ISSN 0253-2778

CN 34-1054/N

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Development of an in situ high-pressure catalytic reactor for synchrotron radiation photoionization mass spectrometry

  • 1.

    National Synchrotron Radiation Laboratory, University of Science and Technology of China, Hefei 230029, China

  • 2.

    School of Mechanical Engineering, Hefei University of Technology, Hefei 230009, China

Cite this:
https://doi.org/10.3969/j.issn.0253-2778.2020.07.002
  • Received Date: 14 April 2020
  • Accepted Date: 01 June 2020
  • Rev Recd Date: 01 June 2020
  • Publish Date: 31 July 2020
    Abstract

  • Abstract

    An in situ high-pressure catalytic reactor which can be coupled with synchrotron radiation vacuum ultraviolet photoionization mass spectrometry was developed. A tapered micro orifice was designed at the top of the high-pressure reaction tube for the first sampling, along with a quartz nozzle downstream connected with the mass spectrometry for the second sampling. Thus, the working pressure range of the reactor could reach from atmosphere to 3.6 MPa. In this design, gas dynamics theory and COMSOL Multiphysics software were applied for simulation, and the simulation results were verified by experimental measurements. The dimethyl ether (DME) carbonylation to methyl acetate reaction under different pressures near working conditions was studied by in situ mass spectrometry simultaneously. It was found that the selectivity of methyl acetate obtained in real time increased significantly with the increase of reaction pressure. The development of the in situ high-pressure catalytic reactor will be helpful to further study gas-solid catalytic reaction mechanism under high pressure.

    Abstract

    An in situ high-pressure catalytic reactor which can be coupled with synchrotron radiation vacuum ultraviolet photoionization mass spectrometry was developed. A tapered micro orifice was designed at the top of the high-pressure reaction tube for the first sampling, along with a quartz nozzle downstream connected with the mass spectrometry for the second sampling. Thus, the working pressure range of the reactor could reach from atmosphere to 3.6 MPa. In this design, gas dynamics theory and COMSOL Multiphysics software were applied for simulation, and the simulation results were verified by experimental measurements. The dimethyl ether (DME) carbonylation to methyl acetate reaction under different pressures near working conditions was studied by in situ mass spectrometry simultaneously. It was found that the selectivity of methyl acetate obtained in real time increased significantly with the increase of reaction pressure. The development of the in situ high-pressure catalytic reactor will be helpful to further study gas-solid catalytic reaction mechanism under high pressure.
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    • References(29)
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    HE T, REN P G, LIU X C, et al. Direct observation of DME carbonylation in the different channels of H-MOR zeolite by continuous-flow solid-state NMR spectroscopy[J]. Chemical Communications, 2015,51(94):16868-16870.
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    CHEUNG P, BHAN A, IGLESIA E, et al. Site requirements and elementary steps in dimethyl ether carbonylation catalyzed by acidic zeolites[J]. Journal of Catalysis, 2007, 245(1): 110-123.
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    董大勤，袁凤隐. 压力容器设计手册[M].北京：化学工业出版社，2005：191.
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    JOUSTEN K. Handbook of Vacuum Technology[M]. Weinheim, Germany: Wiley-VCH, 2016.
    [24]
    HE X, FENG X , ZHONG M, et al. The influence of Laval nozzle throat size on supersonic molecular beam injection[J]. Journal of Modern Transportation, 2014, 22: 118-121.
    [25]
    GASSER I, RYBICKI M. Modelling and simulation of gas dynamics in an exhaust pipe[J]. Applied Mathematical Modelling, 2013, 37(5): 2747-2764.
    [26]
    WANG L P , QIU A C , KUAI B , et al. Study of the gas-puff line mass and density from Laval nozzle[J]. High Power Laser & Particle Beams, 2005, 17(2): 295-298.
    [27]
    HE T, LIU X C, BAO X H, et al. Role of 12-ring channels of mordenite in DME carbonylation investigated by solid-state NMR[J]. Journal of Physical Chemistry C, 2016,120(39): 22526-22531.
    [28]
    HUANG S Y, LI Y, MAX B, et al. Enhanced activity of Ce-incorporated MOR in DME carbonylation through tailoring the distribution of Bronsted acid[C]// 253rd ACS National Meeting & Exposition. Washington DC: American Chemical Society, 2017.
    [29]
    XUE H F, HUANG X M, SHEN W J, et al. Dimethyl ether carbonylation to methyl acetate over nanosized mordenites[J]. Industrial & Engineering Chemistry Research, 2013, 52(33): 11510-11515.)
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    [1]
    MANZER L E. Toward catalysis in the 21st century chemical industry[J]. Catalysis Today, 1993,18(2): 199-207.
    [2]
    SCHMIDT F. The importance of catalysis in the chemical and non-chemical industries[J]. Basic Principles in Applied Catalysis, 2004, 35(17): 3-16.
    [3]
    GIDDEY S, BADWAL S. Review of electrochemical ammonia production technologies and materials[J]. International Journal of Hydrogen Energy, 2013,38(34):14576-14594.
    [4]
    YARULINA I, CHOWDURY A D, GASCON J, et al. Recent trends and fundamental insights in the methanol-to-hydrocarbons process[J]. Nature Catalysis, 2018,1(6): 398-411.
    [5]
    OLSBYE U, SVELLE S, BJORGEN M, et al. Conversion of methanol to hydrocarbons:How zeolite cavity and pore size controls product selectivity[J]. Angewandte Chemie-International Edition, 2012, 51(24): 5810-5831.
    [6]
    AIL S S, DASAPPA S. Biomass to liquid transportation fuel via Fischer Tropsch synthesis: Technology review and current scenario[J]. Renewable & Sustainable Energy Reviews, 2016,58: 267-286.
    [7]
    ZHONG L S, YU F, AN Y L, et al. Cobalt carbide nanoprisms for direct production of lower olefins from syngas[J]. Nature, 2016, 538(7623): 84-87.
    [8]
    WEI J, GE Q J, SUN J, et al. Directly converting CO2 into a gasoline fuel[J]. Nature Communications, 2017, 8: Article number 15147.
    [9]
    JIAO F, LI J J, PAN X L, et al. Selective conversion of syngas to light olefins[J]. Science, 2016, 351(6277): 1065-1068.
    [10]
    HOU Y H, HAN W C, XIA W S, et al. Structure sensitivity of La2O2CO3 catalysts in the oxidative coupling of methane[J]. ACS Catalysis, 2015, 5(3): 1663-1674.
    [11]
    OTSUKA K, JINNO K, MORIKAWA A, et al. Active and selective catalysts for the synthesis of C2H4 and C2H6 via oxidative coupling of methane[J]. Journal of Catalysis, 1986,100(2): 353-359.
    [12]
    NGUYEN T N, NHAT T P, TAKIMOTO K, et al. High-throughput experimentation and catalyst informatics for oxidative coupling of methane[J]. ACS Catalysis, 2019,10: 921-932.
    [13]
    WEN W, YU S S, PAN Y, et al. Formation and fate of formaldehyde in methanol-to-hydrocarbon reaction: In situ synchrotron radiation photoionization mass spectrometry study[J]. Angewandte Chemie, 2020,132(12): 4903-4908.
    [14]
    ZHOU Z Y, DU X W, QI F, et al. The vacuum ultraviolet beamline/endstations at NSRL dedicated to combustion research[J]. Journal of Synchrotron Radiation, 2016, 23(4):1035-1045.
    [15]
    CHEUNG P, BHAN A, IGLESIA E, et al. Selective carbonylation of dimethyl ether to methyl acetate catalyzed by acidic zeolites[J]. Angew Chem Int Ed Engl, 2006,45(10):1617-1620.
    [16]
    HE T, REN P G, LIU X C, et al. Direct observation of DME carbonylation in the different channels of H-MOR zeolite by continuous-flow solid-state NMR spectroscopy[J]. Chemical Communications, 2015,51(94):16868-16870.
    [17]
    LIU J L, XUE H F, SHEN W J, et al. Dimethyl ether carbonylation to methyl acetate over HZSM-35[J]. Catalysis Letters, 2010,139(1-2): 33-37.
    [18]
    XUE H, HUANG X Y, SHEN W J, et al. Selective dealumination of mordenite for enhancing its stability in dimethyl ether carbonylation[J]. Catalysis Communications, 2013, 37: 75-79.
    [19]
    BORONAT M, MARTINEZ C, CORMA A. Mechanistic differences between methanol and dimethyl ether carbonylation in side pockets and large channels of mordenite[J]. Physical Chemistry Chemical Physics, 2011,13(7): 2603-2612.
    [20]
    CHEUNG P, BHAN A, IGLESIA E, et al. Site requirements and elementary steps in dimethyl ether carbonylation catalyzed by acidic zeolites[J]. Journal of Catalysis, 2007, 245(1): 110-123.
    [21]
    董大勤，袁凤隐. 压力容器设计手册[M].北京：化学工业出版社，2005：191.
    [22]
    达道安. 真空设计手册[M].第3版.北京：国防工业出版社，2004：102-103.
    [23]
    JOUSTEN K. Handbook of Vacuum Technology[M]. Weinheim, Germany: Wiley-VCH, 2016.
    [24]
    HE X, FENG X , ZHONG M, et al. The influence of Laval nozzle throat size on supersonic molecular beam injection[J]. Journal of Modern Transportation, 2014, 22: 118-121.
    [25]
    GASSER I, RYBICKI M. Modelling and simulation of gas dynamics in an exhaust pipe[J]. Applied Mathematical Modelling, 2013, 37(5): 2747-2764.
    [26]
    WANG L P , QIU A C , KUAI B , et al. Study of the gas-puff line mass and density from Laval nozzle[J]. High Power Laser & Particle Beams, 2005, 17(2): 295-298.
    [27]
    HE T, LIU X C, BAO X H, et al. Role of 12-ring channels of mordenite in DME carbonylation investigated by solid-state NMR[J]. Journal of Physical Chemistry C, 2016,120(39): 22526-22531.
    [28]
    HUANG S Y, LI Y, MAX B, et al. Enhanced activity of Ce-incorporated MOR in DME carbonylation through tailoring the distribution of Bronsted acid[C]// 253rd ACS National Meeting & Exposition. Washington DC: American Chemical Society, 2017.
    [29]
    XUE H F, HUANG X M, SHEN W J, et al. Dimethyl ether carbonylation to methyl acetate over nanosized mordenites[J]. Industrial & Engineering Chemistry Research, 2013, 52(33): 11510-11515.)
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