• Volume 35,Issue 3,2018 Table of Contents
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    • >Review and monographs
    • Advances of Intermolecular Self-assembled Discotic Liquid Crystal Materials

      2018, 35(3).

      Abstract (442) HTML (0) PDF 0.00 Byte (0) Comment (0) Favorites

      Abstract:In this paper, the development of intermolecular self-assembled discotic liquid crystals were reviewed in past decade. The properties of discotic liquid crystals of self-assembled molecules and supramoleculars by intermolecular hydrogen or metal coordination bond and photoelectric properties and their application in organic potential devices of liquid crystal materials composed of inorganic nanoparticles were mainly discussed. Finally, the advantages of different intermolecular self-assembled discotic liquid crystals were summarized. Comprehensive literature reported that the introduction of intermolecular hydrogen bonds or coordination bonds could better realize the application of discotic liquid crystals in specific functional materials. And self-assembled discotic liquid crystals could also form complexes with nanoparticles to obtain a specific function nanocomposites.

    • >Functional materials
    • Application of ZnPc loaded macroporous silica nanocarrier in the photodynamic therapy

      2018, 35(3).

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      Abstract:Degradable macroporous silica nanoparticle (DMSNs@CS/HA) was prepared from traditionally prepared mesoporous silica using Ca2+ as pore enlarged reagents, and using good biocompatible chitosan (CS) and hyaluronic acid (HA) through layer-by-layer self-assembly technique. The obtained multifunctional nanocarrier was used to load hydrophobic drugs (zinc phthalocyanine) for photodynamics treatment of tumor. Herein, the phase, morphology, pore size distribution, infrared spectroscopy, photodynamics antitumor effect and fluorescence imaging experiment of the as-prepared DMSN@CS/HA were investigated. The survival rate of Hela cells incubated with DMSNs@CS/HA at the concentration of 50 mg/L, reaches up to 93.2%. After loading ZnPc and subjected to the near infrared ray (NIR) irradiation for 10 min, the survival rate sharply decreases to 36.2%. The MTT assay and fluorescence imaging suggest that DMSNs@CS/HA nanocarrier has good biocompatibility, can effectively load ZnPc. And DMSNs@CS/HA@ZnPc shows the excellent photodynamics therapeutic effect under NIR radiation.

    • Preparation and Performance of Particle Size Controllable Polyacrylamide Nano-microspheres with Core-shell Structure

      2018, 35(3).

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      Abstract:Theacrylamide(AM) and acrylic acid(AA)withstrong waterabsorption andexpansibilitywere used as main monomers,with 2-acrylamide-2methyl propane sulfonic acid(AMPS) and methyl acrylyl ethyl trimethyl ammonium chloride(DMC) as functional monomer, and a core-shell typeP(AM-AA-AMPS-DMC)nano-microsphereswas preparedby inverse emulsion secondary polymerization.Thepolyacrylamidenano-microspheres were characterized by using FTIR,TG,XRD,TEM,laser particle size analyzer,rheological analyzer and stability analyzer.The results show that monomers AM, AA, AMPS and DMChavepolymerized completely, and P(AM-AA-AMPS-DMC)microspheres have good thermal stability, with smooth surface,uniform distribution and core-shell type structure.Thestorage stability of the nano-microspheresemulsionismorethan6 months.Theheat resistance and salt resistance of the nano-microspheres were characterized by testing expansion rateof nano-microspheresinmineralized waterwithsalinityand at differenttemperature. The experimental results show thatthe average particle size of nano-microsphereswas expanded from 260nm to1168nm as the prolongating of ageing time. Theexpansion rateincreasedwith temperature increasing andtheexpansion rateof P(AM-AA-AMPS-DMC)nano-microspheresat60℃reached to4.1times.With the increase of shear rate,the P(AM-AA-AMPS-DMC)emulsion shows the shear thinning behavior and it has a particularviscoelasticity.

    • Properties of Organic/Inorganic Si Hybrid Solar Cells based on organic layer incorporating with gold nanoparticles

      2018, 35(3).

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      Abstract:Poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate) (PEDOT:PSS) layers incorporating with Au nanoparticles (NPs) have been explored for fabricating the hybrid Si/organic solar cells. After incorporating with Au NPs, the power conversation efficiency (PCE) of 12.85% has been achieved, which corresponds to ~23% improvement comparing with that of the pristine one. The current density-voltage (J-V), external quantum efficiency (EQE), and capacitance-voltage (C-V) results show that the enhancement of the devices can be ascribed to the optical and electrical effects caused by Au NPs. After incorporating with Au NPs, the reflection of the device where the wavelength regime coincides with the plasmonic region of Au NPs is reduced. Meanwhile, the conductivity of the PEDOT:PSS layer and the built-in electric field (Vbi) of the devices are enhanced, and both of them are beneficial for charge separation and collection, significantly suppressing the recombination process of the devices.

    • Preparation of Tetraphenylporphyrin Cobalt Optical Waveguide Sensing Element and Its Detection of Ethanol Gas

      2018, 35(3).

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      Abstract:In this paper, tetraphenylporphyrin cobalt was synthesized via Alder method, achieving the detection of ethanol. Using the means of NMR (1H-NMR), Field-Emission Scanning Electron Microscope (FE-SEM), Infrared (IR), and Ultraviolet (UV-vis) to characterize. We successfully prepared tetraphenylporphyrin cobalt thin film /K exchanged glass waveguide sensing element, that uses tetraphenylporphyrin cobalt as sensitive reagent, by the method of spin coating to detect a variety of gases. The detection results show that the gas sensing element of ethanol have a good selective response, high sensitivity, the response time and recovery time were 1.5 s and 13s respectively, signal to noise ratio S/N = 4.857, RSD = 0.8% (V/V0 = 1?0-4). In parallel experiment, the results have a good linear relationship (R=0.9924), that proved the accuracy of the sensor element to ethanol gas detection.

    • Synthesis and Characterization of Aqueous Two-Phase Polymerization of PAM-AMPS with High Stability

      2018, 35(3).

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      Abstract:A stable anionic polyacrylamide(PAM-AMPS) emulsion was prepared by using acrylamide (AM) and 2-acrylamido-2-methylpropanesulfonic acid (AMPS) as the reaction monomer,Ammonium Sulphate(AS) aqueous as the dispersed medium of the aqueous two-phase polymerization, Ammonium persulfate and sodium bisulfite redox system as initiators,the Poly 2- acrylamide -2- methyl -1- sodium sulfonate as a steric stabilizer. The structure of PAM-AMPS was confirmed by means of XRD,FTIR,TG and DSC. The PAM-AMPS emulsion was analyzed by TEM and stability analysis.The results show that the copolymer P (AM-AMPS) is an amorphous amorphous molecule with good thermal stability. The stability of PAM-AMPS emulsion was excellent and the PAM-AMPS emulsion destabilisation coefficient(TSI) was less than or equal to 0.4. The copolymer PAM-AMPS is distributed in spherical and elliptical particles in aqueous solution.

    • Preparation and Characterization of Bisphenol F Photosensitive Resin

      2018, 35(3).

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      Abstract:In this work, Bisphenol F epoxy acrylate prepolymer was prepared by using Bisphenol F epoxy resin and acrylic acid as raw materials, followed by mixing with diluent TPGDA and photoinitator BDK at the ratio of 70%︰26%︰4% to produce photosensitive bisphenol F resin. Its Shrinkage ratio and gel content were studied to for the optimum synthesis process. The orthogonal experiment results showed that, at 100℃, with 1.0% tetramethyl ammonium chloride as the catalyst, 0.1% bisphenol as polymerization inhibitor and the mass ratio of 1:0.8 between epoxy resin and acrylic acid, bisphenol F photosensitive resin’s shrinkage ratio was 5.05% after 4 hours’ reaction, which was 30% lower than Bisphenol A epoxy resin. The gel content was 92.25%, which was 3% higher than Bisphenol A epoxy resin. Meanwhile, the sensitivity to UV light and sensitivity and absorption capacity to UV were also improved. It can be used for 3D printing.

    • Synthesis and Application of Transparent Water-repellent Coating

      2018, 35(3):0-0.

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      Abstract:Fluorosilicone water-repellent fluorosilicone resin (FSi-1) was synthesized by the hydrosilylation with Fluorine-containing and hydrogen-containing polysiloxane(FPHMS), perfluorooctane ethylene(vi-F17) and vinyl modified nano-silica sol(VS) which were prepared from γ-Methacryloxypropyl trimethoxysilane(KH570) as modifier and tetraethoxysilane(TEOS) as hydrolysis precursor by sol-gel method. The coating method was used on hydrophobic coating application. Through FT-IR, TEM, TGA, AFM and WCA measurment, the characterizations of products were detereminded. In additon, the influence of the addition of adding VS on the properties of the coating was also discussed. The results demonstrated that on the surface of coatings showed a large amount of nano-convex which distributing evenly, and the addition of VS is 10%, FSi-1 system is stable. As the FSi-1 content was 0.5%, the light transmittance is not affected. Moreover, The coating hardness is 5H. the WAC increased to 120.5˚ and the rub-bing fastness test pointed that the coating could keep good hydrophobic capitity after rub over 1000 times after modifier VS was added.

    • >Catalysis,separation and purification technology
    • Sugaring-out extraction of polyphenols from Lycium ruthenicum Murr. and Inhibitory effect on advanced glycation end products (AGEs)formation

      2018, 35(3).

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      Abstract:Sugaring-out extraction was adopted to separate polyphenols from Lycium ruthenicum Murr.,which was incubated in the simulated systems at different times levels (0.5-3h )and concentrations (0.2-1.0 mg/m L), which was to observe its inhibitory effect on AGEs. different organic solvent /sugar types system were selected for the further study. The optimization sugaring-out extraction system of 25% (w/w) t-butanol and 19% (w/w) glucose were selected, 2% (w/w)of polyphenols crude extract, 94.15% polyphenols, 94.08% flavones and 94.3% anthocyanins were recovered in the upper phase. Compared with salting-out extraction, the present method exhibited higher extraction effect. The maximum relative inhibitory rate of the solution containing polyphenols with the concentration of 1.0mg/mL on AGEs formation was up to 71.93%?1.32% after heated for 2h at 80℃. Polyphenols could be used as functional food ingredients to inhibit AGE formation.

    • Photoelectrocatalytic Reduction of CO2 on Cu2O/CuO Film

      2018, 35(3).

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      Abstract:In this study, the Cu2O/CuO/Cu complex films were prepared with the copper plate as the carrier of catalyst. First, the CuO nanoribbons (CuO NRs) were developed on the copper plate by the surface oxidation method. And then the Cu2O was loaded on the CuO NRs by electrochemical methods. X-ray diffraction (XRD) and transmission electron microscope (TEM) were carried out to characterize complex films. Linear sweep voltammetry, photocurrent-time measurement and electrochemical impedance spectroscopy were used to study the photoelectrocatalytic reduction performance for CO2. The reduction product of CO2 was determined by chromotropic acid spectrophotometry method. The results showed that the CuO films were composed with nanoribbons and the Cu2O/CuO/Cu complex films had excellent photoelectrocatalytic performance. Methanol was the major product of the photoelectrocatalytic reduction of CO2 and its concentration reached 32.2μg/mL after 6h. This study has some guidance for photoelectrocatalytic CO2 reduction.

    • Catalytic Degradation of n-heptane over Cu/Co Composite Oxides

      2018, 35(3).

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      Abstract:A series of copper-cobalt composite oxides were synthesized by co-precipitation with different precipitants and the proportion of Cu/Co. The obtained catalysts were further characterized by XRD, SEM, H2-TPR and O2-TPD. The characterization results indicates that the copper-cobalt catalyst prepared by different precipitants shows significant differences in physical and chemical properties. Meanwhile, catalysts using ammonia as precipitant exhibited stronger redox properties and had more chemisorption oxygen. The catalytic activity of the catalysts for oxidative degradation of n-heptane was investigated in a continuous fixed bed reactor with GHSV of 15000h-1, oxygen concentration of 10%. The results indicated that Cu1Co4 catalyst (n(Cu):n(Co)=1:4) performed the best activity in the case of reaction temperature of 185.61℃ and the conversion of n-heptane was 90%. Moreover, the stability test showed that Cu1Co4 was durable. The characterization results of XRD and TG implied that no structural change and no carbon deposition.

    • Monoglyceride Synthesis by Glycerolysis of Soybean Oil over Zn-Mg Mixed Oxide Catalyst

      2018, 35(3).

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      Abstract:A series of Zn-Mg mixed oxide catalysts with different Zn/Mg molar ratios were prepared by coprecipitation method for the glycerolysis of soybean oil to produce monoglyceride. These catalysts were firstly characterized by XRD, BET, SEM techniques, and the base strength and basicity of catalysts were determined by Hammett indicators. The reaction conditions were then optimized for the preparation of monoglyceride catalyzed by Zn-Mg mixed oxide catalyst. The reusability of Zn-Mg mixed oxide catalyst was studied finally. The results show that changing the Zn/Mg molar ratio can control the base strength, basicity, surface area and pore volume of Zn-Mg mixed oxide catalysts. The activities of Zn-Mg mixed oxide catalysts with different Zn/Mg molar ratio are consistent with the change of basicity, surface area and pore volume, and the maximum activity could be obtained when the Zn/Mg molar ratio reached 0.1. The optimum reaction conditions were as follows: n(glycerol):n(soybean oil)=3:1, reaction temperature 210?C, reaction time 2 h, and catalyst amount 0.6% (base on the mass of soybean oil). Under these conditions, the soybean oil conversion and monoglycerides yield can reach 95.6% and 58.5%, respectively. After recycling five times, the soybean oil conversion remains 80.9%, which means the ZM0.1 catalyst is stable.

    • Adsorption of Rb (Ⅰ) with Potassium Cobalt Ferrocyanide Loaded on Waste Leather

      2018, 35(3).

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      Abstract:otassium cobalt ferrocyanide was loaded on alkali-hydrolyzed waste leather to prepare a kind of adsorbent for Rb+ adsorption, whose structure and morphology were characterized with scan electron microscope (SEM), fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD). The effects of the mass ratio of Co(NO3)2•6H2O and K4Fe(CN)6•3H2O, pH, initial Rb+ mass concentration, adsorbent dosage, and contact time on adsorption capacity of adsorbent for Rb+ were investigated. The results showed that the adsorbent presented higher adsorption capacity for Rb+ when the mass ratio was 3:4. The adsorption efficiency was 93.55% at pH 7, adsorbent dosage of 0.09 g and initial Rb+ mass concentration of 20 mg/L, and adsorption achieved equilibrium at 6 h. The isothermal and kinetics of Rb+ adsorption on KCoFC-AWL were fitted well with Langmuir isotherm model and pseudo-second-order kinetics model. Up to 90% desorption efficiency of Rb+ was achieved with 1.5 mol/L KCl. The adsorption efficiency reached up to 51.19% when the adsorbent was utilised to adsorb Rb+ from saline lake at pH 7, indicating its potential application advantages as an efficient adsorbent.

    • >Drug and cosmetic materials
    • A New Pharmaceuticals Cocrystal of Carbamazepine Synthesis and Characterization

      2018, 35(3).

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      Abstract:A new drug cocrystal CBZ-MTG was synthesed by using carbamazepine (CBZ) as a active pharmaceutical ingredient (API) and methyl gallate (MTG) as a cocrystal coformer (CCF) at room temperature. The crystal structure was investigated by X-ray single crystal diffraction, and the cocrystal was characterized by infrared spectroscopy, X-ray powder diffraction, thermogravimetric analysis and differential scanning calorimetry. In addition, the solubility was measured by HPLC and the stability was also tested. The cocrystal have been significantly improved in the aspect of solubility and bioavailability. The characterization of various structural properties provides the basic data and theoretical basis for its application in the field of drugs, and provides a new choice for carbamazepine-methyl gallate cocrystal as drug applications and in the preparation field.

    • Synthesis of Thermosensitive PEG Copolymers via Thiol - Michael Addition Reaction and the Gelation

      2018, 35(3).

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      Abstract:Thiol-Michael addition reaction has become one of the most popular reaction methods in the field of synthesis of biomedical polymer materials due to the advantages of mild conditions, rapid, efficient in recent years. Well defined thermosensitive polymers poly(PEGDA-alt-EDT) were prepared by thiol-Michael addition reaction between poly(ethylene glycol) diacrylates (PEGDA) and 2,2’-(ethylenedioxy)diethanethiol (EDT). These copolymers aqueous solution exhibit a lower critical solution temperature (LCST), which can be easily tuned by the length of PEG units. These thermosensitive polymers bear acryloyloxy and thiol reactive groups demonstrated by 1H NMR spectrum and molecular weight measured by GPC. The thermosensitive poly(PEGDA-Alt-EDT) hydrogel was further formed coupling-polymerization between the end functional groups of PEG copolymers under the initiation of APS. The results of SEM, rheology and equilibrium swelling coefficient show that the poly(PEGDA-Alt-EDT) hydrogel has a typical 3D microporous structure, hydrogel rheological properties, swelling capacity and temperature responsiveness.

    • >Starch chemicals
    • Microstructure and Trapping Efficiency of Starch Based Heavy Metal Trapping Materials

      2018, 35(3).

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      Abstract:The natural starch has the advantages of low toxicity, easy to be degraded, and can be recycled. It has the ability of capturing heavy metal after multi modification.Using quaternary ammonium type etherification agent, phosphate and urea were used to modify starch molecules, and finally, a variety of charge distribution of starch molecular modified products were obtained.The microstructure, properties and mechanism of starch based collector were studied by means of infrared spectroscopy, solid state nuclear magnetic resonance (NMR), scanning electron microscopy (SEM) and trapping efficiency.The results show that: the starch molecules into the cationic quaternary ammonium groups, anionic phosphate groups and nonionic amide groups; the specific surface area increasesis conducive to trapping heavy metal ions. The removal rate of copper, lead, cadmium and nickel ions in 30mg/L mixed solution was 97.80%, 99.83%, 99.23%, 99.53%, respectively, which were up to the national emission standard. The trapping process is in accordance with the pseudo two stage adsorption model, which is controlled by the combination of electric neutralization reaction and micropore adsorption.

    • >Water treatment technology and environmental protection
    • Preparation of Ca2+ Imprinted Cross Linked Modified Chitosan and Its Adsorption Properties for Cd2+

      2018, 35(3).

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      Abstract:To improve the adsorption performance of chitosan for heavy metal ions, the Ca2+ imprinted cross linked modified chitosan (CK) was obtained by Ca2+ imprint, glutaraldehyde crosslinking, freeze drying and carbon disulfide modification of chitosan (CS). The structure of adsorbents were characterized by FTIR, XRD and BET. The adsorption properties and mechanisms of Cd2+ were investigated by static adsorption experiment. The experimental results showed that the amino groups were successfully protected by Ca2+, the acid solubility of CS was improved by glutaraldehyde crosslinking (when pH=2, CK could be used), the specific surface area was increased to 272.82 m2/g and pore volume was increased to 0.44 cm3/g by freeze-dry method, and the C=S groups were successfully introduced by CS2 modification to improve the adsorption capacity of Cd2+ on CK. The Cd2+ adsorption capacity of CK was 49.43mg/g, adsorption capacity increased by 57.7% than that of CS. The adsorption of Cd2+ on CK was agreed will with the pseudo second order kinetics model, and the rate constant was 0.025 g/(mg•min). The adsorption of Cd2+ on CK accorded with Freundlich equation, and the n was 4.45. The Dubinin Radushkevich model indicated that the adsorption process of Cd2+ on CK was chemical adsorption, and the mean adsorption energy was 2236kJ/mol. The selective adsorption experiment indicated that CK had the properties of specific absorption with Cd2+, and the relative selectivity coefficients were greater than 3.54 besides Ca2+.

    • Synthesis and Flocculation Properties of Succinyl-Chitosan

      2018, 35(3).

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      Abstract:The formation of Schiff base (B-CTS) by chitosan and benzaldehyde protects the amino group of chitosan,and then B-CTS reacted with succinic anhydride to synthesize succinyl chitosan(SACTS).The structure and morphology of SACTS were characterized by FTIR, 1HNMR, XRD and ESEM.The effects of the amount of acid acceptor, the amount of succinic anhydride, the reaction time and the reaction temperature on the carboxyl content and esterification rate of SACTS were discussed.The results showed that the optimum conditions were as follows: m (B-CTS): m (triethylamine) = 1: 4,dosage of succinic anhydride was m (B-CTS): m (SAA) = 1: 5, The reaction time was 6.5 h and the reaction temperature was 65 ℃.Under this process conditions,The carboxyl content and esterification rate of SACTS were 93.01% and 71.13%, respectively.The flocculation experiment was carried out with SACTS and the prepared pheromone dye wastewater,The effects of pH, initial turbidity and temperature on flocculation were investigated.The results showed that when the flocculation conditions were pH = 1 ~ 4, the dosage was 1 ~ 10mg / L, the initial turbidity was 200 ~ 800NTU, the temperature was 20 ~ 30 ℃, the turbidity removal rate of supernatant was More than 95%, pyrotenine dye residual rate of 10% or less.The zeta potential of the supernatant and the XPS spectra of the flocculation showed that the flocculation process of SACTS and Pyrobinum wastewater was achieved by the interaction between the neutralization and the adsorption bridging.

    • Application of Low Phosphorus Scale Inhibitor in Thermal Desalination

      2018, 35(3).

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      Abstract:Low phosphorus scale inhibitor was synthesized with hydrolyses polymaleic anhydride (HPMA), 1-hydroxy ethylidene-1, 1-diphosphonic acid (HEDP) and polyacrylic acid (PAA), and carboxyl-terminated hyperbranched polyester (CHBP) as the main components, and then, its scale inhibiting performance was evaluated by calcium carbonate deposition method and deposition test of copper tube. The molecular structure of CHBP was proved by FTIR. The morphology and crystal structure of scale samples was proved by SEM and XRD. The results shows that the optimum composition of low phosphorus scale inhibitor is the above 4 components with mass ratios of m(HEDP): m(CHBP): m(HPMA): m( PAA) = 1:9:80:10. The scale-inhibiting rate of the composed reagent reached 87.5% when the dosage was 15 mg/L. The carboxyl groups of scale inhibitor prevent the formation of calcium carbonate scale. The introduction of CHBP can obviously reduce the content of total phosphorus, and the changed morphology of scale sample could stable in the water and flow easily, resulting in scale could not grow and aggregate in the surface of the heat exchanger.

    • Photocatalytic Degradation of Bisphenol A in the presence of Ferrum (Ⅲ)

      2018, 35(3).

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      Abstract:The photocatalytic degradation of bisphenol A (BPA) in aqueous solution with the Fe(NO3)3 catalyst by sunlight irradiation was investigated. The effects of dosing quantity of Fe(NO3)3 , PH, initial concentration and irradiation time on bisphenol A are discussed during the degradation process of BPA. CODCr removal of BPA was determined. The experimental results showed that under the optimum condition, i.e., the mole ratio of ferric nitrate and BPA was 0.8:1, pH value was 3 and the concentration of BPA was 10 mg/L, three days irradiation by sunlight, the removal of BPA was 99.4%, and the COD mineralization rate was 66.8%.

    • >Dyeing and finishing auxiliaries
    • Preparation and yellowing resistance of mixed isocyanate based polyurethane

      2018, 35(3).

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      Abstract:A series of different mole ratio of hybrid isocyanate based polyurethane was successfully synthesized via step-by-step polymerization, with isophorone disocyanate (IPDI)/two phenyl methane diisocyanate (MDI) and polytetramethylene ether glycol (PTMG-2000) used as raw materials, dibutyltin dilaurate (DBTDL) as the catalyst, 1,4-butanediol (BDO) as the chain extender and anhydrous ethanol (EtOH) as the blocking agent. The prepared polyurethane was diluted and dispersed with a dispersing machine, and then prepared the polyurethane film. The solid content of the prepared polyurethane was measured; the mechanical properties and the yellowing resistance and UV transmittance before and after ultraviolet aging of the polyurethane film were measured too. Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD) and thermal analysis (TG) were used to characterize the structure and properties of the polyurethane film. The results showed that with the decrease of n(IPDI)/n(MDI), the yellowing resistance of polyurethane film decreased, but its breaking strength increased from 18.73N of IMPU-6 to 42.85N of IMPU-11, as well as the elongation at break was reduced from 763.44% of IMPU-1 to 463.85% of IMPU-11. The color difference before and after UV aging increased from 0.72 in IMPU-1 to 22.92 in IMPU-11, and the yellowing grade decreased from grade 5 of IMPU-1 to grade 1 of IMPU-11. Meantime, the UV transmittance decreased from 89.74% of IMPU-1 to 35.04% of IMPU-11, the crystallinity increased from 2.02% of IMPU-1 to 11.27% of IMPU-11, the residue at 450℃ increased from 1.07% of IMPU-1 to 18.11% of IMPU-11 and the residue at 285℃ was reduced from 97.01% of IMPU-1 to 91.84% of IMPU-11.

    • >Acrylic series chemicals
    • Preparation and Properties of Polyacrylate/Hollow Urchin-like ZnO Composite Film

      2018, 35(3).

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      Abstract:Hollow urchin-like ZnO were successfully fabricated by a two-step hydrothermal method. Then, the polyacrylate/hollow urchin-like ZnO composite emulsion was obtained by physical blending of polyacrylate emulsion and hollow urchin-like ZnO. The water vapor permeability, water resistance, mechanical properties, UV transmittance, and antibacterial activity of polyacrylate/hollow urchin-like ZnO composite film were investigated. The results showed that the diameters of hollow urchin-like ZnO and the length of their nanorods were approximately 2.1μm and 350 nm, respectively. The shell of hollow urchin-like ZnO had mesoporous structure with average pore size of 28.58 nm. The specific surface area and pore volume of hollow urchin-like ZnO were 9.34 m2/g and 0.07 cm3/g, respectively. The polyacrylate/hollow urchin-like ZnO composite film exhibited the better water vapor permeability, water resistance, mechanical properties, UV-shielding and antibacterial activities compared with that of pure polyacrylate film. Among them, water vapor permeability, water resistance and elongation at break of composite film increased by 126.3%, 14.9%, and 112.5%, respectively.

    • >Fine chemical intermediates
    • Synthesis of Coumarin Oxime Ester Compounds

      2018, 35(3).

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      Abstract:A series of coumarin oxime esters were synthesized by two-step reaction with substituted 3-acetyl/butyryl coumarins as the raw material. The reaction of compound 3a was carried out as template reaction, and the effects of the solvent and temperature on the yield of 3a was investigated. The results showed that the yield of the product was the highest when the reaction temperature was 60 ℃ with tetrahydrofuran as solvent. Eleven coumarin oxime esters with different substituent groups were synthesized in 67% ~ 92% yields under the above-mentioned reaction conditions. The struxtures of target compounds have been confirmed by IR, NMR and X-ray crystal diffraction.

    • Design and Synthesis of Phthalate Ester Haptens and Antigens

      2018, 35(3).

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      Abstract:Using 4-nitro phthalic acid as starting material, two phthalate ester haptens dibutyl 4-aminophthalate (1a) and di(hexan-3-yl) 4-aminophthalate (1b) were synthesized by the esterification with n-butyl alcohol and 2-ethylhexanol, respectively, and then via iron powder reduction. Then hapten 5-((3,4-bis(((2-ethylhexyl)oxy)carbonyl)phenyl)amino)-5-oxopentanoic acid (1c) was prepared by the amidation of hapten 1b and dihydro-2H-pyran-2,6(3H)-dione. Their structures were characterized by melting point, 1H NMR and MS. Then haptens 1a-1c were coupled with bovine serum albumin (BSA) and ovi albumin (OVA), respectively, and six antigens 2a-2c and 3a-3c were prepared and analyzed by ultraviolet absorption spectrum.

    • Synthesis of Benzimidazoles from 3-fluoro-4-nitrotoluene by a two-step procedure

      2018, 35(3).

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      Abstract:Using 3-fluoro-4-nitrotoluene as the starting material, N-substituted 2-nitro-4-methyl-anilines were prepared under microwave irradition, then N-substituted 2-nitro-4-methyl-anilines reacted with different aldehydes to synthesize 1,2,6-substituted benzimidazole derivatives. The first step reaction conditions were optimized from the reaction temperature and the feed ratio and the optimum reaction conditions were determined as follows: the temperature was 83℃, the feed ratio was n(3-fluoro-4-nitrotoluene):n(Phenylethylamine): n(K2CO3) = 1: 1.5: 1.8, the yield of 5-methyl-2-nitro-N-phenylethylaniline (IIa) and 2-nitro-N- (3-phenylpropyl) aniline (IIb) was 99.2% and 98.9% respectively. The reaction conditions were optimized for both the amount of catalyst and the reaction temperature in the second step, and the optimum reaction conditions were determined as follows : the amount of aldehyde and N-substituted-2-nitro-4-methylaniline was 2mmol, ethanol was 30mL and 1mol/L Na2S2O4 aqueous solution was 18mL. Under reflux, the reaction time could be shorten from 12h to 40min-2h compared to the literature. 10 kinds of 1,2,6-trisubstituted benzimidazole derivatives were synthesized, nine of them were new compounds. All the structure of compounds were identified by IR, 1HNMR,13CNMR, respectively.

    • Synthesis of 4-methoxy-3-(3-morpholinopropoxy)benzonitrile

      2018, 35(3).

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      Abstract:3-Hydroxy-4-methoxybenzonitrile was synthesized by dehydration of isovanillin and hydroxylamine hydrochloride with the yield of 96%.And 4-methoxy-3-(3-morpholinopropoxy)benzonitrile was synthesized by alkylation of 3-hydroxy-4-methoxybenzonitrile with N-(3-chloropropyl) morpholine. The structures of product were characterized by IR and NMR.The optimum reaction conditions for synthesis of 3-hydroxy-4-methoxybenzonitrile were as follows: n(isovanillin): n(hydroxylamine- hy-drochloride)=1:2, reaction temperature 72℃, reaction for 6 hours with the yield of 96%.The optimum reaction conditions for synthesis of 4-methoxy-3-(3-morpholinopropoxy)benzonitrile were as follows: n(3-hydroxy-4-methoxybenzonitrile): n(4-(3-chloropropyl)morpholine)=1.0:1.1, reaction for 6 hours at reflux temperature with the yield of 96%.After two steps of optimization, we can obtain the target compound that was high yield as well as more suitable for industrial production.

    • Crystal structure and bovine serum albumin binding studies of 4-(4-aminophenyl)-5-ethoxycarbonyl-6- methyl-3,4-dihydropyrimidin-2(1H)-one

      2018, 35(3).

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      Abstract:4-(4-Aminophenyl)-5-ethoxycarbonyl-6-methyl-3,4-dihydropyrimidin-2(1H)-one (AEMD) was synthesized and the crystal structure of AEMD was determined by single crystal X-ray diffraction. This molecule crystallizes in a monoclinic P2(1)/c space group with a=11.237(4)nm, b=5.799(2)nm, c=22.394(7)nm, α=90o, β=91.048(5)o, γ= 90o, Z=4. The interactions between AEMD and bovine serum albumin (BSA) were investigated using fluorescence spectroscopy, the results revealed that AEMD quenched the BSA fluorescence; the corresponding thermodynamic parameters(ΔH?0 and ΔS?0) shown that the action forces were mainly hydrogen bond and van der Waals interaction; the binding distance was estimated to be about 2.19 nm according to F?rster’s non-radioactive energy transfer theory; the synchronous fluorescence showed that the AEMD induced conformational changes of BSA