• Volume 28,Issue 1,2011 Table of Contents
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    • >Review and monographs
    • Recent Advances in Enhanced Treatment Techniques for Tiny-polluted Raw Water

      2011, 28(1).

      Abstract (420) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:It was summarized that the research progress of treatment techniques for potable water production from tiny-polluted raw-water. Based on the status of polluted surface water in China, the development of techniques for tiny-polluted raw-water treatment like pre-treatment techniques, advanced techniques and enhanced coagulation, and so on, were reviewed on the basis of representative references. It was pointed out that among these treatment techniques for tiny-polluted raw-water, selecting effective coagulants for specific raw water under the existing equipment condition of potable water plant, could improve the produced water quality remarkably with lowest cost. And it was an economic method for tiny-polluted raw water treatment and becomes a hot topic of research work in the area of raw water treatment. Furthermore, Based on the wildly used coagulants in domestic industry and combined with the region and season characteristics of the raw water, the development of universal and special coagulants with high quality could improve the techniques of our country in tiny-polluted raw-water treatment markedly and ensure the quality of potable water fundamentally.

    • >Functional materials
    • Study on Synthesis of XG-g-PAA Superabsorbent Resin by Inverse Suspension Method

      2011, 28(1).

      Abstract (928) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:Xanthan gum-g-acrylic superabsorbent resin was prepared by inverse polymerisation using acrylic acid as graft polymerization monomer,cyclohenxane as continuous phase ,N,N-methylene-bis-acrylamide as crosslinking agent and potassium persulfate as initiator. The influence factors of synthesising superabsorbent resin such as the weight ratio of acrylic acid and xanthan, amount of initiator(KPS), amount of crosslinking agent, degree of neutralization of acrylic acid and polymerization temperature were studied .Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and thermogravimetric analyzer(TGA) were used on characterization of the superabsorbent resin. The results showed that: The poly-acrylic acid molecules linked to the molecular chain of xanthan gum through graft co-polymerisation, the preparation of XG-g-PAA superabsorbent resin Under the optimum conditions has good properties of water absorption and salt resistance,the retention performance was inproved in high temperature, the highest water absorption up to 845g.g-1, 0.9% NaCl solution up to 96.3g.g-1,percent grafting up to 126.5%,grafting efficiency up to 82.6%.

    • Synthesizing and Characterizing Various Morphologies of PSt/PGMA Janus Particles

      2011, 28(1).

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      Abstract:The emulsion droplet solvent evaporation method has been used to prepared the PSt/PGMA monodisperse janus particles, as solvent DCM evaporated, the spherical droplets phase separated, resulting in janus morphology composite particles. The different janus morphology PSt/PGMA composite particles were prepared by controlling the molecular weights of PSt and PGMA. The effect of different type of the emulsifier and its concentration on the particles morphology were researched. Fluorescence microscopy observation and EDS energy dispersive spectrometer results confirmed that the large hemisphere mainly is PGMA, the small hemisphere mainly is PSt, the phase-separation process in these two polymer is not yet complete, with the molecular weight increased, PGMA tend to engulf PSt component.

    • Synthesis of high oil-absorption resins modified by organic bentonite with microwave irradiation

      2011, 28(1).

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      Abstract:Bentonite was organically modified with hexadecyl trimethyl ammonium Bromide(HDTMA-Br) by using microwave irradiation technique, high oil-absorption resins were synthesized with butyl acrylate (BA) and butyl methacrylate (BMA) as monomers. The effects of amount of dispersant, initiator, crosslinking agent and microwave power reaction time on oil absorption capacity of resins were studied. Chemical groups of the organic bentonite, thermal stability and morphologies of the resins were characterized respectively by using fourier transform infrared (FT-IR) , scanning electron microscopy (SEM) and thermogravimetric analyzer(TGA). In comparison with the traditional synthesis technique, microwave irradiation method can greatly shorten synthesis reaction time and decrease energy cost, organic bentonite can improve thermal stability of resin. The absorption of the resins to CHCl3 and gasoline could be 35g/g and 16g/g respectively.

    • Preparation and Characteristics of Paraffin Microcapsules

      2011, 28(1).

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      Abstract:Abstract: Microcapsules containing paraffin were prepared through the in-situ polymerization method using melamine-formaldehyde as wall material. The properties and morphology of the microcapsules were characterized by Fourier-transform infrared spectra (FT-IR), Scanning electronic microscope (SEM), Laser particle size analyzer and Differential scanning calorimeter (DSC). The effects of the molar ratio of formaldehyde to melamine (F/M) on morphology and properties of microencapsulated paraffin were investigated. The results showed that when the ratio of F/M was higher than 4, high degree of cross-linking melamine-formaldehyde resin was obtained and the visible agglomeration of the microcapsules was observed. The phase-transforming point of microcapsules was higher than paraffin, the latent heat of microcapsules decreased as the F/M molar ratio increased.

    • Hydrothermal preparation of CdSe and PbSe co-deposited TiO2 nanobelts

      2011, 28(1).

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      Abstract:CdSe or/and PbSe deposited TiO2 nanobelts were prepared using two-step hydrothermal preparation process. Various techniques including XRD, SEM, TEM, UV-Vis absorption and FTIR measurements were used to characterize a series of products. The results show that hexagonal CdSe particles with sphere-like or/and cubic PbSe particles with cube-like deposit on the surface of anatase TiO2 nanobelts, and the CdSe or PbSe particles are mainly with size in a wide range of 100-400 nm or 300-1000 nm, respectively. There is not any organic connection between particles and nanobelts. CdSe and PbSe co-deposited TiO2 nanobelts exihibit very strong absorption in visible-light main region. A fact that a little bit Cd2 or/and Pb2 ions have doped into TiO2 nanobelts for the composite products has been inferred by FTIR measurements.

    • Containing Samarium Metal Complexes Organic Synthesis and Fluorescence Properties

      2011, 28(1).

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      Abstract:a certain proportion of new solid quaternary complexes SmL*L2Phen(L*=MMA,L=SA) of europium adulterated by cheap non-fluorescence lanthanum with the ligands of the cheap and popular methylmethacrylate (MAA), Salicylic Acid(SA) and 1, 10- phenanthroline (Phen). The complexes were characterized by elementary analysis,X-diffraction analysis,FTIR, Electron microscopy and fluorescence analysis. The results show that:Properties of the product was discussed when the mixing amount of La varied. the best result was achieved when the proper amount of La can streng then the red light luminescence of Sm, which comes to the best when mixing amount reaches 70%(mole proportion) Furthermore, the most in fluorescence emission peak of this series of complexeswas at585 nm,616 nm, 662 nm, which was most closed to the photosynthesis spectra ofvegetables.

    • Study of Pervaporation Performance of PVA/P(AA-Co-AN)/ PVA Membrane

      2011, 28(1).

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      Abstract:The PVA/P(AA-Co-AN)/PVA composite membrane was prepared to separate methanol from aqueous solution. Acrylic acid (AA) and acrylonitrile (AN) were synthesized by solution polymerization with nanometer SiO2. The copolymer solution P(AA-Co-AN) was made into main body of the membrane, with the polyvinyl alcohol (PVA) acetal membrane on both sides, to make the composite pervaporation membrane. The swelling behavior of membrane in methanol dense aqueous solution was explored. The effect of dipping temperature and concentration on the swelling degrees was also measured. Mechanical property of the membrane was investigated by stretching test. The performances of the membranes prepared with different n(AA):n(AN) ratio were investigated through pervaporation experiments at different temperatures and different feed composition. The results of swelling and pervaporation experiments show the membrane has an encouraging swelling and pervaporation behavior in methanol dense aqueous solution. The membrane prepared with n(AA):n(AN)=1:1 gave the highest separation factor of 1534 and a permeation flux of 583 g/(m2•h) at 60℃ in pervaporation of w(methanol)=98% aqueous solution.

    • Effects of PVP and Titanate dispersants on stability of ITO suspension

      2011, 28(1).

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      Abstract:Colloidal dispersion of indium tin oxide (ITO) nanoparticles in an butyl acetate solvent was achieved using a milling process in which PVP and Titanate as dispersants. The effect of various parameters such as different PH value, dispersant dosage, zirconium oxide ball diameter and interfaces and milling time factors on dispersion stability was studied, and the dispersing mechanisms on stability of ITO suspension which about the two kinds of dispersant were investigated. The optimum conditions obtained from the tests were that when the PH value of 7.8, dispersant dosage relative to 5.5%, the size of ZrO2 beads is no more than 0.5mm and the quantity of beads was determined to be 2.6 times weight of ITO, shearing time was 24h. Compare with the two kinds of ITO dispersant slurry prepared in the storage time of 0 days and 30 days of the slurry particle size changes, the stability of the latter than the former

    • >Catalysis,separation and purification technology
    • Study on preparation of Cu/ZrO2 catalyst by high gravity co-precipitation method

      2011, 28(1).

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      Abstract:By the help of high gravity co-precipitation, with copper nitrate and zirconium oxychloride solution, using 20% sodium hydroxide as the precipitant, the Cu/ZrO2 catalyst was prepared, which was used for synthesis of iminodiacetic acid from diethanolamine via dehydrogenation. The optimal conditions were obtained by orthogonal experiments: high gravity reactor speed of 800r/min, precipitation end-point pH of 12, aging time of 5h, zirconium/copper atomic ratio of 2:1 and initial concentration of zirconium salt of 0.2mol/L. Under these optimal conditions, the catalyst precursor was roasted 5h at 500℃ and reduced 5h at 220~240℃ to obtain Cu/ZrO2 catalys. The catalyst using for the dehydrogenation effect of diethanolamine was investigated, the reaction yield of iminodiacetic acid sodium was 97.50%, selectivity can reach 98.05%. Via using repeatedly 5 times, the average reaction yield was 95.05%, and the one-way deactivation yield was 1%~2%. The results can be included that it has a relatively stable catalytic activity and long catalytic life. Compared with traditional co-precipitation method, the catalytic performance of the catalyst was better under laboratory test conditions.

    • Baeyer-Villiger oxidation of ketones catalyzed by PEG6000-OSO3H

      2011, 28(1).

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      Abstract:PEG6000-OSO3H was prepared and was characterized by FT-IR, TG and element analysis. Baeyer-Villiger oxidation of ketones catalyzed by PEG6000-OSO3H with 30%H2O2 as oxidant was studied. The influences of the solvents, the reaction time, the temperature, the dosage of catalyst and the oxidant on the catalytic activity are well investigated. The optimizing conditions were concluded as: 0.1mmol of ketones could be well oxidized with 3.0eq of 30 %H2O2 catalyzed by 10 mg of PEG6000-OSO3H in 3mL of acetonitrile at 70 oC for 24 hours. Under the optimum condition, a series of cyclic ketones such as 2-adamantanone, cyclopentanone, cyclohexanone, 2-methylcyclohexanone, 4-methylcyclohexanone and 4-tert-butylcyclohexanone were well transformed into the corresponding lactones with the conversion of 89%~100% and the selectivity of 89%~99%, respectively. Some of the products of lactones from the oxidations were purified by a silica gel column and characterized by 1H NMR and 13C NMR spectra.

    • The Isomers Separation Methods of Paeoniflorin and Albiflorin by Three-zones SMB

      2011, 28(1).

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      Abstract:The isomers separation process of high concentration paeoniflorin and albiflorin by three-zones SMB.was described. The working parameters of SMB were set as follows. Mode: 1-1-2; injection concentration: 40 mg/mL; flow rate of injection : 0.3mL/min; flow rate of elution: 2mL/min; flow rate of extract: 4mL/min; switch time: 25min; mobile phase: methanol∶water(V/V)=30∶70. The paeoniflorin concentration in extraction is 92% by standard curve method, and recovery is 85%; the albiflorin concentration in raffinate is 94%, and recovery is 87%; Simultaneously, the main factors which affect the separation process in SMBC were discussed.

    • >Drug and cosmetic materials
    • Preparation of Liposomes containing Vitamin C and Salicylic Acid

      2011, 28(1).

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      Abstract:Abstract: The liposomes containing both water-soluble vitamin c and fat-soluble salicylic acid were prepared with soya lecithin by multiple emulsion and ultrasound method. Factors including the proportion of components in liposomes,the pH of vitamin c solution, emulsifying temperature and coating on the encapsulation efficiency and stability of liposomes were studied. The results show that the conditions for preparation of liposomes were m(soya lecithin)∶m(cholesterol)∶m(salicylic acid)∶m(vitamin c) =4∶1∶0.75∶1, pH of vitamin c solution at 5,emulsifying temperature of 25℃and 45℃for the first and second step respectively. In this case, the entrapment efficiency of the prepared liposomes were 48.2% and 55.4%. The coating could enhance the stability of liposomes.

    • >Water treatment technology and environmental protection
    • Structure and application of ferrous – modified polyaluminium chloride

      2011, 28(1).

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      Abstract:Abstract: Taking waste liquor from steel-cleaning in hydrochloric acid and aluminum chloride as raw materials, A series of ferrous-modified polyaluminium chloride(Fe2 -PAC) were prepared firstly. Comprehensive analyses by FTIR ,X-ray diffraction and Electron-microscope, the results Indicated that Fe2 and PAC were not simply mixed, but has had certain interaction, its aggregate was stubby ,compacted, uniform, and large sized; The size distribution of Fe2 -PAC indicate that it was a high molecular coagulant; The coagulation experiment for treatment of paper wastewater proved that it is a new kind of highly efficient purifying agent.

    • >Building chemicals
    • Preparation and Performance of Protein-Concrete Foaming Agent from Rapeseed Meal

      2011, 28(1).

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      Abstract:Protein concrete foaming agent was prepared by adding a certain amount of different surfactants to the base fluids of rapeseed proteins which were extracted by sodium hydroxide, ethanol and ammonium sulfate aqueous solution from rapeseed meal as the raw material, and mixed with distilled water at the volume rate of 2:1. Combination scheme was optimized by determining the foaming height and time for foam stabilization of the compounded systems, and surface tensions and viscosities of the systems with optimal foam properties before and after combination were also determined. Results showed that if 3.0 g/L SDS, 0.5 g/L CTAB and 2.0 g/L SDBS(w/v, g/mL)were added to the protein solution extracted by ethanol the synergistic effect exhibited significantly, when the foaming height was 110mm and the time for foam stabilization was 47h. Its surface tension decreased to 25.75mN/m after combination from 43.47mN/m, and its viscosity increased to 4.50mPa.s from 4.20mPa.s. Some properties of the modified foaming agent, such as the foaming ability and the stability of foam, were significantly improved as compared with some commercial foaming agents.

    • >Fine chemical intermediates
    • The synthesis of Propylene carbonate methacrylate

      2011, 28(1).

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      Abstract:Propylene carbonate methacrylate(PCMA) was synthesized by using glycidyl methacrylate(GMA) as the raw material. The structure of PCMA was characterized by IR spectra,1HNMR and element analysis.The effects of catalysts, reaction temperature, atmospheric pressure and reaction time on the fractional conversion of the epoxy groups were discussed in detail. The results showed that when the TBAC and TBAB are used as the co-catalysts, tertiary butylhydroquinone as the inhibitor, with m(TBAC):m(TBAB):m(TBHQ):m(GMA)=1:1:1:200;the reaction temperature and time is 85℃ and 15h respectively,and the carbon dioxide pressure is 1.2MPa, the yield can be reached at 63.3%.

    • Synthesis of An Anti-UV Intermediate 1,3-Dimethoxy-2-Nitrobenzene

      2011, 28(1).

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      Abstract:2-Nitrobenzene-1,3-diol was obtained through a series of physical and chemical processes containing sulfonation, nitration, and hydrolysis etc. and treated with dimethyl sulfate to give an anti-UV intermediate. It has been shown by investigating various technologic conditions mentioned above that resorcinol can be completely two-sulfonated and finally resulting in 2-nitrobenzene-1,3-diol with yield of 63.5% and contents over 99.7% when 20% oleum used as sulfonation reagents and 1,3-dimethoxy-2-nitrobenzene can also be obtained with 75.6% by treating 2-nitrobenzene-1,3-diol with dimethyl sulfate at 80 ℃ for 4 h as the molar ratio of dimethyl sulfate to 2-nitrobenzene-1,3-diol is 2.2 : 1.0.

    • Catalytic Oxidation of toluene to benzaldehyde over Keggin-type heteropoly Compounds

      2011, 28(1).

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      Abstract:Oxidation of toluene to benzaldehyde catalyzed by Keggin-type heteropoly compound Co3H2PV2Mo10O40 using TBHP(tert-butyl hydrogen peroxide) as oxidant and acetonitrile as solvent was investigated. Using infrared spectroscopy(IR),X-ray diffraction (XRD) were used to characterize the catalysts. Experiments showed that reaction temperature 90℃ and reaction time 6h, the conversion of toluene was 28.50% and the selectivity of benzaldehyde was 55.50%.

    • Catalytic Synthesis of Methoxy Polyethylene Glycol Methacrylate with PW12/SiO2

      2011, 28(1).

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      Abstract:Methoxy polyethylene glycol methacrylate-styrene polymer was synthesised with phosphotungstic acid supported on silica(PW12/SiO2),this catalyst was prepared by putting tungstophosphoric acid into the three dimensional structure of silica. The optimized condition for the esterification were determined with orthogonal experiments as:molar ratio of methoxy polyethylene glycol to methacrylic acid was 1:3,amount of catalyst was 1%,amount of inhibitor was 1%,reaction time was 10h, the esterification rate could reach to 93.6% and the yied was up to 83.46%.Under high loading amount, phosphotungstic acid has a great degree of dispersion on silica,and without surface packing of bulk phosphotungstic acid.The catalyst has a low desorption on the reaction and still has a excellent catalytic effect after using many times.

    • Synthesis and Structural Characterization Of N-[(4-bromo-3,5-difluorine)-phenyl]maleimide

      2011, 28(1).

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      Abstract:The N-[(4-bromo-3,5-difluorine)-phenyl]maleimide was synthesized with maleic anhydride and 4-bromo-3,5-difluoroaniline via the solvent azeotropic method, using p-toluene sulfonic acid as the catalyst and toluene / DMF as the mixed solvent. The chemical structure of product was confirmed by means of FTIR, 1HNMR and 13HNMR methods. The synthesis process was optimized, and the suitable conditions were found as follows( based on 38.6 mmol 4-bromo-3,5- difluoroaniline),amount of p-toluene sulfonic acid 0.8778 g, n(maleic anhydride) : n(4-bromo-3,5- difluoroaniline) = 1.2, amine reaction time 1.5 h, cyclization reaction time 2 h, with a yield of 92.6 %.

    • Study of catalytic oxidation of cyclohexane over Cu2P2O7

      2011, 28(1).

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      Abstract:Cu3(PO4)2, Cu2P2O7, Cu5(P3O10) were synthesized by precipitation method. The oxidation of cyclohexane hydrogen peroxide was used as a probe reaction to investigate the influence of catalyst, the sorts and amounts of solvent, catalyst dosage, oxidant dosage, the reaction temperature and time and propose the oxidation mechanism. The results showed that Cu2P2O7 was exhibited the highest catalytic activity, using 10 mL of acetonitrile, 8 mmol of cyclohexane, 0.0300 g of Cu2P2O7 catalyst, 3.00 mL of w (H2O2)=30% hydrogen peroxide at temperature of 65 ℃ for 10 h, the cyclohexane conversion was 54. 1%, the cyclohexanol and cyclohexanone yield were 21.3% and 32.8%, respectively.