PROBING THE POSTGELATION REACTIONS OF EPOXIDIZED NATURAL RUBBER CROSS-LINKED WITH DODECENYL SUCCINIC ANHYDRIDE

2015 ◽  
Vol 88 (4) ◽  
pp. 560-573 ◽  
Author(s):  
Leno Mascia ◽  
Pietro Russo ◽  
Letizia Verdolotti ◽  
Jane Clarke ◽  
Marino Lavorgna ◽  
...  

ABSTRACT Pregelled mixes of an epoxidized natural rubber, known as ENR50, containing dodecenyl succinic anhydride (DDSA) as cross-linking agent and dimethyl benzyl amine (DMBA) as catalyst, were cured isothermally at 160 °C, and the progress of the reactions was followed by both thermal analysis (differential scanning calorimetry and thermogravimetric analysis [TGA]) and infrared spectroscopy (Fourier transform near-infrared and attenuated total reflection). The curing reactions were found to be approximately first order for both heat of reaction associated with cross-linking and the disappearance of the epoxy groups, even though the reduction of epoxy group concentration was found to be substantially greater than the amount expected from reactions with the anhydride, because of the formation of large quantities of vicinal OH groups. The TGA data have indicated that the pregelled mixes undergo more extensive anaerobic degradation at higher temperatures than the un–cross-linked elastomer, which is accelerated by the presence of the DMBA catalyst.

2014 ◽  
Vol 132 (6) ◽  
pp. n/a-n/a ◽  
Author(s):  
Leno Mascia ◽  
Jane Clarke ◽  
Kiat Seong Ng ◽  
Kok Sien Chua ◽  
Pietro Russo

2017 ◽  
Vol 231 (11-12) ◽  
Author(s):  
Tianlin Cao ◽  
Fanyu Zhao ◽  
Zulin Da ◽  
Fengxian Qiu ◽  
Dongya Yang ◽  
...  

AbstractIn this work, an amino-functionalized graphene oxide (AFGO) was synthesized by graphene oxide (GO) and ethylene diamine. A novel amino-functionalized graphene oxide/azobenzene polyimide (AFGO/ACPI) was synthesized with AFGO, azobenzene chromophore and pyromellitic dianhydride (PMDA). The structure, mechanical and thermal property of AFGO/ACPI were characterized and measured by fourier transform infrared, UV-visible spectroscopy, near-infrared spectrum, thermogravimetric analysis and differential scanning calorimetry. To obtain the refractive index of AFGO/ACPI at different temperature and wavelength (532 nm, 650 nm and 850 nm), the attenuated total reflection (ATR) method was used to measure, and thermo optic coefficients (dn/dT) were −7.22×10


2013 ◽  
Vol 33 (7) ◽  
pp. 579-588 ◽  
Author(s):  
S.T. Sam ◽  
H. Ismail ◽  
H.P.S. Abdul Khalil

Abstract In the present study, linear low density polyethylene (LLDPE)/soya powder blends were compatibilized with epoxidized natural rubber (ENR 50) and exposed to natural weathering. The exposure period for the blends was 1 year. It was found that the degradability of the compatibilized blends was higher than that of uncompatibilized blends. Fourier transform infrared (FTIR) spectra, the tensile test, scanning electron microscopy (SEM), and differential scanning calorimetry (DSC) were applied to analyze the degradability of the blends. IR spectra showed that the carbonyl index (CI) of the blends increased as a function of exposure period and soya powder content. The compatibilized blends gave higher carbonyl indices. The retention tensile strength and elongation at break (Eb) of the compatibilized blends after weathering was generally lower than for the uncompatibilized blends. The increase of crystallinity also indicated a reduction of the amorphous portion after degradation. The higher crystallinity in compatibilized blends further confirms the higher degradability of ENR 50 compatibilized blends. The weight loss and molecular weight change indicated that the incorporation of ENR 50 into LLDPE/soya powder blends can enhance the degradability of the blends upon outdoor exposure.


2007 ◽  
Vol 61 (9) ◽  
pp. 928-934 ◽  
Author(s):  
Dagmara Wojtków ◽  
Mirosław A. Czarnecki

The effect of temperature on attenuated total reflection infrared (ATR-IR) and near-infrared (NIR) transmission spectra of pure butan-1-ol, butan-2-ol, 2-methyl-propan-1-ol, 2-methyl-propan-2-ol, and mixtures with a small water content (XH2O ≤ 0.1) have been examined. The spectra were analyzed using a two-dimensional (2D) correlation approach. Two kinds of correlation analysis were performed: IR–IR and NIR–NIR homo-correlation and IR–NIR hetero-correlation. Our results reveal that the addition of small to moderate amounts of water does not destroy the structure of alcohol. The presence of water stabilizes the structure of alcohols and this effect is more evident for sec-butanol and tert-butanol. The ATR-IR spectra provide information on the most associated species, whereas absorption of the smaller associates and the free OH group is hardly seen. On the contrary, in the NIR spectra the absorption of the free OH groups dominates. The ability of resolution enhancement in the hetero-correlation asynchronous spectra is reduced as compared to that in the homo-correlation spectra. On the other hand, peaks may appear in the hetero-correlation synchronous spectra that are not observed in the homo-correlation contour plots. The positions of the synchronous peaks were used for evaluation of anharmonicity constants. These values for the free OH group do not depend on the experimental conditions. In contrast, the anharmonicity constants for the bonded OH groups determined from the spectra of pure alcohols may significantly differ from those obtained from diluted solutions.


2018 ◽  
Vol 51 (5) ◽  
pp. 406-420 ◽  
Author(s):  
Nuttida Srirachya ◽  
Takaomi Kobayashi ◽  
Kumarjyoti Roy ◽  
Kanoktip Boonkerd

In this article, thermoreversible covalent cross-linking of maleated natural rubber (MNR) with glycerol was studied. Firstly, NR was grafted with maleic anhydride using a reactive processing method. The result showed that MNR was successfully obtained without the addition of initiator. The highest grafting was 1.76%. Secondly, the obtained MNR was dissolved in toluene and then mixed with glycerol, which is used in this study as the thermoreversible cross-linking agent. Fourier transform infrared spectra of the casted MNR film mixed with glycerol showed that upon heating, covalent ester cross-links were formed via the reaction of succinic anhydride ring with hydroxyl groups of glycerol. The swelling test indicated that the swelling index (%) decreased with increasing glycerol loading. This indicated that the degree of cross-linking directly depended on the amount of glycerol. The tensile strength and modulus were significantly improved upon increasing the level of cross-linking. The MNR cross-linked with glycerol can be remolded at 150°C more than three times. After remolding, the mechanical properties decreased with increasing recycling round.


2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Lisa Rebers ◽  
Raffael Reichsöllner ◽  
Sophia Regett ◽  
Günter E. M. Tovar ◽  
Kirsten Borchers ◽  
...  

AbstractGelatin methacryloyl (GM) hydrogels have been investigated for almost 20 years, especially for biomedical applications. Recently, strengthening effects of a sequential cross-linking procedure, whereby GM hydrogel precursor solutions are cooled before chemical cross-linking, were reported. It was hypothesized that physical and enhanced chemical cross-linking of the GM hydrogels contribute to the observed strengthening effects. However, a detailed investigation is missing so far. In this contribution, we aimed to reveal the impact of physical and chemical cross-linking on strengthening of sequentially cross-linked GM and gelatin methacryloyl acetyl (GMA) hydrogels. We investigated physical and chemical cross-linking of three different GM(A) derivatives (GM10, GM2A8 and GM2), which provided systematically varied ratios of side-group modifications. GM10 contained the highest methacryloylation degree (DM), reducing its ability to cross-link physically. GM2 had the lowest DM and showed physical cross-linking. The total modification degree, determining the physical cross-linking ability, of GM2A8 was comparable to that of GM10, but the chemical cross-linking ability was comparable to GM2. At first, we measured the double bond conversion (DBC) kinetics during chemical GM(A) cross-linking quantitatively in real-time via near infrared spectroscopy-photorheology and showed that the DBC decreased due to sequential cross-linking. Furthermore, results of circular dichroism spectroscopy and differential scanning calorimetry indicated gelation and conformation changes, which increased storage moduli of all GM(A) hydrogels due to sequential cross-linking. The data suggested that the total cross-link density determines hydrogel stiffness, regardless of the physical or chemical nature of the cross-links.


Polymers ◽  
2021 ◽  
Vol 13 (23) ◽  
pp. 4145
Author(s):  
Kriengsak Damampai ◽  
Skulrat Pichaiyut ◽  
Subhradeep Mandal ◽  
Sven Wießner ◽  
Amit Das ◽  
...  

In this work, studies are carried out to understand the crosslinking reaction of epoxidized natural rubber (50 mol% epoxy, ENR-50) by metal ion namely ferric ion (Fe3+, FeCl3, ferric chloride). It is found that a small amount of FeCl3 can cure ENR to a considerable extent. A direct interaction of the ferric ion with the epoxy group as well as internal polymerization enable the ENR to be cured in an efficient manner. It was also found that with the increased concentration of FeCl3, the crosslinking density of the matrix increased and therefore, the ENR offers higher mechanical properties (i.e., modulus and tensile strength). In addition, the glass transition temperature (tg) of ENR vulcanizate is increased with increasing concentration of FeCl3. Moreover, the thermal degradation temperature (Td) of the ENR-FeCl3 compound was shifted toward higher temperature as increasing concentration FeCl3.


2016 ◽  
Vol 138 (4) ◽  
Author(s):  
Klaus J. Geretschläger ◽  
Gernot M. Wallner ◽  
Ingrid Hintersteiner ◽  
Wolfgang Buchberger

This paper describes and evaluates accelerated aging of a titanium dioxide (TiO2) filled polyamide (PA) based backsheet film for photovoltaic (PV) modules. Damp heat exposure (85%RH, 85 °C) was carried out up to 2000 hrs. The backsheet was characterized using microscopic, spectroscopic, thermoanalytic, chromatographic, and mechanical methods. While Raman microscopy, infrared spectroscopy in attenuated total reflection mode (IR-ATR), scanning calorimetry (DSC), and thermal gravimetric analysis did not reveal aging-induced changes, significant yellowing was detected by ultraviolet visible near infrared (UV/VIS/NIR) spectroscopy. Depending on the stabilizer type (UV-absorbers, hindered amine light stabilizers (HALSs), and antioxidants), rather different consumption rates were ascertained by high-performance liquid chromatography (HPLC) and gas chromatography (GC). Although the ultimate mechanical properties decreased significantly, no full embrittlement was obtained after damp heat exposure of up to 2000 hrs. The observed physical and chemical aging mechanisms were classified as within the induction period without premature failure.


2012 ◽  
Vol 85 (1) ◽  
pp. 147-156 ◽  
Author(s):  
Sa-Ad Riyajan ◽  
Suwit Chaiponban ◽  
Sasitorn Chusri ◽  
Supayang Piyawan Voravuthikunchai

Abstract Properties and antibacterial activity of polymer blend films prepared from polyvinyl alcohol (PVA) and natural rubber (NR) blends, in the presence of maleic acid as a cross-linking agent were studied. The effect of the maleic acid content, curing temperature, and curing time on the properties of the polymer blend was investigated. Cross-linking between PVA and maleic acid was observed by attenuated total reflection mode–Fourier transform infrared spectroscopy at 1152 cm−1. The swelling ratio of the polymer blend decreased as a function of the increase of the maleic acid content. The tensile strength of the polymer blend increased with an increase of both the maleic acid and the curing time. The highest tensile strength of the samples was observed with 40% w/w maleic acid after a 24 h curing time at 120 °C. The elongation at the break of 60/40 NR/PVA was ∼500% at 120 °C for 1 h. In addition, the polymer blend showed good antibacterial activity with Staphylococcus aureus ATCC25923, Escherichia coli ATCC25922, and Acinetobacter baumannii JVC 1053 and could find many applications.


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