• Volume 34,Issue 1,2017 Table of Contents
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    • >Review and monographs
    • Progress on Synthesis and Application of Polysilsesquioxane Micro/ nanospheres

      2017, 34(1).

      Abstract (1334) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Polysilsesquioxane micro/nanospheres (PSQ M/NPs) are a family of novel organic-inorganic hybrid materials in terms of the unique structure and outstanding performance properties. Beside, they were readily obtained. Therefore, they have the major potential to be used in the fields of chemistry and materials as a hot area of research. This paper reviewed recent synthetic methods of the functional polysilsesquioxane micro/nanospheres and their applications in the domains of luminescent materials, absorbent materials, biomedical materials, flame retardents, and functional coatings. Ultimately, the future developing trend and the existing problems have been proposed in the study of polysilsesquioxane micro/nanospheres.

    • >Functional materials
    • Synthesis of Thiolated Chitosan Hydrogel for Redox-responsive Controlled Release of Protein

      2017, 34(1).

      Abstract (1536) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The thiolated chitosan (CS-NAC) was synthesized by grafting N-acetyl-L-cysteine (NAC) onto chitosan chain and the structure was characterized by 1HNMR and FTIR. The content of thiol group in CS-NAC was determined to be 275.8μmol/g by Ellman’s method. The disulfide bond crosslinked CS-NAC hydrogel was prepared by oxidation coupling of thiol with oxygen. The stable hydrogel was obtained in the CS-NAC concentration range of 1.5wt% to 3.0wt%. The swelling ratio of CS-NAC hydrogel decreased from 45.5 to 31.2 and the mesh size (ξ) diminished from 340nm to 242nm with increasing the concentration of CS-NAC from 1.5wt% to 3.0wt%. The redox-responsive degradation of CS-NCA hydrogel was observed. About 80% hydrogel was degraded in 10mmol/L dithiothreitol (DTT) solution within 400min, and complete degradation was observed in 50mmol/L L-cysteine (L-Cys) solution. Bovine serum albumin (BSA) was used as model protein and encapsulated into the CS-NAC hydrogel during the oxidation crosslinking reaction. Redox-responsive release of BSA in vitro from CS-NAC hydrogel was obtained. More than 80% of encapsulated BSA was released from the hydrogel in 10mmol/L DTT solution within 30 h, while only 58% of BSA was released from the hydrogels in PBS. The release kinetics of BSA in 10mmol/L DTT solution is closed to first order and the encapsulated protein was released via a typical Fickian diffusion-controlled form from the CS-NAC hydrogel.

    • Preparation and Characterization of New Type Solid Acid Catalyst SO42-/C-TiO2-CeO2

      2017, 34(1).

      Abstract (1410) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Complex rare earth solid acid catalyst SO42-/C-TiO2-CeO2 was prepared using high temperature sulfonation.The catalytic performance of the catalyst was evaluated by esterification reaction of oil acid and methanol as a probe reaction and the influence of catalytic activity such as the content of the rare earth CeO2,sulfonation temperature and sulfonation time was studied.The results showed that the catalyst SO42-/C-TiO2-CeO2 was prepared under the best preparation conditions of the rare earth CeO2 mol percentage of 2%,the sulfonation temperature of 200℃ and sulfonation time of 10h,under these conditions,the catalytic esterification rate of waste oil with methanol esterification was highest and reached 94.78%.The catalyst was characterized by FTIR,XRD,SEM,DTG and X-ray fluorescence,which shows that the rare earth oxide CeO2 and metal oxide TiO2 cured SO42- role in common, promoted SO42- with bidentate structure, enhanced catalytic activity and improved the stability of the catalyst SO42- /C-TiO2-CeO2.

    • Synthesis, Structure and Electrochemical Performance of SnO2 Nanospheres

      2017, 34(1).

      Abstract (1237) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:SnO2 nanospheres were synthesized by hydrothermal method with Na2SnO3.4H2O as raw material and CO(NH2)2 as surfactant. The crystal structure, surface morphology and specific surface area were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Brunner-Emmet-Teller(BET). Electrochemical performance was analyzed by electrochemical measurement. The results showed that the particle uniform dispersion and emidiameter size was about 400 nm and the Structure is typical of rutile phase. As an active material for lithium-ion batteries,the SnO2 nanospheres material’s first discharge capacity of 2206.6 mAh/g at a current density of 200 mA/g and at 0.01~3.0 V. The specific discharge capacity decreased to 440 mAh/g after 50 cycles. Data from this study indicated that SnO2 nanospheres material with high capacity and superior cycling stability.

    • Preparation and Properties of Nano - SiO2 Hybrid Fluorinated Epoxy Resin Coating

      2017, 34(1).

      Abstract (982) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:The amino silicon sol(TB) was prepared using sol-gel method by ethyl orthosilicate (TEOS) and double [3-(triethoxy silane) propyl] amine (BTA) as the hydrolysis of precursors, sodium dodecyl benzene sulfonate (SDBS) as the surfactant, respectively. Then the resin(NA-FB) was prepared by copolymerization of ring opening of the epoxy group fluorinated epoxy acrylic resin (FBSA) and the nano TB. And the high performance nano-hybrid transparent coating was prepared by NA-FB as the film-forming material. The chemical structurers, morphology and properties of products were studied by FTIR, XPS, TEM and SEM. The effects of SDBS dosage on nano-TB system stability and viscosity was observed and the impact of the amount of nano-TB on coating performance was also studied. The results indicate that nano TB has the microspheres structure of multiphase separation and uniformly dispersed from the microscopic view. The nano-TB has good stability and viscosity when the SDBS concentration is 0.5g/L. The coating has maximum hardness up to 5H, the contact angle of the coated surface up to 138°, the adhesion still remaining level 1 and has high transparency when amount of nano-TB is 10%.

    • Synthesis and Properties Research of Star Type Waterborne Polyurethane Associative Thickener

      2017, 34(1).

      Abstract (1438) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Using PEG and IPDI synthesis pre-polymers,glycerol and TMP used as chain extender,and the hexadecanol used as end-capping reagent,the star type waterborne polyurethane associative thickener(SHEUR) was prepared. FI-IR and GPC was used to characterize the molecular structure of the SHEUR. The viscosity of SHEUR water solution, the emulsion thickened by SHEUR and the rheological property of SHEUR aqueous solution,the effects of thickener on the thickening properties of different structures were studied by NDJ-8s viscometer and Gemini-HR Nano rotational rheometer. The experimental result indicated that the effect of star type structure of HEUR is much better than linear HEUR,add 1% of thickener to acrylic emulsion, it's viscosity increased to 61440 mPa· s , which thickened by SHEUR ,while by LHEUR is just 202 mPa· s. At low shear rate , the viscosity of SHEUR is kept high standard. When shear rate is greater than 100s-1, SHEUR will appear shear-thinning phenomenon. The research of rheologybehavior and grain size after thickened has proved that the synthetic SHEUR has good thixotropy.

    • Study on Preparation and Performance of Waterborne Polyurethane Modified by APTMS-GO

      2017, 34(1).

      Abstract (1192) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:3-aminopropyltrimethoxysilane, as a kind of modifier, was grafted on the surface of graphene nanosheets. The morphology of this kind of APTMS-GO and its properties were investigated by FT-IR, TG, XRD, Raman, AFM and TEM, respectively. APTMS-GO was well dispersed into dispersing agent and then added to the prepolymer to get a series of hybrid emulsion by in-situ polymerization, with the addition of APTMS-GO from 0.00 to 0.55wt.%. The properties, including mechanical property, thermal properties and hydrophobicity, of the APTMS-GO/WPU films, were tested. The cross-sectional morphology and emulsion particle of nanocomposites were also observed by FESEM and TEM, respectively. The results indicated that tensile properties of this hybrid film incorporated by the APTMS-GO via in-situ polymerization were significantly improved, with the tensile strength increasing from 10.13MPa to 28.96MPa. Thermal properties showed that adding 0.22wt.% APTMS-GO into the polymer matrix could enhance the initial thermal degradation(5% weight loss) temperature from 245 to 279oC. Hydrophobicity tests indicated that water contact angle (WCA) of the composite increased from 71.3° to 91.28° with increase in APTMS-GO content of the hybrid emulsion.

    • >Surfactants
    • Preparation and Surface Properties of ImidazoliumGemini Surfactants

      2017, 34(1).

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      Abstract:Five imidazolium Gemini surfactants were synthesized by four chemistry reactions using imidazole and bromide alkyl as the main starting materials. The NH group of the imidazole was protected. Their structures were identified by IR and 1H NMR and their properties were measured. The surface activity data of these surfactants (C10-2-C10, C12-2-C12, C14-2-C14, C14-4-C14 and C14-6-C14)are as follows: CMC : 2.7×10-4, 2.4×10-4, 2.0×10-4, 3.3×10-4 and 3.9×10-4 mol/L; γcmc: 30.60, 30.55, 30.51, 36.32 and 37.41 mN/m; the max values of contact angle on the quartz:70°, 73°, 75°, 72° and 68°; the max values of foam height: 87, 99, 125, 186 and 231 mm; t0.5 : 218, 608, 1157, 2329 and 2770 s. The surfactant C14-2-C14 shows the highest surface activity and the lowest wetting property for quartz. The properties of foams of C14-6-C14 are the most stable among the surfactants. When the hydrophobic chain increases, the surface activity, the efficiency of reduction in the surface tension of the water (pC20 ) and contact angle increase; but while their spacers increase, the physical and chemical parameters above decrease.

    • Preparation and Properties of Sulfonate Fluorosilicone Surfactant

      2017, 34(1).

      Abstract (1168) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Sulfonate fluorosilicone surfactant(FPESS)was synthesized with ring-opening polymerization,hydrosilylation and sulfonate reaction using octamethylcyclotetrasiloxane(D4),1,3,5-trimethyl-1,3,5-tris(3,3,3 -trifluoropropyl)cyclotrisiloxane(D3F),1,1,3,3-tetramethyldisiloxane(D2H),allyl epoxy polyether and potassium hydrogen sulphite as the raw materials. The chemical structure of the FPESS is characterized by Infrared Spectroscopy and Nuclear Magnetic Resonance Spectroscopy,the FPESS sulfonate reaction conditions were optimized,and the surface tension,foam ability,emulsifying ability,acid-resisting,alkali-resisting and salt-resisting ,stability in hard water of FPESS were measured.The optimum sulfonate reaction condition of synthetise FPESS results showed that epoxy group and potassium hydrogen sulphite molar ratio was 1:1.2,reaction temperature was 60癈,reaction time was 6h .The results of performance test showed that the surface tension (γcmc) of FPESS solution was 21.01 m N/m at the critical micelle concentration (cmc) of 2.0 g/L,the foaming power of 0.1% (mass fraction) FPESS solution was 1.47 and foam stability after 5 min was 0.71,the 0.5% (mass fraction) of FPESS had good emulsifying power to kerosene,epetroleum ether,isoamyl alcohol,the FPESS solution had excellent chemical stability of acid-resisting,alkali-resisting and salt-resisting,the stability of FPESS in hard water was grade 4.

    • >Catalysis,separation and purification technology
    • Plasma Preparation of Rare-earthOxide Doped Ni/Mg/Al Catalyst for Dry Reforming of Methane

      2017, 34(1).

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      Abstract:The Ni/Mg/Al catalyst doped with rareearthmetals were prepared by cold plasma decomposition and reduction of hydrotalcite-like compound, and the effects of La and Ce on pyhsico-chemical properties and catalytic performance of dry reforming were studied. The catalysts were characterized by X-ray diffraction (XRD), BET surface area and porosity analysis (BET), X-ray photoelectron spectroscopy and thermogravimetry (TG). The results suggested that hydrotalcite-like precursors were completely decomposed to mesoporous Mg(Ni,Al)O solidsolution which partly reduced to Ni0 by cold plasma jet. The conversion of CO2 and CH4 were 76% and 61.8% at 700 ℃ with V(CH4)/V(CO2)=4/6,GHSV of 30000mL/(h·gcat). The promoter of Ce improved catalyst lattice oxygen concentration and promoted the elimination of carbon species on the catalyst surface,, and the conversion of methane and carbon dioxide were increased by 5% and 7%, respectively. While the promoter of La inhibited the agglomeration of Ni0 and improved the dispersion of Ni0, and the non-active carbon deposition decreased by 70%, showing better anti-coke property.

    • Syntheses of the graphite phase carbonic nitrogen(g-C3N4) for photocatalytically reducing CO2

      2017, 34(1).

      Abstract (5382) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Abstract: The graphite phase carbon nitride (g-C3N4) semiconductors with different morphologies and photocatalytic performance were prepared by polycondensation method, using urea and melamine as precursors respectively. The catalytic performance of the g-C3N4 was measured by the reduction of CO2 in methanol under light irradiation. X-ray diffraction (XRD)、Scanning electron microscope (SEM)、Transmission electron microscope (TEM)、UV-vis spectrophotometry (UV-vis)、Fourier transform infrared spectroscopy (FTIR)、Specific surface area measurements (BET) and Fluorescence spectrum (PL) were applied to analyze the influence of different precursors to the photocatalytic activity of g-C3N4. Results showed that g-C3N4 using urea as precursor had better photocatalytic activity for CO2 reduction and the formation rate of methyl formate (MF) in methanol reached up to 512.8μmol/gcat.h, nevertheless that of the g-C3N4 made from melamine was only 257.3 μmol/gcat.h.

    • Recovery of Lincomycin by Three-phases Liquid Membrane

      2017, 34(1).

      Abstract (990) HTML (0) PDF 0.00 Byte (1) Comment (0) Favorites

      Abstract:Abstracts: This paper built a three-phases system composing of the feed phase, the membrane phase and the stripping phase using supported liquid membrane technique, which made the separation of lincomycin from aqueous solutions come true. The system of lincomycin+isoparaffin(Isopar L) in kerosene+HCl was used. The effects of initial lincomycin concentration (Cb f) in the feed phase, the pH of the feed phase, the pH of the stripping phase and the extraction solvent volume fraction (VF) on the distribution coefficient (D) were studied. Besides, we optimized the operating conditions of membrane module to realize the extraction. We also established a mathematical model to analysis the mass transfer process and the resistance of the process. The results show that the maximum distribution coefficient D=2.34 can be obtained with 11.9 mmol/L of lincomycin, 80% Isopar L(volume fraction) in the extractant, pH=10.1 in the feed phase and pH=1.2 in the stripping phase. The optimum operating conditions of membrane module is 520:500 (mL/min) of tube side flow rate Vf and shell side flow rate Vs. Mass transfer resistances were analyzed, the tube-side resistance is 6.7×105s/m, the shell-side resistance is 3.7×105s/m and the membrane-phase resistance is 2.7×106s/m,showing the resistance from the extraction reaction to be dominant.

    • Hydrogenation of Turpentine Catalyzed by NiCoB/TiO2 Amorphous AlloyHydrogenation of Turpentine Catalyzed by NiCoB/TiO2 Amorphous Alloy

      2017, 34(1).

      Abstract (950) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:NiCoB/TiO2 amorphous alloy catalysts were prepared by the means of the metal inducing electroless plating and these catalysts were characterized by XRD, SEM , EDS, ICP and XPS. The results showed that NiCoB was preferably supported on TiO2 in the form of amorphous alloy, which was good dispersibility with an average diameter of 120 nm or so. Their catalytic properties were evaluated for the hydrogenation of turpentine to cis-pinaneand the factors of affecting the reaction were optimized. The conversion of α-pinene was up to 99.23%, the selectivity of cis-pinane was 95.53% and the yield of cis-pinane was 94.80% at 145 °C for 200 min, 4.5 MPa hydrogen pressure and a catalyst of 10%.

    • >Drug and cosmetic materials
    • Synthesis and Performance of Light-Controlled Release Indometacin Loaded ZnO Particles

      2017, 34(1).

      Abstract (1126) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:ZnO particles of which size was around 180 nm were synthesized by direct precipitation. Indometacin was adsorbed to those particles. The optimal adsorption rate reached up to 74.00±1.11% when the mass ratio was 1:1. The drug release behavior was controlled by the UV radiation, since indometacin largely released under UV radiation while hardly released without UV radiation. The cellular viability of HaCaT was above 78.64±1.24% in the experimental concentration range, showing the good biocompatibility of indometacin loaded ZnO particles.

    • Synthesis of Glucose Derivatives via Improved Williamson Etherification Method

      2017, 34(1).

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      Abstract:An improved Williamson etherification method was reported. Using glucose derivatives, alkali metal hydroxide and benzyl chloride as raw material,n-octane as water-carrying agent, three benzylated glucose derivatives were synthesized. Kinds of water-carrying agent , alkali metal hydroxide, benzylation reagent and the different mole ratio of raw material were selected to investigate the influence on yield. The optimum synthesis conditions were as follows.Hydroxy of substrate, KOH or NaOH and benzyl chloride in mole ratio 1.00﹕1.10~1.15﹕1.10~1.15, using n-octane as water-carrying agent, refluxed at 125~130℃ for 4.0h, gave the three benzylated glucose derivatives in 96.8%~98.2% yields.The structures of compounds obtained were confirmed by FTIR,UPLC-MASS,1HNMR.

    • >Rubber and plastics auxiliaries
    • Preparation of Calcium/zinc mon-2-ethylhexyl maleate and Its Application in PVC Products

      2017, 34(1).

      Abstract (1247) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:2-Ethyl hexanol and maleic anhydride were used to synthesis the mon-2-ethylhexyl maleate, then the mon-2-ethylhexyl maleate were reacted with calcium acetate (zinc acetate) to prepare the calcium(zinc) mon-2-ethylhexyl maleate. The mon-2-ethylhexyl maleate and the final productions verified by FTIR. The thermal stabilities of PVC in the presence of the calcium/zinc mon-2-ethylhexyl maleate were evaluated systematically by means of thermal aging oven test,Congo red test and conductivity test and thermogravimetric analysis(TGA), the mechanism of calcium/zinc mon-2-ethylhexyl maleate thermal stabilizer was investigated by testing the absorption of acid.And then the synergistic effects of layered double hydroxide(LDH) with Ca/Zn system were explored. When the mass fraction of metal ions of the calcium / zinc mon-2-ethylhexyl maleate compound heat stabilizer were 3% and 2%,respectively, the system exhibited the best thermal stability, which provided the initial whiteness time of 50 min and the static thermal stabilization time of 26 min. At the same time when added 0.08g hydrotalcite (LDH), the system’s thermal stability had improved significantly, whoes the static thermal stabilization time reached at 53.5min.

    • >Oil field chemicals and petroleum additives
    • Synthesis and Properties of Acrylamide-Based Copolymer Containing Pyridine Unit as EOR Chemical

      2017, 34(1).

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      Abstract:A hydrophobic association polymer containing pyridine ionic liquid was synthesized by oxidation-reduction initiator system using acrylamide, acrylic acid, N-allyl oleamide and 3-allylaminocarbonyl-1-ethylpyridine bromide. The copolymer was characterized by IR and 1H NMR, and the thickening property, shear thinning, temperature resistance, salt tolerance and flooding capability of it were studied. The results showed that the apparent viscosity of 2000 mg/L copolymer solution could reach 510.3 mPa穝, and it could remain 27.2 mPa穝 under 510 s-1 and 42.8 mPa穝 at 90 oC. When the copolymer was dissolved in 10000 mg/L NaCl、1500 mg/L MgCl2 and CaCl2 solutions, the apparent viscosity of them were 21.8,27.4 and 27.0 mPa穝, respectively. The stimulating displacement experiment indicated that the recovery ratio of copolymer solution was enhanced 11.4%.

    • Study on Corrosion Inhibition of A3 Steel by A Lauryl Imidazoline Sulfuric Ester

      2017, 34(1).

      Abstract (953) HTML (0) PDF 0.00 Byte (1) Comment (0) Favorites

      Abstract:An imidazoline corrosion inhibitor, 1-hydroxyethyl-2-lauryl imidazoline sulfuric ester (LIMS) was synthesized by quaternary ammonium reaction with lauric acid and N-hydroxyethyl-ethylenediamine as raw materials and amino sulfonic acid as the quaternarization reagent. Its corrosion inhibition performance and adsorption behavior to A3 steel in 10% hydrochloric acid solution were investigated by means of weight loss, polarization curve, electrochemical impedance spectroscopy (EIS) and environmental scanning electron microscope (ESEM). The results revealed that corrosion inhibition efficiency of up to 93.1% when LIMS at the mass concentration of 0.80g/L. After adding the corrosion inhibitor, anode/ cathode action coefficient fa and fc were lower than 1, both values were similar, LIMS could inhibit cathode and anode reaction simultaneously, was a mixed type inhibitor. The research also indicated that the adsorption of the inhibitor on A3 steel was in agreement with Langmuir adsorption isotherm and the inhibitor molecule was adsorbed into A3 steel surface spontaneously. In addition, chemisorption was the predominant mode of adsorption. The inhibition efficiency of LIMS was up to 90.6%, superior to that of urotropine(78.5%), benzotrizaole(82.9%), PS-1(84.2%)and IS2129(87.3%)under the same condition.

    • >Acrylic series chemicals
    • Preparation and Performance of P(AM-co-AA) for Capturing and Encapsulating Radioactive Aerosols

      2017, 34(1).

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      Abstract:For radioactive aerosols contaminated nuclear activities that might arise, a kind of water-soluble resin was synthesized based on acrylamide(AM) and acrylic acid(AA) via free radical copolymerization in aqueous solution for remove radioactive aerosols. The resin were characterized by FT-IR, 13CNMR and thermogravimetric(TG). The results shows that AM and AA reaction generated random copolymer P(AM-co-AA); The structure of different monomer ratio were also characterized by SEM , it demonstrates that the microstructure of copolymer with porous crosslinked networks in water phase related to the monomer ratio; Through surface tension analysis, it also shows that the monomer ratio affects the wettability of aerosols. The spray atomization experiment shows that the pressure can accelerate settlement of aerosol, has obvious effect of supressing.