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

design methodology and kinetic analysis

Dariuh Azizi, Mahdi Gharabaghi , Negar Saeedi

School of Mining Engineering, College of Engineering, University of Tehran, Iran

a r t i c l e

i n f o

Article history:

Received 17 July 2012

Received in revised form 23 June 2014

Accepted 24 June 2014

Available online 26 July 2014

Keywords:

Coal otation

Experimental design

Kinetic analysis

Optimization

PlackettBurman methodology

a b s t r a c t

In this paper, the otation method has been used for the preparation and beneciation of coal samples.

The PlackettBurman methodology has been applied to design of experiments and this experimental design

method is based on Hadamard matrix and ash content and efciency index have been considered as responses.

The operating conditions were chosen based on some screening tests. Results showed that ash content and efciency index could be 15.2% and 42.55 respectively when the values of collector, frother and solid percent were

5.29 kg/t, 78 g/t and 10% respectively. The effects of variables were studied by which increasing and decreasing of

responses could be transparently observed. Coal otation kinetic was studied and the results show that the

optimum time is 2 min to complete the otation process. In this investigation, the coal otation procedure was

optimized and the time of otation has been found by which energy consumption would be signicantly

reduced. Also, coal qualities could be improved by which needs of industry can be considerably satised.

2014 Elsevier B.V. All rights reserved.

1. Introduction

Coals are heterogeneous mixtures. The hydrophobicity of the former

depends upon the type of material [1] and the rank [2]. Microscopically,

coal has a crosslink network structure of polymeric molecules [3] and

macroscopically, it is made up of nely mixed discrete organic entities

known as macerals [4]. Coals are often highly variable even when

from the same source. So each time a bulk sample is received, a

complete set of experiments is conducted using the classical method

of treating one variable at a time. Coals are used for coke making in

steel industry around the world. Ash has high adverse effects on the

productivity and coke consumption in blast furnace. An increase in the

ash content of a coal concentrate by 1% over a critical limit results in

an increase in coke consumption by about 45% as well as decreasing

blast furnace productivity by about 36%; therefore there is always a

pressure on coal preparation plants to supply coal with very low ash

[5]. Because of this problem, it is necessary to nd some methods to decrease ash content of coal. Flotation as a mineral processing method is

used to produce low ash coal in some industrial plants. Flotation is

one of the most complex mineral processing operations as it is affected

by a very large number of variables. Many of these are beyond the control of the mineral engineer and some cannot be even measured

quantitatively with the available instruments. The relations between

measured and controlled variables are intricately related. Sometimes,

simultaneously changing various component settings will reinforce a

or counteract each other if changes are not chosen wisely. For coal

nes (b 0.5 mm), froth otation is the most effective method of

separating ash forming mineral matter from the coals [6].

Many investigations about coal otation have been done through

which various methods and chemical materials have been introduced

to perform the otation procedure. Some investigations showed that if

otation is carried out with salt solutions, its performance could be

dramatically improved [712]. The seam-to-steam strategy offers an

entirely different solution for handling of ne coal [13] and the reverse

otation process had also been tested to desulfurize coal otation

concentrate [14,15]. Besides, characteristics of the otation procedure

can be determined by which this procedure could be perfectly

performed and some chemical materials have been found to carry out

otation. For more illustration, the otation studies performed with

low rank coals indicated that the mixtures of oils could be used to

improve otation recovery and selectivity [16]. Some studies have

shown that using surfactants can have inuences on coal otation

because surface of coal can signicantly be changed by surfactants

[1719] and many studies have been conducted to determine the effect

of particle size, shape and degree of particle locking (liberation) on coal

otation [20,21]. Miscellaneous investigations also tried to show the

effect of frother, collector, promoter, solid percent and other variables

on coal otation [2225].

2. Experimental design

University of Tehran, Tehran, Iran.

E-mail addresses: m.gharabaghi@gmail.com, gharabaghi@ut.ac.ir (M. Gharabaghi).

http://dx.doi.org/10.1016/j.fuproc.2014.06.021

0378-3820/ 2014 Elsevier B.V. All rights reserved.

the factorial designed test with analysis of variance [26,27]. There are

112

100

80

1

B1

B

B1

B

B1

B

B1

B

B1

B

@1

1

60

40

20

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1

1 C

C

1 C

C

1 C

C:

1 C

C

1 C

C

1 A

1

0

100

1000

Size (m)

100000

10000

variable at a time method, where one variable is varied at a time. In

statistical design, experiments can be conducted in an organized manner and can be analyzed systematically to obtain much needed

information. The information can be utilized for optimization purpose.

The statistical techniques have been used to study the otation of

minerals [2830] and coal [31,32]. A review of coal processing literature

indicates a lack of statistically based studies on the application and/or

interaction of reagents with coals [33]. Naik et al. [34] carried out a 25

factorial design to study the effect of diesel oil, pH, MIBC, particle size

and sodium silicate on the otation of a low-rank on-coking coal. They

also carried out 23 factorial design experiments [35] on the inuence

of sodium metasilicate, kerosene and MIBC with a higher rank coal.

The PlackettBurman design as one of the most important method of

factorial design has been used as the experimental design. This method

is based on Hadamard matrix by which this experimental design

method has been created.

In an 1867 paper on simultaneous sign-successions, tessellated

pavements in two or more colors, and ornamental tile-work Sylvester

used self-reciprocal matrices, dened as a square array of elements of

which each is proportional to its rst minor [36]. This wide class of

matrices contains orthogonal rows and columns. In 1893 Hadamard

proved that such matrices attain the largest value of the determinant

among all matrices with entries bounded by unity [37]. After that paper

the matrices with entries equal to 1 and mutually orthogonal rows

and columns were called Hadamard. Originally there was an interest in

real Hadamard matrices, Hij|R, which found diverse mathematical

applications, particularly in error correction and coding theory [38] and

in the design of statistical experiments [39]. H8 (8 8 Hadamard

matrix) was chosen to design coal otation tests of this investigation

that it given by:

1 1

1 1

1 1

1 1

1 1

1 1

otation in which the optimum point for this procedure and inuences

of variables has been studied. For this purpose, the PlackettBurman

design experiment method has been used by which this optimization

could be performed as correct as possible.

3.1. Material characterization

For this investigation, a representative sample of coal was taken

from the Hamkar mine, in Kerman province of Iran, and the entire sample was also crushed to a nominal minus 31.5 mm. The crushed sample

was sieved through which its properties can clearly be identied by

which this investigation could precisely be done. The result of sieves

analysis that has been shown in Figs. 1 and 2 shows characteristics of

the representative sample.

The experiments were carried out using a Denver type otation

machine with an impeller speed of 1000 rpm. The volume of this machine

was considered 2.5 L for these experiments. 250 g of the representative

sample was used in each test and solid percent was 10% in these experiments. Moreover, fresh water was applied to prepare slurry for otation

tests and pH of experiments was 7.5. Wetting time and conditioning

time were considered to be 5 min and 90 s, respectively. In addition, different kinds of frother and collector were used to perform otation tests

which their optimum value can be precisely determined by which kinetic

and optimization experiments were carried out as correct as possible. For

doing optimization and kinetic tests, in the rst step, various chemical

materials were chosen to carry out otation tests based on obtained information from primary otation tests. Afterward, optimization and kinetic

tests were done based on chosen materials in the primary experiments.

These experimental results are denitely analyzed in the following sections of this paper.

30

Distribution

Content

Distribution (%)

25

70

60

50

20

40

15

30

10

20

10

0

0

25000

12000

6000

2360

1000

500

300

150

Size (m)

Fig. 2. Characteristics of the representative ash.

75

< 75

Content (%)

10

80

yield

ash

32

40

10

20

Ash (%)

28

20

15

60

Yield (%)

Efficiency index

36

113

24

20

2EX20

Pine oil

A65

90

the operating conditions were determined by which optimization and

kinetic tests could be perfectly performed. For this purpose, different

kinds of frother and collector and various solid percents were analyzed

for which some primary tests were carried out. Consequently, needed

materials and the operating conditions can be completely chosen to

perform otation tests. This stage was done step by step through

which the rst step and considered target have been completely

satised.

Efficiency index

80

Pine oil

90

yield

80

70

70

60

60

50

50

40

40

efficiency index

30

ash

20

10

35

80

125

20

170

215

10

260

A65 (g/t)

90

90

yield

80

Efficiency index

80

70

70

60

60

50

50

efficiency index

40

40

30

30

20

10

20

ash

1.0

1.5

2.0

2.5

3.0

3.5

4.0

4.5

5.0

5.5

10

Collector (kg/t)

3

ash content of tailings=ash content of clean coal:

90

80

Efficiency index

In the rst step of primary tests, the kind of frother must be chosen

and some tests were performed based on operating condition that it

has been exactly described in the previous paragraphs.

As shown in Figs. 3 and 4ab, A65 can be considered as suitable

frother to perform otation experiments, because the value of yield

and efciency index increased when this frother was used to perform

tests. In addition, some tests were carried out to determine effects of

A65 amount on efciency index, yield and ash value. These tests were

performed at the same operation conditions of previous tests that

they were done to nd the best frother.

When these gures were precisely studied, it is clearly obvious that

the change of frother amount has not had a signicant inuence on ash

content and yield, therefore, they cannot be considered for nding the

value of frother. However, if the curve of efciency index is maintained,

it can be concluded that this factor has been importantly inuenced by

frother dosage. Therefore, frother dosage has been determined based on

this curve and 78 g/t has been chosen for this variable which this decision can be denitely reasonable because of studied proofs.

2EX20

30

For doing this study, suitable kind and value of materials should be

found for which some otation tests were needed to be carried out.

For this aim, the special condition was considered for doing tests and

choosing materials. These tests were performed in natural pH, 10%

solid percent and an impeller speed of 1000 rpm. Also, 4 kg/t of gas oil

and fresh water was used to do tests. Wetting time and conditioning

time were 5 min and 90 s respectively. For each test, yield, efciency

index and ash content were studied by which effects of miscellaneous

materials were observed. Efciency index was calculated based on

ASTM Standard Test Method D5114-90, as follow:

H20

Frother type

Dowfroth

H20

Frother type

Dowfroth

90

yield

80

70

70

60

60

50

50

efficiency index

40

40

30

30

20

10

20

ash

5.8

7.0

8.2

9.4

A65

10.6

11.8

10.3

10

14.2

Fig. 4. Effects of (a) frother on the yield ash content, (b) A65 amount on the efciency

index, yield, and ash content, (c) collector amount on the efciency index, yield, and ash

content and (d) solid content on the efciency index, yield, and ash content.

therefore some otation tests were carried out. The same as previous

tests, solid percent and pH were 10% and 7 respectively and 250 g of

114

Table 1

Coded and actual levels of independent variables used in the experimental design.

Variable

Oil gas

A65

Solid content

Symbol

X1

X2

X3

Unit

kg/t

g/t

%

Role

Coded variable

level

Collector

Frother

+1

3.3

39

10

5.3

78

12

conditioning time were 5 min and 90 s respectively and gas oil and

A65 were considered as collector and frother. According to obtained

information in Fig. 4c, the value of collector should be 5.3 kg/t. Because

it was necessary to improve otation tests in efciency index and yield

which it can be obviously shown; if 5.3 kg/t of collector is used,

efciency index and yield could be signicantly increased and ash

content, on the other hand, could be declined. Next, solid percent should

be determined for which some otation tests were carried out and

operating conditions were similar to the previous steps despite the

fact that the value of collector and frother had been consider based on

the obtained results in the previous tests. For nding suitable and

optimum solid percent, relationships between solid percent and yield

and ash content and efciency index are needed to be analyzed by

which the value of solid percent could be perfectly found which is

applied to perform otation tests. For this purpose, solid percent versus

ash content, yield and efciency index were plotted in some curves in as

demonstrated in Fig. 4d.

By studying these graphs, it was concluded that if the value of solid

percent is considered to be close to 10%, satisfactory results could be

transparently obtained and ash content and efciency index could be

better than other conditions signicantly, although yield may be slightly

declined in this condition when it is compared with the value of

lower solid percent. Indeed, efciency index and ash content have

been prioritized to choose the best value of solid percent in optimization

tests.

4.3. Optimization of otation tests

To continue this investigation, nding optimum condition has been

considered and the relationship between miscellaneous variables and

optimum operating conditions has been illustrated by which the

otation procedure could be signicantly optimized. For this purpose,

Hadamard matrix was chosen as an effective method that it has been

known to design experiments. Since, the PlackettBurman (an experimental design method in DX7 software) design depends on Hadamard

matrix based on using the same as mathematic theory; it was applied

to optimize otation tests. By using this experimental design method

and three considered signicant variables to perform tests; some

results are demonstrated in Table 2.

If all variables are assumed to be measurable then the Plackett

Burman can be expressed as

y f X1 ; X2 ; X3 Xi

where y is the output and Xi the variables of action called factors [40,41].

The results inserted to Design Expert (DX) software and a model

among several models were chosen and tted to the results. The nal

equations in terms of coded factors are selected as the following

equations:

y1 Ash content 16:150:65X2 0:075X3 0:28X2 X3

2:35X3 2:23X1 X3 2:00X2 X3 :

Table 3 shows that prediction models of the efciency index and ash

content are signicant; because, P-value of models was under 0.05. Also,

inuences of collector, frother and solid percent were signicant.

Interactions between collector and solid percent and frother and solid

percent were signicant, while, other interactions didn't have a signicant effect on the efciency index.

As shown in Table 4, inuences of frother were signicant on the ash

content and there was an interaction between solid percent and frother.

As Fig. 5 shows the coefcient of multiple determinations (R2) tted

in them by the high value of R2 indicates that the equation is capable to

represent the system under the given experimental domain. Joglekar

and May suggested that for a good t of a model, R2 should be at least

0.80 [42]. R2 was found to be 0.9995 for efciency index and 0.8685

for ash content. The value of R2 shows that there is an acceptable

relationship between predicted and actual values; therefore, the models

were signicantly tted.

4.4. Inuence of miscellaneous variables on responses

The relationships between variables and ash content and efciency

index were studied and their effects on each other were found. In

order to determine these effects, experimental results have been

analyzed by software through which the model can signicantly be

selected and inuences of variable were perfectly portrayed. It was

concluded that the increase in solid content, collector dosage and

frother has increased efciency index. Moreover, interactions between

variables and their inuences on efciency index were maintained in

which some results could be obtained as demonstrated in Fig. 6.

If these interactions are studied, it can rmly be found that there are

interactions between solid content and frother and solid content and

collector dosage and these interactions happened when these variables

Table 2

PlackettBurman design of experiments for the study of three experimental factors in coded and actual levels with experimental results.

Run

1

2

3

4

5

6

7

8

X1

X2

X3

X1

X2

X3

+1

+1

+1

1

+1

1

1

1

1

+1

+1

+1

1

+1

1

1

1

1

+1

+1

+1

1

+1

1

5.3

5.3

5.3

3.3

5.3

3.3

3.3

3.3

39

78

78

78

39

78

39

39

10

10

12

12

10

12

12

10

Efciency

index

Ash content

(%)

33.3

42.5

39

36.9

37.3

32

35.8

22.4

17.3

14.9

15.6

16.1

16.3

15.4

16.9

16.7

115

Source

Sum of

square

df

Mean

square

F value

P-value

prob N F

Model

X2

X3

X2X3

Residual

Cor total

4.03

3.38

0.045

0.61

0.61

4.64

3

1

1

1

4

7

1.34

3.38

0.045

0.61

0.15

8.81

22.16

0.3

3.97

0.0309

b0.0093

0.6158

0.1172

Signicant

Signicant

Ash (%)

Table 4

Analysis of variance of the developed models for ash content.

Table 3

Analysis of variance of the developed models for efciency index.

Sum of

square

Model

252.23

X1

78.13

X2

58.32

X3

44.18

X1X3

39.61

X2X3

32

Residual

0.13

Cor total 252.36

df Mean

square

F value

5

1

1

1

1

1

2

7

776.09

0.0013

1201.92 b 0.0008

897.23

0.0011

679.69

0.0015

609.31

0.0016

492.31

0.002

50.45

78.13

58.32

44.18

39.61

32

0.065

168.55

Fo

P-value

prob N F

Signicant

Signicant

Signicant

Signicant

Signicant

Signicant

could have signicant inuences on efciency index.

Subsequently, inuences of variables on ash content were determined. For this aim, solid percent and frother dosage were chosen as

signicant variables by which ash content could be changed. Results

showed that when frother dosage was increased, ash content was obviously declined; however, the change of solid percent does not have an

important effect on the amount of ash content. Furthermore,

rth

er

(g

/t)

o

Solid c

)

ntent (%

b

Efficiency index

Source

Sol

id

co n

ten

t (%

)

le c

Co l

tor

(kg

/t)

45

efficiency index

c

35

30

25

y = x + 2E-13

R2 = 0.9995

20

20

25

30

35

40

Efficiency index

Observed value

40

45

17.5

ash content

Sol

id

Observed value

17.0

16.5

Fro

the

r (g

/t )

Fig. 6. 3D plot of effect of the interactions (a) between solid percent and frother dosage on

the ash content, (b) between solid percent and collector dosage on the efciency index

and (c) between solid content and frother dosage on the efciency index.

16.0

15.5

15.0

15.0

co n

t en

t (%

)

y = x - 2E-12

R2 = 0.8685

15.5

16.0

16.5

17.0

17.5

Predicted value

Fig. 5. Relationship between predicted and observed values for efciency index and

ash content.

there has been an interaction between solid content and frother dosage

in the middle value of these studied variables approximately.

Afterwards, for doing a more complete study of the relationship

between variables, a 3D graph was needed to be portrayed in which

this aim could be realized. For this purpose, variables versus ash content

and efciency index were plotted in a 3D graph. This kind of graph can

116

Table 5

Results of the process optimization and optimum levels of variables.

Case

Target

Collector

Frother

Solid content

Ash (%)

Efciency index

Desirability

Ash content

Variable

Efciency index

Minimum

In range

Maximum

5.29

78

10

15.2

42.55

provided to understand the mechanism of the otation procedure.

It should be explained that interactions among important variables

solid content and decreasing frother dosage enhanced ash content.

In addition, when each variable was increased, efciency index was

signicantly inuenced through which the value of this important

parameter was sharply raised. In fact, this gure can describe inuences

of variables on ash content and efciency index when there were

interactions between them and it helped to understand this otation

process perfectly.

Finding optimum condition was one of the most important aims of

this investigation through which the performance of the otation

procedure can be signicantly improved. This possibility can be

provided by the PlackettBurman experimental design method which

depends on Hadamard matrices. The otation procedure could be

optimized in which the value of variables have been identied to

perform this procedure as ash content and efciency index have been

obtained in minimum and maximum values respectively as shown in

Table 5.

Understanding the condition of the procedure in optimum point can

help to describe otation tests that can be used to nd effective and

signicant variables in this process. For this aim, inuences of variables

on ash content and efciency index were needed to be maintained by

which increasing and decreasing of responses could perfectly be illustrated. According to signicant interactions among variables and their

inuences on efciency index and ash content, optimum point has

been studied and relationships between interactions and responses

have been portrayed in 3D plots as shown in Fig. 7.

If this gure is studied to understand the otation procedure,

anticipated optimum condition can be justied which can be predicted

by software. It is clearly obvious that inuences of interactions on responses can be understood and studied through which the enhancement

90

80

70

60

50

40

30

20

10

0

0

Fig. 7. 3D plot of effect of the interactions (a) between solid percent and collector dosage

on the efciency index, (b) between solid percent and frother dosage on the efciency

index and (c) between solid percent and frother dosage on the ash content.

25

50

Time (s)

Fig. 8. Cumulative yield for coal in kinetic analysis test.

dosage and decreasing solid content have increased ash content.

4.6. Kinetic analysis

From a practical point of view, the overall otation process can be

generally represented by a rst order system with lumped parameters,

assuming that the collection zone was perfectly mixed. Eq. (7) shows

the rst order model for a perfect mixed batch otation process [43]:

R

kt

1e

R

maximum otation recovery at innite time, and k is the kinetic rate

constant which involves all the microscopic sub-processes.

This has allowed a otation cell to be modeled using the chemical

reactor analogy; whereby the removal of solids from the pulp phase is

dened by a rst order rate equation. This means that a bank of cells

can be approximated by perfectly mixed CSTR's in series [44].

Subsequently, efforts have been made to accurately determine the so

called over-all otation rate constant (or k). This is not trivial, as k is

dependent on particle size, degree of liberation, air ow rate, agitation,

etc. To account for this, various continuous distribution functions of k

have been devised [45]; although previous reviews by Dowling et al.

[46] conclude that no single distribution model could sufciently

represent k; and Roesch et al. [47] suggest that attempts based on the

rst order kinetic assumption are approximative and hide secondary

details.

Determining the time of otation has been one of the most

substantial factors which should be known in every otation procedure.

In fact, it can be applied to nd optimum time in which recovery could

be when maximum value and time of otation would be sharply

declined. In this case, if the time of otation is not exactly observed,

more money and energy should be spent to perform otation. Finding

real otation time could help to decrease costs, because it can denitely

make spending time, consuming chemical materials and operating

conditions decrease transparently. Due to these reasonable proofs, the

kinetic of the otation procedure was studied to determine the otation

time. For this purpose, one otation test was carried out and operating

conditions were chosen based on optimum condition which has been

determined in optimization section. During the otation procedure,

several samples were taken to calculate yield in every sampling time

by which the kinetic could be precisely found. Yield versus time has

been plotted in one curve in which the trend of the kinetic has been

portrayed perfectly (Fig. 8).

Based on this curve, the kinetic rate constant (k) was 0.053 and it

can be understood that recovery has been stabilized in 120 s in which

recovery was 86.72%. It has been concluded that the otation procedure

has been completed in 120 s and if the otation time increases,

performance will never be improved and time, energy and chemical

materials will be surely wasted. Consequently, the otation time can

be optimized when the kinetic is analyzed and designing otation cell,

reagent consumption and choosing otation circuit can be signicantly

inuenced and they will be selected based on more information.

5. Conclusion

In this research work, the PlackettBurman methodology has been

used to optimize the coal otation process and nd important variables.

Representative sample of coal was taken from Hamkar coal mine, in

Iran. Experimental design, analysis of results, optimization and

modeling of the process were done by DX7 software. Predicted values

obtained using the model equations were in very good agreement

with the observed values (R2 value of 0.9995 for efciency index, R2

value of 0.8685 for ash content). Results of optimization showed that

117

ash content and efciency index could be 15.2% and 42.55 respectively

when the values of collector, frother and solid percent were 5.29 kg/t,

78 g/t and 10% respectively. Besides, the kinetic of the procedure was

studied through which the time of 120 s has been considered as the

optimum time and at this time the otation procedure could be rmly

completed.

Acknowledgment

This research work was partly supported by Iran National Science

Foundation (INSF) under contract number 92000649. The authors also

appreciate Mr. Arash Ashra for his help to this paper.

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