CHAPTER-II

REVIEW ON SIVAGANGA GRAPHITE DEPOSIT AND

INVESTIGATION OF PROCESSING OF LOW GRADE ORE

The second chapter describes the geology, reserve, beneficiation and investigation

on Sivaganga graphite deposit. The commercial graphite is relatively expensive industrial

mineral and to obtain good quality graphite concentrate, beneficiation is essential in order

to gain optimal prices for the finished product. The mineral beneficiation plays an

important role in the conservation of mineral resources through recovery of marketable

products from the low grade ore deposits and mineral rejects [13-14]. Comminution is size

reduction to liberate valuable minerals from the gangue and also to prepare feed size

suitable for furher concentration. It is estimated that the world reserves of graphite exceed

1000 million tons. Graphite is found almost in every country.

Graphite deposits like other ore deposits also rarely occur in pure form in nature and

are often associated with worthless and deleterious constituents. The main gangue minerals

often associated with flaky graphite are quartz with subordinate amounts of clay,

goethite/limonite, carbonate, feldspar, hematite and pyrite is noticed in trace amounts.

There are various processes for graphite beneficiation depending upon the nature and mode

of association of gangue minerals present in the graphite ore. It is quite necessary that

harmful and worthless constituents associated with graphite must be separated out and

increased the carbon content to a specific desired extent for making it usable in a particular

industry. The present investigation provides the overall review on Sivaganga graphite and

various beneficiation techniques adopted for its upgradation.

20
2.1. GEOLOGY AND RESERVE OF THE GRAPHITE MINES AT SIVAGANGA

In India, the occurrence of graphite ore is limited to the States of Andhra Pradesh,

Orissa and Tamilnadu. The graphite deposit at Sivaganga in Tamilnadu is the best among

all other occurrences. The Department of Geology and Mining (DGM), Tamilnadu carried

out Sivaganga graphite project investigation at various stages from 1968 to 1971. The

investigation work involved systematic mapping, trenching, and drilling. The deposit in

this area shows pinching and swelling nature and the average width varies from 3 to 18

meters and extends upto 5.6 kms. [15].

2.1.1. Geology

The promising graphite occurrence is located about 7 kms. North-West of

Sivaganga town and is approachable by a metal road from Pudupatti on Sivaganga-Melur

road. The graphite bearing quartzite and quartrtzofelspathic gneisses have been noticed

discontinuously for a stretch of about 18 kms from the village of Komalipatty in the East to

Poovanthi in the West and it trends N80 0 E – S80 0 W .

2.1.2. Origin of graphite

The origin of graphite occurrences at Sivaganga may perhaps be attributed to two

different processes. The regional metamorphism of carbonaceous impurities in the original

argillaceous sediments may be one of the causes for the formation of the graphite in this

area. In addition, the contact metasomatism of the earlier calcareous sediments may also

have yielded graphite in this area. The shear, fractures and joints seem to have provided

channel ways to the younger instrusives like granites and pegmatites to traverse the earlier

rocks and produce the resulted effects. The intrusions which are contemporaneous with the

shearing and may have aided the formation of the graphite within the shear zone. The

contact metasomatic effects are also evidenced by the distinctive high temperature non-

21
metallic mineral assemblages namely wollastonite, epidote, grassularite, andradite, diopside

etc.

2.1.3. Reserve estimation and exploration

As per detailed investigation studies, a total reserve of 25 lakh metric tons of

graphite ore in the fixed carbon ratio of 10 to 30% is estimated in this area for a depth of

15 m, in the existing leasehold area. The estimated reserve of graphite ore in the lease hold

area is proved 25 lakh metric tons and possible 24 lakh metric tons. The detailed

investigation work, over remaining graphite occurrences outside TAMIN leasehold area in

Arasanoor, Keeranoor and Poovanthi block in the western side, has been carried out by

Geological Survey of India (GSI), Chennai from 2005 and 2006.

TAMIN Chennai has lease hold areas of graphite occurrences in Sivaganga District

to the extent of 242.46 hectares, covering four Villages namely Komalipatty,

Senthiudayanathapuram, Kumarapatty and Pudhupatti. Raw ore, thus obtained being

despatched to nearby graphite beneficiation plant for upgrading and to produce high grade

beneficiated graphite to suite the requirements of graphite related down stream industries.

The mining activity over these lease hold areas was commenced during the year of 1982.

2.2. MINING AND PROCESSING OF GRAPHITE

The graphite deposit at Sivaganga is being mined by open cast mining method. The

mined graphite is subjected to size reduction by crushing, grinding, flotation and

dewatering to upgrade the graphite concentrate from other gangue minerals.

2.2.1. Mining

Mining is considered to be easy and safe as regards graphite deposits, in view of

their comparatively soft nature and presence of hard rocks an either side. In order to expose

graphite deposit, thickness of 1 to 2 meters height of top lateritic soil is dozed out by using

dozer or removed by excavator and loaded through dumper and transported to separate

22
dump yard located in non-mineralized zone in lease area. Then drilling operations are

carried out by using compressed air driven wagon driller to depth of 10 feet over side

burden / interburden, to loosen it by carrying out blasting. The loosened overburden /

interburden are excavated out to the separate to dump yard located in non-mineralized area.

After exposing the graphite deposit, again drilling and blasting works are carriedout to

loosen graphite deposit. The graphite ore thus obtained is transported to stock yard for

blending. In stock yard, both high grade and low grade ores are stacked separately.

Depending on plant requirements, blending work is carried out and blended ore is

despatched to beneficiation plant for consumption.

2.2.2. Graphite Beneficiation Process

The Graphite beneficiation plant of Tamilnadu Minerals Limited is located 10 km

away from Sivaganga on Sivaganga – Melur road and 60 km from Madurai. The Sivaganga

graphite is of flaky variety with 14-15% average feed grade fixed carbon content and the

plant has rated capacity to process 200 tons of ore per day to yield graphite concentrate

with fixed carbon content up to 96% purity with 80 to 88 % recovery.

2.2.2.1. Crushing and Screening Circuit

Run of mine ore (ROM) of sizes below 250 mm is being carried out by tipping

truck from mine site to the ROM hopper of 70 tons capacity, provided with fixed grizzly

having square opening size of 275 mm x 275 mm. ROM passing through grizzly is fed to

double deck vibrating screen provided with screening surfaces having openings of 50 mm

and 10 mm dia. The + 50 mm material is fed to a primary double toggle jaw crusher having

capacity of 25 tons per hour to produce 80 to 85% passing 50 mm size particles. Then the

– 50 + 10 mm material is fed to an impactor crusher (hammer mill) having capacity of

20 tons per hour. The crusher section is operated in closed circuit with the double deck

23
screen. The – 10 mm size material from the double deck screen is stored in fine ore bin

(FOB) having a storage capacity of 300 tons.

2.2.2.2. Grinding Circuit

Thus stored fine ore bin (FOB) material is fed to the rod mill having a capacity of

10 tons per hour with the addition of requisite amounts of water, sodium carbonate and

sodium silicate solutions (10 %). The sodium carbonate is used as pH regulator and sodium

silicate is used as silica depressant. Proper functioning of the rod mill is monitored through

measurement of operating variables; a) pulp density and percentage of solids from mill

discharge b) screen analysis of the mill discharge and c) power drawn by the mill.

2.2.2.3. Beneficiation Circuit

The beneficiation of this plant is based on froth flotation techniques. Both

mechanical flotation cells and columns are used for flotation of graphite mineral. Diesel oil

is used as collector whereas MIBC is used as frother.

The beneficiation section is operated in three shifts round the clock. The discharge

from the rod mill (around 98 % passing 600 microns) is conditioned with required reagents

( mixture of MIBC and diesel oil) in a conditioner and is subjected to rougher flotation in

bank of six flotation cells at a pH of 8.5 – 9.0 which is maintained by addition of sodium

carbonate solution. The tailings from the rougher bank are sent to another similar bank of

six cells for scavenging after addition of reagent.

The froth from the rougher cell is fed to a ball mill for secondary stage grinding

through a cyclone, the under flow of the cyclone being fed to the ball mill. The over flow

of the cyclone along with the mill discharge is subjected to first stage cleaning in a flotation

column. The intermediate product from the column is subjected to regrinding in a ball mill

and the mill product is further cleaned in a bank of two cells (one twin cell). The froth

product from this bank is subjected to screening and washing in a screen for further

24
improving the grade and segregating the +210 and -210 micron material, the tailings from

the bank are fed to the scavenger bank.

The undersize of the screen is fed to a regrinding primary ball mill through a

cyclone. The under flow of the cyclone is fed to the ball mill. The overflow of the cyclone

along with the mill discharge is fed to a flotation column for further cleaning. The froth

product from this column is re-cleaned in another column. The froth product from the re-

cleaner is collected in the concentrate thickener as final product.

The tailings from the product cleaner and recleaner in a series of columns are fed to

the scavenger column along with the tailings of the coarse cleaner and the product of the

coarse scavenger cells. The froth from this scavenger column is fed to secondary regrinding

ball mill through a hydrocyclone. The discharge from this ball mill and the over flow from

the cyclone are fed to the column along with the discharge from the primary regrind mill

for cleaning. The tailings from the column are re-circulated to the rougher bank.

2.2.2.4. Dewatering and Drying

The thickener product slurry is dewatered using vacuum drum filters, while the

thickener over flow is reused / sent to re-circulating tank. The filter cake is further dried in

rotary double drum dryer before packing as a product. Similarly the screen over flow

graphite is subjected to dewatering through a horizontal belt filter or vacuum drum filter.

The filtrate is pumped to concentrate thickener. The moist filter cakes are fed in to double

drum rotary drier separately to reduce the moisture from 25 to 30% to 0.2% and the dried

products are bagged for sales.

Due to the technical problems, beneficiation plant of Sivaganga could not achieve

the target. The various research institutes were carried out investigation at different stages

to improve the plant performance.

25
2.3. INVESTIGATION ON SIVAGANGA GRAPHITE BY VARIOUS RESEARCH

INSTITUTES

i) Tamilnadu State Geology and Mining Department during 1968 to 1971 conducted

beneficiation studies on exploratory sample with feed grade of 23 % F.C. The flotation

test at mesh of grind (MOG) of 300 – 400 micron employing pine oil as frother,

kerosene as collector, sodium carbonate as pH regulator and sodium silicate as

dispersant. The test with 4 stages cleaning yielded a concentrate assaying of 83% F.C

with 88% overall recovery [15].

ii) National Metallurgical Laboratory (NML), Chennai in the year 1982 was conducted

beneficiation study [16]. They have observed that the pilot plant test runs enabled

production of acceptable concentrate grade of +85% F.C at –710 micron and

concluded that it is possible to get satisfactory cleaning at natural pH without using

sodium carbonate. Coarse grinding to -850 micron is also possible. It is concluded that

the production of high grade concentrates of +85 % F.C from the ore with recovery of

86 to 90% is possible. Subsequently, NML conducted another beneficiation study

during 1983. The findings of NML suggested that sodium carbonate is required for

slime dispersion. The eucalyptus oil may use as a collector/frother and rougher

flotation concentrate is ground in pebble mill and then cleaned thrice and the final

concentrate is 210 micron. The + 210 micron product is termed as large flakes

concentrate (product–I) and assayed of 95.2% F.C and – 210 micron product ground

in ball mill and after two stages of cleaning, the fine product is assaying 97% F.C

(Product–II). All tailings ground in ball mill and cleaned four times to produce

concentration assaying of 96.5% F.C. The overall recovery of 78% is produced by

total five stages of cleaning.

26
iii) The Indian Bureau of Mines (IBM, Nagpur) conducted beneficiation study during

1982-83 [17]. IBM crushed the graphite ore to – 1.68 mm size and then ground to

-500 micron in a rod mill and carried out rougher flotation tests by adding reagents.

The rougher concentrate was subjected to a pebble mill and floated in first cleaner

flotation cells. The gentle grinding followed by cleaner flotation was continued in

further 4 stages. The final graphite concentrate assaying of 96.69% F.C with

overall recovery of 78% is produced by total five such cleanings. In this, pine oil and

light diesel oil were used as frother and collector respectively and sodium carbonate

was used as a pH regulator. The process route followed by all the above three

laboratories were discussed, out of these three the process route followed by NML was

less complex and all the process data necessary for designing of plant has been

provided, process flow sheet and process data provided by NML, therefore adopted to

design sivaganga graphite beneficiation plant.

iv) Tamilnadu Minerals Limited (TAMIN) established a graphite beneficiation plant at

Sivaganga during the year 1994. TAMIN made an agreement contract with Larson &

Toubro (L&T) for setup a beneficiation plant based on the NML flow sheet and the

plant machineries designed by SALA international, Sweden. In the year 1995, the

plant commissioning work has been completed and started plant production. The L&T

could not achieve the set targets during trial runs, further the NML suggested for

modification of the plant. The modifications suggested by the NML are given below:

• Replacement of roll crusher by impact crusher

• Screen panel of 10mm in lower deck in place of 20mm, in double deck

vibrating screen

• One new ball mill was introduced

• Two flotation cells as one unit

27
 • Six slurry and froth pumps were introduced

• Pipe line facilities to accommodate above.

After modification of the plant, the Ist performance gauranty (PG) test was

conducted, the plant was not capable to achieve the target. However, the L&T decided to

do second modification of the plant with one dryer in fine circuit of 2 tons capacity,

shifting of old fine circuit dryer to flaky circuit and changed four pumps of higher capacity

in beneficiation section. After second modification, TAMIN and L&T have conducted IInd

& IIIrd PG tests. But again they could not able to achieve the targets. During the trail run,

TAMIN has used the eucalyptus oil as frother, sodium carbonate as pH regulator and

sodium silicate used as a depressant. After that in the year 1996, TAMIN has changed the

frother to pine oil and replaced the pine oil with the Nalco chemical. The comparative study

reveals that the Nalco chemical shows the better results than the pine oil. The three PG test

results are given in Table 2.1.

Table 2.1
Results of performance guarantee (PG) tests
Concentrate
Throughput
Feed grade grade
Particulars per day (dry Recovery %
% F.C achieved
basis) m.t
% F.C
As per contract
200 14.2 96.30 92.20
with L&T
Ist PG test 60.58
176 16.14 89.79
(Feb. 1996)
IInd PG test
206 13.82 92.42 75.31
(Aug. 1997)
IIIrd PG test
225 14.44 92.19 76.35
(Dec.1997)

v) The Institute of Minerals and Materials Technology (IMMT, Bhubaneswar) and IBM,

Bangalore suggested that methyl iso butyl carbinol (MIBC) as frother in place of Nalco

chemical and adding diesel oil as collector [18-20]. At present, TAMIN is using the

MIBC as frother; diesel oil as collector and sodium carbonate sodium silicate as pH

28
 regulator and depressant respectively. IMMT approached by L&T studied the plant

operation and process flow sheet to improve the performance of the plant. Plant audit

suggested that the physical and chemical characteristics of samples indicate that rod

mill product is below 600 microns as expected. Ball mill product shows that not much

grinding is taking place in ball mill due to the operational problems. About 3.8 % F.C is

being lost in tailings which contributes 25% overall loss in the circuit. A good amount

of graphite loss was observed in column tailings due to recycling. A product with 94%

F.C is being obtained at 75% recovery during that period.

The rougher flotation studies were carried out on ROM ground to 600 microns rod

mill product collected from the plant indicates that both diesel oil and Nalco reagents are

giving almost similar performance in rougher flotation. The kinetic studies on both the

reagent confirm the same. About 0.6 kg diesel oil per ton of feed is required to float most of

the carbon values. Higher recoveries are observed with diesel oil due to cleaner tails in the

rougher circuits and also better grade product in cleaner circuit as the froth is easily

breakable during the conditioning. Based on the information collected during plant study,

the characteristics of the rod mill product indicate that the performance of the rod mill is as

expected and the required grinding is effected in the mill. It is suggested that the pulp

density in the mill may be measured and controlled regularly to have consistent

performance.

It has been observed that all the columns are not functioning properly due to

operational problems [21-23]. The following parameters are need to be monitored to derive

maximum advantage from the columns (a) wash water system: wash water velocity should

be maintained at 2 to 3 cm/sec in all the nozzles (b) air sparger: proper air rate and water

should be maintained in the air bubbling system to generate required size of bubbles

(c) power and water: continuous power and water supply is very much essential to avoid

29
chocking of air sparger system. Effective water spray is required for derrick screen for

proper size separation. All the nozzles should be operative with proper velocity. In general,

most of the measuring and recording instruments are neglected and not well attended. It is

suggested that all the instruments and control systems should be operated properly to

achieve desired level of performance of the plant.

Even though the plant appears to be simple, the number of unit operations and

controls were more compared to any other similar plant. So, it is essential that the plant

should be operated continuously uninterrupted to achieve the desired performance. The

most essential requirement for this is continuous power and water supply. The plant

performance can be improved by providing more clear water. It is suggested that suitable

flocculant and surfactant may be used in the thickening and filtration to improve clarity of

recycled water. Combination of diesel oil and MIBC may be used as collector and frother

in place of Nalco reagent to improve grade, recovery and overall plant economics.

vi) The Indian Bureau of mines Bangalore officials visited to Sivaganga graphite

beneficiation plant for Ist phase plant auditing work during 1998.The highlights of the

findings of the auditing study are given below. The processing of graphite is unique

and works well if a plant is operated in a controlled manner. The graphite processing is

sensitive to certain parameters such as grind size and collector selection play an

important role to upgrade the ore. The grind size in which the excessive slimes in the

system are harmful to the process. Since, the premium revenue is for production of

flaky, the grinding in the flaky circuit should be a controlled grinding without damage

to the flaky using cylpeb mills. Whereas in the fine circuit for liberating fine graphite

needs control by ball mill grinding. A sequence of grind followed by flotation,

preferably by columns is recommended. In case of collector, the graphite is associated

with ferruginous clay minerals, the usage of reagents like sodium carbonate and

30
 sodium silicate in conjunction with a mixture of hydrocarbon oil and frother like light

diesel oil (LDO) and MIBC was recommended.

The L&T flowsheet and the plant flow sheet indicates the misplacement of the

cleaner tail streams to rougher and scavenger circuit causing tail losses due to low retention

time. Further, grind and flotation operation philosophy is not fully practiced in all the

streams of the current plant circuit. Hence, two flow sheets have been suggested in this

report which eliminates the above misplacements of streams and equipments. A summary

of the bench scale tests were highlighted the process to a limited extent. The bench scale

tests revealed that concentrate assaying 90 to 95% F.C (average 94% F.C) can be produced

at recoveries ranging from 80 to 85% (average 81.5% F.C distribution) under the

conditions of final test. The throughput of the plant may be raised to near stipulated levels

if the recirculating streams are thickened and then recirculated. The limited bench scale

tests also indicated that it is difficult to achieve the concentrate grade of 96% F.C with 92%

recovery.

vii) Indian Bureau of mines, Bangalore and TAMIN jointly conducted the II phase

auditing study. The main objectives of the study were (1) to improve the graphite

recovery in the plant to over 90% and the tailing assay preferably is less than 1.3%

fixed carbon (presently it is around 4% F.C) and (2) the fixed carbon content of the

concentrate is to be over 94% F.C and maintaining the recovery. To increase the

throughput to about 10 tons (dry basis) per hour as compared to the present level of 6

to 7 tons. An attempt should be made to obtain coarse flaky (preferably + 300 micron)

to the maximum extent with grades of about 90% fixed carbon.

The studies conducted by IBM both in the laboratory and at the Sivaganga plant

have clearly shown that there is scope for substantial improvement in plant performance in

respect of throughout, concentrate grade and recovery. The plant can also easily tune to

31
meet the market requirements in respect of concentrate grades (up to 96% F.C) and flaky

proportion (up to 45% of total graphite concentrate in + 250 micron size).

On implementation of this, the plant could operate steady with better concentrate

production due to increased availability and less spillage yielding >96% F.C grade

concentrate (approx.16 TPD). In order to achieve the substantial improvement of plant

performance including increased throughput, recovery and production of concentrate,

additional flotation batteries, samplers, pumps which have to be situated in appropriate

places. Though, in the laboratory locked cycle tests at 850 micron primary grind, it was

possible to achieve composite concentrate grade of about 94% F.C (about 94% F.C flaky

and 95% F.C fines) with overall recovery of 95% F.C and tailing assay of about 1 % F.C.

However, in actual plant conditions this is a very difficult target to achieve. Hence a

realistic target of about 85 to 88% recovery and average grade of 92% F.C is reported for

coarse grind as a basis for deciding on further investment in plant for increasing the

throughput.

viii) Advanced Research Center for Metallurgy and Power Materials (ARC-I), Hyderabad

and Zavalie, Ukraine experts visited the Sivaganga graphite beneficiation plant during

1998 and conducted preliminary investigation study. During investigation as per their

suggestion plant has been operated. They claimed that the technology route adopted

by L&T was very stiff i.e. not flexible for any change or modification and insufficient

preliminary investigation of Sivaganga ore by L&T and its capability of beneficiation

before setting up the full production plant. They found that the rod mill discharge is

very coarse and check points of processing of product at different levels are absent.

Steady and stabilized dosage of reagents is not administrated. Design does not

envisage the regular control and analysis of fixed carbon content during the operation

(shift). There is no easy access for such sampling points. They were also suggested

32
 that the usage of light diesel oil (LDO) as collector. There is no way to measure the

quantity of air and its control into each flotation cell. Establishing a low rate of pH in

flotation pulp and irregular supply of pulp due to frequent stoppage of rod mill

because of overflow and recommended that a prerequisite ore testing laboratory and

its beneficiation scheme before planning the project.

The layout of the plant is very close and cramped, even regular plant maintenance

and servicing of individual unit is unapproachable and difficult. They obtained the F.C

concentrate of 94.33 % graphite recovery of 94.27 % and F.C in tailing was 1.1%. One can

easily note that in the lower range, the ash content is higher and this means that one can get

more high F.C (>96%) in product separation of fines. The above results were under the

following conditions of size +0.630mm, consumption of reagents: frother MIBC, collector

diesel oil, pH 9, sodium silicate as depressant.

The Ukraine experts were carried out the following tests during 1998 for scrutiny of

technology. They found the reasons for unsatisfactory performance and possibility of

achievement were explained by laboratory experiments and it was shown that the real

possibility to reach F.C content in product 94 to 95% and tailing 2% with the existing

equipments. Stable and continuous operation with achievement of F.C in product 95 to

96% and tail less than 1.5% will be possible after implementation of the main part of

technological and organizational measures pointed out in their report.

2.4. IMPORTANCE OF FLOTATION REAGENTS

Flotation requires the formation of a stable bubble-particle aggregate which helps

the particle to be carried out from the pulp. The stability of the aggregate depends on the

interfacial free energies or the corresponding interfacial tension of the solid/liquid,

solid/vapour and liquid/vapour interfaces, which are responsible for attachment process.

The tendency of replacement of solid/liquid by solid/vapour interface depends on the

33
hydrophobicity of the floated particles. Surface chemistry has developed a number of

methods, such as the adsorption of collector and frother, activator, depressant or modifier to

change the hydrophobicity and behavior of the solid in view of selective flotation.

Collectors and frothers may be called primary reagents which primarily control flotation,

depressant and pH regulators have a secondary role to perform in support of the primary

reagents [15].

a) Frothers: A frother has a number of functions in flotation. First, it reduces the surface

tension of the air-liquid interface in order that a stable bubble is produced in the system.

Secondly, it influences the kinetics of bubble-particle adhesion and thirdly, it thins the

liquid layer by interacting with collector molecules and finally stabilizes the bubble-particle

aggregates. In addition to the frother properties like surface activity, surface viscosity of the

medium etc., in the nature of the solids, i.e., the particle size and the hydrophobicity also

play a dominant role in imparting stability to the froth.

The choice of frother is also an important parameter determining the success of

froth flotation. It is only recently that the importance of frothers in determining the froth

structure of the concentrate and its consequences in film drainage is being recognised but

the design and efficiency of frother studies are required for improvement of flotation

performance. It has sufficient load support mechanism to carry the valuable up to launder,

by stabilizing the dual liquid membrance of prime importance to flotation are the adjacent

bubbles. All the frothers have hydrophobic and hydrophilic properties and they are

effective only on the air water interface. The functional groups generally differ in solvation

power, water retention capacity and solubility where as molecular weight, diffusivity

causes difference in life time and tenacity.

b) Collectors: Based on surface characteristics, all minerals are classified mainly into

non- polar or polar types. The non-polar minerals are composed of covalent molecules held

34
together by Vanderwalls forces, so that they displace a natural hydrophobic character.

Minerals coming under this category are coal, graphite, sulphur, molybdenite, diamond and

talc. Minerals with strong covalent or ionic surface bondings are known as polar types and

exhibit high free energy values at the polar surface. These types of minerals react strongly

with water molecule and hence behave naturally in a hydrophilic manner. Some minerals

like coal, diamond, graphite, sulphur etc. have natural hydrophobicity. Precipitates of the

second kind, formed by reaction between ions and certain organic reagents, are also

hydrophobic. Hydrophobicity has to be imparted to most other minerals and precipitates in

order to float them. Towards this purpose, a surfactant that will selectively adsorb on the

material to be floated is added to the suspension in water and conditioned by agitation. This

surfactant, called a collector, possesses at least one non-polar and one polar portion. Owing

to chemical, electrical or physical attraction between the polar portions and the surface

sites, the collectors adsorb on the particles with their non-polar ends.

Graphite comes under non-polar minerals and it has high natural flotability,

achieving greater recovery and first order kinetics with a favorable frother, collector

interaction. In general the petroleum products like kerosene or fuel oil is used as a collector

for coal flotation all over the world. Depending on the graphite ore characteristics, the

amount of collector consumption varies.

c) Depressants and modifiers: These may be called secondary reagents for flotation and

support the activity of primary reagents. For pH control lime, soda ash, caustic soda and

mineral acids are used. The purpose of using depressant in flotation is to prevent the

collector from adsorbing on a particular mineral in the mixture in the flotation pulp. For

siliceous gangue depression, sodium silicate is used.

35
2.5. GAS HOLD-UP [24- 27]

When gas is introduced in to a column, liquid or slurry is displaced. The volumetric

fraction displaced is called the gas hold-up ∈g . The complement (1- ∈g ) is the liquid or

slurry hold-up.

2.5.1. Method for measurement of gas hold-up

Gas hold-up can be measured in a number of ways. Method (a) measure the gas

hold-up for the whole vessel (‘over all’ hold-up) while methods (b) and (c) measure

hold-up over a given section of the vessel (‘local’ hold-up). In method (b) the given section

is defined by the distance between the pressure tapping points while in method (c) it is

defined by the signal path between the probes. Methods (b) and (c) can be used to measure

axial variation in gas hold-up. Method (c) can be modified to measure gas hold-up at

specific points within the column.

Method (b), the pressure method is selected for examination. This method is the

simplest; method (a), for example, is impractical with froth, and method (c) needs

calibration, usually against gas hold-up determined from pressure methods.

2.5.2. Role of gas hold-up and bubble size

Volumetric gas hold-up in a column apparatus affects not only bubble size

distribution but also the process rate and selectivity. It is governed by the flow rate of

phases and by bubble size. The assumption of uniform sized bubbles and uniform phase

velocity distributions can be considered when deriving the relationship. In this case, a

portion of the column cross section occupied by gas is equal to volumetric gas hold-up ρ ;

bubble rise velocity relative to the walls of the apparatus is assessed as u o = v g / ρ . The

layer of rising bubbles displaces a certain volume of the liquid which moves downwards.

Hence, the relative velocity of the bubble and the surrounding liquid (slip velocity) us is not

36
equal to uo. The velocity of the liquid near the bubble is evaluated under the assumption of

a steady volume of bubbly layer as bubbles rise.

2.5.3. Effect of operating variables on gas hold-up

2.5.3.1. Gas rate and liquid rate

A useful method of defining gas and liquid rate is the volumetric flow rate per unit

cross section, or superficial velocity. The superficial velocity is useful since it can be

compared for columns of different cross section.

The relationship between ∈g and Jg is used to define the flow regime. Gas hold-up

increases approximately linearly then deviates above a certain range of Jg. The linear

section is characterized by a homogeneous distribution of bubbles of fairly uniform size

testing a fairly uniform rate. This is called the bubbly flow regime. Above the transition Jg

gas hold-up becomes unstable and the flow is characterized by large bubbles rising rapidly,

displacing water and small bubbles downward.

2.5.3.2. Reagent concentration and solids concentration

The effect of gas and liquid rate at a fixed frother concentration is much impartent.

The addition of frother up to a certain concentration has a pronounced impact on reducing

bubble size. A reduced bubble size means reduced bubble rise velocity and consequently

gas hold-up is increased.

The impact of frother concentration where gas hold-up at a given, Jg, increases

significantly from 0 to 15 ppm. The increase in gas hold-up levels off above a certain

frother dosage corresponding to the known trend of bubble size with frother concentration.

The role of solids is more difficult to describe. A general consideration is that solid

particles may promote or retard coalescence depending upon their surface properties.

Specific to flotation is that the solids distribute between the liquid phase (i.e. remain in

suspension) and the gas phase (i.e. attach to the bubble).

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 Mineral solids in suspension gives slurry density ρ st and a slurry viscosity

μ st which have opposing effects on the bubble rise velocity. Solids attached to the bubble

gives a bubble-particle aggregate density ρ b greater than zero, causing bubble rise velocity

to decrease and therefore, gas hold-up to increase. Predicting the hold-up in the presence of

solids is therefore complicated.

2.5.3.3. Effect of frother dosage on bubble size

The bubble size estimation method can be used to assess the effect of frother dosage

upon bubble diameter in a spared column. An example of this is given in the results of

bubble size measurements in solutions of water-frother for two sparger types: filter cloth

and porous glass frit. There is clearly a strong effect of frother dosage at levels below about

20 ppm, which is similar to the trend reported by Klassen and Mokrousov for bubbles

issuing from a single orifice.

2.5.3.4. Frother addition to the gas phase

Conventionally, frother is added to the liquid phase which diffuses from bulk

solution to the interface. Frother concentrations have a strong impact upon bubble size.

Laboratory experiments have indicated that a more efficient means of frother addition is as

aerosol dropless in the gas phase. Smaller bubbles were produced by the gas phase by

addition of frother.

Addition of frother to the gas phase in an operating column is a plausible method

for a yield of smaller gas bubbles. The minimum aerosol droplet size that is required is

unknown. With a high gas velocity in the gas line it may be possible to add frother solution

by aspirating or pumping. This technique may also permit the use of spargers with larger

holes, which may be less prone to plugging.

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2.6. CHARACTERIZATION AND SELECTION OF FLOTATION REAGENTS

The high quality graphite requirement is raising various down stream industries and

to meet the demand, it requires a basic knowledge about ore and reagents characteristics.

The associated minerals in graphite ore affect the flotation performance. Due to this the

grade and recovery of graphite concentrate in beneficiation process detoriate. Hence, the

detailed characterization study is required on rod mill discharge, float concentrate, tailings

and reagents to understand the influence and effect on beneficiation process [28-36].

2.7. GAS HOLD-UP STUDIES ON GRAPHITE FLOTATION REAGENTS

Gas dispersion is one of the key factors in the mineral flotation process. Flotation

requires the formation of a stable bubble-particle aggregate which helps the particle to be

carried out from the pulp. The stability of the aggregate depends on the interfacial free

energies or the corresponding interfacial tensions of the solid/liquid, solid/vapour and

liquid/vapour interfaces, which are responsible for attachment process. The tendency of

replacement of solid/liquid by solid/vapour interface depends on the hydrophobicity of the

floated particles. Recent publications indicate that type and dosage of frother plays an

important role on the applicability of the drift–flux model. Studies carried out in two-phase

systems (water-air) have shown that frothers (surfactants) n-pentanol, MIBC, DF-250 and

F-150, increase in this order, the drag coefficient of the bubble/water interface, attributed to

the formation of a thin layer of water bonded to the bubble [37-39].

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