DOI 10.

1007/s10556-019-00591-z

Chemical and Petroleum Engineering, Vol. 55, Nos. 1–2, May, 2019 (Russian Original Nos. 1–2, January–February, 2019)

CENTRIFUGAL FRACTIONATION OF FINE PARTICLES

E. V. Semenov,1 A. A. Slavyanskii,1 V. A. Karamzin,2 and A. V. Karamzin2 UDC 66.06

The method of fractionation of fine particles of a certain size is substantiated by theoretical and experi-
mental data obtained by analysis of the sedimentation of a finely ground powdered material suspended
in a liquid in a centrifuge. The adequacy of the theoretical and experimental results is confirmed using
the example of the technology of selecting finely ground particles of a particular size from diamond
powder in a liquid separator.

Keywords: fractionation, liquid system, particle dispersion, critical diameter, setting control.

At present, a serious technical problem of introducing powder technologies is the production of powders of
the required dispersion composition [1, 2]. In most cases, powders with high technological or consumer proper-
ties can be obtained only as a result of their separation into classes according to particle size. The processes
of classification (fractionation) consist in dividing the powder into two parts or more according to particle size
relative to the specified boundary sizes, and small amounts of particles of other fractions are permitted in these
products [3, 4]. Fractionation of powders allows to solve tasks such as obtaining dedusted products with a min-
imum content of the fine phase; obtaining small particles with the removal of large particles; separation of mate-
rial into parts (differing in average particle size) with the additional restrictions on the content of fine and coarse
powder components in each fraction.
In [5–8], for efficient and accurate separation of polydisperse substances into fractions, the authors propose
a method of thin-layer centrifugation on specially developed equipment – a liquid plate separator-classifier, us-
ing the methodology for practical implementation of this process. It is noted that for the classification of pow-
dered materials with different physical and chemical properties and particle size distribution, a liquid separator
(with a working volume in the form of a multi-tiered packet of conical inserts) best meets the requirements that
ensure the homogenization of separation conditions and laminarization of the flow of a moving medium.
The disadvantage of the technique presented in [5–8] is that the kinetics of a particle take into account the
stochastic component (due to such features of the process as the mutual influence of particles, fluctuation of
the system’s parametric characteristics, convective currents, Brownian motion), which is inconsistent with the
assumptions made as part of the task (dilution of the suspension, the layered nature of the flow, the order of dis-
persion of the powder, etc.).
The method proposed in [5–8] for calculating the fractionation of finely dispersed materials in a given size
range, taking into account this drawback and complexity, is not suitable for practical use.
A correct calculating apparatus is required for the development of the process of fractionation of powders
(based on the operating parameters of the equipment) that takes into account its features.
We propose a more reasonable (compared to the well-known analogue) algorithm for fractionation of finely
dispersed powder substances based on a plate separator [9–11], where (based on the data on the initial dispersity

1
Moscow State University of Technologies and Management named after K. G Razumovsky (First Cossack University), Russia; e-mail:
sem-post@mail.ru.
2
AGROMASh, Moscow, Russia; e-mail: oooagromash@rambler.ru.

Translated from Khimicheskoe i Neftegazovoe Mashinostroenie, Vol. 55, No. 2, pp. 22−25, February, 2019.

122 0009-2355/19/0102-0122 © 2019 Springer Science+Business Media, LLC

CENTRIFUGAL FRACTIONATION OF FINE PARTICLES 123

of the powder, separation size, values of synthetic process indicators), the main provisions and the procedure for
the practical application of the method of fractionating a crushed suspension are substantiated and formulated.

Justification of Fractionation Methods

Suppose there is a fine powder of spherical particles specified by a particle size distribution in the size
range δ ∈[δ1, δ 4 ]. From this substance, it is required to select a fraction of target particles with a diameter
δ ∈[δ 2 , δ 3 ], (δ1 < δ 2 < δ 3 < δ 4 ), treating the powder as a suspension in a liquid in a settling tank.
In justifying the method of fractionation of powder with a given dispersion, we will proceed from the analy-
sis of the kinetics of an isolated particle in a liquid. Then (according to the concept of the global critical particle
diameter), as a result of implementing the process of separation of the suspended solid, it is (theoretically) al-
ways possible to ensure that the particle size in the target fraction is δ < δ 3 = δ max . At the same time, when
separating the suspension, the presence in the target fraction of particles of size δ > δ 2 = δ min (due to the pres-
ence in the powder of a certain amount of the smallest particles) can be ensured only in suspension recirculation
mode (with a certain error).
Apparently, in the quantitative analysis of the liquid fractionation of the powder, the following conditions
must be fulfilled: suspension must be diluted, densities of the solid ρs and liquid ρ l must be different, the sol-
id phase must be weakly soluble, suspension must be homogenized in solution, etc. When these conditions are
met (according to the proposed method) for evacuation of particles of size δ > δ 3 from the suspension, this
volume of suspension is left to settle for time T3 , corresponding to the sedimentation time of particles of di-
ameter δ 3 , δ 3 = δ cr 3 . If, according to the process conditions, ρs > ρ l , then the resulting sediment with com-
pletely settled phase of large particles δ > δ 3 in it is removed from the settling tank for subsequent treatment
or disposal.
The clarified suspension (supernatant) is further divided according to the time period T2 corresponding to
the settling time of particles with a critical diameter δ = δ 2 = δ cr 2 , in the same volume of liquid (in the same
settler). As a result, all the particles of the target range δ ∈[δ 2 , δ 3 ] and a number of particles of the finer frac-
tion will settle from the clarified suspension. The resulting supernatant is removed from the settler.
If it is required to obtain (with a certain accuracy) a powder from particles strictly classified according to
a given size range, for further evacuation of small particles from the precipitate, a suspension is prepared (from
this sediment and the same volume of water), which is further treated in the same process regime as in the previ-
ous treatment stage.
The described procedure is repeated until a sufficiently small amount of particles not exceeding size δ < δ 2
remains in the suspension – the minimum particle diameter of the given target interval δ ∈[δ 2 , δ 3 ] , after which
the supernatant is dehydrated.
If the results of particle classification are estimated by the content of the smallest particles in the supernatant
at the last stage of the separation process, the number of separation stages should correspond to the inequality

ε1ε 2 … ε n < ζ ,

where ε j is the entrainment coefficient (specific numeric content of particles in the powder with a diameter not
exceeding the critical diameter), j = 1, 2,…, n ; n is the number of stages of separation; ζ is the permissible
relative content of the smallest particles in the supernatant.
Taking into account the calculated values of the coefficients ε j (for a given ζ ), the number of stages
of separation of the mixture is estimated by the iterative approach. If ε 2 ≈ const approximation is made, then
n < log[ζ/ε1 ]/log ε 2 .
124 E. V. SEMENOV, A. A. SLAVYANSKII, V. A. KARAMZIN, AND A. V. KARAMZIN

Fig. 1. Schematic for calculating the process of separating the suspension in a plate separator.

Along with the considered version of the calculation method (where the sedimentation process is first car-
ried out together with the largest particles, after which the sediment is removed (1st stage), and then the superna-
tant is sedimented (2nd stage)), another version of the method is proposed in [9].
For predictions based on the hydrodynamic method of treatment of the powdered material, data are required
on the values of the parameters controlling the process of sedimentation of the solid phase in the suspension.
The following are selected as such treatment parameters: time (period) – in case of non-stationary mode of pro-
cess flow, device productivity (liquid flow rate) – for stationary mode.

Fractionation of Powder in a Plate Separator (PS)

Since the process of separating a suspension in a PS for fractionation of a fine powder suspended in a liquid
proceeds in a stationary mode, we select the flow rate as the process control parameter.
It is assumed that it is necessary to predict the development of the process of fractionation of particles with
a size δ ∈[δ1, δ 4 ] “dissolved” in a dilute liquid system in order to extract target particles with a diameter
δ ∈[δ 2 , δ 3 ], (δ1 < δ 2 < δ 3 < δ 4 ) from the suspension. As an indicator of the process we use the coefficient of
entrainment [12, 13].
In order to clarify the study of the problem of separating the suspension in the PS, we consider the main
working volume – the inter-plate gap (IP) of the separator-clarifier. When analyzing sedimentation of particles
in the IP, it is assumed that the treated suspension of liquid and powder particles is a low-concentration liquid
mixture, and the separator rotor rotates with a constant angular velocity ω. The flow is limited to the region
R1 ≤ r ≤ R2 (where R1 and R2 are the minimum and maximum longitudinal sizes of the plate, r is the lon-
gitudinal coordinate), 0 ≤ z ≤ h (where h is the magnitude of the IP). The flow moves from the periphery to
the axis of rotation of the rotor in piston mode (Fig. 1).
The expression for determining the coefficient of entrainment in the IP has the form [12]

1
n1
ε(q) = = ∫ F(δ cr x ) dx , (1)
n0 0
CENTRIFUGAL FRACTIONATION OF FINE PARTICLES 125

where n0 , n1 (q) is the number of particles in suspension, respectively, at the IP inlet and in the supernatant;
q is the fluid flow rate through the IP; δ cr is the global value of the critical diameter (separation size); x is
the integration variable of the IP expressed in fractions; F(δ) is the numeric distribution function (NDF) of par-
ticles by size such that
n(δ < δ ′ )
F(δ) = , δ1 ≤ δ ≤ δ 4 ,
n0

where n(δ ≤ δ ′ ) is the number of particles smaller than δ ′ ; n0 is the total number of particles in the initial
powder;

δ cr (q) = kq ; (3)

27µ
k= 2
, (4)
πω (R23 – R13 )Δ sin α cos α

where µ is the dynamic viscosity of fluid; Δ = ρs – ρ l > 0 ; α is the half-angle of the plate taper.
Given the variety of physical and mechanical parameters of the process under study, it is advisable to obtain
expressions of the control parameter in the criterial form.
For this, taking into account equations (3), (4), we assume that

27 sin 2 α q ν
d cr = , (5)
π(ξ − 1) cos α ω(R23 − R13 ) ωh 2 sin α

where d cr = δ cr /h is the specific (in IP fractions) global value of the critical diameter; ξ = ρs /ρ l > 1 is the
specific density.
We introduce the notation:

27 sin 2 α q ωh 2 sin α
κ = , Ro = , λ = , (6)
π(ξ − 1) cos α ω(R2 − R13 )
3 ν

where Ro is the Rossby number; λ is the Ekman (Goldin) number.

Taking into account the notation (6), we obtain the expression (5) as a criterial equation

1/2
⎛ κ Ro ⎞
d cr = ⎜ 2 ⎟ ,
⎝ λ ⎠

wherefrom
2 2
d cr λ
Ro = . (7)
κ

In accordance with expression (7), the dimensionless parameter Rо of control over the fractionation pro-
cess (specific productivity of the working cavity) is strongly dependent on the regime separation parameters λ ,
d cr , κ . In particular, fine powders (when the parameter d cr is small) with a small difference in the densi-
ties ρs and ρ l should be separated at low flow rates.
126 E. V. SEMENOV, A. A. SLAVYANSKII, V. A. KARAMZIN, AND A. V. KARAMZIN

Fig. 2. Histograms of the numeric distribution density of particles in the initial powder (1) and after treatment of the suspension (using
a plate separator) – in the supernatant (2).

Experimental Justification of the Fractionation Technique

The adequacy of the results of calculating the fractionation (based on the proposed methodology) of a pow-
der material and results of experiments on the separation of a fraction of particles of a particular size from a giv-
en material was determined by processing diamond powder microparticles in a liquid separator. In the
experiments, the density of the liquid (water) was ρ l = 10 3 kg/m 3 and the density of the solid phase (diamond)
was ρs = 3.5 ⋅10 3 kg/m 3 .
To weaken the coagulation of particles, the liquid mixture with the mass concentration of the solid
phase c0m = 1% was pre-treated by sonication. The volumetric content of diamond particles in the mixture
was c0 = 0.00286.
Statistical analysis of the results of observations was carried out using the Beckman Coulter LS 13 320 par-
ticle sizing analyzer. From experimental observations on the relative frequency of a number of particles (in per-
cent) (Fig. 2), it follows that the raw material (powdered diamond) consists of 0.04–1.0 micron particles.
It was required on the E795-3152 brand separator to obtain a powder from particles with a size range
of 0.04–0.10 microns. At the same time, due to the specific features of the implementation of the centrifugal
separation process of a two-phase liquid system on a separator with phases differing in density, particles of size
δ > 0.10 microns, according to the calculation, are likely to precipitate.
Numeric density and NDF of the initial powder (according to the particle sizing analyzer data) were charac-
terized by the following values of statistical characteristics: mean δ 0 = 0.09; median – 0.085; mode – 0.073
microns. Since the histogram of numeric density is almost symmetric, as follows from Fig. 2, the mean and me-
dian values are about the same. The following time, the average value δ 0 = 0.09 microns was chosen as the
calculated value; based on it, when the volumetric content of the solid phase is c0 = 0.00286, the quantitative
CENTRIFUGAL FRACTIONATION OF FINE PARTICLES 127

content of diamond particles in a unit of suspension volume was determined:

6 ⋅ 0.00286
n0 = = 7.49 ⋅1018 m – 3 .
π(9 ⋅10 – 8 ) 3

The NDF expression, approximated using Excel software and the Regression tool, has the form

F0 (δ) = 37.029δ 3 – 40.064δ 2 + 14.05δ – 0.6 . (8)

Then the coefficient of entrainment was calculated using (1) assuming that in (2) F(δ) = F0 (δ) , and F0 (δ)
was determined from (8).
At the same time, the separator capacity was

N = q(δ cr )(Z − 1) ⋅ 3600 ≈ 130 L/hr,

where selected δ cr = 0.1⋅10 – 6 m and Z = 59 is the number of plates in the separator.

According to the results of suspension separation (see Fig. 2), particle size in the clarified suspension (su-
pernatant) does not exceed 0.1 microns, the average value is δ1 = 0.057 microns, and the median is 0.055 mi-
crons.
The coefficient of entrainment was determined by calculation

1
6
∫ F0 (δ cr ⋅10 x ) dx = 0.278 . (9)
0

Since the numeric relative content of particles in the volume is proportional to the cube of their arithmetic
average, based on the values of the average values in the initial suspension δ 0 = 0.09 ⋅10 −6 m and in the super-
natant δ 0 = 0.057 ⋅10 −6 m, it was concluded that the ratio ε1′ of the number of particles in the supernatant to
the number in the initial suspension can be estimated as ε1′ = δ13 /δ 03 = (57/90) 3 = 0.254. In other words,
the discrepancy between the calculated and experimental values of the number of particles in the initial suspen-
sion and in the supernatant is (ε1 − ε1′ )/ε1 = (0.278 – 0.254)/0.278 = 0.086, or 8.6%. Therefore, in accordance
with the calculation (with an error on the order of 9%), the number of diamond particles per unit volume of the
supernatant was n1 = n0 ⋅ ε1 = 7.49 ⋅1012 ⋅ 0.278 = 2.08 ⋅1012 cm – 3 .
It is apparent in Fig. 2 that the histogram peak is naturally shifted towards the minimum particle size while
the generally symmetrical nature of the frequency distribution with respect to the median is maintained.
Thus, the process of fractionation of polydisperse powder with homogeneous particles can be implemented
by separating the suspension of powder in a liquid in a separator with conical inserts.
For a quantitative analysis of the process of particle fractionation (along with data on the particle size distri-
bution of the powder), it is necessary to take into account the integrated ratios and dispersion characteristics of
the suspension due to the peculiarities of particle kinetics.

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