Research progress of hydrogen permeation palladium composite membranes
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摘要: 钯复合膜由于其特殊的透氢机制—溶解/扩散机制，对氢具有极高的选择渗透性，是膜反应器中氢气分离的理想材料。为促进高透氢性、高稳定性钯复合膜的研究与应用，本文综述了钯复合膜的化学镀制备法和化学镀与其他方式结合的复合制备法以及不同类型的复合膜。化学镀是钯复合膜最常用的制备方法，通过与真空、连续流结合可提高钯膜的质量；ⅤB族金属、多孔陶瓷和不锈钢作为化学镀钯膜的载体，可减小钯膜厚度，提高机械强度和透氢性能；在钯膜和多孔载体之间掺入难熔氧化物、沸石、天然矿物、聚合物，可进一步减小钯膜厚度，提高热稳定性和化学稳定性；与纯钯膜相比，Pd-Ag、Pd-Cu、Pd-Au二元合金膜和Pd-Au-Ag三元合金膜在低温下不发生氢脆，可不同程度地改善钯膜的透氢性和抗硫性。最后，对未来钯复合膜的研究方向进行了展望。Abstract: Palladium composite membranes have highly selective permeability to hydrogen due to their special dissolution/diffusion mechanism of hydrogen permeation, and are an ideal material for hydrogen separation in membrane reactors. In order to promote the research and application of palladium composite membranes with high hydrogen permeability and stability, the preparation method of the membranes via electroless plating and its combined with other methods, and different types of the membranes are reviewed in this paper. Electroless plating is the most common preparation method of palladium composite membranes, and the quality of the membranes can be improved by combining with vacuum and continuous flow. Using group ⅤB metals, porous ceramics and stainless steel as the matrix of electroless Pd membranes, the membrane thickness can be reduced, mechanical strength and hydrogen permeability can be improved; The thickness of Pd membranes can be further reduced by adding refractory oxide, zeolite, natural mineral and polymer between Pd membrane and porous matrix, and the thermal and chemical stability can be improved. Compared with pure Pd membrane, Pd-Ag, Pd-Cu, Pd-Au binary alloy membranes and Pd-Au-Ag ternary alloy membrane have no hydrogen embrittlement phenomenon at low temperature, and can improve the hydrogen permeability and sulfur resistance of Pd membranes to a certain degrees. Finally, the future research direction of palladium composite membranes is prospected.
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图 1 各种化学镀技术制备钯复合膜的示意图。(a) 化学镀；(b) 辅助抽吸化学镀；(c) 真空化学镀；(d) 真空辅助连续流化学镀；(e) 化学孔镀
Figure 1. Schematic of palladium composite membranes prepared by various electroless plating techniques. (a) Electroless plating; (b) Assisted suction electroless plating; (c) Vacuum electroless plating; (d) Vacuum-assisted continuous flow electroless plating; (e) Electroless pore-plating
图 2 三种方法制备得到的钯复合膜的SEM图：(a) ELP(化学镀)；(b) SELP(辅助抽吸化学镀)；(c) VELP(真空化学镀)和(d) VELP得到的钯膜的截面形貌[10]
Figure 2. SEM images of palladium composite membranes prepared by three methods: (a) ELP(Electroless plating); (b) SELP(Assisted suction electroless plating); (c) VELP(Vacuum electroless plating) and (d) cross-section morphology of Pd membrane by VELP method[10]
图 3 (a)对称载体和(b)非对称载体的结构示意图
Figure 3. Structure diagram of (a)symmetric support and (b)asymmetric support
图 5 在Sil-1掺杂Pd核修饰的α-Al2O3多孔载体上化学镀钯
Figure 5. Palladium electroless plating on the Sil-1 doped Pd core modified α-Al2O3 porous carrier
图 7 基于钯的膜反应器结构示意图
Figure 7. Schematic diagram of membrane reactor structure based on palladium
表 1 各典型难熔氧化物修饰层组成的钯复合膜性能比较
Table 1. Comparison of the properties of palladium composite membranes composed of typical refractory oxide interlayers
Membranes Preparation method Thickness/
μmTemperature/℃ ΔP/kPa H2 permeability H2 flux H2 selectivity Ref. Pd/Fe2O3,Cr2O3/PSS ELP-PP 18 623-723 0-300 2.83-4.04×10−4 mol/
($ {\mathrm{m}}^{2}\cdot \mathrm{s}{\cdot \mathrm{P}\mathrm{a}}^{0.5}) $$ {\mathrm{\alpha }}_{{\mathrm{H}}_{2}/{\mathrm{N}}_{2}} > 2000 $ [55] Pd/YSZ/PSS ELP 3 773 20 9.86×10−2 mol/
($ {\mathrm{m}}^{2}\cdot \mathrm{s}\cdot {\mathrm{P}\mathrm{a}}^{0.5} $)$ {\mathrm{\alpha }}_{{\mathrm{H}}_{2}/{\mathrm{N}}_{2}}=595 $ [56] Pd/CeO2/PSS ELP-PP 15 623-723 100-200 4.74-6.35×10−4 mol/
($ {\mathrm{m}}^{2}\cdot \mathrm{s}\cdot {\mathrm{P}\mathrm{a}}^{0.5} $)$ {\mathrm{\alpha }}_{{\mathrm{H}}_{2}/{\mathrm{N}}_{2}} > 10000 $ [7] Pd/OMC/PSS ELP-PP 10 673 1.03×10−3 mol/
($ {\mathrm{m}}^{2}\cdot \mathrm{s}\cdot {\mathrm{P}\mathrm{a}}^{0.5} $)$ {\mathrm{\alpha }}_{{\mathrm{H}}_{2}/{\mathrm{N}}_{2}}\ge 24000 $ [57] Pd/YSZ/Al2O3
hollow fiberVCFELP 4 773 100 0.075 mol/
($ {\mathrm{m}}^{2}\cdot \mathrm{s} $)$ {\mathrm{\alpha }}_{{\mathrm{H}}_{2}/{\mathrm{N}}_{2}}=\mathrm{\infty } $ [6] Pd/TiO2/PSS ELP 5.0 723 500 1.58×10−3 mol/
($ {\mathrm{m}}^{2}\cdot \mathrm{s}\cdot {\mathrm{P}\mathrm{a}}^{0.5} $)0.355 mol/
($ \mathrm{m}\cdot \mathrm{s} $)$ {\mathrm{\alpha }}_{{\mathrm{H}}_{2}/{\mathrm{N}}_{2}} $=1700 [43] Pd/Al2O3/PSS ELP 4.4 773 800 2.94×10−3 mol/
($ {\mathrm{m}}^{2}\cdot \mathrm{s}\cdot {\mathrm{P}\mathrm{a}}^{0.5} $)$ {\mathrm{\alpha }}_{{\mathrm{H}}_{2}/\mathrm{H}\mathrm{e}}=1124 $ [58] Pd/SiO2/PSS ELP 2-6 773 50 2.7×10−6 mol/
($ {\mathrm{m}}^{2}\cdot \mathrm{s}\cdot \mathrm{P}\mathrm{a} $)$ {\mathrm{\alpha }}_{{\mathrm{H}}_{2}/{\mathrm{N}}_{2}}=300-450 $ [60] Pd/Alumina sol/
γ-Al2O3/α-Al2O3ELP 4.5 723 100 0.16 mol/
($ {\mathrm{m}}^{2}\cdot \mathrm{s} $)$ {\mathrm{\alpha }}_{{\mathrm{H}}_{2}/{\mathrm{N}}_{2}}=2072 $ [63] Pd/Pd-CeO2/PSS ELP-PP 9 350-450 100-200 4.46-6.39×10−4 mol/
($ {\mathrm{m}}^{2}\cdot \mathrm{s}\cdot {\mathrm{P}\mathrm{a}}^{0.5} $)$ {\mathrm{\alpha }}_{{\mathrm{H}}_{2}/{\mathrm{N}}_{2}} > 10000 $ [12] Pd/Pd-TiO2/PSS ELP-PP 9.7 623-723 50-250 2.80-4.17×10−4 mol/
($ {\mathrm{m}}^{2}\cdot \mathrm{s}\cdot {\mathrm{P}\mathrm{a}}^{0.5} $)$ {\mathrm{\alpha }}_{{\mathrm{H}}_{2}/{\mathrm{N}}_{2}}=\mathrm{\infty } $ [32] Notes：PSS is the porous stainless steel; $ {\mathrm{\alpha }}_{{\mathrm{H}}_{2}/{\mathrm{N}}_{2}},{\mathrm{\alpha }}_{{\mathrm{H}}_{2}/\mathrm{H}\mathrm{e}} $ is the ideal separation factor; YSZ is the yttria stabilized zirconia; OMC is the Ordered Mesoporous Ceria; ELP is Electroless plating; . 
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表 2 原位氧化PSS或加入不同难熔氧化物修饰层修饰的PSS的透氢量比较
Table 2. Comparison of hydrogen flux of PSS oxidized in situ or modified with different refractory oxide interlayers
Sample Temperature/K ΔP/kPa H2$ \mathrm{f} $lux/$ ({\mathrm{mol}}{\cdot \mathrm{m}}^{-2}\cdot {\mathrm{s}}^{-1} $) N2 flux/$({\mathrm{mol}} \cdot {\mathrm{m}}^{-2}\cdot {\mathrm{s}}^{-1} $) Ref. PSS 298 1 ~1.12 [32] TiO2/PSS(or Pd-TiO2/PSS) ~0.60 PSS 298 2 ~0.26 ~0.12 [56] YSZ/PSS ~0.11 ~0.03 PSS 673 1 3.61 1.48 [55] Fe2O3,Cr2O3(600℃)/PSS 2.36 0.82
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表 3 各种钯基膜的H2S中毒及氢通量回收率比较
Table 3. poisoning and recovery of hydrogen flux for various Pd-based membranes
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表 4 SMR或NG SR反应下钯复合膜的甲烷转化率比较
Table 4. Comparison of methane conversion for palladium composite membranes under SMR reaction
Membranes Thickness/
μmReactor
feed gasTemperature/
℃Reaction pressure/
kPaCatalyst
base metalSweep
gas rate/
(mL·min-1)$ {X}_{{\mathrm{C}\mathrm{H}}_{4}} $/
%S/C Active
area/cm2GHSV/
h−1Ref. Pd–Ag Tubular 50 CH4 450 300 Ni/Al2O3 98(N2) 50 2/1
(H2O/CH4)~ 3710 [85] Pd/PSS 13 CH4+
6 vol% CO2400 300 Ni 100 84 3.5/1 44 2600 [84] Pd/PSS 4-5 CH4 550 1013 Ru ~ 82 3 175 2000 [87] Pd/PSS 7 CH4 500 500 Ru/Al2O3 ~ 79.5 3 100 1700 [88] Pd/Al2O3 3.8 CH4 550 2500 Ni ~ 91 ~ 155.0 950 [86] Pd72Au28/YSZ/PSS 5.0 CH4 534 2800 Ru ~ 88 3 16.1 342 [90] Pd95.6-Au4.4/ZrO2/PSS 12 CH4 450 300 Ni 100 48 3.5/1 11.3 2600 [92] 86.63 wt%CH4
+5.86 wt%C2H6
+3.50 wt%C3H8、
+1.51 wt%C4H10
+2.50 wt%CO2450 300 Ni 100 37 3.5/1 11.3 2600 450 300 Ni 100 40%以上 3.5/1 11.3 2600 [93] Notes：$ {X}_{{\mathrm{C}\mathrm{H}}_{4}} $ is the methane conversion, S/C is the steam-to-carbon ratio; GHSV is the gas hourly space velocity.
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