2 Sproy drying techniques for food ingredient encopsulolion

I lntroduclion to sproy drying

A¡r heat¡ng system

I.I INTRODUCTION

"7'lr prccess of simultqneously cuoni:ing tuttl clesic'c.ating.fiuid a¡d soli¿l substances, and its tppli<'trtiort
to the pwpose oJ the exhtustioil ofuoísturc fiom su<'lt ntbstar(es, atrl.for lhe preyent¡ofi of.lesm«fh,e
chc»úcal clwtge."
Samuel R. Percy (1872)

'I-he above words are excerpts frorn the first ever detailed description of ar drying technique,
which is now well-known and appreciated as "Spray Drying". Spray drying is a 140 years
young and flourislring drying techrique. Tlroughout all these yea's, this perpetual prccess has
exhibited ari ebullient grcs'th, imbibing innumerable innovations ir telms of its operational
design and widely varied applications.
Spray drying lras its origin in the United States, since the first patented design was registered
there in 1872. World War II was a significant chonological event in the history of spray drying,
rnonopolizing the process in the dairy industries lbr continuous production of rnilk powder.
Since then, the process has adapted ítself to a nunrber of design nrodiñcations, and today has
evolved as an industry-friendly drying technique. Spray drying stands out from other processes
involving liquid drying by its ability to handle f'eedstock ofvarying nature, producing flowiug
ptiwders of specific particle size, high productivity and versatile applications.
By definition. "Spray drying is the translonntrtiott of JZetl .fionr o fluitl snte into u drietl
particulote fonn b¡'spraf ing tlrc feed into a hot drying ntedium." (Masters. 1991)
A spray drver operates on corivection mode. The principle of working is moisture removal
by application of heat l.o the feed product and controlling the humidity of the drying medium.
Here, the uniqueness is tlr{t the evaporatior of moisru¡e is promoted by spraying the léed into a
heated atmospher.e, resulting in improved drying rate. The mechanism can be better understood,
wllen the spray drying process is divided into its constituent unit operati.ons.
A liquid feed entering the spray dryer undergoes it series oftranstbnnations before it becornes
powder The changes are due to the inlluence of each of the four stages (Figure l. I ) involved in
spray drying, namely:
1. Atumizalion of the lccd sululion.
2. Confact ofspray with the hot gas.
3. Evaporation of moisture.
4. Particle separation.
Spttt Dn ing IirLhnitltes lbr Food lngredicnt Encapsulation, Fi.rst Edirioo. C. Allandliara¡nakishnal
and Pudma [shwaya S.
O 201 5 John Wiicy & Sons, Ltd. Publishcd 201 5 by John irviicy & Sons, Ltd.
FigureLI Processstepso[sproydrying.(l]Atomizotion.(2)Sproy-hotoirconioct.{3)Evoporotionof
moisture. {41 Product seporotion.
Each of the above exe¡ts influence on rhe Iinal product quality. Understanding the process
steps, al.ong with lhe hardware systerns involved in it, will enable visualization ofthe operation
on a glinpse of a reading. Hence. subsequent sections will narr¿rte in det¿ril each of the above-
mentioned uuit operations, with a description of the associated lialdw¿ue conlponents.
1.2 STAGE l: ATOMIZATION
Ator¡ization is the lieart ol spray drying, and is the first transfonnatioll process that the teed
undergoes during spray drying. Although several deltnitions of atonrization exist, one of tl¡e
initial defrnitions of the process, by Samuel Percy, is as interesting as it is precise: "bring,ing fluid
or sLtlül substonces into a stote of minute divisiott". The breakup of butk liquid into a large
number ofdroplets drives the rest ofthe spray drying process by teducing the intetnal rcsistances
to moisture ü;uisf'er tlom tlie droplet to the sr.trrounding medium. This is because of the enor-
mous iucrease in surtace area of the bulk fluid as the droplet ñssion proceeds, with its instability
increasing in accordance with the intensity of atomization.
A:omization is central to the spray drying process, owing to its influence on shape,
struc.rrre, r,elocity and size distribution ofthe droplets and, in turn, Ihe particle size and
nature of the final product. A cubic meter of liquid tbnns approxinately 2 x l0rr unifoll
100 rnicron-sized droplets, offering a total surface area ofover 60,000 m'¿(Masters,2002)
This sreater surface-to-volume ratio enablcs spray drying to achieve a faster drying rate (as
dryir g time is proportional to the square of the particle dimensiol). Consequeutly, there is
mini nal Ioss of heat sensitive compounds and, eventually, particles of the desired morphology
and,rl; ysical chxracteristics are obtained.
l
 lntroduction io sproy drying 3 4 Sproy drying lechniques for food ingredient encopsulotion

I.2.1 Principle of otomizqtion Where D is the droplet diameter, which can be obtained as:

The working principle of the atomizers is governed by the liquid disintegation pluromenon
explained by several researchers- It is worth understandirry the progression in the co[cepts on atom-
ization phenomenon across the years. This will also help in appreciating the science of droplet
forrnation fiom an atomizer.
Joseph Plateau was the first to characterize iiquid instability in 1873, tlrough his experimental
observations. A liquid jet, initially of constant radius, falls vertically under gravity. The liquid
length inüeases and reaches a critical value. At this critical value, the jet loses its cylindrical
shape and decomposes into a stream of droplets that occuls primarily due to decrease ilr suúáce
tension (Figure 1.2).
Lord Rayleigtr, in 1 878, coroborated the above stated theory tmd gave an malytical explanation
of the physical obse¡vation: He provided a mathematical insight to the break-up of nou-viscous
liquid under lamina¡ flow conditions, now famously known as tJ.,r- "Liquil jer theorv'. Rayleigh
considered the simple situation of a laminarjet issuing from a circular orifice, and postulated the
growth of small distulbances that produce bleakup when the fastest growing disturbance attains a
wavelength (i.e. ,1.r, of 4.51d, where d is the initial jet diilneter). After heakup, the cylinder of
length 4.5 1d becorires a spherical drop (Figure 1.3) and. hence. can be approximated to a sphere of
equal voiume (Equation 1.1).
4.5td^(L\d, =f.¿]r,
(4./ l.6i
D =1.89¿l (t.2)
Although Rayleigh's analysis considered surface tension and inertial forces, the influence of vis-
cosity, atomization gas and the surrounding nir were neglected. The above gaps in knowledge
were addressed by the work ofWeber (1931) and Ohnesorge (1936). Weber revealed that the aü
friction shofens the oplimum wavelenglh (,l"rr) for drop formaÚon. He obtained a value of,1"o, =
4.44i ¡t zero relative velocity, which is close'to the value of J.51d predicted by Rayleigh for this
case- Weber showed that as the relative velocity increases to 15 r/s, ,loo, becomes 2.8d and the
droplet diameter is I .6¡,L Thus, the increase in relative velociry between the liquid jet and ihe sur-
rouruling air reduces the optimum wavelength forjet breakup and results in a smaller droplet size.
The explanation given by Ohnesorge in 1936 on the mechanism of atomization is credited for
its cldrity. The relationship proposed by him included all the significant factors responsible for
atomization. He proposed üe Reynolds number relationship, and expressed the tendency of the
liquidjet to disintegrate in tems of its viscosity, density, surface tension andjet size. The relation-
ship c:rn be numerically expressed by the dimeusionless Ohnesorge number (Oh) which is the
rafio ofWeber number to Reynolds number (Equation 1.3), as described by fhe equation below:
oh:{il" :-L= Viscous forces
(1.3)
(1.1) Ite ,l pot l(hrerriu
x surfitce tensiott)
where:
W¿ is the Weber number;
Re is the Reynolds number;
p, p and o arc the viscosity, density and surface tension of the feed droplet, respectively;
I
is the characteristic dimension of the feed droplet (i.e. volume per unit area).

Constant radius Disintegration of the liquid at the periphery or tip of the atomizel is by virtue of the turbu-
lence in the emerging liquid jet and the actior of air forces; the l€sistance to disintegration is
Growth of perturbat¡ons offered by viscosity and sudace tension tbrces in the Iiquid. The realignment of shear stresses
Cr¡tical length within the liquid, once the droplet is airborne, contributes to the droplet fission during
Droplet atomization.

1.2.2 Clo¡sificoiion of olomizers

The atomization device is vital to this process, and its selection plays a majol role in utilizing
spray drying as an economical drying method. Prior to exploring the mechanism and working
of the atomizers, understanding the rationale for their classification holds significance. The
atomizers are dillerentiated on the basis of the criteria listed in Table 1.1. The major types
include rotary atomizers and noz:le atomi?Brs. The working principle of different types of
Figure I.2 Schemotic o[ liquid ¡nstobil¡ty (Modif¡ed from Wu el o/., 2014)
atomizers is elaborated subsequently.

1.2..? 1 Rotary otomizers

Principle: Driven by high velocity discharge ofliquid ñom the edge ofa wheel or disc (Figure 1.4).
Feed l,quid is centrifugally accelerated at high velocity to drc cenhe of a rotating wheel wiür a
),opr
peripi:ral velocity of 200 r¡/s. The outward flowing feed with resPect to the lotating wheel sudace
Figure I.3 Mechonism of droplet formoiion {Adopted from Wu et ol.,2Q14l accel,mtes to the periphery and then disintegrates into a spray of droplets'
 lntroduction to sproy drying 5 ó Sproy dryinq iechniques for food ingredient encopsulotion

Toble l.l Rotionolefor olomizerclossificoiion.
Bocis of otomizer clqssification
Energy utilized for olomizolion.
Desired type of sproy.
Required finol size ronge of droplets.
Advantages: The major advantages ofrotary atomizers are that they do not clog, and they tend
to produce more uniformly sized droplets. Since t}te necessary atomization energy is supplied
Quonrifying poromeler by the rotating wheel, the feed supply unit can operate at low pressure than that required in
Cenirifugol, pressure, kinelic, sonic or el«kicol energy. hydraulic and pneumatic nozzle atomizers.
Fine, medium or coorse,
Men droplet size in pm or nm.
Limifations: Rotary atomizers present difficulties i-n handling viscous feed. The lÍuge amount

The relotionship between meon size of droplets
qnd olom¡zotion poromeiers.
Physicol properlies of lhe feed thot con be
hondled by the otomizer.
Copociiy of feed thot the otomizer con hondle.
Need for duplicotion of otomizers.
Direi or inverse relolionship of the mmn droplet size with
qlom¡zqtion pressure or otomizer speed of rolotion,
diometer or eleckic poteniiol ocross the chorged nozle
Viscosity ond obrosiveness of ihe feed.
Feed rote in ml/min or L,/h.
The rótio of increose in the otom¡zer copocity to the
number of qtomizers linked in series,
of fine particles produced can potentially lead to environmental pollution. Furthermore, it is not
possible to accommodate the spray produced by rotary atomizer in a horizontal spray dryer.
1.2.).2 Pressure nozzle (or hydraulic) otomízer
Principle: Facilitated by discharge of liquid under pressure drough an onfice (Figure 1.5).
Pressgre energy is convefied to kinetic energy, aud feed emerging liorn the nozzle orifice as a
high rpeed film readily breaks into a spray of droplets.
Atornization energ¡i: Pressure energy.
Atomization parameters: Nozzle pressure.

ODeratins Dressure ranse: 250-10.000 PSl. ,

Type of spray: Coarse and less homogeneous.

Mean ilroplet size: 120-250 pm.
Driving
motor

Atomizer dr¡ve cas¡ng

Feed¡ng tube

Figure 1.4 Rotqryqlomizer (Muroli ef o1,,2014).

Alomization ener€y: Centritugal energy.

Atomization parameters: Wheel speed in rotation per minute (RPM).

Type of spray: Fine, cou se or meüum.
Mean droplet size: 30-120 prn.
Relationship between mean droplet size (d) and atomization parameters: d is directly
proportional to feed ¡ate and feed viscosit¡ and inversely proportional to wheel speed and
wheel diameter

Physical property of feed: Demorshates ability to handle abrasive lbed-stocks by virtue oI

atomizer vanes and bushings.

Atomizer duplication: Rótary atomizers are l«rowD for their ability to handle high feed rates
without atomizer duplication. Figuré 1.5 Pressurenozzle
 lntroduction lo sproy drying 7 8 Sproy drying techniques for food ingredient encopsulotion

Relationship between mean droplet size (d) and atomization parameters: d is directly Relationship between mean droplet size (d) and atomization parameters: d is directly
proportional to feed rate and viscosity, and inversely related to atomization pressu.re. propofional to feed rale and viscosity and inversely related to atomization pressure.
Physical property of feed: Low viscosity t'eed. Physical property of feed: Can handle highly viscous t'eed.

Atomizer duplication: Prcssure nozzles can be integrated in multiple nozzle arrangements to
obtain ¿n inc¡eased amourt of flow rate and particle size flexibility.
Advantages: Pressure nozzles result in particles with less occluded air when compaled to twin
fluid atomizers. Consequently, the powdered product is of higher density, with good flow char
acteistics. Depending on the specifications of the end product, it is also capable of producing
particles with relatively greater size.
Atomizer duplication: Rather than atomizer duplication, more than one atomization fluid is
employed to transmits the kinetic energy to the feed. The use of fbur fluid nozzles is the latest
advancement (Niwa et al,, Z0l0).
Advantages: Twin fluid nozzles are capable of handling lúglrly viscous feed. These atomizers
also produce much finer and morc homogeneous spray when compared to plessure nozzles.
These nozzles exert better control over the droplet size.

Limitations: At high feed rates, sprays are generally less homogeneous and coarser than rotary Limitation: The requirement of compressed air adds to the cost of operation. TWin fluid noz-
atomizer'-s. zles result in high occluded air content within the particles, resulting in low density. The use
of thr:se nozzles also introduces extra cold air into the spray chamber in the zone of atomiza-
tio[ and, hence, reduces the temperature gradient that exists between the finely divided
1.2.2.3 TwoJluid nozzle otomizer
dropi.e,t and the surrounding drying medium. This impairs the effecúveness of heat transfer
Principle: The operational principle is based on Weber's findings, as explained in section 1.2. l. betweun the droplet and hot drying medium. Twin fluid nozzles exhibit a higher tendency to
Two-fluid atomizers featurc the break-up of liquid on impact with high-velocity air or other clog. especially when the liquid t'eed is of mucilaginous or fib¡ous nature. A further disadvan-
gaseous flow. Cornpressed air crcates a shear field, which atomizes the liquid and produces a tage of tlris type of liquid-gas nozzle is the "downstr¿ant furbLtlence" which causes the fine
wide range ofdroplet sizes (Figure 1.6). particles to be c¿rried away to the atmosphere by the large gas flows used. This phenomenon
has been termed as "overspray"i it tends to contaminate the atmospherc which is in close
Atomization energy: Kinetic energy.
proximity to the nozzle, and demands expensive cleanup and tedious maintenance procedures
Atomization parameters: Nozzle pressure. (Sewe11, 1987).

Operating pressure range: 250-10,000 PSI With the rotary and nozzle atomizers dominating in dreir spray applications and association with
lab scaie and commercial spray dryers, it is also inportant to understand the working principle
§pe of spray: Mediurn coarseness but poor homogeneity
of other rypes of atonúzets: sonic and electrohydrndynamic atomizels. With the continuous
Mean droplet sizer 30-150 pm. advancements in this field, the future spray üying teclnology might be dominated by the use of
these atomizers.

1.2.2.4 Uhrosonic otomizers

Ultrasonic atomization relies on an electromechanical device that vibrates at a very high
fiequency. Two piezoelectric disks, tightened between a mechanical amplifying element and
a support element, constitutes the electromechanical device of the ulüasonic atomizer. The
fluid to be atomized initially passes over the surface of the vibrating piezoelectric disks,
whieh sets ultrasonic vibrations within the liquid. The vibrations within the liquid cause
molecules on the surface of the liquid to move about, disrupting the surface tension of the
liquid. This creates areas on the surface of the liquid with reduced or no surface tension,
which are very similar to holes in a sieve, and through which droplets of rhe liquid can
escape (Loser', 2002t Pyo er al., 2006; Fukumoto er al., 2006). After bypassing the piezo-
electric discs, the fluid passes tlx'ough arr amplifier, the tip of which is a resonant surface.
On reaching the active resonant surlhce" a thin liquid lilm is lbrmed. As the liet¡uency of
vibration approach the resonance tiequency, a square wave pattern tbrms onto the liquid
surface. Further increase in the anplitude of vibration causes the droplet tbrmation and its
detact:mert from the liquid film (Figure 1.7).
Ar the pressure energy does for the pneumatic and hydraulic nozzle atomizers, it is
FiEure I.ó {o) Twefluid nozzle; {b) Sproy emerging lrom iwo-fluid nozle fhe rczzle vibration frequency which aids the &oplet lission in ultrasonic atomizers. In
 lnlroduction to sproy drying 9 fO Sproy dryinq techniques for food ingredient encopsulolion

Piez@lectric disks

Polymer solution

Figure 1.7 Uhrqsonic olomi2er {Dobre ond Bolle, 2002).

addition to the vibration frequency, amplitude and the area of vibrating surface also play a
role in ultrasonic atomization (Lixin et a1.,2O04).
In contrast to conventional pressure nozzle atomizers, which impart a high initial velocity to
wu Monod¡sperse
drcplets
High voltage
DC supply

the droplets, resulting in wider droplet distribution, the velocity of droplets emerging from the crounded collector plale
ultrasonic atomizer is one to iwo orders of magnitude smaller than the fome¡. This is found to II
result in more uniform droplet size distribuúon (Lixin et a1.,2004). Consequendy, the shorter
residence tirne of the unifonn droplets generated by the ultrasonic nozzie results in higher reten- Figurel.S Mechqnismofelectrosproying.{BhushoniondAnondhoromokrishnon,2Ql4.Reproduced
tion of the active components plesent in feed (Semyonov et al.,20ll). The low velocity spray with permission of Elsevier).

also allows the spray drying chamber to be designed with shorter dimensions, thus enabling the
ultrasonic atomizer system to be installed in a laminar flow cabinet or isolator (Freitas et ul.,
2004). Furthermore, in an ultrasonic atomizer, the feed droplet outlet is larger, with no moving
pafts, and this arrangement sen'es to prevent clogging (Semyonov et a1.,2011) and facilitales
easy maintenance and operation.
Because of the properties described above, ultrasonic atornizers have been effectively used
for the drying of plobiotic cells (Semyonov et al., 20ll), in ordel to obtain higher viability.
However, ultrason.ic atomization technology is effective only for low-viscosity Newtonian
fluids. Since reduced pressure acts as the driving lbrce fbr moisture evaporation lrom the atom-
ized droplets, use ofthe ultrasonic spray head demands large quantities of hot air. Nevertheless,
the use of sterile ¿urd l.rot drying medium would render this method appropdate for aseptic
manufaeturing of spray dried particles (Dalnoro et al., 2Ol2).

1.2.2.5 Electrohydrodynomic otomizers

A recent teclmique for atomizing the feed liquid is the use of electrospray or elecrohydrody-
neunic sprays created by electrostatic charging. The mechanism has its roots in the Rayleigh's
theory ofimtability and Taylor's theory. In the electrospra¡ electricai potential is applied to the
needle to introducc fiee charge at the liquid surtáce. The high intensity of electric cunent
applied between the two oppositely charged electrodes of an electrospray system enables the
production of droplets of nanow particle size distribulion. When the electrical potential rises to
kilovolts, the liquid meniscus develops into a conical shape (Taylor cone), having a highly con-
centmted free charge. The free charge accelerates the droplets away from the needle due to the
generated electric stress. Monodispersed particles will be fonned when the jet breaks into fine
particles due to varicose instabilities (Figures 1.8 and 1.9).
Figuré 1.9 A visuol of the sproy emerging from on eleckohydrodynom¡c otomizer

'I
 lntroduclion to sproy drying tl l2 Sproy dryinq techniques for food ingredient encopsulotion

The relationslúp between droplet size and conductivity is given by the Equation 1.4, after In this anangemenl, the atomized droplets entering the dryer are ir contact with the hot inlet
being confirmed by many experiments (Jaworek, 2007): air, but theüJemperature is kept low due to a high rate of evaporation taking place and is
imatelyatthewet-bulFtempéiá-tffi WFFullitém@i[reisthethtffiTte.nergy air used
tbr evaporation { i.e.. the removal of-ia-i
a,=o(Q"'P)". (1.4)
\tToy ) -.--
i3-iéiñEiIa-§-tvaoorative cooling". This allows the particle to be maintained at a temperature
below the out-liltemperatuleiTihe drying air'.) The cold air, in tum, pneumatically conveys the
where: dried particles through the system. The contact time of the hot air with the spray droplets is -o-nly
dn is the droplet size; a fe*;econd*, during whcñ dryin li.
dme of particles, with the added
O is the llow ¡ate;
eo is the pemittivity of vacuum; - merit of less themal degradaúon of heat sensitive products.
p, o and y te the density, conductivity and surface tension of the feed liquid, respectively; In contrmt. iD tle counter-current configumÚoD (Fipure l-10(b)). the product and dryirrg
¿ is a constant which is generally equated to 2.9. medium enter at ttre offiSfiéÉñffii the dliing ct amuei. Here, the outlet prortuct tempelature
is higher than üe exhaust ail temperature, and is almost at the f-eed air temperature, with which
Requirement of solvents for feed preparation and extremely low flow rates limit the usage of it is in contact. This type of arangement is used only for healresistant products. z
electrospray atomization for food applications and commercial exploitation respectively. In irnother type. called mrxed llow, the dryer design incorporniF56[li'iffiuÍent l1ow and
coullt€r-current flow. This type of arrailgement is used for drying coarse free-flowing powde¡
but tlrD drawback is the higher exit temperature of the product. The criteria for spray dryet
1.3 STAGE 2: SPRAY-AIR CONTACT design selection are summarized in Box l. l.

This stage, and the subsequent process steps of spray drying, constitute the parricle formation
phase. With the bulk feed atomized inlo tiny droplets, the next step is to bring the droplets into
intimate contact with the hot gas. This enables rapid evaporation of moisture from the surface Box l.I Ten guidelines on lhe choice of sprqy drying
of all the droplets in a uniform manner. Here, the critical requilement is uniform gas flow to all process Porqmeler§
palts of the drying chamber'.
l. The inlet temperature must be as high as possible in order to achieve a final product
f)uring spray-air contact, the droplets usually meet hot air in the spraying chamber, either in with low rcsidual moisture and a higher thermal efficiency (choice of inlet temperature
co-ctrrent tlow orcounter-cmenlUow@g!fl9(Figure 1.10(a)), the product and drying shoríiáf iñGliiññi1he heat señsiE-vii!6f-iE-EE[óomponents to prevent ürema]
medium passes tlrough the dryer in the same di¡ection. deg¡adation).
p 2- Increasing the feed flow rate lowers the outlet temperature and thus íncreases the
(a) (b) ' temperature difference between fhe inlet temperature and the outlet temperature. This
results in product with higher residual moisture content.
/ 3. High asp.irator speed leads to higher degree of separation in the cycJone.
4. Lower aspirator speed leads to lower residual moisture content. /
-5- The hisher the leed flow mte- lhe lrser is thc size of the Da-rticles iu the lrnal Droducl.
6. I he hlgher [he leed conceltratron, the greatel rs the morslur€ conlent of the parhcles
aM, hence, the greater the possibiüty ofagglomeration and the occurrence ofirregular
particle shapes.
7. The drying air temperature should be below the glass transition temperature in order
to prevent product collapse and stickiness in the spray chamber.
8 . The 7 of the feed material can be made higher for a convenient spray drying operation

by the addition of high moleculal weiglrt components such as maltodexüin.

9. Thepercentageofwatercontentillüefeedisalsoasignificantparameterincontrollirg
the I, since water depresses Z considerably.
10. A shorter residence úme (RI) (1G-15 sec) is recommended for fine particles containhg
an ample amount offree surface moisture contelt, enabling easy evaporation-A medium
RT (25-35 sec) should be applied for fine to semicoarse sprays that needs to be dried
to low residual moisture content. A longer RT is needed for drying coarser sprays in
orde¡ to achieve lower residual moisfwe content.
Figure I.IO Sproy dryer configurotions: (o) co-current (lefi); {b} countercurrent kightl (Ookley, 2004
Reproduced wilh perm¡ssion of Elsevier).
 lnlroduction to sproy drying l3 I4 Sproy drying lechniques for Íood ingredient encopsulotion

An air disperser to ensure unifbrm gas llow, and an appropriately designed drying chambe¡
al'e the importaDt hardu,aLe elements associated with this step. The function of an air disperser is
to create pressure drop by means ofperfbrared plates or vaned channels, through rvhich the gas
is directed to facilitate equilized flow in all directions of the spray drying charnber. The air dis-
perser is normally placed in the roof of tlre dlying chamber, adjacent to the atomizer The dryirg
chiunber usuiLlly h¿s a conic¿¡l bottorn, witlr its height to diameter ratio (aspect ratio) dctermined by
the end applications. The ditt'erent types o1'drying chambers re discussed ir later sectio¡rs. Figure l.I2 A diogrommotic represenlotion of the droplei drying process (Modified from Chorlesworth
ond Morsholl, l9ó0; Wolton ond Mumford, 1999).

I.4 STAGE 3: EVAPORATION OF MOISTURE Wet-bulb temperature ({,,,) is the temperature that the drying gas rerches when it is saturated
with vapor from the liquid (Seydel at r1., 2006). Also, the droplet slrinks due to the evaporation
The most critical step in particle Iorn.)ation, this process step is associated with the moryhology of lhe aqucous phasc { Figure I . ] 2, stcp 1 ),
oI the linal product. Ev:rpoiation ofmoisture during spray drying can be visualized as two stages: The quantitication of evaporation rate at this stdge can be understt¡od by the "rf law" (Law
and Law, 1982). THs is based on the flrct that, during the constant rate period, the evaporiltion
(i) cc¡nstant rate period; and of a liquid droplet of diameter d is proporrional to its surface area. B¡sed on this lilw is the
Peclet nurnber (Pe) relationship given by the er¡uation below (Equation 1.5). With this equation,
tiil firlling rate period.
Peclet number is depicted as the m¿rin controlling palalieter of the droplet drying ptocess and,
hencc, the prticle fbr¡nation (Hu¿ng,20l l):
Examining the drying kinetics of thc spray drying process is critical in predicting the heat il1d
mass transfer in the drying material. This cau be lrest explained by a mathematical model for the
e\rapolalion of a single droplet which is subjected to convective drying in a spray dryer
{: o".c (i.5)
Ar
(Figure 1.8). Initially, when the droplet is exposed to hot gas, rapid evaporatior) takes place.
During this exposure, the dloplet is heated from its initial temperature (20) to the terlpelaturc of where:
equilibrium evaporation tempel?tul€ ({r) (Figure 1. I l, AB). During this period, the removal of C ls the concen[¿rtion of thc solute on weight by weight basis;
moistur€ fbllows the u)nstant rate period of the ú'ying rate curve as the moisture is removed r is the droplet radius;
corrstantly from the surtáce of the droplet keeping it sufhciently cool. The droplet suúhce P¿ is the Peclet number, which is the rertio of evaporation rate to difl'usion rate (Equation 1.6).
remains saturated with moisture at tlis stage antl its temperature is constant at the wet-bulb
temperature (Figure 1.1 1, BC: Doliusky, 2001). P, =LD ( 1.6)

wherc:
K is the evaporation rate;
D is the diffusion rate.

As the tnoisture rernoval tiom the droplet proceeds, the solute dissolved in Lhe liquid reaches a
concentration beyond its saturation concentration and tend to fbrm a thin shell at the droplet
sur1rce described :.s"trutsl.forntation" (step 2, Figure 1.12).
o The comencing o1'crust tbnnation event is an imporlart kinetic characteristic of the spray
E
drying process as it transforms from low to high temperature tlrying. After tlre crust formation,
c tlre moisture remov¿rl turns into a di.ffusiort-controlled process, and the evaporation rtte is
V o
dependelt upon the rate of water vapor dilTnsion through the dried surface shell (Figure 1.12.
-q step 3; Farid, 2003). This consti.tutes the.fhlling roÍe peñod. During the thlling rate period,
e although the particle will begin to lieat (Figure I . t l, CD). it is ahlost at the coolest part of tlie
o
dryer, where the drying gzrs is at or near the outlet tempelature of the dryer. Consequently, the
piu'ticles ae never heated above the outlet temperature of the dryer, despite the lact that the inlet
temperaturc may be considerably higher. The final dried powder will be at a temperature
approxirnately 20'C lower than the air outlet temperature (Gohel ¿¡ «1., 2009).
Time An irteresting phenomenon that luppens during the falling rate peiod is "bubble Jbnnntion"
(Figure l.12, step 4, and Figure 1. t3). When dre parlial pressure ofmoisture vapot at the droplet cenre
Figure l.l ITemperoture history during sproy drying of o liquid droplel {Hondscomb et al., 2OO9
Reproduced with permissioñ of Elsevierj. exceeds albient pressure, it results in bubble fbnnation and a subsequent increase in temperature.
 lntroduclion io sproy drying l5 16 Sproy drying techniques for food ingredient encopsulotion

Oullet gas

))*.e@ Tangential duct type inlet for

particle laden gas from spray ,---

dryer outlet
[4.'r;i¡s.: .i
B,l.;i:4§ÍBñ
w7
-
-
Dry'ns @e"*,۟l&*ffi lnner vorlex

FQurel.l3 Schemoticdiogromofthebubbleinflotionphenomenonduringsproydrying(Erzel etol., 199ó).

A cor.rsiderable amount of energy is required for üis vaporization, which halB üe sensible heating
(Figure 1.I I, DE). The dropiet inflates to the outer radius md finally results in irregular randomly Outer voftex Conical bottom
shaped particles (Figure l. 13; EEel cI a/., 1996). As lnentioned above, a crust is formed as the rnois-
ture content decreases, and the droplet temperahr¡e ultimately rises towards the dry-bulb temperatue
of the air (Figure 1. I l, EF). The varied morphologies of the spray dried particles resulting fiom üe
bubble inflation phenofirenon axe discussed in detail ir ¡he forthcoming section.

1.5 STAGE 4: PARTICLE §EPARATION

Two systems are emp§ed in separating the product trom the drying medium: the ptimary and Outlet for dr¡ed product
secondary separation. Note üat the spray drying chamber often has a conical bottom to lácilitate
the easy collection of the dried powder. Duing the prinary separation, the dry powder is collected
Figure I.t4 A lypicol cycloneseporotor (Utikor elol., 2010. Reproduced with permission of lnlech)

at the base of the dryer, followed by removal using a screw conveyor or a pneuñaúc system with
a cyclone separator at tlre time of seco[dary separation. The gas stream loaded with the evaporated
moisture is drawn from the centre of the cone above the conical bottom and is discharged through
a side oudet. The relatively low efficiency of collection necessitates the use of an additional par-
ticle collection system, compdsing dry collectors followed by wet scrubbeN. The dry collectors
include a cycloue sepa['ator, a bag filter and an e]ectrostatic p[ecipitator, depending on tlrc size of
the particles carried away by the exhaust gzu and the final product specitications.

1.5.I Cyclone seporotor

A cyclone separato¡, otlell integrated with a.sp¡'ay dryer, is a stationary mechanical device that
utilizes centrilugal lbrce to separate the solid pirticles liom a carrier gas (Figure 1.14). It cou-
sists of an upper cylindrical part, rel'erred to as the barrel, and a lower conical part, referred to
as the cone. The gas stream, loaded with sotd panicles, leaving the spray dryer enters tangen-
tially at the top of the barel and travels downward into the cone, forming an outer voftex. The
inoeasing air velocity in the outer voltex exerts a centritugal fbrce on üe particles, separating
them iiom the gas stream. When drc gas stream rcaches the bottom oflhe cone, an i¡ner vortex
is created, thus reversing its direction and exitilg out at the top as clean gas. The particulates Figure ¡.15 Schemotic of sproy dryer with bog filter llindelov ond Wohlberg, 2009. Reproduced with
permission ofJournol on Physics).
fall into the collection chamber attached to the bottom of the cyclone.

1.5.2 Bog filter
The bag filter (Figure l. 15) comprises a metallic housing desigued for continuous operation and
automatic cleaning. The particleJaden air enters unde¡ suction or pressure through the collector in
the cenuE or bottom pafi (i,e. the hopper) of üe bag ñltu-. The air', with particles, uavels through
the ñlter bag, which retains the product panicles on ils surface. The clean air passes out through
bags and plenum to the outlet ofbag filt'el'. Accumulation of dust on bags causes an increase in the
diiTerential pressure across the filter bags. Compressed air is pulsed by a timer-actuated series of
normally closed pulse valves at preset intervals, causing the valves to open- The compressed air is
stored in a reservoir located beside the higher filter chamber. Above each row of bags there is a
tube with holes that are aligned with the central air passage gap, located on 1op of the bags.
 lntroduciion to sproy drying l7 I 8 Sproy dryinq techniques {or food ingredient encopsulqtion

Morphology is one delicate aspect of spray drying wlich makes it versirtile as well as intricate
Flow direction The lireranrre shows it is possible to alter the moryhology of spray dried particles by optimizing
@ the process patameters. At the same tirne, quantitying and assessing the process variables

Negatively charged
?r influencing rlorphology is ditlicult. due to tlie cornplex interactions between the variables and
unique drying pattems of differcnt materials subjected to spray drying. In the case of spray
partic¡e
drying, the interaction l¡etween vriables such as in]et and outlet temperatue, flow rate of
drying gas, the f'eed properties constituting its concertration, solute dilfusion coefticient and
solvent latent heatJ govern the tinal particle rnorphology.
Drying kinetics is central to the understanding of particle rnorphology (Vehring, 2008). The
Cylindrical particle
collecting electrode impact of different dryirg partems on rhe producr rnorphology is depicted in Figure l. t 7. The
(anode) crust fonnation stage is central to the particle fbrmaúon during spray drying. Follou'ing the
cmst formation, the &oplet may fbllow one of the two ptincipal pathways, leading either to
small, sotid particles or large, hollow ptuticles. The first is the "dry.rl¿¿ll" route, whÍch is similar'
to a sluinking core, producing pafiicles which zre susceptible to shattering when dried at lrigh
tempernture. The second route is the "w¿t shell" type, which tends to tblm hollow p;x.ticles
.: which may inllate wlien subjected to higher drying temperature. Thus, the lnolpllology of the
spray drie<l particles also depends on rhe narure of the shell formed (Handscomb c¡ a1..2009).
It is also apparent tiorn the illustration that the drying temperature and solid content of the feed
","?i,?l#ii",113[r solution or suspension ilt the key factors in deciding the particle r.norphology.
Figurel.ló Schemotico[lheworkingprincipleo[eleciroslolicprec¡p¡toior{Leeelol.,20ll). Tlr. scope of further discussion is intended to plovide an insight to the plausible rnorpholog-
ical patterns of spr.ay dr.ied products, and the impact of major influential spray drying parameters
on th: below.
though which complessed air is injected to invert the gas f]ow momentarily. This causes the
particulate material accumulated outside the bags to be removed. .,¡¡ a j\
1.5.3 Electrostoiic precip¡totor No parlicle Shanered Solid particte /
formatron part;c¡e W
t :
Electrostatic precipitation is a method of particle collection in spray drying that uses 1 I j+\ collapse
electrostatic force. An electrostntic precipitator (ESP) cornprises of discharge wircs and col- LowsotidslAp4{t
lectilg plates (Figure 1.1ó). A trigh voltage is applietl to tlre discharge wires to lbrm an concentratnn, Htgh \¡7 -#
¡
electrical field between rhe wires anrl the collecting platc's. This high voltage ionizes the air <t iowtw tetnpetature
around the discharge wires to supply ions. As the drying air that contains the product parti- t ,rr, "n"ln-'lt''t'on I
cles flows between the collecting plates and the dischalge wircs, the particles in the gas are ,ffi. - a¿+-. -i
-:- \^/
\
^. /
charged by the ions. Tlie Coulomb fblce cau§ed by the electric tield causes the charged par-
ticles to bl¡ collected on tlie collectirg plates and the air is purified. The particles collected
on the collecting plates are removed by rapping the collecting plates, scraping off with a
brush or washing off with water, and removiug from a hopper. Furtlier discussion on ESP
@-@-ffir-"*^@_-
lnit¡al droplet Saturated
dry¡ng
surface Crust formation lnternal bubb¡e Uninflaled shell

@
nucleal¡on
will be provided in Chapter 8.
The selection ofparticle separation equipment is governed by various thctors such as collection
efticiency, suitability for product handling, operaúonal t'eatures, cost ¿rnd space requilenrent.

()t\()
I
*
-^
I.ó MORPHOTOGY OF SPRAY DRIED PARTICIES
\-/
\_-/ \)
Paticle morpholo-ly is an indicative signal which inlluences the decision on spray drying pro- Blisteredparticle Shrivelledparticle lnflated'pl:tfed'
cess parameters. Morpholo-uy aff'ects the key quality characteristics ofspray dried products such
as particle size distribution, i-lowability, friabitity, moisture content and bulk and particle density.
t¡gurel.I7 Differentmorphologiesduetobubbleinflotionduringsproydrying{Hondscombetol,2009
Hence, it is yital to understand the variables which decide the morphology, and the lrequently Reproduced with permission of Elsevier).
occuning rnorphology patterns in dte spray dried products.
 lntroduclion lo dr t9 20 Sproy dryinq lechniques for food ingredient encopsulotion

l.ó.1 Skin-forming morphology with hollow iniernol slruclure

A smooth skin-iomring morphology (Figure 1.19(a)) can be described as a particle composed
of a continuous nonJiquid phase üat is polymeric or sub-microcrystalline in n¿ture. The skin-
forming behavior is the result of solid precipitation which covers the droplet, entrapping the
bulk of the droplet liquid inside. It is known that larger Peclet numbers result in an enlargement
of the solute at the surface, which likely leads to shell or skin fornadon.
From Equation 1.6, at large Peclet numbers, the evaporation rate of the solute at the sudace
proceeds at a fastel rate when compared to the diffusioml motion of the dissolved molecules.
Thc high evaporation rate, in tulrr, results in the rapid build-up of solute concentralion at the
sufface. This leads to a local increase in viscositl,, with subsequent skiu o¡ shell formation. In
addition, the skin formation can also be promoted by the presence of surface active molecules
th¿t may accurnulate at the surface and fom a surface layer. The skin formation is impofant in
maintaining the particle shape (Vehring et al., 2007). It is also significant in the retention of
volatile cornpounds during the spray drying prccess (Hassan ¿r rL, 1996). The thster the rale of
skin formation, the bettff the retention of sensitive compounds during splay drying.
The hollow intemal structue of spray dried particles occuls as a lesult of substartially high
evaporation rate experienced by small molecules with high solubility (ex. saccharides). Hollow
particles also result f¡orn high drying gas temperatures of 200"C at the inlet and 90'C at the
outlet, which corresponds to a Peclet number range of approxirnately 2 5 (Elversson zr a/.,
2003). The fate of the hollow particle depends on the thickness and rnechanical propenies of the
skin surounding it. Accordingly, it may eventually collapse or wrinkle.
The impact of drying a¡ temperature on the fbmration of lrollow inter-nal structures can be
best explained with ret'elence to a study on the morphological differences of spray dried malto-
dextrinparticlesproducedundertwodift'erentconditionsofinlet/outlettemperatures: llO"/14"C
and 20U"/173"C (Alamilla-Beltran. 2005). With an understanding ol the d'? /arv discussed in the
previous section, the diil'erence in morphology of the spray dried maltodextrin pafiicles c¿n be
explained in tenns of the Peclet nurnber concept (Figure L 18). At a low inlet-outlet tempelan¡re
combination, P¿ is low due to lower evaporation rate at a higher dilfusion rate, resulting in Figurel.l9 Differentmorphologypotternsofsproydriedporticles.{o)Smoothsurfoce{b)Blow-holeformotion
smaller, solid particles. By contrast, at the higller inlet-outlet temperature combination, Pe is {cl Agglomerote {d) Denfed surfoce. From: {b ond d) Roiom ef oi., 201 2. Reproduced
wilh permission of Elsevier;
higlier', resulting in lager, hollow paticles. Furtbemole, it is observed that there is no recog- {o ond cf Ezhilorosi et ol., 2Q13. Reproduced with permission of .lohn Wiley & Sons.
nizable particle fbmation with f'eed of less solid content.
It is difficult to predict at what solid corcertration the particle formation becornes prominent
during the spray drying process. However, an increase in feed corcentration results in a padicle
which is resistanl to disruption, bubble inflation and eventual collapse. Therefore, on an
industrial scale, a pre-concentration step such as evaporation always precedes spray drying in
order to feed an optimally concentlated solution to the spray dyer. This also enables efticient
utilization of the limited thermal efiiciency of a convective drying plocess such as spray drying.
Anothe¡ commonly encountered llarure in spray dried p¿xticle moryhology is the tbmation of
non-spherical, elongated particlcs. The shape delbnnation is mainly due to incomplete arorÍtjza-
tion, when the action of the viscous fo¡ces and surface tension on the bulk liquid to spiit it into
droplets is not sufEcient enough. Skin-fonning materials are prone to this type of distortion, due
to their pliability during drying.

1.6.2 Blow-hole formotion

Figure I.I 8 Difference in porticle morphology due lo di{ferent Peclet number os influenced by different Blowhole formation is a feature which is typical of spray dried pa.rticles (Figure 1.19(b)). Blow-
inlet/outlet temperoture combinqtions. {o) Peclet No. = 0.7. (b) Peclet No. = 2.1 (Alomillo-Bellron et al., holes are primarily due to the penneable nature ofthe particle, which allows the flow ofwater, water
2005. Reproduced w¡th permissioñ o{ Elsevier).
vapor and dissolved gases from the inte¡ior of the particle to its sruface with ninirnal resistance.
 lnlroduciion lo sproy drying 2l
Lrge particles dried at gas temperaturcs abo\e tlle k)ihng point of the water may inflate after shell
fomatiol. due to build-up of intemal gas pressure. potentrally causing shell rupture or "blow-holes"
in the shells (Walton and Mumf'ord, 1999).
The fbm.ration of structurally rigid panicle shell is favored by rapid drying and high particle
mobility.'fhis evert occurs befble the piúicles in the interior ofthe tlroplet come into contact with
each other. Hele. the dryhg rate is decreased, as the lou,permeability of the shell hinders the
liquid florv to the surface. Evertually, the rigid shell structue leads to the formation of hollow
granules that visually appe:us like craters or "blow- holes", lbnned by an inwarcl collapse of the
shell. The inwnrd collapse can be explained by the formation of a partial vacuum due to the
capillarity-induced movement ofpanicles lion the intedor to the surface shell (Oberacker, 20 l2).
l.ó.3 Agglomerote
Structurally, an agglomerate can be detined as a p¿fiicle composed of individual grains of
material bound together by sub-micron dust or a binder (Figure 1.1 9(c)). Agglomeration between
tlie paÍicles inside the spray drying churber occurs as a result of ¿idhesion (solid link between
the particles) and collision tbrces betrveen them. The collision within the spray ch¿mber can
occur between two liquid droplets, or between a liquid drop and an already dried pnticle, or bet-
ween two dry parricles. Tlie collision can also be between üróre th¿rn tu,o dry parricles. The adhe-
sion depends upon the tbrce of impact and contlrct time between the colliding prticles. The
relati\,e speed ofparticles and the particle nrass de'cide the irnpact o1'adhesior.
The agglomeration also depends upon the nature of particle surflce. cornprising of its cornpo-
sition, viscosity, temperature and water activity, all of which change during dre spray drying
process. As the droplets of the feed solution undergo drying, the water activity of the droplet
surthce decreases while its ternperature increases. The viscosity of'drop suúace also continues to
increase until it reaclres a critical value Q¡.), which is elluivalent to I 07 Pa.s. This critical viscosity
is associ¿ted u,ith stickiness, which eventually leads to tlre tbrmation of viscous bridges between
the particles to fbrm agglomerate. 4, is also related to the glass transition temperature or sticki-
ncss tenlperalurr'. whÍch is c'xplaincd in scction 1.8..1.
In addition, the solubility ofthe material to be dried in waLc'r is also an intluencing firctor on
spray dried pafiicle agglomeration. Generally, insoluble and sparingly soluble solids in the t'eed
result in agglornerates. To a certain extent. agglomeration is beneficial in 'instant', products, such
as instant coff¡e. for achieving better wettability and dispersibility in water. Llowever, excessive
aggkmeration may result in llow diltculties and severc caking problerns (Barbosa-Cánovas
et al.,2005).
1.6.4 Formoiion of denied slructure qnd presence of smqll
port¡cles within lorge porticles
It is also interesting to leam about some unusual morplrological pattems that ae encountercd durilg
spr ay drying ofsorne tbod componerts. One is cap-shaped, slightly dented structLnes (Figure l. I 9(d)),
ruldtheotheristhepresenceof srnallparticleswitlrrlargeparticles(Figurc l.l9(c)),whichareusu-
ally noticed in spray dried coll'ee. The phenomenon of smaller particles inside luger particles cam be
due to the en[y of lomer into the latter tlrough blowlioles, or it may possibly occu'where m¿u'ly
snraller pru'ticles conbine to lbrm luge puticles durirg dryilg.
The lbrmation ofdcntcd oI cap-shapcd stluctures is artributctl to scvcral catrscs b¡'di1]clent
works published in this contcxt. Crosby antl Marshall (19-58) ascertain that the cap-shaped
particles result tiom capillary action of the dried p¿lrticle surtilces drau ing the litluid and solids
22 Sproy dryinq techniques for tood ingredient encopsu¡olion
outward anrl unilbrml¡, around lhe droplet. This creates sub-atmospheric internal pressures.
whiclr eventually result in the collapse of the particles. It mzry nlso be due to ilcorrect cltoice
of inlet drling air temperaturc and insufticient solid content in the feed solution, resulting in
deficient drying of the t'eed droplets. Consequently, the wet particles irnpact on the walls of the
drying clranrber which, in the course of the process, deforms on impact and collapses to result
in the cap-shaped, dented structures. Yet anotlrer reason is that tlre highcr drying rate l€ads lo
rapid wall solidification prior to expansion of the particles, which tbrnrs a slrong crust on the
palticle surlace and restricts the complete bubble inllation. thus [esulted in caved-in or dented
surfaces (Anandharamak¡ishnan et aI.,2O07)- However, surláce dents result tiom a complex
inter¿rction between several factors, such as the drying r¿rte, ¿rtomization mechanism and
uneven shrinkirge at early stages of drying, viscoelastic properties of the rvall materials and
rapid wall solidification.
Thus, an observation of the particle morphology, along u'ith drying kinetics nay etlable the
experts involved in product developmert to a[ive at optimum process settings to achieve desired
product ploperties and qudity.
1.7 SPRAY-DRYING PROCESS PARAMETERS AND THEIR
INFLUENCE ON PRODUCT QUALITY
It isc¡br,ious lrom the previous sections on the spray drying process steps that spray drying
is a method which strongly and equally depends on marerial properties, equipment design
and sctting of operation par¡meters. The above listed factors inlluence the final product
qualit',,, mainly in terrs of residual rnoisture, particle size and rnorphology. Although the
optimization ofthese variables is usually achieved by a "trial and error" approach, an under'
standi,lg of the basic guidelines of spray drying would result in intelligent operation of the
equilunent. The different spray dryiug process parafiIeters, conesponding to each of thr: four
steps of spray drying, are discussed in the following section. General guidelines lbr deciding
the paramefers lor a spray drying operation and intbrmation related to its impact on product
c¡ualty are also listed.
1.7.1 Atomiz<¡tion porometers
'l'he pt-rlbrnance ol'atomizers depends on three pararneters: the atornizirtion pressure, feed flow
rate, \,iscosity and density. These paranreters have an influence on the droplet size.
L/. 1. 1 Atomtzotton pressure
Witlr the same t),pe olnozzle and leed material, as the atomization ptessrtre is increased, droplet
size decreases according to the relationship below (Equation I .7; Masters, l99l ):
D. /¿ \''
,,=le] (1.7)
Wrere D, and D, are the initial and tinal droplet sizes on changing the irtolniz¿tion pressure
tiorn P, to P", respectively, This is due to the requirement of an efficient delivery of the atom-
ization ener-ey to the bulk liquid to drive droplet fission.
 lntroduclion to sproy drying 23 24 Sproy dryinq techniques for food inqredient encopsulotion

1.7-1.2 Feed flow rote I.8 PARAMETERS OF SPRAY-A¡R CONTACT AND

At constant atomizltion pressure, increasing the flow rate increases the droplet size, since the
nozzle's hydraulic energy has to atomize more liquid. As tlie liquid interaction wirh the
atomization energy is minimal, the dropl¿t tjssion is irsufficient to leduce its size. Feed rate is
¿rssociated with the peristaltic pump speed wlúch feeds to the spray solution to the rotary or
nozzle atomizeL
As the atomization pressure is tbr the nozzle ¿rtornizers, wheel rotation speed and dialneter
are fbr the rotary atomizers. The wheel rotation speed and wheel diiureter have rn inverse rela-
tionsliip to tlie droplet size.
1.7.1.3 Feed viscosity.
The feed viscosity has ¿r direct relationship to dropiet size. As the feed viscosity increases, the
atomization energy supplied to the nozzle must overcoute large viscous tbtces to achieve
smaller droplet sizes. Viscous forces tend to reduce the energy available for breaking the
droplets, thus resulting in liirger droplets. The equation clescribing the relationship between
droplet size urd f'eed viscosity (E.luation I .8 ) is given lrelow. The sarne principle also applies
to tlrat of feed density.
[)) 1 t,, )"'
q i.A.]
EVAPORAT¡ON
An important paraneter involved in this process step is the spray angle, wtich is measured at the
nozzle orilice and is related to the nozzle's liquid tangential velocity. The liquid tangential
velociry is rhe speed at which the feed liquid spins inside the nozzle before it is divided into line
droplets irnd sprayed into tlre drying chamber. Widening tlie spray angle increases this velocity
to reduce the &-oplet size. The choice of spray algle is rclated to the type of air f)ow namely
co-currcnt o[ counter-currc¡1. with the wider anglc being used with thc lbrmer ¿rnd thc narrow
angle with the latrer. In the co-cunent operation. the downwarr.l-llowing air narrows tlown the
spray angle. ll the counter-cunent operaúon, the spray moving dowttward is widened by the
upward-flowing air. The other important pararneters in this step are the aspirator rate, air humidity.
inlet and outlet air telnperature, the glass transition temperature, and the residence titne of pafii-
cles in the spray dryer. Each of these is clescribed below. A brief guideline on tlre selection of
these parameterc and their influence on final product is presented in Box 1.1.
t.8.1 Aspirotor flow role (or speed)
The aspirator in the spray dryer is associated with the supply of drying air to the spray chamber
by the aspirator molor under pressure conditions. By altering the aspirator flow rate, the ¿unount
( 1.8) of lreated drying air entering the spray chamber can be regulated.

Where D, and D, ale the initial and ñnal droplet sizes on changing the Ieed viscosrty lrom /r to
I.8.2 lnletlemperolure
¡r", respectively. Inlet iemperaturc. is rhe temperature of the heared drying air. The inlet temperature is significent in
cooh,rg the atomized feed droplets to their wet-bulb temperature. In addition, it has a direct rela-
tionslrip to die wet-bulb temperature of the surrounding hot air (Oldlield et al., 2005; Figure 1.20).
1.7.1.4 Feed surfoce tension

As described in the principle of surlace tension of the liquid plays an important

^tomization,
role in the extent of ¿ltomization. To achieve atomization, the a tolnizer should overcome the d|vcr:. Huwever. a l¡wcr valuc of thc inlcl lcmpcraturc rcdttces thc wcLllglu§]!lpcralurc o[ lbc
surfhce tension of the téed liquid. Hence, a liquid lraving higher surface tension is diflicult surr t ulrdurg lror uir. arñ p.eve,iiitre-uegmdáfiCl¡-.-e.-i¡fifñtite ( ontpounds duiirlTiií-rniri"l
to atomize. This necessitates the preparation of an emulsion with the aid of ernulsifle¡
addition, and a homogenization step prior to spray drying in certain cases, ín order to combat
the surface tension of a feed, especially that invohing multiple components. In addition to
tlie knowledge on atomization parameters, the rationale ibr atomization selection is provided
/(¿
IJ§ o
in Tahle I.2. ao
o52
:§ o
Toble I .2 Criierio for seleciion of sproy dryer design (Modified from Mosiers, I 99 i ).
o
É48
Criterio Selection
I
I1 t
Fineporticle producf (30-l 20 pm). Co current flow with o rotory 244
o
low product temperolure. otomizer.
Coorse-porticle product {1 20-250 ¡rm). Counier-curreni nozle tower
40
High product lemperoture to be reoched for porosily ond bulk design with pressure nozzle
otomizer.
140 160 180 200 220 240 260
deosily.
Mixed flow nozle chomber lnlet temperature ('C)
Coorse produci (1 20-250 pm).
Produci lemperoture io below, bui lhe product is not so heoi-sensitive
ond con tolerote o certoin degree of heot treolment.
Figure I .2O lnfluence ol sproy dryer inlel iemperoiure on the wetbulb iemperolure of the gos
(Anondhoromokrishnon, 2008).
 lniroduction io sproy drying 25 26 Sprqv dryinq techniques for food inqredient encqpsulolion

stages of sprav drying. The lrade-oif between llre albrementioned circumstances is important in 30
deciding an optrmal ililet temperature tbr rhe spray drying process.
c25
1.8.3 Ouiletlemperofure 9¿ 20
3>
o6
The temperature of tlre air laden with solid paticles befbre entering the cyclone is detined as 15

the outlet temperatureJhis tempgl¿lgIg is a result of the heat and mass halance in the drying 'áo 10
cylinder, and therefore cañn6t be regulaterl. Striking the optimum tq!¡psüü¡{qJUffelgnce =O
betweeu the inlet and ourlet te ma o-
ace topography of the
final product (Maas er n1., 201 l). For instance, operation at high ouflet temperature is carried 0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9
out to acllieve high moisture content to obtain agglome¡ated ''instant" powdered products. This Water act¡v¡ty
is because higher outlet aií temperature promotes rapid crust fbrmation while the drying of the
inner co¡e is still Dot complete. Fruthemore, an increase in the outlet temperature also incrcases Figure 1.22 Moislure sorplion isotherm of o WPI powder (Guggenheim-Anderson-De Boer (GAB) sorption
the particlc tempcrature by shiliing the wct-bulb lines on thc psychrometric chart. When the isotherm model doto) (Foster et ol., 2005. Reproduced with permission of Elsevier).
inlet and outlet air temperatures are known, it is possible to calcul¿tte the particle temperature
using the above relationship. Figure l.2l illustrates all example of esrimating the temperature
of whey protein panicles using a psychrometric chart. sorption isotherm (Figure 1.22). The outlet particlc temperatures are thcn calculated flom
The wet-bulb temperature is constant along the dotted lines. Curved lines of constant wet-bulb lines using the lbllowing rclarionships:
water activity, ¿¿*, are also shown in Figufe 1.2i, in which a valve of 5.zEa corlesponds to Mass transfer rate from particle:
the relative humidity of the outlet gas and that of 16%o is the equilibrium relative humidity
corrcspontiing to the whey ploduct bulk moisture contenl, obtained ll'om its moisture -n; :r,.eo(v,' -r,,,,) (1.e)

Heat transfer rate trcm particle:

0.'10 -hr,ni = hA,(7.,, -7,) (r.10)

where
fr js the mass transf'er coelicient (m/s);
0.08 A, i; the surface area ofthe particle (m'?);
lx ii
the heat transfer coefñcient (Wm'? K);
f is the water activity at surface of the porlicles:
0.06
7., iLnd T, are the temperatures of the surrounding air and pardcle respectively.

E, Comb;ning the equarions (1.9) and (1.10):

I
0.04 u, (r,,,, - r,) = t<, A,\, (v,. - Y,,,) (1.1l)

Hence, welbulb lhe is:

o.o2
y. y.,, =_lLF.,, _r,,) (r 12)
ltrqK,'

0.00 The outlet piuticle tempcrature is then estimated by ibllowing the wcrbLrlb lines lrom thc gas ouüet
20 40 60 80 'r00 120 140 160 180 200 220
conditions to the rekrtive humidity line coresponding to the equilibrium relative hurnidity (ERH) on
Temperature ("C)
tlre surface of the whey powder. The ERH of the whey powder is obtained from its water activity

Figure l.2l Psychromelric chort showing typicol gos ond porticle inlet qnd outlet conditions = ERlVlO0), detenniled liom the moisture sorpúon isotherm of whey protein isolate powder
(a,,,

(Anondhoromokrishnon, 2008). (Figure 1.22) at 50'C, reported by Foster ¿l d., (2005) using the rneasuredproduct moisnne content.
 lntroduction to sproy drying 27 28 Sproy drying lechniques for food ingredient encopsulotion

Howeve¡ the above metllod of estimation for particle outlef temperature assumes that there Feed Heater
is no significant effect of temperature, and üe measured moisture content is representative of
the surface moistue content as the panicles exit the spray dryer. But, in reality, the surface
rnoisture content will always be lower than the average rnoisture content and thus the estimated
particle oudet temperatures would be lower than üe actual value.

1.8.4 Gloss trqnsition lemperolure (Ir)

Class transition is a l'eature of second-order úme temperature dependent fansition, which is
characterized by a disconúnuity in physical, mechanical, electrical, üermal, and other properties
of a material (Rahman, 1995). I is the temperature above which the matrix shifts from the struc-
turally rigid glassy state to a rubbery state, wlich is associated wiü product stickiness on the
spray chamber wall in spra! drying. Stickiness is considered to be the rnajor process challenge
in spray drying. It leads to product agglomeration and poses problems of caking and lumping of
the product during packaging of dre spray dded products. The d of fbed depends on the
constituent solutes prescnt in the feed. It is given try the Gordon-Taylor eq uation (Equation I . I 3),
which appiies to a multi-component system:

w.T . +cw"T -
(1. l3)
' wr+cwz Figure I.23 Schemoiic o[ on open cycle sproy dryer.

wherc: the hearilg medium is recycled/reused; as single-stage and two-stago dryers, depending on the

w, atd w, are mass tiactio[ of solute and water; number of passes before the üied product is separated; and as short-form and tall-form, based
Tr,andTrrare Elass transition temperatures (K) ofsolute and water (138 K), respectively on tlre aspect ratio. Each of the above categories of sp¡ay dryer is briefly described as below:
¿ is the ratio of specitic heat change of solute to water at üe glass transiúon temperature.
1.9.t Open cycle sproy dryer
Further discussions on the relevance of d in spray drying process ale presented in detail in
This is the st¿urdard layout of spray dryer, with wide usage. It involves d¡awing the drying air from
Chapter 4,
the annosphere, heaúng and conveying it through rhe chamber once, and üen exhausting it back
to the i¡ünosphere (Figure 1.23). The variations in this layout could be with respect to the type of
1.8.5 Residence fime of port¡cles in the sproy chomber separation equipment used (i.e. use of cyclone separator, bag filter or electrostatic pl€cipitator).

This parameter is important from two perspectives - namely, with respect to complete drying of
feed droplets to achieve optimum product specifications, and in the control of particle temper
atu€ to minimize aroma loss and themal degradation of heat sensitive materials. The particle
residence lime (RT) also affects product qualiry indices such as solubility and bulk density. RT
is divided into two parts: primary and secondary residence times. The primary RT is calculated
from the time taken for droplets leaving the nozzle to impact on the wall or leave at the outlet.
The secondary residence time can be deñned as the time taken fo¡ a particle to slide along the
wall from üe impact position to the exit (Kuriakose and Anandharamakrishnan, 2010). While
prediction of RT in a spray charnber is experirnentally difficult, recent advancements in mod-
eling and powerfulcomputational simulation techniques aid in efñciently calculating the RT.
1.9"2 Closed cycle sproy dryer
Closr:d cycle dryers work on the principie of recycüng and reusing the gaseous medium , which
is us relly a relatively inert gas such as nitrogeu, or air in special cases (Figure 1.24). A closed
cycle dryer is used when the feedstock is prepared by dissolving the solids in flammable sol-
vents. in ordel to rcduce the explosion risk and to obtain a complete recovery of the solvent.
When the spray dried ploduct is susceptible to oxidation, then a closed cycle dlyer is the most
appropriate choice (Gohel et a1.,2009). It is also advantageous to use this type of dryer when a
toxic feed is subjected to drying, and the resultant poilution due to roxious vapors and u¡rdesir-
able particulate emissions or odot are not permitted by the regulatory norms. However, these
conditions are normally not encountered in a food industry.

1.9 TYPES OF SPRAY DRYER

1.9.3 Semi-closed cyc¡e sproy dryer
Spray dryers can be classiñed inro different types, based on dift-erent criteria. They a(e catego- This dryer design is a cross between open and closed cycie dryers. A direcf-fued heater is used,
rized i¡to co-currelt dryers. counter cur'rent dryers and mixed flow dryers, basedon the direction and the air entering the system is limited to that required fbr combustion. An amount of air equal
ofair and fd§d flow; as of'en cycle, closed cycle and semi-closed cycle dryers, based on whether to the combustion air is bled from the system at the other end of the process. The gas (mainly
 lniroduction lo sproy dryinq 29
Air in Air out
Wet scrubber
Figure I.24 Schemotic of q closed cycle sproy dryer.
products of combustion) is recycled tln'ough the dryer. The recycled gas has very low oxygen
content, making it suitable for matedals that cannot be exposed to oxygen due to explosive
heuard or product degmdation (Anundhia et ai., 20I l).
1.9.4 Single-sloge sproy dryer
The single-stage configuraúon is the most prcdominantly used spray dryer design. In a single-
stage dryer, the moish[e is reduced to the target level in a single pass through the spray chamber.
A substantial reduction in weight (about SOVo), volume (about 607o) and diameter (abo* 25Vo\
qf the initial pafiicle has been reporled during single sfage-spray drying (Westergaard, 1994).
The single-stage spray dryers operate at an inlet temperature of 150-200'C and ail outiet tem-
perature of around 95"C (Early, 1998). However, if lower rcsidual moisture content is expected
of the final product, then the relative humidity of the outlet ail' slrculd be lower a¡d, hence, the
outlet temperature should be higher. The resultant particle tempemture would therefore be
higher. which is not suitable lbr heat-sensitive products. Furthermore, walmer tcmpcr¿ttures
would possibly cause the particles to stick together with very weak bindings to form large and
loose agglomerates. At extremely high outlet air temperatures, blow-hole formation might
occur, as discussed earlier (Westergaard, 2010).
t.9.5 Turo-stoge sproy dryer
The two-stage spray dryer is corsidered to be a development over single-stage spray dryers.
In single-stage spray dryers, the need for a higher outlet temperature to achieve lower
residual moistu¡e content might be detrimental to the final product quality. In o¡der to over'-
cone this limitation, in a two-stage spray dryer, the required moisture content is attained in
two stages. After leaving the spray chamber, the moistue content of the particles from the
first stage, which is typically at the le\.el of5-107o, is further reduced during a second stage,
accomplished in a fluidized bed dryer (Figure 1.25). Two-stage spray dryers a¡e therefore
30 Sproy dryinq lechniques for food ingredient encqpsulotion
(a)
Figure 1.25 (ol Schemoiic of two stoge sproy dryer with its conicol bottom ottoched to fluidized bed.
{b) Pilot scole integroted fluidized bed sproy dryer (Schwortzboch ond Moslers, 2001. Reproduced wilh
permission of Toylor ond Froncis).
suitable lbr heat sensitive products because of their cornparatively low temperatue in each
of the two stages relaúve to those used in a single-stage spray dryer.
However, in order 10 combat the lower dillirsion coefficient fbr moisture removal during the
second stage, the fluidized bed dryer should provide sufficie¡t residence time for the puticles
to achieve the requircd tlnal moisture content. The advantages ol two-stage spray dryers include
higher evaporation capacity per unit weight of drying air, lower operation cost, better quality
products and lower powder emission (Westergaard, 2010).
1.9.6 ShoÉ-form
Short-form drlers have hcight-to-diameter ratios (aspect ratio) of around 2 : 1. The short-form
dryers (Figure I.26(a)) are the most widely used, as they accommodate the comparatively l1at
spray rlisk liom a rotary atomizer (Masters, 1991). The llow patterns observed in shorrfbrm
dryer s are more complex than those in tall-form dlyers, with many dryers having no plug-flow
zone aud a wide range of gas resideDce times (Langrish ard Fletcher, 2001). A shon-form dryer
with a bottom outlet is more suitable for drying ofheat-sensitive materials. such as proteins, due
to the low amounts of recirculated gas and, hence, shorter residence time of the particles
(Alandha'amak¡ishnan er a/., 2008).
I.9.7 Toll-form
Tall-fbrrn designs arc characterized by height-to-diarneter aspect ratios of greater üan 5 :I
(Figure 1.26(b)). The spray angle is confined to the smaller diameter of the chamber and nozzle
atomizers are often used in combination widr tall-form dryers. The greater aspect ratio also con-
tributes to the longer residence time of the particles in the dryilg chamber: Computational fluid
dynamics (CFD) simulation studies on tall-form spray dryers have indicated that more than
 lnlroduciion to sproy dr 3t 32 Sproy drying techniques for food ingredient encopsulolion

Figure I.2ó (q) Short-form; lbl Toll-form sproy dryer

figure 1,27 Applicotions of sproy drying.

Box I.2 Advontoges of sproy drying Ioble I.3 Food opplicotions of sproy drying

o The ability to be operated as fully automated control systern, enabling continuous Applicotion
monitodng and recording of all the associated process variables simultaneously. Doiry products {whole milk,
e A variety of spray dryer designs to meet dift'elent product specifications. skim milk, whey protein)
¡ Few moving parts and no moving p¿u'ts are in direct contact with the product, mini- Egg-bosed producis
mizi.ng corrosion problems. lnslont coffee ond teo
¡ The ability to handle vuied nature of feedstock, with the only mandate being that it has
Flovoring compounds
to be pumpable (solution, sluny, paste, gel, suspension or melt tbrm). Meot ond fish products
r The possibility of obtaining tailor-made particle size ald btrlk dersity, depending on end Fruit ond vegetoble products
product specifications, by optimization of nozzle design and operation paramete-rs. Edible profein products
¡ Unique morphology of pretlominantly spherical pa'ticies, with unifbrm size and hollow Corn producls
Wheot bosed products for
structulc, thus reducing the bulk density of the product.
bo[. e'y purpose
Sugor products
Reference
Ye et ol. l2OO7); Fong et o/. 12012); Kin et al. 120091; Fu et ol. 120121;
Anondhoromqkrishnon et ol. (2008)
Kincol (l 987); Ronnou el o/. (201 3)
Yu etoL {2012}
Boyrom el o/. 12005); Ghorsollooui er o/. {201 2}; Yoshii et ol. (20Q1);
Sooititontowot ef o/. {2005}.
Kurozowo et ol- l2OQ9l;Zhong et ol- {201 3}; Anwor ond Kunz, (2Ol 1 )
Kho et o/. (20 t 0); Goulo ond Adomopoulos (2005); Fozoeli et ol. 12012)
Oil¡z et al. {2009); Wong et oi. {2013}
Zhong ond Jin (2009)
Lioo ef o/. (2013)
.Joyosundero et o/. (201 1); Truong er o/. (2005); Adhikori et ol. {2009);
ConoChouco et ol. (2005)

600lo of the panicles impact on the cylindrical wail, which has an adverse eft'ect on the product
quality due to the solids adhedng to the wall for appreciable times, drying out and losing their
wet-bulb protection (Anandharamakrishnan er a/., 2008).
I.IO APPTICATIONS AND ADVANTAGES OF SPRAY DRYING
Tlie maior advantages and applications of spray dryilg ale presented in Box 1.2 and
Figure 1.27, respectively. The applications of spray drying have been categorized as food
and non-food applications in Figure 1.27. The exclusive lood applications of spray drying
are presented in Tablc 1.3.
Thus, in a nutshell, the resourcefulness of splay drying lies in its capacity in terms of con-
tinu(,u.r opemtion, wide range of operating temperatures, short residence times, production of
a powdercd prodrct, suitability fbr both heat-sensitive and heati'esisl.ant materials. rapid
drying and flexibility in capacity design (feed rates range from a few pounds per hour to o\,er
100 turs per hour), to listjust a ftw. In the following chapters, the spray drying technique is
intloduced to readers in its all¡rew dimensiou as an encapsulation process for food ingredi-
ents, l'lle fundarnental aspects of spray drying covered in this chapter are presented with an
intention to assist readers to further relish the "language of spt'tqt tlrytiag" in the new accent of
"encu¡tsulatiort" in the forthcoming chapters.
 lniroduciion to sproy drying 33
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Anexo 6 Anexo 7

Diagaura de equipo del proeeso qufinico "gecEdo l8r'afomizació¡"

Diagrama ile Bloque dei proceso quimico de "Secado por atomDación"

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o
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:
.§ ü §.EH€
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 4.L. Descripción global
:n la descripción global del proceso se encuentra una breve descripción del
Droceso y ¡as reacciones que tienen lugar en el proceso de fabricación.

4.7.7. Resumen del proceso

CAPITULO A=PROCESO DE La fabr¡cac¡ón de los detergentes en polvo parten de la
dodecilbenceno con un agente sulfonante (trióxldo de azufre, ácido sulfúrico,
reacc¡ón del

Oléum..,) para sulfonar la cadena orgánica. obten¡éndose el ácido

dodecilbencensulfón¡co (LAS). Es decir:
FABRICACION DE
Dodec¡lbenceno + Agente sulfonante ) Ác¡do dodecilbencensulfón¡co + Subproducto

DETERGENTE EN POLVO Después. el LAS se hace reacc¡onar con ei h¡dróx¡do de sodio (sosa cáustica)
para formar la sal de éste, es decir, el dodecilbencenosulfonato de sodio que es
el tensoactivo an¡ónico por excelencia de los detergentes en polvo.

Ácido dodec¡blencensuflónico + H¡dróxido de sodio ) Dodec¡lbencenosulfonato + Agua

El dodecilbencenosulfonato de sod¡o es mezclado con los insumos (más adelante

Se presentarán las diferentes fases del proceso de elaboración del detergente en se explica) para formar una masa pastosa denominada slurryl, poster¡ormente es
polvo: env¡ado a la sección de secado, en donde los operarios manipulan los parámetros
de la torre de secado para fijar una densidad y humedad de la pasta según lo
. Descripción Global. establec¡do por Ia f,cha de seguridad del detergente, pasando luego a la zona de
enfriamiento, tamizado, adición de enz¡mas y perfume, finalmente el
. Entradas al Proceso,
empaquetado.
. Etapas y Equipos del Proceso. Se utilizará el Oleúm como agente sulfonante por las ventajas que se obtuvieron
. Generadores.
ll realizar el estud¡o de los diferentes agentes sulfonantes (Ver anexo PFCI)
. Envasado. 4.7.2. Reacc¡ones
. Diagrama de flujo. l-as reacciones que tiene lugar son:

. Automatización. CrzHzsCoHs + H2SO4'SO3 .) H2SO4

Cr:HzsCsH+SO3H + (1)

c12H25c6H4so3H + NaoH ) CrzHzsCoH+SO:Na + H:O (2)

Aprox¡madamente, Ia duración de cada operación de fabricación (excepto el

H2SO4 + 2NaOH ) Na2SO4 + H2O (3)
envasado) será de 40 minutos con una duración total de 4 horas,

A cont¡nuación, se desarrollan fases anteriores.

1
Slurry: Es una mezcla de liqu¡dos y sólidos no disueltos
 Fdbricación de detersente en Dolvo

Las propiedades físicas y químicas son:

Tabla 4.2. Propiedades fís¡cas y químicas det Óleum

4.2. Entradas al Proceso

H2SO4.503
Las entradas al proceso se clasifican en mater¡as pr¡mas, insumos y recursos Fórmula
natu rales. Peso molecular 178 q/mol
Densidad 1840ks/m3
4,2,1, lvlaterias pr¡mas Temperatura de ebullición 339 oC al 98,3olo
Las materiás primas son las sustancias necesarias para la elaborac¡ón del Solubilidad en agua Soluble
tensoactivo, que es la materia activa del detergente. Las mater¡as primas serán
Líquido de ¡ncoloro a amar¡llo
según las reacciones (1), (2) y (3) del apartado 4.1.2 : Aspecto que desprende gases de SO3.
. Dodecilbenceno pH <1

Es un compuesto orgánico con una cadena ¡ineal de 12 carbonos unidos a un

benceno, 9u fórmula es CrzH:sCoHs.
Algunos consejos son: evitar altas temperaturas, sustancias combustibles,
Las prop¡edades físicas y químicas del se reflejan en la siguiente tabla: agentes reductores. Además, las prohib¡ciones serán no fumar y no usar
Tabla 4,1, Propiedades fís¡cas y quimicas del dodecilbenceno lámparas sin protecc¡ón.
Se deberá almacenar y transportar en zonas frescas y b¡en ventiladas. Se
almacenará cerca del hidróxido de sodio, porque si reaccionan se produce una
Fórmula C12H25C5H5
neutralización, formación de agua y la sal (sulfato de sodio).
Peso molecular 246,4 glmol
. Hidróxido de sodio
Densidad 856 ks/m3
Temperatura de ebull¡ción 186,5 0C La fórmula del h¡dróxido de sodio o sosa cáustica es NaOH. Se obt¡ene mediante
métodod de Solvay y el electrolítico. En este caso, se emplea el NaOH para
Solub¡l¡dad en agua Insoluble
neutralizar el LAS y producir la respectiva sal, se utilizará una soluc¡ón del 20 o/o
Aspecto Líqu¡do ¡ncoloro (diluida).
Otros Vapor más denso que el aire Las propiedades fís¡cas y químicas del hidróxido de sodio son:
Tabla 4,3. Propiedades físicas y quím¡cas del hidróxido de sod¡o
Al transportar y almacenar el dodecilbenceno debe haber una buena ventilac¡ón a
ras del suelo para evitar acumulación del vapor en caso de pérdida o fuga. Se
Fórmula NaOH
almacenará y se transportará lejos de los ácidos y bases fuertes.
40 g/mol
Para más información sobre el almá-cénado, transporte y riesgos quím¡cos ver
Peso molecular

anexo de protección y seguridad' Densidad 2700kg/m3

Iemperatura de ebull¡c¡ón 140 oc
. Ó¡eum
Solub¡l¡dad en agua Soluble
La fórmula del Óleum es HzSO+ SOs'
Aspecto Líqu¡do blanco y viscoso
o/o. El Óleum
Para fabricar el LAS se utilizará un óleum de un solución de 20-25 pH >L2
empleado no debe contener hierro en cantidades superiores a 0.01 %, ya que a
cantidadeS ma-yores produciría detergentes amar¡llentos disminuyendo la cal¡dad
del producto.
El almacenam¡ento y transporte debe ser fresco, seco y ventilado, Con suelos de
hormigón, con recubr¡m¡ento res¡stente a la corrosión y con buen drenaje.
La información de las materias primas se ha extraído de las fichas de seguridad
correspondientes. Para más información ver anexo fichas de seguridad
 4.2.2. Insumos
Los insumos son aquellas sustancias que no son la base del detergente, pero se ,- - - - - -l
ñeces¡tan para mejorar las propiedades del tensoactivo y
proporc¡onar un / PROCESO \
aspecto al detergente, como los coadyuvantes, los aditivos y los aux¡liares. La POR LOTES
composición del detergente y la descr¡pción de los insumos se encuentra en los (Reactores
apartados 3.3. Batch)

4.2.3. Recursos naturales

Los recursos naturales son el agua y el aire:
9. Agua
En el proceso de fabricación de detergentes el agua es empleada en las
siguientes etapas:
INGREDIENTES
. Lavados de equ¡pos.

' Para generar vapor en las calderas. Líquidos

. Aguas de enfriam¡ento,
10. Aire
Sólidos
El aire cumple las sigu¡entes funciones en una planta de detergentes:

. En la etapa de secado,
I
. Para enfriar el detergente seco.
Enz¡mas
PROCESO
I
CONT]NUO I
I
4,3. Etapas del proceso
EI proceso de elaboración de detergente en polvo se divide en cuatro etapas Perfumes
pr¡ncipales: pre-adición, torre de secado, post-adicién y envasado. El slguiente
esquema queda r€presentado el proceso.

Figura 4.1. Etapas del praceso

A continuación, se detalla cada etapa del proceso.

4.3.7. Pre-adición
as la primera etapa del proceso de elaboración del detergente en polvo. Como
esta etapa se trabaja con líquidos, soluciones (acuosas) y agua, se denomina
etapa de mezcla húmeda, se puede dividir en: reacción de sulfonación, reacción
de neutrallzac¡én y finalmente pasta slurry,
11. Reacción de sulfonación
En la ¡ndustria de los detergentes es común emplear el dodec¡lbenceno (DDB)
como agente activo. El DDB es sulfonado con el oleum, para formar el respect¡vo
ácido dodecilbencensulfón¡co (LAS). La reacción que t¡ene lugar es la reacción 1
(Ver 4.1.2)
La velocidad de reacción es extremadamente ráp¡da y exotérmica. Es necesario
mantener la temperatura a 55 oC a f¡n de ev¡tar el exceso de sulfonación y el
cons¡gu¡ente oscurecimiento de la mezcla, para mantener la temperatura se
emplea un intercambiador alrededor del reactor, el conjunto del reactor y del
intercamb¡ador de calor se denom¡na reactor con cam¡sa.
La sulfonación produce una conversión del 96% en menos de un minuto. Pero,
para facil¡tar Ios cálcr.llos y los diseños del proceso se ha supuesto una conversión
del 100oá.
Las variables a controlar son:
. Efect¡v¡dad del agente sulfonante.
. Relac¡ón de agente activo y agente sulfonante.
. Temperatura.
. Técn¡ca y tiempo de agregado del agente sulfonante.
. Grado de agitac¡ón en la sulfonación.
. Temperatura y t¡empo de agitación de la mezcla reaccionante.
. Pureza de¡ agente sulfonante.
Actualmente Ia mayoría de las industrias el¡m¡nan la etapa de sulfonación y
adquiren por parte de otras industrias químicas el ácido Sulfónico de
Dodec¡lbenceno como mater¡a pr¡ma para la producción de los detergentes, como
por ejemplo, Henkel, debido a que el coste del LAS es mucho más bajo que
dodec¡lbenceno. En el anexo se hace un estud¡o económico de esto último.
12. Reacción de neutralización
El LAS formado se neutraliza con una solución de sosa cáust¡ca, para formar el
tensoactivo an¡ón¡co, dodecilbencensulfonato de sodio. La reacción es la reacción
2 ver 4.L.2.
La neutralización se efectúa de la siguiente manera: se deposita Ia soluc¡ón de
NaOH (20olo) en el neutral¡zador, después se agrega el LAS y se agita a una
velocidad tal que su temperatura en el neutral¡zador se mantenga en un rango
de 50-55 oC (el cual debe tener una capacidad mínima lgual al doble de la
capacidad del sulfonador).
Durante la neutralización es necesario controlar la temperatura para mantener la
fluidez de ¡a pasta. Esta reacc¡ón es altamente exotérmica, generando de 6 a 8
veces más calor que en la reacción de sulfonación (1).
Los equipos empleados para controlar la temperatura en las etapas de
sulfonación y neutralizac¡ón son intercambiadores de calor de flujo circulante.
ia masa formada en la reacc¡ón (2), se mezcla con los insumos elegidos para
elaborar el detergente. La operación se reallza en tanques de mezcla
,lenom¡nados crouthers (rec¡pientes c¡líndricos de base cónica y dispuesta de una
chaqueta de calentamiento y un agitador), en donde se forma un lodo pastoso
denominado slurry con un conten¡do del 40 al 600/o de sólidos. Es necesar¡o
rnantener un control estricto de la compos¡ción del producto resultante, la
temperatura y el pH.
!)arámetros de la formación de la pasta slurry:
. Temperatura de mezcla: 600 C.
. pH de la mezcla: 10 (básico).
- Comprobación de un pH básico cual¡tativamente:
La mezcla cont¡ene agua y dodec¡lbencenosulfonato de sodio. EI agua es neutra
y la sal del LAS es bás¡ca porque la sal se descompone en cat¡ón sod¡o y en el
anión dodecilbenecenosulfonato, reacción (4). El catión sod¡o no reacciona con el
agua por lo tanto, el pH del med¡o es neutro, pero el anión de la sal del LAS si
que reacciona con el agua, formando LAS y hidroxilos, reacción (5).
CH:(CHz)g(CH)zC6H5SOrNa -> CHr(CHr)r(CH)2C6H5SO3- + Na* (4)
HrO + CH3(CHr)9(CH)rC6H5SO3 ) CH3(CHr)r(CH)rC6H5SO3H + OH (s)
Finalizada la mezcla, el slurry se bombea a la torre de secado. El detergente
desechado del tamiz y los detergente devueltos por el consumidor se vierten en
el mezclador de la pasta slurry, para que no haya residuos.
Ver el anexo de cálculos para conocer más información del dimensionado.
4.3.2. Torre de secado
La pasta slurry contiene entre un 30 y el 40 o/o de humedad (los cálculos se han
realizado con un valor del 360lo de agua, ver anexo de cálculos) hasta un
producto term¡nado del 10 o/o máximo de humedad. El secado se efectúa en la
-orre de aspersión o dispersión.
-a masa pastosa o slurry es bombeada a la torre de dispersión a una pres¡ón de
75 a 150 Psi., las partículas dispersas son puestas en contracorriente con a¡re
caliente (400 oC).
r:n ésta sección se realizan las siguientes operaciones:
. Generación de a¡re caliente.
. Secado del producto.
. Separación de polvo de arrastre.
La producción de a¡re cal¡ente necesar¡a para el secado del producto se obt¡ene
mediante el horno generador de combust¡ón de gas natural (el gas natural
contiene entre un 90Vo y un 95o/o de metano y el resto es n¡trógeno, sulfuro de
h¡drógeno y helio, pero los cálculos se han realizado con el porcentaje máximo
de metano, es decir, 100%). El generador está dotado de los dispositivos para el :as partículas de 0,5 a 1 micras pasan como producto deseado (se recogen en Ia
control de la combust¡ón y la regulación automát¡ca de la temperatura del aire parte ¡nferior del tamizado) y el resto se desecha en el mezclador de la pasta
cal¡ente a 400 oC. Cerca del generador está s¡tuado el vent¡lador que ha de slurry.
enviar el aire cal¡ente a la torre, prov¡sto de válvulas de regulación de caudal y Después de realizar una granulometría se añaden los insumos que no se han
enfr¡am¡ento. .:ñadido en la pasta slurry, porque las altas temperaturas de la torre se secado
El aire de secado entra por la parte inferior de la torre y sale por arriba, en supondría una desactivación de las de las propiedades de las sustanc¡as, como
sentido contrario al descenso de las partículas atomizadas por los ¡nyectores. El por ejemplo, el perfume y enz¡mas mediante dos¡ficadoras.
distribuidor está prov¡sto de numerosas bocas de entrada de aire para garant¡zar
una inyección uniforme y regular del a¡re al interior de la torre. En camb¡o, la
pasta slurry sale atom¡zada por la parte de arriba de la torre. Mtentras el Las tres etapas anteriores (pre-adic¡ón, torre de secado y post-adición) se
producto seco sale por la parte inferior de la torre, el aire (húmedo) lo hace por oueden esquematizar en un diagrama de flujo como es el siguiente.
la parte superior, pasando a través del conducto a la batería de c¡clones.
. Torre de Aspersión o dispersión
Se al¡menta de un gran volumen de aire ca¡¡ente sufjc¡ente
para abastecer el calor necesar¡o para completar Ia
evaporación del agua. La transferenc¡a de masa y energía se
logra med¡ante el contacto drlgclf,-del gas caliente con las
sotkasffi ?ese cáalffi -gasr
saliente por la parte super¡or es enfriado (por el calentam¡ento
global) y las partículas finas se separan del gas por medio de
un f¡ltro (para que las partículas finas no pasen a la atmosfera
contam¡nándola).La torre de aspersión generalmente está
constru¡da con chapa de acero común, está provista de mirillas Figura 4,2. Torre
o puntos de observación, e inyectores de pulverización. de secado
DETERGENTE Tamizado
T¡enen forma y dimensiones estud¡adas para obtener valores óptimos de la EN POLVO
velocidad y temperatura del arre además del t¡empo de contacto. Normalmente
la altura promedio es 24 metros (la torre que se instalará será de 20,4m).
. Batería de cic¡ones

La recolección de finos y n¡eblas en la parte superior de la torre de aspers¡ón son Figura 4.3. D¡agrama de flujo proceso de fabr¡cación.
atrapados por medio de filtros que atrapan más del 90 o/o de los sól¡dos. Los
c¡clones están ajustados con mangas de alta resistencia a la temperatura. Los
f¡nos son cont¡nuamente recogidos y rec¡clados dentro de la torre de dispersión, 4.4. Generadores
así se asegura una aspersión libre de niebla y se evita la operación manual. El
aire sale a la atmósfera con un conten¡do de finos y material part¡culado por Los generadores del proceso de manufactura de los detergentes son: el vapor, el
debajo de 5 mg/m3. ntercamb¡ador de calor y el quemador.

Para ver el dimens¡onado de la torre ver anexos.
. S¡stema de enfriamiento
El producto cal¡ente que sale de la descarga de la torre es transportado por el
conducto en donde sufre un enfriamiento. En el paso por el conducto de
enfriam¡ento, los grumos más pesados se descargan en la parte ¡nfer¡or del
conducto.
4.3.3. Post-adición
La mezcla es seca porque el porcentaje de agua es de un 100/0, esto se considera
un polvo seco. En esta última etapa se realiza la operación de tam¡zado, en que
13.Vapor: Es requerido como sum¡nistro de energía en el crouther, para
mantener las cond¡ciones de temperatura ex¡gidas, la cual es
aprox¡madamente de 60 - 70 oC
L4.Intercamb¡ador de calor: Las reacciones del proceso, son fuente generadora
de energía por cuanto allí se efectúan unas reacciones altamente
exotérm¡cas, por tanto es necesario disponer del agua como fluido de
enfr¡am¡ento que absorba la energía produc¡da. Necesar¡amente las aguas
cal¡entes son env¡adas a un sistema de torres de enfr¡amiento donde son
enfriadas y recirculadas.
;stos intercambiadores cons¡sten de un número de tubos paralelos encerrados en
una carcasa cilíndrica y se clasifican de acuerdo a la construcc¡ón del cabezal de
tubos. En todos los casos los tubos están mandrilados o soldados al cabezal para il c¡rcuito del envaso se puede describir de la siguiente forma: la primera
impedir pérdidas hac¡a ei casco. Los t¡pos de ¡ntercamb¡adores util¡zados son: náqulna del envasado realiza tres operaciones: coge los cartones desplegados,
ios pliega, corta el asa a la d¡stanc¡a adecuada y la inserta en el cartón, es decir,
a) Intercamb¡adores de cabezal fijo: Es el t¡po de ¡ntercambiador más s¡mple. ,nonta la caja para poder llenar el envase con facilidad y sin la ayuda de
pero tiene algunas lim¡tac¡ones:
'rersonal. Después, se transporta a la sigu¡ente máquina que es el llenador de los
. Diferenc¡a de temperatura l¡m¡te de 65 oC entre los flu¡dos, dado que no envases, esta máqu¡na o puede que conjunto de máquinas tiene un dosificador,
hay toleranc¡as para expans¡ón. ,rna báscula y un sensor para detectar el nivel de llenado. La siguiente máquina
se encarga de cerrar el envase y sellarlo (poner una c¡nta adhesiva para
. No se puede l¡mpiar dentro del casco, por lo tanto el líqu¡do del mismo asegurarse de que el envase este cerrado). Luego, se seca Ia cinta adhesiva con
debe estar lo más limp¡o pos¡ble. ,rna máquina que expulsa arre cal¡ente, para que el secado se realice más rápido.
b) Intercambiadores de cabezal flotante: Para permit¡r que los tubos puedan Una vez secado, se imprime un código de barras en cada cartón. La sigu¡ente
expandirse debido a la d¡ferencia de temperatura en el ¡ntercambiador, ináquina agrupa los envases de seis en seis y los envuelve f¡rmemente en papel
uno de los cabezales del tubo se mueve libremente dentro del casco. Esta f¡lm, por lo tanto, debe tener un mecan¡smo de esperar los envases, agruparlos
cabeza debe estar encerrada dentro del casco con una tapa para retornar por lotes de seis en seis. envolverlos (el f¡lm de rodearlos por las 6 caras) y
el fluido de los tubos a la sal¡da. f¡nalmente cortar el f¡lm. Luego, el lote de se¡s cartones se pega la etiqueta
(contiene fecha, ¡dent¡f¡cación de la sustancia y de la empresa, compos¡c¡ón e
c) Intercamb¡adores de tubos en U: Los tubos son de una sola pieza y hechos
información y código). La última máquina va pon¡endo los lotes de se¡s en seis en
para cada caso. Los tubos pueden expandirse y contraerse y sólo un
palees y una vez lleno y con una altura, La últ¡ma etapa del envasado es el
cabezal es necesar¡o. El haz de tubos puede ser sacado para transporte de los palees al almacén de detergente en polvo.
inspecc¡onarlo y limp¡arlo, los cuales sólo pueden ser limpiados med¡ante
el uso de react¡vos quimicos.
15. Quemador: Es el disposit¡vo que sum¡n¡stra la energía necesaria para 4.6. Diagrama de flujo
mantener la temperatura del aire a la entrada de la torre de secado a 400 oC.
En el documento de planos se adjunto el diagrama de flujo del proceso de
Una vez obtenido el detergente en polvo se realiza la operac¡ón de envasado. elaboración de detergente en polvo.

4.5. Envasado 4.7. Automatización

El detergente se envasará en envases de cartón. Cada envase contendrá 2 kg de El proceso de elaboración del detergente de principio a fin, incluyendo envasado.
detergente, en el PFCI se d¡jo de 9 kg, pero esto conlleva una envase más está controlado y regulado por PC's y sistemas electromecánicos, en el que el
grande y el doble de peso que hace desfavorable la venta por su formato. programa simula la función de un trabajador. Si la planta está automatizada
habrá un o var¡os trabajadores visualizando las pantallas del proceso.
La etapa de envasado es una ser¡e de operac¡ones unitarias mecánicas para dar
un aspecto final al detergente en polvo. A continuac¡ón, se observa un esquema Las computadoras especializadas, son ut¡l¡zadas para leer entradas de campo a
del envasado. través de sensores y en base a su programa, generar salidas hac¡a el campo a
través de actuadores.
Existen dos tipos distintos; DCS o Sistema de Control Distr¡bu¡do, y PLC o
:ontrolador Lógico Programable. El primero era antiguamente orientado a
irocesos de t¡po analóg¡co (4-20mA), mientras que el segundo se utilizaba en
lrocesos de t¡po d¡g¡tal (ceros y unos). Actualmente ambos equ¡pos se parecen
:ada vez más, y cualquiera de los dos puede ser util¡zado en todo tipo de
lrocesos.
[,
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Figura 4,5, Esquema de automat¡zación
 Anexo 7
Anexo 6
Diagrama de equipo tlel proceso químico "§ecado por *on¡izaciétf'

Diagraom de Bloqtre del proceso quimico de "§ecado por atonización"

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