微波消解–ICP–OES法测定陶土中铅和镉含量

建立微波消解–ICP–OES法测定陶土中铅和镉含量的方法。采用氢氟酸–硝酸作为消解液,微波消解法处理样品,消解液定容后直接进入耐氢氟酸的进样系统,用ICP–OES法测定陶土中重金属铅和镉的含量。结果表明,Pb和Cd检出限分别为0.027μg/m L和0.011μg/m L,回收率分别为90.5%~98.8%和95.0%~98.4%,测定结果相对标准偏差分别为1.38%和2.17%(n=7)。该方法具有快速、准确、灵敏度高等优点,适用于陶土中铅和镉含量的检测。     

High diffusion barrier and piezoelectric nanocomposites based on polyvinylidene fluoride‐trifluoroethylene copolymer and hydrophobized clay

Nanocomposites based on polyvinylidene fluoride–trifluoroethylene copolymer and up to 4 vol % of hydrophobized clay nanoparticles are investigated. The structure, piezoelectric properties, and oxygen permeability of solvent cast films are analyzed before and after annealing above the Curie temperature of the polymer. Exfoliation of the clay takes place at concentrations up to 1 vol %, beyond which it rapidly drops and is absent at a concentration of 4 vol %. The presence of clay does not change the crystallinity of the polymer, but leads to a threefold decrease of the oxygen permeability at a concentration of 0.5 vol %. Annealing at 130 °C increases the crystallinity, the proportion of β phase up to 94%, and the piezoelectric coefficient by 20–40% at clay fractions below 1 vol %. Annealing also leads to a remarkable 3‐ to 10‐fold decrease of O₂ permeability and to intriguing changes of the activation energy for O₂ transport, which decreases from 56 kJ/mol for the as‐cast polymer to below 10 kJ/mol for the polymer and exfoliated composite. © 2017 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2017 , 55, 1828–1836     

Dephosphatation under UV light of water by Ti-PILC with activation by secondary species (La,Se, and Rb)

Me/Ti-PILC catalysts (Me: La, Se, Rb) were prepared with 60% in weight of Ti-species and 3% in weight of Me-secondary species added under ultrasounds. All materials were characterized by XRF, XPS, XRD, BET, HR-TEM/EDS, FEG-SEM and UV-vis. Three kinds of Ti-oxide nanoparticles were identified: (1) Ti-pillars within the clay layers, (2) rutile nanoflowers, and (3) anatase. In UV-vis spectra, no significant change in the band-gap was observed. In La and Se samples, small variations of the anatase XRD lines are associated with cationic diffusion after deposition of secondary species and calcination. An O1s XPS-peak (533.5 eV) is attributed to oxygen vacancies generated by this diffusion. Phosphate photo-removal in water was studied using phosphoric acid solution (75.97 g L⁻¹). Dephosphatation is significantly improved in the presence of Me-species as La/Ti-PILC > Se/Ti-PILC > Rb/Ti-PILC > Ti-PILC. Partial dephosphatation by adsorption is possible in the dark but is strongly improved by UV irradiation. With a La catalyst and under UV irradiation, phosphates (6.6 × 10⁻³ mol L⁻¹) were recovered in less than 70 min. Therefore, Me/Ti-PILC have a great potential as photocatalysts for the treatment of wastewaters and the recovery of phosphates.     

Effects of TEMED and EDTA on the structural and mechanical properties of NIPAAm/Na+MMT composite hydrogels

N‐isopropyl acrylamide (NIPAAm) hydrogels are known as thermosensitive crosslinked polymer networks. In this work, the network parameters of their composites, i.e., NIPAAm/sodium montmorillonite (NIPAAm/Na⁺MMT) hydrogels synthesized by free radical solution polymerization in the presence of two different types of accelerator (tetramethyl ethylenediamine (TEMED) and ethylenediamine tetraacetic acid (EDTA)) and initiator (potassium persulphate (K₂S₂O₈) and cerium ammonium nitrate ((NH₄)₂Ce(NO₃)₆), Ce(IV)) using five different clay content (in the range of 1.0–5.0 wt % of total monomer concentration) at 25 °C were presented and discussed. FTIR spectra, XRD patterns, SEM photographs, and network parameters of the samples indicated that the presence of COOH groups on EDTA molecules was resulted in the formation of exfoliated structures and the activity of EDTA/KPS redox pair was higher than those of TEMED/KPS and EDTA/Ce (IV) pairs. The compression moduli (G) of the hydrogels initiated with EDTA/Ce(IV) redox pair showed smooth and continual changings with increase in Na⁺MMT content (for swelling equilibrium at 25 °C) on the contrary of EDTA/KPS and TEMED/KPS pairs. It might be related to low initiator efficiency of cerium ammonium nitrate than KPS molecules, having higher effective crosslinking density with increasing clay content. On the other hand, the G moduli of NIPAAm/Na⁺MMT hydrogels (above their phase transition temperature) initiated with TEMED/KPS redox pair were higher than the others because of the more hydrophobic nature of TEMED molecules. © 2010 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 48: 1256–1264, 2010     

Effect of ion exchange by an organic cation on platinum immobilization on clays

Clay-supported platinum catalysts were prepared by ion exchange. The platinum precursor has been reduced either in the presence or in the absence of cinchonidinium cations introduced in the interlamellar space of the cationic clay. The samples were characterized by XRD and TEM. Reduction by NaBH₄ in the absence of cinchonidinium cations and the subsequent introduction of this latter ensured the formation of monodispersed, small platinum crystallites immobilized mostly between the clay sheets. On the other hand, reduction in the presence of the organic cations resulted in migration of the platinum particles on the external surface of the clay.     

Intercalated clay nanocomposites: Morphology,mechanics, and fracture behavior

Intercalated nanocomposites of modified montmorillonite clays in a glassy epoxy were prepared by crosslinking with commercially available aliphatic diamine curing agents. These materials are shown to have improved Young's modulus but corresponding reductions in ultimate strength and strain to failure. The results were consistent with most particulate‐filled systems. The macroscopic compressive behavior was unchanged, although the failure mechanisms in compression varied from the unmodified samples. The fracture toughness of these materials was investigated and improvements in toughness values of 100% over unmodified resin were demonstrated. The fracture‐surface topology was examined using scanning electron and tapping‐mode atomic force microscopies and shown to be related to the clay morphology of the system. © 2001 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 39: 1137–1146, 2001     

Investigation of clay modifier effects on the structure and rheology of supercritical carbon dioxide‐processed polymer nanocomposites

Superior property enhancements in polymer–clay nanocomposites can be achieved if one can significantly enhance the nanoclay dispersion and polymer–clay interactions. Recent studies have shown that nanoclays can be dispersed in polymers using supercritical carbon dioxide (scCO₂). However, there is need for a better understanding of how changing the clay modifier affects the clay dispersability by scCO₂ and the resultant nanocomposite rheology. To address this, the polystyrene (PS)/clay nanocomposites with “weak” interaction (Cloisite 93A clay) and “strong” interaction (Cloisite 15A clay) have been prepared using the supercritical CO₂ method in the presence of a co‐solvent. Transmission electron microscopy images and small‐angle X‐ray diffraction illustrate that composites using 15A and 93A clays show similar magnitude of reduction in the average tactoid size, and dispersion upon processing with scCO₂. When PS and the clays are coprocessed in scCO₂, the “dispersion” of clays appears to be independent of modifier or polymer–clay interaction. However, the low‐frequency storage modulus in the scCO₂‐processed 15A nanocomposites is two orders of magnitude higher than that of 93A nanocomposites. It is postulated that below percolation (solution blended composites), the strength of polymer–clay interaction is not a significant contributor to rheological enhancement. In the scCO₂‐processed nanocomposites the enhanced dispersion passes the percolation threshold and the interactions dictate the reinforcement potential of the clay–polymer–clay network. © 2010 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 48: 823–831, 2010