2014, 31(4).
Abstract:PBMA/GMA-SiO2 adsorbent was synthesized via RAFT polymerization by using butyl methacrylate(BMA) and GMA -functionalized silica particles as monomers. The effects of pH,contact time and initial Pb2+ concentration on adsorption properties were evaluated, as well as adsorption thermodynamics and kinetics were also examined. The results show that the PBMA/GMA-SiO2 adsorbent was effective for Pb2 removal from water, the maximal adsorption capacity for Pb2+ was found to be 423.84 mg/g, the optimum pH value for Pb2+ removal is 5 to 6, and absorption time is 1 h, the removal efficiency increased with the decreasing of initial Pb2+ concentration. Under optimized conditions, 50 mg sorbent could remove 100% of Pb2+ from 50 mL 0.02 g/L Pb2+ solution at pH = 6 and 298K. The adsorption kinetics could be best described by pseudo second-order kinetic model, compared with the Freundlich isotherm equation, the Langmuir isotherm equation is more appropriate to describe the adsorption behavior. The adsorption rate is not only controlled by intra-particle diffusion but also by extra-particle diffusion. Besides, the materials still show good adsorption capacity to Pb2+ after five times of desorption and adsorption.
2014, 31(4).
Abstract:Using 2-acrylamido-2-methyl propane sulfonic acid(AMPS) as monomer, attapulgite (APT) and carboxymethylcellulose (CMC) as composite components, novel eco-friendly carboxymethyl cellulose-g-poly(2-acrylamido-2-methyl propane sulfonic acid)/attapulgite superabsorbent composites were synthesized by means of microwave irradiation.The suitable reaction condition of of superabsorbent resin was investigated .The chemical micstructure of superabsorbent resin were determined by FTIR. The results showed that CMC and APT participated in grafting copolymerization reaction,and the water absorbency of superabsorbent resin is 834g/g in the deionized water and 78g/g in normal saline respectively under the suitable conditions. the water absorbency of superabsorbent was decreased quickly with the increase of salt concentration and the valence of metal cation. The water absorbency, salt-tolerant performance and pH stability of superabsorbent resin could be remarkably enhanced by introducing a proper amount of APT.
2014, 31(4).
Abstract:Ytterbium-doped Tin Oxide Nano-powers were prepared by chemical co-precipitation method using SnCl4•5H2O and Yb(NO3)3•6H2O as precursors and NH3•H2O as precipitant. The effects of processing parameters on the particles were investigated. These parameters include reaction temperature, calcine temperature, kinds of dispersant. The Ytterbium-doped Tin Oxide precursors were studied by means of TG-DTA. The product particles were characterized by means of X-ray diffraction(XRD) and scanning electron microscopy(SEM). The optimized conditions for preparing nanometer Ytterbium-doped Tin Oxide powers were proposed:reaction temperature of 60 ℃, calcine temperature of 600 ℃, non-ionic dispersant of PEG-600.
ZHAO Dong-yan , Qiao Xu-guang , XU Zhi-xiang
2014, 31(4).
Abstract:Modified chitosan was prepared with chitosan, ethyl acetate, and epichlorohydrin at ratio of 30:1:1(v/v). This prepared material was evaluated by FT-IR spectra, SEM images, and UV spectra analysis. FT-IR spectra results indicated that epichlorohydrine might have reacted with chitosan and the modified chitosan had been formed. SEM image analysis showed that the addition of epichlorohydrine had important effect on the crystallinity. The adsorption test indicated that the modified chitosan exhibited a faster kinetics for the adsorption and desorption of olaquindox in 3 hours; modified chitosan offered higher selectivity and adsorption capacity toward olaquindox than that of structurally related compounds.
CHEN Yu-heng , PENG Chao-rong , CHEN Zhu-ping , WANG Jing-xia , NI Mao-jun , LIU Si-yang , BAO Wen-ting
2014, 31(4).
Abstract:Gamma ray graft polymerization was used in this paper to improve the hydrophilicity and cell compatibility of PLA. The materials were investigated by FT-IR, SEM, DSC analysis, water contact angle measurement and water uptake test. The results showed that the modified materials had better hydrophilicity and the contact angle was decreased 8癮nd the water uptake was increased 13.3 times after graft polymerization. The cytotoxicity experiment was carried out to evaluate the biocompatibility of the grafted copolymer. The result indicated that the grafted material has no cytotoxicity and has better biocompatibility; the cell survival rate was 109.3% of 50% leaching liquor and 107.4% of 100% leaching liquor.
2014, 31(4):0-0.
Abstract:Abstract: Acetobacter xylinum strain was screened in our own laboratory,Using coconut water as incubating system,Bacterial cellulose (BC) were prepared by Static fermentation culture method using Acetobacter xylinum. the structure and properties of the BC and commercial BC were tested and compared. Observe the microstructure characteristics of BC. Results showed Preparation of BC and commercial BC are similar in structure and some properties,They are colorless, transparent film and a three dimensional network structure and pores structure, It proves that BC has fine nano fibre-network, it has good moisture absorption and excellent holding water capacity. The BC production cost is low,And according to need a lot of preparation, which has extensive usage in biomedicine areas.
2014, 31(4):0-0.
Abstract:2,4-bis(n-octylthiomethyl)-6-methylphenol was synthesized from o-cresol, o-octanethiol and paraformaldehyde using piperidine as catalyst and N,N-dimethylformamide as solvent under nitrogen protection. The effect of various reaction parameters, including material ratio,the amount of catalyst,reaction temperature and time, was investigated in detail. When the molar ratio n(o-cresol): n(o-octanethiol): n(paraformaldehyde) = 1:2:4, the amount of piperidine was 9.8% of o-cresol, at 110℃ for 8 hours ,the target compound 2,4-bis(n-octylthiomethyl)-6-methylphenol had a higher yield of 94.5%. The product was verified by means of IR and 1HNMR.
2014, 31(4).
Abstract:A kind of polysiloxane defoamer polysiloxane were synthesiszed by the hydrosilylation reaction with polyethylene oxide ethyl polyethylene oxide propyl ether (F - 6) and lauryl methacrylate(LMA) containing hydrogensilicone oil as material, using Karstedt the catalyst. The structure of the molecular of the synthesized defoamer were characterized by infrared (IR) spectrum and nuclear magnetic resonance (1HNMR) spectrum. The author determined the optimum reaction conditions through by investigating the effects on the reaction conversion of the molar ratio of silicon-hydrogen bonds with the carbon-carbon double bond,reaction temperature,reaction time,amount of catalyst. The best technology of the product achieved 94.78 % with the optimum reaction conditions that the molar ratio of silicon-hydrogen bonds was 1:1.20, the amount of catalyst was 50 μg/g, the reaction temperature was 90 ℃,and the reaction time was 8 h. Application test show that the defoamer defoaming and inhibiting performance superior to market similar products.
YUAN yuan , YANG qian-qian , GUO shan-shan , PEI xiao-li , LIU xue-min
2014, 31(4).
Abstract:N,N-bis(dodecylamidoethyl)-N-propyl sulfonate having two alkyl amide chains was prepared using an excess of 1,3-propane sultone and intermediate N,N-bis(dodecylamidoethyl)-amine, which was synthesized by amidation from lauric acid and diethylenetriamine, in toluene/acetone mixed solvent under reflux conditions. The chemical structures of intermediate and this surfactant were characterized by FT-IR, ESI-MS, and 1HNMR methods. The krafft point of this surfactant is 37.3℃ by electrical conductivity method. Its surface tension in aqueous solutions was determined by pendant drop method to study the adsorption behavior at the water/air interface. The values of CMC,γCMC,C20,Γ∞,ΠCMC, Amin were obtained by the γ-lgC curves, with 6.40×10-4 mol/L critical micelle concentration(CMC), and 37.33 mN/m the lowest surface tension (γCMC) at 45℃. The interfacial tensions between different concentration surfactant solutions and n-alkane had been investigated at 45℃ over a wide NaCl dosage range from 0% to 5%. The minimum interfacial tension between 1×10-4mol/L (5% NaCl) surfactant solution and nonane reduced to 3.39×10-3mN/m at 45℃, and at the same time, the salting-out phenomenon does not occur.
2014, 31(4).
Abstract:Immobilization of Gluconobacter oxydans cells and conversion of ethylene glycol to glycolic acid in bubbling reactor were investigated. The optimum of immobilization was 8%PVA, 0.8% sodium alginate and 0.27g cells biomass per milliliter gel. The immobilized cells were more stable than free cells in pH and thermal stability. Conversion of ethylene glycol to glycolic acid was carried out in bubbling reactor. When the initial ethylene glycol was 70g/L, the first cycle conversion was 92.6%, and it could successively convert six cycles, the average conversion was about 85%.
2014, 31(4).
Abstract:By the chemical reduction method, a series of Co-B catalysts were prepared by changing the concentration of the cobalt acetate precursor and used for liquid hydrogenation of ethyl lactate to 1,2-propanediol. The reaction conditions were discussed. The as-prepared catalysts were characterized by means of physical adsorption (BET), X-ray powder diffraction (XRD) and transmission electron microscope (TEM). The results show that all the fresh catalysts showed an amorphous structure, and the thermal stability of the amorphous catalyst increased with increasing the concentration of the cobalt acetate precursor solution. The BET results show that all the catalysts were mesoporous structure. The conversion of ethyl lactate was up to 98.53%, the yield of 1,2-propanediol was 98.32% under the optimum conditions of 160℃, H2 pressure 6 MPa for 9h.
ZHONG Jun-mei , XU Jian-xin , LIU Yu-mei
2014, 31(4).
Abstract:On the basis of deterrmined the pigment content analytical method for anthraquinones pigment content, an Orthogonal test L9(34) was used to observed the optimal extraction process of ethanol extract anthraquinones pigments from walnut green husks, and the effects of the pigment stability on oxidants, reducing agents, light, metal ions were also investigated. The results showed that this analysis method has high precision and accuracy (recovery is 90.44% ~ 103.52%), with well stability and good reproducibility. The linearity with correlation coefficient 0.9997 was found within the range of 0.00416 mg/ml to 0.0250 mg/ml. The highest pigment extraction rate can be obtained when solid-liquid ratio is 1:30(g.ml), ultrasonic time is 30min, extraction temperature is 60℃ and ethanol concentration is 50%. Research results for pigment stability also displayed that the metallic ions K 、Na 、Mg2 、Ca2 and Zn2 have no apparent effect, and Fe3 has hyperchromic effect significantly.
2014, 31(4).
Abstract:Dimethyl 1,4-Cyclohexanedicarboxylate (DMCD) was synthesized by hydrogenation of Dimethyl Terephthalat (DMT) under mild conditions on Nasnoscale RuPd/C Catalysts .Effects of solvent, reaction temperature, pressure and amount of catalyst have been investigated. Under optimal reaction conditions:140℃, 4.0 MPa pressure,isopropanol 2000ml,DMT dosage 1300g, catalyst dosage 65g, conversion of DMT and selectivity to DMCD mount to 99.8% and 96.3% in 5000ml high pressure reactor. After RuPd/C Catalyst was reused for 22 times in the same conditions, the conversion of DMT and selectivity to DMCD still remain at 99.0% and 95.1%, respectively.
LIU Yu-ting , LI Xin , YIN Da-wei
2014, 31(4).
Abstract:Cu(Ⅱ), Ni(Ⅱ), Zn(Ⅱ), Pb(Ⅱ), Cd(Ⅱ) complexes with Schiff base derived from diacetylferrocene and hydrazine hydrate have been prepared. The ligand and its complexed have been characterized by molar conductance, elemental analysis, IR spectra and 1H NMR. All compounds were screened by antibacterial activity. The final results indicate that all compounds had inhibitory activity. Metal complexes 2a–2f had moderate to excellent antimicrobial activity in comparison with the ligand compound. Among these compounds, CdL(CH3COO)2(2f) had the best inhibitory activity.
2014, 31(4).
Abstract:In search of effective antitumor agents, According to substructure link principle, The quinolone compounds and α-hydroxyphosphonates were jogged. Eight O,O' - dialkyl - α - phenyl - α - substituted quinolinylanoxy methylphosphonate derivatives were designed and synthesized. The structures of all the compounds were confirmed by IR, NMR and elemental analysis. The bioassay of target compounds were tested. The result indicated that they exhibited certain antitumor activities. And compounds 3c, 3g showed obvious inhibition effect on SGC-7901 cells growth in vitro at 20 μ mol/L, inhibition ratio reached 50.7 %, 46.4 %, respectively.
JI Hong , WU Liyang , HUANG Biyun , YUAN Mu
2014, 31(4).
Abstract:In order to find new a1-receptor inhibitors with high selectivity, seven 1-(3-benzoyl-1-phenoxyl)-3-(4-phenylpiperazin-1-yl)-propan-2-ol and 1-(4-methoxyphenoxy)-3-(4-arylpiperazin-1-yl)-propan-2-ol derivatives (5a-5g) were synthesized through substitution reaction of 3-chloro-1,2-epoxypropane (2) with 3-hydroxylbenzophenone or 4-methoxylphenol in alkaline condition, followed by the ring cleavage of 3-substituted phenoxy-1,2-epoxypropane (3) with arylpiperazine. All the target compounds were identified by their 1HNMR, MS, IR spectra and elemental analysis. The response of rat anococcygeus muscle to these compounds in vitro was tested, and the bioassay indicated that all the compounds had potent antagonistic activity against 1-receptor(pA2>6), and compound (5g) showed the best potency(pA2=8.13±0.25).
2014, 31(4).
Abstract:A facile enzymatic approach to synthesize feruloylated glucoside derivatives through lipase-catalyzed transesterification of ferulic acid vinyl ester (FAVE) with glucose was developed. The effect of various reaction parameters on the synthesis of feruloylated glucoside was studied systematically. Lipase Novozym 435 was found to have the highest catalytic activity in an anhydrous pyridine/tert-butyl alcohol (2:1, V/V) solvent mixture. FAVE was selectively conjugated onto the primary hydroxyl group of glucose (1:4, n/n), with a yield of 80.9% under optimal conditions.
2014, 31(4).
Abstract:The walnut shell-supported-nano zero valent iron (walnut-nZVIFe) was prepared by NaBH4, FeCl2.4H2O and walnut shell using liquid phase chemical reduction. The materials were characterized by FT-IR, XRD and TEM. The walnut-nZVIFe to Pb2 was investigated. The results had indicated that the maximum adsorption capacity for Pb2 was 199.90 mg g-1 at 293K, pH 5.0 and the amount of the adsorbent was 10 mg when the initial concentration of Pb2 was 200 mg.L-1. The adsorption kinetics data indicated that the adsorption fitted well with the pseudo-second-order kinetic model. The adsorption isotherms of Pb2 could be well described by the Langmuir equation.
YANG Xiao-wu , QIU Lie-wei , LI Pei-zhi , ZHAO Zhi-fang
2014, 31(4).
Abstract:A kind of fluorinated polyacrylate soap-free emulsion textile finishing agent was prepared using perfluoroalkyl acrylate (FEA) as functional monomer by soap-free emulsion copolymerization, and the size and distribution of emulsion particle and the surface activity of polymer solution were studied. With water and oil repellency textile finishing application experiment, the effects of the textile finishing agent dosage and the baked temperature were discussed in detail, and other performances were tested. The result showed that, the textile finished by the said water and oil repellency textile finishing agent had excellent water and oil repellency properity, its dynamic waterproofing score was 90 point and the oil-proofing grade could reach above level 5, the water contact angle is up to 142.5° and oil contact angle is up to 126° through finishing treatment, and it had good washing durability and general performance.
2014, 31(4).
Abstract:Through radical copolymerization, the soluble copolymer dispersant AA/SAS for ceramic powder was synthesized with acrylic acid (AA) and sodium allylsulfonate (SAS). The effect of different reaction conditions on the dispersing property of copolymer has been investigated. The copolymer was analyzed by Fourier transform infrared spectrometer (FTIR), differential scanning calorimetry (DSC), X-ray diffraction (XRD) and gel permeation chromatography(GPC). Meanwhile, the effects of dispersant concentration on the rheological behavior and Zeta potential of the ceramic slurry were also studied. The results show that the optimum condition of synthesis is as follow: the mass ratio of acrylic acid and sodium allylsulfonate 5:1, the reaction temperature 80℃, the dosage of initiator 7.3%, and the amount of chain transfer agent 225.5%. When its mass fraction was 0.3%, its dispersing effect was the best. The Zeta potential absolute value of the slurry increased from 33.7mV to 62.1mV as the mass concentration of the copolymer was 1.2g/L. In comparison with imported products PC-67, the copolymer could show better dispersity.
2014, 31(4).
Abstract:In order to improve the adhesion, stability and mechanical properties of the films, the epoxy styrene acrylic resin was synthesized by free radical solution polymerization ,and then blended with an inorganic Titanium sol to prepare a novel organic-inorganic hybrid films . The main factors influencing the resin synthesis were studied. The composition and structure of the resin and the organic-inorganic hybrid films were characterized by FT-IR, GPC, DSC, TG. It was found that the epoxy styrene acrylic resin with a number-average molecular weight of 6923, a weight-average molecular weight of 17213 and the polydispersity of 2.48 was obtained with 14% (relative to total monomer weight) benzoyl peroxide(BPO) as initiator, 1.5%(relative to total monomer weight) N - methylol acrylamide (NMA) as crosslinking agent and the hard and soft Monomer ratio of 1:1 at a reaction temperature of 90℃. In summary , the organic-inorganic hybrid films has better comprehensive performance compared with the epoxy styrene acrylic resin films , the films features good resistance to water ,saline ,and acid ,adhesion strength of 1 grade and pencil hardness of 5H .
2014, 31(4).
Abstract:1,5-dichloroanthraquinone was nitrated with mixed acid in 1,2-dichloroethane to form 1,5-di chloro-4-nitroanthraquinone, followed by nucleophilic displacing the chlorine atom located opposite the nitro group with an excess of diethanolamine to give a red dye polymerizing monomer containing anthraquinone: 1-[N,N-β-dihydroxyethyl)]amino-5-chloro-4-nitroanthraquinone. It has been found that the optimum process technology of synthesizing 1,5-dichloro-4-nitroanthra-quinine and 1-[N,N-β-di- hydroxyethyl)]amino-5-chloro-4-nitroanthraquinone via investigating some different factors effecting the synthetic process, of which 1,5-dichloro-4-nitroanthraquinone will be obtained in 95% at the foll- owing optimum conditions: n(HNO3) : n(1,5-dichloroan-thraquinone) = 2.00 : 1.00, mixed acid [n(H2SO4) : n(HNO3) = 2.0 : 1.0], reaction temperature 20℃, and reaction time 4h. And 1-[N,N-β-di- hydroxyethyl)]amino-5-chloro-4-nitroanthraquinone will be obtained with ?max1 = 393.5 nm, ?max2 = 514.6 nm, and the yield of 81.5% at the following optimum conditions: n(diethanolamine) : n(1,5-dichloro-4-nitroanthraquinone) = 5.00 : 1.00,reaction temperature 40℃, and reaction time 10h. The chemical structures of the two obtained compounds were characterized with melting point, MS, and 1H NMR.
2014, 31(4).
Abstract:Series of internal crosslinking waterborne polyurethanes were prepared from isophorone diisocyanate (IPDI), propylene carbonate polyols (PPC), dimethylol propionic acid (DMPA) as hydrophilic chain extender and trimethylolpropane (TMP) as crosslinking agent. The structure and properties of the polyurethane were characterized by Fourier transform infrared spectrometer ( FT-IR), thermogravimetric analysis ( TGA) , and its water resistance and contact angle were measured. It is found that, with increase of the TMP amount, the thermal property of the WPU film increases. Meanwhile, the water resistance property and the water repellency of the film are also improved.
ZHOU Qi-fan , YU Miao , CHEN Guo-liang
2014, 31(4).
Abstract:2,6-Dichloropyridine-4-carboxaldehyde was prepared from 2,6-dihydroxy isonicotinic acid with overall yield of 26.2 % via chlorination, amidation, dehydration and reduction. Its structure was confirmed by 1H-NMR and ESI-MS. Meanwhile, another useful intermediate 2,6-dichloro-pyridine-4-methylamine was obtained. The procedure of reduction reaction was optimized and when the molar ratio of 2,6-dichloro-4-cyanopyridine/Diisobutyl aluminum hydride was 1:1.6, the reaction temperature was -15℃ and the reaction time was 12h, the yields of 2,6-dichloropyridine-4-carboxaldehyde and (2,6-dichloropyridin-4-yl)methanamine were 45.4 % and 12.0 % respectively.
2014, 31(4).
Abstract:A series of pyrazoline derivatives were designed and synthesized from acetylferrocene, benzaldehyde, hydrazine hydrate and acyl chloride. The structures of the target compounds were confirmed by 1HNMR, FTIR and ESI-HRMS. Finally,the primary antimycotic activity of the title compounds against four plant fungals (Gibberlla saubinetii, Pythium solani, Gibberlla nicotiancola, Fusarium oxysporium f.s.p. niveum.) had been screened. The final results indicate that some of the compounds have a good plant anti-fungal activity.
QI Jia-juan , LI Shu-an , ZHANG Zhen-ming , WANG Ting , ZHAO Hong-bo , WANG Xuan
2014, 31(4).
Abstract:Novel six compounds of 3,3,6,6-tetramethyl-9- quinolyl-2,4,5,7,9,10- hexahydroacridine-1,8(2H,5H)-dione were synthesized through the multi-component reaction of 2-chloroquinoline-3-carbaldehyde, dimedone and ammonium acetate in 83%~93% yield under mild condition, and was subsequently cultured into a single crystal. The compound was characterized by means of elemental analysis, IR , 1H NMR, MS and the crystal structure was determined by X-ray single crystal diffraction. The results show that the crystal 3a belongs to the monoclinic system with space group Pccn, with a=2.2291(4)nm, b=1.1923(2)nm, c=1.7274(3)nm, α=β=γ=90°, Dc =1.199g/cm3.
2014, 31(4).
Abstract:Experimented the effect of the factors of temperature, St concentration, catalyst amount and reaction time on hydrolysis of stevioside catalyzed by hydrochloric acid or sulfamic acid. The results showed that stevioside conversion was nearly 100% , a yield of steviol reached 83.6% and a yield of isosteviol reached 12.4% catalyzed by hydrochloric acid with the optimum conditions. With the sulfamic acid catalyst, a conversion of stevioside of 100% nearly, a yield of steviol of 81.5% and a yield of isosteviol of 11.7% were obtained with the optimum condition.
2014, 31(4).
Abstract:Isophthalaldehyde was prepared from m-xylylenediamine and hexamethylenetetramine under the control of the reaction pH. The optimum conditions for the synthesis were as follows: n(MXDA):n(HMT)=1:4.5, temperature 104℃, time 4h,pH 3~4, yield 76.2%. FTIR and 1HNMR and ESI-MS analysis identified the desired product. The product properties reached the international quality standards,and detected by HPLC, the purity of the target product was 99.7%.
GONG Zong-xia , LI Bin , ZHANG Fei-yue
2014, 31(4).
Abstract:The ZnFe2O4/ZnO catalyst was prepared by an improved amorphous citric precursor method, and was applied in the cyclodehydration of diamine and 2,3- butanediol to synthesize alkylpyrazines.The catalyst was characterized by means of XRD and FT-IR. The effects of Zn/Fe molar ratio, reaction temperature, carrier gas space velocity on the conversion of 2,3-butanediol and selectivity of alkylpyrazines were studied in detail. The results indicate that the optimum conditions for the synthesis of alkylpyrazines were n(Zn):n(Fe)=2:1, reaction temperature 380℃, material flow rate 0.02mol/min, carrier gas space velocity 1440 h-1. The conversion of 2,3-butanediol was 93.38% and the selectivity of alkylpyrazines was 85.47% . The yield of 2,3-dimethylpyrazine was 22.16%.The yield of 2-methylpyrazine was 63.31%.