SEPARATION OF COPPER FROM A LEACHING SOLUTION OF PRINTED CIRCUIT BOARDS BY USING SOLVENT EXTRACTION WITH D2EHPA

Correa, Mónica Maria Jiménez; Silvas, Flávia Paulucci Cianga; Aliprandini, Paula; Moraes, Viviane Tavares de; Dreisinger, David; Espinosa, Denise Crocce Romano

doi:10.1590/0104-6632.20180353s20170144

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Environmental Engineering • Braz. J. Chem. Eng. 35 (3) • Jul-Sep 2018 • https://doi.org/10.1590/0104-6632.20180353s20170144 copy

SEPARATION OF COPPER FROM A LEACHING SOLUTION OF PRINTED CIRCUIT BOARDS BY USING SOLVENT EXTRACTION WITH D2EHPA

Authorship SCIMAGO INSTITUTIONS RANKINGS

Abstract

Global generation of waste electrical and electronic equipment (WEEE) is increasing quickly. Metals from WEEE can be recovered by using unit operations of chemical engineering. This paper describes a combined hydrometallurgical route (sulfuric oxidant leaching + solvent extraction) to recover copper from printed circuit boards (PCBs). A non-magnetic fraction from comminuted PCBs was used to perform leaching tests at 75ºC for 6 hours in an oxidizing media (sulfuric acid + hydrogen peroxide). In order to separate zinc, aluminum, and copper from the leaching liquor, solvent extraction tests were carried out using D2EHPA. Parameters that influence the process, such as pH, extractant concentration, and the aqueous/organic (A/O) ratio were investigated. Solvent extraction experiments were carried out in two stages: i) separation of zinc, aluminum, and residual iron, and ii) copper separation. The results showed that the leaching obtained around 60% aluminum, 94% copper, 76% zinc, 50% nickel and residual iron from the non-magnetic fraction of PCBs. With the solvent experiments, in the first stage, 100 wt.% zinc, iron and aluminum were extracted at pH 3.5, 2:1 A/O, 10 % (v/v) D2EHPA, while, in the second stage 100% of the copper was extracted at pH 3.5, 1:1 A/O, 20 % (v/v) D2EHPA.

Keywords:
Waste electrical and electronic equipment (WEEE); recycling; printed circuit boards (PCBs); leaching; solvent extraction

Sample	Extractant	Conditions	Reference
Sulfuric acid liquor from PCB waste	1^st step: D2EHPA (10%) diluted in Kerosene; 2^nd step: D2EHPA (20%) diluted in Kerosene.	1^st step: t = 10 min; T = 25 ºC; pH = 3.5; A/O = 2/1; 2^nd step: t = 10 min; T = 25 ºC; pH = 3.5; A/O = 1/1.	This paper
Sulfuric acid from battery waste	CYANEX 272 (0.72M) diluted in Exxol D-80	t = 20 min; T = 50 ºC; pH = 5.5; A/O = 1/1.	Dorella and Mansur (2007)Dorella, G., and Mansur, M. B., A study of the separation of cobalt from spent Li-ion battery residues. Journal of Power Sources, 170(1), 210-215 (2007). doi: http://dx.doi.org/10.1016/j.jpowsour.2007.04.025 http://dx.doi.org/10.1016/j.jpowsour.200...
Sulfuric acid liquor from battery waste	CYANEX 272 (0.6M) diluted in Kerosene	t = 20 min; pH = 3, 6.5.	Provazi et al. (2011)Provazi, K., Campos, B. A., Espinosa, D. C. R., and Tenório, J. A. S., Metal separation from mixed types of batteries using selective precipitation and liquid-liquid extraction techniques. Waste Management, 31(1), 59-64 (2011). doi: http://dx.doi.org/10.1016/j.wasman.2010.08.021 http://dx.doi.org/10.1016/j.wasman.2010....
Sulfuric acid liquor from battery waste	1^st step: Acorga M5640 (20%) diluted in Kerosene; 2^nd step: CYANEX 272 (0.04M) diluted in Kerosene.	1^st step: t = 5 min; T = 30 ºC; O/A = 1/1; 2^nd step: pH = 5; t = 10 min; T = 25ºC; O/A = 1.	Nayl et a. (2015)Nayl, A. A., Hamed, M. M., and Rizk, S. E., Selective extraction and separation of metal values from leach liquor of mixed spent Li-ion batteries. Journal of the Taiwan Institute of Chemical Engineers, 55, 119-125 (2015). doi: http://dx.doi.org/10.1016/j.jtice.2015.04.006 http://dx.doi.org/10.1016/j.jtice.2015.0...
Sulfuric acid liquor from PCB waste	1^st step: TEHA (70%) diluted in kerosene; 2^nd step: LIX 84IC (10%) diluted in kerosene; 3^rd step: LIX 84IC (1%) diluted in kerosene.	1^st step: t = 5 min; T = 30 ºC O/A = 2/1; 2^nd step: pH = 2.5; t = 5 min; O/A = 1/1; 3^rd step: t = 15 min; pH = 4.58; O/A = 2/1.	Kumari et al. (2016)Kumari, A., Jha, M. K., Lee, J.-C., and Singh, R. P., Clean process for recovery of metals and recycling of acid from the leach liquor of PCBs. Journal of Cleaner Production, 112(5), 4826-4834 (2016). doi: http://dx.doi.org/10.1016/j.jclepro.2015.08.018 http://dx.doi.org/10.1016/j.jclepro.2015...
Nitric acid liquor from PCB waste	LIX 984 (50%)	T = 50 ºC; pH = 1.5; A/O = 1/1.5.	Long Le et al. (2011)Long Le, H., Jeong, J., Lee, J.-C., Pandey, B. D., Yoo, J.-M., and Huyunh, T. H., Hydrometallurgical Process for Copper Recovery from Waste Printed Circuit Boards (PCBs). Mineral Processing and Extractive Metallurgy Review, 32(2), 90-104 (2011). doi: 10.1080/08827508.2010.530720 https://doi.org/10.1080/08827508.2010.53...

Metal	Al	Cu	Fe	Ni	Zn	Others
wt.%	2.0	33.9	0.2	0.2	3.8	7.6

Metal	Concentration (g/L)
Al	1.20
Cu	31.72
Fe	0.003
Ni	0.11
Zn	2.91

Ion	Extraction Reaction	Equations
Divalent metal (Adapted from Mansur et al., 2002Mansur, M. B., Slater, M. J., and Biscaia Jr, E. C., Equilibrium analysis of the reactive liquid-liquid test system ZnSO4/D2EHPA/n-heptane. Hydrometallurgy, 63(2), 117-126 (2002). doi: http://dx.doi.org/10.1016/S0304-386X(01)00211-0 http://dx.doi.org/10.1016/S0304-386X(01)... )	$M^{+ 2} + n {(RH)}_{2} \overset{Keq}{\leftrightarrow} {MH}_{2 (n - 1)} R_{2 n} + 2 H^{+}$	$K_{eq} = \frac{[{MH}_{2 (n - 1)} R_{2 n}] {[H^{+}]}^{2}}{[M^{+ 2}] {[{(RH)}_{2}]}^{n}}$	Equation 3
		$D = \frac{[{MH}_{2 (n - 1)} R_{2 n}]}{[M^{+ 2}]}$	Equation 4
Trivalent metal (Adapted from Mohapatra et al., 2007Mohapatra, D., Hong-In K., Nam C W., and Park K H., Liquid-liquid extraction of aluminium(III) from mixed sulphate solutions using sodium salts of Cyanex 272 and D2EHPA. Separation and Purification Technology, 56(3), 311-318 (2007). doi: http://dx.doi.org/10.1016/j.seppur.2007.02.017 http://dx.doi.org/10.1016/j.seppur.2007.... )	$M^{+ 3} + n {(RH)}_{2} \overset{Keq}{\leftrightarrow} {MH}_{2 n - 3} R_{2 n} + 3 H^{+}$	$Keq = \frac{[{MH}_{2 n - 3} R_{2 n}] {[H^{+}]}^{3}}{[M^{+ 3}] {[{(RH)}_{2}]}^{n}}$	Equation 5
		$D = \frac{[{MH}_{2 n - 3} R_{2 n}]}{[M^{+ 3}]}$	Equation 6

Concentration of D2EHPA (% v/v)	Metal	log Keq	n	R
10	Al	-1.21	0.5	0.97
	Fe	-1.91	2.07	0.96
	Zn	-2.82	2.09	0.94
15	Al	-1.32	0.6	0.98
	Fe	-1.78	2.27	0.95
	Zn	-2.91	2.35	0.93
20	Al	-1.54	0.88	0.98
	Cu	-2.36	3.05	0.96
	Fe	-2.71	2.66	0.92
	Zn	-2.24	0.66	0.96

	Separation factor of impurities over copper
	10% v/v D2EHPA, A/O 1:1			15% v/v D2EHPA, A/O 1:1			20% v/v D2EHPA, A/O 1:1			10% v/v D2EHPA, A/O 2:1
pH	Al	Fe	Zn	Al	Fe	Zn	Al	Fe	Zn	Al	Fe	Zn
0.5	6.6	23.8	2.3	6.3	46.5	4.3	5.4	57.5	14.1	4.5	46.3	0.0
1.0	6.7	70.5	14.6	6.4	239.2	17.2	6.3	104.5	28.4	2.1	15.6	2.8
1.5	15.1	250.8	57.7	9.1	281.9	48.4	12.6	525.3	142.9	2.4	23.0	4.2
2.0	20.2	1482.3	185.8	19.1	1922.1	291.1	18.8	1.1E+05	174.9	4.2	281.3	16.0
2.5	21.4	17501.0	566.4	20.1	1.5E+05	1221.0	20.1	5.4E+05	3.6E+05	8.1	2.2E+05	38.6
3.0	23.3	3.8E+05	1.1E+05	20.9	1.8E+06	7.33E+05	20.8	2.9E+05	1.9E+06	15.1	4.1E+05	58.9
3.5	23.5	3.3E+06	6.6E+05	21.8	1.8E+07	1.77E+06	21.6	8.3E+08	3.6E+06	25.6	9.5E+06	208.1

	Separation factor of copper over nickel
pH	10% v/v D2EHPA, A/O 1:1	15% v/v D2EHPA, A/O 1:1	20% v/v D2EHPA, A/O 1:1	10% v/v D2EHPA, A/O 2:1
0.5	1.0	1.0	0.7	0.29
1.0	1.0	1.3	0.5	1.37
1.5	1.0	1.3	0.7	1.56
2.0	1.6	1.4	3.2	1.63
2.5	2.4	1.4	2.9	1.76
3.0	3.1	1.8	5.6	1.93
3.5	4.9	3.7	14.3	1.81

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[1] * corresponding author. monicamariajimenezc@gmail.com; flavia.silvas@itv.org; tavares.vivi@gmail.com; david.dreisinger@ubc.ca; espinosa@usp.br