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in a pilot-scale ball mill using Austin's and Nomura's models

PII: S0032-5910(18)30743-5

DOI: doi:10.1016/j.powtec.2018.09.016

Reference: PTEC 13690

To appear in: Powder Technology

Received date: 5 February 2018

Revised date: 30 August 2018

Accepted date: 6 September 2018

Please cite this article as: Alessandro L.R. de Oliveira, Luís Marcelo Tavares , Modeling

and simulation of continuous open circuit dry grinding in a pilot-scale ball mill using

Austin's and Nomura's models. Ptec (2018), doi:10.1016/j.powtec.2018.09.016

This is a PDF file of an unedited manuscript that has been accepted for publication. As

a service to our customers we are providing this early version of the manuscript. The

manuscript will undergo copyediting, typesetting, and review of the resulting proof before

it is published in its final form. Please note that during the production process errors may

be discovered which could affect the content, and all legal disclaimers that apply to the

journal pertain.

ACCEPTED MANUSCRIPT

Pilot-Scale Ball Mill Using Austin´s and Nomura´s Models

1

Department of Metallurgical and Materials Engineering, Universidade Federal do Rio de

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Janeiro – COPPE/UFRJ, Cx. Postal 68505, CEP 21941-972, Rio de Janeiro, RJ (Brazil)

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2

Centro Federal de Educação Tecnológica Celso Suckow da Fonseca, CEFET/RJ, UnED,

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Angra dos Reis, RJ (Brazil)

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ABSTRACT AN

Prediction of continuous steady-state ball milling using the traditional population balance

model requires knowledge of several functions, namely those describing the rate and

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distribution of breakage products, the mass transfer relationship between the mill hold-up

and the discharge, the mode of transport within the mill, as well as the description of

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internal classification, whenever present. In spite of its long track record, there are

comparatively few instances in which the population balance model of continuous ball

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milling has been validated in great detail under controlled conditions. The work analyzes

how confidently one can predict continuous milling in a dry open-circuit pilot-scale

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operating under a wide range of feed rates, mill speeds, fillings and feed materials (an iron

ore and a spent catalyst) using the population balance model. It relies on measured

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residence time distribution of the solids, the Austin model of grinding and the expressions

recently proposed by Nomura to describe mass transfer from the mill to the discharge to

predict continuous grinding. Breakage parameters of the materials studied were estimated

on the basis of batch grinding tests. Parameters in Nomura’s transport model were fitted on

the basis of a few selected continuous tests and were used to estimate the mill hold up

operating under a range of conditions. A comparison between experiments and predictions

demonstrated that errors in the measurements of hold-up were, on the average, 6.0%,

whereas those associated to the 80% passing size of the product were smaller than 5.6%.

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1. Introduction

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Prediction of the product size distribution in continuous ball milling using the

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population balance model (PBM) requires the description of several relevant

microprocesses, namely rate and distribution of breakage products, mass transfer

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relationship and internal classification, whenever present. With different simplifications,

the traditional population balance model has been successfully used to describe ball milling

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in industry [1-3], being also the basis of well-known model-based scale-up procedures.

Modeling approaches that rely on measurements of material breakage

AN

characteristics in batch grinding mills as the basis for predicting continuous milling [2, 3]

became particularly popular. They rely on the assumption that material breakage

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characteristics, namely breakage rate and distribution functions, may be estimated from

batch grinding tests under controlled conditions, to then simulate the mill operating

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the literature [4-10]. Indeed, Lo and Herbst [6] demonstrated the success in application of

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the PBM in predicting the capacity of the famous Bougainville Copper Mine mill, which

was not reaching the capacity designed on the basis of the Bond method.

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In spite of its importance, there are only a few studies that analyzed in great detail

the confidence in the predictions using the PBM. Mulenga [11] recently carried out a

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sensitivity analysis of parameters of the breakage function and the selection function on

predictions on continuous milling. The researcher observed, for instance, that about 20%

deviations in parameters of the breakage rate function resulted in 32% deviation in the mill

product size, thus demonstrating an important error-propagating effect. In the case of

breakage distribution function parameters, deviations of 20% in its parameters resulted in

deviations of up to 23% in the product size. Mulenga [12] also demonstrated that the model

of transport and mixing in the mill had a significant impact on predictions in continuous

grinding. However, studies that analyze in great detail the deviations on the prediction of

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the continuous population balance model in ball mills operating under a wide range of

conditions are not easily found in the literature.

One key component of the continuous mill model is the residence time, that is, the

relationship between mill hold-up and mill feed/discharge rate. The residence time of solids

in the mill influences the mill performance both directly and indirectly; the latter associated

to the influence of mill voids filling on the rates of breakage [3, 7, 13]. Indeed, the mass

transfer in the mill is closely related to the concept of residence time distribution (RTD),

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which has been the subject of extensive research for more than four decades [14-19]. Such

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studies have been useful in proposing descriptions of the number of mixers which can be

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used to describe the mass transfer from the mill interior to the discharge. Further, Swaroop

et al. [15] demonstrated a linear relationship between hold-up and feed rate for dry

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grinding, whereas Austin et al. [3] proposed an empirical relationship in which the rate of

solids discharge follows a power-law relationship of the hold-up of solids, whose

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parameters must be determined from experiments. More recently, Nomura [20, 21]

proposed a very detailed model that can be used to determine the relationship between the

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mass hold-up and the discharge rate for mills operating under a variety of conditions, with

very limited empiricism. This model, however, has not yet been validated in conjunction to

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scale-up mill models, such as the one proposed by Austin et al. [3].

The present work deals with the validation of the Austin scale-up model and the

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ball mill, analyzing the deviations in great detail for different simulated conditions.

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2. Modeling background

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The ball mill when operated in batch model may be considered a closed reactor, in

which neither material nor input is allowed during the processing period. The result is that

all material contained in the mill (hold-up) will be exposed to exactly the same grinding

time. The fraction of feed contained in a given size i that is broken (leaves its original size)

per unit milling time represents the rate of breakage si. The size distribution of fragments

generated in each breakage event is given by the breakage distribution function bij. As such,

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assuming first order breakage kinetics, the size-mass balance equation for batch grinding is

given by [3]

𝑖−1

𝑑𝑝𝑖 (𝑡)

= − 𝑠𝑖 𝑝𝑖 (𝑡) + ∑ 𝑏𝑖𝑗 𝑠𝑗 𝑝𝑗 (𝑡) (1)

𝑑𝑡

𝑗=1

𝑖>1

where pi is the fraction of material contained in size class i and t is the grinding time. A

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function that has been widely used to describe the effect of size on the rate at which

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particles disappear from size class i is [3]

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𝑆1 (𝑥𝑖 )𝛼

𝑠𝑖 =

𝑥 𝛬 (2)

1 + ( 𝑖)

𝜇

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in which xi is the representative size of particles in size class i, S1 is a parameter of the

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model, which represents the specific breakage rate of 1-mm particles, and α, μ e Λ are

additional parameters that depend on both material and grinding conditions.

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Several studies [2-5, 11-13] demonstrated that, for a given material, the breakage

rates vary with design and operating conditions in ball mills. Detailed studies have shown

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𝑆1 (𝑥𝑖 )𝛼

𝑠𝑖 = 𝐾𝐾 𝐾 𝐾

𝑥𝑖 𝛬 2 3 4 5 (3)

1 + (𝜇 𝐾 )

1

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AC

𝐷 0.2 𝑑𝑏

𝐾1 = ( ) ( )

𝐷𝑇 𝑑𝑏𝑇

𝑑𝑏𝑇

𝐾2 = ( ) (4)

𝑑𝑏

𝐷 0.5

𝐾3 = ( )

𝐷𝑇

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1 + 6.6𝐽𝑇 2,3

𝐾4 = ( ) 𝑒𝑥𝑝(−𝑐 (𝑈 − 𝑈𝑇 ))

1 + 6.6𝐽2,3

𝜑𝑐 − 0.1 1 + 𝑒𝑥𝑝(15.7 (𝜑𝑐𝑇 − 0.94))

𝐾5 = ( )( )

𝜑𝑐𝑇 − 0.1 1 + 𝑒𝑥𝑝(15.7 (𝜑𝑐 − 0.94))

where D is the mill diameter, db is the grinding media size, J the fractional mill filling, U

the void filling fraction and φc the fraction of the critical speed of the mill. The subscript T

T

refers to the parameters used in the standardized batch test, used to fit the model parameters

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in Eq. (2). The parameter c contained in the expression for K4 is usually taken to be equal to

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1.2 for dry milling and 1.3 for wet milling [18].

The discretized breakage function term bij in Eq. (1), represents the proportion of

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material contained in size class i that resulted from breakage of particles originally

contained in size class j. It is generally calculated on the basis of the cumulative breakage

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distribution function, given by

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ED

𝛾 𝛽

𝑥𝑖−1 𝑥𝑖−1

𝐵𝑖𝑗 = 𝜙 ( ) + (1 − 𝜙) ( ) (6)

𝑥𝑗 𝑥𝑗

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in which the parameters ϕ , β e γ vary according to the material and are relatively

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AC

The continuous steady-state ball mill may be described for a perfectly-mixed

volume in a modular form such that [18]

𝑖−1

𝑀ℎ 𝑀ℎ

𝑝𝑜𝑢𝑡,𝑖 = 𝑝𝑖𝑛,𝑖 − 𝑠𝑖 𝑝𝑜𝑢𝑡,𝑖 + ∑ 𝑏𝑖𝑗 𝑠𝑗 𝑝𝑜𝑢𝑡,𝑗 (7)

𝐹 𝐹

𝑗=1

𝑖>1

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ACCEPTED MANUSCRIPT

where Mh is the hold-up of solids inside the mill, F is the feed and discharge rate, si is the

rate of breakage of particles contained in size class i and bij is the breakage distribution

function. pin,i is the fraction of particles contained in size i that enter this well-mixed region

in the mil and pout,i is the size distribution of the discharge of this region. The ratio between

Mh and F is the nominal residence time of solids in this perfectly-mixed volume.

Practical application of Eq. (7) first requires knowledge of the breakage rate sj and

distribution functions bij that describe the breakage response of material in the mill.

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According to Austin´s method, these may be estimated from batch grinding experiments on

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a test mill under controlled conditions, fitting parameters of Eqs. (1), (2) and (6) to data,

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and then applying Eqs. (3) and (4) to account for deviations from the fitted (test) case.

Further, application of Eq. (7) also requires knowledge of the number of well-mixed

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regions which may be used to describe the mill active volume, the relative sizes of these

well-mixed volumes, besides the mass of hold-up of solids in the mill and how it relates to

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the feed or discharge rates. Eq. (7) directly applies to the case of a mill that is described as a

single perfect mixer with no internal classification.

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ED

One key component in Eq. (7) is the estimate of the hold-up of solids inside the

mill, for a given set of design and operating conditions of the mill or, alternatively, the

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mean residence time of solids in the mill. In the absence of any such estimate, one

alternative has been to assume that the fractional voids filling is equal to one [16]. A large

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body of experimental work on continuous mills, however, demonstrates that this is seldom

rigorously valid in practice [3, 14, 15, 17].

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Fortunately, a detailed model has been recently developed by Nomura [21], which

establishes a relationship between the hold-up and the feed rate in tumbling mills based on

the movement of the mill load and a model of the motion of balls and particles. The model,

when applied to the particular case of dry and grate-discharge mills, is briefly reviewed as

follows.

The hold-up mass (Mh) of solids in the mill may be expressed as

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where ρ is the apparent density of the material, L is the length of the mill, A is the cross-

sectional area of the mill, J is the fractional mill filling, εb is the nominal fractional porosity

of the static grinding load (taken as 0.4), U is the fraction of the grinding load occupied by

the material in a static mill and Ah is the cross-sectional area of the hold-up.

The expression used to describe the discharge of the material will depend on the

type of discharge used in the mill. Further, the rate of discharge of the material will depend

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on the speed at which it leaves the milling chamber (υop) and on the fractional open area

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available at the mill outlet (φs), in the case of grate-discharge mills. Under steady-state

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conditions, any infinitesimal change in hold-up of solids will be translated in change in the

discharge rate, since [21]

𝑑𝐹 = 𝜌υop 𝜑𝑠 𝑑𝐴ℎ

US (9)

AN

Combining Eqs. (8) and (9), the differential equation of the hold-up will be

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𝐿

𝑑𝑀ℎ = 𝜌𝐿𝑑𝐴ℎ = 𝑑𝐹 (10)

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υop 𝜑𝑠

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Eq. (10) establishes the linear relation between hold-up and feed rate, under steady-

state conditions, when the material output velocity and percentage of open area in the

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output are constant. Integrating Eq. (10) with the initial conditions Mh = Mh0, the mass of

material retained in the mill when there is no discharge (F = 0), and considering that φs and

υop are constant, gives

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𝐿

𝑀ℎ = ( ) 𝐹 + 𝑀ℎ0 = 𝑐1 𝐿𝐹 + 𝑀ℎ0 (11)

υop 𝜑𝑠

where c1 is the constant that expresses the discharge properties of the material at the outlet

of the mill. For Nomura [21], the mill is capable of retaining material in two ways: through

their adhesion to the grinding media, and through a volume that will remain in the mill even

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after the mill is no longer discharging – called dead volume. This mass of material adhered

to the grinding media is called Mhb, whereas the mass of material in the mill's dead space is

called Mhd, so that Mh0 will be given by

According to Nomura [21] the mass of material adhered in the grinding media (Mhb)

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will depend on the coefficient of friction of the material f and also on the total surface area

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of the grinding media. The total load of the mill, that is, the grinding media and the

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material, is divided into three regions in any cross-section of the mill (Figure 1): grinding

zone, ascending zone and falling zone. When the mill load flows through the three zones, a

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flow of material is created, favoring the transport of material to the exit of the mill.

However, at the same time as the grinding zone and the ascending zone contribute to the

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formation of the material flow, they also hinder the flow since they facilitate the creation of

a bed of grinding media, which is responsible for blocking the passage of the solids. Hence,

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Mhb is proportional to the friction factor f and to the surface area of the grinding media in

the grinding zone and in the ascending zone (Abg) through the expression

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𝑀ℎ𝑏 = 𝑐2 𝜌𝑓𝐴𝑏𝑔 = 𝑐2 𝜌𝑓 ⌈ ⌉ (13)

𝑑𝑏

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where c2 is a constant, f is the coefficient of friction, Vrb is the volumetric flow of balls in

the circumferential direction of the mill, Δtg and Δta are the residence times in the grinding

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and ascending zones, respectively, and db is the diameter of the grinding media. Derivations

of expressions for Vrb, Δtg and Δta, as well as an efficient solution algorithm, are presented

in Appendix A, which follows the work from Nomura [20].

In the case of dry grinding the coefficient of friction may be estimated from the

angle of repose (Θ𝑟 ) using the expression [21]

1 + tan Θ𝑟

𝑓= (14)

3

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The mass of material retained in the dead space (Mhd) will depend on the mill

characteristics, in particular, on the type of discharge control [21]. For instance, in grate-

discharge mills, the grate restricts the passage of material, contributing to the formation of

the dead volume. In this case, Mhd is proportional to the geometry of the estimated dead

space, represented by the area of the dead space (Ahd), i.e.,

T

IP

where c3 is a constant and εb0 is the porosity of the grinding load in the grinding and

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ascending zones. For grate-discharge mills, Ahd will be

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𝑉𝑟𝑏 (∆𝑡𝑔 + ∆𝑡𝑎 )

𝐴ℎ𝑑 = (1 − 𝜑𝑠 ) ⌈ ⌉ (16)

𝐿(1 − 𝜀𝑏0 )

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where φs is the fraction of open area in the grates.

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Nomura's important observation is that the same material can be accounted for in

both Mhb and Mhd. However, the constants c2 and c3 can compensate for the doubled

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Grouping Eqs. (11), (13) and (15) into a single expression, the hold-up of solids

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directly by experiments. They must be fitted on the basis of experimentally measured hold-

up values for mills operating under different feed rates. Indeed, Nomura [21] estimated

these parameters using data from the literature on a variety of ball mills operating under a

range of conditions, having found that c1 and c2 are typically inversely proportional to each

other for one particular mill studied.

3. Experimental

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Samples used in the experiments included an Itabirite iron ore from the Iron

Quadrangle (Minas Gerais, Brazil) and a spent catalyst used in oil cracking from a plant

located in Rio de Janeiro, Brazil. Size analyzes were measured by wet laser diffraction in a

Malvern Mastersizer® 2000 particle size analyzer. A summary of the samples

characteristics is presented in Table 1. The feed size of the iron ore is consistent with that of

a typical concentrate for pellet feed production, containing 80% of the material finer than

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177 µm and 8% of material finer than 10 µm The apparent density used in the computations

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has been estimated assuming a nominal porosity of 40% of the powder, a simplification

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commonly used [3].

The static angle of repose of the samples was measured using the hollow cylinder

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method, following the procedure used by Barrios et al. [22]. Through this, a lot of 2 kg of

material initially filled a PVC tube, which was then lifted, leaving a pile of material from

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which the angle was measured. Such measurement was conducted in triplicate and used to

account for the widely different flowabilities of the samples, evident from Table 1. From

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the measured angle of repose, the coefficient of friction of the material was estimated

(Appendix A).

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The dry milling system used in the present work was composed of a vibratory screw

feeder coupled to a continuous grate-discharge ball mill, which discharges directly on a

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scale (Figure 2). The feeder and its storage silo are placed on load cells, with a precision of

20 g. This feeding system is controlled by a computer in order to guarantee an accurate feed

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rate. The entire system is monitored and controlled by a supervisory system, developed in

LabVIEW®, that allows monitoring the most important variables of the process.

The continuous ball mill has a single grinding chamber (Figure 3), with 32 cm in

diameter (D) and 31 cm in length (L). The mill-motor assembly is positioned on three load

cells, which allow real-time measurement of the hold-up mass during the experiments,

whose maximum weight is 400 kg with an accuracy of 30 grams.

Discharge of material from the mill occurred through a grate, shown in detail in

Figure 3. It has 7 mm diameter apertures, which represent 8% of the total grate area.

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The mill used to perform the batch grinding tests was the same as the one used in

the continuous grinding experiments, thus eliminating any influence of mill dimensions as

well as of internal profile of the grinding chamber when using information from one mode

of operation to predict the other. However, in the case of these batch grinding experiments,

it was necessary to block with a film all apertures in the grate of the mill (Figure 3), so as to

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prevent exit of any particle from the grinding chamber during the tests.

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The batch tests consisted in milling of the samples at different times, followed by

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size analyzes of the ground material for each time by laser scattering in a Malvern

Mastersizer® 2000. The times selected for both spent catalyst and iron ore samples were 7,

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15 and 30 minutes, and the experiments were run under the operating conditions listed in

Table 2. Different values of voids filling fraction were selected for the materials given

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observations of typical values found in the continuous tests, analyzed later in the present

work.

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In order to limit the influence of grinding media size on the grinding experiments,

experiments were all carried out using 16 mm chrome steel balls.

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Continuous tests were performed with the mill under different operating conditions,

varying apparent volume feed rates (68 to 185 cm3/min), fractional mill filling (0.20 and

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0.30) and fraction of critical speed (0.30 and 0.75). The experimental procedure adopted in

all tests consisted in feeding the mill with a set feed rate of solids, operating the mill and

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monitoring the discharge rate of solids through continuously measuring the rate with the

scale. When the discharge rate matched the feed rate within less 5% of this value during a

period of time of at least 20 minutes, it was identified that steady-state conditions were

reached (Figure 4). During this period, samples of the product were collected and identified

so that their particle size distribution could be later determined using the laser scattering

particle size analyzer (Malvern Mastersizer® 2000). After this, the grinding circuit was

switched off and the mill contents were emptied, allowing a direct measurement of the mill

hold-up of solids. A total of 22 experiments were conducted. Unfortunately, in three of

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these experiments problems found in weighting prevented estimating the mill hold-up, with

the data only used in validation of Austin´s model.

4.1. Batch mill model estimation

Results from batch grinding tests are presented in Figures 5 and 6, which

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demonstrate the very good fit of the model to data. Table 3 summarizes the least-squares

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best-fit parameters of the breakage rate and breakage distribution functions. In both cases it

is evident that such good fit could be reached with even simpler functional forms of the

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breakage rate and breakage distribution functions than those presented in Eqs. (2) and (6),

respectively. Indeed, parameters in the denominator of Eq. (2) (μ and Λ) were disregarded

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in the model, considering then the denominator equal to one, so that

𝑠𝑖 = 𝑆1 (𝑥𝑖 )𝛼 (18)

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This is explained by the particularly fine feed (Table 1) when compared to the ball

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size (16 mm) used in the experiments. Further, it was found that the breakage function

could also be described by a simpler form of Eq. (6), with the parameter ϕ equal to one,

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𝛾

PT

𝑥𝑖−1

𝐵𝑖𝑗 = ( ) (19)

𝑥𝑗

CE

AC

presented in Table 4. Results from selected experiments are found in Figure 7, which shows

the relationship between the measured values of solids hold-up and the feed rates. It clearly

shows that the two materials studied present very different mass-transfer relationships,

which are associated to their different flow responses (Table 1). Indeed, for comparable

feed rates, the hold-up of solids of the iron ore was significantly higher than that of the

spent catalyst, which presented much greater flowability than the former.

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The model of Nomura was implemented in Matlab® (Mathworks Inc.) and the least-

squares best fit values of parameters c1, c2 and c3 of Eq. (17) were estimated using the

Nelder-Mead optimization method [23]. From the 22 experiments, 7 were selected for

model fitting, covering different combinations of mill speeds and fillings, so that four and

three of them corresponded to the mill operating at 30 and 75% of critical speed,

respectively. It was found that the same set of values could be used for both materials. This

contrasts with findings from Nomura [21], who observed that such parameters were both a

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function of material and mill. However, different sets of values were required to fit the data

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for the mill operating under the different percentages of critical speed. This requirement can

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be explained by the wide range of values of fraction of critical speed used in the tests (0.30

and 0.75), which is wider than typically covered in practice.

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Figures 7 and 8 compare the experimental data to those from the model, identifying

the seven sets used in fitting the model and the remainder, which corresponded to true

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validation of the model. The dashed lines of Figure 8 represent a dispersion of ± 300g,

showing that only four data points presented differences larger than that. The mean relative

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ED

𝑛

100 𝑀ℎ𝑒,𝑖 − 𝑀ℎ𝑐,𝑖

Mean relative deviation (%) = ∑| | (20)

𝑛 𝑀ℎ𝑒,𝑖

𝑖=1

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where Mhe,i and Mhc,i are the measured and calculated values of solids hold-up for the ith

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experiment, respectively.

Table 5 summarizes the fitted values of the parameters as a function of fraction of

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critical speed. The inverse relationship found by Nomura [21] for the parameters c1 and c2

for different materials ground in the same mill has not been observed here.

Residence time distributions of the solids measured as part of an earlier work [24]

allowed to identify that the flow of solids in the mill in question could be described as three

mixers in series, with fractional residence times given by 0.83, 0.10 and 0.07. A summary

of these results is presented in Appendix B. On the basis of this information and on the

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equation describing continuous milling (Eq. 7), continuous grinding in the mill could be

described by

𝑖−1

(1) 𝑀ℎ (1) 𝑀ℎ (1)

𝑝𝑖 = 𝑝𝑖𝑛,𝑖 − 0.07 𝑠𝑖 𝑝𝑖 + 0.07 ∑ 𝑏𝑖𝑗 𝑠𝑗 𝑝𝑗 (21)

𝐹 𝐹

𝑗=1

𝑖>1

𝑖−1

(2) (1) 𝑀ℎ (2) 𝑀ℎ (2)

𝑝𝑖 = 𝑝𝑖 − 0.10 𝑠𝑖 𝑝𝑖 + 0.10 ∑ 𝑏𝑖𝑗 𝑠𝑗 𝑝𝑗

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𝐹 𝐹 (22)

𝑗=1

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𝑖>1

𝑖−1

(2) 𝑀ℎ 𝑀ℎ

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𝑝𝑜𝑢𝑡,𝑖 = 𝑝𝑖 − 0.83 𝑠𝑖 𝑝𝑜𝑢𝑡,𝑖 + 0.83 ∑ 𝑏𝑖𝑗 𝑠𝑗 𝑝𝑜𝑢𝑡,𝑗 (23)

𝐹 𝐹

𝑗=1

𝑖>1

Eqs. (21) to (23) for the three perfect mixers in series are solved sequentially using

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the recursive method presented by King [18]. A total of six fitting parameters (three for the

breakage rate and breakage distribution functions per material and three for the transport

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function) were required to predict the size distribution of the mill discharge for a given mill

speed, with additional three parameters required for the other speed investigated.

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discharge are presented in Figure 9 for the iron ore. They show that the model provides

reasonable predictions, even considering that the simulated value of fraction of mill speed

is below the range used by Austin et al. [3] in fitting the parameter K5 in Eq. (4), which is

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0.4 to 0.9.

Figure 10 compares the measured to the predicted 80% passing sizes, which

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demonstrate that errors were smaller than 10 µm (with only two exceptions) – a maximum

of 17.8%, with a mean relative error of 5.61%. A summary of the fitting results is presented

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in Table 6. It shows that the errors involved in the predictions were significantly larger in

the case of the experiments conducted at 30% of critical speed, which is a highly unusual

condition, which is beyond of the scope of Austin´s scale-up model.

A sensitivity analysis was then conducted of the model of continuous grinding

considering its different assumptions. First, simulations were conducted using the actual

measured value of solids hold-up in Eq. (21) to (23). Although this is not realistic in

practice, it is useful to estimate some of the assumptions in the continuous mill model, that

is, the validity of describing the continuous mill as three mixers-in-series as well as the

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basic assumption of using data from batch grinding experiments to predict continuous

grinding. Table 6 shows that the errors have similar magnitudes using the measured value

of hold-up and using Nomura model to predict it, being even higher for simulations using

the experimental values of solids hold-up. This shows that the accuracy obtained in fitting

parameters of the Nomura model more than sufficed the needs for predicting the mill

product, so that no error-propagating effect from fitting the Nomura model affected

predictions of product size distribution. It thus shows that errors in predicting the mill

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product were associated to either the breakage parameters, the validity of the mixers-in-

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series model and/or the validity of describing continuous milling on the basis of batch data.

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Additional simulation scenarios are presented in Table 5. For instance, if instead of

considering the model for the three perfect mixers in series (Eqs. 21 to 23) it is assumed

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that the mill could be represented by a single perfect mixer (Eq. 7), mean relative

deviations would increase to 6.45%. Table 6 shows that such increase was mainly

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associated to the increased deviations of the results obtained with the mill running at 30%

of the critical speed, a condition in which mixing of the charge was less vigorous.

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Finally, simulations were conducted of the mill assuming that voids filling would be

constant, equal to U = 1, that is, all voids left in grinding media filled with particles. In that

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case, mean relative deviations would also increase in comparison to the base case, now due

to higher deviations in the results for 75% of critical speed, resulting in an overall relative

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5. Conclusions

A successful implementation of the Austin scale-up procedure coupled to Nomura

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transport model, followed with their application to describe continuous dry grinding in an

open-circuit pilot-scale mill, allowed to conclude that:

The Nomura transport model could successfully fit the data, with a mean deviation

between measured and predicted hold-up values of 6.0%.

The same set of fitting parameters were able to describe transport of two widely

different materials (spent catalyst and iron ore) milled in a range of throughputs and

mill fillings using the Nomura model. However, different sets of parameters were

15

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required to fit the data for the different speeds studied (0.30 and 0.75 of critical

speed).

Batch grinding data for both materials could be successfully fitted to simple

expressions of the breakage rate and breakage distribution functions.

The same mill used for conducted batch grinding tests was used to run continuous

open-circuit tests and predictions with the model considering three mixers in series

were consistent with experimental results, with mean relative deviations of 5.6% in

T

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values of 80% passing size in the product.

Additional simulations of the continuous mill allowed to conclude that no error

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propagation was identified of the Nomura transport model in predicting the product

size distribution. Also, that simplifying assumptions such as in describing the mill

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as a perfect mixer or in assuming that all voids left by the grinding charge are filled

with ground material, resulted in larger deviations between experiments and

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predictions. The magnitude of increase in these errors, however, was only marginal.

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Acknowledgements

The authors would like to thank the Brazilian Council of Research CNPq for

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financial support to the investigation (grant number 310293/2017-0). The authors would

like to express their appreciation to Dr. Shinishiro Nomura, for his guidance in the

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implementation of the transport model. The assistant of Mr. Anderson Chagas in the

implementation of the Austin model was also appreciated.

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List of symbols

AC

Ah cross-sectional area of the hold-up (m2)

Abg surface area of the grinding media (m2)

Ahd area of the dead space (m2)

bij breakage function (-)

Bij cumulative breakage distribution function (-)

C Austin´s scale-up parameter in K4 (-)

c1 constant in Nomura model that expresses the discharge properties of

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c2 constant in Nomura model (m)

c3 constant in Nomura model (-)

D mill diameter (m)

db ball diameter (m)

E(t) residence time distribution (-)

F feed and discharge rate in steady-state conditions (kg/h)

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F coefficient of friction, (-)

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fc fractional volume of voids in the grinding charge (-)

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G acceleration due to gravity (m/s2)

Hab mean falling distance of balls (m)

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Hap mean falling distance of particles (m)

I index for size classes (-)

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J index for size classes (-)

J mill filling – fraction mill volume occupied by ball bed (-)

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L mill length (m)

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Mh hold-up of solids inside the mill (kg)

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Mhb mass of material adhered in the grinding media (kg)

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Mhc hold-up of solids in the mill calculated using the Nomura model (kg)

Mhd mass of material retained in the dead space (kg)

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pi proportion of material contained in size class i (-)

pin,i proportion of material contained in size class i in the feed (-)

pout,i proportion of material contained in size class i in the discharge (-)

si specific breakage rate of material contained in size class i (-)

S1 specific breakage rate constant (-)

T grinding time (s)

Δta mean residence time of balls in the ascending zone (s)

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Δtf mean residence time of balls in the falling zone (s)

Δtfp mean residence time of particles in the falling zone (s)

Δtg mean residence time of balls in the grinding zone (s)

Δtgp mean residence time of particles in the grinding zone (s)

U fraction of ball charge voids filled by bulk of particles in a static mill

(-)

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U0 fraction of ball charge voids filled by bulk of particles in grinding

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zone (-)

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Vm volume of the mill chamber (m3)

Vrb volumetric flow of balls in the circumferential direction of the mill

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(m3/s)

Vrp volumetric flow of particles in the circumferential direction of the

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mill (m3/s)

xi representative size of particles in size class i (mm)

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Greek letters

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φc fraction of critical speed (-)

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µ parameter of Austin´s specific breakage rate model (mm)

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αf ratio of grinding zone particles to total particles charged to mill (-)

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Β breakage function parameter (-)

Γ breakage function parameter (-)

Ψ0 𝑎𝑟𝑐𝑜𝑠(𝑅0 ⁄𝑟) (rad)

Ψ 𝑎𝑟𝑐𝑜𝑠(−𝑟 𝑤𝑟2 ⁄𝑔) (rad)

Φ breakage function parameter (-)

εb fractional porosity of the static grinding load (-)

εb0 fractional porosity of the grinding load in the grinding and ascending

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zones (-)

Θ𝑟 angle of repose (°)

θb0 angle for surface level of grinding zone (rad)

θ1 to θ3 mean residence time of the three mixers (min)

Ρ apparent density of the material (kg/m3)

ωr angular frequency of mill revolution (rad/s)

ξi R0/(D/2) (-)

T

ξs Ras/(D/2) (-)

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Appendix A. Derivation of expressions for Vrb, Δta e Δtg in the Nomura model

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In spite of the thoroughness of the presentation of the model by Nomura [21], the

authors found it important to present in greater detail the key part of the solution procedure

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required to apply it in practice, which is not straightforward to follow in the original

publication. Further, the equations have been reviewed for minor typos in the original

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publication.

Prediction of solids hold-up using the model by Nomura [18] is based on volumetric

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balances, both for the grinding media and material, in the different regions as presented in

Figure 1. The volumetric balance of grinding media and material of a mill in operation is

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given by

𝑉𝑚 𝐽(1 − 𝜀𝑏 ) = (𝑉𝑟𝑏 Δ𝑡𝑔 ) + (𝑉𝑟𝑏 Δ𝑡𝑎 ) + (𝑉𝑟𝑏 Δ𝑡𝑓 ) (A1)

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AC

where Vrb and Vrp are the volumetric flowrates of grinding media and particles which

circulate in the mill, fc is the fraction of the mill occupied by particles and Δt are the mean

residence times for each of these regions. In order to find the dynamic values J0, U0 e εb0 it

is necessary to solve simultaneously Eqs. (A1) and (A2) from the static parameters J, U and

εb. Equations for the three zones in Figure 1 are presented as follows.

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∆𝑡𝑔𝑝 = 𝑉𝑚 𝐽0 𝜀𝑏0 𝑈0 / 𝑉𝑟𝑝 (A4)

𝑉𝑚 (1 − 𝜉𝑖 2 )

𝑉𝑟𝑏 = (1 − 𝜀𝑏0 )𝑤𝑟 ( )[ ] (for 𝜉𝑖 = 𝑅0 ⁄(𝐷⁄2) ) (A5)

𝜋 2

𝑉𝑚 (1 − 𝜉𝑖 2 )

T

𝑉𝑟𝑝 = 𝑈0 𝜀𝑏0 𝑤𝑟 ( ) [ ] (A6)

𝜋 2

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where R0 is the radius of the surface in the grinding zone and wr is the angular velocity of

rotation in and the mill. The parameter J0 is expressed as a function of the geometry in the

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grinding zone, such that AN

𝐽0 = [2𝜃𝑏0 − 𝑠𝑖𝑛(2𝜃𝑏0 )]/ 2𝜋 (A7)

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where θb0 is the angle of the surface level of the grinding zone. It is important to highlight

that cos(θb0) = ξi. The parameters U0 and εb0 are defined according to the amount of

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material in the mill. In the case in which the mill is underloaded (U ≤ 1), the voids filling in

the grinding zone would be given by

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𝑈0 = 𝛼𝑓 𝑓𝑐 / (𝐽0 𝜀𝑏0 ) ≤ 1

{ (A8)

𝜀𝑏0 = 𝜀𝑏

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The fraction of the total of particulate material that is present in the grinding zone

AC

(αf) is given by

𝛼𝑓 = 𝑉𝑟𝑝 ∆𝑡𝑔𝑝 /(𝑉𝑚 𝑓𝑐 ) = ∆𝑡𝑔𝑝 ⁄(∆𝑡𝑔𝑝 + ∆𝑡𝑎𝑝 + ∆𝑡𝑓𝑝 ) (A9)

In case there is overfilling of particles (U > 1), then particles occupy all voids

within the grinding charge, resulting in an expansion of the charge. In this case the

parameters U0 and εb0 will be

𝑈0 = 𝛼𝑓 𝑓𝑐 / (𝐽0 𝜀𝑏0 ) = 1

{ (A10)

𝜀𝑏0 = 𝛼𝑓 𝑓𝑐 / (𝐽0 )

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The volumetric hold-ups of grinding media and particles in the ascending zone of

the charge is given by

𝑉𝑟𝑏 Δ𝑡𝑎 = (1 − 𝜀𝑏 )(𝑉𝑚 ⁄𝜋) 𝐺(𝜉𝑠 ) 𝑓𝑜𝑟 𝜉𝑠 = 𝑅𝑎𝑠 ⁄(𝐷⁄2) (A11)

𝑉𝑟𝑝 Δ𝑡𝑎𝑝 = 𝑈0 (𝑉𝑚 ⁄𝜋) {𝐺(𝜉𝑖 ) − [(1 − 𝜀𝑏 ) 𝐺(𝜉𝑠 )]} (A12)

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where

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1

𝐺(𝜉) = ∫ (Ψ − Ψ0 ) 𝜉 𝑑𝜉

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𝜉

𝑤𝑟2 (A13)

𝑐𝑜𝑠(Ψ) = −𝑟 = − 𝑓𝑤 2 𝜉

𝑔

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{ 𝑐𝑜𝑠(Ψ0 = 𝑅0 𝑟 = 𝜉𝑖 ⁄𝜉 = 2 𝑟⁄(𝐷)

) ⁄ AN

The distance between the surface of the ball layer and the center of the mill in the

ascending zone, Ras or ξs, may also be estimated on the basis of the voids filling value.

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When U ≤ 1, Ras would be equal to R0, and therefore ξi = ξs. Whenever U > 1, grinding

media tend to move towards the wall of the mill, in the ascending zone, during mill

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operation. This would result in segregation of media and particles, so that the porosity of

the layer of grinding media would be equal to a εb. Manipulating Eqs. (A5) and (A11), it

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gives

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AC

With this relationship between ξi and ξs. it is possible to define Δta and Δtap so that

Δ𝑡𝑎𝑝 = {2 𝐺(𝜉𝑠 ) ⁄[𝜀𝑏0 𝑤𝑟 (1 − 𝜉𝑖 )]} {𝐺(𝜉𝑖 ) − [(1 − 𝜀𝑏 ) 𝐺(𝜉𝑠 )]} (A16)

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1⁄

Δ𝑡𝑓 = (2 𝐻𝑎𝑏 ⁄𝑔) 2 (A17)

1⁄

2

Δ𝑡𝑓𝑝 = (2 𝐻𝑎𝑝 ⁄𝑔) (A18)

in which Hab and Hap are the free mean paths of fall of grinding media and particles,

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respectively, which were given by

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𝐻𝑎𝑏 ⁄(𝐷⁄2) = [(1⁄2) 𝑓𝑤 2 (1 + 𝜉𝑖 2 )] + 𝑐𝑜𝑠𝜃𝑏0

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(A19)

(A20)

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− [(1 − 𝜖𝑏0 )⁄𝜀𝑏0 ] {[(1⁄2) 𝑓𝑤 2 (1 + 𝜉𝑖 2 )] + 𝑐𝑜𝑠𝜃𝑏0 }

AN

A detailed analysis of the expressions proposed by Nomura [20, 21] allow to

establish that, of all dynamic variables in the model, that is, J0, U0 and εb0, the only variable

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that represents a challenge in estimating is J0, assuming that the mill is operating under

steady-state conditions. An efficient iterative algorithm that can be used to estimate it is

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Tests used to estimate the RTD distribution in the mill were carried out as part of a

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previous study [24] and are only briefly reviewed here. Experiments were conducted using

manufactured sand rock. Zinc powder (99.9% pure, Merck®) was used as the solid tracer.

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The choice of zinc was due to the fact that this element was not detected in the chemical

analysis of the feed material. The experiment was carried out with the mill operating in

open circuit in steady state with 28% filling of 25 mm steel balls, turning at 75% of the

critical speed, corresponding to 58.7 rpm. Mixed with the feed, introduced at an average

rate of 6.9 kg/h, a total of 120 g of zinc powder were added, with 30 grams added every 15

seconds, as a pulse. In parallel to the addition of the tracer, sampling of the discharge was

started, the entire product being discharged every minute during the two-hour period.

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Measurement of the zinc content of the collected and then quartered samples was

performed by X-ray fluorescence (Shimadzu EDX-720).

It was assumed that the results could be fitted, as is commonly found in practice

[18] by considering three mixers in series with different volumes

𝑡 𝑡 𝑡

𝜃1 (𝜃2 − 𝜃3 )𝑒𝑥𝑝 (− 𝜃 ) + 𝜃3 (𝜃1 − 𝜃2 )𝑒𝑥𝑝 (− 𝜃 ) + 𝜃2 (𝜃3 − 𝜃1 )𝑒𝑥𝑝 (− 𝜃 )

𝐸(𝑡) = 1 3 2 (B1)

(𝜃1 − 𝜃2 )(𝜃1 − 𝜃3 )(𝜃2 − 𝜃3 )

T

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where θ1, θ2 and θ3 are the mean residence times in each of the mixers.

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Results are given in Figure B1, which shows the very good fit of the model to data.

The model was fitted considering the values of the ratio of the three residence times and the

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total residence time in the mill, giving 1/ = 0.07, 2/ = 0.10, 3/ = 0.83.

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References

1. W.J. Whiten, A matrix theory of comminution machines, Chem. Eng. Sci., 29

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(1974) 589-599.

2. J.A. Herbst, D.W. Fuerstenau, Scale-up procedure for continuous grinding mill

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design using population balance models, Int. J. Miner. Proces. 7 (1980) 1-31.

3. L.G. Austin, R.R. Klimpel, P.T. Luckie, Process Engineering of Size Reduction,

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AIME-SME (1984).

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4. L.G. Austin, K. Brame, A comparison of the Bond method for sizing wet tumbling

ball mills with a size-mass balance simulation model, Powder Technol. 34 (1983)

AC

261-274.

using open-circuit wet grinding of phosphate ore as test example, Ind. Eng. Chem.

Res. 26 (1987) 997-1003.

6. J.A. Herbst, Y.C. Lo, Analysis of the performance of large-diameter ball mills at

Boungainville using the population balance approach, Miner. Metal. Process. (1988)

221-226.

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7. L.G. Austin, K. Julianelli, A.S. de Souza, C.L. Schneider, Simulation of web ball

milling of iron ore at Carajas, Brazil, Int. J. Miner. Process. 84 (2007) 157-171.

8. J. Kown, J., Jeong, H. Cho, Simulation and optimization of a two-stage ball mill

grinding circuit of molybdenum ore, Adv. Powder Technol. 27 (2016) 1073-1085.

9. P. Faria, L.M., Tavares, R.K. Rajamani, Population balance model approach to ball

mill optimization in iron ore grinding. In: XXVII Int. Miner. Process. Congr., 2014,

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Santiago, GECAMIN, 2014.

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10. F. Shi, W. Xie, A specific energy-based ball mill model: From batch grinding to

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continuous operation, Miner. Eng. 86 (2016) 66-74.

11. F.K. Mulenga, Sensitivity analysis of Austin’s scale-up model for tumbling ball

mills – Part 1. Effects of batch grinding parameters, Powder Technol. 311 (2017)

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398-407.

12. F.K. Mulenga, Sensitivity analysis of Austin’s scale-up model for tumbling ball

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mills – Part 2. Effects of full-scale milling parameters, Powder Technol. 317 (2017)

6-12.

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batch grinding data for simulation of industrial milling of platinum group minerals

ore, Miner. Eng. 63 (2014) 100-109.

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14. V.K. Gupta, D. Hodouin, M.D. Everell, The influence of pulp composition and feed

rate on holdup weight and mean residence time of solids in grate discharge ball mill

CE

15. S.R.H. Swaroop, D.W. Fuerstenau, A.Z.M. Abouzeid, Flow of particulate solids

AC

16. R. Hogg, Mass Transport models for tumbling ball mills, Control´1984, Society of

Mining Engineers, (Ed. J.A. Herbst), Chapter 7 (1984).

17. P. Songfack, R. Rajamani, Hold-up studies in a pilot scale continuous ball mill:

dynamic variations due to changes in operation variables, Int. J. Miner. Process. 57

(1999) 105-123.

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18. R.P. King, Modeling and Simulation of Mineral Processing Systems, Butterworth-

Heinemann (2001).

19. F. Shi, An overfilling indicator for wet overflow ball mills, Miner. Eng. 95 (2016)

146-154.

20. S. Nomura, Dispersion properties for residence time distributions in tumbling ball

mills, Powder Technol. 222 (2012) 37-51.

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21. S. Nomura, Analysis of Hold-up in continuous ball mills, Powder Technol. 235

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(2013) 443-453.

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22. G.K.P. Barrios, R.M. Carvalho, A. Kwade, L.M. Tavares, Contact parameter

estimation for DEM simulation of iron ore pellet handling, Powder Technol. 248

US

(2013) 84-93.

23. J.A. Nelder, R. Mead, A simplex method for function minimization, Computer

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Journal. 7 (1965) 308–313.

24. A.L. de Oliveira, L.M. Tavares, Simulating a pilot-scale dry ball mill grinding

itabirite using batch grinding data, Proc. 6th Int. Congress on the Science and

M

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Sample F80 (µm)

ρ (g/cm3) µm Θ𝑟 (°)

Iron ore 3.64 177 8.0 31.6

Spent catalyst 2.47 117 0.8 18.6

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AN

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AC

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Materials Spent catalyst Iron ore

Fractional mill filling – J 0.30 0.30

Ball mass (kg) 31.3 31.3

Fraction of critical speed – φc 0.75 0.75

Frequency (rpm) 59.5 59.5

Hold-up (kg) - Mh 1.86 6.11

Void filling fraction – U 0.46 1.04

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AN

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Breakage rate function Breakage distribution function

(Eq. 18) (Eq. 19)

Sample

S1 (min-1) α

γ

Iron ore 3.356 2.395

0.442

Spent catalyst 17.11 2.114

0.533

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AN

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Feed Rate Hold-up

Material mil filling critical speed passing size

J φc (cm3/min) (kg/h) (kg) (μm)

68 6.0 2.68* Na

0.2 0.75 135 12.0 2.86 83

182 16.2 3.32 89

68 6.0 1.65* 79

Spent

0.2 0.30 135 12.0 2.44 93

T

catalyst

182 16.2 3.55 99

IP

67.5 6.0 1.95 72

0.3 0.30 135.0 12.0 2.40* 84

CR

182 16.2 3.05 89

69 9.0 5.51 116

0.2 0.75 137 18.0 6.66* 127

US

188 24.6 7.98 136

69 9.0 4.31 126

0.2 0.30 142 18.6 4.57 140

Iron ore 183 24.0 5.34* 142

AN

69 9.0 5.45 88

0.3 0.75

147 19.2 6.11* 115

69 9.0 4.10* 115

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188 24.6 6.16 138

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* Data used to fit Nomura´s model parameters

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CE

AC

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Fraction of critical speed c1 (s/m) c2 (m) c3 (-)

0.75 334.4 1.00x10-4 1.414

0.30 1595.3 16.3x10-4 0

T

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CR

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AN

M

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AC

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Table 6. Values of relative deviations in 80% passing sizes as a function of mill speed and

simulated scenario

Simulated

Mean Number Mean Number Mean Maximum

conditions

(%) of data (%) of data (%) (%)

Austin model for

three mixers using 4.21 7 7.12 12 6.05 17.4

measured hold-up

T

Austin and Nomura

models for one 3.80 10 8.66 12 6.45 21.1

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perfect mixer

CR

Austin and Nomura

models for three 3.90 10 7.03 12 5.61 17.8

perfect mixers

US

Austin models for

three perfect

5.69 10 6.62 12 6.20 14.9

mixers assuming U

AN

=1

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Modeling and simulation of grinding of spent catalyst and iron ore in pilot dry ball

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mill

Hold-up of continuous mill predicted using Nomura model

Product size predicted using Austin/Nomura models

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Mean relative error of 5.6% for P80 predicted using Austin/Nomura models

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AC

31

Figure 1

Figure 2

Figure 3

Figure 4

Figure 5

Figure 6

Figure 7

Figure 8

Figure 9

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