scholarly journals Novel Silsesquioxane-Derived Boronate Esters—Synthesis and Thermal Properties

Molecules ◽  
2021 ◽  
Vol 26 (14) ◽  
pp. 4107
Author(s):  
Miłosz Frydrych ◽  
Daria Pakuła ◽  
Bogna Sztorch ◽  
Dariusz Brząkalski ◽  
Robert E. Przekop ◽  
...  

The functionalization of mono- and octahydrospherosilicate with vinylboranes and allylboranes via hydrosilylation reaction in the presence of a Karstedt’s platinum (0) catalyst is presented. This is the catalytic route to obtain a new class of silsesquioxanes containing boron atoms in their structure in high yields (>90%) and with satisfactory selectivity. The obtained compounds were fully characterized by spectroscopic (1H, 13C, 29Si NMR) and spectrometric methods (MALDI-TOF-MS), as well as thermal analysis (TGA). The obtained compounds were subjected to thermal tests, characterizing the processes of melting, thermal evaporation, sublimation and thermal decomposition.

2014 ◽  
Vol 59 (3) ◽  
pp. 1023-1027 ◽  
Author(s):  
M. Łucarz ◽  
B. Grabowska ◽  
G. Grabowski

Abstract For the practical and functional reasons the investigation of the thermal decomposition process is of an essential meaning in relation to the thermal stabilisation of materials and obtaining for them the desired thermal properties. On the other side, thermal tests are carried out in order to identify degradation mechanisms, which is important in the environment protection context, including materials reuse. The cycle of investigations in which thermal TG-DTA methods were applied as supplementary ones for the works on the optimisation of the thermal reclamation process is presented in the hereby paper. The thermal reclamation process as a utilisation method of spent moulding and core sands is more costly than other reclamation methods, but in the majority of cases it simultaneously provides the best cleaning of mineral matrices from organic binders. Thus, the application of the thermal analysis methods (TG-DTA), by determining the temperature range within which a degradation followed by a destruction of bounded organic binders in moulding sands, can contribute to the optimisation of the thermal reclamation process and to the limiting its realisation costs.


Energies ◽  
2021 ◽  
Vol 14 (5) ◽  
pp. 1316
Author(s):  
Daniel Mahon ◽  
Gianfranco Claudio ◽  
Philip Eames

To improve the energy efficiency of an industrial process thermochemical energy storage (TCES) can be used to store excess or typically wasted thermal energy for utilisation later. Magnesium carbonate (MgCO3) has a turning temperature of 396 °C, a theoretical potential to store 1387 J/g and is low cost (~GBP 400/1000 kg). Research studies that assess MgCO3 for use as a medium temperature TCES material are lacking, and, given its theoretical potential, research to address this is required. Decomposition (charging) tests and carbonation (discharging) tests at a range of different temperatures and pressures, with selected different gases used during the decomposition tests, were conducted to gain a better understanding of the real potential of MgCO3 for medium temperature TCES. The thermal decomposition (charging) of MgCO3 has been investigated using thermal analysis techniques including simultaneous thermogravimetric analysis and differential scanning calorimetry (TGA/DSC), TGA with attached residual gas analyser (RGA) and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) (up to 650 °C). TGA, DSC and RGA data have been used to quantify the thermal decomposition enthalpy from each MgCO3.xH2O thermal decomposition step and separate the enthalpy from CO2 decomposition and H2O decomposition. Thermal analysis experiments were conducted at different temperatures and pressures (up to 40 bar) in a CO2 atmosphere to investigate the carbonation (discharging) and reversibility of the decarbonation–carbonation reactions for MgCO3. Experimental results have shown that MgCO3.xH2O has a three-step thermal decomposition, with a total decomposition enthalpy of ~1050 J/g under a nitrogen atmosphere. After normalisation the decomposition enthalpy due to CO2 loss equates to 1030–1054 J/g. A CO2 atmosphere is shown to change the thermal decomposition (charging) of MgCO3.xH2O, requiring a higher final temperature of ~630 °C to complete the decarbonation. The charging input power of MgCO3.xH2O was shown to vary from 4 to 8136 W/kg with different isothermal temperatures. The carbonation (discharging) of MgO was found to be problematic at pressures up to 40 bar in a pure CO2 atmosphere. The experimental results presented show MgCO3 has some characteristics that make it a candidate for thermochemical energy storage (high energy storage potential) and other characteristics that are problematic for its use (slow discharge) under the experimental test conditions. This study provides a comprehensive foundation for future research assessing the feasibility of using MgCO3 as a medium temperature TCES material. Future research to determine conditions that improve the carbonation (discharging) process of MgO is required.


2018 ◽  
Vol 53 (15) ◽  
pp. 2053-2064 ◽  
Author(s):  
Tassos Mesogitis ◽  
James Kratz ◽  
Alex A Skordos

Thermochemical properties are needed to develop process models and define suitable cure cycles to convert thermosetting polymers into rigid glassy materials. Uncertainty surrounding the suitability of thermal analysis techniques and semi-empirical models developed for conventional composite materials has been raised for the new class of particle interleaf materials. This paper describes kinetics, conductivity, heat capacity and glass transition temperature measurements of HexPly® M21 particle interleaf material. Thermal models describing conventional, non-particle epoxy systems were fit to the data and validated through a thick-section cure. Results from curing experiments agree with heat transfer simulation predictions, indicating that established thermal analysis techniques and models can describe polymerisation and evolving material properties during processing of a material representing the class of interleaf toughened systems. A sensitivity study showed time savings up to about 20%, and associated energy-efficiency-productivity benefits can be achieved by using cure simulation for particle interleaf materials.


2013 ◽  
Vol 11 (7) ◽  
pp. 1225-1238
Author(s):  
Iliana Medina-Ramírez ◽  
Cynthia Floyd ◽  
Joel Mague ◽  
Mark Fink

AbstractThe reaction of R3M (M=Ga, In) with HESiR′3 (E=O, S; R′3=Ph3, iPr3, Et3, tBuMe2) leads to the formation of (Me2GaOSiPh3)2(1); (Me2GaOSitBuMe2)2(2); (Me2GaOSiEt3)2(3); (Me2InOSiPh3)2(4); (Me2InOSitBuMe2)2(5); (Me2InOSiEt3)2(6); (Me2GaSSiPh3)2(7); (Et2GaSSiPh3)2(8); (Me2GaSSiiPr3)2(9); (Et2GaSSiiPr3)2(10); (Me2InSSiPh3)3(11); (Me2InSSiiPr3)n(12), in high yields at room temperature. The compounds have been characterized by multinuclear NMR and in most cases by X-ray crystallography. The molecular structures of (1), (4), (7) and (8) have been determined. Compounds (3), (6) and (10) are liquids at room temperature. In the solid state, (1), (4), (7) and (9) are dimers with central core of the dimer being composed of a M2E2 four-membered ring. VT-NMR studies of (7) show facile redistribution between four- and six-membered rings in solution. The thermal decomposition of (1)–(12) was examined by TGA and range from 200 to 350°C. Bulk pyrolysis of (1) and (2) led to the formation of Ga2O3; (4) and (5) In metal; (7)–(10) GaS and (11)–(12) InS powders, respectively.


2019 ◽  
Vol 2019 ◽  
pp. 1-8
Author(s):  
Yiping Shang ◽  
Wu Yang ◽  
Yabei Xu ◽  
Siru Pan ◽  
Huayu Wang ◽  
...  

In this study, few-layered tungsten disulfide (WS2) was prepared using a liquid phase exfoliation (LPE) method, and its thermal catalytic effects on an important kind of energetic salts, dihydroxylammonium-5,5′-bistetrazole-1,1′-diolate (TKX-50), were investigated. Few-layered WS2 nanosheets were obtained successfully from LPE process. And the effects of the catalytic activity of the bulk and few-layered WS2 on the thermal decomposition behavior of TKX-50 were studied by using synchronous thermal analysis (STA). Moreover, the thermal analysis data was analyzed furtherly by using the thermokinetic software AKTS. The results showed the WS2 materials had an intrinsic thermal catalysis performance for TKX-50 thermal decomposition. With the few-layered WS2 added, the initial decomposition temperature and activation energy (Ea) of TKX-50 had been decreased more efficiently. A possible thermal catalysis decomposition mechanism was proposed based on WS2. Two dimensional-layered semiconductor WS2 materials under thermal excitation can promote the primary decomposition of TKX-50 by enhancing the H-transfer progress.


2021 ◽  
Author(s):  
Mojgan Zendehdel ◽  
Fatemeh Tavakoli

Abstract A new class of catalyst has been prepared with sulfunic acid functionalized HY zeolite (HY-N-SO3H) and characterized by FESEM, TEM, FTIR, TGA, XRD and BET. The result show that the catalyst has the micro-meso structure without ordering in the mesophase. Then, two sets of organic reaction were examined to consider of catalytic activity. The micro-meso structure HY-N-SO3H was used as an acidic catalyst to synthesis of coumarins via Pechmann reaction and facile transformation of amines to formamides under solvent free condition. This catalyst was compared with NaY-N-SO3H and MCM-N-SO3H and pure porous material to consider of the effect of acidity and kind and size of porous in the catalyst. The significant advantages of HY-N-SO3H respect to other catalyst are short reaction times, high yields, pure products, mild conditions and easy workup. In addition, we report an original and environmentally friendly solvent-free procedures which reusability of catalyst makes this method nearly green and environmental friendly.


2018 ◽  
Vol 39 (4) ◽  
pp. 21
Author(s):  
Gilbert Bannach ◽  
Rafael R. Almeida ◽  
Luis G. Lacerda ◽  
Egon Schnitzler ◽  
Massao Ionashiro

Several papers have been described on the thermal stability of the sweetener, C12H19Cl3O8 (Sucralose). Nevertheless no study using thermoanalytical techniques was found in the literature. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC) and infrared spectroscopy, have been used to study the thermal stability and thermal decomposition of sweetener.


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