Curing Characteristics,Fatigue and Hysteresis Behaviour of Feldspar Filled Natural Rubber Vulcanizates

Curing characteristics, fatigue, and hysteresis behaviour of feldspar filled SMR L vulcanizates and feldspar filled ENR 50 vulcanizates were studied. Two different types of natural rubber, SMR L and ENR 50 having 0 and 50 mol% of epoxide groups were used. The feldspar filled natural rubber vulcanizates were compared at similar filler loading which were used at 0, 10, 20, and 30 phr of filler loading. The curing characteristics such as scorch time (t ₂) and cure time (t ₉₀) slightly increased with increasing feldspar loading for both rubber vulcanizates. Besides t ₂ and t ₉₀, maximum torque (M _HR) significantly increased for both rubbers with increasing feldspar loading. The fatigue test showed that fatigue life decreased with increasing extension ratio, strain energy and filler loading. As the filler loading increased, the poor wetting of the feldspar by the rubber matrix gave rise to poor interfacial adhesion between filler and rubber matrix. Results also indicate that the vulcanizates with the highest feldspar loading exhibited the highest hysteresis. The feldspar filled SMR L vulcanizates showed higher fatigue life and lower hysteresis compare to feldspar filled ENR 50 vulcanizates.     

Effect of filler loading on cure time and swelling behaviour of SMR L/ENR 25 and SMR L/SBR blends

The effect of filler loading on the cure time (t₉₀) and swelling behaviour of SMR L/ENR 25 and SMR L/SBR blends has been studied. Carbon black (N330), silica (Vulcasil C) and calcium carbonate were used as fillers and the loading range was from 0 to 40 phr. Results show that for SMR L/ENR 25 blends the cure time decreases with increasing carbon black loading, whereas silica shows an increasing trend, and calcium carbonate does not show significant changes. For SMR L/SBR blends, the cure time of carbon black, silica and calcium carbonate generally decreases with increasing filler loading. The percentage swelling in toluene and ASTM oil no 3 decreases for both blends with increasing filler loading, with calcium carbonate giving the highest value, followed by silica‐ and carbon black‐filled blends. At a fixed filler loading, SMR L/ENR 25 blend shows a lower percentage swelling than SMR L/SBR blends. © 2003 Society of Chemical Industry     

Effect of carbon black loading on curing characteristics and mechanical properties of waste tyre dust/carbon black hybrid filler filled natural rubber compounds

Curing characteristics, tensile properties, fatigue life, swelling behavior, and morphology of waste tire dust (WTD)/carbon black (CB) hybrid filler filled natural rubber (NR) compounds were studied. The WTD/CB hybrid filler filled NR compounds were compounded at 30 phr hybrid filler loading with increasing partial replacement of CB at 0, 10, 15, 20, and 30 phr. The curing characteristics such as scorch time, t₂ and cure time, t₉₀ decreased and increased with increment of CB loading in hybrid filler (30 phr content), respectively. Whereas maximum torque (M_HR) and minimum torque (M_L) increased with increasing CB loading. The tensile properties such as tensile strength, elongation at break, and tensile modulus of WTD/CB hybrid filler filled NR compounds showed steady increment as CB loading increased. The fatigue test showed that fatigue life increased with increment of CB loading. Rubber–filler interaction, Q_f/Q_g indicated that the NR compounds with the highest CB loading exhibited the highest rubber–filler interactions. Scanning electron microscopy (SEM) micrographs of tensile and fatigue fractured surfaces and rubber–filler interaction study supported the observed result on tensile properties and fatigue life. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Comparative study of silica-, nanoclay- and carbon black-filled EPDM rubbers

Silica-, nanoclay-, and carbon black (CB)-filled ethylene–propylene–diene terpolymer (EPDM) mixtures were prepared and subsequently vulcanized. Rheological properties and cure characteristics of the mixtures and mechanical properties of vulcanizates were measured. Rheological property measurements indicated the storage modulus, loss modulus, and complex dynamic viscosity of silica-filled EPDM mixtures were much higher than those of CB-filled EPDM mixtures while tan δ values were lower. The optimum cure time of silica- and nanoclay-filled EPDM mixtures increased with filler loading, whereas the values for CB-filled mixtures slightly decreased with loading. The hardness, modulus, elongation at break, and tensile strength of all the vulcanizates increased with increasing filler loading. The elongation at break of CB-filled EPDM vulcanizates increased insignificantly with CB loading. Among the three fillers, the increase of the tensile strength and elongation at break was most significant for silica-filled EPDM vulcanizates. Remarkably, for 30 phr silica-filled EPDM vulcanizates, a tensile strength and elongation at break of 23.5 MPa and 1045% was achieved, respectively. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

THE COMPARISON PROPERTIES OF RECYCLE RUBBER POWDER,CARBON BLACK,AND CALCIUM CARBONATE FILLED NATURAL RUBBER COMPOUNDS

The effects of filler loading on the curing characteristics, swelling behavior, and mechanical properties of natural rubber compounds were studied using a conventional vulcanization system. Recycle rubber powder (RRP), carbon black (CB) (N550), and calcium carbonate (CaCO₃) were used as fillers and the loading range was from 0 to 50 phr. Results show that the scorch time, t ₂, and cure time, t ₉₀, decrease with increase in filler loading. At a similar filler loading, RRP shows shortest t ₂ and t ₉₀ followed by CB and calcium carbonate. The tensile strength, tensile modulus, and hardness increase with increase in CB loading, whereas elongation at break, resilience, and swelling properties show opposite trend. For RRP and calcium carbonate filled natural rubber compounds, the tensile strength increases up to 10 phr and starts to deteriorate at higher filler loading. The other properties such as tensile modulus, hardness, elongation at break, resilience, and swelling percentage show a small change (increase or decrease) with increase in RRP and calcium carbonate loading in natural rubber compounds. Overall results indicate that RRP can be used as a cheapener to replace calcium carbonate in natural rubber compounds where improved mechanical properties are not critical.     

The Effect of Filler Loading and Epoxidation on Paper-Sludge-Filled Natural Rubber Composites

The effect of filler loading and epoxidation on curing characteristics, dynamic properties, tensile properties, morphology, and rubber-filler interactions of paper-sludge-filled natural rubber compounds have been studied. Two different types of natural rubber, SMR L and ENR 50, having 0% and 50% of epoxidation and conventional vulcanization were used. Paper sludge was used as a filler and the loading range was from 0 to 40 phr. Compounding was carried out using a laboratory-sized two-roll mill. The scorch time for both rubber compounds decreased with filler loading. The cure time was found to decrease with increasing filler content for SMR L vulcanizates, whereas for ENR 50, the cure time seemed to be independent of the filler loading. Dynamic properties, i.e., maximum elastic torque, viscous torque, and tan delta, increase with filler loading in both grades of natural rubber. Results also indicate that both rubbers show increment in tensile modulus but inverse trend for elongation at break and tensile strength. However, for a fixed filler loading, ENR 50 compounds consistently exhibit higher maximum torque, modulus at 100% elongation, and modulus at 300% elongation, but lower elongation at break than SMR L compounds. In the case of tensile strength, ENR 50 possesses higher tensile strength than SMR L at 10 to 20 phr, but the difference is quite small at 30 and 40 phr. These findings might be associated with better rubber-filler interaction between the polar hydroxyl group of cellulose fiber and the epoxy group of ENR 50.     

Palm oil fatty acid as an activator in carbon black filled natural rubber compounds: effect of vulcanization system

Carbon black filled natural rubber compounds were cured using conventional vulcanization (CV) and semi-efficient vulcanization (semi-EV) systems. The effect of palm oil fatty acid on cure characteristics and mechanical properties was examined. It was found that the cure time t₉₀, and scorch time increased with increasing palm oil fatty acid concentration in both systems. At fixed acid concentration, semi-EV compounds show shorter t₉₀ and scorch time than CV compounds. Results from tensile modulus, hardness, maximum torque-minimum torque M_HR-M_L, and swelling measurements indicate that palm oil fatty acid has some effect on crosslink density. At fixed palm oil fatty acid concentration, CV compounds have better mechanical properties (tensile modulus, hardness, tear and tensile strengths) compared with semi-EV compounds. ©1997 SCI     

Preparation of Cu(II)-Immobilized Chitosan (CIC) and Preliminary Urea Uptake Study

The effect of filler loading and size on commercially available silica (Vulcasil C) and value added silica (ultrafine) as filler in SMR L grade natural rubber were studied. Vulcasil C with particle size ranged from 10 µm–20 µm whilst ultrafine (1 µm–3 µm) was loaded in SMR L compound at 4 different loadings. The curing characteristics, tensile properties and swelling behavior were studied. At similar filler loading, ultrafine-filled vulcanizates exhibited shorter scorch time and cure time. It also shows higher tensile strength and elongation at break up to 20 phr filler loading and exhibit lower swelling ratio compared to Vulcasil C-filled vulcanizates.     

Effects of palm oil fatty acid on curing characteristics,reversion and fatigue life of various natural rubber compounds

The effects of palm oil fatty acid concentration (0, 1, 3, 5, 7 phr) and epoxidation on curing characteristics, reversion and fatigue life of carbon black filled natural rubber compounds have been studied. Three different types of natural rubber, SMR L, ENR 25 and ENR 50 having 0, 25 and 50 mol% of epoxidation and conventional sulphur vulcanization were used. The cure time t₉₀, scorch time t₂, M_HR − M_L (maximum torque − minimum torque) and fatigue life of all rubbers were found to increase with increasing palm oil fatty acid concentration. However, the reversion of all rubbers decreases with increasing palm oil fatty acid concentration. At similar concentrations of palm oil fatty acid, ENR 50 compounds exhibit the shortest scorch and cure times followed by ENR 25 and SMR L compounds. For reversion, SMR L compounds show the lowest value followed by ENR 50 and ENR 25 compounds, whereas for fatigue life, the highest value is obtained with ENR 50 compounds followed by ENR 25 and SMR L compounds. © 1999 Society of Chemical Industry     

Study on Tensile,Electrical, and Thermal Properties of Aluminium Particle Filled Natural Rubber (NR) and Ethylene-Propylene-Diene Terpolymer (EPDM) Composites

Comparative studies on the effect of aluminium particles in natural rubber (NR) and ethylene-propylene-diene terpolymer (EPDM) were conducted. The incorporation of aluminium particles in NR or EPDM composites increased the cure time, t ₉₀, and scorch time, t _S2 . At a fixed filler loading, EPDM composites exhibited longer t ₉₀ and t _S2 than NR composites. The results also indicate that the maximum torque, M _H of aluminium filled NR and EPDM composites increase with increasing filler loading. For tensile properties, EPDM composites show lower tensile properties than NR composites. Thermogravimetric analysis (TGA) results show that aluminium filled EPDM composites have better thermal stability than aluminium filled NR composites.

The results for electrical properties indicate that the electrical properties of aluminium filled NR and EPDM composites increase with increase in filler loading.     

NH3-modified swelling of silica-filled silicone rubber

The NH₃-modified swelling method was used for fume silica-filled silicone rubber compounds and vulcanizates. The method provides an estimation of the polymer–filler interaction in the system. Bound rubber reduction due to the modified swelling is shown to be dependent on the silica surface silanol content in the compound. The swelling behavior of silica-filled vulcanizates was also studied in an NH₃ atmosphere. The fraction of polymer–filler attachments in the vulcanizates was found not to depend on the particle size of silica and its surface modification, depending only on the total polymer–filler contact area in the system. No relation was found between bound rubber content in a compound and swelling of a filled vulcanizate of the same composition. The strong rubber-to-filler adherence found in toluene changed to nonadherence under NH₃-modified swelling conditions. The NH₃-induced cleavage of silica–silicone rubber attachments was found to be nearly completely reversible. In the silica-filled silicone rubber vulcanizates, the fraction of polymer–filler attachments due to polymer–filler interaction represents a substantial contribution to the total number of network chains.     

Effect of silane coupling agent on the curing,tensile, thermal,and swelling properties of ethylene‐propylene‐diene monomer rubber (EPDM)/mica composites

The influence of silane (bis[3‐triethoxysilylpropyl] tetrasulfide) coupling agent on the properties of ethylene‐propylene‐diene monomer rubber (EPDM)/mica composites was studied. Both EPDM/mica composites with silane and those without silane were compounded by using a two‐roll mill at various filler loadings (i.e., 100/0, 100/10, 100/30, 100/50, 100/70). The tensile and thermal properties as well as the fracture surfaces of the composites were investigated by using an Instron Universal Testing Machine, a thermal gravimetric analyzer, and a field emission scanning electron microscope. The results indicated that the optimum cure time (t₉₀) and scorch time (t_s2) values were shorter, whereas the maximum torque (M_H) value was slightly higher, for EPDM/mica composites with silane compared to those without silane. The tensile properties, modulus at 100% elongation, and modulus at 300% elongation increased for the composites made with silane, and the optimum filler loading for those properties was 50 parts by weight per hundred parts of rubber. In addition, thermal stability and swelling ratio for both composites improved with increased filler loading. However, the composites with silane showed better thermal stability and swelling ratio because of stronger linkage at the rubber‐filler boundary, which promoted filler dispersion. J. VINYL ADDIT. TECHNOL., 20:116–121, 2014. © 2014 Society of Plastics Engineers     

Influence of Particle Type and Silane Coupling Agent on Properties of Particle-Reinforced Styrene-Butadiene Rubber

Silica- and carbon-filled styrene butadiene rubber (SBR) were prepared. The influence of particle type and silane coupling agent on cure characteristics, physical and dynamic mechanical properties of particle-reinforced SBR were investigated. Minimum torque, maximum torque and tensile strength increased with increase of the filler content. The tensile strength and elongation at break were highest for presence of bis-(3-triethoxysilylpropyl) tetrasulfide (TESPT) in silica-filled vulcanizates. The dynamic mechanical properties show that tan δ at temperatures of ?20–0°C of the SiO₂/TESPT/SBR vulcanizate was highest of all. Tan δ at temperatures of 50–70°C of the SiO₂/TESPT/SBR vulcanizate was lower than carbon-filled SBR.     

Properties of styrene butadiene rubber (SBR)/recycled acrylonitrile butadiene rubber (NBRr) blends: The effects of carbon black/silica (CB/Sil) hybrid filler and silane coupling agent,Si69

The recycling or reuse of waste rubber by means of blending together with polymeric materials in addition of filler such as hybrid carbon black and silica (CB/Sil) to a polymer system can provides an opportunity to explore alternative product specifications. Therefore, in this work the investigation of recycled rubber blends based on styrene butadiene rubber/recycled acrylonitrile butadiene rubber (SBR/NBRr) blends reinforced with 50/0, 40/10, 30/20, 20/30, 40/10, 0/50 phr of carbon black/silica (CB/Sil) hybrid filler treated with and without silane coupling agent (Si69) were determined. Cure characteristics, tensile properties, and morphological behavior of selected SBR/NBRr blends at a fix 85/15 blend ratio were evaluated. Results showed that, cure time t₉₀, minimum torque (M_L), and maximum torque (M_H) of CB/Sil hybrid fillers filled SBR/NBRr blends with and without Si69 increased as silica content increased. However, t₉₀ and M_L of SBR/NBRr blends with Si69 were lower than without Si69 except for (M_H). The optimum scorch time (t_s2) of SBR/NBRr blends with and without Si69 was obtained at 30/20 phr of CB/Sil hybrid filler. However, t_s2 of SBR/NBRr blends with Si69 were longer than SBR/NBRr blends without Si69. The incorporation of Si69 has improved the tensile properties [(tensile strength, elongation at break (E_b), stress at 100% elongation (M100), and stress at 300% elongation (M300)] of CB/Sil hybrid fillers filled SBR/NBRr blends. These properties were influenced by the degree of crosslinked density as the silica content is increased. Scanning electron microscopy (SEM) of the tensile fracture surfaces indicated that, with the addition of Si69 improved the dispersion of hybrid fillers and NBRr in SBR/NBRr matrix. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Effect of fillers and additives on the properties of SBR vulcanizates

Methacrylic acid (MAA) and methyl methacrylate (MMA) were used as additives for peroxide‐cured styrene–butadiene rubber (SBR) filled with three inorganic fillers with different particle sizes and surface activity, for example, MgO, Mg(OH)₂, and BaSO₄. The experimental results show that the introduction of MAA can improve the mechanical properties of SBR vulcanizates filled with MgO, Mg(OH)₂, or BaSO₄. A small amount of MAA leads to significant increases in the modulus, tensile strength, and tear strength. MMA has little effect on the mechanical properties of the SBR vulcanizates. The SEM micrographs show that MAA can improve the interfacial bonding between SBR and the three kinds of fillers. The SBR–filler interaction was studied by Kraus plots. The relationship between the SBR–filler interaction and the mechanical properties was explored. m, a characteristic constant of a filler–SBR matrix, represents the interfacial bonding between fillers and SBR and the accumulated structure of the fillers. At a given ?, a high value of m means a strong interaction between SBR and the filler and, therefore, strong mechanical properties. The Payne effect of the SBR vulcanizates was observed, and the vulcanizates have low storage moduli at high strains and high storage moduli at low strains, and the moduli are nonlinear and increase the nonlinearity as the filler content increases. The loss moduli and loss factor reach their maximums at moderate and high strain amplitudes, respectively. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 88: 775–782, 2003     

Torrefied agro-industrial residue as filler in natural rubber compounds

This study explored the feasibility of using torrefied biomass as a reinforcing filler in natural rubber compounds. Carbon black was then replaced with the torrefied biomass in elastomer formulations for concentrations varying from 0% to 100% (60 parts per hundred rubber or phr total). Their influence on the curing process, dynamic properties, and mechanical properties was investigated. Results were compared with the properties of vulcanizates containing solely carbon black fillers. Time to cure (t₉₀) for compounds with torrefied biomass fillers increased, while filler-filler interactions (ΔG') decreased, compared to carbon black controls. At low strains, the tan δ values of the torrefied fillers vulcanizates were similar to the controls. Incorporation of torrefied biomass into natural rubber decreased compound tensile strength and modulus but increased elongation. Replacement with torrefied fillers resulted in a weaker filler network in the matrix. Still, results showed that moderate substitution concentrations (~20 phr) could be feasible for some natural rubber applications.     

THE EFFECTS OF A MULTIFUNCTIONAL ADDITIVE ON CURING CHARACTERISTICS,MECHANICAL PROPERTIES,AND SWELLING BEHAVIOR OF NATURAL RUBBER/POLYCHLOROPRENE RUBBER BLENDS

The effects of a diamine salt of fatty acid of general structure [RNH₂ ⁺[CH₂)₃NH⁺] [R′COO^?]₂ referred to as a multifunctional additive (MFA) on curing characteristics and mechanical properties and swelling behavior of natural rubber (SMR L) and polychloroprene (CR) rubber blends were studied. Compared to SMR L/CR blends without MFA, the incorporation of 2 phr (parts per hundred parts of rubber) of MFA in the blends increased mechanical properties, i.e., tensile strength, tensile modulus and hardness, and improved swelling resistance toward toluene and ASTM oil No. 1. However the scorch time, t ₅ and cure index, Δt _L decrease with incorporation of MFA into the blends.     

Structure,morphology, and properties of HNBR filled with N550, SiO2, ZDMA,and two of three kinds of fillers

The vulcanization properties, mechanical properties of hydrogenated nitrile rubber (HNBR) filled with carbon black (N550), zinc dimethacrylate (ZDMA), SiO₂ independently and two of three kinds of fillers together were investigated, respectively. The filler‐dispersion was characterized by the transmission electron microscopy (TEM) and dynamic mechanical properties. The results showed that HNBR composite filled with SiO₂ or ZDMA displayed high tensile strength, elongation at break and compression set. The HNBR composite filled with N550 displayed low compression set, tensile strength and elongation at break. The dispersion of SiO₂ in HNBR compound was better than that in HNBR vulcanizates because of SiO₂ particles self‐aggregation in vulcanizing processing. ZDMA particles with micron rod‐like and silky shape in HNBR compounds changed into near‐spherical poly‐ZDMA particles with nano size in HNBR vulcanizates by in situ polymerization reaction. The N550 particles morphology exhibited no much change between HNBR compounds and vulcanizates. N550/ZDMA have the most effective reinforcement to HNBR and the appropriate amount of ZDMA is about 25% of total filler amount by weights. The theory prediction for Payne effect (dispersion of the filler) shown by the dynamic properties is identical with actual state observed by TEM. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Curing characteristics and mechanical properties of rattan‐powder‐filled natural rubber composites as a function of filler loading and silane coupling agent

Curing characteristics, tensile properties, morphological studies of tensile fractured surfaces using scanning electron microscopy (SEM), and the extent of rubber filler interactions of rattan‐powder‐filled natural rubber (NR) composites were investigated as a function of filler loading and silane coupling agent (CA). NR composites were prepared by the incorporation of rattan powder at filler loading range of 0–30 phr into a NR matrix with a laboratory size two roll mill. The results indicate that in the presence of silane CA, scorch time (t_s2), and cure time (t₉₀) of rattan‐powder‐filled NR composites were shorten, while, maximum torque (M_H) increased compared with NR composites without silane CA. Tensile strength and tensile modulus of composites were enhanced whereas elongation at break reduced in the presence of silane CA mainly due to increase in rubber‐filler interaction. It is proven by SEM studies that the bonding between the filler and rubber matrix has improved. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

On the potential of organoclay with respect to conventional fillers (carbon black,silica) for epoxidized natural rubber compatibilized natural rubber vulcanizates

Onium modified montmorillonite (organoclay) was compounded with natural rubber (NR) in an internal mixer and cured by using a conventional sulfuric system. Epoxidized natural rubber with 50 mol % epoxidation (ENR 50) in 10 parts per hundred rubber (phr) was used as a compatibilizer in this study. For comparison purposes, two commercial fillers: carbon black (grade N330) and silica (grade vulcasil‐S) were used. Cure characteristics were carried out on a Monsanto MDR2000 Rheometer. Organoclay filled vulcanizate showed the lowest values of torque maximum, torque minimum, scorch, and cure times. The kinetics of cure reaction showed organoclay could behave as a cocuring agent. The mechanical testing of the vulcanizates involved the determination of tensile and tear properties. The improvement of tensile strength, elongation at break, and tear properties in organoclay filled vulcanizate were significantly higher compared to silica and carbon black filled vulcanizates. In terms of reinforcing efficiency (RE), organoclay exhibited the highest stiffness followed by silica and carbon black filled vulcanizates. Scanning electron microscopy revealed that incorporation of various types of fillers has transformed the failure mechanism of the resulting NR vulcanizates compared to the gum vulcanizates. Dynamic mechanical thermal analysis (DMTA) revealed that the stiffness and molecular relaxation of NR vulcanizates are strongly affected by the filler–rubber interactions. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 94: 2438–2445, 2004