(DWR) Formulation Organoclick AB

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(DWR) Formulation Organoclick AB Enhancing the durability of fluorocarbon-free Durable Water Repellant (DWR) formulation OrganoClick AB By: Meron Solomon Degree Project in Fibre and Polymer Technology, 30 credits, Royal Institute of Technology (KTH) Supervisors: Salman Hassanzadeh & Juhanes Aydin Examiner: Minna Hakkarainen 1 Abstract The focus of the project was to alter and optimize the water repellant textile coating formulations to reach enhanced durability. For this purpose, the project was approached with three methods. Firstly, bio-based components were implemented in the mother emulsion to act as surfactant and crosslinking agent and to provide hydrophobic properties. Secondly different binders were added to crosslink and increase the coating resistance towards washes. Lastly additives at nano-scale were added to increase surface roughness in order to obtain higher hydrophobicity and improved of crosslinking capacity due to the presence of more functional groups. The stability of all emulsions was controlled using different techniques such as optical microscopy to determine particle size, distribution and any observable instability (flocculation etc.), normal aging at room temperature and accelerated aging using higher temperature. All coatings were applied using a laboratory padder on standard PA and PES pieces of textiles and hydrophobic performance was evaluated through ISO 4920 spray test. By standard washing and repeating spray test, durability could be assessed. Further structure and property studies have been run using other tests such as: contact angle measurement, breathability of the coating and SEM observations. Based on the obtained results the incorporation of low HLB, bio-based surfactants in low amount (~0,25%) resulted in an increase in the hydrophobic performance of the tested textiles. However, a decrease in shelf life could be observed with these surfactants at room temperature. Sonication was successfully used to increase both stability and shelf life significantly. Some binders and nanoparticles proved to be successful in increasing the coating quality and thus the durability. Overall many of the developed formulations could enhance performance on PA compared to the already present commercial product. On PES textile, however, the developed strategies yielded hydrophobic effect close to the commercial product. 2 Sammanfattning Målet med projektet var att ändra och optimera formuleringen av en hydrofoberande textilbehandling för att nå goda vattenavstötande egenskaper och ökad hållbarhet i tvätt. För att uppnå detta testades tre metoder. Den första var att implementera biobaserade komponenter i systemet för att fungera som ytaktiva medel och tvärbindningsmedel med funktionella grupper för att bidra med hydrofoba egenskaper. I den andra metoden tillsattes bindemedel för tvärbindning med syfte att öka kemiska interaktioner och beläggningskvaliteten på textilen. Slutligen tillsattes nano partiklar med funktionella grupper för att öka ytråheten samt tvärbindningar och genom det erhålla högre grad av vattenrepellens och hållbarhet. Stabiliteten hos alla emulsioner observerades genom optisk mikroskopi för bestämning av partikelstorlek, flockulering och andra egenskaper. Visuellt observeras emulsioner i rumstemperatur och i ugn under en längre tidsperiod för att dra slutsatser om livslängden. Alla beläggningar applicerades med en laboratoriepadder på standard PA och PES tyger. Den vattenavstötande prestandan utvärderades genom ISO 4920 spray test. Genom att tvätta och repetera spray testerna kunde man bestämma behandlingens hållbarhet. Att använda bio-baserade surfaktanter visade sig i vissa fall öka den hydrofoba prestandan på tyget. En kortare livslängd på emulsionen kunde emellertid observeras när dessa ytaktiva ämnen inkluderades i behandlingen. Genom att sonikera dessa formuleringar kunde dock en ökad livslängd erhållas. Vissa bindemedel och nano partiklar visade sig vara framgångsrika med syfte att öka beläggningskvaliteten och därigenom hållbarheten. Sammanfattningsvis, gav många av de utvecklade formuleringarna en förbättrad prestanda på PA jämfört med den redan existerande kommersiella produkten. PES var emellertid inte framgångsrik med de utvecklade beläggningarna där resultaten låg under eller i samma nivå som den kommersiella produkten. 3 Abbreviations Contact Angle CA Scanning Electron Microscopy SEM Energy-dispersive X-ray Spectroscopy EDS Polyamide PA Polyester PES Cotton COT Water vapor transmission rate WVTR Nanoparticle NP Hydrophilic-Lipophilic balance HLB Room temperature RT Metal Catalyst MCAT Keywords Hydrophobicity, textile coating, cross-linker, nanoparticles, surface roughness 4 Table of content 1. Introduction ..................................................................................................................................... 7 1.1 Hydrophobicity .............................................................................................................................. 7 1.2 Surface Tension ............................................................................................................................. 8 1.3 Emulsion ........................................................................................................................................ 9 1.4 Surfactants ................................................................................................................................... 10 1.5 Textile industry............................................................................................................................ 11 1.6 Cross-linkers ................................................................................................................................ 12 1.7 Nanoparticles ............................................................................................................................... 13 1.8 Determination of hydrophobicity ................................................................................................ 14 1.9 Analytical measuring ................................................................................................................... 14 2. Purpose of study ............................................................................................................................ 15 3. Experimental Method .................................................................................................................... 16 3.1 Material ....................................................................................................................................... 16 3.3 Textile impregnation ................................................................................................................... 18 3.4 Performance test .......................................................................................................................... 19 3.5 Analytical tests ............................................................................................................................ 20 3.5.1 Contact Angle Measurement ................................................................................................ 20 3.5.2 Stability Test ......................................................................................................................... 20 3.5.3 SEM ...................................................................................................................................... 20 3.5.4 Breathability ......................................................................................................................... 21 4. Results and discussion ................................................................................................................... 22 4.1 Strategy 1: Bio-based surfactants ................................................................................................ 22 4.1.1 Performance .......................................................................................................................... 22 4.1.2 Contact angle ........................................................................................................................ 32 4.1.3 SEM ...................................................................................................................................... 33 4.1.4 Stability and Shelf Life ......................................................................................................... 34 4.1.5 Discussion of Surfactants ..................................................................................................... 41 4.2 Strategy 2: Cross-linking ............................................................................................................. 41 4.2.1 Performance .......................................................................................................................... 42 4.2.2. Properties of Coated Fabrics ............................................................................................... 45 4.2.3 Contact Angle ....................................................................................................................... 45 4.2.4 SEM ...................................................................................................................................... 46 4.3 Strategy 3: Additives ................................................................................................................... 46 4.3.1 NP 1 .....................................................................................................................................
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