• Volume 28,Issue 3,2011 Table of Contents
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    • >Functional materials
    • Effect of Amine Resin on the Property of SiO2/Silicone hybrid Hard Coatings

      2011, 28(3).

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      Abstract:The transparent SiO2/silicone resin was prepared with tetraethoxysilane(TEOS) and organosiloxane as the main materials by the sol-gel method, then the silicone/amine hybrid hard film was prepared on polycarbonate (PC) by adding amine resin. The effects of the proportion of amine resin on the properties of hybrid hard film were discussed. The structure, morphology and transmittance of the hybrid coating were characterized by FTIR, UV, TG, SEM and particle size analyzer etc. The results show that the distribution of the hybrid resin particle size is about 162.5 nm. The alkali resistance of the hybrid film can be significantly improved by adding a small amount of amine resin. After the hybrid film is dipped in the alkali solution for 24h, its light transmittance is still up to 90.7%, and can improve the transparency of PC. When mass percent of amine resin to silicone resin is 2%, the adhesion strength of hybrid film to PC sheet is 1 grade, and pencil hardness is 2H; After heat-treated at 120℃, the hybrid film is smooth, homogenous and densification; However, the thermal stability of the hybrid film is lower slightly than that of the SiO2/silicone hard film.

    • Research of the reaction conditions on the esterification of epoxy soybean oil

      2011, 28(3).

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      Abstract:A serials of acrylated epoxidized soybean oil oligomer were synthesized at different temperature, feeding ratios, feeding model, different dose of inhibitor and catalyst. The UV curing coating was then prepared and the gel content in cured film was analysed. The results show that increasing reaction temperature can be improving the esterification degree of the production, but exorbitant temperature can be make a adverse affection.In our trial, when the reaction temperature is 120℃, the esterification degree was maximum to reaction . Appropriate content of epoxy soybean oil in reaction system is beneficial to improving the esterification. The maximum esterification degree was achieved in cured film when the feed ratio of ESO(epoxidized soybean oil)and acrylic acid is 1.12:1(n:n). Changing the feeding model can be changed the esterification degree of the complex. In our experiment, the feeding model that the inhibitor and epoxy soybean oil were premixed together before the acrylic acid and catalyst was added improved the esterification degree. Increasing the dosage of the inhibitor can be improve the gel content. But when the dosage preponderate over 0.2%(mass fraction),the gel content and the esterification degree of the cured film was decreased . The maximum esterification degree was achieved when the dosage of the inhibitor is 0.15%.

    • Synthesis of Nano-hydroxyapatite with Precipitation Method Based on Ca(OH)2–Na3PO4 System

      2011, 28(3).

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      Abstract:Na3PO4 was prepared using phosphating residue and NaOH as initial materials. Then, Na3PO4 was precipitated with Ca(OH)2 solution under the condition of ultrasonic to obtain nano-hydroxyapatite. The resulting material was characterized by FT IR, XRD and SEM. When the Na3PO4 solution droping speed was 0.3mL/min under the condition of room temperature and ultrasonic, and the prepared precipitation was washed by ethanol before drying and calcination, the nano-hydroxyapatite with the purity of 99.5%, the particle size about 50nm, the high crystallinity and high dispersion could be obtained.

    • Synthesis and fluorescent properties of the polyamidoamine dendrimers modified by phenyl aldehyde

      2011, 28(3).

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      Abstract:Polyamidoamine-phenyl aldehyde of G3.0 and G4.0 dendrimers were prepared with ethylenediamine as center core, methyl acrylate as branch monomer and phenyl aldehyde as terminated functional group by divergent method. The fluorescent property of polyamidoamine-phenyl aldehyde dendrimer was studied. The results showed that fluorescence of the different generation polyamidoamine-phenyl aldehyde dendrimer was all quenched by Fe3+ in the solution and a red shift of the fluorescent emission peak was observed also. The fluorescence of polyamidoamine-phenyl aldehyde dendrimer was increased by Zn2+ in the solution. But, the fluorescence of polyamidoamine-phenyl aldehyde dendrimer decreased when the mole ratio of Zn2+/dendrimer continuously increased.

    • Synthesiss and characterization of a novel bagasse xylan acetates

      2011, 28(3).

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      Abstract:Abstract:Bagasse xylan acetates was synthesized by using bagasse xylan as raw materials, acetic anhydride as esterifying agent, p-toluenesulfonic acid(PTSA) as activation catalyst and acetic acid as the solvent. The influence of reaction conditions on the degree of substitution of bagasse xylan acetates was investigated. The degree of substitution of the product was 0.20 under the donditions of m(xylan)∶m(acetic anhydride)=4∶5, m(xylan)∶m(PTSA)=4∶0.2, m(xylan)∶m(acetic acid)=4∶10.49, reaction temperature 70℃, reaction time 4h. The structure was characterizated by FTIR,XRD and SEM. Gelatinization Characteristics and thermal viscosity of Bagasse xylan acetates was separately determined, which indicated that the gelatinization temperature of Bagasse xylan acetates was lower and the stability characteristics of thermal viscosity was significantly improved.

    • Rapid Analysis of Volatile Oils Chemical Composition in Different Parts of Herba Erigerontis Annui in Guizhou by MAE-HS-SPME Followed by GC–MS

      2011, 28(3).

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      Abstract:The volatile compounds were extracted in the different parts of Herba Erigerontis Annui by microwave-assisted headspace solid-phase micro-extraction(MAE-HS-SPME). Their constituents were analyzed and identified by gas chromatography-mass spectrometry combined with Kovats retention index, The results showed that 67,69 and 69 volatile constituents in the stem, in the leaf and in the flower of Herba Erigerontis Annui were separated and identified. Accounting for 92.71%, 96.72% and 96.16% of the total peak areas, respectively. Which is the main component in stem β-Elemene (5.22%), germacrene d (41.80%) and( )-β- selinene (7.71%).And in the leaves cyclotene (6.43%),β-Elemene (8.45%), germacrene d (40.17%) and (E,E)-α- Farnesene(5.80%).And in the Flowers cyclotene (4.20%), β-Elemene (8.65%) and germacrene d (31.20%).It was also observed that there were significant differences in the relative contents of three parts.

    • >Surfactants
    • Preparation and Properties of Comb-like Amphiphilic Polymers

      2011, 28(3).

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      Abstract:Comb-like amphiphilic polymers SMA-g-MPEG, SMA-g-C12H25OH and SMA-g-MPEG C12H25OH were prepared with grafting poly(ethylene glycol)monomethyl ethers (MPEG) and laurel alcohol (C12H25OH) on poly(St-co-MA)(SMA). The results of FT-IR and 1H NMR confirmed success in the comb-like amphiphilic polymers preparation. The aqueous solubility of the as-prepared samples showed that SMA-g-MPEG could dissolved in water easily with transparent solution up to a mass concentration (ρ) of 100 g/L; the solubility of SMA-g-MPEG C12H25OH was slightly weak and a gel was formed at a concentration of 100 g/L; the solubility of SMA-g-C12H25OH was even bad and a gel was formed at a concentration of 60 g/L. Surface tension measurements indicated that at 25 ℃ the surface tension (?) of SMA-g-MPEG solution was decreased with the decrease of the concentration limitedly without the platform on the surface tension vs concentration curve; For the aqueous solution of SMA-g-MPEG C12H25OH, the surface activity was improved and its critical micelle concentration (CMC) could arrive at 4.22 g/L, in which its surface tension (γCMC) was 43.9 mN/m; SMA-g-C12H25OH gave excellent surface activity with a CMC of 1.21 g/L and a γCMC of 33.2 mN/m.

    • >Electronic chemicals
    • Study of Salt-based Colloid Palladium of Low Concentration In the PCB Electroless Plating

      2011, 28(3).

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      Abstract:By analyzing the effect of the PdCl2 concentration, Sn / Pd (molar ratio), reaction temperature, and NaCl concentration on the activity and stability of colloidal palladium, the optimal preparation conditions of salt-based colloid palladium of low concentration for the PCB electroless plating was obtained that the concentrations of PdCl2 and NaCl were 0.4g/L and 160g/L respectively, mole ration of Sn/ Pd was 30:1, reaction temperature was 60±2℃. Four different additives (tin sodium, urea, vanillin, and ascorbic acid) were added into the activation solution obtained according to the above conditions respectively. The effect of four different additives on the activity and stability of activation solution was investigated. The obtained results showed that the urea had a good effect on improving the activity and stability of the activation solution. The suitable minimum concentration of urea was 10 ~ 15g / L.

    • >Catalysis,separation and purification technology
    • Effect of Forming conditions on Properties of Formed CuO-Ce0.5Mn0.5O2 Support

      2011, 28(3).

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      Abstract:Formed CuO-Ce0.5Mn0.5O2 supports were prepared by extrusion process using CuO-Ce0.5Mn0.5O2 powder as raw material.The influence of the kinds of peptizers,the calcination temperature,calcination time on the formed supports were investigated,and these supports were characterized by crushing strength test,BET and SEM methods.The results show:all the peptizers can improve the crushing strength of the formed CuO-Ce0.5Mn0.5O2 supports;however, peptizers have little effect on the surface area of the supports. The added citric acid can remarkably increase the crushing strength of the formed CuO-Ce0.5Mn0.5O2 supports.Under the preparation conditions of nitric acid mass fraction of 3%,citric acid /binder mass ratio of 4:6,calcination temperature of 600 ℃ and calcination time of 5h,the crushing strength,surface area and pore volume of the formed CuO-Ce0.5Mn0.5O2 supports can reach 98.65 N/cm,36.938 rn3/g and 0.177 cm3/g,respectively. The corresponding catalyst supported by Pd for direct synthesis of diphenyl carbonate(DPC) had better catalytic activity,and the yield of DPC could achieve 9.91% under Pd loading content (mass fraction) 0.5%, p=5 MPa,p(CO)∶p(O2)= 94∶6, reaction time 4h, reaction temperature 65 ℃

    • >Perfumes and essences
    • Study on Perfumery of Fresh Oriental Fragrance

      2011, 28(3).

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      Abstract:In this paper,the components and notes of fresh oriental fragrance was studied with gas chromatography-mass spectrometry(GC-MS) and olfactory sensory evaluation , and the impacts of different aroma compositions and notes against the quality of imitation were investigated according to perfumery. The results showed that there are 61 kinds of aromatic chemicals, including 14 citrus- note chemicals, 13 green- note chemicals,16 floral-note chemicals,5 berry-note chemicals and 10 amber-note chemicals. An optimized formula and the sample have been obtained, and the similarity of imitation measured by odor fingerprint analysis is 94.77%.

    • >Drug and cosmetic materials
    • Synthesis、Characterization and Biological Activities Investigation of tridentate secondary amine complexes

      2011, 28(3).

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      Abstract:A novel tridentate ligand (L), N-(4-methylbenzyl)-N′-(2-(4-methylbenzylamino)ethyl) ethane-1,2-diamine and its transition metal complexes [ML(H2O)2Cl]Cl (M=CuⅡ, CoⅡ, NiⅡ) have been synthesized. Their composition and structures were characterized by elemental analysis,1H NMR, FT-IR and molar conductance. The crystal structure of the Ni-L was determined by single crystal X-ray diffraction method. L is a tridentate ligand, which coordinate to Ni atom with 1:1, and all of the complexes have similar six–coordinated octahedral structures. In addition, the interaction of the complexes with calf thymus DNA was investigated by UV spectroscopy and fluorescence spectroscopy, and the results suggested that the complexes may bind to DNA by electrostatic interaction mode. The binding constants (Cu-L, Ni-L, Co-L) are 2.99×104, 9.78×103 and 3.66×103, respectively.

    • Synthesis, Characterization and Antitumor Activities of Glycine Derivatives Containing 5-Fluorouracil

      2011, 28(3).

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      Abstract:Methyl 2-(5-fluorouracil-1-yl)acetamidoactate was synthesized at room temperature by liquid coupling method with 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (EDCI) and 1-Hydroxybenzotriazole (HOBt) as a condensation reagent, 5-fluorouracil as a starting material, in which the yield was 72%. 2-(5-fluorouracil-1-yl)acetamidoactic acid was obtained by hydrolysis under pH 10-11 and 20-30 ℃ with the yield 75%. The structures of the two compounds were confirmed by 1H NMR, 13C NMR, mass spectroscopy and infrared spectroscopy etc. The antitumor mechanism of the compounds was initialy revealed by UV spectra. The compounds’ in vitro antitumor activities against HL-60 and BEL-7402 were tested by The National Center for Drug Screening. The results indicated that the compounds have some antitumor effect in vitro.

    • >Food and feedstuff chemicals
    • Preparation of Resveratrol-loaded Zein Nanoparticles with Supercritical CO2 Anti-solvent Techniques

      2011, 28(3).

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      Abstract:Supercritical CO2 anti-solvent technology was tested to prepare zein nanoparticles loaded with resveratrol. The effects of different operating parameters, such as pressure, temperature, and ratio on the loading weight of resveratrol were investigated UV, SEM, XRD were used to characterize the products. The release behavior of resveratrol from the prepared nanoparticles was also studied. Results show that the yield of resveratrol is lower when increasing CO2 pressure. However, while temperature and ratio are increased, the loading yield is higher The structure of resveratrol-loaded zein nanoparticle is a Matrix with good sphere shape。Furthermore, in vitro drug release studies show that products exhibit a slower release than the single resveratrol.

    • >Water treatment technology and environmental protection
    • Study on decolorization of Cationic Yellow X-5GL Wastewater by Birnessite-Type Manganese Oxides by Birnessite Type of Manganese Oxides

      2011, 28(3).

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      Abstract:The decolorization of a cationic dye,Cationic Yellow X-5GL,was carried out using birnessite-type manganese oxides prepared by the sol-gel method.On the basis of investigating the influences of factors, such as initial pH,the dose of birnessite-type manganese oxides,the study further discussed the influence of Mg2+,Ca2+,and heavy metal ions(Pb2+,Cd2+,Hg2+).The results showed that birnessite-type manganese oxides have well decolorization effect on Cationic Yellow X-5GL.The decolorization ratio can reach to 98% in five minute when pH was 2.5 and the dose of manganese oxides was 5mg.The metal ions above had no obvious effect on decolorization of dye.The decomposition date at pH 2.5 nearly followed first-order kinetics and the reaction rate constant is 0.2069min-1.

    • Synthesis and application of ternary copolymerization cationic polyacrylamide

      2011, 28(3).

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      Abstract:The new ternary cationic flocculant P(AM-DMC-DMDAAC) was synthesized by aqueous solution polymerization with raw meterials of acrylamide (AM) , methacryloyloxyethyl trimethyl ammonium chloride (DMC) and dimethyl diallyl ammonium chloride (DMDAAC). Effects of Cationic monomer ratio, monomer concentration, reaction time, amount of initiator and reaction temperature on the molecular weight of the products were investigated. Results indicate that the molecular weight of copolymer is up to 5.1?06, and has excellent water-dissolubility. At the same time, the terpolrmer shows high capability of flocculating performance in slurry.

    • >Rubber and plastics auxiliaries
    • Synthesis and Properties of 2,4-Bisbiphenyl-6-(2-hydroxyl-4-

      2011, 28(3).

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      Abstract:Cyanuric chloride was used as raw material to synthesize 2-chloro-4,6-bisbiphenyl-1,3,5-triazine(Ⅳ) successfully via Grignard reaction and Friedel-Craft reaction.Three 2,4-bisbiphenyl-6-(2-hydroxyl-4-alkoxyl)-1,3,5- triazine compounds(Ⅴ1~3) were synthesized by compound Ⅳ and bromoalkane in the presence of K2CO3.The structures of compounds Ⅴ1~3 were characterized by FTIR,MS and 1HNMR. Thermal stability,ultraviolet absorption and light stability of compounds Ⅴ1~3 were tested by TGA and UV-vis.T5 of compounds Ⅴ1~3 was raised 40~60℃ related to  UV-1577.Maximum molar absorption coefficient(εmax) of compounds Ⅴ1~3 was 79448.28 L/(molcm)(max=318.5 nm),80873.51 L/(molcm)(max=319 nm),76774.7 L/(molcm)(max=319 nm) respectively.

    • >Special dyes and pigments
    • Studies on the Synthesis of Fluorescent Dyes of Soluble 1,8-Naphthalimides

      2011, 28(3).

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      Abstract:4-alkoxy-N-lauryl-1,8-naphthalimides were synthesized using 4-bromo-1,8-naphthalic anhydride and laurylamine as starting materials through the imidization and substitution reaction. The single factor experiments showed that optimum imidization reaction conditions were n(4-bromo-1,8-naphthalic anhydride) : n(laurylamine) =1:1.1, reaction temperature 50℃, reaction time 4 h. Under this conditions, the yield of intermediate product 4-bromo-N-lauryl-1,8-naphthalimide was 79.4%. Structures of the final products 4-alkoxy-N-lauryl-1,8-naphthalimides were characterized by IR and 1HNMR. The test results of UV absorption and fluorescent spectrum showed that the target product of the maximum absorption in absolute alcohol was 357nm and 342nm, and the maximum emission was 485nm and 490 nm, respectively. The fluorescent quantum yields of the dyes in DMF were over 0.6.

    • >Fine chemical intermediates
    • Synthesis of free amino acid esters co-catalyzed by ionic liquid

      2011, 28(3).

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      Abstract:Eight kinds of free L-amino acid esters including L-phenylalanine ethyl ester, L-phenylalanine n-butyl ester, L-phenylalanine i-butyl ester, L-tyrosine n-butyl ester, L-tyrosine i-butyl ester, L-tyrosine i-amyl ester, L-aspartic n-butyl diester and L-aspartic i-butyl diester were synthesized by direct esterification of L-amino acid and alcohol with acidic ionic liquid assisted by strong acidic cation resin as catalyst. The structures of free L-amino acid esters were characterized by 1HNMR. Optimal reaction conditions were obtained when synthesizing L-phenylalanine n-butyl ester. Among eleven kinds of the acidic ionic liquids used in this case, [Hmim]HSO4 indicated excellent activity and the catalyst is easily regenerated and reused. By this token, it exhibits its potential application as catalyst and co-solvent in the esterification of amino acid.

    • A Synthesis Route of the 5-(4-chlorophenyl)-4-methylthiazolidin-2-one

      2011, 28(3).

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      Abstract:Abstract: A concise synthetic route was developed for the key intermediate of hexythiazox—5-(4-chlorophenyl)-4-methylthiazolidin-2-one. The cyclocondensation of carbon disulfide with 1-(4-chlorophenyl)-1-hydroxypropan-2-aminium chloride would proceed in one-step at 130 oC, providing (4R,5R)-5-(4-chlorophenyl)-4- methylthiazolidine-2-thione in 82% yield with 99% purity. Subsequently, the intermediate was oxidized by hydrogen peroxide oxidation, producing (4S,5S)-5-(4-chlorophenyl)-4-methylthiazolidin-2-one in 84% yield with 95%purity. It represents a simple and facile method to access (4S,5S)-5-(4-chlorophenyl)- 4-methylthiazolidin-2-one, which shortens the reaction time and reduces the waste discharge. Thus, it is ecology benigh.

    • Synthesis of 3-Methyl-3-buten-1-ol via Thermal Formaldehyde-Isobutene Condensation

      2011, 28(3).

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      Abstract:Synthesis of 3-methyl-3-buten-1-ol (MBOH) from thermal condensation of isobutylene and formaldehyde with methanol as solution was studied in this paper. The effect of reaction parameters such as temperature, pressure, isobutene/formaldehyde molar ratio, and reaction time were investigated. The result revealed that the yield of MBOH increased with the temperature at first and then decreased while increased upon increasing of reaction pressure. Under optimum reaction condition of 498 K, 11.0 MPa, isobutene/formaldehyde molar ratio of 9:1 for 6 h, the yied of MBOH could reach 59.24%.

    • >Other
    • Study on Synthesis and Fluorescence of Novel Coumarin-based Bisulfite Anion Probe

      2011, 28(3).

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      Abstract:Two novel coumarin-based bisulfite anion probes, 4-Methyl-8-formyl-7-hydroxylcoumarin and 4-methyl-8-formyl-7-hydroxyl-6-chlorocoumarin, were synthesized by using resorcinol and 4-chloro resorcinol as the raw material respectively. The structures of the probes were characterized by IR, 1H NMR and MS. The mechanism of determination, selectivity to bisulfite anion, analytic method and the application in the actual samples of the probes were investigated. A fluorescence analytic method for detection of bisulfite anions in water was established.

    • Synthesis of a Dehydroabietyl Dipyridophenazine Derivative and Recognition on Copper Ion

      2011, 28(3).

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      Abstract:A dehydroabietyl dipyridophenazine derivative 6 was synthesized through several steps such as bromation, dinitration, reduction and cyclization by using methyl dehydroabietate as a starting material. The title compound was characterized by 1H NMR, 13C NMR, IR, MS and elementary analysis. Its sensing behaviors toward metal ions were investigated by UV-vis and fluorescence spectroscopy methods. The results showed that compound 6 exhibited a highly selective response to Cu2+.