2017, 34(9).
Abstract:Quaternized chitosan coated humic acid (QCTS/HA) microcapsules as a new kind of water retention materials were prepared using quaternized chitosan (QCTS) as wall materials and humic acid (HA) as the cores. The performances of the microcapsules were characterized by Fourier transform infrared (FTIR) spectroscopy, polarizing microscope (POM) and scanning electron microscope (SEM),respectively. This paper explores the optimum conditions of QCTS/HA microcapsules by three factors: the core-wall ratio [m(HA): m (QCTS)], curing agent content and stirring rate. Micro-structures of microcapsule products prepared under optimal conditions were observed, and the water-absorption and water-retention properties of the product was tested. The results showed that QCTS/HA microcapsule had the best performance when the ration of m(HA) to m(QCTS) was 3:1, combined by 1% curing agent of the total mass for QCTS/HA microcapsule and a stirring rate of 500 r/min. Compared with CTS / HA microcapsules under the same conditions, the pore structure on the surface of QCTS / HA microcapsules is relatively perfect and well-distributed, and the quantity of pores are quite great . In addition, the microcapsule has better water absorption and water retention performance with water absorption rate and water retention rate as high as 348% and 208% in 12 h, respectively.
2017, 34(9).
Abstract:Novel Gum Arabic (GA)graft 2-acrylamido-2-methylpropanesulfonicacid (AMPS) and acrylamido (AM) biomass resin adsorption (GA-g-PAM/AMPS) was synthesized by grafting polymerization. The structure of superabsorbent resin were characterized by FTIR, XRD and SEM, respectively. The effects of various solutions on swelling properties were evaluated. The results showed that GA, AM and AMPS happened the grafting copolymerization reaction. The resin containing10wt% GA showed the highest water absorbency of 835g/g and 96g/g in the deionized water and in normal saline, respectively. Swelling behaviors revealed that introduction of GA simultaneously into the polymeric network could improve the water absorption capacity and pH stability of superabsorbent resin.The resin showed remarkable sensitivity and reversible characteristics in pH solutions. The water absorbency of the superabsorbent decreases with increasing metal ions and concentration of various external saline solutions,surfactant solutions showed greater influence on the swelling behaviors. Superabsorbent polymer had a good performance of water retention capacity.
HUANG Xiao-yu , MA Huan-mei , WANG Tian-yang , ZHOU Xue-qin , TIAN Jian-hua
2017, 34(9).
Abstract:Abstract:In this paper, CoS and CuS were potentiostatic deposited sequentially on the surface of FTO conductive glass substrate to fabricate the FTO/CoS/CuS composite counter electrode for quantum dot sensitized solar cells. FTO/CoS/CuS composite counter electrode was prepared at a suitable voltage and electrodeposition time, and the effects of electrolytic temperature on the morphology and electrocatalytic activity of prepared counter electrode were studied. The morphology and microstructure of counter electrode were determined by SEM and TEM. UV-VIS was used to investigate the optical reflection property of counter electrode. The electrochemical impedance spectroscopy, Tafel-polarization measurments and J-V curves were used to characterize the electrochemical performance. The result indicates that FTO/CoS/CuS composite counter electrode provides higher reflectivity, superior electrocatalytic activity and lower charge-transfer resisitance at the interface of counter electrode/electrolyte. Compared with that of Au, FTO/CoS and FTO/CuS counter electrode, the photovoltaic conversion efficiency of FTO/CoS/CuS composite counter electrode is increased by 132.9%, 46.6% and 26.9%, respectively.
MA Delong , ZHANG Zhe , LEI Ziqiang
2017, 34(9).
Abstract:The cyclotriphosphazene-based epoxy resin named as PNEP was successfully synthesized from hexachlorocyclotriphosphazene, p-hydroxybenzaldehyde and epichlorohydrin. It chemical structure was characterized by NMR spectroscopy and Fourier transform infrared (FTIR) spectroscopy. The prepared resin materials DDM-PNEP and DDS-PNEP were cured with diamino diphenyl methane (DDM) and diamino dipheny sulfone (DDS), respectively. The flame retardant properties, thermal stability and mechanical behavior cured PNEP are investigated and the scanning electron microscopy (SEM) is used to observe the residual carbon. The PNEP cured by DDM shows better result and the LOI of DDM-PNEP is 27.1 %. The thermogravimetric Analysis (TGA) demonstrated that the initial decomposition temperature was lower than E-44 epoxy resin. The initial decomposition temperatures of DDM-PNEP and DDS-PNEP were 152 ℃ and 159 ℃ respectively. The cured PNEP had two decomposition stages, DDM-PNEP are 152 ℃~320 ℃ and 370 ℃~505 ℃, DDS-PNEP are 159 ℃~355 ℃ and 358 ℃~552 ℃. The PNEP cured with DDM had a better carbonization result, which the carbon residue rate was 54.71 % at 600℃. Morphology of the solid residues by SEM exhibit that the carbon residue was dense and uniform, this phenomenon is very helpful in the flame retardancy of the epoxy resin.
WANG Haihua , LUO lu , LI Xiaorui , ZHANG Jingwen , WANG Ruifang
2017, 34(9).
Abstract:Firstly, it has gotten aminization of KH550 modified Fe3O4 nanoparticles, then using it as stabilizer, using toluene as soft template, made Pickering emulsion with aniline . Finally, the electromagnetic composites of PANI/Fe3O4 were prepared by interfacial polymerization method with presence of ammonium sulfate (APS) (as oxidant), hydrochloric acid (HCl) (as dopant). The structural properities of Fe3O4 nanoparticles and composites were characterized by FTIR, SEM, XRD, effects of different concentration of dopant HCl on the composites were inspected by vibration sample magnetism(VSM). The results show that the concentration of hydrochloric acid is 0.1 mol/L, the magnetic saturation intensity of composites reached 24841 A/m. Electromagnetic shielding performance and absorbing properties of composites were analyzed by vector network analyzer (VNA). The results show that the shielding effectiveness of composites were 40.682 dB at frequency of the electromagnetic wave was 10160 Hz, reflection loss reached -47.043 dB at 12400Hz, when HCl concentration is 0.1 mol/L, thickness 1 mm.
HUANG Ling-ling , HUANG Zi-yang , SHEN Qiu-fang , LIANG Lu , HUANG Bao-hua
2017, 34(9):0-0.
Abstract:HA/CS/SiO2/Fe2O3 composite coating was prepared by electrophoretic deposition, and then HA/SiO2/Fe2O3 composite coating was obtained by sintering at 700 癈 for 2 h. The HA/SiO2/Fe2O3 composite coating was tested and characterized by FT-IR, SEM, EDS, XRD, Lloyd LR5K Plus Testing Instrument and Electrochemical Workstation, respectively. The antibacterial performance of HA/SiO2/Fe2O3 composite coating toward Bacillus Subtilis was investigated. The bioactivity of the HA/SiO2/Fe2O3 composite coating was evaluated by immersion in 2-[4-(2-hydroxyethyl)-1-piperazinyl] ethanesulfonic-acid (HEPES) simulated body fluid (H-SBF). The results showed that the bonding strength between HA/SiO2/Fe2O3 composite coating and titanium substrate had reached 31.9 MPa, the surface of the composite coating had been completely carbonated hydroxyapatite after immersion in H-SBF for 14 days. The antibacterial test showed that the bacteriostasis rate of composite coating powder toward Bacillus Subtilis had been 81.9%. It is suitable for human beings bone implant material that the HA/SiO2/Fe2O3 composite coating possesses strong bonding strength and high biological activity and well antibacterial activity.
2017, 34(9).
Abstract:A series of boron-doped TiO2/SO42- photocatalysts were successfully prepared by the solid-state thermolysis method. Several technologies including X-ray powder diffraction ( XRD), Fourier transform infrared spectroscopy (FT-IR), UV-vis diffuse reflectance spectra (UV-vis DRS) and X-ray photoelectron spectroscopy ( XPS) were employed to investigate the phase structures,diffuse reflectance spectroscope (DRS) and surface chemical states. The photocatalytic properties of B-doped TiO2 were evaluated by degrading methylene blue (MB) under UV irradiation and visible-light irradiation. Results showed that B species have been doped into the crystal lattice of TiO2 with B doped in the form of substitutional and interstitial B, and can affect the surface chemical forms and structures of surface hydroxyl groups and SO42- groups. The experimental results of UV-vis DRS further indicate that the as-prepared photocatalysts with different B contents exhibited the stronger absorption in the visible light region and UV region. Compared to P25, B-doped TiO2 samples showed better activities for degradation of methylene blue (MB) under UV irradiation and visible light irradiation, and exhibited the highest photocatalytic activity when the molar doping ratio of B was 0.25. The superior performance of this sample is ascribed to the synergy and interplay among the decrease of the optical energy gap, efficient charge separation and surface hydroxyl groups.
ZHANG Xin-chi , YU De-wei , CHEN Xiao-rong , MEI Hua
2017, 34(9).
Abstract:A series Cu/CeO2 catalysts were prepared by co-precipitation method. The structure and reduction properties of the catalysts were characterized by physical adsorption(BET), X-ray diffraction(XRD) and H2 temperature programmed reduction(H2-TPR). The catalytic performance of Cu/CeO2 catalysts was investigated for diethanolamine dehydrogenation to iminodiacetic acid. The results showed that Cu3Ce1 catalyst calcined at 500oC with Cu:Ce mole ratio of 3:1 had low reduction temperature, appropriate Cu0 active centers and high catalytic performance for diethanolamine dehydrogenation of iminodiacetic acid. Under the reaction condition of m(DEA):m(NaOH):m(H2O)=1.15:1:2.42, 6g CuO/CeO2 used,reaction temperature of 180oC, reaction pressure of 1.1MPa, reaction time of 4h and rotational speed of 600r/min, the conversion of diethanolamine reached 99.63% and the selectivity of iminodiacetic acid was 95.73%.
SHNA Yuan-yuan , LAI Miao , ZHAO Ming-qin , JI Xiao-ming
2017, 34(9):0-0.
Abstract:3,6-Dimethyl-2,5-pyrazinediformyl chloride was synthesized by oxidation and acylating chlorination from 2,3,5,6-tetramethylpyrazine. The aroma precursor compound of di (1-octen-3-yl)-3,6-dimethyl-2,5-pyrazinedicarboxylate was synthesized by esterification with 1-octen-3-ol and 3,6-dimethyl-2,5-pyrazinediformyl chloride. The structure of di (1-octen-3-yl)-3,6-dimethyl-2,5-pyrazinedicarboxylate was confirmed by 1HNMR, 13CNMR, IR and HRMS spectra. The thermal property of DMPOE was measured by the thermogravimetric (TG-DTG-DSC) analysis and pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) analysis. The results showed that: The synthetic product was the target compound; The TG curve showed that the largest mass loss occurred from 220 to 360 ℃, with weight loss of 85.2%. The target compound degraded began from 225.9 ℃, and the weightlessness rate reached the maximum at 312 ℃ with 65.48% of weightlessness. Nine kinds of typical products were identified by pyrolysis analysis, and main pyrolysis products were 2,5-dimethyl pyrazine, 1-octen-3-ol and 2-isobutyl-3-methylpyrazine which were aroma components. With adding of 0.75 mg/kg to typical middle flavor style flue-cured tobacco, it could improve the smoking quality, increase the aroma quantity, reduce offensive odor and irritation and modify the smoke.
2017, 34(9).
Abstract:Paeonol hydrazine was generated by the reaction of paeonol(2-hydroxy-4-methoxyphenylethanone) as raw material with hydrazine hydrate. Night novel N-benzylidene paeonol hydrazones were synthesized in the yields of 50.5%~91.9% by the reaction of paeonol hydrazine with various benzaldehydes respectively. The synthetic conditions were investigated preliminarily. The structures of the products were confirmed by FT-IR, 1H NMR, 13C NMR and LC-MS. The preliminary bioassay showed that some of the title compounds exhibited excellent antibacterial activity, in which the MIC of compound N-(4-fluorobenzylidene) paeonol hydrazones (3c) against S.aureus was 4μg/mL and compound N-(2-fluorobenzylidene) paeonol hydrazones (3b) similar effect against E.coli. than the standard reference drug (rifampin).
ZOU Jia-jia , TIAN Zhi-jin , HUA Yu , LIANG Jiao , WAN Su-cen , LIN Cui-wu
2017, 34(9):0-0.
Abstract:Three L-tryptophan derivatives (S)-2-{4’’-[(1’’’,3’’’-dioxoisoindolin-2-yl)methyl]benzamido}-3-(1’ H-indol-3’-yl)propanoic acid (I), (S)-2-{4’’-[(1’’’,3’’’-dioxoisoindolin-2-yl)methyl]cyclohexanecarboxamido}-3-(1’ H-indol-3’-yl)propanoic acid (II) and (S)-2-[6’’-(1’’’,3’’’-dioxoisoindolin-2-yl)hexanamido]-3-(1’ H-indol-3’-yl)propanoic acid (III) were synthesized through amidation reaction with three hemostatic amine acids protected by phthalic anhydride, including, 4-(aminomethyl)benzoic acid, 4-(aminomethyl)cyclohexane-1-carboxylic acid and 6-aminohexanoic acid. The structures were confirmed by IR, MS and 1H NMR and 13C NMR. Two coagulating target proteins were reversely screened, and positively docked with L-tryptophan and three compounds through MOE, respectively. Blood concretion four items and plasma re-calcification time indicated that compounds I and III showed better coagulating activity with increasing concentration, while compound II showed dose-dependent activity.
MA Shao-yu , CHAI Chun-peng , LUO Yun-jun
2017, 34(9).
Abstract:Abstract: Organic silicon modified waterborne polyurethane extinction resin were prepared by poly(tetramethylene ether) glycol (PTMG), polydimethylsiloxane (PDMS), isophorone diisocyanate (IPDI), and dihydromethyl propionic acid (DMPA) as monomer, triethylamine (TEA) as neutralizer, and ethylenediamine (EN) as chain extender. FT-IR, LPSA, SEM, EDS, and 60° photometer were carried out to investigate the structure and properties of WPU. The effects of R (the molar ratio of —NCO and ¬¬—OH in the reaction raw materials) and PDMS content(characterized by the ratio of moles of PTMG to PDMS) to the gloss of WPU were discussed while the properties of WPU were explored. The results show that when R=2.3, n (PTMG/PDMS) =1:2, the particle size of WPU emulsion is 300.8 nm, and the stability is good. SEM shows that the surface of the WPU film is formed with compact micron grade spherical bulge, and its glossiness gloss reaches a minimum of 10.9, the water absorption is 23%, so its comprehensive performance is excellent.
2017, 34(9).
Abstract:A new kind of composites of polysilicate aluminium magnesium-caboxy methyl cellulose (PSiAM-CMC) was made with Na2SiO3?9H2O, Al2(SO4)3?18H2O, MgSO4?7H2O and CMC. Jar tests were texted that when the n(Al Mg)/n(Si)=0.6, n(Mg)/n(Al)=1:4, m(CMC)/m(Si)=0.3, gelatinization temperature of CMC 60℃ and pH=2, the PSiAM-CMC flocculant has excellent flocculation performance. The micro-morphology and structure of PSiAM-CMC were studied by scanning electronic microscope (SEM), fourier transform infrared spectrum (FTIR) and X-ray diffraction (XRD). The test results showed that psi, Al, Mg and CMC were composited successfully. The flocculant has got excellent purification effect for Songhua River water.
SUN Caiying , DONG Zilin , JIANG Dawei
2017, 34(9).
Abstract:Cotton fabrics require flame retardant finish as they are used extensively and easy to be ignited causing fire. In this paper, cotton was treated with Poly(oxy-1,2-ethanediyl)methylphosphonate(PEMP) as a flame retardant, its properties, such as breaking elongation, flame retardancy, thermal decomposition, fire behavior and water durable, were compared with pure cotton. It was found that loading 20% PEMP, the cotton’s breaking elongation went down from 23.6 % to 18.2 %, LOI rose from 20.4 % up to 30.6 %, after flame time and smoldering time both dropped to 0 s from 54.8 s and 61.2 s respectively, damaged length fell to 11.5 cm from 30 cm, the maximum thermal decomposition rate dropped to 12 %/min from 18 %/min, the residue under 700 ℃ enhanced from 9 % to 24 %, total heat release fell to 0.6 MJ/m2 from 4.2 MJ/m2, the LOI was still 27.9 %. All the results showed that PEMP is a good flame retardant and a charring agent for cotton and can reduce evidently heat release of cotton in fire that can suppress fire behavior and race against time for fire fighting and rescue under fire.
FAN Ya-qin , XIANG Yao , LEI Yong-lin , WANG Xiao-chuan , HUO Ji-chuan
2017, 34(9).
Abstract:The ploybutadiene elastomer was prepared under room temperature (25℃) from liquid polybutadiene rubber (LPB) which was adhesive, benzene-1,4-dicarbohy-droximoyl dichloride which was synthesized and trimethylamine via 1,3-dipolar cycloaddition,to seek the best curing ratio. The structure of benzene-1,4-dicarbohy-droximoyl dichloride was con?rmed by FTIR,1H NMR, MS and melting point. The structure of the polybutadiene elastomer was characterized by FTIRT. The mechanical property of the elastomer was determined by tensile strength, elongation at break and shore hardness. The surface property of the elastomer was con?rmed by contact angle and FSEM. The results indicates that the yield of benzene-1,4-dicarbohy-droximoyl dichloride is 94%. LPB was cured under room temperature after adding trimethylamine. When the mass ratio of the curing agent to LPB was 10%, the mechanical property of the elastomer was best. The tensile strength of the elastomer reaches 0.35MPa, with 53% elongation at break and 0.66KPa modulus. And the contact angle reaches 112.76皐hich shows excellent hydrophobic performance. Room temperature curing made up for the deficiency of traditional curing technology, greatly improving the heat resistance and mechanical properties of the elastomer.
2017, 34(9).
Abstract:Firstly, the microfiber synthetic leather was pretreated with formic燼cid, and then the epoxy resin(1, 4 - butanediol two water loss glycerol ether )was as crosslinking agent, collagen was as modifier to improve the water vapor permeability of microfiber synthetic leather base. The results show that the optimum modification condition are that the collagen dosage is 14%(basing on the weight of dry base), the dosage of epoxy resin is 12%, the treat reaction time by epoxy resin is 3h,and the best treat time by collagen is 2h,the reaction temperature is 40℃.The water vapor permeability, and Hydroscopicity of microfiber synthetic leather base increase by 43.0%and 25.56%, respectively. The Fourier Infrared spectrum analysis (FT-IR) results indicate that the collagen is successfully grafted on the surface of the base throught epoxy resin. The comparison between unmodified and modified bases was carried out with Scanning Electron Microscope (SEM),The results show that the fiber is more loose after being modified. Compare the bases before and after being modified with Atomic Force Microscope (AFM), the results show that the surface of the modified base is smoother and flatter. Moreover, Contact angle analysis also shows that the contact angle of modified base decreases significantly compared with the unmodified bases.
HAN Wei , LI Wei , KANG Jie-qiong , LIU Dong-zhi , ZHOU Xue-qin , YANG Yi-jun , WANG Tian-yang
2017, 34(9).
Abstract:A pharmaceutical intermediate 6-phenyl-[1,2,4]-triazole[4,3-a]pyridine-3-Amine was synthetized from 5-bromo-2-fluoropyridine by substitution, ring-formation and coupling reactions. The product was characterized by 1H-NMR, 13C-NMR and HRMS. The reaction process was optimized by tuning the reaction time, reaction temperature, reactant ratio, solvent ratio and catalyst dosage to study the effect of these factors on the reaction yield. The results showed that the optimum conditions for the synthesis of 6-bromo-[1,2,4]-triazole[4,3-a]pyridine-3-Amine were as follows: temperature was 40℃ , time was 15 min. The optimum conditions for the synthesis of 6-phenyl-[1,2,4]-triazole[4,3-a]pyridine-3-Amine were as follows: the solvent was V(water): V(dioxane)=1.0:2.0, the amount of the reactant was n(6-bromo- [1,2,4] triazolo [4,3-a] pyridin-3-amine): n(phenylboronic acid) =1.0:1.2, the amount of the catalyst was n(6-bromo- [1,2,4] triazolo [4,3-a] pyridin-3-amine): n(Pd (pph3) 2Cl2)=1.0:0.1, temperature was 80 ℃. The final yield of the three steps of reactions was 60%
2017, 34(9).
Abstract:Allyl phosphonic acid diethyl ester, prepared by Michaelis-Arbuzov reaction, reacted as the main reaction substrate with oxalyl chloride, 3-buten-1-ol and asymmetric chain terminated diene molecule containing phosphoru BEAPH was repared.The monomer can be transformed to the polymer having phosphoru in the main chain by non-cyclic diene metathesis polymerization, or be used for preparing heterocyclic alkene molecules containing phosphoru with closed loop metathesis polymerization. Successful preparing and purification of unsaturated monomers was confirmed using H NMR Spectrum. The condensation between molecules was proved by GPC curve and molecular weight, PDI datas,which have very important guiding significance to a conversion of allyl phosphorus-containing monomers and polymers preparation that contains phosphorus.