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A new cocrystal of pyrazinamide with oxalic acid was prepared mechanochemically and characterized by PXRD, Raman spectroscopy, solid-state NMR spectroscopy, DTA-TG, and SEM. Based on powder X-ray diffraction data the structure was solved. The formation pathway of the reaction was studied in situ using combined synchrotron PXRD and Raman spectroscopy. Using oxalic acid dihydrate the initially neat grinding turned into a rapid self-accelerated liquid-assisted grinding process by the release of crystallization water. Under these conditions, the cocrystal was formed directly within two minutes.
The production and processing of ordinary Portland cement are responsible for nearly 5% of the world C02 emissions. Due to the world’s increasing requirement for building materials, this air pollution is growing up in the next decades. Alternative cement such as geopolymers can reduce these emissions effectively, Conventional geopolymer binders, produced ffom fly ash or metakaolin as aluminosilicate source and water-glass or alkali hydroxide Solutions as activator, are often used and studied. It is known that under appropriate conditions the starting materials form a three-dimensional aluminosilicate structure and create a gel-like matrix, In our case, a silica source from wastewater treatment of chlorosilane production and solid sodium aluminate as starting materials are initiated to harden by water. This procedure is known as “just add water” or “one-part” geopolymer formulation. These composites have significant advantages for use on construction site, but their Chemical structure is not extensively analyzed. In this work, a well known one-part geopolymer is investigated by 'H and 27A1 magic-angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy. Furthermore, it is shown that overlapping NMR lines can resolved with echo experiments and
The need to improve the sustainability and the need for innovation in the cement industry has brought to light the practice of using additives to the cement in order to decrease CO2 emissions in industrial plants and increase the quality of cement in terms of durability and performance. Currently some additives have been employed as granulated blast furnace slag, limestone and pozzolan. The additives give mortar and concrete larger energy efficiency, gain in durability and resistance, contributing to buildings with slender structures and cheaper and durable maintenance. Besides natural pozzolan can be used artificial ones, as calcined clays, and over a range of amorphous aluminates and silicates waste, with highly reactive function as a binder material in the presence of water and calcium hydroxide. Calcined kaolinite clays were characterized using various techniques such as XRD, thermal analysis, and NMR observing 27Al and 29Si nuclei. The results showed that there is a structural modification of the samples, from crystalline to amorphous phases with the increasing of temperature in the calcination process. There is an improving in the reactivity of calcined clays by the range of 600ºC to 750ºC temperature in the reaction with calcium oxide, according to data from Chapelle test, indicating the possibility of using them as additives for cement and confirming their pozzolanic potential.
A systematic comparison of chemical interactions and fire behaviour is presented for the thermoplas-tic elastomer (block copolymer styrene-ethylene-butadiene-styrene) (TPE-S)/diethyl- and methylvinylsiloxane (Si)/poly(phenylene oxide) (PPO), flame-retarded with aluminium diethylphosphinate (AlPi)and with ammonium polyphosphate (APP), respectively. TPE-S/APP/Si/PPO performed better in the conecalorimeter test (reduction in peak heat release rate from 2042 to 475 kW m−2), but TPE-S/AlPi/Si/PPO inthe flammability tests (oxygen index (OI) and UL 94). This difference was caused by the different modes ofaction of APP (more in the condensed phase) and AlPi (mainly in the gas phase). Thermogravimetry cou-pled with Fourier transform infrared spectroscopy (TG-FTIR) was used to analyse the mass loss and theevolved gas products, while a Linkam hot-stage cell to investigate the decomposition in the condensedphase. Moreover, a detailed analysis of the fire residues was done using solid-state NMR.13C MAS NMRshowed that both flame-retarded compositions form graphite-like amorphous carbonaceous char, orig-inating from PPO.31P MAS NMR and29Si MAS NMR delivered important information about interactionbetween phosphorus and the siloxane. For TPE-S/AlPi/Si/PPO aluminium phosphate and silicon dioxideoccurred, while also silicophosphate was produced in TPE-S/APP/Si/PPO. The direct comparison of two ofthe most prominent halogen-free flame retardants containing phosphorus delivered meaningful insightsinto the modes of action and molecular mechanisms controlling flame retardancy.
The stability of different theophylline cocrystals under milling conditions was investigated by competitive cocrystal reactions. To determine the most stable cocrystal form under milling conditions, the active pharmaceutical ingredient theophylline was either ground with two similar coformers (benzoic acid, benzamide, or isonicotinamide), or the existing theophylline cocrystals were ground together with a competitive coformer. All competitive reactions were investigated by in situ powder X-ray diffraction disclosing the formation pathway of the milling processes. On the basis of these milling reactions, a stability order (least to most stable) was derived: tp/bs < tp/ba < tp/ina < bs/ina.
Distinct approaches are used to reduce the fire risks of polymers, a key issue for many industrial applications. Among the variety of approaches, the use of synergy in halogen-free multicomponent systems is one of the most auspicious. To optimize the composition of such flame-retardant systems it is essential to understand the mechanisms and the corresponding chemistry in the condensed phase. In this work different methods are used, including cone calorimeter, thermogravimetry (TG), and TG-FTIR, with the main focus on the solid-state NMR analysis of the solid residues. The structural changes in the condensed phase of two thermoplastic elastomer systems based on copolymer styrene-ethylene-butadiene-styrene (TPE-S) were investigated: TPE-S/aluminium diethylphosphinate (AlPi)/magnesium hydroxide (MH) and TPE-S/AlPi/zinc borate (ZB)/poly(phenylene oxide) (PPO). Strong flame inhibition is synergistically combined with protective layer formation. 13C-, 27Al-, 11B- and 31P MAS NMR (magic angle spinning nuclear magnetic resonance) experiments using direct excitation with a single pulse and 1H31P cross-polarization (CP) were carried out as well as double resonance techniques. Magnesium phosphates were formed during the pyrolysis of TPE-S/AlPi/MH, while for the system TPE-S/AlPi/ZB/PPO zinc phosphates and borophosphates were observed. Thus, the chemistry behind the chemical interaction was characterized unambiguously for the investigated systems.