Novel Advanced Polyethylene Membrane Structures

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specialty engineered products and materials Novel Advanced Polyethylene Membrane Structures Magda Avramescu, John op den Kamp & Danny Hendricks THIS DOCUMENT, OR AN EMBODIMENT OF IT IN ANY MEDIA, DISCLOSES INFORMATION WHICH IS PROPRIETARY, IS THE PROPERTY OF LYDALL, INC. AND/OR ITS AFFILIATE (COLLECTIVELY, LYDALL ), IS AN UNPUBLISHED WORK PROTECTED UNDER APPLICABLE COPYRIGHT LAWS AND IS DELIVERED ON THE EXPRESS CONDITION THAT IT IS NOT TO BE USED, DISCLOSED, OR REPRODUCED, IN WHOLE OR IN PART (INCLUDING REPRODUCTION AS A DERIVATIVE WORK), OR USED FOR MANUFACTURE FOR ANYONE OTHER THAN LYDALL WITHOUT ITS WRITTEN CONSENT. NO RIGHT IS GRANTED TO DISCLOSE OR SO USE ANY INFORMATION CONTAINED HEREIN. ALL RIGHTS RESERVED. LYDALL, INC.

Novel Advanced Polyethylene Membrane Structures Presentation outline New filtration microporous UHMwPE products & applications Conclusions High flux filtration UHMwPE membranes Typical Properties and performance Potential applications High flux hydrophilized UHMwPE membranes Functionalization technologies Typical Properties and performance Potential applications UHMwPE membranes with improved mechanical and/or thermal stability

Filtration/separation: high flux structures Goals Develop a new generation of UHMwPE membranes: hydrophobic high flux membranes Develop composites suitable for customer processing Market applications Sterile venting vessels and tanks (fermentation) Biopharma Food and Beverage Medical Gas turbine Air pollution control 3

Higher efficiency / flow rate ratio Unique Layered Fibular Structure Improved structure 4

High Flux UHMwPE membranes: air filtration Flow rate [L/min cm²] 7 6 5 4 3 2 1 0 Airflow new HF UHMwPE v.s. Competitor materials (0.2 µm membranes) HF UHMwPE eptfe PVDF UHMwPE 0 0.2 0.4 0.6 0.8 1 1.2 Differential pressure [Bar] Today Future

UHMwPE membranes technical data Thickness Naturally : hydrophobic (water 20 repellant) 150 mm Base Low weight: extractable 3 16 g/m 2 Pore Mechanical size: robustness 0.1 10 mm Porosity: Good abrasion and impact 70 resistance 95 % Continuous Easy to handle/to use temperature: convert 80 C Air permeability: Biocompatible (USP class IV) 1 20 s/50 ml Gas Environmentally permeability: friendly: contains up to 40.000 no m 3 /m 2 h bar Chemical fluoropolymers resistance: or halogens Acids, Bases, Chlorine All HF UHMwPE (<2 mm) have >99.9% filtration efficiency for aerosol particles (0.1 0.2 mm) F9, H10, H12, H13, H14 products have 95.0 99.99993 % 0.3 µm DOP Efficiency UHMwPE lasts where eptfe, cellulose and spunbonds does not: hydrocarbon loading & challenging dust loading 6

H10 to H12 Efficiency Minipleat or Deep Pleat Filters Would you do this in your application? New UHMwPE lasts where eptfe eptfe UPLA does not: hydrocarbon loading Highly Water repellent eptfe HEPA Handles Hydrocarbon Loading Exceptionally Well Extremely low pressure drop Builds on success of pulsed cartridge program MicroGlass HEPA UHMwPE HEPA H12 eptfe UHMwPE HEPA 1.92 mg/cm2 is equivalent to loading a standard 24 x 24 V-bank filter with 12 ounces of oil.

F9 to H12 Efficiency Pulsable Cartridges Development of residual pressure drop before & after aging Test conditions: Test Temperature: conditions: 20 C Temperature: Relative humidity: 20 C <50% Relative Dust humidity: type: Pural <50% NF Dust Dust type: feed Pural rate: NF 5g/m 3 Dust Pulse feed pressure: rate: 5g/m5 3 bar Pulse Filter pressure: face velocity: 5 bar 2 m/min Filter face velocity: 2 m/min New UHMwPE lasts where spunbonds New UHMwPE do not: lasts where challenging cellulose do dust not: loading challenging dust Exceptional loading Dust Release Long Exceptional Filter Life Dust in Release Challenging Ambient Long Filter Applications Life in Challenging Extremely Ambient Applications low pressure drop Builds Extremely on success low pressure of pulsed drop GT cartridge Builds on program success of pulsed GT cartridge program Spunbonds H12 UHMwPE Poly Cell. 80/20 100% Cell. H12 UHMwPE

Filtration/separation: liquid filtration Goals Develop a new generation of high flux hydrophilized UHMwPE membranes Develop composites suitable for customer processing Market applications Membranes suited for prefiltration and clarification in biopharmaceutical processes FDA grades (Food, Beverage & Drinking Water) Diagnostic media (Ultra)pure water Membrane biorectors (MBR) 9

Modification of hydrophobic high flux UHMwPE membranes Hydrophilic UHMwPE Membranes Bicomponent structures designed for liquid filtration as permanently hydrophilized highly porous UHMwPE backbone Polyamide surface polymer High temperature resistance Superior water take-up Resistant to a wide range of chemicals Autoclavable, 121 C Ethylene Vinyl Alcohol (EVOH) surface polymer High water permeability Low surface charge at neutral ph Low adsorption of proteins, platelets and anticoagulants Negligible rest extractable ph stable from 2-10 @ room temperature Biocompatible

Filtration/separation: liquid filtration Tuned hydrophilic UHMwPE Membranes Pore size (0,1 10,0 micron) (Surface) Properties degree of hydrophilicity Porosity (70-80%) Charge Pore size control

Zeta Potential [mv] Filtration/separation: liquid filtration Hydrophilic UHMwPE Zeta Potential 20 10 0-10 Zeta potential of outer membrane surface as f(ph) for differently modified polyethylene membranes 2 4 6 8 10 12-20 -30-40 -50-60 -70 ph E-modified N-modified Low surface charge for the EVOH modified membranes Negative surface charge for polyamide modified membranes

Filtration/separation: liquid filtration Clean water permeability, l/(h x m 2 x bar) Clean water permeability, l/(h x m 2 ) Hydrophilic UHMwPE Water Permeability 20000 No compaction under pressure 30 psi HL 0.2 HL-E micron 5H01A 10000 High water permeability 15000 20 psi 20 psi 10000 8000 6000 4000 HL 0.2 micron HL-E 5H02A 5000 15 psi 15 psi 10 psi 5 psi 10 psi 5 psi 2000 0 0 2000 4000 6000 8000 0 0 10 20 30 40 50 60 Permeate volume, ml Filtration time, min

Filtration/separation: liquid filtration Filtration/separation: liquid filtration The beads retention m based on a downstream particle count of 500.000 latex particles in the upstream flow of 3.78 l/min. Latex beads added to ultra high purity DI stream (via syringe pump) Particle counts are taken up- and down-stream High efficiency (log reduction > 4) HL - 0.2 micron (customer data) Latex Beads log % (m m) reduction Efficiency 0.24 > 4 99.999 0,2 > 4 99.999 0.173 > 4 0.15 > 4 99.999 99.998 0.138 > 3 > 99.9 0.125 2 99

Filtration/separation: liquid filtration Hydrophilic UHMwPE Level of extractable Various extractable test: 24h, demi-water, 60 C, UV spectra 200 800 nm TOC Weight loss Low extractable level for the hydrophilized UHMwPE membranes 0.1 0.3% extractable

Polyamide surface polymer: improved thermal stability Thermo-dimension stability test at 140 C 2.5 µm 1 2 3 1.0 µm 0.2 µm 1. Reference heated UHMwPE membrane 2. Heated modified UHMwPE membrane 3. Reference (non-heated) UHMwPE membrane

Polyamide surface polymer Improved mechanical & thermal stability - DMA tests Polyamide treated membrane Reference membrane Increased modulus [E ] Increased temperature stability 17

Hydrophilic UPE Typical Properties Hydrophilic UHMwPE Typical Properties High water permeability High filtration efficiency Tunable pore size & porosity Tunable surface charge Low adsorption of proteins, platelets and anticoagulants Low rest extractable Resistant to a wide range of chemicals (acids, base, NaOCl) Improved thermal & mechanical stability Thickness (µm) Grade Pore Size (µm) Water permeability (L/m 2 hbar) 20 0.1 Up to 3,000 20 0.2 Up to 8,000 35 0.45 Up to 20,000 35 1 Up to 100,000 80 2 Up to 150,000 75 7 Up to 250,000

Hydrophilic UHMwPE in MBR applications Preliminary MBR filtration tests performed in parallel with commercially available MBR membranes and hydrophilyzed UHMwPE membranes Influent Permeate The sludge inoculums was taken from Aquafin s domestic wastewater treatment plant in Leuven, BE The filtration was operated continuously without relaxation or back-wash. A maintenance cleaning was conducted whenever the TMP reached a critical value > 20 kpa. Air Waste sludge

TMP, kpa Hydrophilic UHMwPE in MBR applications N-UHMwPE Maintenance cleaning E-UHMwPE Analysis of feed and effluent quality: COD Feed 533 mg/l COD C1 = 60.8 mg/l COD C2 = 8.7 mg/l COD N-UHMwPE = n.d. COD E-UHMwPE = n.d. Good performance for the hydrophilic UHMwPE hydrophilized membranes Time, h

Conclusions - New UHMwPE membranes New generation high flux UHMwPE membranes Various grades ( 0.2, 0.45 & 1.0 mm as well as F9, H10, H12 & H14 grades) developed for e.g. venting, biopharma, gas turbine, clean spaces, dust collectors, respirators, vacuum cleaner applications. Flexible functionalization technology with broad modification capabilities combines the unique structure of UHMwPE membranes with the desired functionalities of other polymers Fine-tuning of: hydrophilicity / hydrophobicity / oleophobicity; Pore size / porosity / pressure drop; Other properties: temperature stability, extractable, charge, etc. Novell hydrophilic UHMwPE membranes Various grades (0.1, 0.2, 0.45, 1.0, 2.0 & 10 mm) with permeability, retention & extractable level within market specifications; Currently investigating various application fields: pharma & food industry, water technologies, diagnostics, etc. 21

Thank you for your attention! Contact: Dr. Magda Avramescu mavramescu@lydall.com www.lydallfiltration.com 22