• Volume 34,Issue 2,2017 Table of Contents
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    • >Catalysis,separation and purification technology
    • Oxidation of benzyl alcohol to Benzaldehyde Catalyzed by V/Mo-HMS

      2017, 34(2).

      Abstract (435) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:ammonium metavanadate, phosphomolybdic acid as active component were used to HMS mesoporous materials by sol-gel method to obtain V/Mo-HMS catalysts, and the modified catalysts were characterized by X-ray differential(XRD), scanning electron microscopy(SEM), N2 adsorption- desorption(BET), H2 temperature-programmed reduction (H2-TPR), X-ray photoelectron spectroscopy (XPS), thermal analysis(TG-DTA). The catalytic performance the V/Mo-HMS was investigated in the oxidation of benzyl alcohol to benzaldehyde using aqueous hydrogen peroxide(mass fraction 30% H2O2) as oxidant and the effect of HMS modified by various matal on catalytic oxidation reaction was tested. The results indicated that the specific surface area, pore volume and mean pore size of V/Mo-HMS were decreased Compared with HMS. The catalytic activity of V/Mo-HMS was better than the HMS modified by other matals. Conversion rate of benzyl alcohol reached 68.16 % with the selectivity of 89.02% to benzaldehyde when benzyl alcohol was 0.1mol, 30% H2O2 was 0.8 mol, catalyst amount was 0.07 g at 90 ℃ for 6h and ethyl acetate as solvent. The catalyst can be recycled and reused.

    • >Functional materials
    • Synthesis of MCM - 41 of Mesoporous Carbon Materials and Electrochemical Performance

      2017, 34(2).

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      Abstract:In this paper, a highly ordered mesoporous carbon material was synthesized by a soft template method with sixteen alkyl three methyl ammonium bromide (CTAB) as the template and soluble starch (Starch) as the carbon source. The structures of ordered mesoporous carbon were characterized by thermal gravimetric analysis (TG), X-ray diffraction (XRD), N2 adsorption desorption and transmission electron microscopy (TEM). The results show that MCM-41 ordered mesoporous carbon materials was got when the mass ratio of template and soluble starch was 1 to 1.5, carbonized for 3 h at 650 oC and removing the silica with hydrofluoric acid . The BET surface area of MCM-41 mesoporous porous carbon materials (OMC-650) was 985 m2/g with uniform and abundant mesoporous structure with pore size (2.5 nm). XRD and TEM analysis show that OMC-650 has typical MCM-41 structure with good order. These merits lead to a big specific capacitance (150 F•g-1) using OMC-650 as work electrode materials , mercuric oxide as reference electrode and platinum as auxiliary electrode with 6 mol.L-1 KOH as the electrolyte. After 1000 cycles, the specific capacitance of OMC-650 is 138 F/g with capacitance retention of 92 % and an excellent cycling stability in 6 mol•L-1 KOH aqueous electrolytes.

    • Research on NaHCO3 superfine powder processed by using impact mill

      2017, 34(2).

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      Abstract:The sodium bicarbonate (NaHCO3) superfine powder was grinded by using LNI-180A impact mill. NaHCO3 powder particle size, specific surface area, power consumption and the characteristics of morphology were discussed under different classifier speed. The results showed that with the classifier speed decreased from 1 050 r/min to 540 r/min, the superfine powder size decreased from d90=45.630 μm to 13.090 μm, the specific surface area turned from 0.86 m2/g to 1.83 m2/g, the yield was reduced to 65%, whereas energy consumption was decreased by 2.6 times. Combined with particle size and energy consumption, the optimal classifier speed of LNI-180A impact mill is 750 r/min for sodium bicarbonate powder, in this parameter, the output size d90 is 24.950 μm, specific surface area is 0.94 m2/g, unit power consumption is 70.66 kW•h/t. The grinded NaHCO3 powders were taken lamellar or porous structure, the particles sizes and distributions are uniform, which has favorable dispersibility, and better using as a fire extinguishing and desulfurization material.

    • Synthesis and Properties of P(AA/AM/APEG)/nano-SiO2 Composite High Absorbent Resin

      2017, 34(2).

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      Abstract:P(AA/AM/APEG)/nano-SiO2 as an efficient inorganic/organic super absorbent polymer composite was synthesized by a aqueous solution polymerization method with acrylic acid (AA) , acrylamide (AM), allyl polyoxyethylene ether (APEG) as monomers, and added to nano-SiO2, with ammonium persulfate(APS) as initiator, N,N'-Methylene bisacrylamide(MBA) as crosslinking agent. The impact factors of synthesizing superabsorbent resin, such as the amount of initiator, crosslinking agent and nano-SiO2, were discussed. Fourier Transform Infrared Spectrometer (FTIR) and Scanning electron microscopy (SEM) was performed to demonstrate the physical characterization. The results showed that the resin particle size had a great influence on the water absorbent rate and the temperature had little effect on resin absorbent rate; when the particle size was 80 ~ 120 mesh, the resin showed the best water absorbency of 1860 g/g; The pH of the solution had a great influence on the water absorbent rate of resin, when the pH was 6 ~ 8, samples exerted the best performance on water absorbency; Besides, super absorbent polymer prepared in this report also had a good performance of water retention capacity. Fourier Transform Infrared Spectrometer (FTIR) and Scanning electron microscopy (SEM) showed that the nano-SiO2 successfully grafted to the polymer and spongy structure was formed.

    • Changes of Surface Morphology of Star-like SEBS Block Copolymers Aggregate Studied by Atomic Force Microscopy

      2017, 34(2).

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      Abstract:The morphologies of films spin coated from star-like poly(styrene-b-ethylene/butylene-b-styrene) triblock copolymer (SEBS)/toluene solution onto a mica substrate were studied by atomic force microscopy (AFM). The results showed that the solution concentration determined the morphology of the aggregates, which displayed from single coil, spheres, network structure and continuous film with the increasing concentration. The size of aggregates could be influenced by the solubility of the solvent. With the increase of the solubility, the solvent could easily penetrate into the macromolecules, which resulted in the height of the aggregates on the surface of the film decreasing. The size of the aggregates could evolve to perfect spheres with heat treatment temperature. A lot of bubbles and pores could be observed at the morphology from the film spin coated immediately after ultrasonic treatment. Comparing the AFM patterns of linear SEBS (L-SEBS) with star-like SEBS (S-SEBS) under the same conditions, it was found that the size of aggregates of L-SEBS was smaller and the morphology was more difficult to change due to the steric hindrance and poor mobility of molecule chains of S-SEBS.

    • Preparation and Flame Retardant Performance of DOPOHM/Acrylic Resin Composites

      2017, 34(2).

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      Abstract:In this paper, The flame retardant 2-hydroxyethyl-2-methyl-3-(6-oxido-6H-dibenzo[c,e][1,2]oxaph-osphinin-6-yl)propanoate(DOPOHM) was prepared by 9-Oxa-10-phospha-phenanthr-ene 10-oxide(DOPO),and the flame retardant composites was prepared using acrylate resin(AR) as matrix and DOPOHM as the flame retardant. The thermal stability and flame retardancy of composites was characterized by TGA and Limit Oxygen Index(LOI), and flame retardancy mechanism was studied by SEM, XPS and EDS. The decomposition activation energy(Ea) of composites was calculated by Horowitz-Metzger theory. The result show that Ea of DOPOHM/AR composites improved as DOPOHM content increased. The DOPOHM exertinhibited effect on thermal degradation of polymer chain, and catalyze matrix formed dense char layer covering the surface of composites to be barrier to prevent heat and decomposition products escaped. The LOI of materials is found to be 26 and class V-0 of UL-94 test is passed when DOPOHM content is 25 wt%.

    • Effect on The Properties of Waterborne Polyurethane Emulsion Modified by Hydrophobic Chain Extension Agent Complex

      2017, 34(2).

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      Abstract:In this paper,the modified waterborne Polyurethane emulsion(E-WPU) was synthesized based acetone on self-emulsified process by using of Polybutylene adipate(PBA),isophorone diisocyanate(IPDI) and dimethylol propionic acid (DMPA) as the main raw material, hydrophobic chain extension agent epoxy resin (E44),1,4-cyclohexane dimethyl (CHDM) and isophorone ketone diamine (IPDA) as modifier.Modified and unmodified emulsion coating properties were characterized by the FT-IR,Tg,,adhesion,hardness and Tafel polarization curves.The results showed that using of E44,IPDA and CHDM had significantly improved the water resistance,hardness and adhesion on the metal of the E-WPU coating.When the mass fraction of E44,CHDM and IPDA were respectively 7%,2% and 3% in the prepolymer,and the molar ratio of the —NCO and the active hydrogen of the —OH/—NH/—NH2 group in the prepolymer (R) was 1.2,the coating had the best comprehensive performance.The water absorption rate,the hardness and the adhesion on metal surface were respectively 3.5%,HB-H and grade zero.The corrosion potential of E-WPU coating was -0.6608v,and the corrosion current density was 9.778e-7 A/cm2.

    • The Synthesis of Large Hexagonal Boron Nitride Particles using Triethanolamine Borate as Precursor

      2017, 34(2):0-0.

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      Abstract:The triethanolamine borate was synthesized by triethanolamine reacting with boric acid and using toluene as water carrying agent. The h-BN particles were prepared by sintering triethanolamine borate as precursor in ammonia gas atmosphere. The precursor and product were respectively characterized by IR, XRD, SEM and NMR analyses. The results indicated that the precursor is treated at 1200℃ for 4h to receive high purity and good crystals of h-BN particles with a average particle size of 20μm. After high-temperature refining of h-BN particles with high crystallinity and compactness, the particle size can reach more than 30μm and 98.5% purity can be obtained.

    • >Surfactants
    • Effect of Alginate Derivative on the behavior of Water Emulsion on Target Surface

      2017, 34(2).

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      Abstract:Abstract:Effect of cholesteryl grafted sodium alginate derivative (CSAD) on wettability and deposition capacity of lambda-cyhalothrin in water emulsion on the banana leaf surface was investigated in terms of dynamic and static surface tension, contact angle, retention and pesticide adsorption capacity by the inverse emulsion method, which was adopted to prepare the lambda-cyhalothrin in water emulsion by alkyl indican (APG) as the emulsifie. The results showed that both the CSAD+APG system and the APG system stable water emulsion had a similar critical micelle concentration(i.e., 0.1 g/L of CAPG). In addition, for the two systems as the CAPG was equal to 0.1 g/L, the maximum retention capacity on leaves was 0.0104 and 0.00778 g/cm2, the adhesion tension was 24.32 and 16.14 mN/m and the adhesion work was 55.23 and 46.47 mN/m, respectively. Furthermore, the CSAD+APG system showed a much higher pesticide adsorption capacity on leaves that was 524 μg/L, while the corresponding value of the APG system was only 412 μg/L. In general, the addition of the amphiphilic CSAD could effectively enhance the retention and adsorption capacity of water emulsion on banana leaves due to the formation of CSAD-APG complexes adsorbed at the solid-liquid interface.

    • Synthesis, Properties of Gemini Surfactants using Adamantane as Spacer Group

      2017, 34(2).

      Abstract (1041) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Three Gemini surfactants using adamantane as spacer group with different carbon chain length, nP-Ad-Pn (n=12, 14, 16), were synthesized from 1,3-adamantanedicarboxylic acid. The success of synthesis was confirmed by FT-IR spectra, 1H NMR spectra, and ESI-MS spectra. The surface-active properties, thermodynamic parameters and micropolarity of the Gemini surfactants containing adamantane were investigated through surface tension, electrical conductivity measurement and steady-state fluorescence. The results show that the values of CMC are 6?0-4, 1?0-4 and 2.5?0-5 mol?L-1 respectively. the standard Gibbs free energy change (?G0m) and the standard enthalpy changes (?H0m) are negative, indicating that the micellization is spontaneous and exothermic. Further, the antimicrobial activity of the synthesized compounds against S. aureus, B. subtilis, E. coli, P. aeruginosa, V. Parahemolyticus was also investigated, and this study showed that the MIC of 12P-Ad-P12 was between 0.2 mg/L and 4.2 mg/L, which showed that this compounds have excellent antibacterial activity against five studied bacteria.

    • Synthesis and Performance of Sulfonic Gemini Surfactant

      2017, 34(2).

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      Abstract:Sulfonic gemini surfactant 1,6 -bis (N-dodecyl-N-propane sulfonate sodium)-hexane (12-6-12(SO3)2) was prepared with dodecylamine, 1,6-dibromohexane and 1,3-dibromopropane as starting materials by the polar head group joining method and the spacer joining method.The structure of the intermediates and final product was characterized, and the surface activity of the final product was measured.The structures of intermediates and target products were confirmed with 1H NMR and ESI-MS. The performance results showed that the critical micellar concentration (CMC) of 12-6-12(SO3)2 at 30oC is 0.015 mmol/L and its surface tension is 33.50 mN/m. The CMC of 12-6-12(SO3)2 is only 0.002 times of the similar sulfonic salt surfactant of SDS (25oC, 8.0 mmol/L), and it is of about 0.31 times of the similar sulfonic gemini surfactant 1,3 -bis (N-dodecyl-N-propane sulfonate sodium)-propane (12-3-12(SO3)2)(25oC, 0.048 mmol/L).

    • >Catalysis,separation and purification technology
    • Study on the operating parameters of total caffeoylquinic acid ester of Erigeron multiradiatus with macroporous resins

      2017, 34(2).

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      Abstract:Abstract: Thirteen microporous resins with different polarity were evaluated for the adsorption properties of the total caffeoylquinic acid ester(TCaf) from Erigeron multiradiatus. Macroporous resin NKA-2 with strong polarity displayed the best adsorption capacity among the tested resins. The static adsorption and dynamic adsorption test of NKA-2 for TCaf from Erigeron multiradiatus were investigated.The results show that the optimal purification parameters were sample concentration of 300 g/L,the loaded amount of 6 mL/g,and loaded flow rate of 2 BV/h. By analyzing the TCaf from Erigeron multiradiatus washed out from the resin,it was shown that the desorption effect of 60% ethanol of 8 BV was the best.The purity of TCaf increased to 58.06% after the purification,and the yield was 94.78%.NKA-2 is an ideal resin with the best enrichment efficiency for the TCaf of Erigeron multiradiatus.

    • Performance of Anodic Pd-Ni/C Catalyst Prepared by Reduction

      2017, 34(2).

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      Abstract:Three types of alkaline fuel cell catalysts(Pd2Ni3/C、PdcoreNishell/C、NicorePdshell/C) with different structures have been prepared by reduction, using pretreated active carbon as the support, CeO2 as the decorator and NaBH4 as the reducing agent. According to physical characterization and electrochemistry test, NicorePdshell/C catalyst has better catalytic oxidation activity of ethanol and stability under the alkaline medium. The highest current density was 160mA穋m-2 in NicorePdshell/C with 100mV/s of sweep speed, and its stable current density was higher than Pd2Ni3/C and PdcoreNishell/C catalysts.

    • Synthesis and Metals-Modification of Cu-SSZ-13 Molecular Sieve and Its Catalytic Performance in MTO Reaction

      2017, 34(2):0-0.

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      Abstract:Cu-SSZ-13 was in situ hydrothermally synthesized using a template of a low-cost copper amine complex (Cu-TEPA). The effects of two copper salts and n(Na2O):n(Al2O3) on the crystal phase and morphological were studied, the catalyzation of methanol to olefins(MTO) of Cu-SSZ-13 prepared with two copper salts and metal cation modified Cu-SSZ-13 was tested. The catalysts were characterized by XRF, XRD, SEM, BET and NH3-TPD. The results show that alkalinity has a great influence on the crystallinity of Cu-SSZ-13, if the alkalinity was excessively high or low, zeolite analcime as an impurity or pure phase would be produced; During the reaction of MTO, hydrogen transfer reaction of Cu-SSZ-13 prepared with cupric nitrate is intense, the propane selectivity reached 40% in the early stage of the reaction, far higher than the 19% of Cu-SSZ-13 prepared with cupric sulfate. Cu-SSZ-13 modified with Mn exhibits a stronger ability in resisting pore blockage deactivation, under the reaction condition of reaction temperature 440℃ and WHSV 5h-1, its lifetime extended from 30minutes to 65minutes.

    • >Drug and cosmetic materials
    • Synthesis of 5-(thiophen-2-yl)-2-p-tolyloxazole

      2017, 34(2).

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      Abstract:5-(thiophen-2-yl)-2-p-tolyloxazole was synthesized via an oxidative cyclization reaction between 2-bromo-1-(thiophen-2-yl)-1-ethanone and p-tolylmethanamine in the presence of a catalyst amount of iodine and tert-butyl hydroperoxide (TBHP). The structure of the targeted product was confirmed by Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR) and mass spectroscopy (MS). The results indicated that the optimum synthetic conditions were determined as follows: the amount of 2-bromo-1-(thiophen-2-yl)-1-ethanone, p-tolylmethanamine, iodine, TBHP (mass fraction 55%) and sodium bicarbonate was 1 mmol, 1.3 mmol, 0.2 mmol, 1.2 mmol and 1.0 mmol, respectively, at room temperature for 12 h. The yield of the product reached 89.7 % under the above synthetic condition. The zone of inhibition showed that this compound exhibited a remarkable antibacterial activity against Escherichia coli.

    • >Water treatment technology and environmental protection
    • Study on Preparation of Pressed Active Carbon Based on Sewage Sludge and Fine Semi-coke and Properties of Adsorption

      2017, 34(2).

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      Abstract:A kind of pressed active carbon was prepared by H2SO4 and ZnCl2 complex activation method, using dehydrated sewage sludge and fine semi-coke as the raw materials. The following factors were considered such as pH, solid-to-liquid ratio and adsorption time in treating semi-coking wastewater which had been diluted 10 times. And then pressed active carbon was revived after adsorption. The single factor experiment and orthogonal experiments showed that the influencing factors of iodine sorption value by pressed active carbon were activation temperature, activation time and immersion ratio in turn. The optimum technological conditions were: the activation temperature was 750 ℃, the activation time was 2 h and the immersion ratio was 1:2.5 g/mL. The charring process of sewage sludge and fine semi-coke compound was made up of four steps, the first stage was adsorption water escape phase from room temperature to 200 ℃, while in the second stage between 200~338 ℃ sewage sludge released volatile matter such as CH4, CO2 and N2. Sewage sludge pyrolysized and formed semi-coke in the third stage from 338~642 ℃. Annaline decomposed and released sulfur dioxide exothermic peak at 640 ℃.The last stage semi-coke turned to coke and zinc chloride volatilized after 642 ℃. The pressed active carbon had the average hole diameter of 9 nm and specific area of 194 m2/g. Furthermore, the product contained alkane , arene, alcohol, hydroxybenzene and many other kinds of alkanes and oxygen containing functional groups.The results indicated that while in the condition of pH≈8, solid-to-liquid ratio was 1:30 g/mL and adsorption time was 32 h, the remove effect of ammonia nitrogen and chromaticity were best, which can reach to 83 % and 42 %.While after five times recondition,the iodine sorption value and compression strength of pressed active carbon reduced by 31 % and 62 % separately.

    • >Oil field chemicals and petroleum additives
    • Synthesis and Evaluation of Fluid Loss Additive for High Temperature Resistant and Salt Tolerant and Inhibitor Drilling Fluid

      2017, 34(2).

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      Abstract:In this paper, a new kind of salt resistance, high temperature resistance, strong inhibition of drilling fluid loss agent SN-K is prepared with monomers AA, AM, AMPS and DMDAAC by aqueous solution polymerization, and the initiator system are (NH4)2S2O8 and NaHSO3. The best monomer molar ratio is produced by single factor experimental method and the molar ratio is n(AM):n(AMPS):n(AA):n(DMDAAC)=1:2:2:1. In addition, the optimum reaction conditions as follows: the reaction temperature and time are 65 ℃ and 4 h, the mass concentration of monomer is 20%, the adding amount of initator is 0.5%, and then KOH solution is used to adjust the pH value of reaction system, at the same time, the strong inhibition ion K is also introduced. It was found that the drilling fluid have a good fluid loss effect after a pretreatment of high temperature 180 ℃ and 16 h, when the adding amount of drilling fluid loss agent SN-K is 1.5%, in a such condition, the FLAPI is 6.5 mL. And then, the scroll shale recovery experiment shows that cuttings recovery is higher than the system of KCl. Additionally, the micro structure of HTHP filter cake is conducted by scanning electron microscopy (SEM), the results shows that the HTHP filter cake have a dense grid structure.

    • Synthesis of Molybdate Ionic Liquide and Its Tribological Performance

      2017, 34(2).

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      Abstract:Metal-based room-temperature ionic liquid methyltri-n-octylammoniummolybdate ( [(CH3)N(n-C8H17)3]2MoO4 ) was synthesized with methyltri-n-octylammoniumchloride, sodium molybdate dihydrate and silver nitrate, and characterized by FT-IR, 1H NMR, API-ES-MS and elemental analysis, which have been extended to new families and generations of functionalized ILs. Its tribological performances as additive in base oil 400SN were examined on a four-ball tester. Adding 0.5% (mass concentration) molybdenum ionic liquid in base oil 400SN improved the PD value of base oil one lever, increased the PB value by 23.8% and dropped WSD by 34.6%. The tribofilm [(CH3)N(n-C8H17)3]2MoO4 generated on the worn surface was analyzed by scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS). The results showed that [(CH3)N(n-C8H17)3]2MoO4 blend oil exhibited excellent anti-wear ability and extreme-pressure performance, which could be attributed to tribo-chemically boundary films formed on the rubbing surface consist of MoOx and FeOx.

    • Synthesis of Polyaspartic Acid/O-carboxymethyl Chitosan Graft Copolymer and Its Scale Inhibition Performance for Barium Sulfate

      2017, 34(2).

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      Abstract:Polyaspartic acid/ O-carboxymethyl chitosan graft copolymer (denoted as PASP/O-CMC) was synthesized via the reaction of water soluble O-carboxymethyl chitosan (O-CMC) and polysuccinimide (PSI).The obtained graft copolymer (PASP/O-CMC) was characterized by FTIR and 1H NMR. The static scale inhibition method was used to evaluate the scale inhibition behavior of PASP/O-CMC and PASP against barium sulfate. The experimental results showed that PASP/O-CMC possessed the best scale inhibition property against BaSO4. Inhibition efficiency of PASP/O-CMC reached 93.6%, but that of PASP was only 78.4% when the dosage was 100 mg/L in the experiment. The scale inhibition mechanism of the scale inhibitor against BaSO4 was analyzed by means of environmental scanning electron microscopy (SEM), X-ray diffraction (XRD), and electrical conductivity measurement techniques. And it was found that the scale inhibition was mainly caused by lattice distortion of BaSO4, adsorption dispersion and complexation of the scale inhibitor and Ba2+.