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Production of Annatto Concentrates in Spouted Beds

- PEQKOPPE, Federal University of Rio de Janeiro, RJ, Brazil
- DEQ, Federal University of Minas Gerais, P.O. 1294, 30.000 - Belo Horizonte, MG, Brazil
- DPO/EQ, Federal University of Rio de Janeiro, RJ, Brazil
AnMttO is composed of a natural reddish-yellow pigment, which is commonly used in thefood, cosmetic and phar-
maceutical industries. This pigment iseasily extracted from Bixa orellanu seeds by particle impact and attrition rather
than by solvent extraction. Seeds must be dried at a safe temperature to preserve thepigment quality. Experiments
show that the annatto powder produced in a non-conventional spouted bedhasa high pigment content and is thus suitable
for commercial use. A comparativeanalysis of thebixin extraction in different systems demonstrates that this spouted
bedunit can becompetitivefor commercial applications. Hydrodynamic and drying parameters werestudied to improve
the powder production ratein this unit.
Lannatto est composedun pigment nature1 jaune-rouge, qui est communkment utilisi dans lindustrie de lalimenta-
tion, des cosmktiques et des produits phannaceutiques. Cepigment est facilement extrait des graines de Bku Orellanu
par Iimpact et Iattrition des particules plutBt que par Iextraction au solvant. Les graines doivent Ctresichkes ?tune
tempkraturepennettant de priserver la qualitk du pigment. Les experiences montrent que la poudredannatto produite
dans un lit jaillissant non conventionnel prtsente uneforte teneur enpigment et quelleconvient 2 uneutilisation com-
merciale. Une analysecomparativedelextraction debixine dans diffkrents systbmes montre quecette unitt de lit jail-
lissant peut Ctrecompktitive pour des applications commerciales. On a 6tudi6 les parambtres hydrodynamiques et de
skhage afin damtliorer letaux deproduction dannatto dans cette unitk.
Keywords: conical spouted bed, particle attrition, annatto production, drying seeds.
ixa orellana is a tropical shrub which grows quickly
B in Brazil, the Caribbean, India, East Africa, etc. Its
seeds are composed of an inner seed with a shelled kernel
containing oils, waxy substances, mineral ash and a
poisonous alkaloid (Dendy, 1966), a peel comprised of cel-
lulose and tannins, and an outer covering containing pig-
ments, moisture, cellulose, sugar and a small amount of oils.
The chief pigment in this outer covering is the red carote-
noid bixin (about 90% of the total pigments). The bixin must
be removed and concentrated to form annatto. Annatto is
widely used for coloring foodstuffs, wax polishes, cosmetic
and pharmaceutical products. The bixin is preferred to syn-
thetic pigments due to its lack of toxicity. Annatto is avail-
able in powders, pastes and oil or alkaline solutions.
The popular technique to obtain this pigment is organic
solvent extraction (Dendy , 1966). A high transportation cost
for untreated seeds and a low percent (2 to 4%) of useful
pigment extracted from the seed are the main reasons for
reducing the applicability of this technique in Brazil. As a
result, B. orellana seeds normally are exported. A search
for a practical technique to produce annatto concentrates
becomes economically interesting nowadays, because of
increasing regulation of the use of synthetic additives in food
As shown by GuimarIes et al. (1989), the bixin can be
extracted from dried seeds by particle impact and attrition.
This technique involves the use of simple equipment suitable
to be installed at the plantation. This allows a low operation
cost for annatto production. To apply this technique, seeds
must be dried at a low temperature to preserve the pigment
quality. As pointed out by McKeown and Mark (1962), the
bixin undergoes a complex series of isomerization and degra-
dation reactions at high temperature, resulting in a yellow
product with a little pigmentary value.
A high particle attrition rate and a safe seed drying tem-
perature can be simultaneously achieved in a single spouted
bed unit. The main objective of this work is to identify the
~. _ _ _ ~_
*To whomcorrespondence may be addressed
appropriate hydrodynamic and drying operation parameters
for producing annatto concentrates in a conical spouted bed.
A draft-tube is also inserted in this unit in order to reduce
the pressure drop and the air flowrate at minimum spouting.
To analyze the applicability of this proposed system, a
comparative study of the bixin extraction efficiency in
different mechanical systems is developed.
Experimental program
Figure 1 shows a schematic of the experimental spouted
bed unit. The spouted bed (SB) column with 60 conical base
was made of galvanized iron. An acrylic window in the cylin-
drical section allowed observation of the spouting regime
operation. A standard 2 Sch. 40 pipe (i.e. =5.25 cm) was
used as the inlet nozzle.
Air flowrates were measured by a pitot tube connected to
a water manometer. Static taps located at the inlet nozzle
pipe and at the bed top recorded the total pressure drop and
the spouting pressure drop. These taps were also connected
to water manometers.
The draft-tube used was 5.25 cm diameter by 50 cmlong,
adjustable at three entrainment lengths (0.06, 0.08 and
0.11 m).
B. orellana seed properties are described in Table 1. Phys-
ical properties were measured following the procedures
presented by Barreto et al. (1989). The initial moisture con-
tent (m,) was determined by weighing samples dried over
24 h in an oven at 105C. The correlations proposed by
Becker (see Passos, 1991) were used to determine the seed
solid density at m,. The seed bixin content (cb) was deter-
mined by spectrophotometric methods following extraction
using chloroform as the solvent (Guimariies, 1988). Seed A
was composed of different B. orellana species from several
SB column
spect ro-
photometer concent rat e <
a 0
L u
m m
0. 4
cont r ol E pv-
t herio I pressure
con t ro 1
l-, top
vo I ve
u p i l o t tube
heat er t herwcoup I es
b l o w
Figure 1 - Schematic of experimental apparatus. (All dimensions
in mm).
Seed Characterization
Measured value
seed A seed B (%)
d,, (mm) 3.32 3.21 1
E, , q ( -)
0.45 0.44 3
P, (kg/m3) 1310* 1310* 1
4 (-) 0.64 0.79 1-3
q, (kg waterikg dried seeds) 0.150 0.165 3-4
ch (%)
2.03 1.25
*at m =0.08 (kg water/kg dried seeds)
plantations in Rio de J aneiro. Seed B was from a single plan-
tation also located in Rio de J aneiro. Both seeds had an
irregular pyramidal shape. The thickness of their outer
covering was between 0.07 to 0.1 mm (Electronic Micro-
scope, Cambridge - 250MK3).
The minimum spouting conditions were determined
from pressure drop vs. air flowrate curves obtained at
different bed heights (0.20 <H <0.40 m). The blower
(IBRAM - ER6) limited the experiments to H <0.30 m in
beds without a draft-tube (NDT beds). The ambient air tem-
perature and relative humidity were, respectively, 22C and
65%. The inlet air temperature (TG,) was maintained at
Solids circulation rates (& were measured following the
technique proposed by Muir et al. (1990). A conical sepa-
rator collected the solids emerging from the spout top over
a given time. This separator was located few centimeters
above the spout or draft-tube top.
Annatto powder rates ( I!'p) were determined from the
amount of collected powder vs. operating time curves. The
time elapsed for starting-up the system was calculated to be
one hour. The bixin recovery was estimated by measuring
the powder bixin content (chp) and comparing this with the
seed bixin content (q,).
Each experiment was replicated at least twice. The mean
experimental errors were, respeccvely, 3%, 4.5% and less
than 3% for AP vs. V; curves, M and
The following procedure has been established to determine
the maximum drying temperature (T,,,) above which the
l a
0 10 20 30 40
Figure 2 - Spouting pressure drop vs. inlet spouting air veloclty
curve in beds of seed B for decreasing the air flowrate. No draft
tube. H =0.28 m.
bixin thermal degradation occurs: ( I ) collect the amount of
powder produced during the spouting operation performed
at ambient temperature; (2) sample the powder fraction with
size distribution lower than 100 standard Tyler mesh;
(3) measure chp of these samples; (4) dry each sample in the
oven over 24 h at a constant temperature (40 to l0OOC). The
powder temperature is supposed to be equal to the oven tem-
perature after 24 h; (5) measure cl,,, of each dried sample:
(6) determine TM from the powder bixin content vs. drying
temperature curve assuming 5% as the maximum permis-
sible variation of Ch9.
Batch drying experiments were also carried out in the con-
ical SB unit to specify the time required to dry the seeds.
The mass of seeds used (M) varied from 10 to 12.5 kg.
Ambient air flowrate was fixed at 0.066 m3/s with
40 <TGi <120C. Samples collected each 10 minutes
were used to determine the seed temperature and the moisture
content as a function of the drying time. The seed tempera-
ture was measured following the procedure described by
Becker and Sallans (1961).
Experimental results and discussion
A typical AP vs. V; curve obtained i n NDT beds by
decreasing the air flowrate is illustrated in Figure 2. This
curve can be divided into three regions based on the flow
regimes observed: a stable spouting with well defined foun-
tain, annulus and spout regions (Vi >V,, - I .5 Y,,,,,,); an
unstable spouting characterized by large pressure fluctuations
(Vi,,,, <V; <Vis.v); a fixed bed regime characterized by the
decrease of the spouting pressure drop with the reduction
of air flowrates (Vi <V,,n,$).
Pham (1983) and Passos (1991) have reported a similar
unstable regime at minimum spouting. The internal spout-
jet discontinuously breaks the bed surface, resulting in
pressure fluctuations. The annulus, fountain and spout
regions are not well formed, and solids circulate around
the internal spout cavity. Such an instability retards the
traditional spouting regime. Passos (1991) suggests that
this instability is characteristic of the SB systems with a
low inlet jet momentum. Both the low sphericity of the
B. orelluna seeds and the high inlet nozzle diameter used
_J z
curve I
c1 /,
c n
L 1 I L L
<*> 0 1 -
LL /' 8
"' 0 6 . '
. .
0 70 0.25 0.30 0.35 0.40
BED HEIGHT - H ( n )
I' ,
. .
0.70 0.25 0.30 0.35 0.40
BED HEIGHT - H ( n )
contribute to reduce the inlet air jet momentum at minimum
spouting .
obtained are presented in
Figures 3a and 3b, as a function of H. The effect of bed height
on these parameters has been analyzed by PovrenoviC et al.
(1987). These authors developed a semi-theoretical model
to predict the minimum spouting conditions in conical beds
of spherical particles. Charbel (1992) modified this model
by introducing the effect of particle sphericity in the equa-
tions proposed by PovrenoviC et al. (1987). The predicted
curves (APlns vs. H and vi m, vs. H ) obtained from this
modified model are also plotted in Figures 3a and 3b.
As seen in Figure 3a, this model can predict quite well
AP,,, vs. H data. However, it underestimates the V,,n,, vs.
H data (Figure 3b). This disagreement between the predicted
and experimental data should be related to the inlet fluid-jet
characteristics. PovrenoviC et al. (1987) have assumed that
the fluid velocity in the top of the spout at minimum spouting
is equal to the minimum fluidization velocity. However, this
velocity should behigher than the minimum fluidization one
The values of AP,, and
Minimum Spouting in Conical Beds with Draft-tubes
(Seed B)
L,. =0.06 m
M H v,,,, AP,,,, v,,,,, AP,,,,
(kg) (m) Ws) (Pa) (in/\) (Pa)
10.0 0.28 12.0 302 13.9 359
15.0 0. 33 12.8 331 16.3 406
20.0 0.36 12.8 354 16.3 434
L, =0.08 I l l
in SB systems with a low inlet jet momentum, as suggested
by the results of Epstein and Chandnani (1987). The best
equation for predicting V;,,,s vs. H data is that of Wan-
Fyong et al. (1969) (Mathur and Epstein, 1974). as shown
in Figure 3b.
The experimental values of AP,,, and V,,,,, obtained in
beds with a draft-tube are presented in Table 2 . A compar-
ison between these data and those predicted in Figure 3
. . . . . . . . . . . . . . . . . . . . . . .
AP, , , , =kl APtIlsINDT ( 1 )
V,,,,/L, =k2 Vlnr~NDT . . . . . . . . . . . . . . . . . . . . . . . . . . ( 2 )
with k l =0.43 and k2 =0.66 for L , =0.06 m; k , =0.52
and k2 =0.82 for L, =0.08 m.
Equations (1) and (2) are in agreement with the results of
Claflin and Fane (1984). As pointed out by these authors,
minimum spouting is reached at lower pressure drop and air
flowrate due to the reduction of the amount of fluid flowing
from the spout to the annulus with the insertion of the
The experiments show a considerable reduction of the total
pressure drop (up to 40%) when a draft-tube i s inserted. This
pressure drop is required to operate the unit. and it includes
mainly the frictional loss for nozzle enlargement and top con-
traction, the cyclone and the spouting pressure. Therefore,
the use of a draft-tube assures lower investment and opera-
tion costs for the blower for producing annatto concentrates.
Solids circulation rates (& obtained in beds with a draft-
tube are presgnted in Figure 4, as a function of V, , L,, and
H. Data of M in NDT beds are too few to be plotted in
Figure 4. As mentioned earlier, the blower power capacity
limited these experiments to H <0.30, m and V, - V, , , .
However, for H =0.28 m, the value of Mobtained is almost
constant (= 0.47 kgi s) in the range of 35.6 5 V, 5
42.6 m/s.
From Figure 4, it %an beinferrsd that the effect of draft-
tubes is to decrease M (0.09 <M <0.3 kg/s). The effect
of bed height on solids circulation seems negligible in the
range of 0.23 5 H 5 0.39 m.
Muir et al. (1990) developed a very elucidative analysis
about the effect of draft-tubes on solids circulation. They have
shown that the spout-jet expazsion at the draft-tube inlet
affects decisively the value of M. The solids circulation rates
increases, passes through a ma5imum and then decreases as
Vi increases. The maximum M occurs when thc spout-jet
diameter equals to draft-tube diameter. The solids motion
at the draft-tube entrance is characterized by fluctuations of
the solids inflow to the jet and by the formation of particle
Annatto Powder Production in Conical Beds with Draft-tube
(Seed A)
0.01 1
19.5 24.5 29.5 34. 5 39.5
Figure4 - Solids circulation rates vs. inlet spouting air velocity
curves in beds of seed B with draft tube.
fl 10 20 30 40
Figure5 - Annatto powder production vs. operation timecurves
in beds of seeds A.
Curves 1 , 2 and 3: 6 =33.4 m/s, L, =0.06 m and H =0.23;
0.30 and 0.39 m, respectively. Curve 4: V, =33.4 m/s, L, =
0.08 m and H =0.40 m. Curve5: V, =29.3 m/s, L, =0.11 m
andH =0.40 m.
clusters. The intensive motion at the draft-tube entrance can
improve the impact and attrition between the seeds and the
draft-tube wall. Therefore, an increased production should
occur in beds with a draft-tube.
To analyze the powder production mechanism in beds with
a draft-tube, Wp vs. t is plotted in Figure 5 as a function of
H and L, . (Seed A had to be used in these experiments due
to the large amount of seed required). As shown in Figure 5,
the initial period of producing annatto powder is character-
ized by a constant value of kp (=dWp /&). This initial
period extends up to Wp - 50 g/kg, where kp changes to
a lower value.
Upon decreasing L,, kp increases, at least for the initial
period. From Figures 4 and 5, it can be inferred that be$
with a draft-tube of L, =0.06 m should present a low M,
but a high kp. Experiments confinnoan increase of 15% in
kP against a reduction of 53% in M, when the draft-tube
has been inserted into the bed at L, =0.06 m. The inten-
sive solids motion at the draft-tube entrance is presumed to
bethe main reason for this result. A reduction of L, causes:
(a) the draft-tube entrance to be closer to the inlet solids
M H " i L, % t
(kg) (m) (m/s) (m) (g/kg . h) (h)
25.0 0.40 29.3 0.11 2.6 6 - 15
25.0 0.40 33.4 0.08 3.9 6 - 12
23.5 0.39 33.4 0.06 6.1 3 - 8
12.5 0.30 33.4 0.06 12.4 2 - 5
6.0 0.23 33.4 0.06 26.4 I - 2.5
Bixin Recovery in the Conical Spouted Bed Unit
(Seed A)
~~ ~~
6.0 0.06 30 164 11.0 89
12.5 0.06 30 118 12.4 72
23.5 0.06 30 90 15.7 70
25.0 0.08 30 92 14.8 67
25.0 0.11 30 64 18.3 58
entrainment region; (b) the amount of inlet air to be larger
in the draft-tube entrance. Both should contribute to improve
the particle-wall impact and attrition. Experiments are in
progress in a half conical column to analyze the effect of
the draft-tube and spout-jet dimensions on the particle-wall
From Table 3, it is seen that kp increases monotonically
with the reduction of H (or M) at the initial powder produc-
tion period. This behavior can be explained by the decreay
of the average particle cycle time as Hi s reduced. Since M
does not vary with H for a given L,, the average particle
cycle time (= M/M) is directly proportional to M or H. There-
fore, in a given time interval, more powder is produced as
there are more particle passes through the draft-tube inlet.
These results also suggest the use of internal solid baffles
and/or inert rigid particles to improve the particle-wall
impact and attrition. However, caution is needed to prevent
particle grinding and breakage.
The annatto production and the bixin recovery results
obtained at 30 hours of spouting operation in beds with a
draft-tube are presented in Table 4. The first observation is
about the high level of the bixin recovery obtained, mainly
with L, =0.06 m. Measurements of cbp in the four
different size fractions of the powder produced indicate the
following distribution:
Particle size cbp (%o)
(Tyler standard sieve)
+48 mesh 6.1 fine size
-48 +65 mesh
-65 +100 mesh ::::I ultrafine size
-100 mesh 20.2 ( cbp =16.1%).
("+" =greater than or equal to, "-" =lower than).
Annatto Production in Different Equipment
(Seed A)
n Lu
2 4 -
D a
~~ ~~~
Mill'b' 25.0 - 35 65 23.9 77
50.0 - 35 42 22.2 46
(120 L; 12.5 6.25 10 97 14.5 69
0.7 s-I) 21.0 10.50 10 74 14.4 53
Lab. 0.500 0.732 2 21 11.4 12
Mill"' 0.500 0.732 3 41 8.7 18
(1 L; 0.500 1.027 3 83 7.7 31
1.2 s-I) 0.335 1.540 2 215 5.4 57*
(a) porcelain balls with diameter =2 cm.
(b) "Metalin Indlistria de MBquinas Ltda.", J aragua do Sul,
(c) "Chiarotti", MauB, Sfio Paulo, Brazil.
*seed grinding.
Santa Catarina, Brazil.
The commercial annatto powder concentrate (Meer Cor-
poration, 1980) has a cbp between 8 to 12%, with 97% of
fines lower than 60 mesh. These data assure a possible com-
mercialization of the ultrafine annatto powder produced in
the unit proposed. A sample of the powder produced here
has been used to color cheeses by a Brazilian butter and
cheese producer. The results obtained are excellent, sur-
passing the annatto powder color quality used in that specific
The results obtained by Barreto et al. (1989) in other
mechanical systems suitable to perform the bixin extraction
are summarized in Table 5. The ball mill equipment is com-
petitive with the SB unit. The operating time to produce the
same amount of annatto powder at the same bixin recovery
is one-third that of the conical bed with L, =0.06 m.
Although the ball mill equipment seems more attractive, the
powder must be safely dried in other equipment; the conical
SB unit can perform both processes, the safe seed drying
and the mechanical bixin extraction. The powder obtained
in the SB unit has a lower moisture content (- 0.06) and is
ready for storage.
The maximum temperature to dry B. orellanu seeds
without loosing the bixin pigment quality is 60"C, as shown
in Figure 6.
The preliminary data from the batch drying operation in
the conical beds show that m varies linearly with the drying
time form, I m I 0.75 m, and 40 <TGi <120C. One
hour is the time required to reduce m to 0.75 m,. The
maximum TGi to assure a safe seed drying operation is
Experiments are in development to identify the effect of
TGi on the amount and size of the powder produced in the
unit with draft-tube.
The conical spouted bed unit with a draft-tube can well
perform mechanical bixin extraction from Bixu orellanu
seeds, especially when Le =0.06 m and 0.23 I H
5 0.30 m. The use of a draft-tube assures a good
hydrodynamic operation, a low blower power requirement
30 45 60 15 90 I05
Figure 6 - Powder drying temperaturevs. bixin content curve
(Seed B).
Operation Conditions for the Conical Spouted Bed Unit
Geometric parameters
L, (m) 0.06
H (m) (or M =6 kg) 0.23
Air flowrate (m3/s) 0.07
Hydrodynamic parameters*
Total pressure drop (Pa) 4,400
Drying parameters
TGI ("(3 60- 114
Drying time (h) 2 - 1
Bed Temperature ("C) 5 60
Final moisturecontent 0.75 ni,,
*reference: ambient air.
and a high annatto powder production rate. The mechanism
of powder production in these beds seems to be governed
by the characteristics of the spout formation in the inlet nozzle
region. A low draft-tube entrainment length and a low bed
height lead to a large annatto powder production rate. The
powder bixin content and the bixin recovery are high, and
permit commercialization of the proposed conical spouted
bed with draft-tube process.
The minimum spouting parameters required to operate the
unit are specified as a function of draft-tube entrainment
lengths and bed heights. For L, =0.06 m and 0.23 I H
I 0.30 m, 9.5 I Vim, I 12.2 m/s; 263 I APmr I
318 Pa and the blower power less than 0.3 kW.
The maximum seed temperature for preserving the bixin
pigment and the maximum air inlet temperature for one hour
of drying seeds are also determined as being 60 and 114"C,
The appropriate hydrodynamic and drying operation
parameters obtained here for producing annatto concentrates
in the proposed conical SB unit are summarized in Table 6.
Under these conditions, the annatto powder production rate
is expected to increase (up to 1.5 of the powder production
rate obtained at 40C) due to the reduction of the seed
moisture content.
=seed bixin content (kg bixin/kg wet seed)
=powder bixin content (kg bixinikg wet powder)
=volume-equivalent particle diameter (mor mm)
=expanded bed height (m)
k , and k, =constants in Equations (I ) and (2) (-)
=draft-tube entrainment length (m)
=seed moisture content - dry basis (kg water/kg
=initial seed moisture content - dry basis (kg
=mass holdup (kg)
=solids circulation rate (kg/s)
=no draft tube
=spouted bed
=time (h or min)
=temperature (C)
=inlet spouting air temperature (C)
=maximum temperature for drying seeds (C)
=inlet spouting air velocity, based on the inlet
=inlet minimum spouting air velocity (m/s)
=inlet stable spouting air velocity (m/s)
=amount of powder produced/amount of seed
=rate of powder produced/amount of seed processed
dried seed)
waterlkg dried seed)
nozzle area (m/s)
processed (g/kg)
Wkg h)
Greek letters
h Z /
P, =solid density (kg/m3)
4 =particle sphericity (-)
=spout pressure drop (Pa)
=minimum spouting pressure drop (Pa)
=void fraction at minimum fluidization or minimum
spouting (-)
Barreto, D. W. , L. M. J aeger and G. Massarani, Production of
Bixin Concentrates, in Proceedings of XVII Meeting of Flow
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PovrenoviC, D. S. , DZ. E. HadiismajloviC, Z. B. GrbavtiC, D. V.
VukoviC and H. Littman, Minimum Fluid Flowrate. Pressure
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(1984), pp. 137-141.
Manuscript received October I , 1991; revised manuscript
received J une 12, 1992; accepted for publication J une 16. 1992.