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Several attempts have been made to compatibilize immiscible blends by introducing suitably-chosen polymer additives. This work studies the EPDM elastomer, chemically modified with maleic anhydride (MA), through reaction in solution of EPDM and MA, using dibenzoyl peroxide as an initiator. The best conditions for obtaining the maximum grafting were...
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... anhydride (Merck) and dibenzoyl peroxide (VETEC) were recrystallized from chloroform and ethanol respectively, and were employed according to standard procedures. The EPDM was used as received without any additional purification. Small pieces of EPDM elastomer were added to chlorobenzene and heated while stirring. When the temperature reached 80 °C, solutions of maleic anhydride and dibenzoyl peroxide in chlorobenzene were added to the vessel and reacted for different times at this temperature. Then, the graft EPDM-g-MA was precipitated in methanol and it was washed several times with acetone, maintaining it under vacuum at 40 °C for 24 h. The physical mixtures (EPDM/MA) were prepared by dissolving undiluted components in chloroform by stirring and maintaining them at room temperature until complete solvent evaporation. FTIR spectra of EPDM, EPDM-g-MA and EPDM/MA films were carried out in a 16 PC Perkin Elmer spectro- photometer, equipped with a multiple reflectance acces- sory, resolution 4 cm -1 , and performing 20 scans. The films were supported on KRS-5 crystal. In the case of the presence of close bands in the analysis, the spectra can be fitted to evaluate the real contribution of each one, using Origin 4.1 software with Gaussian or Lorentzian bases. The same band height relations were obtained for both functions. Initially, we describe the procedure for determining the extent of grafting of maleic anhydride on to the backbone of the EPDM macromolecule by FTIR spectrum. Figure 1 shows the multiple internal reflectance infrared spectrum of EPDM and EPDM-g-MA, where the inside numbers indicate the assignment according to absorption group as described in Table 1. We may observe the C=O stretching band of maleic anhydride at 1856 (low intensity) and 1780 cm -1 (medium intensity) 5,6 , and a band at 1707 cm -1 due to the C=O stretching group of hydrolised MA in EPDM-g- MA 6 . The band at 922 cm -1 is due to angular deformation outside the plane of the OH hydrogen bonding, which is indicative of MA incorporated in the EPDM rubber. However, the maleic anhydride is partially converted to the acid form under room conditions, and the control of probable mixture of the two extreme forms is very difficult because it is a function of many variables. In order to avoid quanti- ties in both forms, maleic anhydride was totally converted to maleic acid, maintaining it above a water vapour for 4 h, as shown in Fig. 2. We may observe the rise of a band at 1707 cm -1 and the disappearance of bands at 1856 and 1780 cm -1 . This process is reversible, if this sample is heated at 100 °C under vacuum for 24 h 7 . Figure 3 shows the infrared spectrum of maleic anhydride and maleic acid, with only one clear band at 1707 cm -1 in the range of 1690 and 1890 cm -1 . No shifts are observed in the characteristic bands of maleic anhydride grafting or in the physical mixture with EPDM, indicating no change in the group vibration according to whether the components are covalently linked or not. This observation can facilitate the obtention of the calibration curve for the physical mixture. The calibration curve was prepared from the spectrum of physical mixtures of different compositions of maleic acid and EPDM, using the ratio from band heights at 1707 (maleic acid) and 1460 cm (EPDM). These two characteristic bands of each component permit the use of infrared as a quantitative method. However, it is necessary to obtain the calibration curve for the same EPDM, due to a possibility of variable content of ethylene and propylene in the main elastomer chain. The fitting of the spectrum bands was necessary in order to evaluate the ability of different mixtures to abolish the contribution of the band at 1430 cm -1 in the total absorbance and also to avoid intrinsic error . The Lorenz and Gauss mathematical functions give comparable band heights which are different, rising when the MA concentration increases without curve fit. This behavior is expected because the rise of maleic acid increases the band overlay. Figure 4 shows a typical spectrum of EPDM/maleic acid physical mixture with and without fit. Figure 5 shows the band ratio, h 1707 /h 1460 , as a function of different maleic acid concentrations. The linear relation is observed when the fit is used, in contrast to results without fit for the upper concentration of 4%. The grafting of maleic acid on EPDM can be estimated by the curve shown in Fig. 5 as 1.9% weight or 1.9 x 10 -4 mol/g. The determination of grafting maleic anhydride grade was made on a commercial sample of EPDM-g-MA, after being changed into the maleic acid form. The h 1707 /h 1460 ratio was determined in the infrared spectrum (Fig. 6) as equal to 0.07, and the grafting maleic anhydride was obtained from the graph in Fig. 5 as equal to 0.6%. This value agrees with that given by the company supplying the product. There is no effect of maleic anhydride concentration on the degree of maleic anhydride grafting of EPDM (1.7% of diene) rubber, using 2.0 g of EPDM and 0.15 g of dibenzoyl peroxide, at 80 °C for 3 h. The conversion reached a maximum value at 1.9 % weight for all MA ranges studied. This value corresponds to at least 2.9 x 10 -3 g or 2.9 x 10 -4 mol of MA, indicating an equimolar relation with the diene percentage in EPDM monomeric units. The maleic anhydride grafting, at 80 °C and 0.15 g of dibenzoyl peroxide, 2.9 x 10 -3 g maleic anhydride and 2.0 g of EPDM, rises to a maximum after 3 h of reaction (Fig. 7). The conditions described above were used in all experiments to evaluate the MA grafting content. The presence of maleic anhydride grafting on EPDM was made evident by infrared analysis, and it was possible to detect the carboxyl group band of maleic anhydride at 1856 and 1780 cm -1 . The infrared spectrum with band fit minimizes the error in determining the content of maleic acid and it is a simple and useful method for evaluating the percentage of grafting, using the ratio from band heights of the infrared spectrum at specific wave numbers correspond- ing to each component in the ...
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... These peaks correspond to the asymmetric and symmetric bending vibrations of methyl groups, namely, CH 3 [40]. Meanwhile, the 720/cm absorption band signifies the ethylene characteristics inherited from the EPDM structure [41]. ...
... PP/EPDM exhibited a melting peak at ∼167°C in addition to a slight melting peak at ∼51°C. The higher melting peak was dominated by PP (propylene component) while the lower melting peak was dominated by EPDM (ethylene component) [33,41]. With the addition of MgO to PP/EPDM, the higher melting peak reduced to ∼164°C. ...
Thermoplastic polypropylene (PP) has garnered a significant attention in power cable insulation research because of its exceptional thermal tolerance and dielectric properties. Due to its poor impact strength at room temperature, PP has been blended with various elastomers, including ethylene-propylene-diene monomer (EPDM), to improve the mechanical stiffness of the final material. This, however, comes with compromised dielectric properties of the material. Recently, the addition of nanofillers to polymers has demonstrated promising properties that can be tailored for various dielectric applications, provided that nanofiller and polymer interactions are appropriately formulated. Nevertheless, the effect of nanostructuration in PP/elastomer blends, especially from the perspective of dielectrics, have yet to be systematically explored. In the current work, magnesia (MgO) nanofiller is added to a model PP/EPDM blend system to determine the effect of MgO on the breakdown properties of PP/EPDM. The results show that adding 0.5 wt% of MgO to PP/EPDM reduces the AC and DC breakdown strengths by 7% and 16%, respectively. As the amount of MgO increases to 3 wt%, the AC and DC breakdown strength reduces further by 25% and 29%, respectively. Significantly, appropriate modification of the nanocomposites with polypropylene-graft-maleic anhydride (PP-g-MAH) can result in 5% higher breakdown strength of the nanocomposites with respect to comparable nanocomposites without modification. The mechanisms surrounding these breakdown effects are discussed with the aid of materials structure interpretations. Overall, the results demonstrate that appropriate modification of nanocomposites with PP-g-MAH is crucial in tailoring breakdown properties of PP blend nanocomposites.
... The stretching vibration due to the O-H stretching could be observed at 3616 cm − 1 and 3629 cm − 1 in rGO-CdS and CdS-rGO-WO 3, respectively [70]. The C --O stretching of COOH groups in reduced graphene oxide (rGO) was observed at 1856 cm − 1 and 1850 cm − 1 in CdS-rGO-WO 3 and rGO-CdS, respectively [71]. The peak at 630 cm − 1 corresponded to the Cd-O stretching [72] and the stretching peaks near 969 cm − 1 could be ascribed to W --O and W-O bond formation [73]. ...
Reduced graphene oxide (rGO) solid state mediator based Z scheme photocatalyst CdS-rGO-WO 3 heterojunction comprising of nano-rods of CdS and nanoplates of WO 3 was fabricated in-situ by a facile hydrothermal process, characterized and tested for solar hydrogen generation. The systematically designed heterojunction created separated oxidative and reductive sites for photo generated electron hole pairs with enhanced redox ability, improving the charge separation and photo-stability, mitigating the problem of photo-corrosion of CdS. This was evident from an enhanced photocatalytic activity of 11.69 mmolg − 1 h − 1 which was almost 2.3 times than pristine CdS (4.9 mmolg − 1 h − 1), in presence of simulated solar light. Due to the high electron mobility property of gra-phene sheet, rapid transport of electrons was possible at the interface between CdS and WO 3. The charge transfer via Z scheme mechanistic pathway was verified by X-ray Photoelectron Spectroscopy (XPS), Photoluminescence (PL) and photocurrent measurement studies. This research study will provide a newer insight in engineering nano-hetero-structures for enhanced photocatalytic hydrogen evolution, in an attempt to make the process commercially viable.
... This means that the t of MA in the PVDF/MA blend and PVDF/MA/EG composites is enhanced the strong interaction between the MA and the PVDF. Furthermore, th PM14G7 samples exhibit an obvious symmetric stretching band of the (C=O) of MA at 1781 cm −1 [42][43][44], which is red-shifted relative to that of th cm −1 ). Simultaneously, the PVDF, PG3, and PG7 samples exhibit a deform the CH2 groups of PVDF chains at 1382 cm −1 , as can be seen in Figure 10b tion of MA, the characteristic peak at 1382 cm −1 shifts to 1380 cm −1 . ...
... This means that the thermal stability of MA in the PVDF/MA blend and PVDF/MA/EG composites is enhanced, which confirms the strong interaction between the MA and the PVDF. Furthermore, the PM14 and the PM14G7 samples exhibit an obvious symmetric stretching band of the carbonyl group (C=O) of MA at 1781 cm −1 [42][43][44], which is red-shifted relative to that of the neat MA (1774 cm −1 ). Simultaneously, the PVDF, PG3, and PG7 samples exhibit a deformed vibration of the CH 2 groups of PVDF chains at 1382 cm −1 , as can be seen in Figure 10b. ...
Maleic anhydride (MA) is introduced to fabricate poly(vinylidene fluoride)/expanded graphite (PVDF/EG) composites via one-step melt mixing. SEM micrographs and WAXD results have demonstrated that the addition of MA helps to exfoliate and disperse the EG well in the PVDF matrix by promoting the mobility of PVDF molecular chains and enhancing the interfacial adhesion between the EG layers and the PVDF. Thus, much higher thermal conductivities are obtained for the PVDF/MA/EG composites compared to the PVDF/EG composites that are lacking MA. For instance, The PVDF/MA/EG composite prepared with a mass ratio of 93:14:7 exhibits a high thermal conductivity of up to 0.73 W/mK. It is 32.7% higher than the thermal conductivity of the PVDF/EG composite that is prepared with a mass ratio of 93:7. Moreover, the introduction of MA leads to an increased melting peak temperature and crystallinity due to an increased nucleation site provided by the uniformly dispersed EG in the PVDF matrix. This study provides an efficient preparation method for PVDF/EG composites with a high thermal conductivity.
... The FTIR spectrum of SEBS-MA shows the bands characteristic to aliphatic and aromatic C-H bonds and aromatic C=C, similar to SEBS. In SEBS-MA, maleic anhydride can be in a ring form or in a hydrolyzed form, showing dicarboxylic acid groups; the ring form shows the peaks characteristic to the vibrational coupling of the two C=O groups at 1856, 1780, and 1720 cm −1 [27,28] and maleic acid shows signals at 1707 cm −1 , characteristic to the intramolecular H-bonded C=O stretch, at 1733 cm −1 , characteristic to C=O stretch, and Interestingly, the band at 1728-1720 cm −1 changes the shape in the case of composites by broadening and by the evidence of an obvious shoulder at about 1743 cm −1 , charac-teristic of the ester bond ( Figure 4c, marked with a red circle). This shift from a lower wavenumber to a higher one in the range 1720-1743 cm −1 shows the transformation of aldehyde or acid groups in ester groups. ...
... The FTIR spectrum of SEBS-MA shows the bands characteristic to aliphatic and aromatic C-H bonds and aromatic C=C, similar to SEBS. In SEBS-MA, maleic anhydride can be in a ring form or in a hydrolyzed form, showing dicarboxylic acid groups; the ring form shows the peaks characteristic to the vibrational coupling of the two C=O groups at 1856, 1780, and 1720 cm −1 [27,28] and maleic acid shows signals at 1707 cm −1 , characteristic to the intramolecular H-bonded C=O stretch, at 1733 cm −1 , characteristic to C=O stretch, and at 1262 cm −1 , due to C-O-C stretching vibrations [29]. ...
The structure–property relationship of dielectric elastomers, as well as the methods of improving the control of this relationship, has been widely studied over the last few years, including in some of our previous works. In this paper, we study the control, improvement, and correlation, for a significant range of temperatures, of the mechanical and dielectric properties of polystyrene-b-(ethylene-co-butylene)-b-styrene (SEBS) and maleic-anhydride-grafted SEBS (SEBS-MA) by using graphite (G) as filler in various concentrations. The aim is to analyze the suitability of these composites for converting electrical energy into mechanical energy or vice versa. The dielectric spectroscopy analysis performed in the frequency range of 10 to 1 MHz and at temperatures between 27 and 77 °C emphasized an exponential increase in real permittivity with G concentration, a low level of dielectric losses (≈10−3), as well as the stability of dielectric losses with temperature for high G content. These results correlate well with the increase in mechanical stiffness with an increase in G content for both SEBS/G and SEBS-MA/G composites. The activation energies for the dielectric relaxation processes detected in SEBS/G and SEBS-MA/G composites were also determined and discussed in connection with the mechanical, thermal, and structural properties resulting from thermogravimetric analysis, differential scanning calorimetry, Fourier-transform infrared spectroscopy and X-ray photoelectron spectroscopy analyses.
... Two distinct peaks at 2952 and 2869 cm −1 corresponded to Polymers 2022, 14, 4100 7 of 16 the asymmetrical and symmetrical stretching of CH 2 , respectively. As for MA, the C=O peaks of MA were found at 1861 (low intensity) and 1785 cm −1 (medium intensity) due to the C=O stretching group of low and high intensity hydrolysed MA, respectively [60]. PCL-g-MA was successfully generated by grafting MA onto PCL since two characteristic shoulders of anhydride carboxyl groups appeared at 1790 and 1867 cm −1 [61]. ...
... Two distinct peaks at 2952 and 2869 cm −1 corresponded to the asymmetrical and symmetrical stretching of CH2, respectively. As for MA, the C=O peaks of MA were found at 1861 (low intensity) and 1785 cm −1 (medium intensity) due to the C=O stretching group of low and high intensity hydrolysed MA, respectively [60]. PCLg-MA was successfully generated by grafting MA onto PCL since two characteristic shoulders of anhydride carboxyl groups appeared at 1790 and 1867 cm −1 [61]. ...
The plastic waste problem has recently attracted unprecedented attention globally. To reduce the adverse eff ects on environments, biodegradable polymers have been studied to solve the problems. Poly(ε-caprolactone) (PCL) is one of the common biodegradable plastics used on its own or blended with natural polymers because of its excellent properties after blending. However, PCL and natural polymers are difficult to blend due to the polymers’ properties. Grafted polymerization of maleic anhydride and dibenzoyl peroxide (DBPO) with PCL is one of the improvements used for blending immiscible polymers. In this study, we first focused on the effects of three factors (stirring time, maleic anhydride (MA) amount and benzoyl peroxide amount) on the grafting ratio with a maximum value of 4.16% when applying 3.000 g MA and 1.120 g DBPO to 3.375 g PCL with a stirring time of 18 h. After that, the grafting condition was studied based on the kinetic thermal decomposition and activation energy by the Coats–Redfern method. The optimal fitting model was confirmed by the determination coefficient of nearly 1 to explain the contracting volume mechanism of synthesized PCL-g-MA. Consequently, grafted MA hydrophilically augmented PCL as the reduced contact angle of water suggests, facilitating the creation of a plastic–biomaterial composite.
... As shown in Fig. 2a, sulfur was inactive in the frequency range of 4000-400 cm − 1 . In the IR spectrum of PI-g-MA (Fig. 2b), the three absorption bands at 1850, 1790, and 1720 cm − 1 can be attributed to the carboxylic anhydride of the maleic anhydride ring and the two weak absorption peaks at 3050 and 1650 cm − 1 can be attributed to the CH stretching vibration of -C=C-H and C=C stretching vibration of polyisoprene, respectively [49]. After cross-linking, the IR spectrum of VPI-g-MA (Fig. 2c) shows three distinct absorption bands. ...
Vulcanized polyisoprene-graft-maleic anhydride (VPI-g-MA) has been utilized as an in situ cross-linked binder for silicon (Si) anodes. PI-g-MA was vulcanized with sulfur at 180 °C to form an elastic polymer with a glass transition temperature of −45.5 °C measured via differential scanning calorimetry. The results of infrared spectroscopy confirm the formation of C-S bonds. The Si anode with the VPI-g-MA binder exhibited a high initial charge capacity of 4005 mAh g⁻¹ at a charge/discharge rate of 0.1 C and demonstrated significant cycle-life performance of up to 200 cycles at a C-rate of 0.5 C. Furthermore, the peeling test results showed that the Si electrode with the VPI-g-MA binder has better adhesion strength than the Si electrode with either PVDF, PI-g-MA, or SBR/CMC binder. Scanning electron microscopy images showed that the VPI-g-MA binder could effectively maintain the integrity of the Si electrode throughout the cycling process. Thus, the VPI-g-MA binder can enhance the cycle-life performance of Si anodes.
... As shown in Fig. 2a, sulfur was inactive in the frequency range of 4000-400 cm − 1 . In the IR spectrum of PI-g-MA (Fig. 2b), the three absorption bands at 1850, 1790, and 1720 cm − 1 can be attributed to the carboxylic anhydride of the maleic anhydride ring and the two weak absorption peaks at 3050 and 1650 cm − 1 can be attributed to the CH stretching vibration of -C=C-H and C=C stretching vibration of polyisoprene, respectively [49]. After cross-linking, the IR spectrum of VPI-g-MA (Fig. 2c) shows three distinct absorption bands. ...
... The symmetric and asymmetric bending of methyl groups was observed at 1460-1380 cm − 1 [58]. PEMAH peaks at 1715 and 1792 cm − 1 were the carboxylic acid and symmetric stretching of cyclic anhydride, respectively [59]. The TPS/PEMAH showed a shoulder peak of MAH at 1715 cm − 1 due to the MAH groups remaining inside the PEMAH phase. ...
Thermoplastic starch (TPS) was prepared from cassava starch blended with glycerol (70:30 w/w). Gelatin (Gel) was incorporated into the TPS in water. The TPS/Gel was melt-blended with polyethylene-grafted-maleic anhydride (PEMAH). Maximum tensile strength of the TPS/PEMAH/Gel10 (29.3 MPa) increased significantly compared to the TPS/PEMAH blend (6.3 MPa), while elongation at break was 70%. The morphology of the TPS/PEMAH showed co-continuous morphology, while phase inversion occurred with the addition of Gel. The Gel was dispersed in the TPS matrix and covered the PEMAH. The TPS/PEMAH/Gel was nanoparticles (200 nm) in the TPS matrix. It showed two melting temperatures for PEMAH due to two structures with different crystal sizes. Melt viscosity of the TPS/PEMAH was enhanced with increasing Gel as the reaction induced chain extension. FTIR and rheology measurements confirmed the reaction between –NH groups of Gel and MAH groups of PEMAH. This reaction improved interfacial adhesion, morphology, and the mechanical properties of the blends.
... These features Mare characteristic of b-glycosidic linkages between the anhydroglucose units in cellulose [33,34]. According to the FT-IR results in Fig. 3c, the ring-opening reaction and grafting of MAc groups in the backbone of the copolymer were confirmed by the presence of a new absorption band at 1730 cm −1 , which is attributed to the steric groups of MAc [13,35]. In Fig. 4d, the further modification using HEMA and IA, which also contain C_O, leads to an increase in the same peak at 1720 cm −1 , corresponding to the vibrational stretching of the carbonyl groups (C=O) of HEMA, MAc and, IA. ...
Superdisintegrants have an important function in Fast dissolving tablets (FDT). It's believed that an increase in surface to the mass (size reduction) can enhance their performance. Due to the obligation of pharmaceutical excipients being in GRAS (generally recognized as safe) list, we've devoted our research to modify one of the routinely used and important natural polymer, cellulose, as superdisintegrant. Nanocrystalline cellulose (NCC) was extracted from microcrystalline cellulose (MCC) via the sulfuric acid hydrolysis process. NCC derivatives have been synthesized by Itaconic acid/Hydroxyethyl methacrylate (IA/HEMA) via maleic anhydride (MA) to acquire unique swellability properties in to achieve superabsorbent cellulose-based nano hydrogel with the cross-linking system. The disintegration performance of prepared tablets was compared with tablets composed of sodium starch glycolate (SSG) and MCC as positive and negative controls. The results show that the disintegration time of tablets formulated with synthesized modified NCC (m-NCC) decreased dramatically compared to other disintegrants. The dissolution analysis showed suitable condition for complete drug release in a shorter time. The in vitro cytotoxic experiments proved the biocompatibility of newly synthesized superdisintegrant. The dissolution Analysis findings suggest that our developed novel superdisintegrant paves the way for the formulation of fast dissolving tablets containing rapidly acting medicines such as zolpidem.
... Band assignments in EPDM-P-S and EPDM-EB-S samples. Aromatic skeletal vibrations caused by holocellulose (wood sawdust) [82] C=O stretch in non-conjugated ketones, carbonyls, and ester groups [82,83] 1640 C=C stretching vibration (1630 cm −1 ) from EPDM [68][69][70] 1642-1646 (EPDM-EB-S) Typical bands assigned to cellulose-Vibration of water molecules absorbed in cellulose [62] 1539, 1540 (EPDM-P-S) Aromatic skeletal vibrations caused by lignin (wood sawdust) [82] C=O stretch in non-conjugated ketones, carbonyls, and in ester groups [82,83] CH2 bending and rocking vibrations from EPDM [64][65][66][67] The previously mentioned presence of wood components (cellulose, hemicellulose, and lignin) in EPDM-EB-S samples confirms their origin from the sawdust used for obtaining composites (Table 1). In Figure 10a,b, notable differences in band widths and intensities can be observed due to the cross-linking method and S loading. ...
A natural fiber reinforced composite, belonging to the class of eco composites, based on ethylene-propylene-terpolymer rubber (EPDM) and wood wastes were obtained by electron beam irradiation at 75, 150, 300, and 600 kGy in atmospheric conditions and at room temperature using a linear accelerator of 5.5 MeV. The sawdust (S), in amounts of 5 and 15 phr, respectively, was used to act as a natural filler for the improvement of physical and chemical characteristics. The cross-linking effects were evaluated through sol-gel analysis, mechanical tests, and Fourier Transform Infrared FTIR spectroscopy comparatively with the classic method with dibenzoyl peroxide (P) applied on the same types of samples at high temperature. Gel fraction exhibits values over 98% but, in the case of P cross-linking, is necessary to add more sawdust (15 phr) to obtain the same results as in the case of electron beam (EB) cross-linking (5 phr/300 kGy). Even if the EB cross-linking and sawdust addition have a reinforcement effect on EPDM rubber, the medium irradiation dose of 300 kGy looks to be a limit to which or from which the properties of the composite are improved or deteriorated. The absorption behavior of the eco-composites was studied through water uptake tests.
