Powder Technology 291 (2016) 186192

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Powder Technology

journal homepage: www.elsevier.com/locate/powtec

An experimental study on the ultra-ne grinding of gypsum ore in a dry

ball mill
Bilge kszolu a, Metin Uurum b,
a
Nigde University, Graduate School of Natural and Applied Sciences, Nigde, Turkey
b
Bayburt University, Materials Science and Nanotechnology Engineering Department, Bayburt, Turkey

a r t i c l e i n f o a b s t r a c t

Article history: Gypsum is a crystalline form of hydrated calcium sulfate (CaSO42H20) generally used in cements and plasters in
Received 18 June 2015 the construction industry, though also in paints, fertilizers, medicines, papers, and textiles. For use in these ma-
Received in revised form 28 August 2015 terials, gypsum must be ground nely (b 100 m), if not ultra-nely (b10 m), for which ball mills are most ef-
Accepted 21 December 2015
fective. Despite gypsum's widespread use and the regular need to grind it, studies concerning the grinding of
Available online 21 December 2015
gypsum ore remain scarce. In response, in this study, we have systematically investigated how certain grinding
Keywords:
parameters (i.e., mill speed, ball lling ratio, ball size distribution, powder lling ratio, grinding aid ratio, and
Gypsum ore grinding time) of conventional dry ball mills affect the grindability of gypsum ore. We determined the properties
Ultra-ne grinding of the micronized gypsum products obtained in optimal grinding conditions, and the results showed that the dry
Dry ball mill ball mill grinding process can effectively produce ultra-ne gypsum products.
Product features 2015 Elsevier B.V. All rights reserved.

1. Introduction Gypsum is found in various regions of Turkey, mainly in Denizli and

Gypsum has been known for centuries as a building material. The
earliest known use of gypsum as a building material was in Anatolia, ap-
proximately 6000 B.C. Gypsum has been found on the interiors of the
great pyramids in Egypt, which were erected in approximately
3700 B.C. Gypsum is found on every continent in the world and is
among the most widely used minerals. Pure gypsum is a white-to-
transparent mineral, though impurities can give the mineral a gray,
brown, or pink coloration. Its chemical name is calcium sulfate dehy-
drate, and its chemical formula is CaSO42H2O. When gypsum is heated,
it loses approximately three-quarters of its water and becomes hemihy-
drate gypsum (CaSO4H2O), which is soft and can easily be ground to a
powder called hemihydrate gypsum plaster or plaster of Paris. If the
powder is mixed with water to form a slurry or paste, it will dry and
set rock hard. As the plasterwater mixture dries, the water will chem-
ically recombine with the hemihydrate gypsum, and the material will
revert back to the original composition of gypsum. While the hemihy-
drate gypsum plaster is in slurry form, it can be poured between two
paper and adhesive layers to make wallboard, poured into molds, or
used to ll cracks and crevices. Gypsum makes an ideal building materi-
al because it is abundant, economical, re resistant, strong, and versatile.
It can also reduce the transmission of sound, and its use can have other
environmental benets, such as reducing the waste delivered to land-
lls [1].
Corresponding author.
E-mail address: mucurum@bayburt.edu.tr (M. Uurum).
Ankara, it is widely used as special llers, supplementary white pig-
ment, fertilizer in farming, supplementary cementing material in vari-
ous construction activities, and as molds in dentistry and medicine,
among other applications. In all of these industries, gypsum is needed
in ultra-ne ground form [2]. Grinding has been utilized in manufactur-
ing ne and ultra-ne powders for the development of new materials
and for improving product quality. For a long time, grinding processes,
especially in ball mills, have been subjected to statistical and kinetic
analysis [3,4]. One of the predominant technologies in mining, the pro-
duction of minerals, and material treatment is grinding. Ball mills are
mainly used for that purpose [5].
Industrial grinding machines used in the mineral processing indus-
tries are mostly of the tumbling mill type. These mills exist in various
forms, e.g., ball, rod, pebble autogenous, and semi-autogenous. Balls
and rods are the traditionally used media shapes in tumbling mills [6].
Ball mills are typically operated close to their maximum power draw.
At the maximum power draw, it is assumed that the ball charge is
well mixed and that the void spaces between the balls are lled with
particles. In reality, however, particles can inuence the ball charge in
various ways, causing the maximum power draw to shift depending
on the nature of the inuence. The ball load contributes to the bulk of
the charge mass; consequently, a change in the location of its center of
gravity signicantly affects the power drawn by the mill. It is therefore
worthwhile to study the behavior of the ball charge and the inuence
of particles on it. From such a study, one can infer the conditions within
the charge that lead to maximum power draw and optimal throughput
[7].

http://dx.doi.org/10.1016/j.powtec.2015.12.027
0032-5910/ 2015 Elsevier B.V. All rights reserved.
 B. kszolu, M. Uurum / Powder Technology 291 (2016) 186192
Fig. 1. Particle size distribution of the crushed sample.
As such, the objective of this study was to examine how grinding pa-
rameters such as mill speed, ball lling ratio, ball size distribution, pow-
der lling ratio, grinding aid ratio, and grinding time impact the
grinding of gypsum ore. For this purpose, batch dry grinding tests
were performed in a laboratory-scale ball mill to determine the particle
size, width of PSD (particle size distribution), total surface area, and
color parameters of the nal micronized gypsum products.
2. Materials and methods
Gypsum ore (K Global, from UluklaNide, Turkey) containing
29.67% CaO, 46% SO3, and 20.93% LOI was used in this study. The sample
was crushed to a nominal maximum size of 2 mm using a jaw crusher
in a closed circuit with a 2 mm screen. The particle size distribution of
the crushed sample was determined by dry screening, the results of
which appear in Fig. 1. As shown, the sample contained particle sizes
of approximately d80 = 1.10 mm.
The grinding machine was a laboratory-scale ball mill made of stain-
less steel with the dimensions 200 200 mm. The grinding media were
stainless steel balls with a density of 8.000 kg/m3 and with three differ-
ent diameters (i.e., 2, 3, and 4 cm). Powder density was found to be
2.3 g/cm3. The grinding experiment was performed as a batch process;
after each test, all media and ground samples were removed from the
mill and the media separated from the products by dry sieving.
To investigate the effect of the experimental grinding parameters,
including mill speed (% of critical speed), ball lling ratio (Jb), ball size
distribution, powder lling ratio (fc), grinding aid ratio (% of powder
mass), and grinding time (min), on the micronized gypsum product
size, a series of experiments were conducted. Poly-acrylic acid
(CH2CHCOOH)n was used as a grinding aid, and to analyze the ground
products, a dry screen was constructed using 0.5000.3000.212
0.180 and 0.106 m sieves. Full size distributions were measured, after
which product sizes ner than 80% were passed through a sieve (d80)
diameter derived from the results of a sizer. The nal micronized prod-
ucts were measured using a dry laser sizer (Sympatec, NJ, USA).
Table 1
Experimental conditions of mill speed.
Condition Variable
Operational speed (% of Nc) 5060708090
Ball lling ratio (Jb) 0.25
Ball size distribution (234 cm) 304030
Powder lling ratio (fc) 0.10
Grinding aid ratio (% of powder mass) 0.0
Grinding time (min) 5.0
187
Fig. 2. Particle size distribution of products obtained in different mill speeds.
The critical speed (Nc), ball lling ratio (Jb), and powder lling ratio
(fc) were calculated using Eqs. (1), (2), and (3), respectively:
h i
Nc 42:3=Dd
0:5
rpm D mill diameter and d 1
ball diameter; in meters
Jb mass of balls=ball density=mill volume  1=0:6 2
f c mass of powder=powder density=mill volume  1=0:6 3
There are several ways that have been used to describe the particle
size distribution (PSD) width [8]. An additional property is the steep-
ness of the particle size distribution curve, dened by the steepness
factor (SF) [9]. This value is the quotient of the d50 and the d20 values
corresponding to the particle size such that 20% by weight of the parti-
cles present are ner. A curve with SF greater than 2 is described as
broad and curves with a factor of less than 2 as narrow or steep.
[10]. The SF value is calculated from d50/d20. The ratio (d90d10)/d50
can also be used [11,12] in addition to the ratio d80/d20 [13]. The d80/
d20 ratio is the simplest to calculate and is related to d80, the value
most commonly used in mineral processing to describe the product
size. As the product size distribution becomes narrower, both ratios
(d90d10)/d50 and d80/d20 decrease [8]. In addition, the particle size
ratio of d90/d10 becomes more useful for representing the PSD width,
and therefore this ratio was used in this study.
An organization called Commission Internationale del'Eclairage
(CIE) determined the standard values that are used worldwide to mea-
sure color. The values used by CIE are called L*, a*, and b*, and the color
Fig. 3. d80 values of products obtained in different mill speeds.
188 B. kszolu, M. Uurum / Powder Technology 291 (2016) 186192

Table 2
Experimental conditions of ball lling ratio.

Condition Variable

Operational speed (% of Nc) 80

Ball lling ratio (Jb) 0.150.200.250.300.40
Ball size distribution (234 cm) 304030
Powder lling ratio (fc) 0.10
Grinding aid ratio (% of powder mass) 0
Grinding time (min) 5

measurement method is called CIELAB. Symbol L* represents the differ-

ence between light (where L* = 100) and dark (where L* = 0); a* rep-
resents the difference between green ( a*) and red (+ a*); and b*
represents the difference between yellow (+b*) and blue (b*) [14].
The total color difference (E) was calculated using the measurements
and Eq. (4), by using L*, a* and b* values [15,16]. The color parameters
(L*a*b*) of micronized gypsum products were measured using a Fig. 5. d80 values of products obtained in different ball lling ratios.
Datacolor Elrepho450 xs in the study.

h i0;5
2 3.2. Inuence of ball lling ratio (Jb)
E L0 L2 a0 a2 b0 b 4

Ball mills are typically operated close to their maximum power

where subscript o refers to the color reading of the control feed
gypsum sample used as the reference, and a larger E indicates greater
color change from the reference gypsum sample.
3. Results
3.1. Inuence of mill speed
The speed of rotation of the mill inuences the power draft through
two effects: the value of N and the shift in the center of gravity with
speed. The center of gravity rst begins to shift to the left as the speed
of rotation increases, but as critical speed is reached, the center of grav-
ity moves towards the center of the mill as more and more of the mate-
draw. At the maximum power draw, it is assumed that the ball charge
is well mixed and that void spaces between the balls are lled with par-
ticles. In reality, however, particles can inuence the ball charge in var-
ious ways, causing the maximum power draw to shift depending on the
nature of the inuence. The ball load contributes to the bulk of the
charge mass; consequently, a change in the location of its center of grav-
ity signicantly affects the power drawn by the mill. It is therefore
worthwhile to study the behavior of the ball charge and the inuence
of particles on it. From such a study, one can infer the conditions within
Table 3
Experimental conditions of ball size distribution.

rial is held against the shell throughout the cycle. As the critical speed is Condition Variable
larger at smaller radii, the centrifuging layer becomes thicker and Operational speed (% of Nc) 80
thicker as the speed increases until the entire charge is centrifuging Ball lling ratio (Jb) 0.30
and the net power draw is zero [17]. It is well known that the rotational Ball size distribution (234 cm) Group I:05050
speed of any ball mill is important to efcient mill operation. The oper- Group II:50050
Group III:50500
ating variables for the optimization of mill speed appear in Table 1; the
Group IV:304030
mill speed varied between 50 and 90% of the critical speed in this work. Group V:206020
The experimental results are shown in terms of cumulative undersize Group VI:108010
(Fig. 2) and d80 values (Fig. 3), which were best at 80% and 90% of critical Powder lling ratio (fc) 0.10
speed, as shown by the results in which ground products have a particle Grinding aid ratio (% of powder mass) 0
Grinding time (min) 5
size of d80 = 340 m. As a lower mill speed consumes less energy, 80% of
the critical speed (i.e., 85 rpm) was preferred for studying the next
parameter.

Fig. 4. Particle size distribution of products obtained in different ball lling ratios. Fig. 6. Particle size distribution of products obtained in different ball size distributions.
 B. kszolu, M. Uurum / Powder Technology 291 (2016) 186192 189

Fig. 7. d80 values of products obtained in different ball size distributions.

Fig. 8. Particle size distribution of products obtained in different powder lling ratios.
the charge that lead to maximum power draw and optimal throughput
[7]. The energy input to a mill increases with the ball charge, and
reaches a maximum at a charge volume of approximately 50% [18]. In be reduced in size. If, after some time, the grinding medium is worn,
this study, the ball lling ratio (Jb) of the mill was increased from 0.15 then it is simply replaced [20]. In this experimental study, the inuence
to 0.40, and experiments were conducted at different operating param- of the gypsum lling ratio was observed using the conditions shown in
eters, shown in Table 2. The results are provided in Figs. 4 and 5 based Table 4. The results are reported in Figs. 8 and 9 in terms of cumulative
on the cumulative undersize and d80 values, respectively; better results undersize and d80 values, respectively, the latter showing that the parti-
were obtained at ball lling ratios of 0.30 and 0.40. Based on d80, the cle size decreases linearly with a decreasing gypsum lling ratio. The
products have a particle size of 320 m. As increased grinding media ll- best results were obtained at a lling ratio of fc = 0.05. As shown by
ing ratios in ball mills use more energy, a ratio of Jb = 0.30 was applied the results, micronized products had a particle size of d80 = 200 m.
as the optimal value in this study.
3.5. Inuence of grinding aid ratio
3.3. Inuence of ball size distribution
Generally, in many industries handling ne powders, various chem-
The efciency of grinding depends on the surface area of the grind-
ical additives and treating agents are used in several processes after the
ing medium. Grinding in a ball mill is effected by contacts between
grinding process for purposes such as the prevention of agglomeration
the ball and ore particles. The angle of nip is important, and ball sizes
between particles, the stabilization of the powder surface and the en-
must be carefully chosen in relation to the largest and hardest particles
hanced formation of ceramic powder. Therefore, if these chemical addi-
in the feed [19]. As not all industrial grinding processes in ball mills are
tives can be used as grinding aids, process simplication of the process
performed with the same ball diameter, using a mixture of different ball
diameters and ratios is common. The effect of parameters is particularly
important in ultra-ne grinding processes in ball mills. The experimen-
tal conditions and range of variables used as parameters in the ball mill
tests are summarized in Table 3. The results are given as a function of
the cumulative undersize and d80 values in Figs. 6 and 7, respectively.
These gures reveal a slight decrease in particle size as the ball size dis-
tribution changes. However, the results indicate that the particle size of
gypsum is not sensitive to variation in ball size distribution in this range.
Groups 4, 5, and 6 showed the same results: the d80 values for the
ground products were approximately 320 m. Therefore, Group 5, in
which 20% of diameters were 2 cm, 60% were 3 cm and 20% were
4 cm, was preferred for studying the next parameter.

3.4. Inuence of powder lling ratio (fc)

Ball mills are relatively simple grinding devices from an operational

perspective. The typical operational philosophy is to put as much grind-
Fig. 9. d80 values of products obtained in different powder lling ratios.
ing medium in a rotating tube as it can take and then introduce a feed
material. If the feed material is softer than the grinding media, it will

Table 4 Table 5
Experimental conditions of powder lling ratio. Experimental conditions of grinding aid ratio.

Condition Variable Condition Variable

Operational speed (% of Nc) 80 Operational speed (% of Nc) 80

Ball lling ratio (Jb) 0.30 Ball lling ratio (Jb) 0.30
Ball size distribution (234 cm) 206020 Ball size distribution (234 cm) 2060-20
Powder lling ratio (fc) 0.050.0750.100.150.20 Powder lling ratio (fc) 0.05
Grinding aid ratio (% of powder mass) 0 Grinding aid ratio (% of powder mass) 00.51.01.52.03.0
Grinding time (min) 5 Grinding time (min) 5
190 B. kszolu, M. Uurum / Powder Technology 291 (2016) 186192
Fig. 10. Particle size distribution of products obtained in different grinding aid ratios.
and a remarkable improvement in energy efciency may be expected in
the ne powder industries [21]. In this study, poly-acrylic acid
(CH2CHCOOH)n was used as the grinding aid chemical. Operating vari-
ables for the optimization of the grinding aid ratio used in the ball mill
tests are shown in Table 5. The cumulative undersize results that appear
in Fig. 10, and Fig. 11 also show the relationship between the grinding
aid ratio and the d80 particle size values. The d80 of ground gypsum
products decreased with increasing additive dosage from 0% to 0.05
by weight of the powder. Beyond this dosage, an upward trend in ne-
ness can be observed. Therefore, a 0.05% additive concentration was
chosen as the best dosage for further experiments. The product particle
size of the ratio was d80 = 90 m.
Higher grinding aid consumption resulting in lower product neness
has been reported by Zheng et al. [22] as follows: the use of grinding
aids can result in benecial or detrimental effects depending on the ad-
ditive type and the concentration. It may be noted that excessively high
uidity may result in less contact and interaction between the medium
and particles, and thus in lower grinding.
3.6. Inuence of grinding time and properties of micronized gypsum
products
The percentage of particles in the 1100 m range is used by gypsum
handlers as a limit on the neness of ground products. To obtain prod-
ucts with different particle sizes, different grinding times were thus
used in this study. In this way, ve different products were obtained
in terms of particle size. Other than particle size, the width of PSD
values, total surface area, and color parameter values were determined
Fig. 11. d80 values of products obtained in different grinding aid ratio.
Table 6
Experimental conditions of grinding time.
Condition Variable
Operational speed (% of Nc) 80
Ball lling ratio (Jb) 0.30
Ball size distribution (234 cm) 206020
Powder lling ratio (fc) 0.05
Grinding aid ratio (% of powder mass) 0.5
Grinding time (min) 510152030
for each product. A summary of the ranges of operating variables used in
the ball mill tests appears in Table 6. The particle sizes (d50 and d80) of
products after grinding for various specied grinding times (5, 10, 15,
20, and 30 min) are provided in Fig. 12. With each test, particle size con-
sistently became ner according to the grinding time, and the nest
product was obtained at a grinding time of 30 min. As the results indi-
cate, the product had a particle size of d50 = 4.25 m.
In this study, four different PSD width calculations were performed
for ve micronized gypsum products, the results of which are reported
in Fig. 13. The d50/d20 values showed a nearly stable trend with grinding
times of 530 min when the grinding time increased from 5 to 30 min.
All of them have greater values than 2; namely, micronized gypsum
products show broad properties according to SF. In addition, the results
of (d90d10)/d50, d80/d20 and d90/d10 PSD width calculations showed
that their values increased with grinding time. Because of batch opera-
tion, separation was not possible, and therefore broad results have
emerged.
The surface area of ne mineral products also affects the marketing
of gypsum, which is especially important when used as mineral ller.
The total surface areas of the ve micronized gypsum products were ob-
tained from the Sympatec particle size distribution measurement de-
vice. As expected, when milling time increased, the total surface area
of the products increased in parallel. As shown by the experimental re-
sults in Table 7, the surface area increased with grinding time between 5
and 30 min. The best results were thus naturally obtained at a grinding
time of 30 min, the product of which showed a value of 10.855 cm2/g.
Whiteness is an important specication of micronized mineral ller
products, and it is important for marketing purposes that whiteness be
high (95%). The L*, a*, and b* values of feed ore and ground gypsum
products are given in Figs. 14, 15, 16, respectively. Notably, the L* values
of the micronized gypsum products increased as grinding time in-
creased from 5 to 30 min. The value of a* decreased signicantly
when the grinding time increased to 30 min, while b*, the second
most important color value after L*, decreased from 2.51 to 1.83, reveal-
ing increased yellowness. The total color difference was calculated for
grinding times of 5, 10, 15, 20, and 30 min. The results are reported in
Fig. 17, which shows that E increases with increasing grinding time,
apparently reaching a maximum at 1.78. With values N1, there is a slight
Fig. 12. d80 and d50 values of obtained gypsum products.
 B. kszolu, M. Uurum / Powder Technology 291 (2016) 186192
Fig. 13. d50/d20, (d90-d10)/d50, d80/d20 and d90/d10 values of obtained products.
color difference between the feed and micronized gypsum products,
which is considered to be a natural result of the grinding process.
4. Conclusions
In this study, batch grinding tests of gypsum ore were performed
using a ball mill to investigate the effects of grinding parameters such
as mill speed, ball lling ratio, ball size distribution, powder lling
ratio, grinding aid ratio, and grinding time. The properties of the mi-
cronized gypsum products obtained were determined, among which
the best set of results was obtained with 80% of critical speed
(85 rpm) for operation speed, 0.30 as the ball lling ratio (Jb), 20%
(2 cm), 60% (3 cm) and 20% (4 cm) as the ball size distribution, 0.05
as the powder lling ratio (fc), 0.5% of powder as the grinding aid
ratio, and a grinding time of 30 min, which produced particle sizes of
d50 = 4.25. The results show that the grinding operation was highly
sensitive to the mill speed, ball and powder lling ratio, grinding aid
Table 7
The total surface area values of micronized gypsum products.
Grinding time (min) Total surface area (cm2/g)
5 7.365
10 8.395
15 9.218
20 9.905
30 10.855
Fig. 14. L* values of feed and micronized gypsum products.
191
Fig. 15. a* values of feed and micronized gypsum products.
ratio, and grinding time at unusually high levels. In the conditions ap-
plied, the impact of other variables such as ball size distribution on
product size was minor. In addition, four different measures of PSD
width were calculated for each ultra-ne gypsum product obtained.
This work shows that a narrower product particle size distribution can-
not be achieved with the lack of separation. Surface area increased from
7.365 to 10.855 cm2/g with increased grinding times between 5 and
30 min. Because it is well known that the specic surface area is in-
creased as the particle size becomes small, the L* color parameter
value of gypsum ore increased from 95.75 to 97.38, while the b* value
decreased from 2.51 to 1.83 due to the grinding process. As expected,
L* values of ultra-ne samples increased and b* values decreased, prob-
ably due to a clean particle surface on which agitation can cause the oc-
currence of a new mineral surface. The results show that the dry
grinding technique in conventional ball mills for gypsum ore can effec-
tively obtain ne and ultra-ne products.
Acknowledgments
The authors would like to thank K Global Company from Ulukla
Nide, Turkey to their colleagues.
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