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Synthesis, Curing and Properties of Silicone-Epoxies

  • Huang, Wei;Yuan, Youxue;Yu, Yunzhao
    • Journal of Adhesion and Interface
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    • v.7 no.4
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    • pp.39-44
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    • 2006
  • A new kind of silicone-epoxy composite is reported in this research. The silicone-epoxy resin was synthesized by the hydrosilylation of tetramethycyclotetrasiloxane and 4-vinyl-1-cyclohexene 1,2-epoxy with a high reaction yield. It was found that the obtained silicone-epoxy resin shows a high reactive activity to the aluminum complex-silanol catalyst. The resin could be cured under the catalysis of $(Al(acac)_3/Ph_2Si(OH)_2$ at a concentration below 0.1 wt% to give a hard cured resin showing excellent optical clarity, UV resistance and thermal stability. It was also found that the Si-H groups facilitated the curing reaction and the silicone-epoxy resin bearing Si-H group could be cured effectively even if $Ph_2Si(OH)_2h$ was absent. Moreover, the UV resistance and thermal stability were improved significantly by the introduction of Si-H groups. This is possibly due to the reductive property of Si-H groups which can annihilate radical and peroxide effectively. This kind of silicone-containing epoxy composite might have very promising applications as optical resin, optical adhesive and encapsulation materials for electronic devices.

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Effect of Resorcinol as Free Formaldehyde Scavenger for Fabric Finished with Urea-formaldehyde Precondensate. (Urea-Formaldehyde 수지가공포에 있어 Resorcinol의 유리 Formaldehyde 포착효과)

  • Kang, In-Sook;Kim, Sung-Reon
    • Textile Coloration and Finishing
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    • v.9 no.2
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    • pp.41-49
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    • 1997
  • To control free formaldehyde release from fabric finished with N-methylol compounds, resin finished cotton fabric was treated with resorcinol solution, dried and cured. Factors affecting to control formaldehyde release have been investigated. It was shown that the aftertreatment with resorcinol greatly suppressed the free formaldehyde release. Up to concentration of about 5% of resorcinol, the concentration of resorcinol effected on the control of free and evolved formaldehyde. And at high concentration of resorcinol, however, the concentration became rather insensitive to contol formaldehyde release. Addition of some salt catalysts such as ammonium chloride, zinc nitrate, sodium acetate and ammonium acetate, was effective in decreasing formaldehyde release. Considering the effect on the control of formaldehyde and crease recovery, ammonium acetate was concidered to be the best catalyst. It was observed that the optimum curing temperature for the resorcinol treatment was about 15$0^{\circ}C$, and that the curing time did not affected formaldehyde release over three minutes. Although the treatment of resorcinol had a little adverse effect on crease recovery of resin finished fabric, this effect could be negligible.

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Development of High Performance Curing Agent and Effective Dispersion Method of Nanomaterials (고성능 피막양생제 개발 및 나노물질의 분산방안 평가)

  • Son, Ho-Jung;Yoo, Byung-Hyun;Lee, Dong-Gyu
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.12
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    • pp.230-236
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    • 2019
  • Recently, issues related to the quality of concrete have continuously resulted in surface quality problems, such as the exfoliation of concrete surfaces due to the cost reduction of cement and poor quality fine aggregate, scaling of surfaces caused by laitance, and plastic shrinkage cracks. Prompted by social issues, the application of a photo catalyst to road structures is being attempted to solve the environmental problems caused by fine dust and automobile exhaust. In this study, chemical admixtures were developed to improve the surface quality of concrete and to apply and distribute titanium dioxide in nanoscale sizes to provide basic data for the development of a photocatalyst-curing agent. As a result of the experiment, silicon and silane were reviewed as a raw material as a curing agent to develop a high performance curing agent with better film performance than conventional curing agents because they could form a film quickly on a fresh concrete surface. The distributed stability of the ultrasonic disperser showed the best performance through an outdoor test for four weeks to review the dispersion measures for the application of nanomaterials.

Curing and Coating Properties of Photo-Curable Self-Photoinitiating Acrylate (광경화형 자가광개시 아크릴레이트의 경화특성 및 도막물성)

  • Han, A-Ram;Hong, Jin-Who;Kim, Hyun-Kyoung
    • Journal of Adhesion and Interface
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    • v.15 no.1
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    • pp.22-30
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    • 2014
  • Self-photoinitiating acrylate (SPIA) which can undergo self-initiation under UV irradiation was synthesized by a Michael addition in the presence of a base catalyst. The SPIA polymerizations were investigated by photo-differential scanning calorimeter (photo-DSC) and surface physical properties such as pendulum hardness and pencil hardness. The results showed that the SPIA can cure upon UV irradiation by itself without a photoinitiator. But we found out that both the curing rate and the conversion were too low for the self-curing reaction of SPIA. In order to improve the SPIA curing properties, we introduced the SPIA/cationic hybrid system and observed the effects of the addition of commercial free radical type monomer and photoinitiator on the curing behaviors. SPIA/cationic hybrid system was the best suitable to improve the SPIA curing properties. The kinetic analysis indicated that the cationic monomer and photoinitiator apparently accelerated the cure reaction and rate of the hybrid SPIA system, mostly due to the synergistic effect of cationic monomer and photoinitiator increasing the mobility of active species and the generation of reactive species (free radical, cation) during the photopolymerization process. The physical properties showed that, unlike typical free radical system, the hybrid systems did not show oxygen inhibition effect because of cationic reaction on the coating surface.

Thermal Properties and fracture Toughness of Difunctional Epoxy Resins Cured by Catalytic Initiators (촉매형 개시제로 경화된 이관능성 에폭시 수지의 열적 특성 및 파괴인성)

  • 박수진;허건영;이재락
    • Polymer(Korea)
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    • v.26 no.3
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    • pp.344-352
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    • 2002
  • In this work, two thermal cationic latent catalysts, i.e., triphenyl benzyl phosphonium hexafluoroantimonate (TBPH) and benzyl 2-methylpyrazinium hexafluoroantimonate (BMPH) were newly synthesized. And the thermal and mechanical properties of difunctional epoxy (diglycidylether of bisphenol h, DGEBA) resins initiated by 1 phr of either TBPH or BMPH catalyst were investigated. As experimental results, the epoxy/TBPH system showed higher curing temperature and critical stress intensity factor ($K_{IC}$) than those of epoxy/BMPH. This could be interpreted in terms of slow thermal diffusion rate and bulk structure of four phenyl groups in TBPH. However, the decomposed activation energy determined from Coats-Redfern method was lower in the case of epoxy/TBPH. This result was probably due to the fact that broken short chain structure was developed by steric hindrance of TBPH.

A Study on the Early Strength Prediction of Lightweight Polymer Mortars by the Maturity Method (적산온도법에 의한 경량 폴리머 모르터의 초기강도 예측에 관한 연구)

  • 이윤수;대빈가언;연규석
    • Magazine of the Korea Concrete Institute
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    • v.10 no.6
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    • pp.191-202
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    • 1998
  • The maturity method in which the strength increase of cement concrete is expressed as a function of an intergral of the curing period and temperature of the concrete has often been applied to its strength prediction. For the purpose of the application of the maturity method to the compressive strength prediction for lightweight polymer mortars using an unsaturated polyester resin as a binder, the lightweight polymer mortars with various catalyst and accelerator contents, are prepared. tested for compressive strength, and the datum temperatures for the maturity equations are estimated. The maturity is calculated by using the maturity equations with the estimated datum temperature. The compressive strengths of the lighweight polymer mortars are predicted from the maturity-compressive strength relationships.

Synthesis of Novel Hydroxy-terminated Polyether for Solid Propellent Polyurethane Binder (고체 추진제용 폴리우레탄 바인더를 위한 새로운 폴리에테르 공중합체 디올(HTPE)의 합성)

  • Shin, Bum-Sik;Lee, Bum-Jae;You, Ho-Joon;Park, Young-Chul
    • Proceedings of the Korean Society of Propulsion Engineers Conference
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    • 2008.05a
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    • pp.221-226
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    • 2008
  • Novel synthetic routes were proposed for hydroxy-terminated Poly(EO-co-THF) by Cationic ring-opening copolymerization of Tetrahydrofuran(THF) and Ethylene oxide(EO). It was carried out using Boron trfluoride tetrahydrofuranate($BF_3$ THF complex) as catalyst in the presence of 1,4-butandiol. The resultant products are well-defined linear polyetherpolyol. Polyurethane(TPU) were prepared using resultant polyetherpolyol with IPDI/N-100 as curing agent and TPB(Triphenylbismuth) /MA(Maleic anhydride) mixture as cure catalyst. Mechanical properties of TPU prepared from poly(EO-co-THF) polyol were investigated and compared with polyurethane using ATK HTPE.

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Effect of Metal Complexes as a Catalyst on Curing Behavior and Mechanical Properties of Silica Filled Epoxy-Anhydride Compounds (촉매로서 금속 착화합물이 실리카가 충전된 에폭시-산무수물 복합체의 경화 거동 및 물성에 미치는 영향)

  • Seo, Byeongho;Lee, Dong-Hoon;Lee, Noori;Do, Kiwon;Ma, Kyungnam;Kim, Wonho
    • Elastomers and Composites
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    • v.49 no.1
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    • pp.59-65
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    • 2014
  • In this study, in order to complete curing reaction of the molding compound comprising an epoxy/anhydride at $71^{\circ}C$ for 40 hours, metal coordination complexes such as cobalt (II) acetylacetonate, potassium acetylacetonate, iron (III) acetylacetonate and chromium (III) octoate as a catalyst were applied to the epoxy/anhydride compounds respectively. The weight ratio of an epoxy part/an anhydride part was adjusted to improve the mechanical properties of the molding compound. According to the experimental results, an epoxy/anhydride compound containing chromium (III) octoate showed a high conversion at $71^{\circ}C$ for 40 hours as well as a proper processability at room temperature among the several metal coordination complexes. For the mechanical properties of the cured epoxy/anhydride compound, the compounds containing weight ratio from 0.9/1 to 0.5/1 of the epoxy part/anhydride part with chromium (III) octoate showed the high flexural strength, and higher compressive strength was shown with increasing of the hardener part.

Effects of Equivalent Weight of Epoxy Resins and Content of Catalyst on the Curing Reaction in Cationic Catalyst/Epoxy Cure System (양이온 촉매/에폭시 경화계에서 에폭시 수지의 당량 및 촉매 함량이 경화반응에 미치는 영향)

  • Kim, Youn Cheol;Park, Soo-Jin;Lee, Jae-Rock
    • Applied Chemistry for Engineering
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    • v.8 no.6
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    • pp.960-966
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    • 1997
  • The effects of epoxy resins and content of catalyst on the cure characteristics were studied by FT-IR, DSC and dynamic viscometer for the thermal properties and rheological properties of the catalytic (N-Benzylpyrazinium hexafluoroantimonate, BPH) epoxy thermosetting system. Compared with DSC results of DEGBF containing 0.5wt% BPH, the DSC thermograms of DGEBA containing 0.5wt% BPH indicated that the reaction was faster than that of DGEBF/BPH and the conversion rate of DGEBA/BPH was high in the initial stage of the reaction. As the concentration of BPH increases, the reaction and conversion rates show similar value in both the cases. The influence of hydroxyl group of epoxy resin on gel point defined from the crossover point of storage modulus (G') and loss modulus (G") could be explained by the formation of 3-dimensional network in the initial stage owing to the curing reaction between epoxides and hydroxyl groups of epoxy resin. This was consistent with the gel point obtained from DSC, FT-IR and moduli crossover. The activation energy (Et) obtained from the crossover point (G'/G"=1) are $31-39kJ.mol^{-1}$ for various BPH compositions in case of two epoxy systems.

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A Comparative Study on Polyurethane Coating Films Prepared Using 4,4'-Methylenebis(2-chloroaniline) and 1,3-Propanediolbis(4-aminobenzoate) as Crosslinking Agents (4,4'-Methylenebis(2-chloroaniline)과 1,3-Propanediolbis(4-aminobenzoate)를 가교제로 사용하여 제조한 폴리우레탄 코팅 필름의 특성 비교)

  • Lee, Youn-Sik;Lee, Sung-Il;Kim, Duk-Bae;Park, Young-Deok;Kim, Jung-Kee;Hahn, Yoon-Bong;Nahm, Kee-Suk
    • Elastomers and Composites
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    • v.39 no.1
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    • pp.71-76
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    • 2004
  • 4,4'-Methylenebis(2-chloroaniline)(MOCA) has been widely used as a crosslinking agent, but classified as a toxic chemical. Thus, its use will be limited in the near future. In this research, polyurethane coating films were prepared using 1,3-propanediolbis(4-aminobenzoate)(PDBA) as an alternative to MOCA. The base part was prepared by melting MOCA or PDBA in polyoxypropylene($M_n$=2000), followed by the addition of the various additives. The NCO-terminated toluene diisocyanate prepolymer was used as a curing agent. The polyurethane coating films were prepared by mixing the base part with the curing agent in an appropriate ratio at room temperature. The polyurethane coatings prepared using PDBA exhibited higher initial viscosity, but much longer pot lift, compared to those prepared using MOCA under the same conditions, due to lower reactivity of PDBA. The tensile strength and tear strength of the coating films were much weaker. However, the pot life, tensile strength, elongation, and tear strength of the coating films, prepared using PDBA in the presence of an increased amount of Pb(II)-octoate, were close to those of the coating films prepared using MOCA. Thus, it was concluded that PDBA can substitute MOCA in the preparation of polyurethane coatings as long as the reactivity of PDBA is enhanced using appropriate amounts of the catalyst or other appropriate catalyst.