• Polymer(Korea)
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• v.39 no.2
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• pp.240-246
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• 2015

Formation of a strong 3-dimensional interfacial network structure via chemical reaction between hydroxyl group on silica surface and NR chain by the addition of bis(triethoxysilylpropyl)tetrasulfide (TESPT) into silica-filled NR compound was observed by using Py-GC/MS and SEM. Addition of TESPT into silica-filled NR compound decreased scorch time ($t_{10}$) due to increased sulfur content, and reduced cure rate index (CRI) via continuous reaction between sulfur atoms in TESPT, which acted as a sulfur donor, and activators and/or accelerators. Addition of TESPT in the compound improved processability and mechanical properties of the compound. Overall, we observed that the addition of TESPT into the silica-filled NR compound formed a silica-TESPT-NR network, and thus the degree of crosslinking was increased resulting in improved mechanical properties.

• Elastomers and Composites
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• v.37 no.4
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• pp.217-223
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• 2002

Silica-filled rubber compounds show poor filler dispersion and slow cure characteristics compared to carbon black-filled ones. In general, a silica-filled rubber compound contains silane coupling agent (bis-(3-(triethoxysilyl)-propyl)-tetrasulfide, TESPT) and diphenylguanidine (DPG) to improve the filler dispersion and to make fast cure characteristics. Acrylonitrile-butadiene rubber (NBR) improves the filler dispersion in silica-filled styrene-butadiene rubber (SBR) compounds. In this study, effect of NBR on the properties of silica-filled SBR compounds was investigated. Properties of the compounds which contain NBR without DPG or with small amount of TESPT (Compound A) were compared with those of the compounds which contain TESPT and DPG without NBR (Compound B). Scorch time of Compound A is faster than those of Compound B. Modulus and tensile strength of Comound A are slightly lower than those of Compound B. Traction property of the Comound A is better than that of the Compound B. Addition of NBR leads to reduction of the used amount of TESPT and DPG.

• Polymer(Korea)
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• v.37 no.3
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• pp.308-315
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• 2013

In this study, we performed surface modification of silica nanoparticles with bis[3-(triethoxysilylpropyl)]tetrasulfide (TESPT) silane coupling agent to study the effects of treatment temperature, treatment time, and amount of TESPT used on the silanization degree with Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), elemental analysis (EA) and solid state $^{13}C$ and $^{29}Si$ cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR). We found peak area of isolated silanol groups at $3747cm^{-1}$ decreased, but peak area of $-CH_2$ asymmetric stretching of TESPT at $2938cm^{-1}$ increased with the amount of TESPT from FTIR measurements. We also used universal testing machine (UTM) to study mechanical properties of styrene butadiene rubber (SBR) nanocomposites with 20 phr (parts per hundred of rubber) of pristine and TESPT modified silicas, respectively. The tensile strength and 100% modulus of modified silica/SBR nanocomposite were enhanced from 5.65 to 9.38MPa, from 1.62 to 2.73 MPa, respectively, compared to those of pristine silica/SBR nanocomposite.

• Elastomers and Composites
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• v.45 no.2
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• pp.112-121
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• 2010

In this study, styrene butadiene rubber(SBR)/organoclay nanocomposites were manufactured using the latex method with 3-aminopropyltriethoxysilane(APTES) as a modifier. The X-ray diffraction(XRD), transmission electron microscopy(TEM) images, Fourier transform infrared(FTIR) spectroscopy, swelling ratio and mechanical properties were measured in order to study the interaction between filler and rubber according to the mixing temperature in the internal mixer. In the case of SBR/APTES-MMT compounds, the dispersion of the silicates within the rubber matrix was enhanced, and thereby, the mechanical properties were improved. The characteristic bands of Si-O-C in APTES disappeared after hydrolysis reaction in the MMT-suspension solution and the peak of hydroxyl group was increased. Therefore the formation of chemical bonds between the hydroxyl group generated from APTES on the silicate surface and the ethoxy group of bis(triethoxysilylpropyl) tetrasulfide(TESPT) was possible. Consequently, the 300% modulus of SBR/APTES-MMT compounds was further improved in the case of using TESPT as a coupling agent. However, the silanization reaction between APTES and TESPT was not affected significantly according to the increase of mixing temperature in the internal mixer.

• The Korean Journal of Rheology
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• v.7 no.1
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• pp.60-67
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• 1995

EPDM/BR 블렌드의 물성에 미치는 커플링결합체의 영향을 조사하였다. N,N＇ -(bis(2-methyl-2-nitroprpyl))-1,6-diamino hexane) (MNPDH)와 bis(3-triethoxysilyl propyl)-tetrasulfide (TESPT)의 두가지 종류의 커플링결합제를 사용하였다. EPDM/BR 블 렌드 및 EPDM/BR/MNPDH 또는 EPDM/BR/TESPT 블렌드의 용융점도, 탄성률 및 tan $\delta$ 를 모세관 점도계, 동적점탄성장치 및 동적응력 완화측정장치로 조사하였다. 동적점탄성 및 형태학적 연구 결과 MNPDH 또는 TESPT를 첨가할 경우 결합고무 함량이 증가하고 카본 블랙의 분산성이 좋아져 가황된 EPDM/BR 블렌드의 인열강도 및 내피로성등의 물성이 향 상되었다.

• Elastomers and Composites
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• v.49 no.3
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• pp.239-244
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• 2014

Reaction between silica and silane coupling agent without solvent was investigated using transmission mode Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis (TGA). Bis[3-(triethoxysilylpropyl) tetrasulfide] (TESPT) was used as a silane coupling agent. After removing the unreacted TESPT, formation of chemical bonds was analyzed using FTIR and content of reacted TESPT was determined using TGA. Content of the coupling agent bonded to silica increased with increase in the coupling agent content, but the oligomers were formed by condensation reaction between coupling agents when the coupling agent was used to excess. In order to identify bonds formed among silica, coupling agent, and rubber, a silica-coupling agent-BR model composite was prepared by reaction of the modified silica with liquid BR of low molecular weight and chemical bond formation of silica-coupling agent-BR was investigated. Unreacted rubber was removed with solvent and analysis was performed using FTIR and TGA. BR was reacted with the coupling agent of the modified silica to form chemical bonds. Polarity of silica surface was strikingly reduced and particle size of silica was increased by chemical bond formation of silica-coupling agent-BR.

• Elastomers and Composites
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• v.55 no.1
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• pp.26-39
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• 2020

The physical properties of silica-filled SBR compounds (WSBR) prepared using silica-SBR wet masterbatches (WMB) were systematically investigated to understand the effect of the surface treatment of silica on the reinforcement performance of SBR. Treatment of silica with bis(triethoxysilylpropyl)tetrasulfide (TESPT) in the liquid phase, followed by mixing with an SBR solution and recovery by water stripping, easily produced silica-SBR WMB. However, insufficient surface treatment in terms of the amount and stability of the incorporated TESPT led to considerable silica loss and inevitable TESPT elution. Pretreatment of silica in the gas phase with TESPT and another organic material that enabled the formation of organic networks among the silica particles on the surface provided hydrophobated silica, which could be used to produce silica-SBR WMB, in high yields of above 99%. The amount and type of organic material incorporated into silica greatly influenced the cure characteristics, processability, and tensile and dynamic properties of the WSBR compounds. The TESPT and organic material stably incorporated into silica increased their viscosity, while the organic networks dispersed on the silica surface were highly beneficial for reducing their rolling resistance. Excessive dosing of TESTP induced low viscosity and a high modulus. The presence of connection bonds formed by the reaction of glycidyloxy groups with amine groups on the silica surface resulted in physical entanglement of the rubber chains with the bonds in the WSBR compounds, leading to low rolling resistance without sacrificing the mechanical properties. Mixing of the hydrophobated silica with a rubber solution in the liquid phase improved the silica dispersion of WSBR compounds, as confirmed by their low Payne effect, and preservation of the low modulus enhanced the degree of entanglement.

• Elastomers and Composites
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• v.46 no.1
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• pp.45-53
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• 2011

The effect of the silane coupling agent, bis(triethoxysilypropyl)tetrasulfide (TESPT), on mechanical properties of a silica-filled NBR compound for oilseal was investigated. Curing behavior and crosslinking density of the compounds were measured using ODR (oscillating disk rheometer) and swelling ratio in toluene. UTM (universal testing machine) and shore A hardness tester were used in order to study the characteristics of mechanical properties of original vulcanizates and aged ones with heated air and ASTM No. 3. oil. Recovery of elasticity which influences the performance and service life of oilseal was investigated by giving bending deformation to vulcanizates in aging condition. After bending aging test, recovery distance was measured and calculated angle of recovery from it. TR (temperature retraction) test was performed on these vulcanizates to determine the low temperature recovery behavior. Wear resistance was measured by Taber type abrasion tester. In addition, SEM was used to characterize the morphology of the worn surface of vulcanizates. The result showed that addition of TESPT into silica-filled compound improves not only compound flow-ability, interaction between NBR and silica and crosslinking density, but also hardness, 100% modulus, recovery of elasticity, wear resistance, heat resistance and ASTM No.3 oil resistance of vulcanizates.

• Elastomers and Composites
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• v.53 no.3
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• pp.109-123
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• 2018

The effect of the silica content on the state and properties of silica-filled styrene-butadiene rubber/butadiene rubber (SBR/BR) compounds containing coupling and dispersion agents was evaluated by varying the content of silica from 50 to 120 phr. Bis-[(triethoxysilyl)propyl] tetrasulfide (TESPT) and zinc 2-ethylhexanoate (ZEH) were used as the coupling and dispersion agents, respectively. The maximum silica content in the pristine material was 80 phr, which increased to 120 phr upon the addition of TESPT and ZEH. The incorporation of TESPT considerably improved most of the rubber properties due to its coupling action and the suppression of silica flocculation, while further addition of ZEH resulted in additional improvements. The properties of the rubber compounds with different silica contents can be fully explained either by an enhancement of the rubber-silica interactions or by their deterioration due to an excessive amount of silica aggregates.

• Elastomers and Composites
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• v.56 no.1
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• pp.32-42
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• 2021

The vulcanizate structure of silica-filled compounds is affected by the filler-rubber interaction (FRI) due to the silica-rubber coupling reaction and the chemical crosslink density (CCD) of the matrix rubber. In this study, the vulcanizate structure changes of silica-filled compounds according to the silane and sulfur variation were quantitatively analyzed using the Flory-Rehner and Kraus equations. In efficiency vulcanization (EV) conditions with low sulfur content, FRI increased when the bis-[3-(triethoxysilyl)propyl]tetrasulfide (TESPT) content increased, and the CCD clearly decreased. By contrast, in semi-EV conditions with high sulfur content, as TESPT content increased, the FRI increased the same way EV conditions, but the CCD was unchanged. Based on these results, it was confirmed that FRI of the silica-filled compounds increased as TESPT content increased, but CCD decreased or retained similar values according to the vulcanization system, indicating that the formation reaction of FRI was preferred over CCD.