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PARTICLE COATING USING DRY POWDER TECHNOLOGY 
Page 5 
L. Bilancetti1, M. Hayert2, C. Loisel2, D. Poncelet2, 
1,2) ENITIAA, Rue de la Géraudiére, F-44322 Nantes Cedex 03, France 
ABSTRACT 
The coating technology is very commonly applied to modify or improve powders properties. 
The dry coating is one technology to coat particles without using of organic solvent or water dispersion. 
Compared to solvent and water based coating, the dry coating method is favourable regarding environmental 
friendliness, safety and cost. It might be a very suitable coating method in order to coat foods and drugs which are 
sensitive to organic solvents or water. Dry particle coating, consists in coating relatively large particle size (core 
material or host) with fine particles (guest). The adhesion of these particles is made using mechano-chemical 
treatment or using plasticizer. The using of plasticizer is particularly indicated to coat particles that are relatively 
soft and very sensitive to heat and can be deformed by severe mechanical forces. 
The object of this work is the study of coating of particles with modified polysaccharides, using pan coater 
equipment. 
The mechanism of coating on particles surface and process parameters are being further investigated to be able 
to obtain a homogeneus coating shell and to reach the desired particle attributes. 
1. INTRODUCTION 
Modification of powders’ properties, such as flowability, 
wettability, flavour, colour, etc., is very important for 
many applications in food products [1]. Even more and 
more biologically active substances are used in various 
industries because of their beneficial functional 
properties and effects on the environment and human 
health [2]. 
The coating process of food materials can be 
employed to enhance, time or tune the effect of 
functional ingredients and additives [3]. 
The process consists of two steps: sprayed coating 
solution, through a nozzle, on the particles; evaporate 
the solvent, in order to obtain a coating layer onto 
particles surface. 
During the traditional coating process based on 
organic solvent, the solvent needs to be recovered due 
to environmental pollution. Coating processes with 
aqueous dispersions are time and energy consuming 
[4] caused by the low concentration of coating polymer 
and large amounts of water which need to be 
evaporated. 
Dry coating is not really a new technology. It had been 
applied in chemical, aeronautical, metallic, wood and 
paper industries mostly for coating or recovering 
woods, metals or any desired surface by paints, 
varnishes, different polymers or precious metal to 
protect them against corrosion or to reinforce them. Its 
application to food area is quite recent and is still in its 
infancy. 
Dry particle coating, consists in coating relatively large 
particle size (core material or host) with fine particles 
(guest). The adhesion of these particles is made using 
mechano-chemical treatment or using plasticizer. The 
using of plasticizer is particularly indicated to coat 
particles that are relatively soft and very sensitive to 
heat and can be deformed by severe mechanical 
forces. 
Compared to solvent and water based coating the dry 
coating method is favourable regarding environmental 
friendliness, safety and cost. It might be a very 
suitable coating method in order to coat foods and 
drugs which are sensitive to organic solvents or water. 
2. MATERIALS AND METHODS 
2.1. Materials. 
Core particles: Microcrystalline Cellulose Spheres 
(CELLETS®1000-1400μm, IPC Process-Center GmbH 
& Co. KG, Dresden, Germany) as inert support. 
Coating powder: Hydroxypropyl methylcellulose 
acetate succinate (AQOAT®, Shin-Etsu Chemical Co., 
Niigata, Japan), Eudragit E PO (Degussa AG, 
Düsseldorf, Germany), Shellac (SSB®55 Pharma, de-waxed 
fine powder, Syntapharm Ges. f. 
Pharmachemie GmbH, Mülheim an der Ruhr, 
Germany), modified Polysaccharides modified (Matrix 
1, Matrix 2, Matrix3, confidential) 
Plasticizer: Triethyl citrate (TEC, Merck KGaA, 
Darmstadt, Germany). 
2.2. Equipments. 
Wurster bottom spray coater (Glatt, Binzen, Germany). 
Rotary disk coater (prototype designed and 
manufactured in our laboratory). Pan Coater (prototype 
designed and manufactured in our laboratory).
Page 6 
2.3. Methods. 
2.3.1. Polymer analysis. 
Particle size of coating polymers was measured by 
laser light diffraction (Mastersizer, Malvern, United 
Kingdom). 
2.3.2. Coating efficiency. 
The coating efficiency was calculated by this relation: 
% 
− 
E Mass of coated particles Mass of uncoated particles C 
Mass of sprayed coating material 
= 
2.3.3. Coating film thickness and surface 
morphologies. 
Surface and cross-sectional morphologies of coated 
particles were observed with a stereo-microscope 
(WILD MC3, Leica, Germany), and particles size were 
determined by a computer based image analysis 
software (VISILOG, Noesis, France). 
3. RESULTS AND DISCUSSION 
In the present study, dry coating process is carried out 
applying three different equipments, Wurster, Rotary 
Disk, and a Pan Coater (fig.1). 
3.1. Process with Wurster: 
Experiments conducted with Wurster equipment have 
shown results below the 5% of coating efficiency. 
During the coating process, a large amount of coating 
powder gets lost onto the filter placed on the top of 
reaction chamber. 
This problem has had to the large difference of size 
between core particles and guest particles that 
influence the segregation of powder’s particles. 
3.2. Process with Rotary Disk: 
In experiments conducted with Rotary disk equipment, 
we have observed problems of abrasion between the 
particles and the surfaces of reactor chamber. The 
results have been around 0% of coating efficiency. 
However we are working to improve design and 
efficiency of this equipment. 
3.3. Process with Pan Coater: 
Experiments conducted with Pan Coater equipment 
have shown results around 85% of coating efficiency 
(Fig.2). 
In Table 1 are reported the manufacturing parameters 
used for the production of coated particles. 
3.4. Selection of polymer. 
All the polymers used have shown a high value of 
coating efficiency (Fig. 2). The polysaccharides Matrix 
2 and Matrix 3 have given the best results. These are 
food compounds, therefore excellent for food 
applications. 
As reported in Fig. 3, the particles coated with Shellac 
and Matrix 1 (large particles size) shown an 
unhomogeneous coating layer, due to presents of 
some aggregates (pictures B and D). The particles 
stretch to aggregate together before the adhesion onto 
the surface of core particles. 
A B C 
Fig. 1. Schematic representation of Wurster spray coater (A), Rotary disk coat er (B), Pan Coater (C).
Page 7 
As reported in Fig. 4, particles coated with Eudragit E 
PO (picture A), AQOAT (picture A), Matrix 2 (picture E) 
and Matrix 3 (picture F) we can observe a 
homogeneous coating layer. 
Tab.1 Manufacturing parameters used for the productionof coatedparticles 
100 
90 
80 
70 
60 
50 
40 
30 
20 
10 
Tab.1 Manu fact uring para meters used for th e pr odu ction of coated pa rticle s 
The micrographs of cross-section of particles coated 
with Matrix 3 (A) and Matrix 2 (B) (Fig. 3) shown the 
film thickness of the coated pellets, and we can 
observe a continuous film without many unevenness. 
4. CONCLUSION 
The dry coating process opens many possibilities for 
developing innovative formulation, for food and 
pharmaceutical applications. 
The results have shown that the best equipment for dry 
coating process is Pan Coater. The use of formulation 
with polysaccharides has shown a capability to 
produce coated particles with a high coating efficiency. 
The perspectives are: study of coated particles 
morphology; study of coating layer mechanism 
formation; study of coated particles’ application field. 
Fig. 3. Stereo-micrographs cross-section of coated 
particles with Matrix 3(A) and Matrix 2(B). 
Polymer Temperature Process 
Time Mean diameter Coating Efficiency Observations 
E PO 20C 14 min 40 m 78 % Continuous layer onto core 
particles surface 
Shellac 20C 15 min 90 m 83 % Guest particles aggregates 
onto core particles surface 
AQOAT 20C 23 min 25 m 85 % Continuous layer onto core 
particles surface 
Matrix 1 20C 21 min 50 m 87 % Guest particles aggregates 
onto core particles surface 
Matrix 2 20C 21 min 15 m 95 % Continuous layer onto core 
particles surface 
Matrix 3 20C 25 min 30 m 95 % Continuous layer onto core 
particles surface 
78 
83 85 87 
95 95 
0 
Eudragit EPO Shellac AQOAT M 1 M 2 M 3 
Coating efficiency % 
A 500 μμμm 500 μm B 
μμm
500 μμμm 
Page 8 
A B 
500 μμμm 
500 μμμm D E F 
REFERENCES: 
[1] M. Naito (1993). ISIJ International 33(9)915–924. 
[2] Ivanova et al. (2005) Encapsulation of water 
sensitive products: effectiveness and assessment of 
fluid bed dry coating. J of Food Engineering (71)223– 
230. 
[3] Arshady, R. (1993) Microcapsules for food. J. 
Micro-encapsulation (10)413-435. 
[4] Wheatley (1997) Latex emulsion for controlled drug 
delivery. Int. J. Pharm. (154)167–178. 
500 μμμm 500 μμμm 
500 μμμm 
C 
Fig. 4. O p tical s te re o -ph otomicr ograph s of p a rtic le s c oate d wi th Eudragit E PO (A ), Sh e lla c (B) , AQOA T (C ), 
Mat rix 1 (D ), M atrix 2 (E ) and M atrix 3 (F ).

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Coating 5

  • 1. PARTICLE COATING USING DRY POWDER TECHNOLOGY Page 5 L. Bilancetti1, M. Hayert2, C. Loisel2, D. Poncelet2, 1,2) ENITIAA, Rue de la Géraudiére, F-44322 Nantes Cedex 03, France ABSTRACT The coating technology is very commonly applied to modify or improve powders properties. The dry coating is one technology to coat particles without using of organic solvent or water dispersion. Compared to solvent and water based coating, the dry coating method is favourable regarding environmental friendliness, safety and cost. It might be a very suitable coating method in order to coat foods and drugs which are sensitive to organic solvents or water. Dry particle coating, consists in coating relatively large particle size (core material or host) with fine particles (guest). The adhesion of these particles is made using mechano-chemical treatment or using plasticizer. The using of plasticizer is particularly indicated to coat particles that are relatively soft and very sensitive to heat and can be deformed by severe mechanical forces. The object of this work is the study of coating of particles with modified polysaccharides, using pan coater equipment. The mechanism of coating on particles surface and process parameters are being further investigated to be able to obtain a homogeneus coating shell and to reach the desired particle attributes. 1. INTRODUCTION Modification of powders’ properties, such as flowability, wettability, flavour, colour, etc., is very important for many applications in food products [1]. Even more and more biologically active substances are used in various industries because of their beneficial functional properties and effects on the environment and human health [2]. The coating process of food materials can be employed to enhance, time or tune the effect of functional ingredients and additives [3]. The process consists of two steps: sprayed coating solution, through a nozzle, on the particles; evaporate the solvent, in order to obtain a coating layer onto particles surface. During the traditional coating process based on organic solvent, the solvent needs to be recovered due to environmental pollution. Coating processes with aqueous dispersions are time and energy consuming [4] caused by the low concentration of coating polymer and large amounts of water which need to be evaporated. Dry coating is not really a new technology. It had been applied in chemical, aeronautical, metallic, wood and paper industries mostly for coating or recovering woods, metals or any desired surface by paints, varnishes, different polymers or precious metal to protect them against corrosion or to reinforce them. Its application to food area is quite recent and is still in its infancy. Dry particle coating, consists in coating relatively large particle size (core material or host) with fine particles (guest). The adhesion of these particles is made using mechano-chemical treatment or using plasticizer. The using of plasticizer is particularly indicated to coat particles that are relatively soft and very sensitive to heat and can be deformed by severe mechanical forces. Compared to solvent and water based coating the dry coating method is favourable regarding environmental friendliness, safety and cost. It might be a very suitable coating method in order to coat foods and drugs which are sensitive to organic solvents or water. 2. MATERIALS AND METHODS 2.1. Materials. Core particles: Microcrystalline Cellulose Spheres (CELLETS®1000-1400μm, IPC Process-Center GmbH & Co. KG, Dresden, Germany) as inert support. Coating powder: Hydroxypropyl methylcellulose acetate succinate (AQOAT®, Shin-Etsu Chemical Co., Niigata, Japan), Eudragit E PO (Degussa AG, Düsseldorf, Germany), Shellac (SSB®55 Pharma, de-waxed fine powder, Syntapharm Ges. f. Pharmachemie GmbH, Mülheim an der Ruhr, Germany), modified Polysaccharides modified (Matrix 1, Matrix 2, Matrix3, confidential) Plasticizer: Triethyl citrate (TEC, Merck KGaA, Darmstadt, Germany). 2.2. Equipments. Wurster bottom spray coater (Glatt, Binzen, Germany). Rotary disk coater (prototype designed and manufactured in our laboratory). Pan Coater (prototype designed and manufactured in our laboratory).
  • 2. Page 6 2.3. Methods. 2.3.1. Polymer analysis. Particle size of coating polymers was measured by laser light diffraction (Mastersizer, Malvern, United Kingdom). 2.3.2. Coating efficiency. The coating efficiency was calculated by this relation: % − E Mass of coated particles Mass of uncoated particles C Mass of sprayed coating material = 2.3.3. Coating film thickness and surface morphologies. Surface and cross-sectional morphologies of coated particles were observed with a stereo-microscope (WILD MC3, Leica, Germany), and particles size were determined by a computer based image analysis software (VISILOG, Noesis, France). 3. RESULTS AND DISCUSSION In the present study, dry coating process is carried out applying three different equipments, Wurster, Rotary Disk, and a Pan Coater (fig.1). 3.1. Process with Wurster: Experiments conducted with Wurster equipment have shown results below the 5% of coating efficiency. During the coating process, a large amount of coating powder gets lost onto the filter placed on the top of reaction chamber. This problem has had to the large difference of size between core particles and guest particles that influence the segregation of powder’s particles. 3.2. Process with Rotary Disk: In experiments conducted with Rotary disk equipment, we have observed problems of abrasion between the particles and the surfaces of reactor chamber. The results have been around 0% of coating efficiency. However we are working to improve design and efficiency of this equipment. 3.3. Process with Pan Coater: Experiments conducted with Pan Coater equipment have shown results around 85% of coating efficiency (Fig.2). In Table 1 are reported the manufacturing parameters used for the production of coated particles. 3.4. Selection of polymer. All the polymers used have shown a high value of coating efficiency (Fig. 2). The polysaccharides Matrix 2 and Matrix 3 have given the best results. These are food compounds, therefore excellent for food applications. As reported in Fig. 3, the particles coated with Shellac and Matrix 1 (large particles size) shown an unhomogeneous coating layer, due to presents of some aggregates (pictures B and D). The particles stretch to aggregate together before the adhesion onto the surface of core particles. A B C Fig. 1. Schematic representation of Wurster spray coater (A), Rotary disk coat er (B), Pan Coater (C).
  • 3. Page 7 As reported in Fig. 4, particles coated with Eudragit E PO (picture A), AQOAT (picture A), Matrix 2 (picture E) and Matrix 3 (picture F) we can observe a homogeneous coating layer. Tab.1 Manufacturing parameters used for the productionof coatedparticles 100 90 80 70 60 50 40 30 20 10 Tab.1 Manu fact uring para meters used for th e pr odu ction of coated pa rticle s The micrographs of cross-section of particles coated with Matrix 3 (A) and Matrix 2 (B) (Fig. 3) shown the film thickness of the coated pellets, and we can observe a continuous film without many unevenness. 4. CONCLUSION The dry coating process opens many possibilities for developing innovative formulation, for food and pharmaceutical applications. The results have shown that the best equipment for dry coating process is Pan Coater. The use of formulation with polysaccharides has shown a capability to produce coated particles with a high coating efficiency. The perspectives are: study of coated particles morphology; study of coating layer mechanism formation; study of coated particles’ application field. Fig. 3. Stereo-micrographs cross-section of coated particles with Matrix 3(A) and Matrix 2(B). Polymer Temperature Process Time Mean diameter Coating Efficiency Observations E PO 20C 14 min 40 m 78 % Continuous layer onto core particles surface Shellac 20C 15 min 90 m 83 % Guest particles aggregates onto core particles surface AQOAT 20C 23 min 25 m 85 % Continuous layer onto core particles surface Matrix 1 20C 21 min 50 m 87 % Guest particles aggregates onto core particles surface Matrix 2 20C 21 min 15 m 95 % Continuous layer onto core particles surface Matrix 3 20C 25 min 30 m 95 % Continuous layer onto core particles surface 78 83 85 87 95 95 0 Eudragit EPO Shellac AQOAT M 1 M 2 M 3 Coating efficiency % A 500 μμμm 500 μm B μμm
  • 4. 500 μμμm Page 8 A B 500 μμμm 500 μμμm D E F REFERENCES: [1] M. Naito (1993). ISIJ International 33(9)915–924. [2] Ivanova et al. (2005) Encapsulation of water sensitive products: effectiveness and assessment of fluid bed dry coating. J of Food Engineering (71)223– 230. [3] Arshady, R. (1993) Microcapsules for food. J. Micro-encapsulation (10)413-435. [4] Wheatley (1997) Latex emulsion for controlled drug delivery. Int. J. Pharm. (154)167–178. 500 μμμm 500 μμμm 500 μμμm C Fig. 4. O p tical s te re o -ph otomicr ograph s of p a rtic le s c oate d wi th Eudragit E PO (A ), Sh e lla c (B) , AQOA T (C ), Mat rix 1 (D ), M atrix 2 (E ) and M atrix 3 (F ).