Preparation and Characterization of Degradable Poly(silyl ester) and the Self-Crosslinking Reaction of Poly(silyl ester) without Solvent

2010 ◽  
Vol 129-131 ◽  
pp. 862-866
Author(s):  
De Jie Zhou ◽  
Nian Feng Han ◽  
Xin De Tang

The new poly(silyl ester) has been prepared by the polycondensation reaction of 1,5-dichloro-1,1,5,5-tetramethyl-3,3-diphenyl-trisi1oxane with di-tert-butyl fumarate by the elimination of tert-butyl chloride as a driving force. To investigate the self-crosslinking reaction of the unsaturated poly(silyl ester), poly(1,1,5,5-tetramethyl-3,3-diphenyltrisiloxane) was self- crosslinked in the presence of 2, 2'-azobis(isobutyronitri1e) (AIBN) as a radical initiator without solvent. After the self-crosslinking, the unsaturated poly(silyl ester), which was viscous liquids, turned into solid product. The characterization of the poly(silyl ester) and the self-crosslinked product included 1H-NMR spectroscopy, differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). Comparisons were made between the linear poly(silyl ester) and the self-crosslinked products. It was found that after crosslinking, the important resonance signal for ethenylene (C=C) of the poly(silyl ester) reduced, which show that the crosslinking reaction is carried out. The self-crosslinked product exist the structures of linear isomer and four-membered ring isomer. The glass-transition temperatures of the self-crosslinked poly(silyl ester) was higher than that of the uncrosslinked poly(silyl ester), and the thermal stability of the self-crosslinked poly(silyl ester) was better than that of uncrosslinked poly(silyl ester).

2010 ◽  
Vol 129-131 ◽  
pp. 113-117
Author(s):  
Nian Feng Han ◽  
De Jie Zhou ◽  
Xin De Tang

The unsaturated poly(silyl ester) has been prepared by the polycondensation reaction of 1, 3-dichloro-tetramethyldisiloxane with di-tert-butyl fumarate. To investigate the crosslinking reaction of the unsaturated poly(silyl ester), poly(tetramethyl disilyloxyl fumarate) was self-crosslinked and cocrosslinked with styrene in the presence of 2, 2'-azobis(isobutyronitri1e) (AIBN) as a radical initiator. After the crosslinking, the unsaturated poly(silyl ester)s, which were viscous liquids, turned into solid products. The characterization of the poly(silyl ester) and the crosslinked product included infrared (IR) spectroscopy, differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). Comparisons were made between the linear poly(silyl ester) and the crosslinked products. It was found that after crosslinking, the important resonance signal for ethenylene (C=C) of the poly(silyl ester) disappeared, which show that the crosslinking reaction is carried out progressively. The glass-transition temperatures of the self-crosslinked and cocrosslinked product were higher than that of the uncrosslinked poly(silyl ester), and the thermal stability of the crosslinked poly(silyl ester)s was better than that of uncrosslinked poly(silyl ester). In degradation tests, the self-crosslinked product degradable completely in 35 minutes and the cocrosslinked product complete mass loss in 5 days and the release of PNA followed the degradation of the crsslinked product. The rate of degradation of the poly(silyl ester) decreased after the crosslinking.


2019 ◽  
pp. 089270571987822
Author(s):  
Saud Aldajah ◽  
Mohammad Y Al-Haik ◽  
Waseem Siddique ◽  
Mohammad M Kabir ◽  
Yousef Haik

This study reveals the enhancement of mechanical and thermal properties of maleic anhydride-grafted polypropylene (PP- g-MA) with the addition of nanocrystalline cellulose (NCC). A nanocomposite was manufactured by blending various percentages of PP, MA, and NCC nanoparticles by means of a twin-screw extruder. The influence of varying the percentages of NCC on the mechanical and thermal behavior of the nanocomposite was studied by performing three-point bending, nanoindentation, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and Fourier-transform infrared (FTIR) spectroscopy tests. The novelty of this study stems on the NCC nanoparticles and their ability to enhance the mechanical and thermal properties of PP. Three-point bending and nanoindentation tests revealed improvement in the mechanical properties in terms of strength, modulus, and hardness of the PP- g-MA nanocomposites as the addition of NCC increased. SEM showed homogeneity between the mixtures which proved the presence of interfacial adhesion between the PP- g-MA incorporated with NCC nanoparticles that was confirmed by the FTIR results. DSC and TGA measurements showed that the thermal stability of the nanocomposites was not compromised due to the addition of the coupling agent and reinforced nanoparticles.


2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
Emi Govorčin Bajsić ◽  
Vesna Rek ◽  
Ivana Ćosić

The effect of the addition of talc on the morphology and thermal properties of blends of thermoplastic polyurethane (TPU) and polypropylene (PP) was investigated. The blends of TPU and PP are incompatible because of large differences in polarities between the nonpolar crystalline PP and polar TPU and high interfacial tensions. The interaction between TPU and PP can be improved by using talc as reinforcing filler. The morphology was observed by means of scanning electron microscopy (SEM). The thermal properties of the neat polymers and unfilled and talc filled TPU/PP blends were studied by using dynamic mechanical analysis (DMA), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). The addition of talc in TPU/PP blends improved miscibility in all investigated TPU/T/PP blends. The DSC results for talc filled TPU/PP blends show that the degree of crystallinity increased, which is due to the nucleating effect induced by talc particles. The reason for the increased storage modulus of blends with the incorporation of talc is due to the improved interface between polymers and filler. According to TGA results, the addition of talc enhanced thermal stability. The homogeneity of the talc filled TPU/PP blends is better than unfilled TPU/PP blends.


2020 ◽  
Vol 2020 ◽  
pp. 1-9 ◽  
Author(s):  
Jiangtao Xing ◽  
Weili Wang ◽  
Wenzheng Xu ◽  
Tianle Yao ◽  
Jun Dong ◽  
...  

In order to improve the safety of hexanitrohexaazaisowurtzitane (CL-20), submicron CL-20 particles were prepared by a siphon ultrasonic-assisted spray refining experimental device. The samples were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and differential scanning calorimetry (DSC), and the impact sensitivity of the samples was tested. The results show that the particle size of siphon-refined CL-20 is about 800 nm~1 μm, which is more smooth, mellow, and dense than that of CL-20 prepared by a traditional pressure-refined method. The peak diffraction angle of pressure- and siphon-refined CL-20 is basically the same as that of raw CL-20, and their crystal forms are ε type. The peak strength of pressure- and siphon-refined CL-20 decreased obviously. The apparent activation energy of pressure-refined CL-20 and siphon-refined CL-20 is 13.3 kJ/mol and 11.95 kJ/mol higher than that of raw CL-20, respectively. The thermal stability of CL-20 is improved. The activation enthalpy (ΔH#) is significantly higher than that of raw CL-20, and the characteristic drop is 70.4% and 82.7% higher than that of raw CL-20. The impact sensitivity of siphon-refined CL-20 is lower than that of pressure-refined CL-20, so the safety performance of an explosive is improved obviously.


2012 ◽  
Vol 727-728 ◽  
pp. 1552-1556
Author(s):  
Renata Barbosa ◽  
Dayanne Diniz Souza ◽  
Edcleide Maria Araújo ◽  
Tomás Jefférson Alves de Mélo

Studies of degradation have verified that the decomposition of some quaternary ammonium salts can begin to be significant at the temperature of about 180 ° C and like most thermoplastics are processed at least around this temperature, the thermal stability of the salt in clay should always be considered. Some salts are more stable than others, being necessary to study the degradation mechanisms of each case. In this work, four quaternary ammonium salts were characterized by differential scanning calorimetry (DSC) and thermogravimetry (TG). The results of DSC and TG showed that the salts based chloride (Cl-) anion begin to degrade at similar temperatures, while the salt based bromide (Br-) anion degrades at higher temperature. Subsequently, a quaternary ammonium salt was chosen to be used in organoclays, depending on its chemical structure and its thermal behavior.


2000 ◽  
Vol 15 (7) ◽  
pp. 1617-1621 ◽  
Author(s):  
Jan Schroers ◽  
Konrad Samwer ◽  
Frigyes Szuecs ◽  
William L. Johnson

The reaction of the bulk glass forming alloy Zr41Ti14Cu12Ni10Be23 (Vit 1) with W, Ta, Mo, AlN, Al2O3, Si, graphite, and amorphous carbon was investigated. Vit 1 samples were melted and subsequently solidified after different processing times on discs of the different materials. Sessile drop examinations of the macroscopic wetting of Vit 1 on the discs as a function of temperature were carried out in situ with a digital optical camera. The reactions at the interfaces between the Vit 1 sample and the different disc materials were investigated with an electron microprobe. The structure and thermal stability of the processed Vit 1 samples were examined by x-ray diffraction and differential scanning calorimetry. The results are discussed in terms of possible applications for composite materials.


2011 ◽  
Vol 327 ◽  
pp. 115-119 ◽  
Author(s):  
Duo Wang ◽  
Jie Gao ◽  
Wei Fang Xu ◽  
Feng Bao ◽  
Rui Ma ◽  
...  

Graphene oxide (GO) was made by a modified Hummers method. Graphene oxide modified phenolic resin nanocomposites (GO/PF) were prepared by Steglich esterification, catalyzed by dicyclohexyl carbodiimide and 4-dimethylaminopyridine. The composites were characterized by Fourier transform infrared spectrometry, differential scanning calorimetry, X-ray powder diffraction, and scanning electron microscopy. The result revealed that the graphene oxide was absolutely exfoliated and covalent linked GO/PF composite was obtained. The thermal stability of PF is remarkably improved by modification with GO.


2021 ◽  
pp. 152808372110417
Author(s):  
Zhou Zhao ◽  
Ningning Tong ◽  
Hong Song ◽  
Yan Guo ◽  
Jinmei Wang

In this work, a phase-change energy storage nonwoven fabric was made of polyurethane phase-change material (PUPCM) by a non-woven melt-blown machine. Polyethylene glycol 2000 was used as the phase transition unit and diphenyl-methane-diisocyanate as the hard segment to prepare PUPCM. Thermal stability of the PUPCM was evaluated through thermal stability analysis. The performance of pristine PUPCM was determined by Fourier transform infrared spectroscopy and differential scanning calorimetry to analyze the spinning technology of spinning temperature and the stretching process. Phase-change energy storage nonwoven fabric (413.22 g/m2) was prepared, and the morphology, solid–solid exothermic phase transition, mechanical properties, and the structures were characterized. The enthalpy of solid–solid exothermic phase transition reached 60.17 mJ/mg (peaked at 23.14°C). The enthalpy of solid–solid endothermic phase transition reached 67.09 mJ/mg (peaked at 34.34°C). The strength and elongation of phase-change energy storage nonwoven fabric were found suitable for garments and tent fabrics.


2013 ◽  
Vol 8 (2) ◽  
pp. 155892501300800 ◽  
Author(s):  
Weixing Xu ◽  
Yichao Lu ◽  
Bin Wang ◽  
Jianjun Xu ◽  
Guangdou Ye ◽  
...  

A convenient method for preparing the thermal regulating fibers with high latent heat has been developed. PVA thermal regulating fibers were prepared via a wet spinning process, with paraffin being the phase change material. The structures and properties of these fibers were investigated by SEM, TGA, DSC and tensile strength tester. With the paraffin content in the fibers increasing from 30wt% to 70wt%, the latent heat of the fibers increases from 42.8J/g to 87.8J/g and the paraffin phase structures change from separation into partial interconnection. PVA matrix can not wrap paraffin effectively when the paraffin content increases up to 50wt%, so the paraffin loss in the spinning process increases. The thermal stability of fibers with low paraffin content is better than that of fibers with high paraffin content. After 100 heat-and-cool cycles, the latent heat of fibers lose a little. The tensile strength of these thermal regulating fibers is good enough for application in wrapping, filling, and nonwovens.


2008 ◽  
Vol 62 (4) ◽  
Author(s):  
Hamada Abdel-Razik

AbstractSynthesis, characterization and application of diaminomaleonitrile (DAMN)-functionalized polystyrene grafts were studied. Dibenzoyle peroxide (BP) was used as an initiator. Optimum conditions for grafting were found to be c(DAMN) = 0.5 M, c(BP) = 0.016 M, θ = 85 °C and t = 4 h. Water uptake of the polystyrene graft membranes was found to increase with the increase of the grafting yield. The chemical structure, thermal characteristics and thermal stability of the obtained membranes were investigated by means of FTIR spectroscopy, differential scanning calorimetry, and thermal gravimetric analysis. Polystyrene graft membrane with the degree of grafting of up to 96 % was found to be useful for the pervaporation separation of phenol/water mixtures.


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