• Title/Summary/Keyword: 3(trimethoxysilyl)propyl methacrylate

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Spectroscopic Studies on the Reaction between Amino Groups on Silica Nanoparticle Surface and Glycidyl Methacrylate (실리카 나노입자 표면에 결합된 아미노기와 Glycidyl Methacrylate의 반응에 관한 분광학적 연구)

  • Lee, Sangmi;Ha, KiRyong
    • Polymer(Korea)
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    • v.37 no.6
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    • pp.777-783
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    • 2013
  • We used dipodal type bis[3-(trimethoxysilyl)propyl]amine (BTMA) silane coupling agent to modify silica nanoparticles to introduce secondary amino groups on the silica surface. These grafted N-H groups were reacted with glycidyl methacrylate (GMA) to introduce polymerizable methacrylate groups on the silica surface. After modification reaction, we used several analytical techniques such as Fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and solid state $^{13}C$ cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR) to analyze the effects of reaction time, reaction temperature and used GMA concentration on the modification degree between N-H groups on the silica surface and epoxide groups of GMA. We found increased introduction of methacrylate groups on the silica surface by ring opening reaction of epoxide groups of GMA with N-H groups on BTMA treated silica with increased reaction time, reaction temperature and used GMA concentration within our experimental conditions.

Spectroscopic Analysis on Michael Addition Reaction of Secondary Amino Groups on Silica Surface with 3-(Acryloyloxy)-2-hydroxypropyl Methacrylate (2차 아미노기가 결합된 실리카 나노 입자 표면에 3-(Acryloyloxy)-2-hydroxypropyl Methacrylate의 마이클 부가 반응에 대한 분광학적 분석)

  • Lee, Sangmi;Ha, Ki Ryong
    • Polymer(Korea)
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    • v.38 no.2
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    • pp.257-264
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    • 2014
  • In this study, we modified silica nanoparticles with bis[3-(trimethoxysilyl)propyl]ethylenediamine (BTPED) silane coupling agent, which has two secondary amino groups in a molecule, to introduce amino groups on the silica surface. After modification of silica, we used acrylate group containing 3-(acryloyloxy)-2-hydroxypropyl methacrylate (AHM) to introduce polymerizable methacrylate groups by Michael addition reaction. We used Fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and liquid and solid state cross polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR) to understand the reactions between N-H groups of BTPED modified silica surface and acrylate groups of AHM monomer. We confirmed Michael addition reaction between BTPED modified silica and AHM completed in 2 hr reaction time. We also found increased methacrylate group introduction with increase of mol ratio of the acrylate group of AHM to N-H group of BTPED modified silica by increase of C=O peak area of measured FTIR spectra. These results were also supported by EA and solid state $^{13}C$ and $^{29}Si$ NMR results.

Quantitative Analysis of Grafted Methacrylate Groups by Michael Addition Reaction between Primary and Secondary Amino Groups on the Silica Nanoparticle Surface with 3-(Acryloyloxy)-2-Hydroxypropyl Methacrylate (실리카 나노 입자 표면에 결합된 1차 및 2차 아미노기와 3-(Acryloyloxy)-2-hydroxypropyl Methacrylate의 마이클 부가 반응에 의해 도입되는 메타크릴레이트기의 정량적 분석)

  • Lee, Sangmi;Ha, KiRyong
    • Polymer(Korea)
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    • v.39 no.2
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    • pp.300-310
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    • 2015
  • In this study, we modified silica nanoparticles with N-[3-(trimethoxysilyl)propyl]ethylenediamine (TPED) silane coupling agent, which has one primary and one secondary amino groups in a molecule, to introduce amino groups on the silica surface. After modification of silica, we used 3-(acryloyloxy)-2-hydroxypropyl methacrylate (AHM) to introduce methacrylate groups by Michael addition reaction. We found about 30% of N-H groups on the TPED modified silica surface reacted with acrylate groups of AHM compared to about 85% of reaction between N-H groups of pure TPED with acrylate groups of pure AHM. This lower degree of Michael addition reaction for heterogeneous reaction between N-H groups on the solid TPED modified silica and liquid AHM compared to homogeneous reaction between pure liquid TPED and pure liquid AHM may be caused by lower mobility of grafted amino groups of TPED moiety and higher steric hindrance caused by solid silica particles.

Self-Curable Humidity-Sensitive Polyelectrolytes Attached to the Alumina Substrate for the Humidity Sensor and their Stability in Water (알루미나 기재에 부착된 습도센서용 자기 가교형 감습성 전해질 고분자의 내수성)

  • Han, Dae-Sang;Gong, Myoung-Seon
    • Polymer(Korea)
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    • v.34 no.4
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    • pp.313-320
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    • 2010
  • New cinnamate group-containing copolymers for a self-curable, humidity-sensitive polyelectrolyte and polymeric anchoring agents were prepared by copolymerization of [2-[(methacryloyloxy) ethyl]dimethyl]propyl ammonium bromide(MEPAB), methyl methacrylate(MMA), 3-(trimethoxysilyl) propyl methacrylate(TMSPM) and 2-(cinnamoyloxy)ethyl methacrylate(CEMA). Photocrosslinkable copolymer composed of MEPAB/MMA/TMSPM/CEMA=70/20/0/10 were used for humidity-sensitive membrane, and those of 50/0/20/30 and 0/0/50/50 were used for polymeric anchoring agents. 3- (Triethoxysilyl)propyl cinnamate(TESPC) was also used as a surface-pretreating agent for the comparison of capability of attachment of polyelectrolyte to the electrode surface with polymeric photocurable silanecoupling agents. Pretreatment of the electrode substrate with anchoring agents was performed to form a cinnamate thin film on the electrode through covalent bonds. When the sensors were irradiated with UV light, the anchoring of a polyelectrolyte into the substrate was carried out via the [2$\pi$+2$\pi$] cycloaddition. The resulting sensors using polymeric anchoring agents and TESPC showed water durability with increase of resistance by 60~85%, which is corresponding to the reduction of 2.25~3.15%RH, after soaking in water for 24 h. They showed good hysteresis (-0.2%RH), response time (90 sec) and long-term stability at high temperature and humidity.

Improvement of Superhydrophobicity of Multi-Walled Carbon Nanotubes Produced by Fluorination

  • Meng, Long-Yue;Park, Soo-Jin
    • Carbon letters
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    • v.13 no.3
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    • pp.178-181
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    • 2012
  • In this work, we synthesized superhydrophobic coatings by chemical surface functionalization of multi-walled carbon nanotubes (MWCNTs). This was accomplished through the radical polymerization of 3-(trimethoxysilyl) propyl methacrylate modified MWCNTs and fluoro acrylate/methyl methacrylate. The chemical compositions and microstructures of the prepared MWCNT surface were investigated using X-ray photoelectron spectroscopy, Fourier transform infrared spectrometry, and scanning electron microscopy, respectively. The wettability of the MWCNTs surface was determined through contact angle assessments in different liquids. The resulting surface exhibited a water contact angle of $157.7^{\circ}$, which is clear evidence of its superhydrophobicity. The 3D MWCNT networks and the low surface energy of the -C-C- and -C-F- groups play important roles in creating the superhydrophobic surface of the MWCNTs.

Fabrication of Large-Area Photovoltaic Crystal with Modified Surface Using Trimethoxysilyl Propyl Methacrylate (TMSPM) for Solar Cell Protection

  • Kang, Kwang-Sun
    • Current Photovoltaic Research
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    • v.2 no.3
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    • pp.84-87
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    • 2014
  • Protection of solar cell surface is important to prevent from dust, pollen, sand, etc. Therefore, development of large area antifouling film is urgent for high performance of solar cells. The surface of silica spheres was modified to fabricate large area antifouling film. The surface of monodisperse silica spheres has been modified with 3-(trimethoxysilyl) propylmethacrylate (TMSPM) to fabricate large area photonic crystal. Although the surface modification of silica spheres with TMSPM has been failed for the base catalyst, the second trial using acid catalyst showed the following results. The FTIR absorption peak at $1721cm^{-1}$ representing C=O stretching vibration indicates that the TMSPM was attached on the surface of silica spheres. The methanol solution comprised of the surface modified silica spheres (average diameter of 380 nm) and a photoinitiator was poured in the patterned silicon wafer with the dimension of 10 cm x 10 cm and irradiated UV-light during the self-assembly process. The result showed large area crack and defect free nanostructures.

Spectroscopic Analysis on the Michael Addition Reaction between Secondary Amino Group Containing Silica Nanoparticles with (Meth)acrylate Monomers (2차 아미노기를 갖는 실리카 나노입자와 (메타)아크릴레이트 단량체와의 마이클 부가반응에 대한 분광학적 분석)

  • Jeon, Ha-Na;Ha, Ki-Ryong
    • Polymer(Korea)
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    • v.36 no.5
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    • pp.668-676
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    • 2012
  • In this study, we modified silica nanoparticles with bis[3-(trimethoxysilyl)propyl]amine (BTMA) silane coupling agent to introduce secondary amino groups on the silica surface. After modification of silica, we investigated effects of different types of (meth)acrylate group containing monomers on the Michael addition reaction to introduce reactive (meth)acrylate groups on the BTMA modified silica surface. We used two kinds of (meth)acrylate monomers, trimethylolpropane ethoxylate triacrylate (TMPET) which has three identical acrylate groups, and 3-(acryloyloxy)-2-hydroxypropyl methacrylate (AHM) which has one acrylate and one methacrylate group. We used fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and solid state cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR) to understand reactions between NH groups on the silica surface with (meth)acrylate groups of TMPET and AHM monomers. We found almost complete Michael addition reaction between all three acrylate groups of TMPET with NH groups on the BTMA modified silica. But, for the AHM treatment of BTMA modified silica, we found Michael addition reaction occurred only between acrylate groups of AHM and NH groups of silica surface, not between methacrylate groups of AHM and NH groups of BTMA modified silica surface.

Humidity-Sensitive Properties of Polyelectrolytes Containing Alkoxysilane Crosslinkers

  • Gong, Myoung-Seon;Lee, Chil-Won;Park, Hyung-Seok
    • Macromolecular Research
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    • v.12 no.3
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    • pp.311-315
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    • 2004
  • We have prepared new polyelectrolytes containing trialkoxysilyl groups by copolymerizing 3-(trimethoxysilyl)propyl methacrylate (TSPM) with either [2-(methacryloyloxy)ethyl]trimethyl ammonium chloride (METAC), [2-(methacryloyloxy)ethyl]dimethyl propyl ammonium bromide (MEDPAB), or [2-(acryloyloxy)ethyl]trimethyl ammonium chloride (AETAC). The copolymers TSPM/METAC, TSPM/MEDPAB, and TSPM/METAC having compositions of 15/85, 10/90, and 5/95, respectively, were self-crosslinkable polyelectrolytes that possess humidity-sensitive properties. We measured the impedances of the copolymers at various relative humidities (RHs) and found that the resistance was dependent on the content of METAC, MEDPAB, or AETAC. The impedance changed from 10$\^$7/ $\Omega$ at 20% RH to 10$^3$ $\Omega$ at 95% RH, which is quite a suitable range for a humidity sensor that is to be utilized at ambient humidity. We also performed tests of the materials temperature dependence, hysteresis, response time, and water durability.

Silane-crosslinked Proton Exchange Membranes Prepared by a Stepwise Radiation Grafting (방사선 그래프트를 순차적으로 진행하여 제조된 실란 가교구조의 수소이온교환막)

  • Lee, Ji-Hong;Choi, Hongsuk;Song, Ju-Myung;Sohn, Joon-Yong;Shin, Junhwa
    • Polymer(Korea)
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    • v.36 no.6
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    • pp.816-821
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    • 2012
  • In this study, silane-crosslinked proton exchange membranes were prepared by step-wise radiation grafting of styrene and 3-(trimethoxysilyl)propyl methacrylate (TMSPM) onto an poly(ethylene-co-tetrafluoroethylene) (ETFE) film and followed by sol-gel processing and sulfonation. The sequentially grafted films with styrene to provide the proton conductivity and TMSPM to form the crosslinked structure were prepared by different grafting order. The structural changes and thermal properties of the prepared films were investigated by FTIR and TGA, respectively. After the introduction of sulfonic acid functional groups, the distributions of sulfonic acid group and silicon atoms at the inside of the sulfonated membranes were analyzed by SEM-EDX.

ZrO2/TiO2/Organosilane Hybrid Composites via Low Temperature Sol-Gel Process for Hard and Transparent Coating (저온 졸-겔 법을 이용한 투명 하드코팅 필름용 ZrO2/TiO2/Organosilane 복합체 연구)

  • Lee, Su-Hyeon;Choi, Jongwan
    • Journal of the Korean Applied Science and Technology
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    • v.35 no.1
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    • pp.80-88
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    • 2018
  • In this study, we prepared hybrid composites by using low temperature sol-gel process for transparent and hard coating film. The hybrid composites consist of $ZrO_2/TiO_2/organosilane$, of which organosilane was introduced 3-(trimethoxysilyl)propyl methacrylate due to the role of a photocurable ceramic material for low temperature process. The ceramic composites with various composition ratios were coated on a polycarbonate substrate using a sol-gel process of low temperature process, and characterized optical and mechanical properties of coated thin film. The transparencies of coated thin films were 97.5 % or more, and the pencil hardness were 9H or more. In the case of the ZTS-2-1, the nano-indentation hardness was measured at the highest value of 1.14 GPa.