals obtained by pyrolysis of waste integrated circuit boards into a smelting furnace, and adding a covering agent for smelting and blending under 1250° C. with 0.5 hour to obtain an alloy solution; adopts carbon powder or coal powder as the covering agent, and the amount of covering agent added is 10% of the mass of multi-metal.

[0045] (2) Atomization: atomize the alloy solution obtained in step (1) to obtain atomized powder and atomized gas; the atomization water pressure is 12 MPa, the oxygen pressure is 1.1 MPa, and the nozzle aperture is 2.5 mm.

[0046] (3) Acidolysis and filtration: the atomized powder obtained in step (2) is immersed in an acidolysis solution for acidolysis, the acidolysis solution and acidolysis slag are obtained by filtration, and the acidolysis slag is preciously recovered to obtain rare and precious metals; during the acidolysis and filtration process, 180 Kg/m.sup.3 sulfuric acid is used as acidolysis solution, the solution-solid ratio is 12 L:1 Kg, the atomization gas is stirred with a flow rate of 100 L/min per liter acidolysis solution, acidolysis process adopts 98% mass percent industrial concentrated sulfuric acid for acidity adjustment, the acidolysis time is 2 hours, the pH at the end of the reaction is 3.5.

[0047] (4) Copper extraction and back extraction: the acidolysis solution obtained in step (3) is subjected to copper extraction and back extraction to obtain copper sulfate and copper raffinate;

[0048] (5) nickel extraction and back extraction: copper raffinate obtained in step (4) is subjected to nickel extraction and back extraction to obtain nickel sulfate and nickel raffinate, and the nickel raffinate returns to the acidolysis and filtration process as a supplementary solution of acidolysis solution. The copper recovery rate is 99.0%, the nickel recovery rate is 98.5%, and the precious metal recovery rate is 98.3%.

Embodiment 6

[0049] Follow the steps below to recover:

[0050] (1) Melting and blending: adding multi-metals obtained by pyrolysis of waste integrated circuit boards into a smelting furnace, and adding a covering agent for smelting and blending under 1300° C. with 1 hour to obtain an alloy solution; adopts carbon powder or coal powder as the covering agent, and the amount of covering agent added is 8% of the mass of multi-metal.

[0051] (2) Atomization: atomize the alloy solution obtained in step (1) to obtain atomized powder and atomized gas; the atomization water pressure is 13 MPa, the oxygen pressure is 1 MPa, and the nozzle aperture is 2.8 mm.

[0052] (3) Acidolysis and filtration: the atomized powder obtained in step (2) is immersed in an acidolysis solution for acidolysis, the acidolysis solution and acidolysis slag are obtained by filtration, and the acidolysis slag is preciously recovered to obtain rare and precious metals; during the acidolysis and filtration process, 160 Kg/m.sup.3 sulfuric acid is used as acidolysis solution, the solution-solid ratio is 11 L:1 Kg, the atomization gas is stirred with a flow rate of 200 L/min per liter acidolysis solution, acidolysis process adopts 98% mass percent industrial concentrated sulfuric acid for acidity adjustment, the acidolysis time is 1.5 hours, the pH at the end of the reaction is 3.6.

[0053] (4) Copper extraction and back extraction: the acidolysis solution obtained in step (3) is subjected to copper extraction and back extraction to obtain copper sulfate and copper raffinate;

[0054] (5) nickel extraction and back extraction: copper raffinate obtained in step (4) is subjected to nickel extraction and back extraction to obtain nickel sulfate and nickel raffinate, and the nickel raffinate returns to the acidolysis and filtration process as a supplementary solution of acidolysis solution. The copper recovery rate is 98.3%, the nickel recovery rate is 98.7%, and the precious metal recovery rate is 99.0%.