SLIDE 1
23-Sep-2010
- D. W. Staggs
1 ISPE - Pellet Coating Process
23-Sep-2010 1 ISPE - Pellet Coating Process D. W. Staggs Fluid - - PowerPoint PPT Presentation
23-Sep-2010 1 ISPE - Pellet Coating Process D. W. Staggs Fluid - - PowerPoint PPT Presentation
23-Sep-2010 1 ISPE - Pellet Coating Process D. W. Staggs Fluid Bed Pellet Coating Process: An Exercise in Process Engineering Fundamentals Darrell Staggs, P.E. Associate Engineering Consultant Process Engineering Center Coated Pellet
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Coated Pellet Formulation
23-Sep-2010
- D. W. Staggs
ISPE - Pellet Coating Process 3
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23-Sep-2010
- D. W. Staggs
ISPE - Pellet Coating Process 4
Understanding the Process Technology
The pellets are spray-coated with layer after layer of other materials, including API, while being blown around inside the MP10, a large stainless-steel vessel
that works something like a giant hot-air corn popper,
said Nic Chornet, team leader for manufacturing at IndyDry. MQ News
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23-Sep-2010
- D. W. Staggs
ISPE - Pellet Coating Process 5
Fluidized Bed Pellet Coating The Basics
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- D. W. Staggs
ISPE - Pellet Coating Process 6
Define the Process
Everything Else
- Solution / Suspension Preparation
- Air Preparation and Delivery
- Solution / Suspension Delivery
- Droplet Formation
- Pellet Transport and Coating
- Film Formation and Drying
- Pellet Classification
- … 70+ Variables
Critical Process Parameters
- Suspension T, Mill Speed, Product T during Coating
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- D. W. Staggs
ISPE - Pellet Coating Process 7
The Mass Balance
Solids Applied Water Evaporation Coating Efficiency Pellet Potency
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- D. W. Staggs
ISPE - Pellet Coating Process 8
Pellet Coating Layers A Consistent Quality Product
Analysis of Spheres SEM and Image Analysis Eric Olson 6/30/03 API Sugar Core Subcoat Enteric Color
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- D. W. Staggs
ISPE - Pellet Coating Process 9
Pellet Coating Integrated Unit Operations
Pump Skid Filter Skid Coater Baghouse Suspension Makeup CIP System
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23-Sep-2010
- D. W. Staggs
ISPE - Pellet Coating Process 10
DEFINE the Process
Process Thermodynamics - Air Preparation and Drying
Psychrometric Chart
RH = 20% R H = 4 % R H = 6 % R H = 8 %
h = 30 kJ/kg ⎯⎯→ h = 50 kJ/kg⎯⎯→ h = 70 kJ/kg ⎯⎯→ h = 90 kJ/kg ⎯⎯→
0.0000 0.0020 0.0040 0.0060 0.0080 0.0100 0.0120 0.0140 0.0160 0.0180 0.0200 0.0220 0.0240 0.0260 0.0280 0.0300 0.0320 0.0340
5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100
Dry Bulb Temperature (C) Humidity Ratio (kg H2O per kg dry air)
D e h u m i d i f y 8 C d e w p t
Heat Drying
30 C 60% RH
Exhaust 40 C 48% RH Inlet 80 C
SLIDE 11
23-Sep-2010
- D. W. Staggs
ISPE - Pellet Coating Process 11
Process Thermodynamics-
Increased Inlet Air T
Psychrometric Chart
RH = 20% R H = 4 % R H = 6 % R H = 8 %
h = 30 kJ/kg ⎯⎯→ h = 50 kJ/kg⎯⎯→ h = 70 kJ/kg ⎯⎯→ h = 90 kJ/kg ⎯⎯→
0.0000 0.0020 0.0040 0.0060 0.0080 0.0100 0.0120 0.0140 0.0160 0.0180 0.0200 0.0220 0.0240 0.0260 0.0280 0.0300 0.0320 0.0340
5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100
Dry Bulb Temperature (C) Humidity Ratio (kg H2O per kg dry air)
D e h u m i d i f y 8 C d e w p t
Heat Drying
30 C 60% RH
Exhaust 40 C 60% RH Inlet 95 C
SLIDE 12
23-Sep-2010
- D. W. Staggs
ISPE - Pellet Coating Process 12
Process Thermodynamics- Favorable Coating Conditions vs. System Capacity
Psychrometric Chart
RH = 20% R H = 4 % R H = 6 % R H = 8 % h = 30 kJ/kg ⎯⎯→ h = 50 kJ/kg⎯⎯→ h = 70 kJ/kg ⎯⎯→ h = 90 kJ/kg ⎯⎯→
0.0000 0.0020 0.0040 0.0060 0.0080 0.0100 0.0120 0.0140 0.0160 0.0180 0.0200 0.0220 0.0240 0.0260 0.0280 0.0300 0.0320 0.0340 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100
Dry Bulb Temperature (C) Humidity Ratio (kg H2O per kg dry air) AHU + Coating 95 Inlet, 8 D.P.
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ISPE - Pellet Coating Process 13
Process Thermodynamics: Conclusions
Evaporative Capacity AND Relative Humidity Environment Increase with increasing Inlet Temperature BUT, That does NOT fully define the coating environment.
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ISPE - Pellet Coating Process 14
Sustain the Process Equipment Qualification
All Columns performing equally
- Air Flow Distribution
- Atomization Air Control
- Spray Rate Control
- Temperature Response
How to QUALIFY a Precision Coater™?
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23-Sep-2010
- D. W. Staggs
ISPE - Pellet Coating Process 15
Temperature Mapping a Precision Coater™
50 55 60 65 70 75 80 85 90 95 100 9:10:05 9:38:53 10:07:41 10:36:29 11:05:17 11:34:05 12:02:53 Time Temp, C TC1 TC2 TC3 TC4 TC5 TC6 TC7 TC8 TC9 TC10 Setpoint Inlet Temp
Column Inlet T
- vs. Inlet Air T
- vs. Set Point
- vs. Time
90 90.5 91 91.5 92 92.5 93 93.5 94 94.5 95 95.5 96 13:14:53 13:17:46 13:20:38 13:23:31 13:26:24 13:29:17 13:32:10 13:35:02 13:37:55 Time Temp, C TC1 TC2 TC3 TC4 TC5 TC6 TC7 TC8 TC9 TC10 Setpoint TT5209B
Column Inlet T Variability
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- D. W. Staggs
ISPE - Pellet Coating Process 16
Improve the Process - Secondary Loop
The Problem: Pellet Agglomeration
10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 Oversize Pellets, kg CT506492 CT507303 DTS23810 DTS23818 CT507304 CT508801 7RA52 7RA53 7RA54 7RH05 7SG37 7RH06 7SG28 7SG29 7SG30 7SG31 7SG32 7SG33 7SG34 7SG35 7SG36 7SG38 8RD01 8RD02 8RD04 8RD05 8RD30 8RF93 8RF94 8RF95 8RF96 8RF98 8RF99 8RH26 8RH28 8RF97 8RH29 8RH30 8RH31 8RJ82 8RL13 8RL14 8RL15 8RL53 8RL54 8RL55 Lot Avg=16.82 UCL=56.54
Individual Measurement of Oversize Pellets, kg Control Chart Coating=Active
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- D. W. Staggs
ISPE - Pellet Coating Process 17
Pellet AGGLOMERATION Wet Pellets
Free Moisture Condensation Outside Air Leak Cold Surface Poor Spray Large Droplets Inadequate Drying Water Leak Spray Nozzle Atomization Air Diffusion Limiting Drying Curve Mis-Alignment Nozzle Tip Wear Low Pressue Low Flow Fouled nozzle Data: UofC Spray tests Slurry Properties Viscosity Aeration Solids Air Flow API (compare to talc) Particle Size Distribution Aspect Ratio Crystal Habit and Morphology Delivery System Tank/ Agitator design / operation API solids prop's HPMC? UC spray data Solids Concentration variability control valve clearance / shear API solids prop's
Duloxetine Pellet Coating Process
DWS 1-Sep-2004 Agglomeration Mechanisms rev-3.vsd Air distribution Bed vs. Column Pellet Distribution column loading Insert size Plate pluggage Low Energy Input Air flow rate Inlet Temperature Low initial temperature API solids prop's High Relative Humidity Environment High Spray Rate Low Exhaust Temperature Air flow mal- distribution Low Pellet Circulation "Flooded" Column
SLIDE 18
23-Sep-2010
- D. W. Staggs
ISPE - Pellet Coating Process 18
Spray Nozzle Testing
Spray Using MP-10 Nozzle for API Solution
Studies On The Spray Pattern of Nozzles Used In Niro MP-10 And MP-1 Precision Coaters November 12, 2004 J. Zhou Process Engineering Center
SLIDE 19
23-Sep-2010
- D. W. Staggs
ISPE - Pellet Coating Process 19
Improve the Process Pellet Agglomeration
10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 Oversize Pellets, kg CT506492 CT507303 DTS23810 DTS23818 CT507304 CT508801 7RA52 7RA53 7RA54 7RH05 7SG37 7RH06 7SG28 7SG29 7SG30 7SG31 7SG32 7SG33 7SG34 7SG35 7SG36 7SG38 8RD01 8RD02 8RD04 8RD05 8RD30 8RF93 8RF94 8RF95 8RF96 8RF98 8RF99 8RH26 8RH28 8RF97 8RH29 8RH30 8RH31 8RJ82 8RL13 8RL14 8RL15 8RL53 8RL54 8RL55 Lot Avg=16.82 UCL=56.54
Individual Measurement of Oversize Pellets, kg Control Chart Coating=Active
Fundamental Process Changes:
- Atomization Air P
- Initial Inlet air T
- Initial Air Flow
SLIDE 20
23-Sep-2010
- D. W. Staggs
ISPE - Pellet Coating Process 20
Process Engineering Fundamentals
“There is no result in nature without a cause; understand the cause and you will have no need of the
- experiment. “
“Therefore O students study mathematics and to not build without foundations.” “He who thinks little makes many mistakes.” Leonardo Da Vinci
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23-Sep-2010
- D. W. Staggs
ISPE - Pellet Coating Process 21