催化学报

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第36卷第5期目次

2015, 36 (5): 0-0.

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Recent progress on core-shell nanocatalysts

Qiang Sun, Xiang-Qian Zhang, Yang Wang, An-Hui Lu

2015, 36 (5): 683-691. DOI: 10.1016/S1872-2067(14)60298-9

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Molecular sieve membranes: From 3D zeolites to 2D MOFs

Yanshuo Li, Weishen Yang

2015, 36 (5): 692-697. DOI: 10.1016/S1872-2067(15)60838-5

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Synthesis and characterization of sulfur-titanium dioxide nanocomposites for photocatalytic oxidation of cyanide using visible light irradiation

E. S. Baeissa

2015, 36 (5): 698-704. DOI: 10.1016/S1872-2067(14)60320-X

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A sol-gel method was used to prepare TiO₂ and sulfur-TiO₂(S-TiO₂) nanocomposites, which were characterized by N₂ adsorption-desorption, X-ray diffraction, X-ray photoelectron spectroscopy, photoluminescene, ultraviolet visible and transmission electron microscopy measurements. The photocatalytic performance of TiO₂ and S-TiO₂ nanocomposites, with respect to the photocatalytic oxidation of cyanide under visible light irradiation, was determined. The results reveal that S is well dispersed on the surface of TiO₂ nanoparticles. Additionally, the surface area of the S-TiO₂ nanocomposites was observed to be smaller than that of the TiO₂ nanoparticles because of blocked pores caused by doping with S. The S-TiO₂ nanocomposite (0.3 wt% S) exhibited the lowest band gap and the highest photocatalytic activity in the oxidation of cyanide. The photocatalytic performance of S-TiO₂ (0.3 wt% S) nanocomposites was stable, even after the fifth reuse of the nanoparticles for the oxidation of cyanide.

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A Fe₃O₄@Nico@Ag nanocatalyst for the hydrogenation of nitroaromatics

U. Kurtan, Md. Amir, A. Baykal

2015, 36 (5): 705-711. DOI: 10.1016/S1872-2067(14)60316-8

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We report the fabrication and characterization of a magnetically recyclable Fe₃O₄@Nico@Ag catalyst for reduction reactions in the liquid phase. Fe₃O₄ is a magnetic core and nicotinic acid was used as the linker for Ag. The characterization was done with X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, thermogravimetric analysis, vibrating sample magnetometry (VSM), and ultraviolet-visible spectroscopy. VSM measurements proved the superparamagnetic property of the catalyst.

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Cu, Fe, or Ni doped molybdenum oxide supported on Al₂O₃ for the oxidative dehydrogenation of ethylbenzene

Tiago Pinheiro Braga, Antônio Narcísio Pinheiro, Edson R. Leite, Regina Cláudia R. dos Santos, Antoninho Valentini

2015, 36 (5): 712-720. DOI: 10.1016/S1872-2067(14)60313-2

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Molybdenum-based catalysts supported on Al₂O₃ doped with Ni, Cu, or Fe oxide were synthesized and used in ethylbenzene dehydrogenation to produce styrene. The molybdenum oxide was supported using an unconventional route that combined the polymeric precursor method (Pechini) and wet impregnation on commercial alumina. The samples were characterized by X-ray diffraction (XRD), N₂ adsorption-desorption isotherms, temperature-programmed reduction of H₂ (H₂-TPR), and thermogravimetric (TG) analysis. XRD results showed that the added metals were well dispersed on the alumina support. The addition of the metal oxide (Ni, Cu, or Fe) of 2 wt% by wet impregnation did not affect the texture of the support. TPR results indicated a synergistic effect between the dopant and molybdenum oxide. The catalytic tests showed ethylbenzene conversion of 28%-53% and styrene selectivity of 94%-97%, indicating that the addition of the dopant improved the catalytic performance, which was related to the redox mechanism. Molybdenum oxides play a fundamental role in the oxidative dehydrogenation of ethylbenzene to styrene by its redox and acid-base properties. The sample containing Cu showed an atypical result with increasing conversion during the reaction, which was due to metal reduction. The Ni-containing solid exhibited the highest amount of carbon deposited, shown by TG analysis after the catalytic test, which explained its lower catalytic stability and selectivity.

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对甲苯磺酸/活性炭/双氧水体系选择氧化苯乙烯生成苯甲醛

李念哲, 高远, 张欣欣, 玉占君, 石雷, 孙琪

2015, 36 (5): 721-727. DOI: 10.1016/S1872-2067(14)60314-4

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以双氧水为氧化剂, 研究了对甲苯磺酸和活性炭体系选择氧化苯乙烯生成苯甲醛反应性能。考察了反应时间、温度、催化剂用量、苯乙烯和双氧水摩尔比等对苯乙烯选择氧化性能的影响. 结果表明, 对甲苯磺酸和活性炭的用量和用量比是一个重要因素, 但对甲苯磺酸的酸性对氧化反应活性影响不大. 对甲苯磺酸和双氧水相互作用, 经非自由基过程氧化苯乙烯. 通过分解双氧水产生氢氧自由基, 活性炭显著提高对甲苯磺酸和双氧水体系氧化苯乙烯活性. 在惰性或还原气氛中高温处理活性炭能降低其表面含氧基团数量, 增加碱性, 有效分解双氧水, 产生相对较多的OH自由基. 与未处理的活性炭相比, 高温处理的活性炭进一步提高了对甲苯磺酸和双氧水体系氧化苯乙烯活性, 但降低了苯甲醛选择性. 经磺化, 在活性炭表面引入的-SO₃H基团比含氧基团(-OH, -COOH)更有效与双氧水作用氧化苯乙烯.

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4-(Succinimido)-1-butane sulfonic acid as a Brönsted acid catalyst for the synthesis of pyrano[4, 3-b]pyran derivatives using thermal and ultrasonic irradiation

Nader Ghaffari Khaligh, Sharifah Bee Abd Hamid

2015, 36 (5): 728-733. DOI: 10.1016/S1872-2067(14)60307-7

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4-(Succinimido)-1-butane sulfonic acid was shown to be an efficient and reusable Brönsted acid catalyst for the synthesis of pyrano[4,3-b]pyran derivatives using thermal and ultrasonic conditions. The catalyst was prepared by mixing succinimide and 1,4-butanesultone, which is simpler and safer than the preparation of succinimide sulfonic acid. This method has the advantages of high yield, clean reaction, simple methodology, and short reaction time. The catalyst can be recycled without loss of activity.

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Efficient, environmentally benign, one-pot procedure for the synthesis of 1, 5-benzodiazepine derivatives using N-methyl-2-pyrrolidonium hydrogen sulphate as an ionic liquid catalyst under solvent-free conditions

Hossein Naeimi, Hossein Foroughi

2015, 36 (5): 734-741. DOI: 10.1016/S1872-2067(14)60304-1

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A powerful and environmentally benign method has been developed for the one-pot synthesis of 4-substituted-1,5-benzodiazepines via the three-component reaction of a series of aldehydes with dimedone and o-phenylenediamine using [H-NMP][HSO₄] as a Brönsted acidic ionic liquid catalyst under solvent-free conditions. The key benefits of this new method over existing techniques include high yields, the use of a green catalyst, short reaction times and facile catalyst separation.

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Photocatalytic activity of mesoporous microbricks of ZnO nanoparticles prepared by the thermal decomposition of bis(2-aminonicotinato) zinc (II)

Keyvan Bijanzad, Azadeh Tadjarodi, Omid Akhavan

2015, 36 (5): 742-749. DOI: 10.1016/S1872-2067(14)60305-3

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Hollow microblocks of [Zn(anic)₂], as a novel coordination compound, were synthesized using 2-aminonicotinic acid (Hanic) and zinc (II) nitrate tetrahydrate. The chemical composition of the zinc complex, ZnC₁₂H₁₀N₄O₄, was determined by Fourier transform infrared (FTIR) spectroscopy and elemental analysis. The synthesized zinc complex was used as a precursor to produce ZnO nanostructures by calcination at 550 ℃ for 4 h. Morphological studies by scanning electron microscopy and transmission electron microscopy revealed the formation of porous microbricks of ZnO nanoparticles. N₂ adsorption-desorption analysis showed that the obtained ZnO microbricks possess a mesoporous structure with a surface area of 8.13 m2/g and a pore size of 22.6 nm. The X-ray diffraction pattern of the final product proved the formation of a pure ZnO composition with a hexagonal structure. Moreover, FTIR analyses showed that the 2-aminonicotinic acid ligand peaks were absent after the calcination step. Diffuse reflectance spectroscopy was used to determine the band gap energy of the produced ZnO and it was about 3.19 eV. To investigate the photocatalytic activity of the porous ZnO nanostructure, a series of photocatalytic tests were carried out to remove Congo red, as a representative toxic azo dye, from aqueous solution. The results show that the product can be used as an efficient photocatalyst for waste water treatment with high degradation efficiency.

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MoO_x促进的Pt基催化剂用于低温水汽变换反应

许学俊, 傅强包信和

2015, 36 (5): 750-756. DOI: 10.1016/S1872-2067(14)60294-1

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通过浸渍还原法制备了不同比例的Pt-Mo/SiO₂催化剂, 采用X射线衍射、透射电镜、X射线近边吸收谱和X射线光电子能谱表征了Pt-Mo/SiO₂催化剂的组成、结构及价态. 研究结果表明, 少量MoO_x修饰Pt-Mo/SiO₂催化剂在低温水汽变换反应中表现出比Pt/SiO₂催化剂更高的催化活性, 过量MoO_x包覆的Pt-Mo/SiO₂催化剂活性较低. 低温水汽变换反应活性来自于Pt与表面MoO_x的界面协同作用, 限域在Pt纳米颗粒表面的MoO_x表现出较低价态, 高分散MoO_x纳米岛修饰的Pt纳米颗粒是低温水汽变换反应的活性结构.

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Fructose-catalyzed synthesis of tetrahydrobenzo[b]pyran derivatives: Investigation of kinetics and mechanism

Sayyedeh Shadfar Pourpanah, Sayyed Mostafa Habibi-Khorassani, Mehdi Shahraki

2015, 36 (5): 757-763. DOI: 10.1016/S1872-2067(14)60302-8

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Fructose was used as an efficient catalyst for three-component condensation reactions of aryl aldehydes, malononitrile, and dimedone in a mixture of EtOH and H₂O as green solvents. The advantages of this method are a short reaction time, high yields, low cost, easy accesses, and simple work-up. The mechanism of the synthesis of a derivative of 4H-tetrahydrobenzo[b]pyran was clarified using spectroscopic kinetic methods. The activation energy (E_a = 65.34 kJ/mol) and related kinetic parameters (ΔG^‡ = 69.14 kJ/mol, ΔS^‡ = 20.99 J/(mol·K), and ΔH^‡ = 62.89 kJ/mol) were calculated, based on the effects of temperature, concentration, and solvent. The first step in the proposed mechanism was identified as the rate-determining step (k₁), based on the steady-state approximation.

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Synthesis and structural studies of copper(II) complex supported by -ONNO- tetradentate ligand: Efficient catalyst for the ring-opening polymerization of lactide

Anita Routaray, Nibedita Nath, Somanath Mantri, Tungabidya Maharana, Alekha Kumar Sutar

2015, 36 (5): 764-770. DOI: 10.1016/S1872-2067(14)60293-X

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The -ONNO- tetradentate Schiff base ligand N,N'-bis(2-hydroxy-3-methoxybenzaldehyde)benzene-1,2-diamine (HMBBD) has been synthesized. The ligand was attached to copper (Cu-HMBBD) in methanol under N₂ atmosphere to give a mononuclear complex. The reactivity of this complex in the ring-opening polymerization (ROP) of lactide has been studied. The complex has a square planner geometry, as determined by X-ray diffraction studies. The copper complex is highly active towards the ring-opening polymerization of lactide, and the rate of polymerization is heavily dependent on the initiator used. The copper complex allows controlled ring-opening polymerization, as shown by the linear relationship between the percentage conversion and the number average molecular weight. Based on the literature, a mechanism for the ROP of lactide has been proposed.

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Preparation and characterization of HypoGel-supported Pd nanocatalysts for Suzuki reaction under mild conditions

Kin Hong Liew, Wan Zurina Samad, Norazzizi Nordin, Poh Lee Loh, Joon Ching Juan, Mohd Ambar Yarmo, Badrul Hisham Yahaya, Rahimi M. Yusop

2015, 36 (5): 771-777. DOI: 10.1016/S1872-2067(14)60282-5

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A new heterogeneous catalyst composed of Pd nanoparticles immobilized within a HypoGel resin has been prepared in the absence of any ligands using an extensive cross-linking method. This newly developed nanocatalyst was characterized by N₂ adsorption-desorption, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray (EDX), Fourier transform infrared spectroscopy and inductively coupled plasma-mass spectrometer (ICP-MS) techniques. TEM and XRD results revealed that the Pd nanoparticles were well dispersed with diameters in the range of 4-12 nm, and an average size of about 8 nm. The cross-linked Pd catalyst demonstrated excellent catalytic activity towards the synthesis of a series of biaryl compounds by the reaction of various aryl halides (e.g., bromides andiodides) with phenylboronic acid in the presence of tetrabutylammonium bromide. ICP-MS analysis indicated that there was only 0.25% weight loss of Pd (0.55 ± 0.02 ppm) from the supported catalyst after the first cycle reaction. Furthermore, the catalyst showed excellent reusability (up to five uses) with consistently high levels of catalytic activity following its recovery by filtration.

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Efficient synthesis of 3, 3'-bisindoles catalyzed by Fe₃O₄@MCM-48-OSO₃H magnetic core-shell nanoparticles

Alireza Khorshidi, Shahab Shariati

2015, 36 (5): 778-784. DOI: 10.1016/S1872-2067(14)60281-3

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Magnetite nanoparticles coated with sulfuric acid-functionalized mesoporous MCM-48 were synthesized and used as a catalyst in three-component domino reactions of indoles, arylglyoxal monohydrates and N-arylenaminones to furnish the desired 3,3'-bisindoles by formation of two C-C and one C-N bonds in a smooth cascade with good yields under mild reaction conditions. The catalyst was recovered easily and maintained activity in successive runs.

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