• Title/Summary/Keyword: Vulcanization reaction

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Rubber bound phenolic antioxidant and its application in thermoplastic elastomer

  • Klinpituksa, Pairote;Kiarttisarekul, Anyarat;Kaesaman, Azizon
    • Advances in materials Research
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    • v.3 no.3
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    • pp.175-183
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    • 2014
  • Natural rubber bound phenolic antioxidant, 2,6-di-tert-butyl-4-vinylphenol (2,6-DBVP), was prepared from natural rubber and 2,6-DBVP in both solution and melt state. The 2,6-DBVP had been synthesized from 3,5-di-tert-butyl-4-hydroxybenzaldehyde and methyltriphenylphosphonium iodide ($MePPh_3I$) by Wittig reaction ($0^{\circ}C$ for 2 hrs, $N_2$ atmosphere). The conditions for preparation of natural rubber bound 2,6-DBVP (NR-DBVP) were optimized for both solution state (1 phr BPO and 8 phr 2,6-DBVP at $70^{\circ}C$ for 2 hrs) and for melt state (1 phr BPO and 8 phr 2,6-DBVP at $70^{\circ}C$ for 10 mins, with rotor speed of 60 rpm). A thermoplastic vulcanizate was obtained using a compatibilizer, polypropylene modified with phenolic resin (PhHRJ-PP), in a closed mixer ($180^{\circ}C$ for 3 mins, rotor speed 60 rpm). The antioxidant properties of vulcanized NR-DBVP, using phenolic as the vulcanization system, were similar to NR with the conventional antioxidant BHT. In addition, the antioxidant, water leaching property of the thermoplastic vulcanizate of NR-DBVP/PP were good in comparison to a NR blend with BHT; the morphologies of these thermoplastic vulcanizates were similar.

Influence of Process Oil Content on Properties of Silica-SBR Rubber Compounds

  • Kim, Jung Soo;Kim, Dong Hyun
    • Elastomers and Composites
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    • v.55 no.3
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    • pp.184-190
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    • 2020
  • In the wet master batch process, process oil is used to improve the workability of silica-SBR. The process oil expands the polymer and provides lubrication to soften the stiff rubber chain. However, addition of excess process oil can interfere in the crosslinking reaction between rubber molecules and reduce the crosslinking density of silica-SBR. Controlling the amount of process oil is an important aspect for properly controlling the workability and crosslinking density of silica-SBR. In this study, silica-SBR was prepared by adjusting the amount of process oil to confirm its effect on silicaSBR. Vulcanization characteristics of silica-SBR were examined using a moving die rheometer. Dynamic viscoelasticity was measured using a dynamic mechanical thermal analyzer, and the mechanical properties were investigated using the universal testing machine according to ASTM D412. As a result, all silica-SBR compounds with 10 to 40 phr of process oil have effects of improving the processability and the silica dispersibility. Also, the optimum condition was determined when 10 phr of processed oil was added because the abrasion resistance was improved 65% compared to that at 40 phr.

Electrochemical Reduction on the -S-N= Bond of N-Tert-butylbenzothiazole-2-sulfenamide (N-Tert-butylbenzothiazole-2-sulfenamide의-S-N = 결합에 대한 전기화학적 환원)

  • Kim, Hae-Jin;Jung, Keun-Ho;Choi, Qw-Won;Kim, Il-Kwang;Leem, Sun-Young
    • Journal of the Korean Chemical Society
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    • v.35 no.6
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    • pp.673-679
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    • 1991
  • The electrochemical reduction of N-tert-butylbenzothiazole-2-sulfenamide (TBBS; vulcanization accelerator) was investigated by direct current, differential pulse polarography, cyclic voltammetry and controlled potential coulometry. The electrode reduction of TBBS proceeded E-C-E-C reaction mechanism by four electrons transfer at irreversible one wave (-2.31 volts vs. Ag/0.1M AgN$O_3$ in AN). As the results of controlled potential electrolysis, mercaptobenzothiazole (MBT), benzothiazole disulfide (MBT dimer) and extricated sulfur were products which followed by cleavage of the sulfenamide (-S-N=) bond. Upon the basis of products analysis and polarogram interpretation with pH variable, electrochemical reaction mechanism was suggested.

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Electrochemical Reduction on the -S-N= Bond of N-Oxyldiethylenebenzothiazole-2-sulfenamide (N-Oxyldiethylenebenzothiazole-2-sulfenamide의 -S-N= 결합에 대한 전기화학적 환원)

  • Kim, Hae-Jin;Jung , Keun-Ho;Choi, Qw-Won;Kim, Il-Kwang;Leem, Sun-Young
    • Journal of the Korean Chemical Society
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    • v.35 no.6
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    • pp.680-688
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    • 1991
  • The electrochemical reduction of N-oxyldiethylenebenzothiazole-2-sulfenamide (ODBS; vulcanization accelerator) was investigated by direct current polarography, differential pulse polarography, cyclic voltammetry and controlled potential coulometry. The irreversible electrode reduction of ODBS proceeded E-C-E-C reaction mechanism by three electrons transfer with irreversible one wave (-1.86 volts vs. Ag/0.1 M AgN$O_3$ in AN). As the results of controlled potential electrolysis, mercaptobenzothiazole (MBT), benzothiazole disulfide (MBT dimer) and extricated sulfur were products which followed by cleavage of the sulfenamide (-S-N=) bond. Upo the basis of products analysis and polarogram interpretation witli pH variable, electrochemical reaction mechanism was suggested.

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A Study on the Characteristics of IR/CR Rubber Blends by Surface Treatment with Chlorine (염소의 표면처리에 따른 IR 및 CR Blend의 특성 연구)

  • Park, Ji-Hye;Lee, Chang-Seop;Park, Hyun-Ho
    • Journal of the Korean Chemical Society
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    • v.54 no.6
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    • pp.749-754
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    • 2010
  • In this study, rubber vulcanization property, change in physical property, morphology and chemical characteristics of blended rubber depending on various IR/CR ratio were investigated for the purpose of the improvement of material property and durability. The effect of surface treatment by chlorine on the friction coefficient was also studied with various conditions of surface treatment. In terms of vulcanization property, as the amount of CR content increased, the speed of cure was decreased, while the density of crosslinking stayed constant. It means hardness and modulus were increased as the CR content increased. It is related to change in cure property and mechanical strength was improved by the effect of crystallization reaction. In the aging property, as the CR content increases, the changed amount of basic properties were decreased, which acts as a reducing factor in change of aged property by complementing weak point in mechanical property. It was found that the degree of property change for surface treated samples were reduced. According to the microscopic result, the degree of surface dispersion on rubber blends was increased by increasing CR content. Rubber surface showed uniform direction in pattern with increased smoothness and luster by treatment with chlorine. The degree of rubber reforming was measured by the remaining amount of chlorine and the friction coefficient was dependent on the amount of chlorine combined with rubber. In the initial stage of surface treatment, from 10 to 40 phr, the friction coefficient of specimen was rapidly reduced. However, as the concentration of chlorine solution increased, the change in friction coefficient was decreased.

The Effects of Cure System on Vulcanization Reaction Constant and Physical Properties of Rubber Compounds (가황시스템 변화가 배합고무의 가황반응속도 및 물리적 특성에 미치는 영향)

  • Lee, Seag;Park, Nam Cook
    • Applied Chemistry for Engineering
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    • v.10 no.3
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    • pp.419-426
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    • 1999
  • In this study, the reaction rate constant, activation energy, total crosslinking density, elastic constant, cure properties ($t_5,\;t_{90}$), modulus, and abrasion resistance of rubber compounds were investigated as a function of cure temperatures, cure systems and reinforcing filler loadings. Reaction rate constants showed strong dependence on thc carbon black loading, cure temperature and cure system, and increased sharply with increasing the reaction temperatures. The lowest activation energy was obtained in the efficient cure (EC) system which corresponds to the high level of sulfur to accelerator ratio, and the activation energy was decreased with decreasing the carbon black loadings. The change of carbon black loadings directly affects the modulus and abrasion resistance, but the change of cure system showed various effects on the rubber compounds. Increased carbon black loadings showed the high modulus, improved abrasion resistance and short scorch time but decrease in crosslinking density and elastic constant. Higher crosslinking density and elastic constant were shown in the EC cure system regardless of carbon black loadings, but scorch timc ($t_5$) was not affected by the change of the ratio of sulfur to accelerator. Rapid optimum cure time ($t_{90}$) were showen in the EC cure system. Also, the equivalent cure curve coefficient of rubber compound was 0.96 for conventional cure (CC) system, and 0.94 for semi-efficient cure (SEC) and EC system regardless carbon black loadings. As regarding the abrasion resistance, wear volume showed the logarithmic increase for the loaded weight.

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Magnetorheological Elastomer Based on Reactive Blend of Maleic Anhydride Grafted Chloroprene Rubber and Epoxidized Natural Rubber (말레무수물로 개질된 클로로프렌 고무와 에폭시화 천연고무의 반응 블렌드에 기초한 자기유변 탄성체)

  • Choi, Jinyoung;Chung, Kyungho
    • Elastomers and Composites
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    • v.49 no.4
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    • pp.267-274
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    • 2014
  • Self vulcanizable blend system for magnetorheological elastomer (MRE) has been studied by dispersing magneto responsible particle (MRP) on elastomeric matrix. Chloroprene rubber was modified with maleic anhydride (MAH) using heat and pressure which is called dynamic maleation process. The optimum graft ratio of MAH was found at 10 phr contents and reaction temperature of $100^{\circ}C$. This could be confirmed by FT-IR analysis. Epoxided natural rubber (ENR) was blended with modified CR-g-MAH for self vulcanization. The optimum amounts of ENR was 30 wt% in terms of scorch time and curing rate. MRE was manufactured by electromagnetic equipment and orientation of MRE was confirmed by SEM. Finally, it was found that the tensile strength of anisotropic-MRE was higher than that of isotropic-MRE and the hardness was reverse.

A Study on Effects of Vulcanization Systems on Cross-linking and Degradation Reactions of NR/CR Blends Using Dynamic DSC and TGA (Dynamic DSC와 TGA를 이용한 NR/CR 고무블렌드의 가황시스템이 가교 및 열화반응에 미치는 영향 연구)

  • Min, Byung-kwon;Park, DongRyul;Ahn, WonSool
    • Korean Chemical Engineering Research
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    • v.47 no.2
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    • pp.169-173
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    • 2009
  • Effects of variations sulfur/accelerator ratio on cross-linking and thermal degradation behavior of NR/CR rubber compounds were studied using both dynamic DSC and non-isothermal TGA. DSC thermograms of the given samples were obtained with several different heating rates, and after cross-liked in DSC, TGA thermograms with the same samples also obtained. Kissinger analysis was applied to assess the activation energies for the cross-linking and thermal decomposition processes. Results showed that the formation and thermal decomposition reaction of the samples occurred in the overall temperature range of $120{\sim}180^{\circ}C$ and $350{\sim}450^{\circ}C$, respectively, exhibiting that data could be well-fittable by Kissinger method. Furthermore, formation activation energy by DSC was estimated as $83.0{\pm}5.0kJ/mol$, which was much smaller than that of degradation by TGA, $147.0{\pm}2.0kJ/mol$. From these results, it was considered that, although variations of sulfur/accelerator ratio in the present experiments affected little on the formation mechanism and/or thermal degradation, they could play roles as the catalysts which lower the activation energy of formation. Because of stabilization after formation reaction, however, they have no more effects on the lowering the activation energy, showing higher values when decomposition, caused by main-chain scissions.

A Study on the Mechanical Properties of Surface Activated Waste EPDM and The Analysis of Odor Materials (표면 활성화된 폐 EPDM 분말의 물성과 냄새 성분 분석 연구)

  • Choi, J.;Kim, S.;Chung, K.;Chung, J.;Yoo, T.;Yang, J.
    • Elastomers and Composites
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    • v.42 no.4
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    • pp.249-258
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    • 2007
  • In this study, the EPDM powder which was surface activated by high temperature and shear pulverization process was prepared and the mechanical properties and odor material analysis were investigated. Analysis for particle size and size distribution of waste of the EPDM powder has been performed. The waste EPDMs used in this study were 4 types of solid, sponge, solid+sponge, and solid+metal. According to the results, the solid type showed the smallest particle size among the 4 types of EPDM powder. Effective surface devulcanization of EPDM powder could be obtained by the addition of the reclaiming agent. The dicumyl peroxide was considered as the best crosslink agent for dynamic vulcanization when the surface activated EPDM powder was blended with polyolefin in order to make TPE. Also, the optimum amounts of DCP was 6 phr in terms of surface crosslink reaction and mechanical properties of EPDM powder. The processes of water adsorption and rose oil addition were employed to remove the odor of EPDM powder caused by reclaiming agent. The GC/MS was used to analyze the odor compounds.