Studies on influence of hydrogen and carbon monoxide concentration on reduction progression behavior of molybdenum oxide catalyst

Temperature programmed reduction (TPR) analysis was applied to investigate the chemical reduction progression behavior of molybdenum oxide (MoO₃) catalyst. The composition and morphology of the reduced phases were characterized by X-ray diffraction spectroscopy (XRD), X-ray photoelectron spectroscopy (XPS), and field emission scanning electron microscopy (FE-SEM). The reduction progression of MoO₃ catalyst was attained with different reductant types and concentration (10% H₂/N₂, 10% and 20% CO/N₂ (%, v/v)). Two different modes of reduction process were applied. The first approach of reduction involved non-isothermal mode reduction up to 700 °C, while the second approach of reduction involved the isothermal mode reduction for 60 min at 700 °C. Hydrogen temperature programmed reduction (H₂-TPR) results showed the reduction progression of three-stage reduction of MoO₃ (Mo⁶⁺ → Mo⁵⁺ → Mo⁴⁺ → Mo⁰) with Mo⁵⁺ and Mo⁴⁺. XRD analysis confirmed the formation of Mo₄O₁₁ phase as an intermediate phase followed by MoO₂ phase. After 60 min of isothermal reduction, peaks of metallic molybdenum (Mo) appeared. Whereas, FESEM analysis showed porous crater-like structure on the surface cracks of MoO₂ layer which led to the growth of Mo phase. Meanwhile, the reduction of MoO₃ catalyst in 10% carbon monoxide (CO) showed the formation of unstable intermediate phase of Mo₉O₂₆ at the early stage of reduction. Furthermore, by increasing 20% CO led to the carburization of MoO₂ phase, resulted in the formation of Mo₂C rather than the formation of metallic Mo, as confirmed by XPS analysis. Therefore, the presented study shows that hydrogen gave better reducibility due to smaller molecular size, which contributed to high diffusion rate and achieved deeper penetration into the MoO₃ catalyst compared to carbon monoxide reductant. Hence, the reduction of MoO₃ in carbon monoxide atmosphere promoted the formation of Mo₂C which was in agreement with the thermodynamic assessment.     

In situ construction of oxygen deficient MoO3-x nanosheets/porous graphitic carbon nitride for enhanced photothermal-photocatalytic hydrogen evolution

In this work, the photocatalysts containing oxygen-deficient molybdenum oxide and macroscopic three-dimensional porous graphitic carbon nitride phase composite (MoO_3-x/PCN) were prepared by in situ self-assembly method. The crystal phase and structure were characterized by XRD, XPS, FT-IR, SEM, and TEM measurements. Hydrogen production results showed that introducing of MoO_3-x resulted in a higher hydrogen production rate of MoO_3-x/PCN composite catalyst than that of PCN. Among them, the highest hydrogen production rate of 2336.15 μmol g⁻¹ h⁻¹ was achieved for MoO_3-x-10/PCN, which was 2.23 times higher than PCN (1048.00 μmol g⁻¹ h⁻¹). When the reaction system temperature was 100 °C, the photothermal hydrogen production rate of MoO_3-x-10/PCN was 8902.00 μmol g⁻¹ h⁻¹, which was 3.81 times higher than that at room temperature. PL spectra, UV–vis spectra and photoelectrochemical measurements showed that the localized surface plasmon resonance (LSPR) effect of MoO_3-x effectively enhanced the photo response range and increased the temperature of the reaction system. ESR measurements showed that he composites should follow the Z-scheme charge transfer mechanism, the electrons in the CB of MoO_3-x further migrate to the VB of PCN, which hinders the charge complexation in MoO_3-x and PCN, improving the hydrogen production activity. This study provides a new idea for constructing a plasma-based photothermal synergistic catalytic hydrogen production strategy.     

Hydrogen production by catalytic decomposition of methane over Fe based bi-metallic catalysts supported on CeO2–ZrO2

Methane decomposition to produce hydrogen was studied over iron based bimetallic catalysts supported on cerium-zirconium oxide in a continuous flow fixed bed reactor at 700 °C. 15 wt% Fe/CeZrO₂ was prepared by wetness impregnation and the promoted Fe catalysts (15 Fe-5 Co/CeZrO₂ and 15 Fe-5 Mo/CeZrO₂) were prepared by co-impregnation technique. Mo promoted Fe catalyst exhibited the maximum surface area of 24.08 m²/g. X-ray diffraction studies revealed that Fe₂O₃, Co₃O₄ and MoO₃ were the phases present in freshly calcined catalysts, while the reduced catalysts consisted of phases including elemental Fe, Mo and Fe–Co alloys. Both X-ray diffraction and temperature programmed reduction studies confirmed the complete reduction of metal oxide species under H₂ at 700 °C. The catalytic activity of Fe/CeZrO₂ was enhanced upon addition of Co and Mo as promoters. The initial hydrogen yield on 15 Fe-5 Mo/CeZrO₂ was ~90% and it decreased with increase in time on stream (TOS), and finally stabilized around ~50% after 125 min of TOS. The Co promoted catalyst exhibited similar activity while the initial hydrogen yield on 15 Fe/CeZrO₂ was ~83% and dropped to ~33% after 125 min of TOS. Graphitic carbon, Fe₃C and Mo₂C phases were observed in the XRD patterns of spent catalysts along with elemental Fe and Fe–Co alloy. It was evident from temperature programmed oxidation results that coke formation which deactivates the catalyst was dominant in 15 Fe/CeZrO₂ when compared to the promoted (Co and Mo) Fe catalysts where carbon nanostructures were dominant. Both scanning electron microscopy (SEM) and transmission electron microscopy (TEM) confirmed the formation of carbon nanostructures on the surface of spent catalysts. The Fe based catalysts supported both tip and base-growth mechanisms for the growth of carbon nanostructures.     

The effect of SnO2 on enhancing electrocatalytic property of palladium toward formic acid oxidation

Although palladium (Pd) based materials are considered the best catalyst for formic acid oxidation reaction (FAOR), they are still confronted with a lot of barriers, such as the growth/sintering of Pd nanoparticles (NPs) and the accumulation of adsorbed poisoning intermediates. Herein, tin dioxide (SnO₂) decorated carbon black was utilized as the catalyst carrier to synthesize Pd/SnO₂/C for FAOR. The introduction of SnO₂ significantly reduced the particle size of Pd NPs and forming the Pd–O–Sn structure. Compared with Pd/C, Pd/SnO₂/C owned higher concentration of O_ads and less adsorption amount of poisoning intermediates. The oxygen atoms adsorbed on Pd surface were rapidly transferred to SnO₂ due to the spillover effect. The FAOR reaction kinetic results showed that the introduction of SnO₂ accelerated the diffusion rate of formic acid on the electrode surface. Pd/SnO₂/C exhibited high specific activity (5.97 mA cm⁻²), excellent durability, and high anti-CO poisoning ability toward FAOR due to the introduction of SnO₂.     

Synthesis of ultrafine low loading Pd–Cu alloy catalysts supported on graphene with excellent electrocatalytic performance for formic acid oxidation

Here, surfactant free composite catalysts (Pd–Cu/rGO) with Pd–Cu alloy nanoparticles uniformly distributed on graphene sheets are successfully prepared via a facile hydrothermal approach. Compared with pure Pd/rGO catalyst, the introduction of copper could dramatically enhance the performance of the catalyst in the electrocatalytic formic acid oxidation (FAO) due to the strain effect and the ligand effect. With the optimized atomic ratio of 3:1 between palladium and copper, the alloy nanoparticle shows the smallest size of 2.12 nm, thus endowing the composite catalyst with highest catalytic efficiency. With Pd load as low as 14.5%, a maximum mass current density of 1580 mA mg_Pd⁻¹, and residual current of 69.93 mA mg_Pd⁻¹ at 3000 s was achieved with our Pd₃Cu₁/rGO catalyst in the electrocatalytic FAO process.     

Biomass-derived carbon nanosheets coupled with MoO2/Mo2C electrocatalyst for hydrogen evolution reaction

Transition metal carbide such as molybdenum carbide has been widely used in electrolytic water for hydrogen production due to its potential catalytic property. The synthesis of molybdenum carbide-based high-efficient catalysts by simple process remains great challenges. Herein, Mo oxide/carbide material with hybrid morphology was synthesized by carbonizing mixture of lotus roots and Mo salt. The as-obtained material consists of MoO₂/Mo₂C (MOMC) anchored on biomass-derived nitrogen-doped carbon (NC) matrix. The results show that as-prepared material displays leaf-like and belt-like nanosheets, and the MOMC/NC catalyst with optimal Mo contents exhibits an excellent activity with a low overpotential of 138 mV to drive 10 mA cm^?2 and Tafel slope is 56.7 mV dec^?1 in alkaline medium, indicating that as-prepared catalyst will have promising application in the field of catalysis.     

Top-down preparation of Ni–Pd–P@graphitic carbon core-shell nanostructure as a non-Pt catalyst for enhanced electrocatalytic reactions

Electrochemical reactions such as the oxygen evolution reaction (OER), oxygen reduction reaction (ORR), and methanol oxidation reaction (MOR) are essential for energy conversion applications such as water electrolysis and fuel cells. Furthermore, Pt or Ir-related materials have been extensively utilized as electrocatalysts for the OER, ORR, and MOR. To reduce the utilization of precious metals, innovative catalyst structures should be proposed. Herein, we report a bi-metallic phosphide (Ni₂P and PdP₂) structure surrounded by graphitic carbon (Ni–Pd–P/C) with an enhanced electrochemical activity as compared to conventional electrocatalysts. Despite the low Pd content of 3 at%, Ni–Pd–P/C exhibits a low overpotential of 330 mV at 10 mA cm^?2 in the OER, high specific activity (2.82 mA cm^?2 at 0.8 V) for the ORR, and a high current density of 1.101 A mg^?1 for the MOR. The superior electrochemical performance of Ni–Pd–P/C may be attributed to the synergistic effect of the bi-metallic phosphide structure and core-shell structure formed by graphitic carbon.     

A study on the catalytic hydrogenation of N-ethylcarbazole on the mesoporous Pd/MoO3 catalyst

Mesoporous MoO₃ shows an apparent activity in the catalytic hydrogenation of N-ethylcarbazole (NEC), where a significant amount of tetrahydro-N-ethylcarbazole (4H-NEC) and perhydro-N-ethylcarbazole (PNEC) are detected with the hydrogen uptake of 0.97 wt% after 6 h when the temperature rises to 220 °C. 0.5 wt% Pd/MoO₃ catalyst shows a superior catalytic efficiency than the traditional precious metal catalysts 0.5 wt% Ru/Al₂O₃ and 0.5 wt% Pd/Al₂O₃, especially in the conversion of Octahydro-N-ethylcarbazole (8H-NEC) to PNEC. The hydrogenation mechanism of MoO₃ is completely different from the traditional precious metal catalysts. With the presence of a small amount of Pd, the breaking of HH bond is greatly accelerated, result in the promotion of hydrogen spillover rate and the increase of the concentration of hydrogen molybdenum bronze H_xMoO₃, which improves the catalytic efficiency of the MoO₃ catalyst. Rise the temperature also helps increasing the concentration of H in H_xMoO₃.     

One‐pot synthesis of Pd‐MoO2/C by microwave sintering as an efficient electrocatalyst for ethanol oxidation reaction

The composite catalysts of Pd‐MoO₂/C for ethanol oxidation reaction (EOR) were prepared by microwave sintering. MoO₃ was thermally reduced to MoO₂ by carbon black in the preparing process of the Pd‐MoO₂/C material. The TEM analysis showed that Pd‐MoO₂ was well polymerized. Chronoamperometric, cyclic voltammetry, and electrochemical impedance spectra methods were applied to reveal the performance for EOR at room temperature. The Pd‐MoO₂/C electrode exhibited considerable high activity and stability. MoO₂ as a co‐catalyst significantly improved the catalytic activity of Pd‐MoO₂/C for EOR.     

A “special” anhydrous system for the preparation of alloyed Pd1Ce0.5 nanonetworks catalyst supported on carbon nanotubes with high electrochemical oxidation activity for formic acid

Herein, Pd₁Ce_0.5 alloy nanonetworks (ANNs) on multi-walled carbon nanotubes (MWCNTs) supported bimetallic catalyst (referred to Pd₁Ce_0.5/MWCNTs-D) was prepared in deep eutectic solvents (DESs). The Pd₁Ce_0.5/MWCNTs-D catalyst shows remarkable catalytic performance toward formic acid oxidation (FAO) (1968.5 mA mg_Pd^?1) and better CO anti-poisoning capability compare with Pd/MWCNTs-D, Pd/MWCNTs-W (prepared in water) and commercial Pd/C catalysts. The excellent network structure and synergistic effect are the main reasons for the improvement of electrochemical activity of Pd₁Ce_0.5/MWCNTs-D catalyst. This study provides a new method for preparation of high performance Pd-based electrocatalysts for direct formic acid fuel cell (DFAFC) applications.     

The role of hydrogen bronzes in the hydrogenation of polyfunctional reagents: cinnamaldehyde,furfural and 5-hydroxymethylfurfural over Pd/HxWO3 and Pd/HxMoO3 catalysts

Differences in the activity of Pd/WO₃ and Pd/MoO₃ (Pd loading 0.4–4 wt%) catalysts in competitive hydrogenations of the CC and CO groups in polyfunctional reagents have been studied as a function of two effects: (1) the in situ formation of hydrogen bronzes, H_xWO₃ and H_xMoO₃, and (2) the electronic interaction between the supports and the metallic Pd. The cinnamaldehyde (CAL), furfural (FU) and 5-hydroxymethylfurfural (HMF) were hydrogenated under mild reaction conditions. The formation of hydrogen bronzes in Pd/WO₃ and physical mixture of Pd/WO₃ with supporting WO₃ oxide upon exposure to H₂ was also studied using the gas flow-through microcalorimetry. In both Pd/MoO₃ and Pd/WO₃ catalysts, the electronic interactions contributed to the promotion of selectivity toward the CO hydrogenation in CAL and FU, yet in Pd/MoO₃ this effect was much more pronounced. On the other hand, apart from increasing the overall reaction rate, the formation of hydrogen bronzes remarkably enhances the CC hydrogenation in CAL, as well as the decarbonylation of FU to furan and hydrogenolysis of C–OH in HMF to 5-methylfurfural. The bronze effects are significantly stronger in H_xWO₃, compared to H_xMoO₃, which may be related to higher H-species mobility and weaker H-bonding in the W–O–H (54 kJ/mol H₂) than in the Mo–O–H (100 kJ/mol H₂). This may also explain very high tendency of Pd/WO₃ to furan ring hydrogenation in FU and HMF as well as almost selective (>98%) hydrogenation of furfuryl alcohol to tetrahydrofurfuryl alcohol.     

Synthesis of highly active and stable Pd/C catalysts toward HCOOH dehydrogenation by a simple NH3 adsorption method

Pd catalysts supported on activated carbon (Pd/C–NH₃) toward HCOOH dehydrogenation were prepared by a simple adsorption method using ammonia (NH₃) and Ar as the working gas. The results show that the TOF_initial of Pd/C–NH₃ was 459.8 h⁻¹ at 50 °C. When the reaction was carried out for 4 h, the HCOOH dehydrogenation ratio over Pd/C–NH₃ was about 81.2%, which was 1.15 and 1.13 times, respectively, as that of the as-prepared Pd/C catalyst without any treatment (Pd/C–As) and the Pd/C catalyst purchased from Sigma-Aldrich (Pd/C-CM). The total amount of H₂ and CO₂ produced by using Pd/C–NH₃ to decompose HCOOH in the third cycle was 99.4% of the gas produced by the first reaction cycle, and 1.80 and 12.60 times, respectively, as that of Pd/C–As and Pd/C-CM. The characterization results indicated that the Pd active species in Pd/C–NH₃ migrated to the outer surface of the carbon support during the reaction, and the pore volume of the carbon support became larger, which were beneficial to the reaction. These factors made Pd/C–NH₃ exhibit excellent HCOOH dehydrogenation activity and stability. NH₃ adsorption is a simple and effective method for preparing high-performance Pd/C HCOOH dehydrogenation catalysts, and has important guiding significance for the preparation of other carbon supported noble metal catalysts.     

Effect of chemisorbed CO on MoOx–Pt/C electrode on the kinetics of hydrogen oxidation reaction

The influence of poisoning of MoO_x–Pt catalyst by CO on the kinetics of H₂ oxidation reaction (HOR) at MoO_x–Pt electrode in 0.5 mol dm⁻³ HClO₄ saturated with H₂ containing 100 ppm CO, was examined on rotating disc electrode (RDE) at 25 °C. MoO_x–Pt nano-catalyst prepared by the polyole method combined with MoO_x post-deposition was supported on commercial carbon black, Vulcan XC-72. The MoO_x–Pt/C catalyst was characterized by TEM technique. The catalyst composition is very similar to the nominal one and post-deposited MoO_x species block only a small fraction of the active Pt particle surface area. MoO_x deposition on the carbon support can be ruled out from the EDAX results and from the low mobility of these oxides under used conditions. Based on Tafel–Heyrovsky–Volmer mechanism the corresponding kinetic equations from a dual-pathway model were derived to describe oxidation current–potential behavior on RDE over entire potential range, at various CO coverages. The polarization RDE curves were fitted with derived polarization equations according to the proposed model. The fitting showed that the HOR proceeded most likely via the Tafel–Volmer (TV) pathway. A very high electrocatalytic activity observed at MoO_x–Pt catalyst for the hydrogen oxidation reaction in the presence of 100 ppm CO is achieved through chemical surface reaction of adsorbed CO with Mo surface oxides.     

NH3 plasma synthesis of N-doped activated carbon supported Pd catalysts with high catalytic activity and stability for HCOOH dehydrogenation

Plasma is a simple and effective method to prepare N-doped carbon materials and supported metal catalysts. In this work, Pd/C–C(NH₃) and Pd/C–P(NH₃) catalysts are prepared by heat treatment and cold plasma methods using Ar and NH₃ as the working gas. The activity and stability of obtained catalysts are tested by formic acid dehydrogenation reaction. The results show that TOF_initial of Pd/C–P(NH₃) is 527.1 h⁻¹ at 50 °C, and the HCOOH decomposition rate is about 89.2% at 4 h. The hydrogen production of Pd/C–P(NH₃) when used in first and third cycle are 1.14 and 1.14 times than that of Pd/C–C(NH₃), and 1.24 and 13.24 times than that of commercial Pd/C. Various characterization techniques are used to characterize the structure of the prepared Pd/C catalysts. The results indicate that NH₃ plasma is milder than NH₃ thermal treatment. The high activity and stability of Pd/C–P(NH₃) are mainly due to the NH₃ cold plasma effectively achieving N-doping of the carbon support, and Pd nanoparticles with a small size and high dispersion. Atmospheric pressure NH₃ cold plasma provides an effective method to prepare high-performance Pd/C catalysts for HCOOH dehydrogenation and plays a guiding role in the preparation of high-performance carbon-supported noble metal catalysts.     

Improved hydrogen storage performance of defected carbon nanotubes with Pd spillover catalysts dispersed using supercritical CO2 fluid

Hydrogen storage properties of carbon nanotubes (CNTs) modified by oxidative etching and decoration of Pd spillover catalysts are investigated. A mixed H₂SO₄/H₂O₂ solution containing ferrous ions (Fe²⁺) is useful to open the caps, to shorten the length, and to generate defects on CNTs. The Pd catalysts are deposited on the CNTs with the aid of supercritical carbon dioxide (scCO₂); as a result, a highly dispersed Pd nanoparticles and an intimate connection between Pd and carbon surface can be obtained. Combination of the two approaches can optimize a hydrogen spillover reaction on CNTs, resulting in a superior hydrogen storage capacity of 1.54 wt% (at 25 °C and 6.89 MPa), which corresponds to an enhancement factor of ∼4.5 as compared to that of pristine CNTs.     

Atomic interface engineering: Strawberry-like RuO2/C hybrids for efficient hydrogen evolution from ammonia borane and water

Efficient hydrogen production plays a key role in establishing hydrogen economy in the current world. In this study, we fabricated ultrafine RuO₂ nanoparticles on carbon black to form a strawberry-like RuO₂/C hybrid, using by a solid-phase grinding and subsequent low-temperature annealing. The synthesized hybrid displays very low reaction activation energy (28.5 KJ mol^?1) for hydrogen evolution from ammonia borane. In case of hydrogen evolution from alkaline water, it also exhibits a remarkably improved electrocatalytic activity than a commercial Pt/C, with an ultra-low overpotential of 8 mV (at 10 mA cm^?2). For the above bifunctional catalyst, the formed C–Ru–C bonds between the ruthenium oxide and carbon result in the ultrahigh activity of the hybrid, as evidenced by DFT results. This work offers a guideline to synthesize efficient metal-based (Ru, Pd, Rh, Ir, Au, etc.) catalysts with smart structures for catalysis.     

Oxidative catalytic steam gasification of sugarcane bagasse for hydrogen rich syngas production

Reactive Flash Volatilization (RFV) is an emerging thermochemical method to produce tar free hydrogen rich syngas from waste biomass at relatively lower temperature (<900 °C) in a single stage catalytic reactor within a millisecond residence time. Here, we show catalytic RFV of bagasse using Ru, Rh, Pd, or Re promoted Ni/Al₂O₃ catalysts under steam rich and oxygen deficient environment. The optimum reaction conditions were found to be 800 °C, steam to carbon ratio = 1.7 and carbon to oxygen ratio = 0.6. Rh–Ni/Al₂O₃ performed the best, resulting in highest hydrogen concentration in the synthesis gas at 54.8%, with a corresponding yield of 106.4 g-H₂/kg bagasse. A carbon conversion efficiency of 99.96% was achieved using Rh–Ni, followed by Ru–Ni, Pd–Ni, Re–Ni and mono metallic Ni catalyst in that order. Alkali and Alkaline Earth Metal species present in the bagasse ash and char, that deposited on the catalyst, was found to enhance its activity and stability. The hydrogen yield from bagasse was higher than previously reported woody biomass and comparable to the microalgae.     

Insight towards kinetics and stability of carbon supported Pd–Y2O3 as cathode catalyst for polymer electrolyte fuel cells

Pd–Y₂O₃ on carbon (Pd–Y₂O₃/C) in different mass ratios of Pd to Y₂O₃ (1:1, 2:1, 3:1) were prepared and subjected as cathode electrocatalyst for polymer electrolyte fuel cells (PEFC). X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used to determine the structure, crystalline size and dispersion of Pd–Y₂O₃/C respectively. The electrochemical characterizations of the electrocatalysts were evaluated from Cyclic Voltammetry (CV) and Linear Sweep Voltammetry (LSV). These electrocatalysts were evaluated for their catalytic activity towards oxygen reduction reaction (ORR) in fuel cell. Pd₂–Y₂O₃/C catalyst shows higher power density of 325 mW cm^?2 than Pd₁–Y₂O₃/C, Pd₃–Y₂O₃/C and Pd/C.     

Carbon nanotubes-promoted Co–B catalysts for rapid hydrogen generation via NaBH4 hydrolysis

In this work, multiwalled carbon nanotubes (MWCNTs) promoted Co–B catalysts for NaBH₄ hydrolysis have been designed and synthesized. The structural features of as-prepared catalysts have been investigated and discussed as a function of MWCNTs contents by X-ray diffraction, X-ray photoelectron spectra, N₂ adsorption/desorption isotherms, scanning electron microscope. The results show that the catalysts still maintain an amorphous structure with the addition of carbon nanotubes promoter. However, the appropriate amount of MWCNTs promoter in Co–B catalysts leads to large specific surface area, fine dispersion of active components, increased active sites and high electron density at active sites. Moreover, hydrogen spillover on the catalyst is promoted, which contributes to regeneration of active sites and accelerating catalytic cycle. Among all the experimental samples, it is found that the Co–B catalyst promoted by 10 wt% carbon nanotubes exhibits optimal catalytic activity with remarkably high hydrogen generation rate of 12.00 L min⁻¹·g_catalyst⁻¹ and relatively good stability.     

Preparation of dandelion-like Co–Mo–P/CNTs-Ni foam catalyst and its performance in hydrogen production by alcoholysis of sodium borohydride

A dandelion-like CNTs-Ni foam composite carrier supported Co–Mo–P ternary alloy catalyst (Co–Mo–P/CNTs-Ni foam) was prepared by electroless plating. The structure of Co–Mo–P/CNTs-Ni foam catalyst is characterized by XRD, SEM, XPS and EDS. The particle size of Co–Mo–P ternary alloy nanoparticles is about 80 nm. The Co–Mo–P/CNTs-Ni foam completely retains the tubular structure of carbon nanotubes and the gaps between carbon nanotubes of CNTs-Ni carrier, which increases the specific surface area of the catalyst and the flow space of reactants and products. Co–Mo–P/CNTs-Ni foam catalyzes sodium borohydride alcoholysis to produce hydrogen at a maximum rate of 2.64 L ·min⁻¹ ·g⁻¹, and the reaction activation energy is 47.27 kJ ·mol⁻¹, which is far lower than that of the spontaneous alcoholysis reaction of sodium borohydride. After the Co–Mo–P/CNTs-Ni foam catalyst was reused 8 times, the catalytic hydrogen production rate was reduced by 23% compared with the initial rate.