YANG Xiao-lan , 钟国清 , LIANG Kai
2013, 30(12).
Abstract:A novel bis-Schiff base of 5,5′-methylene-bis(salicylaldehyde)-5-methyl-2-[(2-aminophenyl) amino]thiophene-3-carbonitrile was synthesized with 5,5′-methylene-bis(salicylaldehyde) and 5-methyl-2-[(2-aminophenyl)amino]thiophene-3-carbonitrile as raw materials, and the 5,5′-methylene-bis(salicylaldehyde) was derived from salicylaldehyde and trioxane. The results of elemental analysis and mass spectrometry confirmed that the molecular formula of Schiff base was C39H30N6O2S2. The structure of the Schiff base was characterized by FT-IR and 1HNMR. The antibacterial activities of the Schiff base were screened by the Oxford cup agar diffusion method. The experimental results showed that the Schiff base had certain antibacterial activities against four bacteria and the diameter of the inhibition zone was 15.0 mm against Escherichia coli with the concentration of 1.5 mg•mL-1. The antibacterial activities of the sequence were Escherichia coli, Bacillus subtilis, Staphylococcus aureus and Staphylococcus epidermidis, respectively.
WANG Xue-chuan , BU Qiao-qiao , QIANG Tao-tao
2013, 30(12).
Abstract:The characteristics of adsorption of Cr3+ on the collagen fiber(CF) were studied with chromium solution as target; The effects of temperature, time, pH, adsorbent dosage, initial concentration and salt ion concentration (Na+, Ca2+) on the adsorption process were reseached through the single factor experiments, respectively. The results indicated that the collagen fibers have strong adsorption abilities to Cr3+ and the adsorption capacity can be up to 90mg/g, the optimal pH and temperature of adsorption were 4.5 and 40℃, respectively; For a certain amount of chromium solution, the adsorption capacity was increased with the increasing of initial concentration of Cr3+, but decreased along with the increasing of adsorbent dosage. With the extension of time, the adsorption capacity increased gradually and finally reached adsorption equilibrium. The salt ions in the solution will have inhibitory effect on the adsorption process, and the inhibition enhanced with the increasing of ion concentration. The adsorption thermodynamics and adsorption dynamics were studied, by comparison, it was found that the Freundlich equation and Pseudosecond-order kinetic model can better describe adsorption behavior of Cr3+ on the collagen fiber.
YE Li-ping , LI Shuai , LUO Yong
2013, 30(12).
Abstract:The removal performances of trace amount of carbon monoxide in liquid propylene at low temperature was studied on the CuO-ZnO-ZrO2 catalyst prepared by an optimized co-precipitation method. The catalyst was characterized by means of XRD, BET and SEM. It is found that ZrO2 existed in amorphous form, which could increase surface area and pore volume, and improve the dispersion of CuO and ZnO particles. The pre-treatment of catalyst was necessary for its application in the removal of CO, and the reduction temperature influenced the catalyst activity significantly. The experiments revealed that the catalyst activated at 160℃ with proper reduction degree of 77.3% exhibited the excellent removal performance of trace amount of carbon monoxide which could remove the CO in liquid propylene from 10 ppm to lower than 0.02 ppm with good stability of 1500 min under the conditions of 50 ℃ and 3.0 MPa. The introduced CO2 into the feed reduced the removal depth of CO on CuO-ZnO-ZrO2 catalyst, which indicated that CO2 had a certain degree of inhibitory effect in CO oxidation.
QIN Xiao-ping , YE Zhong-bin , LAI Nan-jun
2013, 30(12).
Abstract:A functional monomer (DAMA) was prepared with 1,3-Diaminopropane and maleic anhydride, and then a water-soluble AM-AA-NVP-DAMA tetra-copolymer was polymerized by free radical polymerization using DAMA, N-Vinyl-2-pyrrolidone (NVP), acrylamide (AM), and acrylic acid (AA) as raw materials. The synthesis conditions were as follows: m (AM): m (MA) was 3:2, initiator was 0.5 wt%, temperature was 40 oC, reaction time was 8 h, and pH was 7.0. The AM-AA-NVP-DAMA copolymer was characterized by infrared spectroscopy (IR), 1H NMR, and scanning electron microscope (SEM). It was found that the viscosity retention rate of AM-AA-NVP-DAMA was 16.2 % higher than that of partially hydrolyzed polyacrylamide (HPAM) at 95 oC, the viscosity retention rate of this copolymer in 1.8 wt% NaCl brine was 8.7 % higher than that of HPAM, the viscosity retention rate of this copolymer in 0.09 wt% CaCl2 brine was 9.4 % higher than that of HPAM, and the viscosity retention rate of this copolymer sheared at 500s-1 for 5 min was 16.3 % higher than that of HPAM. It was also found that the enhanced oil recovery (EOR) of 0.2 wt% copolymer solutions was 5.07 % higher than that of HPAM at 60 oC.
BAO Xiao-rong , JI Xiao-ming , ZHAO Ming-qin , Lai Miao
2013, 30(12).
Abstract:Abstract: Under the action of the thionyl chloride, different pyrazinamide derivatives were gotten from 2, 3 - pyrazinedicarboxylic acid and α-amino acids (glycine, valine, leucine) by fractional steps and one-step. Its structure was confirmed by 1H NMR, 13C NMR, IR and HR MS spectral analysis. The effect of different reaction conditions on the synthesis of pyrazinamide derivatives was discussed. The results showed that: In the presence of thionyl chloride, N-(2-carboxy-3-formyl-pyrazine)-α-amino acid methyl ester and N-(2, 3-acyl dimethyl pyrazine)-α-amino acid methyl esters were obtained by the sub-step or step, respectively.
SUN Kan , SHI Meng , WU Han-bing , ZHU Yan-ping , NIE Hua-li , QUAN Jing , ZHU Li-min
2013, 30(12).
Abstract:The glycomonomer 6-O-vinyladipoyl-D-glucopyranose (OVAG) was synthesized by lipase catalyzed transesterification of divinyladipate with D-glucopyranose. Poly(NIPAAm-co-OVAG) with narrow polydispersity (PDI) and thermosensitivity was prepared via Reversible Addition-Fragmentation Chain Transfer (RAFT) polymerization. The Poly(NIPAAm-co-OVAG) was characterized by 1H NMR, FTIR and gel permeation chromatography (GPC). Measurement by transmission electron microscopy (TEM) revealed that Poly(NIPAAm-co-OVAG) was able to self-assemble into nano micelle with well-defined structure and uniform size in aqueous solution. The characterization of UV-visible spectroscopy showed that the low critical solution temperature (LSCT) can be controlled by the molar ratio of monomers. When the molar ratio of NIPAAm and OVAG was 14:1, the LCST of Poly(NIPAAm-co-OVAG) was 36oC in aqueous solution, which can form nano micelle in the human body environment and has great potential in drug carrier.
2013, 30(12).
Abstract:guar gum-g-poly(acrylic acid)/loess(GG-g-PAA/LOESS) superabsorbent composites were prepared by graft polymerization in aqueous solution using guar gum (GG), acrylic acid (AA), loess as raw materials, ammonium persulfate (APS) as initiator and N,N-methylenebisacrylamide (MBA) as crosslinker. The structure of superabsorbent composites was characterized by FTIR and SEM. Effects of loess content on swelling capabilities and swelling kinetics of superabsorbent composites was studied. Water-retention properties at various temperatures, reswelling capabilities and water absorbency at various pH solutions of superabsorbent composites were also investigated. The results indicated that GG and LOESS participated in graft polymerization reaction with AA. The prepared GG-g-PAA/LOESS superabsorbent composites have the good properties of water absorbency, water absorption rate, water-retention and reswelling. In addition, the superabsorbent composites showed excellent pH-stability in various pH solutions.
2013, 30(12).
Abstract:H3PW12O40/ZrO2-WO3 was prepared by impregnation, and it was sensitized by H2O2 solution, its catalytic activity under simulated natural light was improved significantly. Degradation of methyl orange was used as a probe reaction to explore the influencing factors of the photodegradation reaction. The optimum conditions is that initial concentration of methyl orange is 5 mg/L, and the pH is 2.5, catalyst dosage is 0.3 g, the degradation ratio of methyl orange is as high as 91.16% after 2 h simulated natural light irradiation. The reaction of photocatalysis for methyl orange can be expressed as first-order kinetic model. The photodegradation of methyl orange, rhodamine B, basic fuchsin and methylene blue were also tested, and the degradation rate of dyes can reach 70%-91.16%.
Gao Wei , Pang Yu-xia , Lou Hong-ming , Qiu Xue-qing
2013, 30(12).
Abstract:The adsorption properties of 3 types of macroporous resins NKA-9, AB-8, H103 with different polarity for sodium lignosulphonate were evaluated. Macroporous resins NKA-9 with strong polarity displayed the best adsorption capacity among the tested resins. The static adsorption and desorption characteries of NKA-9 for sodium lignosulphonate were investigated. Results showed that decreasing of temperature and pH was favor of adsorption. With the mass concentration increasing the static adsorption capability of sodium lignosulphonate by NKA-9 resin increased. The adsorption reached equilibrium after 180 minutes. The desorption effect of methanol was the best. By analyzing sodium lignosulphonate washed out from the resin, it showed that the sodium lignosulphonate with higher content of phenolic hydroxyl group, lower content of carboxyl and sulfonic group is easier to be adsorbed.
XU Shou-wei , ZHENG Chang-zheng
2013, 30(12).
Abstract:Two complexes,Co(LPy)2(1) and Ni(LPy)2(2) were synthesized from the reaction of Benzylidene Acetone Salicylhydrazone (HL) with Co(NO3)2, Ni(NO3)2,and characterized by FTIR,thermal analysis,single crystal X-ray diffrac-tion and XRD.The results of structuralanalysis indicate that both complexes aredistorted octahedral.Complex 1 belongs to triclinic system,space group P-1 witha=1.0347(3)nm,b=1.0052(4)nm,c=1.4541(4)nm;α=92.830(4)?β=109.054(3)?γ= 96.091(4)?V=1.9792(10)nm3,Z=2,F(000) =814,R1=0.0506.Complex 2 belongs to triclinic system,space group P-1 with a=1.0435(5)nm,b=1.3940(7)nm,c=1.4542(7)nm;α=92.41(2)?β=109.73(2)?γ=95.80(2)?V=1.9745(17)nm3,Z=2,F(000) =816,R1=0.0438.The result of TG analysis shows that the title complexswere stable under 200 ℃.
ZHANG Chun-yan , JIA Chun-man , ZHANG Qi , CHEN Da , CAO Li
2013, 30(12).
Abstract:Abstract: The amphiphilic chitosan derivative N-succinyl-N'-decyl low degree of polymerization (DP) and narrow relative molecular weight distribution chitosan (SDLNCS20) was prepared from low DP and narrow molecular weight distribution chitosan (LNCS20, DP=20; Mw/Mn=1.20). Its structure was characterized by FTIR and 1HNMR. The solubility, emulsifying and wetting properties were also studied. Surface activity and critical micelle concentration (cmc) of SDLNCS20 were studied with the method of surface tension and fluorescence spectrum. The results showed the hydrophilic succinyl group and hydrophobic long alkyl chains were successfully introduced to the amine group of LNCS20. The cmc value of SDLNCS20 is 3.55×10-4 g•mL-1, and corresponding surface tension is 30.01 mN•m-1. Besides, SDLNCS20 was showed excellent water solubility and emulsifying property.
2013, 30(12).
Abstract:A polycarboxylate superplasticizer for ceramics of linear MA/AA/AMPS was prepared using aqueous solution polymerization with the major monomers including maleic anhydride (MA), acrylic acid (AA), 2-acrylamide-2-methyl propane sulfonic acid(AMPS). The effects of mole fraction of monomers, dosage of initiator and polymerization temperature on the flow time of ceramic body slurry with the polycarboxylate superplasticizer for ceramics of linear MA/AA/AMPS at a dosage rate of 0.35% (based on the absolute dry slurry) were investigated by orthogonal experiments. The structure of the functional group and crystal structure of the polycarboxylate superplasticizer for ceramics of linear MA/AA/AMPS were respectively characterized by means of FT-IR and XRD. The POM and SEM photographs were respectively employed to observe the dispersion of the ceramic body slurry and the cross-section of the shape of the ceramic body samples. The best polymerization conditions of the polycarboxylate superplasticizer for ceramics of linear MA/AA/AMPS are when the polymerization temperature is 90 ℃, the initiator ammonium persulfate accounts for 8% of the total mass of the polymerized monomers, n(MA)∶n(AA)∶n(AMPS) equals 1.0∶3.5∶1.5, and the reaction time is 4 h. The ceramic body slurry's viscosity decreases from 689.5 mPa穝 to 56.8 mPa穝 when the concentration of polycarboxylate superplasticizer for ceramics of linear MA/AA/AMPS is 0.35% (based on the absolute dry slurry).
2013, 30(12).
Abstract:MeSiOMeRSiMe3〔R=O(CH2)2N(CH3)2〕was synthesized in solvent-free with dimethylethanolamine (DMEA ) and Heptamethyltrisiloxane(MDHM)as raw materials. Reaction time, reaction temperature, reactant molar ratio,catalyst concentration on the reaction conversion rate influence was discussed. Through orthogonal experiment, the solvent-free synthesis technique of MeSiOMeRSiMe3〔R=O(CH2)2N(CH3)2〕 was optimized. The purification of the target product by reduced pressure distillation and the The purity of the purified product measure by gas phase chromatography. The structure of the product was characterized by mass spectrum and 1H NMR.
2013, 30(12).
Abstract:A carboxymethyl cellulose/poly(ethylene glycol)/acrylic acid (CMC/PEG/AA) superabsorbent composite was prepared in aqueous solution using glow-discharge electrolysis plasma (GDEP) induced graft copolymerization of carboxymethyl cellulose (CMC), poly(ethylene glycol) (PEG) and acrylic acid (AA), in which N,N'-methylenebisacrylamide (MBA) was used as a crosslinker. The influences of temperature, various pH values and salts solutions on the equilibrium swelling ratio were studied in detail. The adsorption of methylene blue (MB) on the CMC/PEG/AA was preliminarily investigated. The results showed that the maximum equilibrium swelling ratio of CMC/PEG/AA in distilled water was 1115 g/g at 30 ℃. The CMC/PEG/AA superabsorbent composite was responsive to pH and salts, and it had excellent on-off switching behavior as reversible swelling and deswelling. In addition, the maximum adsorption capacity of CMC/PEG/AA for MB was 1878.8 mg/g. The adsorption kinetics fitted the pseudo-second-order model.
2013, 30(12).
Abstract:A novel thermo-sensitive poly (N-isopropylacrylamide) (PNIPAAm)/ silica nano-composite has been prepared via in situ one-pot method . Effects of factors, such as reaction temperature, reaction time, monomer dosage and initiator dosage on the influence of contact angles were investigated. The optimum surface modification conditions were determined as: reaction temperature was 73℃, reaction time was 6 h, monomers and KH-570 molar ratios is 1, The amount of initiator monomer is 2.5 (wt%)of the total mass amount of monomer and KH-570. The samples were characterized by fourier transform infrared transmission emission microscope (TEM) and dynamic light scatter (DLS). Moreover, the thermo-sensitive property of PNIPAAm was retained in the nano-composite, which had a lower critical solution temperature similar to that of pure PNIPAAm.
2013, 30(12).
Abstract:Three four-armed star-shaped poly(ɛ-caprolactone)-b-poly(gluconamidoethyl methacrylate)(4sPCL-b-PGAMA) copolymers with porphyrin core were synthesized via ring-opening polymerization and atom transfer radical polymerization.The structure of the result products was characterized by 1HNMR,GPC and UV-vis.DSC result shows that degree of crystallinity decreased from 73.9 to 0.9,with increasing the weight fraction of hydrophilic poly(gluconamidoethyl methacrylate)(PGAMA) within the copolymers from 0% to 79%,indicating that PGAMA can improve efficiently the crystallization of poly(-caprolactone)(PCL).The fluorescence quenching extent(△I) of tetrakis(4-hydroxylphenyl)-porphyrin(THPPH2),4sPCL24 and 4sPCL24-PGAMA37 with the equal number of potential porphyrin core was investigated by fluorescence probe method,exhibiting △ITHPPH2>△I4sPCL24>△I4sPCL24-PGAMA37,demonstrating that the polymeric skeleton can delay successfully the self-quenching of the porphyrin core.Morphology of 4sPCL-b-PGAMA self-assembled aggregates varied from spherical micelles at 70nm,to worm-like aggregates,finally to vesicles at 200nm, with decreasing the weight fraction of PGAMA from 79% to 21%.Moreover,the UV-vis absorbance increased greatly with adding concanavalin A(Con A) to the copolymer micelles solution,indicating the formation of the bigger cross-linked aggregates in aqueous.This demonstrates that 4sPCL-b-PGAMA has specific recognition with Con A
2013, 30(12).
Abstract:To investigate the effect of various surfactant in the microstructure, using four surfactants as templates, Al doped titanium dioxide (Al-TiO2) powder with various properties were prepared by the same condition. And the materials microstuctures were characterized and analyzed. The results showed that carbon atomicity of hydrophobic groups in surfactant is negative to the crystallite size of Al-TiO2 powder and positive to the distorting stress. Moreover, the more the mass fraction that Al3 entered into TiO2 crystal lattice induced by the surfactant, the more the distorting stress produced by crystal lattice. Visible light degradation property of pyridine on the Al-TiO2 powder surface is mostly determined by the molecule structure of surfactant and thus the oxygen vacancy concentration induced by surfactant rather than the band gap width. In the controlling range of anion surfactant on the materials structure, SDS is stronger than that cation surfactant, but the ampholytic surfactant is poor.
ZHU Hai-lin , HU Zhi-yong , WANG Jian-long , CAO Duan-lin
2013, 30(12).
Abstract:A serial of cation gemini surfactants with dibenzyl ether spacer (10-B-10,12-B-12,14-B-14) were synthesized from 1-bromoalkane, N,N-dimethylethanolamine and α,α'-dibromo-p-xylene. Their structures were identified by FT-IR, 1HNMR and ESI-MS. Aggregation number of micelle of these surfactants was determined by steady-state fluorescence method. The results showed that the CMC determined by steady-state fluorescence method was in agreement with that determined by surface tension method. The critical micelIe concentration (CMC) decreased from 3.24 to 0.056 mmol.L-1 with the alkyl chain length increasing from 10 to 14. The critical aggregation number was 6.98(10-B-10),3.87(12-B-12) and 1.62(14-B-14). The salt-induced vesicle to micelle transition was found in the aqueous solution of these surfactants by dynamic light scattering(DLS).
Wang Jia-xiang , Liu Xiang , Su Bi-yun , Xiao Ming-yang , Li Lei
2013, 30(12).
Abstract:Using 2-acetylpyrrole and a couple of aromatic amines, such as 3-chloroaniline and 4-chloroaniline as the raw materials, two chloroaniline based mono(imino)pyrroles 2-{1-[(3-chlorophenyl)l)imino]ethyl}pyrrole (1a) and 2-{1-[(4-chlorophenyl)l)imino]ethyl} pyrrole (1b) were prepared under the microwave irradiation. No indication showed the reaction occurred between 2-acetylpyrrole and 2-chloroaniline. These structures were characterized by X-ray single crystal diffraction, 1H NMR, IR, MS and elemental analysis. 1a belongs to monoclinic system, space group C2/C with a = 23.722 (15) Å, b = 5.720 (4) Å, c = 16.868 (11) Å, β = 98.404 (10)°, V = 2264 (3) Å3, Z = 8, Dc = 1.283 g·m-3, R1 = 0.0419, ωR2 = 0.1195. 1b also belongs to monoclinic system, space group P21/C with a = 13.323 (3) Å, b = 9.802 (2) Å, c = 9.107 (2) Å, β = 109.212 (4)°, V = 1123.1 (4) Å3, Z = 4, Dc =1.293 g·m-3, R1 = 0.0472, ωR2 = 0.1189. Reaction mechanism between the position of deactivation group on the aromatic amines and the Schiff base condensation was also discussed.
2013, 30(12).
Abstract:Skeleton isomerization of n-butene over ZSM-35 Zeolite with high Si/Al ratio on a fixed-bed reactor was investigated. The used catalyst was regenerated by high temperature oxidation method. Information about the effect of carbon deposition was obtained by TPO、BET、NH3-TPD and Py-IR measurements.. The results indicated that the catalyst exhibits good stability and regenerability, furthermore, the conversion of butene was 45% and the selectivity of iso-butene was 95%, when increasing TOS to 390h, the yield of iso-butene was still maintained above 32%. Deposited carbon was substantially formed during the initial period in micropore preferentially on strong acid sites and was mainly graphite carbon which was difficult to be removed.
ZHENG wen , ZENG Wen-bo , LI Jian-jun , PENG Xiao-hong , CAO Xi-min , ZHANG Ya-sheng , GUANG Zhong-xiang
2013, 30(12).
Abstract:With isophorone diisocyanate (IPDI) and polytetramethylene glycol (PTMG) as main materials, dihydroxy methyl propionic acid (DMPA) as hydrophilic chain extender, A95 and hydrazine hydrate as small molecule chain extender, a low gloss waterborne polyurethane(WPU) dispersion was prepared by prepolymer dispersing method. The structure and surface of the WPU film were investigated by FTIR,AFM and TEM. Results show that WPU film surface microstructure fit with the extinction mechanism of low gloss. When wBismuth acid catalyst=0.016%,w hydrazine hydrate = 45%, wDMPA = 2.6%, wA95 = 0.84%, the WPU film has a good low gloss performance.
2013, 30(12).
Abstract:Epoxidized fatty acid methyl esters was synthesized by epoxidation in pipeline reactor by a continuous process with high concentration of 70% hydrogen peroxide,many disadvantages of the traditional batch process in tank reator were overcomed. The influencing factors on the epoxy value of the product,such as amount of H2O2, amount of HCOOH,reaction time,reaction temperature were discussed. The optimum conditions were determined as follows:m(fatty acid methyl esters):m(H2O2) :m(HCOOH)= 1∶0.6∶0.05,reaction time 15min,reaction temperature 90℃,The epoxy value of the product was up to 6.0% under these conditions.
XUE Qiang , QIANG Xi-huai , ZHANG Hui , WANG Yan-jiao
2013, 30(12).
Abstract:A novel series of acrylic resin/gelatin composite latexes (PA-G) with an ambient temperature self-crosslinkable function and excellent stability were prepared by seed, semi-continuous copolymerizing a functional monomer acetyl acetyethyl methacrylate (AAEM) with other normal monomers and adding a certain amount of gelatin as crosslinking agent into the resin emulsions (PA). FTIR spectra showed that the crosslinked structure had emerged in the composite films. Contact angles (CA), atomic force microscopy (AFM) and differential scanning calorimeter (DSC) were employed to characterize the PA-G films. The results indicated that the influences of AAEM-gelatin on some PA-G film properties differed greatly. Hardness and glass transition temperature (Tg) of PA-G films were both markedly enhanced, and tensile strength was evidently reinforced while elongation at break was in reducing trend. Suitable dosage of AAEM-gelatin crosslinked structure could render PA-G film with good water resistance, causing little change on its relative surface roughness.