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1.
J Microencapsul ; 32(4): 336-48, 2015.
Article in English | MEDLINE | ID: mdl-26057257

ABSTRACT

Poly(styrene-co-maleic anhydride) was imidized with ammonium hydroxide and palm oil, resulting in an aqueous dispersion of hybrid nanoparticles with diameters 85-180 nm (dispersed) or 20-50 nm (dried). The reaction conditions were optimized for different precursors by evaluating the relative amount ammonium hydroxide and maximizing the incorporated palm oil up to 70 wt.%. The interactions between palm oil and polymer phase have been studied by TEM, IR, Raman spectroscopy and thermal analysis (TGA, [TM] DSC). From Raman spectra, the amount of imide and reacted oil were quantified. Through concurring effects of imidization and coupling of fatty acids, the imidization needs a slight excess of NH3 relatively to maleic anhydride. The oxidative stability highly depends on oxidative crosslinking of free or non-reacted oil. Comparing the imide content from spectroscopic and thermal analysis suggests that a complex rigid imide phase without strong relaxation behavior has formed in combination with oil.


Subject(s)
Maleates/chemistry , Maleimides/chemistry , Nanoparticles/chemistry , Plant Oils/chemistry , Polystyrenes/chemistry , Ammonium Hydroxide/chemistry , Nanoparticles/ultrastructure , Nanotechnology , Palm Oil , Particle Size , Water/chemistry
2.
Materials (Basel) ; 8(7): 4363-4388, 2015 Jul 16.
Article in English | MEDLINE | ID: mdl-28793445

ABSTRACT

A synthesis route is presented for the subsequent intercalation, exfoliation and surface modification of kaolinite (Kln) by an imidization reaction of high-molecular weight poly(styrene-co-maleic anhydride) or SMA in the presence of ammonium hydroxide. In a first step, the intercalation of ammonolyzed SMA by guest displacement of intercalated dimethylsulfoxide has been proven. In a second step, the imidization of ammonolyzed SMA at 160 °C results in exfoliation of the kaolinite layers and deposition of poly(styrene-co-maleimide) or SMI nanoparticles onto the kaolinite surfaces. Compared with a physical mixture of Kln/SMI, the chemically reacted Kln/SMI provides more efficient exfoliation and hydrogen bonding between the nanoparticles and the kaolinite. The kaolinite nanocomposite particles are synthesized in aqueous dispersion with solid content of 65 wt %. The intercalation and exfoliation are optimized for a concentration ratio of Kln/SMI = 70:30, resulting in maximum intercalation and interlayer distance in combination with highest imide content. After thermal curing at 135 °C, the imidization proceeds towards a maximum conversion of the intermediate amic acid moieties. The changes in O-H stretching and kaolinite lattice vibrations have been illustrated by infrared and FT-Raman spectroscopy, which allow for a good quantification of concentration and imidization effects.

3.
Appl Spectrosc ; 66(5): 552-65, 2012 May.
Article in English | MEDLINE | ID: mdl-22524961

ABSTRACT

Palm oil, soy oil, sunflower oil, corn oil, castor oil, and rapeseed oil were analyzed with Fourier transform infrared (FT-IR) and FT-Raman spectroscopy. The quality of different oils was evaluated and statistically classified by principal component analysis (PCA) and a partial least squares (PLS) regression model. First, a calibration set of spectra was selected from one sampling batch. The qualitative variations in spectra are discussed with a prediction of oil composition (saturated, mono- and polyunsaturated fatty acids) from mid-infrared analysis and iodine value from FT-Raman analysis, based on ratioing the intensity of bands at given wavenumbers. A more robust and convincing oil classification is obtained from two-parameter statistical models. The statistical analysis of FT-Raman spectra favorably distinguishes according to the iodine value, while the mid-infrared spectra are most sensitive to hydroxyl moieties. Second, the models are validated with a set of spectra from another sampling batch, including the same oil types as-received and after different aging times together with a hydrogenated castor oil and high-oleic sunflower oil. There is very good agreement between the model predictions and the Raman measurements, but the statistical significance is lower for mid-infrared spectra. In the future, this calibration model will be used to check vegetable oil qualities before using them in polymerization processes.


Subject(s)
Plant Oils/classification , Spectrophotometry, Infrared/methods , Spectrum Analysis, Raman/methods , Brazil , Least-Squares Analysis , Plant Oils/chemistry , Plant Oils/standards , Principal Component Analysis
4.
Langmuir ; 27(13): 8509-21, 2011 Jul 05.
Article in English | MEDLINE | ID: mdl-21650187

ABSTRACT

Celluloses are preferred renewable substrates, but hydrophilicity and porosity disfavor their water resistance. We present here an ecofriendly application of imidized nanoparticles and a method to flexibly tune the surface wettability of papers. The soft nanostructured coating is sensitive to thermal curing, which affects both the surface chemistry and morphology. The thermal stability of the coating is first investigated with conventional and modulated differential scanning calorimetry, revealing influences of the imide content and an endotherm reaction below the glass transition temperature at 120-150 °C. The latter is studied in detail for an appropriate selection of the copolymer precursors. According to diffuse reflection infrared spectroscopy, Raman spectroscopy, and UV/vis spectroscopy, the endotherm corresponds to an imidization reaction. The morphology of the coatings is followed at various scale levels by contactless roughness measurements and atomic force microscopy. Finally, the experimental values are fitted to the parameters of the Wenzel wetting model, and so-called calibration curves for the relation between contact angles, surface roughness, and surface chemistry are presented. They allow the prediction of the water contact angle of coated papers from the hydrophilic to the hydrophobic range, with a maximum in hydrophobicity after increasing the imide content at 120-150 °C curing.

5.
J Mater Sci Mater Med ; 19(11): 3399-409, 2008 Nov.
Article in English | MEDLINE | ID: mdl-18545943

ABSTRACT

OBJECTIVE: To create scaffolds with silkworm cocoon, spider egg sac and spider dragline silk fibres and examine their use for chondrocyte attachment and support. METHODS: Three different kinds of scaffolds were developed with Bombyx mori cocoon, Araneus diadematus egg sac and dragline silk fibres. The attachment of human articular cartilage cells were investigated on these bioprotein matrices. The chondrocytes produced an extracellular matrix which was studied by immunostaining. Moreover, the compression behaviour in relation to the porosity was studied. RESULTS: The compression modulus of a silkworm silk scaffold was related to its porosity. Chondrocytes were able to attach and to grow on the different fibres and in the scaffolds for several weeks while producing extracellular matrix products. CONCLUSION: Porous scaffolds can be made out of silkworm and spider silk for cartilage regeneration. Mechanical properties are related to porosity and pore size of the construct. Cell spreading and cell expression depended on the porosity and pore-size.


Subject(s)
Bombyx/metabolism , Chondrocytes/metabolism , Silk/metabolism , Spiders/metabolism , Tissue Scaffolds/chemistry , Aggrecans/metabolism , Animals , Biocompatible Materials/chemistry , Biocompatible Materials/metabolism , Cartilage, Articular/cytology , Cells, Cultured , Collagen Type I/metabolism , Collagen Type II/metabolism , Extracellular Matrix/metabolism , Fibroins/metabolism , Fibroins/ultrastructure , Humans , Immunohistochemistry , Materials Testing , Microscopy, Electron, Scanning , Porosity
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