Continuous three-phase 2-butanone ammoximation process via spray forming TS-1 microspheres in a highly efficient jet loop reactor

Chu, Qingyan; Wang, Ping; He, Guangke; Li, Mingdang; Zhu, Hongjun; Pei, Fubin

doi:10.1016/j.cej.2017.05.071

Cited by 18 publications

(8 citation statements)

References 39 publications

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“…A hysteresis loop appeared between 0.5 and 1.0, which was attributed to the mesopores. 29 The surface areas and pore volumes of these samples are shown in Table S4. The Brunauer–Emmett–Teller (BET)-specific surface area (427 m 2 /g) and the microporous surface area (335 m 2 /g) of the sample with the solid content of 25.0% were higher than those of other samples, which would be one of the reasons for its higher catalytic activity.…”

Section: Resultsmentioning

confidence: 99%

“…The spray-forming sample showed a similar catalytic performance to the TS-1 powders . The spray-forming process could prohibit membrane fouling and improved the catalytic stability . Furthermore, the spray-forming process could also reduce the loss of the catalysts.…”

Section: Introductionmentioning

confidence: 81%

“…22 The spray-forming process could prohibit membrane fouling and improved the catalytic stability. 29 Furthermore, the spray-forming process could also reduce the loss of the catalysts.…”

Section: Introductionmentioning

confidence: 99%

“…The spray-forming process has been reported by several research studies. , Samples prepared by the spray-forming process possessed microsphere morphology and showed high activity. The molar ratio of silica to TS-1 should be controlled within the range of 0.05 to 0.11, − and the silica could improve the mechanical strength of the formed body.…”

Section: Introductionmentioning

confidence: 99%

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Fabrication of Microspheres by Nano-TS-1 Crystals via a Spray-Forming Process: From Screening to Scale-up

Niu

Liu

Gao³

et al. 2019

ACS Omega

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The spray-forming process of the nano-titanium silicalite (TS-1) zeolite was investigated and optimized in the lab in order to obtain materials with microsphere morphology and superior catalytic activity in cyclohexanone ammoximation on the industrial scale. The effects of spray-forming parameters, such as the state of the TS-1 raw material, load ratio, solid content, binder content, and calcination temperature, on the physicochemical and catalytic properties of TS-1 microspheres were investigated in detail. It was interesting to find that the shape of the spray-forming sample formed by wet powders was more intact than the sample formed by dried powders. Furthermore, the spray-forming process was successfully scaled up to a large spray device (LGZ-1000) according to the similarity principle of load ratio, and the shape of the TS-1 microspheres was as perfect as the spray-forming samples in the lab. The similarity principle of the load ratio for the spray-forming of titanium silicate was established and verified for the first time. The spray-forming TS-1 microspheres produced in the industry were used in cyclohexanone ammoximation, and ketone conversion and oxime selectivity were as high as 99.9 and 99.4%, respectively.

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 81%

“…22 The spray-forming process could prohibit membrane fouling and improved the catalytic stability. 29 Furthermore, the spray-forming process could also reduce the loss of the catalysts.…”

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Fabrication of Microspheres by Nano-TS-1 Crystals via a Spray-Forming Process: From Screening to Scale-up

Niu

Liu

Gao³

et al. 2019

ACS Omega

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“…For example, cyclohexanone oxime is a key intermediate in the production of caprolactam as nylon-6 monomer [1], and methyl ethyl ketoxime (MEKO) can also be used as an important raw material to synthesize silicone crosslinkers, silicon curing agents, and the blocking agents of isocyanate, etc. [2][3][4]. The traditional synthesis method of oxime is the hydroxylamine method, which is a convenient and valuable method and a non-catalytic oximation of ketone with hydroxylamine derivative like (NH 2 OH) 2 •H 2 SO 4 .…”

Section: Introductionmentioning

confidence: 99%

Nickel-Modified TS-1 Catalyzed the Ammoximation of Methyl Ethyl Ketone

Yang

Wang

et al. 2019

Catalysts

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In this paper, five kinds of transition metal-modified titanium silicalite-1 (M-TS-1) were prepared by an ultrasonic impregnation method. We studied their catalytic performances in the ammoximation of methyl ethyl ketone (MEK). The various M-TS-1 catalysts revealed distinct differences in their MEK ammoximation activity. The nickel-modified TS-1 (Ni-TS-1), especially 3 wt % Ni-TS-1, exhibited a satisfactory conversion of MEK (99%) associated with a high selectivity of methyl ethyl ketoxime (MEKO) (99.3%), which was 6% higher than that of TS-1 under the same conditions. Moreover, the catalyst showed excellent recyclability and the reactivity could be completely recovered after regeneration. The catalysts were characterized by Powder X-ray Diffraction (XRD), Fourier Transformed Infrared Spectra (FT-IR), X-ray photoelectron spectroscopy (XPS), and so on. It was demonstrated that the skeleton structure of TS-1 was basically maintained and the electron environment of the Ti active site was changed after the nickel modification, which can optimize the adsorption capacity and the activation for H2O2. Meanwhile, the surface nickel species reduced the surface acidity of the catalyst, which provided an appropriate pH and inhibited the deep oxidation of oxime.

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Two‐ and Three‐Phase Chemical Reactors

Pangarkar¹

2018

Kirk-Othmer Encyclopedia of Chemical Technology

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This article presents a discussion on three major types of two/three‐phase reactors: bubble column or two/three‐phase sparged reactor, stirred reactor, and venturi loop reactor. The aim is to provide appropriate process design philosophy. The basics of mass transfer accompanied by a chemical reaction are initially presented followed by experimental methods used for discerning reaction kinetics of a multiphase reaction. Metrics for reactor selection have been outlined. A simplified design philosophy that is based on identification of the rate‐controlling step and the associated rate equation has been presented. The intrinsic reaction kinetics do not vary with the type/size of the reactors used. Therefore, the problem reduces to prediction of reactor type and size‐dependent mass transfer coefficients. Subsequent discussion deals with individual reactors with respect to (i) advantages/drawbacks, (ii) areas of application, (iii) hydrodynamic regimes, (iv) gas‐phase holdup, (v) gas–liquid and solid–liquid mass transfer coefficients, k L a and K SL , respectively. The focus is on presenting reliable correlations for k L a and K SL that allow estimation of the rates of corresponding mass transfer steps. Comparison of these with the intrinsic reaction rate yields the rate‐controlling step and associated rate expression for reactor design. The article concludes with a comparison of the performance of the three types chosen for discussion. For the specific reaction chosen, it is concluded that the venturi loop system yields superior performance.

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Continuous three-phase 2-butanone ammoximation process via spray forming TS-1 microspheres in a highly efficient jet loop reactor

Cited by 18 publications

References 39 publications

Fabrication of Microspheres by Nano-TS-1 Crystals via a Spray-Forming Process: From Screening to Scale-up

Fabrication of Microspheres by Nano-TS-1 Crystals via a Spray-Forming Process: From Screening to Scale-up

Nickel-Modified TS-1 Catalyzed the Ammoximation of Methyl Ethyl Ketone

Two‐ and Three‐Phase Chemical Reactors

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