Co-reporter:Sheng Li Wu;Tie Jun Shi;Li Yuan Zhang
Journal of Applied Polymer Science 2016 Volume 133( Issue 11) pp:
Publication Date(Web):
DOI:10.1002/app.43117
ABSTRACT
This study describes a simple and effective method of synthesis of a polyurethane/graphene nanocomposite. Cationic waterborne polyurethane (CWPU) was used as the polymer matrix, and graphene oxide (GO) as a starting nanofiller. The CWPU/GO nanocomposite was prepared by first mixing a CWPU emulsion with a GO colloidal dispersion. The positively charged CWPU latex particles were assembled on the surfaces of the negatively charged GO nanoplatelets through electrostatic interactions. Then, the CWPU/chemically reduced GO (RGO) was obtained by treating the CWPU/GO with hydrazine hydrate in DMF. The results of X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and Raman analysis showed that the RGO nanoplatelets were well dispersed and exfoliated in the CWPU matrix. The electrical conductivity of the CWPU/RGO nanocomposite could reach 0.28 S m−1, and the thermal conductivity was as high as 1.71 W m−1 K−1. The oxygen transmission rate (OTR) of the CWPU/RGO-coated PET film was significantly decreased to 0.6 cm3 m−2 day−1, indicating a high oxygen barrier property. This remarkable improvement in the electrical and thermal conductivity and barrier property of the CWPU/RGO nanocomposite is attributed to the electrostatic interactions and the molecular-level dispersion of RGO nanoplatelets in the CWPU matrix. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016, 133, 43117.
Co-reporter:Guomei Xu, Tiejun Shi, Yu Xiang, Wei Yuan and Quan Wang
RSC Advances 2015 vol. 5(Issue 94) pp:77429-77436
Publication Date(Web):26 Aug 2015
DOI:10.1039/C5RA10083F
A Mo-CPF/P1B hybrid has been prepared from molybdenum modified cardanol phenolic resin (Mo-CPF) and cardanol benzoxazine with phosphorus (P1B). Cardanol benzoxazine with phosphorus (P1B) has been synthesized from cardanol-allylamine-based benzoxazine (BZc-a) and DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide). Cardanol phenolic resin modified with molybdenum (Mo-CPF) has been synthesized by reacting cardanol-based phenolic resin (CPF) with ammonium molybdate tetrahydrate at 150 °C, where the CPF was synthesized from cardanol and paraformaldehyde in the presence of sodium hydroxide at 65 °C. The synthesized CPF and Mo-CPF were characterized by 1H-NMR and size exclusion chromatography (SEC). Mo-CPF was mixed with P1B, and the mixtures were cured at 110 °C for 4 h and got the Mo-CPF/P1B hybrid. The properties of the Mo-CPF/P1B hybrid were investigated; the results demonstrated that the mechanical and thermal properties, together with flame retardance, were greatly improved. Dynamic Mechanical Analysis (DMA) measurement results indicated that CPF, Mo-CPF and Mo-CPF/P1B could all sustain a large amount of stress and the elongations at break were different. DMA measurements suggested that the Tg of CPF, Mo-CPF and Mo-CPF/P1B was 98 °C, 170 °C and 131 °C respectively. Mo-CPF/P1B exhibited better flame retardance after conjugating with molybdenum and phosphorus. TGA results suggested that Mo-CPF/P1B exhibited better thermal properties. Field emission electron microscopy (FE-SEM) suggested that molybdenum was randomly distributed in Mo-CPF and Mo-CPF/P1B, and EDX indicated that molybdenum and phosphorus were randomly distributed in Mo-CPF/P1B.
Co-reporter:Guomei Xu;Quan Wang;Jianhua Liu;Yang Yi
Journal of Applied Polymer Science 2015 Volume 132( Issue 11) pp:
Publication Date(Web):
DOI:10.1002/app.41634
ABSTRACT
The design, preparation, and properties of two DOPO-containing compounds based on a cardanol-allylamine-paraformaldehyde benzoxazine (abbreviated as BZc-a) were described in this article. By controlling the amount of DOPO, it could react with BZc-a and generated different products. When DOPO: BZc-a <1 : 1, DOPO reacted only with allyl group, and generated a containing single DOPO group benzoxazine (P1B); When DOPO: BZc-a ≧ 1 : 1, DOPO reacted not only with allyl group but also nucleophilic addition reaction, got a N-substituted derivative P2B, which contain double DOPO groups. The chemical structure of P1B and P2B was characterized by 1H-NMR and 13C-NMR. Effect of DOPO on characteristics of BZc-a was investigated. Fire test demonstrated that P1B and P2B showed better flame retardance than BZc-a, and prepared two kinds of flame-retardance resin based on BZc-a. However, Field emission electron microscope observations showed the surface of P1B and P2B was very fragility, graphene oxide (GO) was chosen as to improve the surface performance. P1B/GO-3 wt % and P2B/GO-3 wt % composites were prepared by solution blending, and the thermal stability was studied by thermogravimetric analysis. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015, 132, 41634.
Co-reporter:Haiou Zhou;Xun Zhou
Journal of Applied Polymer Science 2014 Volume 131( Issue 2) pp:
Publication Date(Web):
DOI:10.1002/app.39761
ABSTRACT
Multi-hollow or hollow polymer particles are of great interest in many fields. Here we successfully fabricate polystyrene microspheres with aqueous cores through w/o/w Pickering emulsion stabilized by modified SiO2 nanoparticles. The final structure and constituents of the microspheres is investigated via SEM, X-ray photoelectron spectra, and thermo-gravimetric analysis. The results demonstrate that the size and amount of aqueous cores in the microspheres can be tuned by the original structure of the multiple emulsions: when the volume fraction of inner water is 0.2, the inner structure of the microspheres obtained is porous and each pore is not interconnected; when the volume fraction of inner water is increased to 0.7, the resulting products are hollow microspheres and when 0.3% wt/vol of salt is added to the inner aqueous phase, the inner pores of the resulting microspheres enlarge or even coalesce. The multi-hollow or hollow polystyrene microspheres with aqueous cores are expected to be candidates for encapsulation in biotechnology. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014, 131, 39761.
Co-reporter:Guo-mei Xu;Jianhua Liu;Qidong Wang
Journal of Applied Polymer Science 2014 Volume 131( Issue 11) pp:
Publication Date(Web):
DOI:10.1002/app.40353
ABSTRACT
A novel liquid benzoxazine was synthesized by Mannich reaction of cardanol, paraformaldehyde, and allylamine. The benzoxazine structure was characterized by 1H-NMR and FTIR. The liquid benzoxazine could dissolve easily in many solvents. The curing behavior of the benzoxazine was characterized by differential scanning calorimetry (DSC) and its curing temperature was about 233°C. A benzoxazine-functional silane coupling agent (BFSca) was synthesized with paraformaldehyde, phenolphthalein, and aminopropyltriethoxysilane. Graphene oxide (GO) was also made via improved Hummer's method. Then benzoxazine/GO composites were prepared using BFSca by solution blending and the curing behaviors of the composites were also characterized by IR, DSC, and thermogravimetric analysis. The minimum curing temperature and the highest 5% weight loss temperature for the composites was, respectively, 185 and 399.8°C. The SEM images of benzoxazine/GO composites demonstrated that BFSca had improved the dispersion of GO in the benzoxazine and also enhanced the thermal decomposition temperature of the composites. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014, 131, 40353.
Co-reporter:Xun Zhou, Tiejun Shi, Jing Wu, Haiou Zhou
Applied Surface Science 2013 Volume 287() pp:359-368
Publication Date(Web):15 December 2013
DOI:10.1016/j.apsusc.2013.09.156
Highlights
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The hydrothermal and lyophilization methods can reduce GO and anchor TNT to RGO sheets synchronously.
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The RGO-TNT can enhance the photocatalytic degradation of methylene blue, superior to pure TNT.
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The photocatalytic activity can be changed by adjusting mass ratios of TiO2 powder to GO used for preparation of RGO-TNT.
Co-reporter:Haiou Zhou, Tiejun Shi, Xun Zhou
Applied Surface Science 2013 Volume 266() pp:33-38
Publication Date(Web):1 February 2013
DOI:10.1016/j.apsusc.2012.11.054
Abstract
In this paper, polystyrene (PS)/SiO2 microspheres were successfully prepared via Pickering emulsion polymerization stabilized solely by ethacryloxypropyltrimethoxysilane (MPTMS) modified SiO2 nanoparticles. The formation mechanisms of PS/SiO2 microspheres with different morphology were investigated under various Pickering emulsion polymerization conditions. The results showed that SiO2 concentrations and initiator sorts would synergistically impact on the morphology of products corresponding to distinct formation mechanisms. When SiO2 concentrations was low and water-solute initiator potassium persulfate (KPS) was used, aqueous nucleation was dominant, which was deduced to the formation of dispersive microspheres sparsely anchored by SiO2 particles. When SiO2 concentrations was increased and oil-solute initiator azobisisobutyronitrile (AIBN) was applied, nucleation in oil phase prevailed which lead to the formation of microspheres densely packed by SiO2 particles.
Co-reporter:Xun Zhou, Tiejun Shi
Applied Surface Science 2012 Volume 259() pp:566-573
Publication Date(Web):15 October 2012
DOI:10.1016/j.apsusc.2012.06.113
Abstract
A one-pot hydrothermal synthesis was used to obtain a mesoporous SiO2–graphene hybrid from tetraethylortho silicate and graphene oxide without any surfactant. Graphene obtained from hydrothermal reduction, with a certain oxygen-containing groups, plays a key role in attaching SiO2 nanoparticles, as examined by X-ray diffraction, Raman spectroscopy, transmission electron microscopy and scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and atomic force microscopy. The synthesis technique combines protection, reduction and functionalization in one step. Nitrogen adsorption/desorption isotherms showed that the hybrid was tunable in surface area (244.7–524.61 m2/g), pore size (8.9–69.26 nm) and its distribution by simple adjustment of the mass ratio of tetraethylortho silicate and graphene oxide.
Co-reporter:Xun Zhou, Tiejun Shi, Haiou Zhou
Applied Surface Science 2012 Volume 258(Issue 17) pp:6204-6211
Publication Date(Web):15 June 2012
DOI:10.1016/j.apsusc.2012.02.131
Abstract
Hydrothermal method was utilized to prepare reduced graphene oxide (RGO) and fabricate ZnO–RGO hybrid (ZnO–RGO) with zinc nitrate hexahydrate and graphene oxide (GO) as raw materials under pH value of 11 adjusted by ammonia water. During the process of reduction of GO, hydrothermal condition with ammonia provided thermal and chemical factors to synthesize RGO. The retained functional groups on RGO planes played an important role in anchoring ZnO to RGO, which was characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning and transmission electron microscopy and photoluminescence spectra. The various mass ratios of zinc nitrate hexahydrate to GO used to prepare ZnO–RGO impacted significantly on the morphology of ZnO nanostructures such as nanoparticles and nanorods. And, the RGO sheets wrapped ZnO nanoparticles and nanorods very tightly. After the emission of photo electrons from ZnO, RGO in ZnO–RGO can effectively transfer the photo electrons to exhibit a high performance and reproducibility in photocatalytic degradation toward methylene blue (MB) absorbed on the surface of RGO through π–π conjugation.
Co-reporter:Dexin Tan;Zhong Li
Research on Chemical Intermediates 2011 Volume 37( Issue 8) pp:831-845
Publication Date(Web):2011 October
DOI:10.1007/s11164-011-0291-1
Vinyltri(phenylethynyl)silane ((ph–C≡C)3–Si–C=CH2; VTPES) and phenyltri(phenylethynyl)silane ((ph–C≡C)3–Si–ph; PTPES) were synthesized by Grignard reaction. Their molecular structures were characterized by means of 1H NMR, 13C NMR, 29Si NMR, and FT-IR spectroscopy. Their nonisothermal thermal curing processes were characterized by DSC, and the corresponding kinetic data, for example activation energy (E), pre-exponential factor (A), and the order of the reaction (n), were obtained by the Kissinger method. The results showed that the melting points of VTPES and PTPES were 84 and 116 °C, respectively. Their curing reaction rates were consistent with first-order kinetic equations. VTPES monomer had a lower activation energy and curing temperature as a result of coordination between reactive groups.
Co-reporter:Liying Guo;Zhong Li
European Journal of Wood and Wood Products 2011 Volume 69( Issue 3) pp:383-389
Publication Date(Web):2011 August
DOI:10.1007/s00107-010-0438-6
Ionic liquid of 1-(2-hydroxylethyl)-3-ethyl imidazolium chloride ([HeEIM]Cl) was synthesized and its chemical structure was examined by FTIR and 1HNMR. Dissolution of the fir powder which was activated with 25% NaOH under different conditions in the ionic liquid was studied. Acrylamide (AM) was grafted onto the dissolved fir powder in [HeEIM]Cl and aqueous medium, respectively. Technologic conditions for graft copolymerization were optimized by orthogonal test. The results showed that the ionic liquid exhibited good solubility for the fir powder, the dissolution rate was as high as 18.3%. The graft copolymer prepared in [HeEIM]Cl had higher grafting degree and grafting efficiency than in aqueous medium. The most suitable conditions for graft copolymerization were: mass fraction of AM 25%, fluid ratio of [HeEIM]Cl to wood 30:1, and mass proportion of wood to AM 1:4. FTIR and SEM suggested that AM had been grafted onto the fir powder. XRD and TG indicated that the crystalline structure of the wood fiber had been destroyed thoroughly after being grafted, and the thermal stability of graft copolymer had been improved.Die ionische Flüssigkeit 1-(2-Hydroxyethyl)-3-ethyl-imidazolchlorid ([HeEIM]Cl) wurde synthetisiert und ihre chemische Struktur wurde mittels FTIR und 1HNMR überprüft. Die Auflösung von Tannenholzmehl, das mit 25 % NaOH unter unterschiedlichen Bedingungen aktiviert worden war, wurde in ionischer Flüssigkeit untersucht. Acrylamid (AM) wurde auf das aufgelöste Tannenholzmehl in [HeEIM]Cl sowie in einem wässrigen Medium aufgepfropft. Mittels orthogonaler Versuche wurden die technologischen Bedingungen der Pfropfcopolymerisation optimiert. Die Ergebnisse zeigten, dass die ionische Flüssigkeit für die Auflösung von Tannenholzmehl gut geeignet war. Die Auflösungsrate betrug bis zu 18,3 %. Das in [HeEIM]Cl hergestellte Pfropfcopolymer wies einen höheren Pfropfgrad und eine höhere Pfropfeffizienz auf als dasjenige, das in wässrigem Medium hergestellt worden war. Die am besten geeigneten Bedingungen einer Propfcopolymerisation ergaben sich bei einem Massenanteil von AM von 25 %, einem Flüssigkeitsverhältnis von [HeEIM]Cl zu Holz von 30:1 und einem Massenverhältnis von Holz zu AM von 1:4. FTIR- und REM-Untersuchungen lassen darauf schließen, dass AM auf das Tannenholzmehl gepfropft wurde. Röntgendiffraktometrie (XRD) und thermogravimetrische Analyse (TG) zeigten, dass die kristalline Struktur der Holzfaser nach der Pfropfung vollkommen zerstört worden war und sich die Wärmebeständigkeit des Pfropfcopolymers verbessert hatte.
Co-reporter:Honglu Xie
Wood Science and Technology 2010 Volume 44( Issue 1) pp:119-128
Publication Date(Web):2010 February
DOI:10.1007/s00226-009-0273-2
The results of wood liquefaction by allyl alkyl imidazolium ionic liquids indicated that wood (Metasequoia glyptostroboides) without any pretreatment is liquefied in ionic liquids at temperatures below 100°C within 40 min. Acidic ionic liquids show low residue even at 70°C and 30 min. The liquid/wood ratio of the reactants affects the reaction course. After the reaction is over, ionic liquids can be separated from the products and recycled at least five times maintaining good liquefaction activity. The suitability of the ionic liquids for wood liquefaction is ascribed to the functional groups of the ionic liquids. Influencing factors of wood liquefaction are discussed in relation to the ionic composition of the ionic liquids.
Co-reporter:J Wang;TJ Shi;XC Jiang
Nanoscale Research Letters 2009 Volume 4( Issue 3) pp:
Publication Date(Web):2009 March
DOI:10.1007/s11671-008-9232-3
This work demonstrates the synthesis of core-shell ZrO2/PAAEM/PS nanoparticles through a combination of sol–gel method and emulsifier-free emulsion polymerizaiton. By this method, the modified nanometer ZrO2cores were prepared by chemical modification at a molecular level of zirconium propoxide with monomer of acetoacetoxyethylmethacrylate (AAEM), and then copolymerized with vinyl monomer to form uniform-size hybrid nanoparticles with diameter of around 250 nm. The morphology, composition, and thermal stability of the core-shell particles were characterized by various techniques including transmission electron microscopy (TEM), X-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and thermal-gravimetry analyzer (TGA). The results indicate that the inorganic–organic nanocomposites exhibit good thermal stability with the maximum decomposition temperature of ~447 °C. This approach would be useful for the synthesis of other inorganic–organic nanocomposites with desired functionalities.
Co-reporter:Qiu-Sheng Song;Tie-Jun Shi;Hai-Hong Ma
Polymer Bulletin 2008 Volume 61( Issue 4) pp:473-480
Publication Date(Web):2008 October
DOI:10.1007/s00289-008-0972-0
Two kinds of hybrid PAN/SiO2 sols were prepared via either sols blend or
in-situ polymerization, respectively, and their spinnability was investigated.
Hydrolysis time (t1) and spinnable time (t2) of both hybrid
sols increased with PAN content. The hybrid fibers were characterized with FTIR, DSC, SEM and TG. As
evidenced from the FT-IR spectra and DSC measurements, different chemical structures of hybrid fibers
were different with CN groups hydrolyzed in the hybrid fibers via in-situ
polymerization. SEM measurements showed the interior structures of the hybrid fibers via in-situ
polymerization were more homogeneous. TG measurements suggest both of the hybrid fibers show better
resistance to heat than pure PAN.