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Preparation of aldoxime through direct ammoximation using titanium silicalite-1 catalyst

Chinese Journal of Chemical Engineering 2022年第7期35卷 11-17页

作者： Zhigang Xu Xiongfei Jin Tao Zhou Qian Zou Longcheng Liu zhongbo Wang Hanbing Sheng Huasheng Xie Hunan Provincial Key Laboratory of Efficient and Clean Utilization of Manganese Resources College of Chemistry and Chemical EngineeringCentral South UniversityChangsha 410083China Kopperchem Industry Corp. LTDSolvent Extraction Engineering Research CenterChongqing 401221China Cangzhou Dahua Group Co. Ltd.Cangzhou 061000China

The liquid phase direct ammoximation of 5-isooctyl salicylaldehyde with ammonia and hydrogen peroxide was studied using titanium silicalite-1(TS-1)*** effect of reaction parameters on the yield of the product was studied,which include reaction temperature,reaction time,molar ratio of ammonia to aldehyde as well as hydrogen peroxide to *** influence of the amount of catalyst on the reaction results was also *** maximum 5-isooctyl salicylaldoxime yield of 98.76%was achieved under the following optimal reaction conditions:the molar ratio of 5-isooctylaldehyde to hydrogen peroxide and ammonia of 1:1.4:1.6,the reaction temperature of 70℃,the amount of TS-1 of 17.5 g·mol^(-1)(5-isooctyl salicylaldehyde),and the feeding time of 2 *** method has the mild reaction conditions and avoids the shortcomings of traditional ***,useless inorganic salts by-products are avoided,and there is no environmental pollution.

关键词： titanium silicalite-1 Ammoximation Aldoxime Extractant Process optimization

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Effect of sodium ions in synthesis of titanium silicalite-1 on its catalytic performance for cyclohexanone ammoximation

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Frontiers of Chemical Science and Engineering 2014年第2期8卷 149-155页

作者： Pengxu YAO Yaquan WANG Teng ZHANG Shuhai WANG Xiaoxue WU Key Laboratory for Green Chemical Technology of the Ministry of Education School of Chemical Engineering & Technology Tianjin University Tianjin 300072 China

titanium silicalite-1 （TS-1） has been hydrothermally synthesized with tetrapropylammonium hydroxide （TPAOH） as the template in the presence of various amounts of Na＋, characterized by inductively coupled plasma, X-ray diffraction, scanning electron microscope, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and ultro-violet-visible spectroscopy and studied in cyclohexanone ammoximation. The characterization results show that with the increase of Na＋ concentration in the synthesis, both the crystal sizes of TS- land extra framework Ti increase but framework Ti decreases. The addition of Na＋ below 3 mol-% of TPAOH in the synthesis does not influence the catalytic properties with above 98% conversion of cyclohexanone and 99.5% selectivity to cyclohexanone oxime. However, at the concentrations of Na＋≥3mol-% of TPAOH in the synthesis, the catalysts are deactivated faster with the increase of Na＋ addition, which can be attributed to more high molecular weight byproducts deposited in the large TS-1 particles and the loss of the frame-work titanium. The results of this work are of great importance for the industry.

关键词： titanium silicalite-1 sodium ion crystal size,extra framework Ti cyclohexanone ammoximation

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Effect of triethylamine treatment of titanium silicalite-1 on propylene epoxidation

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Frontiers of Chemical Science and Engineering 2014年第4期8卷 478-487页

作者： Juan XU Yaquan WANG Wenping FENG Yi LIN Shuhai WANG Key Laboratory for Green Chemical Technology of the Ministry of Education School of Chemical Engineering & Technology Tianjin University Tianjin 300072 China

titanium silicalite- 1 （TS- 1） treated with triethy- lamine （TEA） solution under different conditions was characterized by X-ray powder diffraction （XRD）, Fourier- transform infrared spectrum （FTIR）, ultraviolet-visible diffuse reflectance spectrum （UV-Vis）, nitrogen physical adsorption and desorption, scanning electron microscopy （SEM） and transmission electron microscopy （TEM）. The characterization results show that many irregular hollows are generated in the TS-1 crystals due to the random dissolution of framework silicon and the volume of the hollow cavities increase with increasing the TEA con- centration, and the treatment temperature and time. The modified TS-1 samples improved in varying degrees the catalyst life for the epoxidation of propylene in a fixed-bed reactor probably due to the generation of the hollows to make it easy for the reactants and products to diffuse out of the channels.

关键词： titanium silicalite-1 triethylamine hollowcavity epoxidation of propylene catalyst life

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Preparation of Magnetic TS-1 and Its Catalytic Activity

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Chemical Research in Chinese Universities 2015年第3期31卷 430-433页

作者： LI Yu XUE Zehui ZHANG Qi SUN Cuitao LI Junping LIU Laishuan School of Chemical Engineering and Environment North University of China Taiyuan 030051 P.R.China

Magnetic TS-1 was synthesized thesis and solvent vaporation method. The with nanosized nickelferrite particles prepared samples were characterized as nuclei via the hydrothermal syn- with N2 adsorption-desorption iso- therms, FTIR spectrometry, Raman spectrometry, X-ray diffraction, Ultraviolet-visible spectroscopy and Vibrating sample magnetometry. The results show that the composite obtained was composed of TS-1 with MFI structure and NiFe204 with spinel structure, its specific surface area was about 316 m2/g, pore volume was 0.12 cm3/g and pore size distribution was in the range of 0.5-0.7 nm. The catalytic activity of the composite was also investigated by its catalyzing the decomposition of rhodamine B oxidized by H2O2 in aqueous solution. In this case Rhodamine B pollutant could be completely degraded within 150 min. Magnetic TS-1 exhibited high photocatalytic efficiency and super paramagnetic nature for cleaning polluted water with the help of magnetic separation.

关键词： Magnetic catalyst titanium silicalite-1 Catalytic decomposition

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