lead recovery from metallurgical slag by flotation paulo f. a. braga, joão a. sampaio, carlos a. m....

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Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

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Page 1: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

Lead recovery from metallurgical slag by flotation

Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

Page 2: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

•Brazil does not have a primary production of refined metallic lead. The whole production is based upon the recycling of automotive, industrial and telecommunication batteries.

•In 2010 the battery recycling industry produced 115,000 t of metallic lead from 2nd production.

•Moura is the largest recycler/ manufacturer of batteries in Brazil (7.106 units/y).

INTRODUCTION

Page 3: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

•Operated at 90% efficiency (the ratio of the number of recycled batteries and the number of new batteries produced).

•With the increase in price of metallic commodities such as lead, several studies were carried out, aiming to:

minimize the loss of this metal in the industrial processes or;

for an additional recovery of the lead from metallic slags.

INTRODUCTION

Page 4: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

• Recycling process starts with the removal of metallic parts such as connectors and screws and subsequently with the reduction of the battery scrap and separation of the plastic casing from the lead grates and lead paste.

• Lead paste follows the process of separation, casting, refining and manufacturing of new batteries.

• Plastic is recovered and reused in the production of casing and cover for the new batteries.

• Acid solution is neutralized by lime or limestone.

INTRODUCTION

Page 5: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

•A typical automotive battery scrap contains:

INTRODUCTION 32% Pb

3% PbO

17% PbO2

36% PbSO4

• The main reactions of the metallurgical processes are:

2PbSO4 + Na2CO3 + Fe + 9C → 2Pb + FeS.Na2S + 9CO + CO2 (1)

PbO2 + C → CO + PbO (2)

2PbO + C → CO2 +2Pb (3)

PbSO4 + 2C → PbS + 2CO2 (4)

Page 6: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

• The present research work aimed to study the flotation process on pilot scale for the

recovery of lead from metallurgical slags rising from the recycling process of

automotive batteries.

• There were also several tests carried out in gravity concentration equipment with the

purpose of assessing this process route for the recovery of lead concentrate.

OBJECTIVE

Page 7: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

Chemical analysis of the slag sample:

Compounds Grade (weight %) Compounds Grade

(weight %) Compounds Grade (weight %)

Cr2O3 0.60 K2O 0.21 ZnO 0.80TiO2 0.07 P2O5 0.28 CaO 1.20

CuO 0.12 BaO 0.31 SiO2 2.58

MnO 0.14 Cl 0.66 Na2O 4.37Al2O3 0.16 SnO2 0.72 PbO 16.90Fe2O3 41.60 SO3 29.80

METHODOLOGY

X-ray diffraction (XRD):

metalic lead, magnetite (Fe3O4), hatrurite (Ca3SiO5), galena (PbS); jamesonite (Pb4FeSb6S14) and cotunnite (PbCl2).

Page 8: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

Nominal aperture size (µm) Weight (%) Pb Grade (%)

3,800 3.62 17.321,680 1.30 23.641,190 1.42 17.51840 1.31 17.47590 2.49 19.09420 1.60 12.56297 1.34 12.31210 2.64 17.40149 3.41 22.63105 3.80 20.1374 6.12 19.8053 3.00 20.0544 8.22 19.0637 7.78 15.34-37 51.91 12.61

Average 100.00 15.37

Screen size distribution and lead grade per size fraction.

METHODOLOGY

3,8001,680

1,190840

590420

297210

149105 74 53 44 37 -37

0

10

20

30

40

50

60Weight (%)

Pb grade (%)

screen size, mm

Page 9: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

Equipments:• jaw crushers• vibrating screen• conditioners• reagent feeder• flotation cells type Denver nº 7 Sub-A• Wilfley laboratory concentrating table• Humphreys spiral concentrator• crossflow 2x4 .

METHODOLOGY

Metering pumps

Flotation Cells

Flotation Circuit

potassium amyl xanthate ( PAX) – collector; methyl isobutyl carbinol (MIBC) - frother;sulphuric acid (H2SO4) - pH adjuster.

Reagents:

Page 10: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

Sample Preparation

METHODSSlag of lead (25 t)

Jaw crusher (1”)

Screening (2 mm) Jaw crusher (1/2”)

Screening (2 mm)

Hammer mill (5 mm)

Screening (2 mm)

Screening (-0,7 mm)

Homogenization pile

Discard (+ 0,7 mm)

Page 11: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

Flotation Procedure

Slag : 105 - 37 µm (size);

pH: 8 (sulphuric acid);

50 kg/h: slag (flow rate);

150 g/t: PAX (collector);

50 g/t: MIBC (frother).

Reagent system and operating conditions in laboratory scale for flotation tests were previously defined by Baltar (2005).

conditioner tank

Bomba

pump

rougher

Concentrate

feed tank

dosage pump

flotation cell

collector: potassium amyl xantate

frother: MIBC

Tailings

METHODS

Page 12: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

Weight recovery (%) Pb (%) Pb recovery (%)Rougher concentrate 38.4 48.8 79.8

Rougher tailings 61.6 7.7 20.2Feed 100 23.5

Flotation test

RESULTS

Page 13: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

Wilfley laboratory shaking table test

Products Bulk samplePb (%) Pb recovery (%)

Concentrate 55.9 37.2Middlings 15.6 8.3

Tails 11.8 54.4Feed 17.2 -

ProductsRougher concentrate

Pb (%) Pb recovery (%)Concentrate 72.3 56.5

Middlings 24.4 30.4Tails 19.1 13.1Feed 48.8 -

RESULTS

Page 14: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

Products Weight recovery (%) Pb (%) Pb recovery (%)Concentrate 14.4 46.0 34.7

Tailings 85.6 14.6 65.3Feed 100.0 19.1 100.0

Crossflow hydraulic classifier test (elutriation test)

Spiral concentrator testProducts Mass recovery (%) Pb (%) Pb recovery (%)

Concentrate 28.8 22.9 42.1Tailings 71.2 12.7 57.9

Feed 100 15.6 100.0

RESULTS

Page 15: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

• Main composition of lead metallurgical slag is: 16.9% PbO, 29.8% SO3 and 41.6% Fe2O3.

• The main mineralogical species are: magnetite (Fe3O4); hatrurite (Ca3SiO5); galena (PbS); jamesonite (Pb4FeSb6S14); cotunnite (PbCl2) and metallic lead.

• The fine fraction -37 m represented 51.9% of the bulk sample and contained 12.61% of lead.

FINAL REMARKS

Page 16: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

• The flotation at pilot scale produced lead concentrates at 48.8% Pb and a concentration ratio of 2 and 80% recovery. These results were obtained after fine fraction removal (-37 μm);

• Shaking table tests produced a concentrate at high grade, 55.9% Pb, and 37.2% recovery from the bulk sample;

• Reprocessing the rougher flotation concentrate in the shaking table produced a final concentrate at 72.3% Pb, concentration ratio of 1.5 and 56.5% recovery.

FINAL REMARKS

Page 17: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

ACKNOWLEDGMENTS

Page 18: Lead recovery from metallurgical slag by flotation Paulo F. A. Braga, João A. Sampaio, Carlos A. M. Baltar, Arnolfo M. Coelho, João A. F. Nunes

THANK YOUMUCHAS GRACIAS

[email protected]