Professional Documents
Culture Documents
Chemical Engineering 3: Lecture 9: Spray Drying
Chemical Engineering 3: Lecture 9: Spray Drying
Engineering 3
Feed
parAcle slurry (lactose) salt soluAon (NaCl) milk powder dried at different temperatures
Process parameters
! Feed concentraAon
ParAcle size
! Droplet size (atomisaAon pressure)
and
! Choice of solvent* morphology
! Choice of addiAves
! Feed flowrate
! Drying gas flowrate Product
temperature
! Drying gas humidity and residual
! Drying gas temperature* moisture
Mass and enthalpy balance
X in Yin A … solvent assumpAons:
B … dry gas 1) non-volaAle solids
m˙ C m˙ B C … dry solids 2) non-condensible gas
mA
€ € moisture content in solids X=
mC
€ vap € mA
m˙ A moisture content of gas Y=
mB
€
moisture mass balance:
€ m˙ C ( X in − X out ) =
€m˙ B (Yout − Yin ) = m˙ Avap
X out Yout
⇒ evaporaAon rate m˙ vap
m˙ C m˙ B€ ⇒ gas consumpAon
A
m˙ B
Mass and enthalpy balance
X in TC ,in TB,in Yin TB,ambient assumpAon:
isenthalpic drying
m˙ C m˙ B
specific enthalpy of wet solids
H A + HC
Q˙ J= = (Xc p,A + c p,C )T
€ € € € € mC
specific enthalpy of wet gas
€ €
m˙ vap I=
HA + HB
= (Yc pg,A + c p,B )T + YΔhvap,A
A € € mB
enthalpy balances:
€ m˙ B Iin = Q˙ + m˙ B Iambient
€ m˙ C J in + m˙ B Iin = m˙ c J out + m˙ B Iout
X out Yout esAmate of minimum heaAng duty
€
m˙ C TC ,out = TB ,out m˙ B Q˙ = m˙ Avap Δhvap,A
€
Mass and enthalpy balance
Condi&on: RelaAve humidity at outlet < 100 %
HA + HB
specific enthalpy [kJ/kg] I= = (Yc pg,A + c p,B )T + YΔhvap,A
mB
mA
moisture content [kg/kg] Y=
€ mB
M
pA xA P P nA P Y M ww ,B,A
relaAve humidity [%] ϕ = sat = = =
pA (T) pAsat (T) pAsat (T) n A + n B pAsat (T) 1+ Y MM ww ,B,A
€
sat b
saturated vapour pressure [Pa]
€ log10 p A =a−
c +T
(Antoine equaAon)
€
Graphical representaAon: Ramzin diagram
Step 1:
1) Take air at 20 °C
and 60 % RH
2) Find Y and I
Step 2:
1) Take air from step 1
2) Heat it up to 120 °C
3) Find I
Step 3:
1) Take air from step 2
2) Find its adiabaAc
saturaAon
temperature
ProperAes of wet solids
Equilibrium moisture sorpAon isotherm Same material, different temperatures
! Feed flowrate
! Drying gas flowrate Product
temperature
! Drying gas humidity and residual
! Drying gas temperature* moisture
Single droplet drying
Drying curve 1st period of drying:
PRODUCT DRYING CURVE EvaporaAon from free surface
Wet bulb temperature
VOLATILE CONTENT POWDER TEMPERATURE
Time
Single droplet drying
Wet bulb temperature evaporaAon rate
mass transfer (
m˙ A = km S pAsat (Tsurf ) − pAbulk )
droplet
heat-transfer rate
boundary layer
€
( )
Q˙ = kq S Tbulk − Tsurf = m˙ A Δhvap,A
1 1
Nu = 2.0 + 0.6Re 2 Pr 3
udρ
Reynolds number Re =
€
η
k d € ηρ
Sherwood number Sh = m Schmidt number Sc =
D D
€ kq d η
Nusselt number Nu = Prandtl number Pr =
λ λ cp
€ €
Droplet morphology evoluAon
Fig. 1. Example of the evolution of RH and sample mass of physical mixture of amorphous Valsartan and PVP during a single DVS measurement.
media were aqueous buffers at pH 6.8 with 0.001% (w/v) SDS confirmed by XRD porous par7cles
analysis as shown in Fig. 3. The spray drie
(sodium dodecyl sulphate) and pH 2 with 0.001% (w/v) Tween 20. samples were compared with the reference sample of semicrys
The rotational speed was 75 rpm at pH 6.8 and 100 nuclea7on
rpm at pH 2. The talline Valsartan. The stability of the amorphous form unde
dissolution profile was obtained at 37 C by the paddle method from
!
storage conditions was also measured after 45 days. No crystallin
the powder. The concentration of Valsartan in the solution was form of the API was noticed in the stability study of the soli
non-skin forming
determined using the UV technique at predetermined time points dispersion after this period. Pure Valsartan used in the physica
(2, 5, 10, 15, 20, 25, 30, 40, 50, 60, 70, 80, 90 min and at pH 2 also 100, mixtures was prepared by milling step and the volume-mea
110 and 120 min). The wavelength of 250 nm was used for particle diameter of the amorphous semi-crystalline particles wa
measurements. 34 mm and 82 mm, respectively.
smooth par7cles
3. Results and discussion 3.2. Sorption of water
3.1. Characterisation of solid dispersions “strong” skin A water sorption isotherm provides information about th
affinity between the material and water. The water sorptio
SEM micrographs of spray dried solid dispersions and physical isotherms of pure polymers are shown in Fig. 4. From the teste
mixtures of microparticles are shown in Fig. 2. SEM analysis polymers, the most hygroscopic character was revealed by PVP K3
revealed a particle size distribution between 2 mm and 30 mm and (87.7% change of mass at 95% RH). The polymer Soluplus also show
skin forming
a hollow spherical particle shape of the spray dried particles. The a hygroscopic character with 37.6% change of mass at 95% RH
amorphous form of Valsartan in the solid dispersions was However, the water sorption of Eudragit EPO shows a hydrophobi
collapsed shells
buckling
“puffing”
“weak” skin
Droplet morphology evoluAon
Skin forming vs. Non skin forming Strong vs. weak shell
CompeAAon:
- EvaporaAon rate
- Internal diffusion rate
dS dt
α=
Deff
“baAscafo” equaAon
TECHNOLOGICAL BREAKTHROUGH condiAon for shell buckling
€ Direct observaAon:
- AcousAc levitaAon
- High-speed camera
- Contactless thermometer
- Raman spectroscopy