Design of Experiment for Optimizing Microencapsulation by the Solvent Evaporation Technique
We employed microemulsion combined with the solvent evaporation technique to produce biodegradable polycaprolactone (PCL) MCs, containing encapsulated isophorone diisocyanate (IPDI), to act as crosslinkers in high-performance adhesive formulations. The MC production process was optimized by applying...
| Main Authors: | , , , , , |
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| Format: | Article |
| Language: | English |
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MDPI AG
2023-12-01
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| Series: | Polymers |
| Subjects: | |
| Online Access: | https://www.mdpi.com/2073-4360/16/1/111 |
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| author | Mónica V. Loureiro António Aguiar Rui G. dos Santos João C. Bordado Isabel Pinho Ana C. Marques |
| author_facet | Mónica V. Loureiro António Aguiar Rui G. dos Santos João C. Bordado Isabel Pinho Ana C. Marques |
| author_sort | Mónica V. Loureiro |
| collection | DOAJ |
| description | We employed microemulsion combined with the solvent evaporation technique to produce biodegradable polycaprolactone (PCL) MCs, containing encapsulated isophorone diisocyanate (IPDI), to act as crosslinkers in high-performance adhesive formulations. The MC production process was optimized by applying a design of experiment (DoE) statistical approach, aimed at decreasing the MCs’ average size. For that, three different factors were considered, namely the concentration of two emulsifiers, polyvinyl alcohol (PVA) and gum arabic (GA); and the oil-to-water phase ratio of the emulsion. The significance of each factor was evaluated, and a predictive model was developed. We were able to decrease the average MC size from 326 μm to 70 µm, maintaining a high encapsulation yield of approximately 60% of the MCs’ weight, and a very satisfactory shelf life. The MCs’ average size optimization enabled us to obtain an improved distributive and dispersive mixture of isocyanate-loaded MCs at the adhesive bond. The MCs’ suitability as crosslinkers for footwear adhesives was assessed following industry standards. Peel tests revealed peel strength values above the minimum required for casual footwear, while the creep test results indicated an effective crosslinking of the adhesive. These results confirm the ability of the MCs to release IPDI during the adhesion process and act as crosslinkers for new adhesive formulations. |
| first_indexed | 2024-03-08T14:59:23Z |
| format | Article |
| id | doaj.art-736678f54df44a38a4258e866314a009 |
| institution | Directory Open Access Journal |
| issn | 2073-4360 |
| language | English |
| last_indexed | 2024-03-08T14:59:23Z |
| publishDate | 2023-12-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Polymers |
| spelling | doaj.art-736678f54df44a38a4258e866314a0092024-01-10T15:06:52ZengMDPI AGPolymers2073-43602023-12-0116111110.3390/polym16010111Design of Experiment for Optimizing Microencapsulation by the Solvent Evaporation TechniqueMónica V. Loureiro0António Aguiar1Rui G. dos Santos2João C. Bordado3Isabel Pinho4Ana C. Marques5CERENA—Centro de Recursos Naturais e Ambiente, Departamento de Engenharia Química, Instituto Superior Técnico, Universidade de Lisboa, Avenida Rovisco Pais, 1049-001 Lisbon, PortugalCERENA—Centro de Recursos Naturais e Ambiente, Departamento de Engenharia Química, Instituto Superior Técnico, Universidade de Lisboa, Avenida Rovisco Pais, 1049-001 Lisbon, PortugalCERENA—Centro de Recursos Naturais e Ambiente, Departamento de Engenharia Química, Instituto Superior Técnico, Universidade de Lisboa, Avenida Rovisco Pais, 1049-001 Lisbon, PortugalCERENA—Centro de Recursos Naturais e Ambiente, Departamento de Engenharia Química, Instituto Superior Técnico, Universidade de Lisboa, Avenida Rovisco Pais, 1049-001 Lisbon, PortugalCIPADE—Indústria e Investigação de Produtos Adesivos, SA. Av. Primeiro de Maio 121, 3700-227 São João da Madeira, PortugalCERENA—Centro de Recursos Naturais e Ambiente, Departamento de Engenharia Química, Instituto Superior Técnico, Universidade de Lisboa, Avenida Rovisco Pais, 1049-001 Lisbon, PortugalWe employed microemulsion combined with the solvent evaporation technique to produce biodegradable polycaprolactone (PCL) MCs, containing encapsulated isophorone diisocyanate (IPDI), to act as crosslinkers in high-performance adhesive formulations. The MC production process was optimized by applying a design of experiment (DoE) statistical approach, aimed at decreasing the MCs’ average size. For that, three different factors were considered, namely the concentration of two emulsifiers, polyvinyl alcohol (PVA) and gum arabic (GA); and the oil-to-water phase ratio of the emulsion. The significance of each factor was evaluated, and a predictive model was developed. We were able to decrease the average MC size from 326 μm to 70 µm, maintaining a high encapsulation yield of approximately 60% of the MCs’ weight, and a very satisfactory shelf life. The MCs’ average size optimization enabled us to obtain an improved distributive and dispersive mixture of isocyanate-loaded MCs at the adhesive bond. The MCs’ suitability as crosslinkers for footwear adhesives was assessed following industry standards. Peel tests revealed peel strength values above the minimum required for casual footwear, while the creep test results indicated an effective crosslinking of the adhesive. These results confirm the ability of the MCs to release IPDI during the adhesion process and act as crosslinkers for new adhesive formulations.https://www.mdpi.com/2073-4360/16/1/111microencapsulationDoEpolycaprolactoneisocyanateadhesives |
| spellingShingle | Mónica V. Loureiro António Aguiar Rui G. dos Santos João C. Bordado Isabel Pinho Ana C. Marques Design of Experiment for Optimizing Microencapsulation by the Solvent Evaporation Technique Polymers microencapsulation DoE polycaprolactone isocyanate adhesives |
| title | Design of Experiment for Optimizing Microencapsulation by the Solvent Evaporation Technique |
| title_full | Design of Experiment for Optimizing Microencapsulation by the Solvent Evaporation Technique |
| title_fullStr | Design of Experiment for Optimizing Microencapsulation by the Solvent Evaporation Technique |
| title_full_unstemmed | Design of Experiment for Optimizing Microencapsulation by the Solvent Evaporation Technique |
| title_short | Design of Experiment for Optimizing Microencapsulation by the Solvent Evaporation Technique |
| title_sort | design of experiment for optimizing microencapsulation by the solvent evaporation technique |
| topic | microencapsulation DoE polycaprolactone isocyanate adhesives |
| url | https://www.mdpi.com/2073-4360/16/1/111 |
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