Slide 1: How Does Particle Characterization Enhance Research & Scale-Up, Validate Production, and Increase Your Bottom Line
How Does Particle Characterization Enhance Research & Scale-Up, Validate Production, and Increase Your Bottom Line PRESENTED BY: WILLIE HENDRICKSON CEO & FOUNDER Particle Processing Services Toll Manufacturing Research & Development Innovative Solutions
Slide 2: Presentation Outline
Presentation Outline • Overview of AVEKA • Why Do We Care About Particle Processing? • General Challenges for Industrial Particle Processing • The Economics of Particle Processing • Examples • Future Directions • Conclusions
Slide 3: AVEKA Group Overview
AVEKA Group Overview • Employee Owned and Operated • Particle technology company focused on contract manufacturing and process development • Spin-off of 3M in 1994 • Comprised of 5 Manufacturing Sites in Minnesota and Iowa • ISO certifications / food-grade certifications • Currently 280 employees
Slide 4: The AVEKA Group – A Different Type of CMO
The AVEKA Group – A Different Type of CMO • Broad Range of Unit Operations & Industry Areas • Active Research & Development Group • Extreme Technical and Collaborative Business Model 2000+ 600+ 300+ Inquires Project Proposals Customers Per Year Per Year Per Year
Slide 5: Who Cares About Particle Processing?
Who Cares About Particle Processing? 1930’s Taconite Processing and its Effects Cement Manufacturing and Energy Costs Xerography and the Information Age COVID-19 and the Pandemic
Slide 6: Big Challenges in Industrial Particle Processing
Big Challenges in Industrial Particle Processing Operations • Economics • Technology Readiness Levels Technology • Water • Powder Flow • Grinding Efficiency
Slide 7: Economics of Particle Processing
Economics of Particle Processing The Economics Spray of Drying - an Illustrative Example Particle Processing – Spray Drying, an Cost of Spray Drying Equipment: Illustrative Example $30,000,000 • Process Parameters: • Input Solids • Drying Rate • Yields: 98-99% • Operating Income: $500-700/hour
Slide 8: Spray Drying Economics I
Spray Drying Economics I 4667 3000 Output 2000 kg/hr 1333 857 500 222 20.2 1 10 20 30 40 50 60 70 % Solids of Solution
Slide 9: Spray Drying Economics II
Spray Drying Economics II Assumptions • 19%, 20%, and 21% solids • 80%, 90%, and 95% Operational Time • 2000 kg/hr Water Evaporation Rate % Solids Dried Product 80% 90% 95% kg/hr (7008 hr/yr) (7884 hr/yr) (8322 hr/yr) 19 469 3,286,752 3,697,596 3,903,018 20 500 3,504,000 3,942,000 4,161,000 21 532 3
Slide 10: The AVEKA Group – A Characterization Focused CMO
The AVEKA Group – A Characterization Focused CMO • Broad Range of Characterization Methods • Characterization for Process Control, Quality, Materials, Understanding & Development • Focus on Data Development & Analysis 50,000+ 20,000+ 30+ Analyses Particle Size Analytical Per Year Distributions Per T
Slide 11: Particle Characterization at AVEKA
Particle Characterization at AVEKA Particle Size Analysis Formulation Analysis • Particles 1 nm to 2+ mm ◦ High performance liquid chromatography (HPLC) • Particle size distribution (PSD) ◦ Thermogravimetric analysis (TGA) • Sonic sieving ◦ Spectrophotometer • Rototap ◦ Differential scanning calorim
Slide 12: The Examples…Finally
The Examples…Finally Spray Drying Optimization Density, Shape, Final Understanding Classification Efficiency Maximizing Yields Grinding Controlled D50 Characterization Methods Beyond Particle Size Distribution New Methods and Uses Statement of Need How We Approached the Problem What Went Right (or W
Slide 13: Spray Drying Density
The Result Spray Drying Density Statement of challenge Depending on Dryer used Product Would Not Fit in Bag Dryer 1 Dryer 2 D10 20.3 µm D10 26.3 µm ➢ Sodium Acetate D50 43.8 µm D50 65.1 µm ➢ Large Scale D90 112 µm D90 224 µm Optimization Sphericity 0.895 Sphericity 0.857 Understanding Tap Density0 0
Slide 14: SEM Images
SEM Images Spray Dryer 1 Spray Dryer 2
Slide 15: High Magnification SEM Images
High Magnification SEM Images Spray Dryer 1 Spray Dryer 2
Slide 16: Spray Drying Spherical Powder
Spray Drying The Result Spherical Spay drying after bead milling produced the desired material Powder Starting Material Mean PSD = 11.7 µm Statement of challenge Spray Drying produced correct size, but not desired sphericity Milled Material Mean PSD = 1.9 µm
Slide 17: SEM Spray Drying Milled Starting Material
SEM Spray Drying Milled Starting Material SEM (5000x) of spray-dried silica without (left) and with (right) prior bead milling
Slide 18: Spray Drying Density
The Result Spray Drying Most process changes did not work. % Solids in slurry did work. Density Slurry 23% Solids Statement of challenge Mean PSD = 11.4 µm Maximize Tap Density Tap Density = 0.28 g/cc With Small Changes in PSD ➢ Inorganic Material Slurry 30% Solids ➢ Spray Drying Methods Mean PSD =
Slide 19: What is Really Happening Here?
What is Really Happening Here? Characterization and Analysis can be Misleading Without an Understanding of the Process and the De Souza Lima, Powder Technology 359, 161-171, 2020. Materials
Slide 20: Classification Optimization
The Result Classification Small cut points had huge yield results Optimization Statement of challenge Maximize yields during classification ➢ Glass beads ➢ Air classified AVEKA
Slide 21: Glass Bead Classifications & Yields
Glass Bead Classifications & Yields Objective: Increase yield after classification Glass Beads Starting Material Glass Bead Classification (2 Versions) <10% <25% <50% <75% <90% Starting Glass 19.01 μm 25.08 μm 33.10 μm 41.56 μm 48.29 μm Classification (red) 23.95 μm 28.22 μm 35.82 μm 43.94 μm 50.41
Slide 22: Glass Bead Classification & Yields
Glass Bead Classification & Yields Broad Cut (24-50 μm) 73% Yield Narrow Cut (25-48 μm) Starting Beads 43% Yield Opportunity: Increased yields using characterization
Slide 23: Two Step Classification - Silica
Two Step Classification - Silica First Pass Classification – 11.43 µm Raw Material - 10.97 µm Second Pass Classification – 12.08 µm
Slide 24: Two Step Classification - Silica
Two Step Classification - Silica Raw Material First Pass Classification Second Pass Classification 10.97 µm 11.42 µm 12.08
Slide 25: Milling and Classification Optimization
Milling and The Result Classification Jet Milling step followed by air classification step. Particle size measurement using number not Optimization volume distribution Statement of challenge Control PSD to enhance flow for Additive Manufacturing ➢ Polymer Powder ➢ Jet Milled ➢ Air classified
Slide 26: Jet Milling and Classification of Polymer
Jet Milling and Classification of Polymer Jet Milled Polymer – Volume Distribution Jet Milled and Classified Polymer – Volume Distribution Jet Milled Polymer – Number Distribution Jet Milled and Classified Polymer – Number Distribution AVEKA
Slide 27: Jet Milling and Classification of Polymer
Jet Milling and Classification of Polymer Jet Milled and Classified Polymer Starting Material Jet Milled Polymer AVEKA
Slide 28: Grinding Optimization
The Result 3x reduction in grinding time Grinding D50 tightened from 15-35 µm to 17-19 µm Optimization Statement of challenge Tighten Distribution and Reduce Processing Time of Ceramic Substrates ➢ Multi-step grinding ➢ Grinding aid addition
Slide 29: Multi-Step Grinding Line
Multi-Step Grinding Line Grinding Optimization • Tote Tipper Feeder • Komar Industries auger crusher • Pneumatic conveying to screener • Ball Mill and final screening
Slide 30: Multi-Step Grinding Line
Multi-Step Grinding Line 2003 D50 = 15-35µm Crushing and Ball Milling 2006 D50 = 18-24µm Hammer and Ball Milling 2013 D50 = 16-19µm Crushing, Hammer Milling and Ball Milling 2015 D50 = 17-19µm Added Grinding Aid Opportunity: Process and yield optimization CAVEAT, CAVEAT, CAVEAT
Slide 31: You are Never Really Done
You are Never Really Done PSD of Sample that Passed Final Requirement PSD of Sample that did not Pass Final Requirement Small number of large particles not measured with laser diffraction method Wet Screening with visual inspection required to count large particles
Slide 32: Process and Material Unknowns
Process and The Result Process not optimized as received from customer Material Unknowns Desired product not purified cellulose, but rather microfibrilated bran Statement of challenge Produce Cellulose Fiber with High Water Holding Ability (20X weight) ➢ Removal of lignin and hemicellulose from corn
Slide 33: What Went Wrong / Solution
What Went Wrong Solution • Yields were poor • Analyze • Process Incredibly Inconsistent • Understand • Water Holding Results were inconsistent
Slide 34: TGA of Cellulose and Hemicellulose
TGA of Cellulose and Hemicellulose Wood Cellulose Hemicellulose
Slide 35: TGA of Corn Bran and Purified Cellulose
TGA of Corn Bran and Purified Cellulose Corn Bran Processed Cellulose New Characterization Method Required for Process Understanding
Slide 36: Process Scale-Up Analysis
Process The Result Scale-Up Scale-up of prilling process using DSC (Differential Scanning Calorimetry) Analysis Statement of challenge Define equipment parameters for heating ➢ Organic Materials ➢ Alloyed ➢ Melted and atomized
Slide 37: Determination of Process Heating Requirements using DSC
Determination of Process Heating Requirements using DSC Process for reacting & prilling a plurality of components to form an alloy Component 1 Component 2 Component 3 Alloy Representation of Prilling Process
Slide 38: DSC data to calculate heating requirements
DSC data to calculate heating requirements For each component and the alloy Calculate effective specific heat capacity for each components plus the alloy. It will require significantly less heating power to heat the reacted alloy than predicted by the heat capacities of the individual reactants.
Slide 39: Characterization and Particle Processing
Characterization and Particle Processing • It’s always the economics E. W. Merrow Chem Eng 24, 89-92, • Small changes in processing can 1988 have profound effects on profitability “Estimating Startup Times for Solids-Processing Plants” • How do you optimize your processes or develop new materials wi
Slide 40: Where We Go from Here?
Where We Go from Here? Horiba/AVEKA Webinars - 2023 (proposed) International Fine Particle Research Institute (IFPRI) • Spray Drying • New Merrow Report Commissioned by IFPRI • Agglomeration • Current and Past Projects on Most Areas • Industrial Challenges of Particle Processing Mentioned in this Ta
Slide 41: Summary
Summary • We are in the broadest and most exciting field in the world • This is a challenging field, but characterization can help with understanding and profitability • Let us know if we can help AVEKA Group Contact Information: aveka@aveka.com 651-730-1729