Ammonium polyphosphate-aluminum trihydroxide antagonism in fire retarded butadiene-styrene block copolymer

In this paper the effect of aluminum trihydroxide (Al(OH)₃—ATH) on the surface protection from fire for a styrene butadiene rubber (SBR) provided by ammonium polyphosphate ([NH₄PO₃]_n—APP) is studied.The combustion behaviour is studied by means of Cone Calorimetric tests: a maximum fire retardant effect is observed with 10-12 wt.% of APP. ATH, less effective as fire retardant, has been added at 60 wt.% to reach comparable results as measured by cone calorimetry for 12 wt.% APP.Replacement of ATH in the best performing SBR + 12 wt.% of APP shows an antagonistic effect with as little as 1 wt.% of ATH.The combustion behaviour is explained with the mechanism of interaction between SBR, APP and ATH, in which formation of aluminum phosphates negatively affects the surface protection provided by the ultraphosphate surface coating formed on heating APP in SBR.     

Enantioselective hydrogenation of alkenes and imines by a gold catalyst

A new neutral dimeric gold(I) complex bearing the 1,2-bis[(2R,5R)-2,5-dimethylphospholanebenzene] [(R,R)-Me-Duphos] ligand has been synthesized which catalyzes the asymmetric hydrogenation of alkenes and imines under mild reaction conditions.     

Thermal degradation of phosphonated polystyrenes: Part 2—The volatilisation step

On heating at volatilisation temperatures, polystyrene (PS) and telechelic chloromethoxyphosphonated polystyrene (TPPS) behave differently in the very early stage of the process. The initial rate of volatilisation of PS is zero and increases with conversion whereas TPPS polymers volatilise at an initial high rate which decreases with conversion. However, in the main stage of volatilisation (from 10–20 to 70% weight loss) both polymers liberate the same volatile products through the same basic mechanism of depolymerisation. Nevertheless, the overall rate of volatilisation of TPPS polymers in this stage is much lower than that of PS. This is attributed to the creation in degrading TPPS polymers of less reactive chain carriers of the depolymerisation process which are stabilised by the phosphoryl group.     

Study of the mechanism of intumescence in fire retardant polymers: Part I—Thermal degradation of ammonium polyphosphate-pentaerythritol mixtures

Interactions are shown to take place between ammonium polyphosphate and pentaerythritol in thermally degrading mixtures. Up to 500°C, gaseous products are evolved on programmed heating above 200°C in two steps with maximum rate temperatures differing by about 100–150°C. Swelling of the degrading mass seems, however, to be mainly due to gases evolved in the step occurring at the higher temperature. A strong dependence of the degradation process on the experimental conditions is observed.     

Thermal degradation of copolymers of methyl methacrylate and 2,6-dimethoxycarbonyl-1,6-heptadiene

The thermal degradation under vacuum of copolymers of methyl methacrylate and 2,6-dimethoxycarbonyl-1,6-heptadiene of different compositions has been investigated. It has been found that the presence in the polymer chains of small amounts of cyclic structural units from the diene monomer considerably reduces the amount of degradation which occurs in poly(methyl methacrylate) at temperatures lower than 300°C. On the basis of the results of the analysis of the degradation products, a mechanism is suggested which accounts for this effect.     

The use of POSS as synergist in intumescent recycled poly(ethylene terephthalate)

Fire retarded poly(ethylene terephthalate) (PET) has been obtained by the incorporation of octamethyl polyhedral oligomeric silsesquioxane (OMPOSS) and Exolit OP950, a phosphinate-based compound, in recycled PET. The presence of Exolit OP950 only leads to intumescence explaining the improvement of the flame retardancy. The addition of OMPOSS leads to a synergistic effect considerably increasing the fire retarding performances of the polymer in terms of cone calorimetry and limiting oxygen index even if a small thermal stabilisation as well as a very poor dispersion of OMPOSS and OP950 into the matrix has been observed.     

Gold(I)-carbenes derived from 4-pyridylisocyanide complexes: supramolecular macrocycles supported by hydrogen bonds, and luminescent behavior

Monomeric gold(I) carbenes of the type [AuR[C(NR1R2)(NHPy-4)]] (Py-4 = 4-pyridyl) have been prepared with R = C6F5, Fmes (2,4,6-tris(trifluoromethyl)phenyl) by reaction of the corresponding isocyanide compounds [AuR(CNPy-4)] with primary or secondary amines. The single crystal X-ray diffraction structures of [Au(C6F5)[C(NEt2)(NHPy-4)]].OH2, [Au(Fmes)[C(NEt2)(NHPy-4)]], and [Au(Fmes)[C(NHMe)(NHPy-4)]] show that the presence of the NHPy-4 moiety formed induces the formation of supramolecular macrocycles only supported by hydrogen bond interactions, either with N-H groups of other molecules (tetrameric macrocycles), or with water molecules (dimeric macrocycles). Dimeric gold(I) carbenes were also produced using a diamine to form a bridging carbene, or using octafluorobiphenyl to form a Au-C6F4-C6F4-Au bridge, but the solid state structures of these dimers could not be solved. Most of the complexes herein described display luminescent properties.     

Layer-by-layer assembly of silica-based flame retardant thin film on PET fabric

A novel method to improve flame retardant properties of textile fabric using multilayered thin films was evaluated. In this work, PET fabrics were coated with silica nanoparticles using layer-by-layer assembly. Five bilayers of positively and negatively charged colloidal silica (<10 nm average thickness) increased time to ignition and decreased heat release rate peak of PET fabric by 45% and 20%, respectively. In vertical burn test, this same nanocoating dramatically reduced burn time and eliminated melt dripping. This study demonstrates the ability to impart flame retardant behavior using a water-based, environmentally-friendly protective coating.     

Ultra‐performance liquid chromatography MS/MS method for the determination of parabens in compost from sewage sludge: Comparison of the efficiency of two extraction techniques

The efficiency of two extraction techniques—ultrasound‐assisted extraction and pressurized liquid extraction—are compared and evaluated in the determination of parabens in compost samples. The extraction parameters for each technique were accurately optimized. The selected compounds were detected and quantified using ultra‐performance LC MS/MS, operating in negative ESI and in SRM mode. The analytes were separated in less than 5 min. Ethylparaben (ring‐¹³C₆ labeled) was used as an internal standard. Two selective, sensitive, and accurate analytical methods were developed and validated. The LODs of the methods ranged from 3 to 7 ng/g and the LOQs from 10 to 23 ng/g, while inter‐ and intraday variability was under 6% in all cases. The methods were validated separately by using matrix‐matched calibration and recovery assays with spiked samples. Recovery rates ranged from 94.0 to 105.0%. Compost samples were taken from different composting plants. Although the statistical comparison demonstrated no statistically significant differences between the two extraction techniques, the method based on pressurized liquid extraction was more sensitive than the ultrasound extraction based method.