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Amenability of a Plant Slimy Tails to a Nil Waste Process for Reuse

B P Ravi1*, K G Sanjaykumar1, G.Abhishek1, G.Shyala2 and P Sharathkumar2


1 TVJ Mineral Processing Projects P Ltd, Bangalore 560091
2 Mineral Processing Department, VSKU PG Centre, Nandihalli 583119,
1
*Corresponding Author Email: ravibelavadi@gmail.com,

B P Ravi
Adviser [Mineral Processing], Bangalore.
Ex Professor and Head, Mineral Processing Dept., VSK University, Nandihalli
Ex Head and ODO, RMPL, IBM, Ajmer
Ex Metallurgical Officer, BGML, KGF,
Ex Asst. Metallurgist, HGML [CU], Kalyadi.
CONTENTS
1. Introduction
2. Experimental
3. Results and Discussion
4. Bulk flotation of sulphides and arsenide
4.1 Characteristics of the sample
4.2 Effect of activator Copper sulphate dosage on bulk flotation of sulphides and arsenide
4.3 Effect of collector dosage on bulk flotation of sulphides and arsenide
4.4 Effect of % solids on bulk flotation of sulphides and arsenide
4.5 Final bulk flotation of sulphides and arsenide for bulk production
5 Micro pelletization / granulation studies on desulphurized tails
5.1 Characteristics of the desulphurized tails
5.2 Effect of pelletizer rpm
5.3 Effect of angle of inclination of pelletizer
5.4 Effect of binder OPC concentration
5.5 Effect of combination of binder concentration
6 Final test and Conclusions
Acknowledgements

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1. Introduction
Minerals are site specific, non renewable resources which have to be carefully utilized.
Unlike weed in agriculture, the minerals may be high revenue low availability, high demand
and , low revenue, high availability and low demand type only. Nil waste process evolution
revolves around characterisation and processing of minerals associated in rocks for almost
100% utilization with nil solid waste, minimal environmental damage and optimum
revenue leading to sustainable development. Yanful (2013) reviewed the role of binders for
Cemented Paste Tails [CPT] as mine backfill and recommended use of cement kiln dust,
fly ash in addition to cement for cemented paste backfill [CPB] Annon (2012). Alternatively,
a mix or standalone of granulated tails with binders like cement, granulated blast furnace
slag sand, granulated fly ash is being investigated to solve the vexed problem of mine back
fill, acid mine drainage and contamination of sub surface waters by heavy metals, As etc.
In view of the above CIP tails were received from HGML to study the concept of recovery
of S and As bearing minerals from tails followed by granulation of desulphurised tails for
subsequent use in mine back fill.
The general specifications are; The agglomerate shall have size range from 0.2 to
5mm with mean size of 3 mm. The agglomerates should have a minimum drop number of
10 and a compressive strength of 2kg/cm 2 and the S+As Content < 0.5% and Au ppm <0.2
ppm. Such cured agglomerates mixed with granulated slag sand and may be used as back
fill and should be pumpable during hydraulic back filling.
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2. Experimental
2.1 Material
The materials consist of CIP tails, Commercial grade (>90% assay / purity) potassium amyl
xanthate (KAX) Pine oil. CuSO 4, CaO, H2SO4, NH4OH, NaOH Ordinary port land cement [OPC]
and Anhydrous gypsum [CaSO 4] of -100 mesh [-0.15mm].
MPE 175 x 350 mm ball mill with 10 kg 25 mm steel balls, MPE SA Laboratory flotation
machine, Elico pH meter, were used. 600 mm dia Disc pelletizer of M/s MPE Co Ltd. Mumbai
was used for granulating.
2.2 Methods
The as received sample was subjected to was dried and subjected to standard
feed preparation and sampling methods followed by the following studies.
[1] Characterization studies; It consists of physico-chemical analysis,
size analysis, mineralogical studies, and diagnostic amenability tests.
[2] Bulk sulphide arsenide flotation; Bulk flotation to concentrate
S, As and Au values varying the dosages of activator CuSO 4, collector Potassium amyl
xanthate and % Solids.
[3] Micro pelletization studies; The standard granulation / pelletization method as enumerated by
the manufacturer and hand books was followed. The micro pellet / granulated product was
subjected standard tests for determining % Moisture after drying, strengths, drop tests and size
analysis after curing the pellets forXIV
72NSMTA-2018
hours. During the Pelletization experiments, the choice of
MCP HCL 2122018
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binder, binder dosage, effect of machine parameters like rpm and inclination were studied. 4
3 Results and Discussion
The results pertaining to experimental results are discussed as under.
1 Characteristics of the sample ; It consists of physico-chemical analysis, size
analysis, mineralogical studies, and diagnostic amenability tests
2. Bulk sulphide Arsenide flotation; Bulk flotation to concentrate S, As and Au values
varying the dosages of activator copper sulphate, collector Potassium amyl xanthate
and % Solids
3. Micro pelletization studies; During the Pelletization experiments, the choice of binder,
binder dosage, effect of machine parameters like rpm and inclination were studied. The
micro pellet / granulated product was subjected standard tests for determining %
Moisture after drying, strengths, drop tests and size analysis after curing the pellets for
72 hours.
4. Final analysis of concept - results and conclusions

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4 Bulk flotation of sulphides and arsenide
4.1 Characteristics of the sample
The physico-chemical analysis indicated that the as received sample was dark grey coloured
fine powder of ~3.0 specific gravity.
The sample analysed 0.35 ppm Au, 28.6 ppm Ag, 0.74% As, 1.27% S, 76.51% SiO2, 7.24%
Fe, 4.85% Al2O3, 2.83% CaO, 1.74% TiO2, 1.55% Alkalis
The sample contains mainly quartz (50 – 55%) occurs as aggregates with minor to
subordinate amounts of arsenopyrite, pyrite, iron oxides-carbonates. Sink and float tests
yielded a heavy fraction rich in Au, As and S.
The size analysis indicated that D100 ; 0.106 mm, D80; 0.060mm, D50; 0.050mm and
D25;0.025mm
Fig 1 Size Analysis for Feed
120

100 100

80 85
C wt% for U/s

80
60
46
40
40
33.3
20 25
0
10 100
Size in Micron Size vs C Wt% for
U/s

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4.3 Effect of activator copper sulphate dosage;
The activator copper sulphate dosage was varied from 0, 1 and 2 kg/t at MOG D80
0.06mm, %S, 0.1 kg/t KAX collector and 20 % Solids. The results are shown in Fig 2. The
results indicate that optimum results with selectivity and 85% S recovery was obtained at
1 Kg/t CuSO4 similar to findings of Ravi et.al. (2003 and 2013).
Fig.2; Effect of CuSO4dosage
86

84

82

80
%S Distn.

78

76

74

72
0 0.5 1 1.5 2 2.5
CuSO4Kg/t

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4.2 Effect of activator KAX Collector dosage;
The collector KAX dosage was varied from 0.10, 0.18 and 0.24 kg/t at MOG D80
0.06mm, 1 kg/t CuSO4 activator and 28 % Solids. The results are shown in Fig 3. The
results indicate that optimum results with selectivity and 85% S recovery was obtained
0.18 kg/t KAX, similar to findings of Ravi et.al. (2003 and 2013).

Fig. 3.Effect of KAX dosage


90

80

70

60

50
%S Distn.

40

30

20

10

0
0.08 0.1 0.12 0.14 0.16 0.18 0.2 0.22 0.24 0.26
KAX kg/t

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4.3 Effect of % Solids
The % S was varied from 20, 28 and 36 at MOG D80 0.06mm, 1 kg/t CuSO4 activator and
0.1 kg/t KAX collector . The test results are shown in Fig 4. Increase in %S increases %S
recovery. The optimum %S was found at 28%S as 85.2 S was recovered.

Fig. 4Effect of % Solids

85.4
85.2
85
84.8
84.6
%S Distn

84.4
84.2
84
83.8
83.6
83.4
18 20 22 24 26 28 30 32 34 36 38
% Solids by wt.

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4.4 Final bulk flotation test for production of products
The material for granulations studies were prepared by bulk flotation tests at natural pH8,
0.25kg/t ammonium hydroxide, 1kg/t CuSO4, 0.18kg/t KAX,0.16 kg/t Pine oil and 28% S. The
bulk float at 16% yield, assayed 1.4ppm Au, 6.68%S and 4.08% As, which may reused in the
plant for recovery of gold after breaking open the aresenopyrite lattice by chemical processing,
while the flotation tails which is the feed for granulation studies assayed 0.15%As, 0.25%S,
0.15ppm Au. The results are given in Table 1.
Table 1; Final bulk flotation desulphurization test under optimum conditions
pH 8 natural, D8060 microns, 28%S, 0.25kg/t Ammonium hydroxide and1kg/t CuSO 4 with conditioning time of1’ and
15’ each, 0.18kg/t KAX in 2 stages with conditioning time of 1’,0.16 kg/t Pine oil in 2 stages with conditioning time of
1’ each. The bulk flotation time was 2’ and 4’ respectively for 1 and 2 stage.

Product Wt% %S %As Ppm Au %Distn S %Distn As % Distn Au


Bulk float 16.0 6.68 4.08 1.40 80.4 83.8 64.0
Bulk tails 84.0 0.25 0.15 0.15 19.6 16.2 36.0
Head Cal 100.0 1.07 0.79 0.35 100.0 100.0 100.0
Feed Actual 100.0 1.27 0.74 0.35 100.0 100.0 100.0

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5 Micro pelletization / granulation studies on desulphurized tails
Pelletization experiments were conducted varying angle of inclination and rpm for the disc
pelletizer. The disc pelletizer was chosen as the product size of granules can controlled through
observation as compared with drum pelletizer. In the material parameters the experiments were
conducted varying the dosage of OPC and to choose between Portland cement [OPC], mix of
OPC – anhydrous gypsum – fly ash at optimum binder dosage. Since, the aim of the experiment
was to obtain granules <5mm, the feed rate and residence time was controlled. Residence time
data indicated that pellet diameter increases with residence time. Hence to avert production of
pellets larger than 5 mm the quantum of material fed to pelletizer was reduced to ¼ that is
normally practiced for ore Pelletization process, whose aim is to produce pellets of -30+6 mm
pellets. The micro pelletization process was carried out in batches to avert oversize pellet
production due to assimilation – snow ball growth with fresh material. The atomized water
addition was place at the top of free falling cascading balls to avert over size pellet growth The
chemical analysis of desulpharized tails is given in Table 2
Table 2; Chemical assay of pellet feed

%S %As Ppm Au %Distn S %Distn As % Distn Au


Bulk tails
0.25 0.15 0.15 19.6 16.2 36.0

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5.1 Effect of pelletizer rpm
The pelletizer rpm was varied from 25 to 45 keeping other parameters like angle of inclination [45
degrees], OPC binder dose [5%], moisture [11%] as constant. The results are given in Table 3 and Fig 5
The results indicate that the size of agglomerate is large at very low rpm and the agglomerate is non-
spherical and weak. Further increase in rpm reduces the size to minimum and subsequently increases
the size at high rpm which is not acceptable for hydraulic mine back fill. Optimum results were obtained
at rpm of 25. This may be due to extreme low or high angles the charge may not be lifted leading to
formation of coarse and fine agglomerates. respectively
Table 3 Effect of pelletizer rpm
%-6mm of Wt% CS
Particulars RPM Yield +0.2mm Drop No
yield Sand Kg/Cm2
Variable rpm, 15rpm 50 42 21.0 1 0.8
45 degrees, 25rpm 90 50 45.0 17 3.0
moisture 11%, 35rpm 97 34 33.0 17 3.4
binder OPC 5% 45rpm 98 40 39.2 13 2.7

50
Fig5 Effect Of Rpm 4
45 45 3.4
3.5
40 37.5

C -STRENGTH
3 3
35
30 2.7 2.5
25 33 2
% SAND

20 21 1.5
15
1
10 0.5
5 0.5
0 0
10 15 20 25 30 35 40 45 RPM
50VS %SAND
RPM RPM VS C-STRENGTH"
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5.2 Effect of binder OPC concentration
Review of literature indicated that OPC consumption for mine back fill varied from 4 to8% in CPB.
Hence, OPC binder dose was varied from 5 to 10% with 2.5% step. The results are shown in Table 4 &
Fig 6 The results indicate that the crushing strength and drop number increased with binder dosage.
Hence, the binder dosage was kept at maximum of 10%.
Table 4 ; Effect of Binder OPC concentration
Yield %-6m Wt% Drop CS
Particulars %OPC
+0.2mm of yield Sand No Kg/Cm2
Variable OPC% 5.0 % 90 50 45.0 17 3.0
45 degrees, 7.5% 98 50 49.0 17 3.0
moisture 11%, rpm 25 10.0% 99 45 44.6 25 3.5

Fig6 Effect of %OPC Concentration


50 49 3.6
49 3.5 3.5
48 3.4

C -STRENGTH
47 3.3
% SAND

3.2
46
45 3.1
45 3 3
44.6
44 3
2.9
43 2.8
42 2.7
4 5 6 7 8 9 10 11
%OPC %OPC VS %SAND
%OPC VS C-STRENGTH
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5.3 Effect of angle of inclination
The angle of inclination of the disc pelletizer was varied from 30 to 60 degrees keeping rpm, moisture, OPC
% constant. The results are given in Table 5 & Fig 7. Balling mainly depends on inclination of disc which
primarily affects the angle of repose. The extent to which charge is lifted along the kidney shaped trajectory
and size of the zone occupied by charge are functions of the angle of repose of the material being pelletized
which itself is dependent on angle of inclination of disc. At lower inclination the angle of repose will be small.
This yields coarser pellets. At too steep an angle, not all the charge would no longer be lifted by friction
leading formation of small pellets which is needed. The tilt angle for high production rates with a minimum
diameter of 6 mm varies between 45-60 o depending on the frictional coefficient of ore and the lifting
coefficient. The rim height is also determined by the tilt angle. Filling volume is dependent on both factors.
With increasing in inclination the % desired size increased. Increase in angle of inclination and rpm favors
formation of micro pellets.
Table 5 ; Effect of angle of inclination
Fig 7 Effect of Angle
Wt 100 89.1 3.6
% % CS 90 3.5 3.5
Ang % Dr 80 3.5
Particulars +0.2 -6 Kg/ 3.4
le Sa No 70 3.3
mm mm Cm2

C -STRENGTH
60
nd 3.2

% SAND
50
35 44.6 3.1
40
3 3
Variable angle 30o 97 34 33.0 17 3.0 30
20 2.9
moisture 45o 99 45 44.6 25 3.5 10 2.8
11%,rpm 25 0 2.7

binder OPC 10% 60o 99 90 89.1 25 3.5 25 30 35 40 45 50 55 60 65


ANGLE Angle vs %Sand
Angle vs C-Strength
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5.4 Effect of combination of Binders ratio
With regard to the aforementioned statistics, PC appears to be the most expensive component of
operations and hence becomes the primary setback in its use as a sole binder. Atari and E.K. Yanful
(2013) reviewed the role of binders for CPT as mine backfill and recommended use of cement kiln dust,
fly ash in addition to cement for cemented paste backfill [CPB]. Peyronnard and Benzaazoua
(2011)have tested waste gypsum as hydration activator for cemented mine backfill applications and
found that 4.5 wt% binder (42%PCe 40%waste glass 18%anhydrite) mixed with mining waste can
produce a monolith with UCS of 0.6 MPa after 14 days of curing. In view of the above the ratio of OPC
with anhydrous gypsum was varied from 0, 50 and 80% keeping total binder consumption at maximum
level of 10%. The results are given in Table 6.& Fig 8 The results indicate the dilution of cement binder
with anhydrous gypsum reduced the drop number and quality was affected significantly when the OPC -
anhydrous gypsum ratio was less than 1. The overall OPC consumption was 5%.
Table 6; Effect of Binder and additive ratio
Fig 8 Effect of Ratio of Binder & Additive
Yield %-
Dr CS 90 89.54
Ratio % 6mm Wt% 89
89.3 3.5
Particulars op kg/ 3.5
% +0.2 of Sand

C -STRENGTH
88 3 3
No Cm2 2.5
mm yield 87

% SAND
85.5 2
Variable binder % 100:0 99 90 89.1 25 3.5 86
1.5 1.5
85
OPC : CaSO4 50:50 90 95 85.5 17 3.0 1
84 0.5
Angle 60o, moisture 11%, 20:80 94 95 89.3 7 1.5 83 0
rpm 25, Binder 10% 10 20 30 40 50 60 70 80 90 100 110

Ratio of Binder & Aditive


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6 A Amenability to conceptual nil waste test of bulk S’ flotation – granulation
Table 7 ; Final test results involving Bulk S’,As’& Au flotation and granulation of dried Bulk float rejects

Particulars of bulk flotation for Product Wt% %S % Ppm %Distn %Distn % Distn
desulpharization As Au S As Au
pH 8 natural, D8060 microns, 28%S, Bulk float for reuse 16.0 6.68 4.08 1.40 80.4 83.8 64.0
0.25kg/t Ammonium hydroxide and1kg/t Pellet feed 84.0 0.25 0.15 0.15 19.6 16.2 36.0
CuSO4 with conditioning time of1’ and Head Cal 100 1.07 0.79 0.35 100.0 100.0 100.0
15’ each, 0.18kg/t KAX in 2 stages with The size analysis indicated that D100 ; 0.106 mm, D80; 0.060mm, D50; 0.050mm and
conditioning time of 1’,0.16 kg/t Pine oil D25;0.025mm. The sample contains mainly quartz (50 – 55%) occurs as aggregates with
in 2 stages with conditioning time of 1’ minor to subordinate amounts of arsenopyrite, pyrite, iron oxides-carbonates
each. The bulk flotation time was 2’ and
4’ respectively for 1 and 2 stage
Particulars of final micro pelletization test on Yield %-6mm Wt% Drop C Strength
deslulpharized dried flotation product +0.2mm of yield Sand No Kg/Cm2
1;1 binder OPC : CaSO4,Angle 60o,
90 95 89.1 25 3.5
moisture 11%, rpm 30, Binder 10%
6B Conclusions

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Acknowledgements

The authors are thankful to:


1. M/s HGML for providing the sample and assays.
2. M/s VSKU Ballari for permission to undertake the work and present the findings
3. M/s TVJ MMPL, Bangalore for encouragement
4. The conveners of XIV NSMTA-2018, Malanjkhand Copper Unit, HCL for providing the
opportunity to share the concept.
5. The August Audience for their patient listening.
 

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