YAN Guang-yao , LI Chang-you , SUN Jie , YANG Quan-zhu , PANG Xue-lian , ZHANG Bao-hua
2020, 37(8).
Abstract:Spodoptera exigua nuclear polyhedral virus (SeNPV) is a kind of environmental-friendly biological pesticide with low drug resistance. However, SeNPV is inactivated easily under high ultraviolet (UV) and high temperature. In this paper, sodium alginate(SA) microbeads were prepared by atomization solidification method for embedding SeNPV, and functionalized modified by polydopamine(PDA)-coated. Furthermore, the composite microbeads were characterized by FTIR, DSC, TGA, SEM and particle size and distribution. The results showed that the D50 of the prepared PDA/SA-NPV (P/S-N) microbead was 132 μm, the stability of microbead structure at high temperature was good. The insecticidal activity of the compound microbead was higher than SeNPV suspension after UV treatment, which indicated the anti-ultraviolet property of the virus was enhanced under the double protection of calcium alginate and polydopamine.
YANG Langlang , WANG Weilin , MENG Fanhui , ZHANG Min , ZHENG Huayan , LI Zhong
2020, 37(8).
Abstract:Bifunctional catalysts can hydrogenate carbon monoxide or carbon dioxide (CO/CO2) directly to synthesize lower olefins, aromatics and gasoline, etc., which has the advantages of short process flow and low energy consumption. Bifunctional catalysts are composed of metal oxides and zeolites. The specific cavity structures, acidic properties and the combination with metal oxides of zeolites can significantly affect their catalytic performances. The research progress of zeolites used in CO/CO2 hydrogenation over bifunctional catalysts in recent years is reviewed. The effects of the types of zeolites, acidic properties, morphology and particle size, metal modification, combination of zeolite and metal oxide on the catalytic performance are summarized. The development trend of zeolites in bifunctional catalysts is prospected.
2020, 37(8).
Abstract:Measurement equipments and methods of dye solubility in supercritical CO2 fluid were reviewed. Influence rule of supercritical CO2 fluid process parameters and dye chemical structures on the solubility of disperse dyes was analyzed. Solubility data of disperse dyes in supercritical CO2 fluid in recent 20 years were then summarized, and solubility increasing techniques in supercritical CO2 were introduced. It is pointed out that the deep analysis for the action principle and influence law of dye structures on their solubilities, the establishment of dye dissolution behavior database in supercritical CO2 and the research on combination dyeing and color matching should be carried out in the future.
2020, 37(8).
Abstract:As an important kind of organic chemical intermediates, 2- (substituted ethynyl) benzaldehyde derivatives have a high chemical reactivity due to the special conjugate system and constituted with benzene ring, substituted ethynyl group and aldehyde group. So, they have been widely applied to build up variety of the novel benzo-fused ring compounds, N-containing benzoheterocyclic compounds, O-containing benzoheterocyclic compounds, muti-membered benzoheterocyclic compounds and so on. In this paper, the application of 2- (substituted ethynyl) benzaldehyde derivatives in the field of organic synthesis are reviewed, the prospects of this compounds are also discussed. It is hoped that this review can be referred to the future application of 2- (substituted ethynyl) benzaldehyde derivatives in organic synthesis.
CAO Haiyong , LIU Wenqin , WAN Pingnan , LIN Yan , CUI Han-feng
2020, 37(8):0-0.
Abstract:Dienones, a kind of unsaturated ketones with multiple chemical reaction sites, can achieve different types of chemical conversion with a variety of substrates, and construct organic compounds with different functions efficiently. In this paper, the chemical transformation of dienones with different substrates in recent years was reviewed. Firstly, the series of tandem Michael-Smiles cyclopropanation reaction, cycloaddition reaction, three-component Ritter reaction, photoinduced rearrangement reaction and direct oxidative coupling reaction of cyclohexa-2,5-dienone with different reagents were studied. The cyclopropane derivatives, fluoroalkylated N,O-ketal derivatives, ring-fused indoles, amides and unsymmetrical biaryls were constructed respectively. Secondly, the double Michael addition of penta-1,4-dien-3-ones with malononitrile, nitromethane, sodium hydrosulfide, oxindole, pyrazolone, fluorene and barbituric acid were analyzed, and the multi-substituted cyclohexanones, diaryltetrahydrothiopyran-4-ones, spirocyclic oxindoles, spirocyclic pyrazolones, spirofluorenes and spirobarbituric acid derivatives were synthesized. Then, we studied the 1, 4-conjugate addition, Aza-Michael addition, intramolecular Morita–Baylis–Hillman (IMBH) reaction, intramolecular reductive Aldol reaction, intramolecular Aldol reaction and intramolecular [4+2] cycloaddition reaction of penta-2,4-dien-1-ones realizing the preparation of organic sulfur compounds, organic nitrogen compounds, multi-substituted indanones and key intermediate of Tofogliflozin. Finally, the potential application of dienones in the subsequent chemical reactions was prospected.
2020, 37(8):0-0.
Abstract:As a phase transition metal oxide, the phase transition temperature of vanadium dioxide (VO2) is 68℃. VO2 presents an insulating monoclinic phase below 68?C and a rutile phase above 68?C. Because of the change in crystal structure, VO2 exhibits reversible mutations in optical and electrical properties, thus becoming a darling in the field of photoelectric switches. Based on this, this paper reviewed the preparation methods of VO2 and the main measures taken to regulate the phase transition temperature and performance of VO2. The advantages and disadvantages of different preparation methods and the factors that regulate the phase transition temperature and performance of VO2 were generalized. The application progress of VO2 in recent years was also summarized. Finally, the future development trend of VO2 was prospected. It was expected to provide guidance for researchers in related fields.
ZHANG Tian-tian , XIN Xiu-lan , SONG Nan , JIANG Bing , XU Bao-cai
2020, 37(8).
Abstract:Using aluminum isopropoxide as the raw material and dilute nitric acid as the solving agent, the spherical γ-Al2O3 with porous structure was successfully prepared by the sol-oil-ammonia drop method. The effects of alcohols with different carbon chain lengths as pore-expanding agents on their porous structure were investigated. The structure was characterized by XRD, FT-IR, SEM, TG, DTG and specific surface area and pore size analyzers. The results show that the type of organic alcohol has an effect on the porous structure of spherical γ-Al2O3. The longer the carbon chain alcohol, the richer the pore structure of the spherical γ-Al2O3 prepared; Larger, can reach 270.9 m2 / g. The spherical γ-Al2O3 with high sphericity and rich pore structure can be further used in catalysis, adsorption and other fields.
2020, 37(8).
Abstract:Gallic acid substituted zinc phthalocyanine (GA-ZnPC) was synthesized from 4-hydroxybenzaldehyde and 3,4,5-trimethoxybenzoyl chloride. Its structure and spectral characteristics were characterized utilizing FTIR, 1HNMR, MALDI-TOFMS, UV-Vis spectra, and Fluorescence Spectroscopy.The results reveal that GA-ZnPc is soluble in multiple organic solvents. When the concentration of GA-ZnPc is 2×10-6~1.0×10-5 mol/L, it exists in the monomeric form in DMF with Q-band maximum absorption peak appearing at 692 nm. Spectral titration was performed with GA-ZnPC DMF solution at a concentration of 2×10-6 mol/L, and the results confirm that GA-ZnPc maintains its monomer form, possessing apparent alkali-sensitive fluorescence characteristics owing to the intramolecular electron transfer enhanced by phenol to phenate transition.
Gao Yu-yang , LIU Shao-ying , WANG Qing-yin , WANG Gong-ying
2020, 37(8).
Abstract:A series of hydroxyl terminated polydimethylsiloxane (PDMS-OH) grafted MF resins (MF-PDMS) were synthesized via an effective method that employing dimethylacetamide (DMAc) as the solvent. The structure and surface chemical composition of MF-PDMS materials were characterized by FT-IR, solid state 1H NMR, XPS and SEM-EDS. The hydrophobicity and thermal properties of MF-PDMS materials were studied by contact angle, immersion and thermogravimetric (TG) analysis. The results indicated that the PDMS-OH has been directly grafted and copolymerized with melamine and formaldehyde in DMAc solvent, MF-PDMS resins have been successfully synthesized. PDMS-OH provided excellent hydrophobicity and thermal stability with MF-PDMS material, when the amount of PDMS-OH was 1.0% (based on the mole of melamine), the water contact angle of MF-PDMS-01 material increased to 91.81°, the surface free energy decreased to 28.1 mN/m, the water adsorption decreased to 2.83%, the residue at 400 ℃ and 700 ℃was 58.03% and 16.60%, respectively.
2020, 37(8).
Abstract:The polyaspartic acid-polyacrylic acid interpenetrating network hydrogel (PASP/PAA IPN) were successfully prepared by solvent-free processes. The preparation process was optimized by orthogonal design. The structure and properties of PASP/PAA IPN hydrogel were characterized by FT-IR, SEM and TG. The water absorption at different temperatures and pH conditions was also investigated. Finally, the prepared hydrogel were used as water retaining agent for pot experiment. The results show that the composition of the interpenetrating network has a significant effect on the stability and water absorption of the hydrogel. Based on the combination of stability and water absorption, the final process was selected to 2 mL of acrylic acid, 1 g of EDGE and 16 mg of MBA. The obtained PASP / PAA IPN hydrogel has a liquid absorption rate of 266 g/g and a saline absorption rate of 63 g/g, and has good thermal properties, pH sensitivity and temperature sensitivity. Pot experiment show that the growth, photosynthetic rate, and chlorophyll content of the PASP/PAA IPN hydrogel were better than those of commercially available PAA water-retaining agents under normal watering or drought stress. The photosynthetic rate was 7.82% (normal watering) and 53.44% (drought stress) higher than PAA water-retaining agent, respectively. The chlorophyll content was 58.33% (normal watering) and 249.7% (drought stress) higher than PAA water-retaining agent, respectively.
YAO Jin-huan , ZHANG Zhu-liu , YANG Yong-de , LI Yan-wei
2020, 37(8).
Abstract:Fe2O3 electrode materials with two-dimensional flake morphology were prepared by a facile su-crose-assisted one-step sintering method from Fe(OH)3 colloid. The effect of sintering temperature on the microstructure and lithium storage performance of Fe2O3 electrodes was investigated systematically. The results demonstrated that the sample sintered at 400 ℃ is the composites of α-Fe2O3/Fe3O4; while the samples sintered at higher temperatures (500 ℃, 600 ℃, and 700 ℃) are single phase α-Fe2O3. With the increase of sintering temperature, the tight connected irregular particles in the flake gradually get separated so that the two-dimensional flake structure tends to collapse. The results of electrochemical performance tests showed that the sample sintered at 500 ℃ has the best lithium storage performance. For example, a high specific discharge capacity of 628.6 mA·h/g can be retained after 450 cycles at a current density of 1 A/g, and a reversible capacity of 352.3 mA·h/g can be maintained even at 4 A/g. Ki-netic and the cycling stability analysis of electrode indicated that the sample sintered at 500 ℃ has the largest Li+ diffusion coefficient (the diffusion coefficient values corresponding to reduction peak and oxidation peak are 1.57×10-13 cm2/s and 4.60×10-13 cm2/s, respectively) and the best structural integrity stability among the studied samples.
wnagxuechuan , liuxuan , hanqingxin , zhujingbo , yinruojun
2020, 37(8):0-0.
Abstract:Ag/AgCl nanoparticles were synthesized in situ under 395 nm UV light with Cl- in reverse osmosis water (RO) and AgNO3 as raw materials. The morphology and size distribution of the samples were characterized by transmission electron microscopy (TEM) and dynamic light scattering (DLS).The crystal structure, element valence and photocatalytic performance of the composite were characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), ultraviolet-visible absorption spectra (UV-Vis) and fluorescence spectra separately. The results show that the Ag/AgCl composite are spherical particles with an average size of 100 nm. At the same time, the formation process of composite nanoparticles can effectively degrade rhodamine 6G. The degradation rate and quenching rate of rhodamine 6G can reach 96.5% and 95% when the silver ion solution was irradiated 3 min.
ZHANG Guo-rui , NIU Wen-bin , WANG Yun-peng , ZHANG Shu-fen
2020, 37(8):0-0.
Abstract:A photoelectric double response sensor using a structured color hydrogel as conductive electrode was prepared. The structured color hydrogel was prepared by bilayer self-assembly method using dodecyl glyceride itaconate (DGI), sodium dodecyl sulfate (SDS), sodium chloride as raw materials. The photoelectric double response sensor was combined by structured color hydrogel and traditional capacitive sensor.SEM, LCR meter, Tensile testing machine, Fiber optic spectrometer were used to characterize the device structure, optical, electrical and mechanical performance. Results show that in the tensile state (0~100%) and the compressed state (0~60.9 kPa), the capacitance of the sensor changes by 31% and 44% respectively, and the color of the sensor can changes dynamically and reversibly from red to purple in the visible light spectrum. After 15,000 times of cyclic stretching, the performance of the sensor remains stable. By using the stimulus response of sensor's color, the surface of the sensor can clearly shows the location and the shape of the strain source when the sensor is deformed. So the sensor can realize visualization effect during detection.
ZHOU Tian-zi , LYU Wei-zhong , ZHOU Qiao-ting , HUA Yue , HUANG Chun-bo , LI Liang-pu
2020, 37(8):0-0.
Abstract:Using graphene oxide powder (GO), vanadium pentoxide(V2O5), oxalic acid(C2H2O4·2H20) and ammonium tungstate((NH4)10H2(W2O7)6)as raw materials, tungsten-doped vanadium dioxide /graphene composite were prepared by hydrothermal method. The effects of W doping and graphene oxide on the phase transition temperature and thermal conductivity of the composites were investigated. XRD, SEM, DSC, FTIR, and laser thermal conductivity measuring instruments were used to characterize the structural morphology and phase transition properties of composites. The results show that the agglomeration of vanadium dioxide particles is effectively improved after graphene compounding, and is uniformly compounded on the surface of graphene. When the atomic percentage of tungsten is 2.5% and the content of graphene oxide composite is 4% (based on the quality of V2O5), compared with the pure vanadium dioxide, the phase transition temperature of the tungsten Doped Vanadium Dioxide / graphene composite decreased from 68 ℃ to 32.2 ℃, and the thermal conductivity was increased from 0.700 W/(m·K) to 16.341 W/(m·K). The composite material can meet the requirements of good thermal insulation and high thermal conductivity at the same time, and overcome the unity of opposites between thermal insulation and heat dissipation.
YV Biao , SUN Li-xia , XV Da-peng , ZHOU Li-qing , ZHANG You-quan , LIAO Dan-kui
2020, 37(8):0-0.
Abstract:Hafnium doped zinc oxide(Hf-ZnO) was prepared from tetrachloride hafnium (HfCl4) and zinc nitrate by hydrothermal method. Tyr/Hf-ZnO/CS/GCE was obtained by modifying tyrosinase (Tyr)、Hf-ZnO and chitosan (CS) onto Glassy carbon electrode (GCE). The structure and properties of the Hf-ZnO was characterized by FESEM, XRD, DLS and XPS. Electrochemical tests were conducted on the modified electrode Tyr/Hf-ZnO/CS/GCE by cyclic voltammetry (CV) and chronoamperometry (IT). The results showed that Tyr/Hf-ZnO/CS/GCE electrode had the best detection ability for catechol at a low potential of -50 mV and pH 5. The linear range of catechol detection was 0.5~47 μmol/L, the sensitivity was 195 μA/(mmol/L), and the detection limit was 0.1215 μmol/L(S/N=3). In addition, the biological electrode has good stability and repeatability, and can effectively avoid the electrical activities similar with catechol interference of urea, dopamine, and ascorbic acid.
TAN Yu , YAO Jin , ZHU Heping
2020, 37(8):0-0.
Abstract:A series of silicone rubber foam (SF)/hollow glass beads (HGB) composites were prepared by room temperature vulcanization. The effects of HGB content on the crosslinking density, cell structure, mechanical properties, dynamic thermomechanical properties of SF/HGB composites were studied. The results indicated that SF/HGB composite which prepared with 6.0 wt% HGB content had the optimal comprehensive performance. The cushioning properties of SF/HGB composites were investigated by the static compression test. The cushioning coefficient of SF/HGB composite was very close to polyethylene foam (EPE). Moreover, the fatigue properties of SF/HGB composites were investigated by the dynamic compressive fatigue test. SF/HGB composite exhibited long fatigue life (6.0 million times) and high height retention rate (98.4 %), which was far greater than those of EPE (0.29 million times, 54.5 %), and its cushioning coefficient was almost no changed before and after fatigue test, which was obviously superior to traditional cushioning materials EPE and could be used as a cushioning material in the packaging field.
Zhang Jun , hujiwen , guixuefeng
2020, 37(8):0-0.
Abstract:Liquid organosilicon is easy to produce "atomization" in the process of high-speed coating. Cross-linked organosilicon polydimethylsiloxane viscoelastic liquids was adopted as anti-fogging agent synthesized by and hydrogen-containing polysiloxane, and further studied the influence of the network structure on the anti-fogging efficiency. The gel rate of anti-fogging agent was affected by the molar ratio of n(C=C)∶n(Si-HSi—H) in polysiloxane. When the relative molecular mass of vinyl-terminated polydimethylsiloxane increased from 5759 g/mol to 33750 g/mol, the anti-fogging efficiency increased from 85.9% to 95.9%. When the hydrogen content of hydrogen-containing polysiloxane is 5.5 mmol/g, it is more conducive to the improvement of anti-fogging efficiency. These factors will affect the crosslinking network structure of anti-fogging agent, while low cross-linking density and orderly cross-linking structure will improve anti-fogging efficiency.
ZHOU Ping , WU Zhong-jun , HUANG Cai-huan , ZHANG Yanjie , ZHENG Jie
2020, 37(8):0-0.
Abstract:Anthocyanin is a flavonoid, widely found in various plant organs. It is not only an important water-soluble pigment in nature, but also has good biological activities such as antioxidant property, anticancer, disease prevention, etc., so it is widely used in food, pharmaceutical and cosmetic industries. The extraction and purification of anthocyanins from natural plants is a prerequisite for their application of anthocyanins. The latest research advances on extraction and purification of anthocyanins are reviewed. The effects of different extraction and purification methods on the extraction efficiency and purity are analyzed and compared. The review will provide reference for further research on anthocyanins and the realization of efficient extraction and high-value utilization of anthocyanins.
WANG Hong-wu , HE Jian-li , LIU Yan-qing
2020, 37(8):0-0.
Abstract:In order to ensure food safety and realize the rapid and sensitive detection of mequindox residue in food, carboxylated high purity single-walled carbon nanotubes were fixed on the surface of the gold electrode to construct a novel mequindox electrochemical sensor. Cyclic voltammetry (CV), differential pulse voltammetry (DPV) and electrochemical impedance (EIS) were used to investigate the performance of the sensor. The results showed that the performed sensor had remarkable catalytic performance on the electrochemical reduction of mequindox. The peak current of the modified electrode reached as 128.4 A, which was 1,160 times that of the bare gold electrode. The factors affecting the performance of the performed sensor were also optimized. The optimal conditions for the experiment were that the coated volume of cSWCNTs were 4 μL, the stirred speed was sat as 1000 rpm, and the performed electrode was enriched at 0.5 V in 0.2 mol/L PBS buffer (pH=7.0) for 30 min. Under the optimal experimental conditions, the peak current of the sensor had a good linear relationship with mequindox in the concentration range of 1.0~500.0 nmol/L, the correlation coefficient was 0.998, and the detection limit of the method was 0.76 nmol/L. The sensor was successfully applied to the actual sample detection with the standard recovery rate of 81.7%-124 %.
2020, 37(8).
Abstract:Low molecular weight polyethylenimine (PEI) was used as raw material, modified polyamines containing silica and hydrophobic were prepared by hydrophobic grafting of diglycidyl ether oxypropyl trimethoxy silane (KH560) 1-chlorooctane. The structure and properties of the modified polyamine scale inhibitor were analyzed by ir spectroscopy, the conclusions were drawn: the thermal stability, viscosity, surface tension and solution particle size of the modified products were improved. The modified polyamine scale inhibitor was used to disperse sodium aluminosilicate particles, the particles before and after treatment were characterized by infrared spectroscopy, and the dispersion performance of polyamine scale inhibitor was evaluated and its dispersion mechanism was preliminarily discussed by testing the stability and particle settling of the suspended dispersion solution. When the modified mass ratio was m(PEI(polyethylenimine MW=10000)):m(KH560(with -glycidyl ether oxypropyl trimethoxy silane)):m(1-chlorooctane)= 10:2:0.5, the reaction time was 6 h, and the reaction temperature was 75 ℃, the dispersion performance of the synthesized scale inhibitor was the best. When the mass concentration of scar is 30 g/L, the settlement rate of suspension particles reaches the lowest value of 0.047 /d, the settlement rate decreases to 94.8%, and the dispersion is significantly improved. The modified polyethylenimine has a highly effective effect of scale inhibition in the industrial production of alumina, which can be further replaced by the traditional strong acid scale inhibitor by optimizing the conditions in the factory, so as to reduce the degree of pipeline corrosion and reduce the energy consumption.
WANG Mian , CHEN Shuang , LIU Huie , NING Tengfei , YU Yunfei , LIU Yanru
2020, 37(8):0-0.
Abstract:The effects of three kinds of cosurfactants (n-butanol, isobutanol and sec-butanol) and their additions on the phase behavior of microemulsion were explored. In the microemulsion, fatty alcohol polyoxyethylene ether (AEO-9) was used as surfactant, NaCl as inorganic salt, octane and diesel as oil phase. It was found that with the increase of the addition of cosurfactants, the phase behavior of the microemulsion system changed from Winsor I through Winsor III to Winsor II. In octane microemulsion systems, the maximum volume fractions of the microemulsion phase were 91.63%, 80%, and 65.49% corresponding to n-butanol, isobutanol and sec-butanol respectively. Similarly, in diesel microemulsion systems, the maximum volume fractions of the microemulsion phase were 68.42%, 68.29%, and 63.33%, respectively, which suggesting that these three kinds of cosurfactants microemulsion systems have better solubilization properties for octane. The formulations of Winsor I and Winsor III microemulsion were screened out for each cosurfactant and oil phase by alcohol scanning experiments, and the effect of oil/water ratio on the phase behavior was explored. It was found that with the increase of the oil/water ratio, the final phase type of microemulsion was Winsor I. The microemulsion system which was initial Winsor Ш needed lager oil/water ratio to change into Winsor I microemulsion.
LIU XIAO-fei , SONG JIE , MA JING-qiu , HOU YAN , ZHENG ZHI-hui
2020, 37(8).
Abstract:A strain that has the ability to degrade cellulose was selected from the cold region and black glebe, and the morphological characteristics of the strain were observed and molecular biological identification was carried out. The response surface method was used to optimize the conditions for the degradation of corn stalk by this strain, and the structural changes and the main component changes of corn stalk before and after degradation were observed and determined. The results showed that the strain number was GS-4-21, and the ratio (D/d) of the transparent circle of the colony diameter was 5.54 ± 0.20. The enzyme activities of filter paper, exocellulase, endocellulase and β-glycosidase were 11.94±0.51, 12.07±0.43, 32.94±0.83 and 30.87±1.04 U/mL, respectively. The identified strain GS-4-21 belongs to the genus Streptomyces. When inoculated into the fermentation medium with pH 6 at a volume fraction of 3% and fermented at 28 ℃ and 160 r/min for 5 d, the degradation rate of corn stover reached 23.54%. SEM results show that the strain GS-4-21 had better cellulose degradation ability. The degradation rates of cellulose, hemicellulose and lignin in corn stover were 30.33%, 31.95% and 18.91%, respectively.
WU Huachu , ZHANG Hongbo , CEN Lian , YU Fengbin
2020, 37(8):0-0.
Abstract:In order to study the degree of reconstruction of irregularly shaped bone defect models using 3D printing technology and the effect of 3D printed degradable biomaterials on the repair of vertebral bone defects in three months. Biodegradable biomaterials, polycaprolactone (PCL) were used as the printing ink to print scaffold materials for repair. An irregular three-dimensional spine defect model was constructed using CT data from a randomly chosen patient. An artificial bone scaffold with a height that matches the patient's bone defect was first printed using 3D printing. At the same time, a rabbit spinal defect model was established, and a defect-sized stent was transplanted into the rabbit using 3D printing technology. The defect was removed from the rabbit after 3 months of surgery and sections of the defect area were made for Hematoxylin and Eosin (H&E) staining. The repair indicated that 3D printed bone scaffold has a promising application on the treatment of irregular bone defects formed during spinal surgery.
WANG Weilin , LI Zhong , ZHENG Huayan
2020, 37(8).
Abstract:This paper systematically investigates the influence of azeotropic solvent and reflux ratio on separation efficiency of DMC-CH3OH mixture after azeotropic distillation with various solvents: n-C7H16, n-C6H14, C6H12 (hexamethylene), CH2ClCH2Cl, CCl4 and C6H6, respectively. It is experimentally proved that azeotropic distillation method is highly efficient for the separation of DMC-CH3OH mixture. The results indicate that the composition of residue can be effectively regulated by modifying azeotropic solvent and reflux ratio. For azeotropic solvents investigated, the optimal reflux ratios are 7:1 or 8:1, which can lead to higher separation efficiency for DMC-CH3OH mixture. Moreover, at the same reflux ratio (7:1), the content and yield of DMC after azeotropic distillation are dependent on different solvents as the following order: CH2ClCH2Cl > CCl4 > C6H12 > C6H6 > n-C6H14 > n-C7H16.
SUN Yue , HUO Xinyu , WANG Zhaoxu , HAN Xiaoqiang , ZHANG Jie
2020, 37(8).
Abstract:In order to find novel pesticide leading compound with high bioactivity, ten bis-β-carboline derivatives linked by benzimidazole were synthesized starting from ethyl 1-substituted-β-carboline-3- carboxylate via alkylation, oxidation, and condensation. The structure of all novel compounds was confirmed by 1H NMR, 13C NMR and HRMS. Their antifungal activities were evaluated in vitro against five phytopathogenic fungi (Cotton Fusarium, Rhizoctonia solani, Sunflower sclerotinia, Rape sclerotinia, and Botrytis cinerea) using myvelium growth rate method. The preliminary results showed that most of the compounds possessed some fungicidal activity to five phytopathogenic fungi at 50 mg/L. These compounds have exhibited a significant inhibitory effect against sunflower sclerotinia rot in which compounds Ⅴb, and Ⅴi had inhibitory rates of 100%, and 92.4%, respectively. The information obtained from the studies may be useful for the design of novel agricultural fungicides.
ZHAO Peng-da , NI Shanmei , ZHOU Zhuoqiang
2020, 37(8):0-0.
Abstract:A copper-catalyzed visible light induced difluoroalkylation reaction of 8-aminoquinoline derivatives at the C5- position was developed at room temperature. The C—C coupling reaction between 8-aminoquinoline derivatives and free radicals of ethyl difluoroacetate produced by ethyl difluorobromoacetate was carried out with blue LED as light source, fac-Tris[2-(2-pyridinyl)phenyl] iridium(Ⅲ) complexes (fac-Ir(ppy)3) as photosensitizer. Fifteen difluoroalkylated 8-aminoquinoline derivatives (Ⅲa~Ⅲo) at the C5 position were synthesized in the presence of a catalytic amount of cuprous iodide. These products were characterized by 1HNMR, 13HNMR, FTIR, and HR-MS. The conversion rates of starting materials were50%~90%, and yields of products was in the range from 21% to 58%. The reaction conditions are mild, and the substrates containing halogen, thioether, and cyan functional groups can react. Free radical scavenger2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO) could capture free radicals of ethyl difluoroacetate, indicating that the reaction process may undergo free radical single electron transfer.
LIU Pei-ying , GE Yuan-yuan , LI Zhi-li , CUI Xue-min
2020, 37(8).
Abstract:A metakaolin-based geopolymer microsphere (GM) was prepared from metakaolin and modified water glass by a dispersion suspension and solidification method. The morphology of the GM was characterized by SEM, XRD, FTIR and BET studies. Its adsorption performance and mechanism of GM towords Methylene blue (MB) were studied. The results showed that the adsorption process of MB onto GM could be described by the pseudo-first-order model and Langmuir adsorption isotherm model. The maximum theoretical adsorption capacity of MB onto GM was 100.1 mg/g. The adsorption process of MB by GM was a spontaneous and endothermic process. Furthermore, after using GM for 5 cycles, the removal rate of MB by GM can still reach 81.56%, which is easy to recycle and regenerate. GM had strong selective adsorption ability to cationic dyes, by comparing adsorption ability of cationic and anionic dyes. The GM was low-cost, efficient, green and sustainable adsorbents for removal of cationic dyes in water.
2020, 37(8).
Abstract:A composite filter-loss reducer, P(ST-g-ACA)/BT, was prepared with corn starch, acrylamide, 2-acrylamido-2-methylpropanesulfonic acid, diallyl dimethyl ammonium chloride and bentonite by monomer intercalation. The filter-loss reducer was characterized with FTIR, XRD , TGA and TEM, the rheological properties and filtration loss of the filter-loss reducer were evaluated. In addition, the mechanism of fluid loss was presented. The results indicated that the filter-loss reducer possessed a “egg coil ” structure and a good thermal stability. Evaluation of P(ST-g-ACA)/BT in a water base drilling fluid showed that, at 2% (mass fraction) concentration of P(ST-g-ACA)/BT, the filter loss of the fresh water-based drilling fluid is 4 mL(normal temperature and medium pressure). The HTHP filter loss of the 10% salt water-based drilling fluid is 22 mL (150 ℃、3.5 MPa). Evaluation results showed that the filter-loss reducer could improve the properties of the thermal stability, salt tolerance, and fluid loss control of water-based drilling fluids. In the 10% salt water-based drilling fluid, the P(ST-g-ACA)/BT is better than other filter-loss reducers in filtration control.
2020, 37(8).
Abstract:Silicon-containing polyurethane pre-polymer (IPDI-Si) was prepared from γ-mercaptopropyltriethoxysilane (TMPS), isophorone diisocyanate (IPDI) and hydroxyethyl methacrylate (HEMA). Then, a series of silicon-containing polyurethane modified acrylic resins with different additive amount of IPDI-Si were prepared with isopropyl alcohol (IPA) as solvent and 2,2'-azobis(2-methylpropionitrile) (AIBN) as initiator. Finally, a series of waterborne acrylic resin dispersions were prepared by emulsification with triethylamine as neutralizer in the presence of water. The dispersions and cured resin coatings were characterized by FTIR, XPS, TGA, TEM and SEM. And the storage stability of the dispersion, and the hardness, adhesion and other properties of the coatings were tested. The results showed that when the additive amount of IPDI-Si was 3% (based on the total mass of polymerized monomers, the same below), the prepared dispersion had better storage stability and excellent resin coating performance. The prepared coating exhibited good compactness. The hardness was 2 H and the adhesion was grade 1. The water contact angle was 96.1 °. And the tensile strength of the coating was 9.4 MPa and the elongation at break reached 385%. The thermogravimetric analysis demonstrated that the temperature at 10% weight loss (T10%) of the coating reached 306.1 ℃
QUAN Hai-yuan , WANG zhi-nan , WU Chang-cai , MEI Xiang-dong , NIN Jun , SHE Dong-mei
2020, 37(8).
Abstract:13C1-N-Acetylimidazole (—CO13CH3) was synthesized by reacting 2-13C1-acetic acid with N,N'-carbonyldiimidazole, and then reacted with p-aminophenol to obtain 13C1-paracetamol (—CO13CH3). The influences of factors such as temperature and reaction time on the yield of products were investigated. The results showed that the optimal reaction temperature and time for the product synthesis were 40 ℃ and 12 h, respectively. The product was characterized by GC-MS, FTIR, 1HNMR and 13CNMR. The results showed that paracetamol contained one 13C atoms. The chemical purity was better than 99% and 13C enrichment was more than 98.7 atom%. The yield of product was 87%. Synthetic product can be used as an isotope internal standard in quantitative analysis testing.