Table of Content

23 May 2007, Volume 25 Issue 3

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Synthesis of 3,5-Dicyano-2,4,6-Trimethylpyridine by Photoinduced Aromatization of 1,4-Dihydro-3,5 Dicyano-2,4,6-Trimethylpyridine

CHEN Bin, WANG Deng-hui, WU Li-zhu, ZHANG Li-ping, TONG Zhen-he(TUNG Chen-ho)

2007, 25(3):  161-164.  DOI: 10.7517/j.issn.1674-0475.2007.03.161

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3,5-Dicyano-2,4,6-trimethylpyridine is a promising synthetic precursor for novel optoelectronic functional materiels.In this paper,3,5-dicyano-2,4,6-trimethylpyridine was prepared in high yield by photoinduced aromatization of 1,4-dihydro-3,5-dicyano-2,4,6-trimethylpyridine in CCl₄ solution.

Study on Photocatalytic Activity of TiO₂ Photocatalysts Doped with Metal Ions in Nitrogen Removal

LIU Li-fen, ZHANG Yang, YANG Feng-lin, Jimmy C YU

2007, 25(3):  165-175.  DOI: 10.7517/j.issn.1674-0475.2007.03.165

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Titanium dioxide photo-catalysts doped/co-doped with Ce³⁺,La³⁺/Ag⁺/Fe³⁺ by using the sol-gel method were prepared and tested to evaluate their photo-catalytic activities on nitrogen removal from solution which contained ammonium and nitrite.The catalysts were characterized using UV-Vis,XRD and TEM.Also investigated were the influencing factors such as different kinds and concentration of doped metal ion,dipping times (thickness of catalyst films),addition of Fe²⁺ to the solution,different substrate (glass or stainless steel net),different designs of reactor and different light sources (UV or solar light) on photocatalytic N removal efficiency.After 2 hours UV irradiation,simultaneous removal of ammonium and nitrite could be achieved.The removal efficiency for TN was about 30% when TiO₂ film was used.A higher removal rate of 41.7% could be achieved by using TiO₂ powders.

Synthesis and Fluorescence Properties of Two Oxadiazole-Based Multibranched Chromophores

RUI Wen-wen, JIANG Wan-li, DING Xue-xia, WANG Xiao-mei

2007, 25(3):  176-182.  DOI: 10.7517/j.issn.1674-0475.2007.03.176

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Two new multibranched chromophores,named as NO-G2 and BO-G2,with the same peripheral branch of oxadiazole-unit,but different molecular core,that is,carbazole for NO-G2 and benzonitrile for BO-G2,were synthesized and characterized by mass spectra and 1H NMR spectra,respectively.These two oxadiazole-based multibranched chromophores show the molecular architecture of "D-A-A’-A-D" for BO-G2 and"D’-A-D-A-D’"for NO-G2, which have the different ability of intramolecular charge transfer.The measured absorption and fluorescence spectra have shown that NO-G2 exhibits nonlinear absorption than BO-G2,owing to the former possessing pn junction and resultant more obvious intramolecular charge transfer.

Sensitization on Cubic Silver Bromide Emulsion Doped with Oxalate

MA Wang-jing, XIA Pei-jie

2007, 25(3):  183-190.  DOI: 10.7517/j.issn.1674-0475.2007.03.183

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In the emulsifying process of AgBr microcrystals in the double-jet apparatus controlled by a microcomputer,a certain amount of oxalate salt was injected at specific time and pAg into a reactor to prepare cubic AgBr grain emulsions in which oxalate ions were doped at subsurface of AgBr microcrystals.The observation results from the whole experiments and sensitometric results from these emulsions showed: 1) the sensitivities (S_d) of oxalate-doped emulsions,relative to those (S₀) of the corresponding undoped ones as the controlled,regardless of whether it is primitive,or sensitized chemically and spectrally,were remarkably increased (S_d/S₀≥1.5); 2) fog level of oxalate-doped emulsions,regardless of whether it is primitive,or sensitized chemically and spectrally,were kept low; 3) sensitization gains of oxalate-doped emulsions were nearly same as one of formate-doped emulsions; 4) the preparation of cubic AgBr emulsions doped with oxalate was more simple than those of cubic ones doped with formate,and the formers’ shape was more sharper than the latters’.

Study on the Influence of Pt⁴⁺ Doping on the Photocatalytic Efficiency of TiO₂ by Technique of Laser Flash Photolysis

LI Guang-qin, LIU Chun-yan, LIU Yun

2007, 25(3):  191-197.  DOI: 10.7517/j.issn.1674-0475.2007.03.191

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By using nanosecond laser to excite colloidal particles of pure and Pt⁴⁺ doped TiO₂ in aqueous solution,we have monitored the absorption spectrum of O^- at about 440 nm which is the signal of trapped holes and an active species in the photocatalytic reaction.Results showed that the absorption spectrum decayed within microseconds,the concentration and the decay rate of O^- determined the photodegradation efficiency.Thus,nanosecond laser flash photolysis has been carried out to elucidate the drastic enhancement of Pt⁴⁺ doping on the photocatalytic efficiency of TiO₂.

Synthesis and Characterization of the Non-Ionic Photoacid Generator-Phthalimidotosylate

LI Ping, WANG Xia, LIU Jian-guo, LI Ping

2007, 25(3):  198-203.  DOI: 10.7517/j.issn.1674-0475.2007.03.198

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Phthalimidotosylate (PIT) was synthesized from ophthalic anhydride,hydroxylamine hydrochloride and p-toluenesulfonyl chloride. It was characterized with FTIR and 1H NMR.Experiments showed that PIT has good transparence in 248 nm wavelength (absorbance=0.375) and good solubility in organic solvents.So it is a good potential photoacid generator (PAG) in the deep-UV 248 nm photoresist system.

The Application of Photochromic Diarylethene Mask Layer in the Near-Field Optical Storage

SHI Ming, NIU Li-hong, TONG Qing-xiao, TANG Ying-wu, ZHANG Fu-shi

2007, 25(3):  204-208.  DOI: 10.7517/j.issn.1674-0475.2007.03.204

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Two kinds of diarylperfluorocyclopentenes which are suitable for the use of mask layer and recording layer materials in Super-rens were synthesized and the sample disc was developed as well.The initial near-field storage experiment demonstrated that the size of recording laser focus could be decreased by the photochromic diarylethenes mask layer.Thus the decreased recording information was obtained.It also showed the concentration of diarylethene in the mask layer strongly influenced the size of recording marks.An optimum concentration existed,in which the smallest size of recording information was obtained.

Study on Synthesis and Spectral Properties of Phthalocyanine Conjugating Luminols

HUANG Xin, LI Zhong-yu, BIN Yue-jing, HUANG Lei, ZHANG Fu-shi

2007, 25(3):  209-213.  DOI: 10.7517/j.issn.1674-0475.2007.03.209

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α-Tetra-amino-phthalocyanine zinc (Ⅱ) conjugating luminols was designed and synthesized by diazotization method.The electronic absorption spectra and fluorescence spectra of the compound in DMF have been measured and studied.The phenomena of intramolecular electron transfer are found and the fluorescence of phthalocyanine was quenched significantly by luminol moiety.These results showed potential applications in fluorescence data storage.

3.5 G PAMAM-Stabilized Au Nanoparticles Prepared by Microwave Irradiation

QIAO Yan, DU Ming-chun, YANG Ping, DU Yu-kou

2007, 25(3):  214-222.  DOI: 10.7517/j.issn.1674-0475.2007.03.214

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Using 3.5 G PAMAM as a stabilizing agent,Au nanoparticles were prepared by reducing HAuCl₄ with microwave irradiation.The influence of microwave irradiation at the same ratio of 3.5 G PAMAM to HAuCl₄ for the different time and at the different ratios of 3.5 G PAMAM to HAuCl₄ for the same time on Au nanoparticles’ size and shape was studied.Au nanoparticles were characterized by UV-Vis spectra and TEM.At the same ratio of 3.5 G PAMAM to HAuCl₄,the microwave irradiation time has a little influence on the Au nanoparticles’ size and shape,meanwhile more dispersed Au nanoparticles were obtained with the appropriate increase of reactive time.At the same irradiation time,bigger and more aggregative Au nanoparticles were acquired as the ratio of 3.5 G PAMAM to HAuCl₄ was decreased.

Study on the Performance of F-Doped TiO₂

JIANG Hong-fu, ZHOU Zuo-xing, LIU Xing-qin, MENG Guang-yao

2007, 25(3):  223-229.  DOI: 10.7517/j.issn.1674-0475.2007.03.223

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F-doped TiO₂ photocatalyst was prepared by sol-gel method with NH₄F as dopant.The catalyst was characterized by XRD,XPS,and PL.It was found that the phase formation of rutile was suppressed by F-doping due to the formation of Ti-F ligand.Moreover,the surface defect of TiO₂ was increased while the binding energy of Ti2P was decreased by F-doping.It was also found that the surface OOH concentration was decreased by F-doping due to the F ions replacing Ti-OH bond.The results of photocatalytic reaction indicated that the photocatalytic activity of F-doped TiO₂ was 1.5 times higher than that of undoped TiO₂.

Study on the Effect of Photocatalytic Reduction of Hg²⁺ by Using Nano TiO₂ with Three-Wavelength Spectrophotometry

LU Wei-wei, CHEN Guo-song, ZHANG Hong-man, ZHANG Zhi-yi, LU Xiao-hua

2007, 25(3):  230-237.  DOI: 10.7517/j.issn.1674-0475.2007.03.230

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A self-made micro-reactor of nano-TiO₂ photocatalysis was used to carry out photocatalytic reduction experiments of Hg (Ⅱ) with different initial concentrations.Then the residual Hg (Ⅱ) in the solutions was determined by using spectrophotometry with Thiocyanate-Rhodamine B-Polyvinyl Alcohol.Considering the influence of TiO₂ suspension system on the absorbency,three-wavelengths spectrophotometry was proposed to eliminate the interference of TiO₂.The optimum conditions and effect of photocatalytic reduction of Hg²⁺ by TiO₂ as well as its application in removing toxic Hg (Ⅱ) in industrial waste water samples were investigated.It was showed that photocatalytic reduction of Hg²⁺ by TiO₂ had a remarkable effect on low concentrations of mercury and the reduction rate was over 90%.The method could dramatically reduced the content of toxic Hg (Ⅱ) in industrial waste water samples.