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D I E T A G R I C U L T U R E
E N V I R O N M E N T
Recent improvements in lactose crystallization and in drying parameters for
improving quality and uses of acid whey and of related powders
P Schuck1,2, A. Mimouni1,2,3, MH Famelart1,2, D Naegele3, S Bouhallab1,2
1 INRA, UMR1253, F-35000 Rennes, France2 Agrocampus Rennes, UMR1253, F-35000 Rennes, France
3 Eurosérum, F-70170 Port sur Saône, France
D I E T A G R I C U L T U R E
E N V I R O N M E N T
Content
Å Background and Objectives
Ñ Conclusions
É Stickiness
Ç Lactose Crystallization and Thickening
Å Background and Objectives
D I E T A G R I C U L T U R E
E N V I R O N M E N T
Milk
Microfiltration Ultrafiltration
Retentate PermeateMF / UF
Acidification
Renneting
Standardization
Whey
Cheese
Casein
WPC / I
± acid / sweet
Cooling
Heat Treatment Mineral addition
± rich in minerals
UltrafiltrationTT ± rich in proteins
± rich in residual fat
± rich in lactose
± rich in µ-organisms
D I E T A G R I C U L T U R E
E N V I R O N M E N T
Proteins § 0 to 6 g.L-1
Minerals
Lactose
pHLactic acid
Lactate
Glucose, Galactose, etc.EPS, etc.
± denaturated
Residual fat, Phospholipides
NPN (0 to 2 g.L-1), aa, NH3§ 0 to 6 g.L-1
2 to 71 to 7 g.L-1
1 to 7 g.L-1
§ 30 to 50 g.L-1
1 to 5 g.L-1
Traces§ Traces
Biochemical composition of wheyand derivates
D I E T A G R I C U L T U R E
E N V I R O N M E N T
Permeate and Whey
MineralspHLactic AcidLactate
Lactose, Glucose, Galactose, EPS, …
Fat residual, Phospholipides
Proteins± denaturatedNPN, aa, NH3
D I E T A G R I C U L T U R E
E N V I R O N M E N T
Crystallized Concentrated Whey
Concentrated Whey TS = 55 % (w/w)
Whey Powder TS = 98 % (w/w)
TS = 5 % (w/w)Whey
- Heat Treatment- Whey Fractionation (MF, UF, NF, IEC, ED)- Vacuum Evaporation
Lactose Crystallization
Spray Drying
Storage
Processing of whey powders & derivates
D I E T A G R I C U L T U R E
E N V I R O N M E N T
Whey
Concentrated Whey
Crystallized Concentrated Whey
Whey Powder
- Heat Treatment- Whey Fractionation (MF, UF, NF, IEC, ED)- Vacuum Evaporation
Lactose Crystallization
Spray Drying
Storage
TS = 5 % (w/w)
TS = 55 % (w/w)
TS = 98 % (w/w)
Fouling
Heat-Induced Protein Denaturation
CaHPO4 Precipitation
Variability in Kinetics and Crystal Size
Extensive Thickening
Stickiness
Caking
Maillard Reactions
Loss of Solubility
Variability in Kinetics and Crystal Size
Extensive Thickening
Stickiness
Processing of whey powders & derivates
D I E T A G R I C U L T U R E
E N V I R O N M E N T
Å Background and Objectives
Ñ Conclusions
É Stickiness
Ç Lactose crystallzation and ThickeningÇ Lactose crystallization and Thickening
Content
D I E T A G R I C U L T U R E
E N V I R O N M E N T
Four blade paddle stirrer
Fill level
Water jacket
30 mm diameter cup
AR 2000 Rheometer head
(Mimouni et al. 2007)
Viscosity = Shear stress
Rate of Shear Strain=
k . Torque
k’ . Angular VelocityMaintained Constant
Torque = f (time)
Controlled conditions of T°Cand stirring speed / geometry
Experimental outline
D I E T A G R I C U L T U R E
E N V I R O N M E N T
Thickening at lab scale
0 100 200 300 400 50040
45
50
55
60
2000
3000
4000
5000
6000
7000
8000
Concentrated Acid WheyRefraction index (°Brix)
Time (min)
Lactose Crystallization Torque (µN.m)
1. Decrease in the concentration of
soluble phase 2. Lactose crystals counterbalance viscosity decay
3. Sharp increase in viscosity = Thickening
(Mimouni et al. 2007)
D I E T A G R I C U L T U R E
E N V I R O N M E N T
UF membrane
Proteins
• Concentration
• Lactose Crystallization
• Centrifugation
• Filtration
• Concentration
• Lactose Crystallization
• Centrifugation
• Filtration
Lactic Acid Whey
Lactose Crystal-Free Concentrated UF of Acid Whey
Lactose crystals
(Mimouni et al. 2007)
Separation of proteins and lactose crystals from concentrated whey
D I E T A G R I C U L T U R E
E N V I R O N M E N T
Rheology
0 100 200 300 400 50040
45
50
55
60
2000
3000
4000
5000
6000
7000
8000
Time (min)
Torque (µN.m)
Concentrated Acid Whey
Thickening occurred regardless of the
presence of proteins or crystals of lactose
Lactose Crystal-Free ConcentratedUF of Acid Whey
(Mimouni et al. 2007)
D I E T A G R I C U L T U R E
E N V I R O N M E N T
Structure
0 100 200 300 400 50040
45
50
55
60
2000
3000
4000
5000
6000
7000
8000
Refraction index (°Brix)
Time (min)
Torque (µN.m)
(Mimouni et al. 2007)
A A
A
Calcium Lactate Crystals
Viscosity of particle suspensions:• increases with volume fraction of particles (Petrie, 1999)• strongly increases with the particle aspect ratio (i.e. elongation) (Pabst, 2006)
B
B
D
D
C
C
D I E T A G R I C U L T U R E
E N V I R O N M E N T
Torque Amplitude (µN.m) (¨)
3.5 4.0 4.5 5.0 5.5 6.00
2000
4000
6000
8000
10000
12000
(Mimouni et al. 2007)
Influence of pH
D I E T A G R I C U L T U R E
E N V I R O N M E N T
pH
3 4 5 6 7H3PO4 H2PO4 - HPO4
2- PO43-
3.0 5.8 6.63.9
RCOOH RCOO -
(Holt et al.,1981)H2PO4
- 11HPO4
2- 642PO4
3- 2.88.106
RCOO - 15
Anions Association constant with Ca2+ (L.mol-1)
(Mimouni et al. 2007)
Lactic Acid Whey
ä pH
Influence of pH
D I E T A G R I C U L T U R E
E N V I R O N M E N T
Influence of Ph Example
Torque amplitude (∆F, 10−4 N.m) of calcium lactate supersaturated solutions ([Ca] = 1.34 g.100 g-1 of H2O), at different pH, during stirring at 120 rad.s-1 and 20°C, with and without phosphate ions.
(Mimouni et al. 2007)
5.0 ± 1.5
60.4 ± 0.9
64.7 ± 2.4
4.4 ± 0.5
40.2 ± 4.1
25.0± 4.7
3.5
5.1
6.1
0 1.5
Phosphate concentration (g.100 g-1 H2O)pH
40.2 ± 4.1
64.7 ± 2.4
D I E T A G R I C U L T U R E
E N V I R O N M E N T
Å Background and Objectives
Ñ Conclusions
É Stickiness
Ç Lactose crystallzation and Thickening
É Stickiness
Content
D I E T A G R I C U L T U R E
E N V I R O N M E N T
ð Acid lactic whey / permeate, mono & disaccharides,polyols, hydrolyzed compounds, minerals
Low Tg / ö Stickiness
ø Inlet θ & Flow rate
ø Outlet air θ & AH
ø θ Droplet & Powder
Tg Lactic acid = - 60°C
Tg Lactose = + 90°C
Low Tg
Integration of Tg
D I E T A G R I C U L T U R E
E N V I R O N M E N T
BB
II
OO
NN
OO
VV
Pilot workshop : Research and development for evaporation / drying
«MSD type» drying tower80 kg of water evaporated
per hour
Materials
D I E T A G R I C U L T U R E
E N V I R O N M E N T
[ALW]
[ALW]
Inletθ°C
Outletθ°C
AHg.kg-1DA
[C]kg.h-1
€ /ton Water
€ / ton Powder
Powderkg.h-1
233 258 78.5 61.689 41 185
155 129 99.9 78.575 26 92
ð [Acid lactic whey] at ≈ 55% TS, at ≈ 80% crystallized lactose
Spray drying
D I E T A G R I C U L T U R E
E N V I R O N M E N T
Å Background and Objectives
Ñ Conclusions
É Stickiness
Ç Lactose crystallzation and Thickening
Ñ Conclusions
Content
D I E T A G R I C U L T U R E
E N V I R O N M E N T
10 µm
High [Ca] High [Lactate] pH ~ 4.5+ +
To improve the quality of the lactic acid whey powder
ð Modify the calcium lactate supersaturationà(pH; Phosphate; Citrate; TS; Temperature)
ð Modify the spray drying parameters à(æ [C] flow rate, inlet and outlet air θ, outlet air AH)
Origin of thickening is due to the formation of calcium lactate crystals
Concentrated lactic acid wheys are likely to thicken because of:
Origin of stickiness during spray drying is due to the low Tg value of lactic acid (- 60°C)
Conclusions
D I E T A G R I C U L T U R E
E N V I R O N M E N T
MERCI
THANK YOU
