Ke Guojun , Zhang Lin , Yang Pengfei
2017, 34(10).
Abstract:Different morphology Mg-Al layered double hydroxides(Mg-Al LDHs)were synthesized by hydrothermal method, using magnesium nitrate and aluminum nitrate as raw material and urea as precipitation reagent. The prepared samples were characterized by SEM、XRD、BET and EDS etc., respectively. The adsorption performance of the LDHs and their calcined products for chloride ion were also investigated. The results showed that the rodlike Mg-Al LDHs could be synthesized by hydrothermal method when adding glycol. Hexagonal platelet-shaped and cube- shaped LDHs appeared when adding ethanol and tetrapropylammonium hydroxide. The specific surface area of the hexagonal platelet-shaped LDHs were 115.311m2/g, which had regularly and uniformly distributed morphology and can easily form a cross between support structure, showed good adsorption capability for chloride ion. The maximum adsorption capacity was 24.72 mg/g when the temperature was room temperature. The maximum adsorption capacity of the products calcined after 450 ℃ increased greatly, which was 96.07 mg/g in the same conditions. Optimal adsorption condition: the temperature is 35 ℃, the dosage of LDO-2 is 2.0 g/L, the value of pH is 8,the calcination temperature is 450 ℃.
2017, 34(10).
Abstract:Drug delivery system has great significance for the targeted treatment of cancer. A cyclized & branched amphiphilic block copolymer was synthesized by DE-ATRP with brominated polyethylene glycol (PEG2KBr) as initiator and di(2-acry-loyloxy ethoxy)-[4-methoxy-phenyl]methane (ACD) as hydrophobic monomer and explore for its potential application to drug delivery. The structure of polymer was characterized by hydrogen spectrum nuclear magnetic resonance (1HNMR) and gel permeation chromatography (GPC). The size and morphology of micelles was measured by dynamic light scattering (DLS) and transmission scanning microscopy (TEM). The structure was identified to be branched-cyclized. The blank micelles were spherical with the size of 70 nm, and Doxorubicin hydrochloride loaded micelles were with the size of 90 nm. The drug loading efficiency was 48.7%, DOX-loaded micelles have good pH-responsive and drug release. It is proved that the polymer has a certain application value in drug delivery system.
2017, 34(10).
Abstract:The SiO2@TiO2-Ag@SiO2 core-shell microspheres were prepared with monodispersed SiO2(Stöber mothod) as core using sol-gel method, interface deposition method and surfactant template in turn. The structure and morphology of microspheres were investigated and analyzed by FT-IR, SEM, XRD, UV-vis, N2 adsorption desorption and XPS. The results show that average pore size and specific surface area of SiO2@TiO2-Ag@SiO2 microspheres is 2 nm, 72.73 m2/g, respectively. TiO2 diffraction peaks of anatase phase are not observed in XRD under the influence of the outer layer SiO2. UV-visible diffuse reflectance spectroscopy confirms that the core-shell microsphere is absorbed at 365 nm. Under simulated solar light source, the photocatalytic decolorization rate of methylene blue was 97.6% by SiO2@TiO2-Ag@SiO2. And the decolorization rate of methyl orange was 99.7% with 40 min flocculation precipitation under natural light.
GAO Chengyong , ZHANG Zhe , LIU Ya-ni , Yang Zhiwang , Lei Ziqiang , MA De-long , GUO Xing , XU Xiao-huan
2017, 34(10).
Abstract:A novel amino-functionalized magnesium hydroxide (DETA-AA-MH) was synthesized and used as curing agents for epoxy resins.DETA-AA-MH was characterized by Fourier transform infrared spectroscopy (FTIR), X-ray power diffraction (XRD), Solid state nuclear magnetic resonance(SSNMR), nano particle analyzer, field-emission scanning electron microscopy(FESEM) and thermogravimetric analysis (TGA). Crosslinking behavior was found by FTIR and differential scanning calorimetry (DSC), the best mass ratio of curing reaction was epoxy resin(DGEBA, 84.03%) and DETA-AA-MH1 (5.97%), the optimum curing temperature were 80 and 110 ℃. Flame retardance of the EPs was evaluated by LOI tests, compare the data of DGEBA/DETA with DGEBA/DETA-AA-MH, the LOI of DGEBA/DETA-AA-MH was improved by 10.15%. SEM and EDS was employed to investigate the burning residues of EP, confirming that DETA-AA-MH could promote the formation of a protective char layer during burning. The experiments for determining the mechanic properties of DETA-AA-MH cured EPs were also conducted, which indicated that compared to EP (mass fraction 7.38% DETA), Comparing with, the flexural strength, flexural modulus and impact strength of EP(mass fraction 15.97% DETA-AA-MH) were efficiently increased by 669.70%, 33.12%, 228.57%, respectively.
Guo Yao-nan , Li Yin-tao , Liu Xing-hao , Long Chun-hua , Zhou Yuan-lin
2017, 34(10).
Abstract:The emulsion of methyl methacrylate-methacrylic acid copolymer [P(MMA-co-MAA)] was modified by nano-silica (SiO2). The structure and properties of the composite emulsion were determined by infrared spectroscopy (FTIR), thermogravimetry (TG), X - ray diffraction (XRD) and scanning electron microscopy (SEM). The results show that the aggregation structure ofP(MMA-co-MAA) has been changed after the addition of nano-SiO2, resulting in the change of self-embritting morphology of the emulsion. The main performance is that, with the increase of nano-silica content, crisps have a big trend and shrinkage is more obvious, which promotes the self-embrittlement and stripping performance of P(MMA-co-MAA). This performance has the advantage of removing radioactive waste from the surface of the equipment.
XING Yu , GUO Xue-hui , XU Bei , LI Jing-jing , LIU Zhen-xin , FANG Shao-ming
2017, 34(10):0-0.
Abstract:Ferrous oxalate was employed as iron source to synthesize LiFePO4 (i.e., a cathode material for Li-ion batteries) via a hydrothermal route. XRD and FESEM were used to analyze the structure and texture features of products, while coin-cell charge/discharge tests were conducted to measure the electrochemical performance of products. Conditions for hydrothermal crystallization were optimized. The results demonstrate following information: The temperature of 190℃ is the minimum feasible crystallization temperature. The crystallization time for hydrothermal synthesis should be shorter (e.g., 10 h) rather than longer (e.g., 24~57 h), because a long crystallization time may cause the LFP’s relative diffraction intensity to deviate the standard XRD pattern, which is a sign for structural change, as well as the huge disparity of particle sizes. As the crystallization temperature for hydrothermal synthesis reaches 280℃, a part of Fe(II) within the carbon-free product may be oxidized to Fe(III) and form FePO4•2H2O impurity, while an addition of glucose (i.e., a carbon source) may suppress the conversion from Fe(II) to Fe(III). LiFePO4 with less-aggregated particles and a specific discharge capacity of 154 mAh/g may be hydrothermally synthesized at suitable crystallization temperature (e.g., 240~260℃) and time (e.g., 10 h) using ferrous oxalate as the iron source, which consumes 6339 mol of lithium source (LiOH) compared with 19016 mol consumed by the hydrothermal method using ferrous sulfate.
WU Qi-chao , QIU hai-ling , XIE bo-wen , ZHU hui-dan , ZHANG Wei-ming , HAI jie-feng , LU Zhen-huan
2017, 34(10).
Abstract:Two asymmetric perylene diimide small molecules were synthesized, namely N, N’-di(2-ethylhexyl)-1- (2-methoxyethoxy)-7- nitryl - perylene -3, 4, 9, 10-tertracarboxylic acid diimide (Ⅲ) and N, N’-di(2-ethylhexyl)-1- (2-methoxyethoxy)- 6, 7- dinitryl - perylene-3, 4, 9, 10-tertracarboxylic acid diimide (Ⅳ). It was synthesized from 3, 4, 9, 10-perylenetetracarboxylic dianhydride by via connect 2-methoxyethoxy and nitryl to the opposite sides of the molecular bay-positions. The structures were characterized by 1H NMR, 13C NMR and MS. We have used density functional theory to optimize the calculation of molecular spatial stereoscopic conformation, the molecular twisted backbone and distribution of electron cloud was also studied; Ultraviolet-Visible absorption spectra (UV-Vis) showed that there is obvious red-shift on the maximum absorption peak, and the peak width at half height broaden; Through the cyclic voltammetry (CV), we calculated that the HOMO and LUMO energies of molecule Ⅲ are −5.85 eV and −3.55 eV, the molecule Ⅳ are −5.87 eV and −3.62 eV. Finally, at a relative humidity of 50% in atmospheric environment, the device of organic solar cell was constructed that Ⅲ and Ⅳ were respectively blended with polymer of benzodithiophene-alt-polythiophene (PTB7-Th). The performance of the device that the JSC= 3.6 mA/cm2, VOC=0.30V, FF= 0.40, PCE= 0.42% and JSC= 4.00 mA/cm2, VOC= 0.25 V, FF= 0.41, PCE= 0.40%.
2017, 34(10):0-0.
Abstract:Carboxyl-terminated itaconic acid based polypropylene glycol (400) monoester (IPM) was synthesized by itaconic anhydride (IAn) and polypropylene glycol 400 (PPG 400) as the raw material through esterification reaction, and its structure was characterized by Nuclear Magnetic Resonance (1H NMR) and Infrared Spectrometer (FT IR). And then the itaconic acid based polypropylene glycol (400) monoester carboxylate Bola surfactant (Saa-K) was synthesized by neutralization of IPM with potassium hydroxide (KOH). The surface tension, critical micelle concentration (CMC), foaming characteristics, etc. were studied. The surface tension of Saa-K was 32.46 mN/m, CMC was 2.193×10-3 mol/L; TK1 was less than 0 °C, TK2 was 54.3 °C, foaming volume was 55.13 mL, and foaming life was 1940 min.
2017, 34(10):0-0.
Abstract:A Schiff base compounds containing both rhodamine and coumarin L was synthesized by using Schiff base functional groups as linker, coumarin and rhodamine as chromogenic groups. The structure of the probe was characterized by 1HNMR, 13CNMR and HRMS. The recognition mechanism of Ca2+, Cd2+ and Al3+ were also investigated. The results show that L can selectively recognize Ca2+, Cd2+ and Al3+ in ethanol system and have some anti-interference ability over other metal ions. L and L+ions at pH 7~12 have significant fluorescence enhancement effect. High resolution mass spectrometry and the Job curve show that L can form complexes with Ca2+, Cd2+ and Al3+ in molar ratios of 1:1, 2:1 and 2:1, respectively.
ZHANG Wei-wei , WEI Yu , ZHANG Hong-juan , JIAO Qing-cai , LIU Jun-zhong
2017, 34(10).
Abstract:A method for the preparation of D-alanine by continuous catalyzed of aspartic acid racemase and D-amino acid transaminase was established. DL-aspartic acid was obtained by racemization of L-aspartic acid with whole cell of aspartic acid racemase, and then the whole cell was removed by centrifuging, and the residual aspartic acid racemase was inactivated by heating. Then, added D-amino acid transaminase purified by Ni-column affinity chromatography, D-aspartic acid (D-Asp) and pyruvic acid (PA) were converted to D-alanine. The optimal catalytic conditions of aspartate racemase were as follows: the reaction temperature was 40 oC, 0.2 mol/L of potassium phosphate buffer solution (pH=7.0), 100 g/L of L-aspartic acid. The optimal catalytic conditions of D-amino acid transaminase were as follows: the reaction temperature was 42 oC, 0.2 mol/L of potassium phosphate buffer (pH=7.0), 4 mmol/L of pyridoxal phosphate, 50 g/L of DL-aspartic acid, the molar ratio of PA and D-Asp is 1:10. The transformation product D-alanine was obtained by the method of isoelectric point crystallization and cationic resin separation. The conversion of D-aspartic acid was 94%, the yield of D-alanine was 84%, and the ee value of D-alanine was 98%.
MA Na , FU Xiaoqian , SUN Weipeng , DANG Yanyan
2017, 34(10):0-0.
Abstract:Abstract: Microwave-assisted Salting-out Extraction of Phenolic Compounds and Lutein from marigold flowers were studied by acetone/ammonium sulfate system.The effects of microwave time, microwave power, solid-liquid ratio, and other factors on the partitioning behavior of the target products were investigated by single factor experiments and the optimization of extraction technology of microwave assisted salting-out extraction polyphenols from marigold by response surface method. The study showed that the extraction rates of total phenolics (TP), total flavonoids (TF) and lutein were 85.76 mg/g, 6.70 mg/g, 0.85 mg/g, respectively. The recoveries were 96.64%, 98.15%, 95.98%, respectively. The extraction rate was 86.24 mg/g under the optimum extraction conditions of microwave power 500 w, microwave irradiation time 95 s, solid-liquid ratio 1:45, crushing the mesh 160. The antioxidant activity of the extracts was also studied preliminarily.
YANG Jing , SHEN Jian , SHI Weiwei
2017, 34(10).
Abstract:The adsorbent of Cu-β/SBA-15 was synthesized by the impregnation method,and the samples were characterized by means of XRD,N2 adsorption-desorption,NH3-TPD,Py-FTIRThe results indicated that Cu-β/SBA-15 could retain the micro-mesoporous composite structure and has a good weak acidity.Using the β/SBA-15 as adsorbent,the static reaction of adsorption removal dibenzothiophene in a bath micro-reactor.The influences of reaction temperature、reaction time and reagent oil mass ratio to oil on adsorption capacity were investigated.Morever,experimental study of adsorption kinetics was performed.The results showed that the desulfurization rate of simulated diesel oil was 54.62% and the adsorption capacity was 2.27 mg/g at the reaction temperature of 120 ℃,reaction time of 120 min and reagent oil mass ratio of 1:30.In the initial stage of Cu-β/SBA-15 adsorption to dibenzothiophene,the pseudo-second-order kinetics equation and Elovich equation could well reflect the adsorption model.As well as,the correlation coefficient R2>0.99 in the entire stage,and the calculated equilibrium adsorption capacity qe=2.54 mg/g and the difference between the observed equilibrium adsorption capacity was 2.27 mg/g,which indicated that the pseudo-second-order kinetics equation could be more comprehensively describe the adsorption process of Cu-β/SBA-15 to dibenzothiophene and its controlled by both film diffusion and particle diffusion.
2017, 34(10).
Abstract:A series of composite bi-functional catalysts, used to hydroalkylation of BZ into CHB, were prepared by incipient wetting method on the carrier of β. The synergistic effects between catalyst components were investigated by using XRD, BET, TPD and HR - TEM characterization methods. The catalytic performance stability of different catalysts was compared in a fixed bed reactor. And the effect of catalyst composition on BZ conversion and CHB selectivity was examined. The results show that: adding different metals as co-catalysts into Ni/Hβ can regulate the loading particle size, active center dispersion, B/L acidic site concentration on the surface of the catalyst, and the matching of metal catalytic hydrogenation and acid catalytic alkylation of the bi-functional catalyst.The catalytic performance of hydrogenation and alkylation is matched well over 4%Ni-0.2%Pd-3%La/Hβ. Accordingly, the conversation of benzene and the selectivity of cyclohexylbenzene can reach 34.44% and 74.67%, respectively, under the conditions of 220℃, H2 GHSV of 2500 h-1 and benzene LHSV of 2.0 h-1 over the catalyst, and the catalytic performance has no obvious decline within 240 hours.
Shen Yixiu , Lv Xinyu , Qiu Tao
2017, 34(10):0-0.
Abstract:CuxZn1-xCr0.5Al1.5O4 spinels were prepared by chemical co-precipitation method using Cu(NO3)2, Zn(NO3)2,Cr(NO3)3,Al(NO3)3 and NaOH as raw materials. The structure, physical and chemical properties of spinels were characterized by XRD, ICP, SEM and BET. CuxZn1-xCr0.5Al1.5O4 spinels with different compositions were used as catalysts in the fixed bed reactors for the catalytic synthesis of NMA. The influence of such factors as spinel compositions, reaction temperature, space velocity (WHSV) and molar ratio of reaction raw materials on the catalytic reaction was investigated. The experimental results indicated that reaction temperature of 265℃, WHSV of 0.15h-1 and 3:1 molar ratio of methanol to PA was optimal reaction conditions, and Cu0.5Zn0.5Cr0.5Al1.5O4 had the best catalytic performance. The conversion per pass of PA and the selectivity of NMA were 90.95% and 94.93% respectively.
ZHANG Li-li , SUN Ying , KONG Yan , ZHANG Yu-yu
2017, 34(10).
Abstract:In order to preparing the thermal reaction recipe of the sweet and sour spareribs flavoring, basing on the spareribs soup flavoring, single-factor analysis, orthogonal test and the sensory evaluation were used. The final optimization results for the thermal reaction formula were as follows: Longmen rice vinegar concentrate 9.30g, sucrose 7.30g, glucose 5.00g, xylose 1.00g, yeast extract 0.90g, pig bone oil 7.20g, HVP 1.35g, I G 0.16g, VB1 0.27g, cysteine 0.73g, glutamate 0.73g, arginine 0.73g, proline 0.73g, tomato sauce 3.50g, pepper oil 1.00g, braised soy sauce 2.30g, cooking wine 3.00g, spices accounted for 0.10% of the whole, enzymatic hydrolysate of porcine bone 18.75g, pork enzymatic hydrolysate 18.75g.
JIA Pengfei , WANG Juan , LI Xiaolin , HAN Xiaomin
2017, 34(10).
Abstract:4-(8-Chlor-5,6-dihydro-11H-benzo[5,6]cyclohepta[1,2-b]pyridine-11-ylidene)-1-piperi-dine carboxylic acid ethyl ester (Loratadine) was prepared from ammonia and methyl acrylate through Michael addition, Dieckmann cyclization, decarboxylation, ethoxy carbonylation and McMurry reaction. The conditon of McMurry reaction was conducted under ultrasound irradiation, and technological parameters involved in McMurry reation were optimized. Structures of the title compound and the intermediates were confirmed by 1HNMR. The results show that n(8-chloro-10,11-dihydro-4-aza-5H-dibenzo[a,d]cyclohepten-5-one):n(N-ethoxycarbonyl-4-piperidone):n(TiCl4):n(Zn)= 1:1.2:4:6.8 reacted under 25kHz and 67℃(under reflux)for 30min to give the intermediate in 88.5%, and the total yield of target compound(Loratadine) was 57.8%.