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Synthesis of ZSM-22/ZSM-23 intergrowth zeolite as the catalyst support for hydroisomerization of n-hexadecane

SONG Cheng-ye MENG Ji-peng LI Chuang ZEYAODONG Pahaer LIANG Chang-hai

宋成业, 孟记朋, 李闯, 帕哈尔·泽耀东, 梁长海. ZSM-22/ZSM-23共晶分子筛的合成及其正十六烷加氢异构催化性能[J]. 燃料化学学报. doi: 10.1016/S1872-5813(21)60061-0
引用本文: 宋成业, 孟记朋, 李闯, 帕哈尔·泽耀东, 梁长海. ZSM-22/ZSM-23共晶分子筛的合成及其正十六烷加氢异构催化性能[J]. 燃料化学学报. doi: 10.1016/S1872-5813(21)60061-0
SONG Cheng-ye, MENG Ji-peng, LI Chuang, ZEYAODONG Pahaer, LIANG Chang-hai. Synthesis of ZSM-22/ZSM-23 intergrowth zeolite as the catalyst support for hydroisomerization of n-hexadecane[J]. Journal of Fuel Chemistry and Technology. doi: 10.1016/S1872-5813(21)60061-0
Citation: SONG Cheng-ye, MENG Ji-peng, LI Chuang, ZEYAODONG Pahaer, LIANG Chang-hai. Synthesis of ZSM-22/ZSM-23 intergrowth zeolite as the catalyst support for hydroisomerization of n-hexadecane[J]. Journal of Fuel Chemistry and Technology. doi: 10.1016/S1872-5813(21)60061-0

ZSM-22/ZSM-23共晶分子筛的合成及其正十六烷加氢异构催化性能

doi: 10.1016/S1872-5813(21)60061-0
详细信息
  • 中图分类号: O643.32

Synthesis of ZSM-22/ZSM-23 intergrowth zeolite as the catalyst support for hydroisomerization of n-hexadecane

More Information
  • 摘要: 在二甲胺与二乙胺双模板剂体系中,通过控制二甲胺/二乙胺的摩尔比为24,动态水热合成了ZSM-22/ZSM-23共晶分子筛。采用XRD、FE-SEM、TEM、N2物理吸附、NH3-TPD和吡啶吸附红外等表征手段,考察了ZSM-22/ZSM-23共晶分子筛样品的物理化学性质,并对其负载Pt后在正十六烷加氢异构化反应中的催化性能进行了研究。结果表明,针状的ZSM-22/ZSM-23分子筛具有与ZSM-22和ZSM-23不同的拓扑结构,其Brönsted酸量及中强酸比例较高。对于正十六烷加氢异构化,相比于单一分子筛和机械混合分子筛催化剂,采用共晶分子筛通过浸渍法制备的双功能Pt/ZSM-22/ZSM-23催化剂同时具备Pt/ZSM-22高选择性以及Pt/ZSM-23高转化率的优势,表现出更高的异构体收率,并具有一定的择形效应,异构化产物以单甲基异构体为主。
  • Figure  1.  XRD patterns of the as-synthesized zeolite samples for the gel of 1 SiO2 : 0.01 Al2O3 : w DMA : x DEA : y H2O : m NaOH at 180 °C for z h: (a) varying DMA/DEA ratio; (b) varying crystallization time; (c)varying NaOH amount; (d) varying water quantity

    Figure  2.  XRD patterns of Pt/ZSM-22/ZSM-23, Pt/ZSM-22, Pt/ZSM-23 and Pt/MZSM-22/ZSM-23

    Figure  3.  FE-SEM images of (a) ZSM-22/ZSM-23, (b) ZSM-22, (c) ZSM-23 and (d) MZSM-22/ZSM-23

    Figure  4.  N2 adsorption-desorption isotherms and pore size distribution of various zeolites and catalysts

    Figure  5.  TEM images of (a) Pt/ZSM-22/ZSM-23, (b) Pt/ZSM-22, (c) Pt/ZSM-23 and (d) Pt/MZSM-22/ZSM-23

    Figure  6.  27Al MAS NMR spectra of (a) ZSM-22/ZSM-23, (b) ZSM-22, (c) ZSM-23, and (d) MZSM-22/ZSM-23

    Figure  7.  29Si MAS NMR spectra of (a) ZSM-22/ZSM-23, (b) ZSM-22, (c) ZSM-23, and (d) MZSM-22/ZSM-23

    Figure  8.  NH3-TPD profiles of (a) ZSM-22/ZSM-23, (b) ZSM-22, (c) ZSM-23, and (d) MZSM-22/ZSM-23

    Figure  9.  Py-IR spectra of as-prepared zeolites at different desorption temperatures

    Figure  10.  Conversion of n-C16 (a), selectivity to i-C16 (b), and yield of i-C16 (c) as a function of temperature over different catalysts

    Table  1.   Effect of gel composition and synthetic conditions on the crystallization products

    EntryDMA/DEASDA/SiO2$ {\rm{O}}{{\rm{H}}^ - }/{\rm{Si}}{{\rm{O}}_2} $H2O/SiO2Time (h)ProductRC (%)
    1300.930.15a4572ZSM-23+ Cristobalite
    2240.750.15a4572ZSM-22/ZSM-23+ZSM-571
    3240.750.10a4566ZSM-22/ZSM-23100
    4241.000.15a4572ZSM-22/ZSM-23+ZSM-569
    5180.570.15a4572ZSM-22+ Cristobalite
    6120.390.15a4572ZSM-22+ Cristobalite
    780.810.15a4572ZSM-22+Cristobalite
    8240.750.3a4572ZSM-22/ZSM-23+Cristobalite32
    9240.750.2a4572ZSM-22/ZSM-23+ZSM-549
    10240.750.12a4572ZSM-22/ZSM-23+Cristobalite61
    11240.750.12a4566ZSM-22/ZSM-23+ Cristobalite79
    12240.750.08a4572ZSM-22/ZSM-23+Amorphous83
    13240.750.05a4572Amorphous
    14240.750.3b4572ZSM-22/ZSM-23+Cristobalite
    15240.750.2b4572ZSM-22/ZSM-2373
    16240.750.15b4566ZSM-22/ZSM-2387
    17240.750.10b4566ZSM-22/ZSM-2378
    18240.750.10a4584ZSM-5+Cristobalite
    19240.750.10a4578ZSM-5+ZSM-22/ZSM-23+Cristobalite45
    20240.750.10a4572ZSM-22/ZSM-23+Cristobalite86
    21240.750.10a4560ZSM-22/ZSM-2392
    22240.750.10a4554ZSM-22/ZSM-23+Amorphous49
    23240.750.10a3866ZSM-22/ZSM-23+Cristobalite86
    24240.750.10a3066ZSM-22/ZSM-23+Cristobalite67
    note: a: The alkali source was NaOH; b: The alkali source was KOH
    下载: 导出CSV

    Table  2.   Textural properties of as-prepared zeolites and catalysts

    SampleSurface area (m2/g)Pore volume (cm3/g)Average pore width d (nm)
    SBETaSMicrobSExbVTotalcVMicrob
    ZSM-22/ZSM-23198101970.620.050.51
    ZSM-2216169920.620.030.50
    ZSM-23208109990.510.050.53
    MZSM-22/ZSM-23209981110.660.050.52
    Pt/ZSM-22/ZSM-23203106970.360.050.51
    Pt/ZSM-22157401170.590.020.46
    Pt/ZSM-23198109890.300.050.53
    Pt/MZSM-22/ZSM-232111111000.420.050.53
    note: a: Calculated by Multi-BET equation; b: Measured by t-plot method, SEx = SBETSMicro; c: Determined at P/P0 = 0.99; d: Derived by HK method
    下载: 导出CSV

    Table  3.   SiO2/Al2O3 ratios, 27Al NMR data and NH3-TPD analysis results of various zeolites

    SampleAcidic density (NH3 mmol/g)SiO2/Al2O3 aAl(VI) b (%)
    weakmediumstrongtotal
    ZSM-22/ZSM-230.130.050.050.24799
    ZSM-220.110.050.060.227421
    ZSM-230.180.040.140.35788
    MZSM-22/ZSM-230.150.050.100.307415
    note: a: Determined by ICP-AES; b: Derived from the 27Al-NMR spectra
    下载: 导出CSV

    Table  4.   Acidity distribution of as-synthesized zeolites derived from Py-IR

    SampleLewis acid, CL (mmol/g)Brönsted acid, CB (mmol/g)
    150 °C300 °C450 °C150 °C300 °C450 °C
    ZSM-22/ZSM-230.0600.0450.0250.3150.3120.283
    ZSM-220.1050.0630.0450.0930.0870.078
    ZSM-230.0250.0160.0110.4340.4160.386
    MZSM-22/ZSM-230.0860.0660.0510.2480.2320.228
    下载: 导出CSV

    Table  5.   Product distribution of the n-hexadecane hydroisomerization over different catalysts

    Carbon numberProductDistribution a (wt%)
    Pt/ZSM-22/ZSM-23Pt/ZSM-22Pt/ZSM-23Pt/MZSM-22/ZSM-23
    ≤4≤C48.810.219.77.2
    52M-C43.42.66.03.4
    n-C55.76.09.36.2
    62M-C52.51.72.72.4
    3M-C51.30.81.31.2
    n-C64.34.76.55.3
    72M-C62.21.42.52.7
    3M-C61.40.61.41.6
    n-C73.83.76.45.5
    82M-C71.80.62.02.2
    3M-C70.80.30.91.1
    n-C81.62.32.72.4
    92M-C80.70.60.60.5
    n-C910.80.70.5
    12n-C121.51.81.81.5
    13i-C131.93.52.01.9
    162M-C158.816.25.17.5
    3M-C158.59.76.07.8
    4M-C155.95.23.55.6
    5M-C155.76.74.06.0
    6M-C153.75.53.54.8
    7M-C151512.66.813.2
    DiMe-C149.72.84.79.9
    note: a: Reaction conditions: H2/feed ratio, 300 mL/mL, contact time, 1.12 min, 320 °C and 4.0 MPa
    下载: 导出CSV
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  • 网络出版日期:  2021-03-15

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