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Size exclusion chromatography characterization of poly (ether ether ketone), PEEK, after chemical modification
Authors: Aboelanin Hamza Mahmoud | Arndt Jan-Hendrik | Macko Tibor | Podzimek Štěpán | Bruell Robert
Year: 2023
Type of publication: článek v odborném periodiku
Name of source: Journal of Applied Polymer Science
Publisher name: Wiley-Blackwell
Place: Hoboken
Page from-to: e54259
Titles:
Language Name Abstract Keywords
cze GPC charakterizace poly(ether ether ketonu), PEEK, po chemické modifikaci Charakterizace distribuce molární hmotnosti PEEKu je velmi obtížná v důsledku jeho nerozpustnosti v běžných rozpouštědlech. Jeho rozpustnost může být zlepšena jeho sulfonací pomocí 98 % kyseliny sírové. Přítomnost sulfo skupin v PEEKu byla potvrzena pomocí NMR a IR spektroskopie. Stupeň sulfonace byl stanoven pomocí 1H NMR v deuterovaném DMSO a TGA metodou. Molární hmotnost sulfonovaného PEEKu byla stanovena pomocí SEC ve třech rozpouštědlech (N,N-dimethyl acetamid, N,N-dimethyl formamid, N-methyl pyrrolidon) pomocí PS/SDV kolon kalibrací pomocí PMMA standardů. LiBr byl přidán do mobilní fáze pro potlačení nežádoucích interakcí. Sulfonovaný PEEK byl též analyzován pomocí SEC s detektorem víceúhlového rozptylu světla (MALS). Bylo zjištěno, že absolutní molární hmotnost SPEEKu z MALS detektoru je o hodně bližší hodnotě stanovené kalibrací v N,N-dimethyl acetamidu než v ostatních dvou rozpouštědlech. GPC; technické polymery; PEEK
eng Size exclusion chromatography characterization of poly (ether ether ketone), PEEK, after chemical modification Characterization of the molar mass distribution (MMD) of poly (ether ether ketone) (PEEK) is very troublesome due to the insolubility of PEEK in common solvents. The solubility of PEEK may be substantially improved after its sulfonation. Sulfonated PEEK (SPEEK) was prepared by sulfonation of PEEK with 98% concentrated H2SO4 at room temperature. The presence of sulfonic acid group (-SO3H) in PEEK matrix was confirmed by nuclear magnetic resonance and Fourier transform infrared spectroscopy. The degree of sulfonation (DS similar to 95%) was determined by proton nuclear magnetic resonance in deuterated dimethyl sulfoxide and by thermal analysis methods. The equivalent molar mass and MMD of sulfonated PEEK was determined at 30 degrees C in three polar solvents (N,N-dimethylacetamide, N,N-dimethylformamide N-methyl-2-pyrollidone) in PS/DVB column using calibration with PMMA standards. A salt (LiBr) was added to the solvents for suppression of undesired interactions of analytes with the column packing. Moreover, the sulphonated PEEK was separated with size exclusion chromatography (SEC) coupled to a multi-angle light scattering (MALS) detector. It was found that the absolute average molar mass of SPEEK from the MALS detection is much closer to the value measured by SEC in N,N-dimethylacetamide +LiBr than the values determined in N,N-dimethylformamide and N-methyl-2-pyrollidone. engineering polymers; PEEK; size exclusion chromatography

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