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H. Hernaandez

1

, C.O. G oomez, J.A. Finch

*

Department of Mining, Metals & Materials Engineering, McGill University, 3610 University, Montreal, Qc., Canada H3A 2B2

Received 14 March 2003; accepted 2 May 2003

Abstract

The role of four gas dispersion parameters in ink particle collection was investigated in 4

00

and 20

00

otation columns. Gas holdup

(e

g

) and supercial gas velocity (J

g

) were measured on-line and bubble size (d

b

) was estimated using drift ux analysis that enabled

bubble surface area ux (S

b

) to be calculated. Operating with approximately zero froth depth ink recovery as a function of retention

time (controlled by underow rate) was determined. Using a mixing model, the collection zone otation rate constant (k

c

) was

estimated from the recoverytime data. The rate constant was not related to J

g

or d

b

but was linearly dependent on e

g

and S

b

,

similar to ndings in mineral otation studies.

2003 Elsevier Ltd. All rights reserved.

Keywords: Froth otation; Flotation kinetics; Modeling

1. Introduction

Flotation involves contacting particles (typically

<150 lm) in a pulp (slurry) with a dispersion of bubbles

(typically 0.52.5 mm). The properties of this bubble

(gas) dispersion clearly play an important role. Recent

developments have permitted reliable measurement of

some gas dispersion parameters, notably supercial gas

rate (J

g

), gas holdup (e

g

) and bubble size (d

b

). In a series

of papers on mineral otation systems, Gorain et al.

(1995a,b, 1996, 1997, 1998) found the pulp zone ota-

tion rate constant (k

c

) (i.e., excluding the froth) did not

correlate with any of these parameters individually but

was linearly dependent on a derived parameter the

bubble surface area ux (S

b

), the bubble surface area per

unit time per unit cross-sectional area of the otation

cell, given by S

b

6 J

g

=d

b

(Finch and Dobby, 1990).

The relationship, typically expressed k

c

PS

b

, seemed

independent of machine type, S

b

appearing to dene the

key machine contribution to otation with P (o-

atability) lumping all other factors such as particle size

and hydrophobicity eects. The observation has at-

tracted considerable attention, including a critique of

the database (Heiskanen, 2000). We have argued that e

g

can substitute for S

b

, supported by data from various

sources including de-inking in a otation column (Finch

et al., 2000). This communication continues to explore

the relationship between rate constant and gas disper-

sion parameters using de-inking of recycled paper in a

otation column.

In this, the system oers some advantages over min-

eral otation in mechanical machines. The low solids

content in de-inking,

2

typically 1% w/w solids, means

the bubbles are unlikely to fully load, meeting an as-

sumption for calculating a rst-order otation rate

constant. The low % solids and absence of mechanical

agitation enables gas holdup to be measured simply and

reliably by dierential pressure.

2. Experimental method

2.1. The columns

The experiments were performed on industrial paper

recycle pulps using a 4

00

laboratory (10 cm, H 600

cm) and a 20

00

pilot column (50 cm, H 550 cm)

installed at Bowaters Gatineau (Qc, Canada) de-inking

plant (Fig. 1). Three pressure transmitters were installed

at intervals along the length of both columns to measure

*

Corresponding author. Tel.: +1-514-398-1452; fax: +1-514-398-

4492.

E-mail address: jim.nch@mcgill.ca (J.A. Finch).

1

Now with PyroGenesis Inc. 2000 Willian St., Montreal, Qc.,

Canada H3J 1R8.

2

In de-inking % solids by weight is known as consistency.

0892-6875/03/$ - see front matter 2003 Elsevier Ltd. All rights reserved.

doi:10.1016/S0892-6875(03)00170-5

Minerals Engineering 16 (2003) 739744

This article is also available online at:

www.elsevier.com/locate/mineng

the gas holdup and to control the position of the pulp/

froth interface (i.e., level). The air rate was regulated by

a mass owmeter/controller. A peristaltic pump (with I/

O card) and a centrifugal pump controlled the ow of

feed and underow,

3

respectively. The feed and un-

derow rates were measured by magnetic owmeter with

signal conversion and were regulated using control

valves. Bubble generation used three porous stainless

steel spargers supplied by Mott Industrial with nominal

pore size 0.5, 2 and 20 lm. The temperature was mea-

sured with an ICTD probe. All instruments were mon-

itored using a serial communication interface OPTO and

a computer. The software package for data collection

and column operation was FIXDMACS version 6.1.

The general set-up and layout is shown in Fig. 2.

2.2. Procedure

The columns were fed continuously with pulp (45

C, 1.2% w/w solids, pH 10 (NaOH) and surfactant,

a blend of stearic and oleic fatty acid soaps) from the

feed end of the de-inking plant otation circuit (ca. 1.2%

w/w solids). The chemical conditions were not altered.

Level was controlled with the feed rate and set to within

12 cm of the column overow lip, i.e., operation with

essentially zero froth depth. The feed and underow

rates, gas rate and gas holdup were monitored during

each experiment. Samples of 1 L were taken from the

underow and feed streams as a function of time when

steady-state conditions were achieved. The particle re-

tention time was controlled with the underow rate. Ink

recovery was measured according to Bowaters proce-

dure and calculated as follows:

R

ink

C

i

S

i

Q

i

q

i

C

o

S

o

Q

o

q

o

C

i

S

i

Q

i

q

i

1

where S is the % w/w solids, Q the volumetric owrate, q

the stream density and the subscripts refer to initial (i)

and nal (o) values. The ink concentration C (ppm) was

measured using the reectance of paper pads at a

wavelength of 950 nm in a Technidyne Micro TB-1C

machine. An average of 10 values (5 per side) was ob-

tained.

2.3. Pulp (collection) zone mixing model

Recovery in the collection zone (R

c

) is a function of

the rate constant (k

c

), ink particle residence time (s

p

) and

degree of mixing, represented by the vessel dispersion

number (N

d

). One extreme of mixing is plug ow

(N

d

!0), where all elements have the same residence

time and there is a concentration gradient of oatable

particles along the axis of the column. The other ex-

treme is a completely mixed reactor (N

d

!1), where a

distribution of residence time exists and the concentra-

tion is the same throughout the vessel (Levenspiel,

1999). For a rst-order rate process with plug ow and

perfect mixing transport R

c

is given by Eqs. (2) and (3)

respectively:

R

c

R

eq

1 expk

c

s

p

2

R

c

R

eq

1

_

1

1 k

c

s

p

_ _

_

3

where R

eq

is the equilibrium (or maximum) recovery at

long otation time.

For vessels with levels of mixing between the two

extremes, the relationship between R

c

and N

d

can be

given by the axial dispersion model (Levenspiel, 1999):

Fig. 1. Column otation test facility at Bowaters de-inking plant.

3

In de-inking the underow is called the accepts.

Fig. 2. General experimental set-up.

740 H. Hernaandez et al. / Minerals Engineering 16 (2003) 739744

R

c

R

eq

1

_

_

4Aexp

1

2N

d

_ _

1 A

2

exp

A

2N

d

_ _

1 A

2

exp

A

2N

d

_ _

_

_

4

where: A 1 4k

c

s

ink

N

d

1=2

An expression for the vessel dispersion number N

d

as

a function of design and operating variables for the

system had been previously derived (Hernandez et al.,

2001) based on the form suggested by Luttrell et al.

(1990), namely:

N

d

1:3

D

c

H

c

J

g

J

l

1

_

_

e

g

_

_

0:67

5

where D

c

and H

c

are column diameter and height, re-

spectively. With the estimate of vessel dispersion num-

ber from Eq. (5) substituted in Eq. (4) the rate constant

was calculated.

2.4. Bubble size

In the absence of direct bubble size measurement,

which is only now becoming available for otation

systems (Hernandez-Aguilar et al., 2002; Grau and

Heiskanan, 2002; Randall et al., 1989), bubble size is

estimated. A method derived from drift ux analysis

using gas rate and gas holdup is employed (Banisi and

Finch, 1994).

3. Results

The rate equations require R

eq

, which, from inspec-

tion of the data, was 87%, a consistent nding in test

work at this Bowater operation (Watson, 1996; Leichtle,

1998; Hardie, 1998). In the lab column where the height/

diameter ratio is 60 plug ow can be assumed (Finch

and Dobby, 1990) where the otation rate constant (k

c

)

is the slope of the plot ln1 R

c

=R

eq

against residence

time (s

p

). Fig. 3 shows this assumption is supported.

Nevertheless to be consistent the rate constants for all

tests, lab and pilot scale, were determined using the axial

dispersion model given by Eq. (4).

The dependence of k

c

on the various gas dispersion

parameters was explored. Against gas rate (Fig. 4) the

data divide into a set for each column while against gas

holdup a reasonably linear dependence was found (Fig.

5). Against bubble size (Fig. 6) no relationship is ap-

parent (if anything, an inverse dependence is antici-

pated) while the dependence on S

b

shows agreement

with a linear relationship (Fig. 7). The slope (i.e., P) is

ca. 10

4

(dimensionless).

Fig. 3. Test of plug ow assumption for lab column (sparger, 0.5 lm).

Fig. 4. Flotation rate constant as a function of supercial gas velocity.

0

0.2

0.4

0.6

0.8

1

1.2

1.4

0 5 10 15 20 25 30 35

Gas holdup, Eg (%)

F

l

o

t

a

t

i

o

n

r

a

t

e

c

o

n

s

t

a

n

t

,

k

c

(

1

/

m

i

n

)

4" Lab 20" Pilot

Fig. 5. Flotation rate constant as a function of gas holdup.

H. Hernaandez et al. / Minerals Engineering 16 (2003) 739744 741

4. Discussion

To test the dependence of rate constant on the gas

dispersion parameters requires integration of several

measurements. The work of Gorain et al., Heiskanen

(2000) and Heiskanen et al. (2001) illustrate some of the

issues. The system employed here oered the advantages

of operation without a froth (thus collection rate con-

stant is determined directly rather than having to de-

couple from froth eects) and low % solids (thus

approaching the assumption of a rst-order process,

which Fig. 3 indicates was met. The disadvantages are

the need to estimate the rate constant from a mixing

model and the need to compute d

b

. Experience in col-

umns suggests the estimate of d

b

is within 15% of the

Sauter mean (Yianatos et al., 1988). The particle size

range may be considered wide, ink particles are typically

<100 lm (Lindsay and Mostafa, 1995), but it is not

unusual to ascribe a single rate constant to a otation

feed, as for example in the work of Gorain et al.

The results are similar to those reported elsewhere.

The rate constant is linearly related to e

g

, as anticipated

in a previous communication (Finch et al., 2000), and to

S

b

, which agrees with the claim of Gorain et al. (1997,

1998). The P, ca 10

4

, is of the same order as found by

Gorain et al. (1998) (after converting their values to

dimensionless form), although correspondence with P

for Zn minerals in mechanical machines may simply be

fortuitous. Relating the two parameters, S

b

5:5 e

g

as

before (Finch et al., 2000) but given S

b

is in part derived

from e

g

(via d

b

estimated by drift ux) the two param-

eters are not strictly independent. The lack of depen-

dence on J

g

and d

b

, mirroring the ndings of Gorain

et al. (1995a,b, 1996), has at least two sources: the

variation in bubble size with gas rate (d

b

tends to in-

crease with J

g

), and variation in the J

g

d

b

relationship

between machines, which probably explains why for the

two columns the k

c

J

g

data divide into two sets (Fig. 4).

The dependence on bubble surface area ux implies

an inverse dependence on bubble size whereas the liter-

ature supports k

c

/ 1=d

n

b

with n from 0 to 2 (Ahmed and

Jameson, 1989) and even 3 (Yoon, 1993). An n > 1

implies that bubble size has more impact on the rate

constant than a linear dependence on S

b

would indicate.

It may be that the variation in bubble size is too limited

(Fig. 6 shows a range of only 0.1 to 0.2 cm) and a linear

dependence on S

b

emerges as an approximation. The

range of bubble size available in an operating machine

tends, however, to be limited and thus the approxima-

tion may be practical. Bubble size is controlled by ma-

chine design and operating variables, most of which are

xed except for gas rate and frother dosage. If frother

concentration is constant the d

b

J

g

relationship could

be calibrated, then S

b

becomes a function of J

g

only

(Xu et al., 1991; Gomez and Finch, 2002). Fig. 4 hints at

this (surfactant dosage was not varied in our tests): the

rate constant is reasonably correlated with gas rate for

the two columns individually.

The linear k

c

S

b

relationship has excited much at-

tention, forming the basis of one approach to otation

modeling (Gorian et al., 2000; Harris and Harris, 2002).

Apart from the database being limited in bubble size

range it is also dominated by relatively ne particles

(again the case here). Heiskanen et al. (2001) found

linearity was approached only for the nest particles

(<32 lm). Some question remains, therefore, regarding

the range of applicability. In addition to the rate con-

stant, bubble surface area ux inuences entrainment

and froth behaviour since water transport depends on S

b

(Xu et al., 1991; Ventura-Medina and Cilliers, 2002).

The otation models are progressively incorporating

these components.

Regardless of modeling, the gas dispersion parame-

ters become powerful diagnostics. The measurements

Fig. 6. Flotation rate constant as a function of bubble size.

Fig. 7. Flotation rate constant as a function of bubble surface area

ux.

742 H. Hernaandez et al. / Minerals Engineering 16 (2003) 739744

have been used to remedy instrument and machine

malfunctions and dene the cell operating range (Dahlke

et al., 2001). We have used measurement of S

b

to help

unravel summer/winter metallurgy swings (communica-

tion in preparation); to evaluate changes in rotor speed

and location in a mechanical machine (as reported by

Kerr et al., 2003); and, in scaling up a de-inking column,

to select from among candidate sparger types, nding

that while all operated on the same recoveryS

b

line

some could not deliver sucient S

b

(Finch et al., 1999).

Surveys show S

b

in the range 2050 s

1

(Deglon et al.,

2000) with a maximum ca. 100120 s

1

before the

cell oods (or boils) (Finch et al., 1999; Gorain

et al., 1997; Xu et al., 1991). Being well below the

maximum may imply the operating S

b

seeks a compro-

mise among rate of otation, entrainment and froth

transport. In a bank of cells, a certain prole of S

b

may be optimal (Gomez and Finch, 2002; Dahlke et al.,

2001).

5. Conclusions

De-inking in a otation column was used to test the

dependence of the pulp zone rate constant on the gas

dispersion parameters. A linear relationship with bubble

surface area ux was found as reported in mineral o-

tation in mechanical machines. A linear dependence on

gas holdup was also found supporting a previous sug-

gestion that these two gas dispersion parameters can be

interchanged.

Acknowledgements

The authors wish to thank Bowater Gatineaus mill

for providing equipment and test facilities. Special

thanks are also given to the Mechanical and Chemi-

mechanical Wood-Pulps Network (Natural Sciences and

Engineering Council of Canada Network of Excellence)

for their nancial support, and the Consejo Nacional de

Ciencia y Tecnologa (CONACYT) of Mexico for a

scholarship to H.H.

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