Zero waste process evolution for a low grade limestone

Chitriki Rudrappa1, Belavadi Ravi*2, P.Sharathkumar3, Siregere Gopalkrishna4, Mahesh Patil 5 ,

Prakash Naganoor 6and M.V.Rudramuniyappa7
1to 7
Department of Mineral Processing, VSK University PG Centre, Nandihalli, Karbataka State, India 583119

Abstract
A low grade Limestone from ACC mines, Madukkarai, Coimbatore district, Tamilnadu
assaying 45% CaO, 80% TC, 18% SiO2, 1.3% MgO, 1.30% Fe2O3, 2.50% Al2O3, 0.33% alkalis and
36.00% LOI yielded a cement grade composite concentrate ( non-float and slimes) assaying 9.51%
AI, 90% Total carbonates at wt% yield of 88 by a process comprising of grinding to MOG D80 400
microns, desliming/ screening over 400 mesh, rougher conditioning with 0.4kg/t SOKEM565C for
2minutes at 50%S, rougher flotation for 4 minutes at pH 8 and 28%S. The non-float (-16+400 mesh)
sand fraction assaying 80.30% AI, 18% total carbonates may be used as eco sand. The evolved nil
waste process is stable, selective

Key words; Flotation,cement grade limestone, ecosand limestone plant tail.

1 INTRODUCTION

Limestone is a sedimentary origin calcite associated with quartz, mica, clay, iron oxides and
feldspar in varying amounts. It is used mainly in cement industry followed by metallurgical industries.
Though India is bestowed with large lime stone deposits, the quality of limestone required by cement
manufacturing industries could not be met due to high amounts of silica and iron- aluminum content.
The specification for limestone for cement industry is CaO >42%, MgO <4%, SiO2 <15%. Many
workers Rao et. al. (2009), Suresh et. al. (2002). Rachappa et. al. (2013) have carried out flotation
studies by floating calcite and separated from siliceous gangue employing anionic fatty acid salt
collectors depressing gangue using sodium silicate as depressant. Straight flotation route was
practiced for quite a long time. However, inverse flotation of limestone by floating the siliceous
gangue is practiced ( Rao et.al. (2009) and Rachapp et.al. (2015) owing its ease to float less quantum
of gangue float, availability of custom made cheap surfactants having an edge in cost over direct
flotation involving large frothy mass handling with a number of cleaner steps.

2 MATERIAL AND METHODS;

Low grade Limestone samples of 200 kgs was collected from lime stone mining area of Madukkari,
Tamilnadu. The flotation regents were collected from m/s Somu organics ltd., Bangalore. The as
received sample was stage crushed to -10 mesh using primary lab jaw crusher[150 x225mm], lab roll
crusher [200mm x 150mm] 300 mmx600mm 10 mesh screen. The crushed sample was subjected to
standard feed preparation by adopting sampling procedures. The sample was ground at 67%s in
175mm x 350 mm rod mill 5 kg rod charge -10 nos of 40mm, 25mm and 20mm dia varying grinding

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time. The ground pulp was subjected to froth flotation using D12 Denver type lab sub aeration
flotation machine. The feed and products after dewatering followed by drying were weighed, sampled
and subjected to characterization studies.

3 RESULTS AND DISCUSSION

Based on characterization studies,. Flotation tests were carried out varying mog, choice and
dosage of collector, , effect of conditioning time, % solids and effect of reclaimed water on flotation
under optimum conditions. The results are discussed below

3.1 Characterization studies

The whitish gray coloured limestone sample had bulk density of 1.81t/m 3 and 350 angle of
repose. The work index of the sample was found to be 11.5 KWh/short ton. The sample contained
fine grained calcite intimately associated with minor amounts of fine grained aggregates of quartz,
iron oxides, clay and trace amounts of feldspar. The sample was siliceous low grade granular
limestone with fair degree of liberation at -65 mesh size. The sample analyzed 41% CaO, 18%SiO 2,
1.23% MgO, 1.30% Fe2O3, 1.50% Al2O3, 0.33 alkalis 80% total carbonates and 36% LOI.
Representative samples were ground in rod mill for varying time from 5 to 15 minutes and samples
were subjected to size analysis. The data is given in Table 1. The grindability data indicated that the
sample was medium soft in nature
Table: 1 Size analysis of rod mill grindability
Wt % retained
Mesh
0’ 5’ 10’ 15’
-16+22 10.0 1.6 0 0
-22+30 12.0 5.6 0 0
-30+52 38.0 27.2 2.4 3.2
-52+72 15.0 19.2 15.2 1.6
-72+120 8.0 20.0 28.8 28.8
-120+200 5.0 8.0 15.2 23.2
-200+277 4.0 5.6 8.8 13.6
-277+400 6.0 1.6 3.2 3.2
-400 2.0 11.2 26.4 26.4
100.0 100.0 100.0
D 80 microns 730 400 200 150

3.2 Effect of mesh of grind [MOG]

Inverse flotation tests were conducted varying mesh of grinding time 5’/10’/15’ with
respective D80 400/200/150 microns respectively at natural pH of 8, with 1 Kg/t anionic collector
SOKEM 565 C. The results have been tabulated Table -2. The results indicated that the grade of silica
content reduced to a minimum at mesh of grind of 400 microns and hence was chosen. The fall in
grade in coarse grind of 150 microns was due to lack of liberation of silica values while the fall in
grade in very fine grind of 200 microns was attributed to interference of slimes. Rao et.al. (2009),
Vijayakumar et.al. (2009) and Rachappa Kadli et.al. (2015) obtained optimum MOG at grinds finer

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than 150 microns. Incidentally the present direct soap flotation process at Madukkarai plant employs a
finer grind of 105 microns. From the experimental studies, it has been concluded that with mesh of
grind of 5’ D80 at 400 microns results obtained are encouraging
Table-2: Effect of MOG on inverse flotation
Conditions; Mesh of grind 5’/10’/15’has D80 400/200/150microns Flotation pH 8, % S 19,
Stage Cell Rpm Reagent Dosage kg/t CT min FT min
RF 250 1200 SOKEM 565C 1 2 4
Results:
Acid insoluble %
Mesh of grind Product Wt%
Assay Distn
5’ Float reject 40.8 41.60 98.2
D80 400 microns Non float 59.2 0.60 1.8
Head Cal 100.0 18.40 100.0
10’ Float reject 44.8 33.43 98.0
D80 200microns Non float 55.2 0.68 2.0
Head Cal 100.0 18.83 100.0
15’ Float reject 59.2 31.10 97.8
D80 150microns Non float 40.8 1.00 2.2
Head cal 100.0 18.79 100.0

3.3 Choice of collector

Inverse flotation tests were conducted at D 80 size of 400 microns varying collectors like
SOKEM 565C, SOKEM 524C, SOKEM 522C and SOKEM 503C and maintaining dosage of 1 kg/t.
The results are shown in Table 3. The results indicated that SOKEM 565C was more selective in
flotation of siliceous gangue similar to results obtained by Rao et. al (2009), Vijayakumar et.al.
(2009) and Rachappa Kadli et.al (2015) flotation of low grade limestone to get cement grade
Table-3: Choice of collector on flotation
Conditions; Mesh of grind 5’ D80 400microns, Flotation pH 8, and % S 19
Stage Cell Rpm Reagent Dosage kg/t CT min FT min
RF 250 1200 SOKEM 565C/524C/522C/503C 1 2 4
Results:
Collector Product Wt% Acid insoluble %
Assay Distn
Float reject 50.8 41.60 98.2
SOKEM Non float 49.2 0.60 1.8
565C Head Cal 100.0 18.96 100.0
Float reject 47.2 44.20 90.4
SOKEM Non float 52.8 4.20 9.6
524CC Head Cal 100.0 23.09 100.0
Float reject 46.4 39.50 88.1
SOKEM Non float 53.6 4.60 11.9
522C Head Cal 100.0 20.78 100.0
Float reject 46 33.10 88.4
SOKEM Non float 53.6 3.80 11.6
503C Head Cal 100.0 17.56 100.0

3.4 Collector dosage variation

Tests were conducted at D80 size of 400 microns by varying collector SOKEM 565C dosage
from 0.4 to 1.2 kg/t. The results are shown in Table 4. Result indicated that the increase in collector

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dosage decreased Wt % yield and % AI grade. 0.4 kg/t collector is jusrt sufficient to reduce silica to
stipulated levels. Rao et.al (2009) obtained optimum results at 0.6kg/t SOKEM 565C for cement
grade concentrate.
Table-5: Effect of collector SOKEM 565 C Dosage variation
Conditions; Mesh of grind 5’, D80 400microns, Flotation pH 8, and % S 19
Stag Cel Rpm Reagent Dosage kg/t CT min FTmin
e l
RF 250 1200 SOKEM 565C 0.4/0.6/0.8/1.0/1.2 2 4
Results;
SOKEM 565 C Acid insoluble %
Product Wt%
dosage kg/t Assay Distn
Float reject 32.8 41.30 75.2
0.4 kg/t Non float 67.2 6.60 24.8
Head Cal 100.0 18.00 100.0
Float reject 47.2 35.00 92.1
0.6 kg/t Non float 52.8 2.70 7.9
Head Cal 100.0 17.90 100.0
Float reject 48.8 34.30 92.9
0.8kg/t Non float 51.2 2.50 7.1
Head Cal 100.0 18.00 100.0
Float reject 50.8 41.60 98.2
1.0 kg/t Non float 49.2 0.60 1.8
Head Cal 100.0 18.96 100.0
Float reject 56.8 31.00 98.8
1.2kg/t Non float 43.2 0.90 2.2
Head Cal 100.0 18.00 100.0

3.5 Effect of % S
Flotation tests were conducted varying % of solids from 20/47. Increase in % of solids though
increases yield, but reduces selectivity. Tests were conducted by varying pulp density 19/33/47 % S.
The results are given in Table-6
Table-6: Effect of %Solids on inverse flotation
Conditions; Mesh of grind 5’has D80 400microns Flotation pH 8, Collector 0.4 kg/t
Stage Cel Rpm Reagent Dosage kg/t CT min FT min
l
RF 250 1200 SOKEM 565C 0.4 2 4
Results:
Acid insoluble %
%Solids Product Wt%
Assay Distn
Float reject 40.8 41.60 98.2
19 Non float 59.2 0.60 1.8
Head Cal 100.0 18.40 100.0
Float reject 44.8 33.43 98.0
33 Non float 55.2 0.68 2.0
Head Cal 100.0 18.83 100.0
Float reject 59.2 31.10 97.8
47 Non float 40.8 1.00 2.2
Head cal 100.0 18.79 100.0
Incidentally similar results were obtained by Rao et.al(2009) by working on flotation of low grade
limestone samples of Andrapradesh. This may be attributed to better dispersion of air bubbles in the

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pulp and better dropping of entrapped silica in the froth. But to obtain low silica metallurgical grade
concentrate 20 % solids seems to be optimum. Shandilya and Jha (2012) while working in ACC
Madukkarai flotation plant opined that 20-24% S was found optimum for maximum selectivity, total
carbonate recovery and productivity.
3.5 Test under optimum conditions
Test under optimum conditions of 20% solids, MOG D 80 400 microns, natural pH 8,
collector conditioning time of 2 minutes and flotation time of 4 minutes in each stage with
0.4 kg/t SOKEM 565C in I stage. The results are given in Table 7.The I stage flotation with
0.4 kg/t collector produced concentrate assaying 52.00% CaO, 6.6% SiO 2, 1.17% MgO, 1.7%
Fe2O3, 1.0% Al2O3, 37.0% LOI with weight % yield of 67.2, meeting the cement grade
specifications.

Table 7– Result of final test under optimum conditions

Conditions; MOG D80 400 microns, pH 8, SOKEM 565C dosage 1.0kg/t, % S 20
Stage Cell Rpm Reagent Dosage kg/t CT min FT min
RF1 250 1200 SOKEM 565C 0.4 2 4
RF2 250 1200 SOKEM 565C 0.6 2 4
Results;
Product Wt% Acid insoluble %
Assay Distn
RF1 reject 32.8 41.38 75.4
NF1 Cement grade conc. 67.2 6.60 24.6
Head Cal 100.0 18.00 100.0

3.7 Final test for cement grade concentrate production

The test comprised of grinding the sample to MOG D 80 400 microns, desliming/ screening
over 400 mesh, rougher conditioning with 0.4kg/t SOKEM565C for 2minutes at 50%S, rougher
flotation for 4 minutes at pH 8 and 28%S. The non-float and slimes constituted the final concentrate.
The test was carried out to simulate the industrial condition. The results are given in Table 8

Table 8 – Result of final test simulating plant conditions

Conditions; MOG D80 400 microns, wet screening over 400 mesh for removing slimes in -400 mesh fraction ,
+ 400 mesh sand subjected to flotation.
Stage Cell Rpm Reagent Dosage kg/t CT FT
%S min %S min
RF 250 1200 SOKEM 565C 0.4 50 2 28 4

Results;
Product Wt% Acid insoluble %
Assay Distn
-400 mesh slimes conc. 12.0 12.00 8.0
Non float conc. 76.0 9.12 38.5
Float reject sand 12.0 80.30 53.5
Head Cal 100.0 18.00 100.0
-400#+RNF Conc (Cem grade) Cal 88.0 9.51 46.5

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The results indicate that a composite of slime and deslimed non float yielded a cement grade assaying
9.51% AI, 90% Total carbonates at wt% yield of 88.The concentrate size was coarse [D 800.3mm]
w.r.t. ACC concentrate[D800.2mm]. The non-float sand fraction assaying 80.30% AI, 18% total
carbonates may be used as eco sand. Incidentally, Shandilya (2012) recommended the flotation rejects
as ACC eco sand for plastering and concrete works. The above desliming- inverse flotation nil waste
process appears to be stable, easily adaptable at site,- producing raw materials for civil construction
like ACC Eco sand as an alternative to river sand and cement grade limestone .

4 CONCLUSIONS

A low grade Limestone from ACC mines, Madukkarai, Coimbatore district, Tamilnadu assaying 45%
CaO, 80% TC, 18% SiO2, 1.3% MgO, 1.30% Fe2O3, 2.50% Al2O3, 0.33% alkalis and 36.00% LOI
yielded a cement grade composite concentrate ( non-float and slimes) assaying 9.51% AI, 90% Total
carbonates at wt% yield of 88 by a process comprising of grinding to MOG D 80 400 microns,
desliming/ screening over 400 mesh, rougher conditioning with 0.4kg/t SOKEM565C for 2minutes at
50%S, rougher flotation for 4 minutes at pH 8 and 28%S. The non-float (-16+400 mesh) sand fraction
assaying 80.30% AI, 18% total carbonates may be used as eco sand. The evolved nil waste process is
stable, selective, and easily adaptable in the existing anionic soap direct flotation plant at ACC
Madukkarai cement works
REFERENCES
1. IBM ,(2013), Indian Mineral Year Book, Limestone, Chapter 32, pp32.1-32.6
2. TV Vijaykumar, DS Rao,S.Subba Rao, G Bhaskar Raju and S Prabhakar (2003) Beneficiation
of a low grade limestone by Flotation,MPT-2003 Panjim, pp-194-207.
3. AT Sutone and Amanullah,(2004), Performance Evaluation of Limestone Beneficiation Plant
of M/S. Associated Cement Company Limited at Madukkarai Cement Works, Proc MPT
2004, IMMT Bhubaneshwar pp MPT-21.1 -21.4.
4. TV Vijayakumar, DS Rao, S Subba Rao, S Prabhakar and G Bhaskar Raju, (2009), Direct and
reverse flotation studies on a siliceous limestone, Proc.MPT2009 IMMT Bhubaneshwar, pp
MPT 73.1-73.6.
5. DS Rao, T.V.Vijaya Kumar, S.Prabhakar and G.Bhaskar Raju, (2009): AT Mineral
Processing., vol.50. pp. 36-47.
6. A.Shandilya (2012), sage of froth flotation reject as sand, XXVI IMPC,New Delhi, pp-
675.4922-675.4930.
7. Rachappa Kadli, Gajula Suresh Ram, M V Rudramuniyappa and B P Ravi (2014),
Beneficiation of Limestone from Bagalkot, Karnataka for Metallurgical Industry, IJERT, 3(3)
pp 2095-7.