Hydrodeoxygenation Performance Research Articles

Selective hydrodeoxygenation of guaiacol to cyclohexanol over NixCoyAlz catalysts under mild conditions

Hydrodeoxygenation is one of the key steps to upgrade of biomass derived bio-oil into valuable biofuels and chemicals. Developing of highly reactive and cost-effective catalysts for bio-oil hydrodeoxygenation is highly desired. Layered NixCoyAlz catalyst was prepared using layered double hydroxide (LDH) as the precursors. The optimized Ni1Co3Al2-600 catalyst exhibits excellent catalytic performance for guaiacol hydrodeoxygenation. Guaiacol could completely converted with 90.0% of cyclohexanol selectivity under relatively mild reaction conditions. The XRD and HRTEM characterizations of the as prepared catalysts confirmed the formation of Ni-Co alloy and the XPS analysis revealed the strong interaction between Al species with both Ni and Co in catalyst Ni1Co3Al2-600, which should contribute to its high catalytic activity for guaiacol hydrodeoxygenation. Catalyst Ni1Co3Al2-600 also demonstrated excellent versatility for the hydrodeoxygenation reactions of guaiacyl and syringyl compounds as well as high stability. The results from this work could provide a new approach for the constructing of effective catalysts from non-noble metal LDHs.

Upgradation of Eugenol to ASTM D 1655 standard Bio-Jet(A) fuel range hydrocarbons via hydrodeoxygenation process over Ru-Ni supported KIT-6/HZSM-5

A novel hierarchical Zeolite composite was successfully synthesized for bio-fuel application via catalytic hydrodeoxygenation of Lignin-Derived Phenolic Model Compound (LDPMC) in a downflow fixed bed reactor. The utilization of massive noble metals in the hydrodeoxygenation process in factories leads to an increase in the total cost of LDPMC technology. A fractional replacement of Ruthenium (Ru) by another transition metal Nickel (Ni), is a potentially effective method. The core asset of the novel synthesized catalyst displayed the advantageous properties of both micro- and mesoporous. This could be confirmed by the results of XRD, BET, and surface analyzing microscopes. The synthesis of Rux-Ni10-x/KIT-6-HZSM-5 (x = 2, 4 & 6) bimetallic-monometallic catalysts and their catalytic performance for hydrodeoxygenation of Eugenol are reported in the present study. The hierarchical Zeolite composite catalysts were synthesized by a wet-chemistry method. The active catalysts were characterized by ATR-IR, H2-TPR, NH3-TPD, HR-SEM, HR-TEM, XPS, and TGA techniques. The synthesized 2 %Ru-8 %Ni/KIT-6-HZSM-5 exhibited 100 % conversion with a maximum yield of 48.70 % of the complete deoxygenated product (Jet A range fuel) due to the synergistic effect between Ru and Ni on hierarchical Zeolite composite support and superior catalytic activity compared to the other synthesized catalysts with the highest metal dispersion. The stability and reproducibility of catalysts were steady even after 4 cycles. The Ruthenium and Nickel loaded hierarchical Zeolite composite support showed superior activity related to other reported catalysts even at atmospheric pressure under variable experimental conditions.

Quantitative synergy between metal and acid centers over the Ni/Beta bifunctional catalyst for methyl laurate hydrodeoxygenation to bio-jet fuel

The synergistic effect of metal and acid centers influences performance of bifunctional hydrodeoxygenation (HDO) catalyst significantly. However, seldom work concerning this point has been performed quantitatively. Herein, the Ni/Beta catalysts were prepared for HDO of methyl laurate to bio-jet fuels. The ratios of metal to acid centers (nNi/nA) were used to quantitatively express the synergistic effect and correlated to the HDO performance. The transformation of methyl laurate mainly stagnates at fatty acid over the mono-functional catalyst (nNi/nA = 0), while the acid centers are indispensable for the efficient transformation of methyl laurate at relatively mild reaction conditions. The TOF and selectivity to C11 and C12 alkanes increase and then keep constant with the increasing nNi/nA. The turning point at the nNi/nA of 0.67 implies that one nickel center over the Ni/Beta catalyst can balance ca. 1.5 acid centers in the HDO of methyl laurate. Besides, the higher nNi/nA favors the HDO reaction pathway compared with the decarbonylation or decarboxylation ones. It increases the selectivity to C12 alkanes and improves efficiency of atomic utilization during the hydrodeoxygenation of methyl laurate. This work provides a deeper insight into the quantitative synergy of active sites over the bifunctional HDO catalyst for production of bio-fuels.

Efficient hydrodeoxygenation of lignin-derived phenolic compounds by using Ru-based biochar catalyst coupled with silicotungstic acid

Hydrodeoxygenation (HDO) is an effective technology for the conversion of bio-oil to high quality liquid fuels, in which an active and stable catalyst is crucial to gain a high reaction efficiency. In this work, a novel bifunctional catalyst of different Ru-based biochar catalyst coupled with silicotungstic acid (HSiW) was proposed to conduct the HDO of lignin-derived phenolic compounds under mild reaction condition. Ru/C-bamboo catalyst exhibited a better HDO performance than other Ru-based biochar catalysts and commercial Ru/C catalyst. Catalyst characterizations showed that Ru/C-bamboo catalyst possessed a rich mesoporous structure of 0.06 cm3/g mesopore volume and 0.07 cm3/g micropore volume, with a large specific surface area of 209 m2/g. A high metal dispersion and a good hydrogen adsorption ability were achieved in Ru/C-bamboo catalyst. And Guaiacol can be completely converted to cyclohexane with 87.7% selectivity at the temperature of 140 °C. Other typical phenolic compounds were also transformed into corresponding cycloalkanes with high yields above 90% in most cases. Besides, the lignin-oil also had a great improvement on the stability and the heat value after upgradation, with an increase of hydrocarbon content from 9.7% to 31.9%. This result indicated the potential of the bifunctional catalyst in the field of lignin-oil valorization.

The selective hydrodeoxygenation of guaiacol to cyclohexanol over cobalt-modified TS-1 catalysts

A Co-modified zeolite (Co/TS-1) catalyst is prepared and evaluated for the catalytic hydrodeoxygenation (HDO) of the lignin-derived model compound guaiacol under mild conditions at 1 MPa H2 and 200 °C. According to the systemic experimental investigations including reduction temperatures, metal loading and reaction time, it is found that the guaiacol conversion and cyclohexanol selectivity over guaiacol HDO are significantly improved by regulating the Ti content, Co content and reduction temperature, in which 5.0%Co/TS-1 (Si/Ti = 110) reduced in 600 °C shows the superior HDO performance with 94.3% guaiacol conversion and 88.7% cyclohexanol selectivity. Combined with XRD, TEM, BET, NH3-TPD, Py-IR, H2-TPR, UV–Vis and XPS characterizations, it is confirmed that the introduction of appropriate Ti could modulate the catalyst Lewis acid sites and the interaction between Co and support to affect the metal reduction degree, to realize the improvement of the substrate adsorption and exposing more metallic Co0 active sites, resulting in higher HDO performance. In addition, the reaction pathway of guaiacol HDO to cyclohexanol over Co/TS-1 is proposed via demethoxylation of guaiacol to generate reaction intermediate phenol.

Co-Based Catalysts Supported on Ceria with Different Shape Structures for Hydrodeoxygenation of Guaiacol

CeO2 with three different morphologies of nanorods (CeO2-r), particles (CeO2-p), and cubes (CeO2-c) was prepared, and the guaiacol hydrodeoxygenation over their corresponding Co-based catalysts was performed at 160–220 °C, 2 MPa, a H2 flow rate of 80 mL/min, and a weight hourly space velocity of 0.7 h–1. Compared with Co/CeO2-p and Co/CeO2-c, Co/CeO2-r has smaller Co particle sizes, a higher Brunauer–Emmett–Teller surface area, and larger amount of Co active centers, oxygen vacancies, and weak acid sites. These better physicochemical properties for Co/CeO2-r provide more Co active sites for guaiacol hydrodeoxygenation, favor the adsorption and activation of guaiacol, and contribute to the cleavage of C–O. Therefore, Co/CeO2-r presents a maximum guaiacol conversion of 97.1% and the highest yield of cyclohexanol of 91.7% among these catalysts. The result shows that the shape structure of CeO2 has an important influence on the guaiacol hydrodeoxygenation performance over its corresponding catalysts.

Comparison of Co-Mo-S and remote control model for designing efficient Co-doped MoS2 hydrodeoxygenation catalysts

Co-promoted MoS2 catalysts as good candidates can effectively remove the oxygen in bio-oil through the hydrodeoxygenation (HDO) of phenolics. However, it is of great importance to maximize the synergistic effect between Co and MoS2 which is conductive to the design of highly efficient Co-doped MoS2 HDO catalysts. Herein, two model catalysts with Co-Mo-S and CoS2/MoS2 (remote control model) as the active phases were successfully constructed and evaluated in the HDO of p-cresol. It was found that Co-Mo-S catalyst showed a significantly higher intrinsic HDO activity than CoS2/MoS2 catalyst, and the synergy factor between Co dopant and MoS2 of Co-Mo-S was 3.1 times that of CoS2/MoS2. The greatly enhanced HDO performance of Co-Mo-S catalyst is attributed to remarkably weakened strength of MoS bond, which can facilitate the sulfur vacancies (Vs) formation on the sulfur edges and promote the reaction rate of direct deoxygenation (DDO) pathway. This work revealed that Co-Mo-S model could better promote the CoMo synergy than the remote control model so as to design more efficient MoS2-based catalysts for HDO reactions.

Hydrodeoxygenation of lignin-derived phenolic compounds over Ru/TiO2 catalyst: Effect of TiO2 morphology

Hydrodeoxygenation (HDO) reaction is a necessary refinery process for lignin-derived phenolic compounds to be used as high quality liquid fuels. Catalyst morphology makes a big difference on the HDO performance through changing the properties of metal site and acid site, while the catalytic mechanism is still not very clear. In this work, four kinds of Ru/TiO2 catalysts with different morphology were prepared by photochemical method and all of them achieved a high Ru metal dispersion. A series of catalyst characterizations were carried out, including XRD, BET, SEM, TEM, H2-TPD and NH3-TPD, in order to explore the crystal structure, surface property, Ru metal dispersion, hydrogen adsorption capacity as well as acid properties. Results showed that Ru/TNP catalyst possessed a large surface area, an abundance of medium strength acid sites and a good hydrogen adsorption capacity. The HDO performances on lignin-derived phenolic compounds were also compared, in which Ru/TNP catalyst presented the best HDO performance. The guaiacol conversion and the selectivity of cyclohexane product were both close to 100 % at 250 °C under 1 MPa hydrogen pressure. Moreover, the content of hydrocarbons increased from 11.1 % to 60.8 % in the lignin-oil upgrading process.

Catalytic hydrodeoxygenation of phenolic compounds over Ru-MoFeP/Al2O3 catalyst

Catalytic converting the lignin-derived bio-oil to liquid fuel is one promising methodology to reduce the dependence on petroleum-based fuel while easing the atmospheric carbon dioxide burden. Hydrodeoxygenation (HDO) is one commonly used method to convert and upgrade bio-oil from biomass. In the present work, a Ru-promoted MoFeP/Al2O3 catalyst was prepared and evaluated the HDO performance by converting two model compounds, guaiacol and anisole with a batch reactor at 250 °C. This catalyst shows a quite good HDO performance over the two model compounds, in which, oxygen was removed from the phenolic and hydrocarbons were produced as the product. Kinetic studies were also performed to build the reaction network and elucidate the reaction pathway of guaiacol and anisole HDO reactions. The primary, secondary, and tertiary products can be identified for the HDO reactions. A better understanding of HDO chemistry from the fundamental study can lead to more efficient catalysts for the target products.

An efficient bifunctional Ni-Nb2O5 nanocatalysts for the hydrodeoxygenation of anisole

The anisole is almost completely transformed into cyclohexane by the synthesized Ni-Nb 2 O 5 nanocatalysts following the HYD reaction route. The Ni-Nb 2 O 5 nanocatalysts have been prepared by the sol–gel method, and the catalytic hydrodeoxygenation (HDO) performance of anisole as model compound is studied. The results show that Nb exists as amorphous Nb 2 O 5 species, which can promote Ni dispersion. The addition of Nb 2 O 5 increases the acidity of the catalyst. However, when the content of niobium is high, there is an inactive Nb-Ni-O mixed phase. The size and morphology of Ni grains in catalysts are different due to the difference of Nb/Ni molar ratio. The Ni 0.9 Nb 0.1 sample has the largest surface area of 170.8 m 2 ·g −1 among the catalysts prepared in different Nb/Ni molar ratios, which is mainly composed of spherical nanoparticles and crack pores. The HDO of anisole follows the reaction route of the hydrogenation HYD route. The Ni 0.9 Nb 0.1 catalyst displayed a higher HDO performance for anisole than Ni catalyst. The selectivity to cyclohexane over the Ni 0.9 Nb 0.1 sample is about 10 times that of Ni catalyst at 220 °C and 3 MPa H 2 . The selectivity of cyclohexane is increased with the increase of reaction temperature. The anisole is almost completely transformed into cyclohexane at 240 °C, 3 MPa H 2 and 4 h.

Comparative study of hydrodeoxygenation performance over Ni and Ni2P catalysts for upgrading of lignin-derived phenolic compound

To deeply understand the different hydrodeoxygenation (HDO) behavior of the monometallic Ni and Ni2P catalysts in HDO processes, the Ni/SiO2 and Ni2P/SiO2 catalysts were prepared, respectively. The as-prepared catalysts were characterized by X-ray diffraction (XRD), N2 adsorption–desorption, X-ray photoelectron spectra (XPS), H2 temperature-programmed reduction (H2-TPR), transmission electron microscope (TEM), NH3 temperature-programmed desorption (NH3-TPD), and CO uptakes. Taking the lignin-derived phenolic compound as raw material, the HDO performance and reaction route of the monometallic Ni and Ni2P catalysts were compared. The results showed that the phosphorization contributed to highly dispersion of active sites, formation of smaller active sites and significantly enhanced acid sites, showing Ni2P/SiO2 catalyst is a bifunctional metal–acid catalyst. For both of the Ni/SiO2 and Ni2P/SiO2 catalysts, the HDO of m-cresol mainly proceeded by the hydrogenation (HYD) step. However, the acid sites on Ni2P/SiO2 catalyst can significantly promote the conversion of oxygenated 3-methylcyclohexanol (MCHnol) to deoxygenated methylcyclohexane (MCH) owing to its strong hydrogenolysis of C–OH bond originated from the bifunctional metal–acid sites. In addition, the unique electron structure of Ni2P phase involved in two different types of sites (tetrahedral Ni(I) and square pyramidal Ni(II)) and the highly dispersed smaller Ni2P particles also contributed to the outstanding HDO performance. Density functional calculation (DFT) calculations clarified that the Ni2P active phase possessed prior ability to cleavage of C–OH bond in comparison with the metallic Ni species. As a result, Ni2P/SiO2 catalyst showed a significantly higher selectivity to MCH (96.3 %) than that of Ni/SiO2 (14.1 %) catalyst at the conditions of 250 ℃ for 240 min.

Structural and electronic effects boosting Ni-doped Mo2C catalyst toward high-efficiency C[sbnd]O/C[sbnd]C bonds cleavage

The selective cleavage of CO and CC is facing a challenge in the field of catalysis. In the present work, we studied the influence of doped Ni on the structure and electronic properties, as well as the selective CO/CC bond cleavages in the hydrodeoxygenation of palmitic acid over Ni-Mo2C catalyst. The catalytic activity on Ni doped Mo2C with TOF of 6.9 × 103 h−1 is much superior to intrinsic Mo2C catalyst, which is also higher than most noble metal catalysts. Structurally, the doped Ni raises the active particle dispersion and the coordination numbers of Mo species (Mo-C and Mo-O), improves the graphitization degree to promote the electron transfer, and increases the amount of Lewis and Brønsted acid, which are responsible for the excellent hydrodeoxygenation performance. The Ni promotes simultaneously CO and CC bonds cleavage to produce pentadecane and hexadecane owing to the increase of electron-rich Mo sites after Ni doping. These findings contribute to the understanding of the nature of Ni-doped Mo2C on the roles as catalytic active sites for CO and CC bonds cleavage.

Tuning support acidity of Ni-based catalysts to improve hydrodeoxygenation activity for dibenzofuran

Controlling the oxygen-free product selectivity in catalytic hydrodeoxygenation is essential for producing high-quality fuel from coal- and biomass-derived liquids. In this paper, the selectivity of oxygen-free products and efficiency of hydrodeoxygenation of dibenzofuran as a model compound of coal- and biomass-derived liquids have been controlled by varying the Si content in the prepared catalysts (Ni/xSi-OMA, where x = SiO2/(SiO2 + Al2O3) and OMA = ordered mesoporous alumina). In comparison, the hydrodeoxygenation of dibenzofuran was performed using Ni/SBA-15, which displayed the lowest selectivity of oxygen-free products at 36.4%. On the other hand, doping Si in OMA introduces the Brønsted acid sites, which desirably enhances the selectivity of oxygen-free products. Above 99% selectivity of oxygen-free products has been attained for Ni/30Si-OMA and Ni/40Si-OMA catalysts. The Lewis acid sites of the OMA promote the deoxygenation efficiency through the enhanced adsorption of oxygen-containing intermediates. Besides, the Brønsted acid sites generated in OMA as the result of Si-doping promote the ring-opening and dehydration reactions of the oxygen-containing intermediates, which further lead to an overall enhanced hydrodeoxygenation performance for dibenzofuran.

Spray pyrolysis-derived MoO3@Al2O3@TiO2 core-shell structures with enhanced hydrodeoxygenation performance

Developing highly active and stable hydrodeoxygenation (HDO) catalysts is an industrial challenge. In this work, γ-Al2O3 microspheres incorporating high levels of Mo catalyst (30 wt%; MoO3@Al2O3) were effectively and rapidly prepared by ultrasonic-assisted spray pyrolysis. The MoO3@Al2O3 microspheres were then decorated by a hydrophobic TiO2 layer to obtain core–shell-structured microspheres dubbed MoO3@Al2O3@TiO2. HDO experiments revealed that catalysis by reduced MoO3@Al2O3@TiO2 microspheres afforded ~96% palmitic acid (PA) conversion and ~ 67% hydrocarbon selectivity, surpassing the uncoated catalyst. Furthermore, the prepared TiO2-coated MoO3@Al2O3 microspheres retained excellent HDO catalytic activity under water-containing feed for 24 h. This study's results suggest that combining spray pyrolysis and coating with a TiO2 shell produces a synergetic effect that enhances the catalyst's activity and stability.

Unsupported MoS2-Based Catalysts for Bio-Oil Hydrodeoxygenation: Recent Advances and Future Perspectives.

In recent years, unsupported MoS2-based catalysts have been reported as promising candidates in the hydrodeoxygenation (HDO) of bio-oil. However, preparing MoS2-based catalysts with both high activity and good stability for HDO reaction is still challenging and of great importance. Hence, this mini-review is focused on the recent development of unsupported MoS2-based HDO catalysts from the understanding of catalyst design. The three aspects including morphology and defect engineering, metal doping, and deactivation mechanism are highlighted in adjusting the HDO performance of MoS2-based catalysts. Finally, the key challenges and future perspectives about how to design efficient catalysts are also summarized in the conclusions.

Insights into the catalytic performance of Ni/Nb2O5 catalysts for vanillin hydrodeoxygenation in aqueous phase: The role of Nb2O5 crystal structures

Hydrodeoxygenation (HDO) in aqueous phase is green and efficient approaches to convert the biomass and its derivative to high value-added chemicals and renewable fuels. However, it remains a great challenge for synthesizing catalysts with the excellent hydrodeoxygenation performance. Three kinds of Ni/Nb2O5 catalyst with different crystal structures (Ni/TT-Nb2O5, Ni/T-Nb2O5, Ni/H-Nb2O5) were prepared for vanillin hydrodeoxygenation. Compared with the Ni/TT-Nb2O5 and Ni/H-Nb2O5 catalyst, the Ni/T-Nb2O5 catalyst had the most concentration of oxygen vacancies (Ov), which resulted in the excellent hydrodeoxygenation performance. At 180 ℃, 1 MPa H2, and the water/ethanol ratio of 8/12, 96.1% conversion of vanillin and 79.2% selectivity of 2-methoxy-4-methylphenol (MMP) were obtained. The abundant Ov of Ni/T-Nb2O5 adsorbed and activated the C-OH bonds of vanillyl alcohol (VA), while water formed a stronger transition state with VA to further reduce the disassociation energy of C-OH bonds. The synergistic effect between Ov and water promoted the hydrodeoxygenation of vanillin in aqueous phase, achieving the high yield of MMP. This work provides a new idea for the preparation of catalysts with high catalytic performance in aqueous phase.

Efficiency conversion of jatropha oil into high-quality biofuel over the innovative Ni-Mo2N based catalyst

Mo2N catalyst can effectively remove oxygen from biomass oil under harsh reaction conditions. Herein, the innovative Ni-Mo2N/γ-Al2O3 catalyst was synthesized through conventional impregnation method and NH3 or N2/H2 pretreatment. The hydrodeoxygenation performance of Ni-Mo2N/γ-Al2O3 catalyst is significantly improved in comparison with Mo2N. At 320 °C and 3 MPa, the oxygen of jatropha oil is completely removed and high-quality biofuel with high selectivity of C15-C18 hydrocarbons are obtained over the Ni-Mo2N/γ-Al2O3 catalyst. This good reactivity for Ni-Mo2N/γ-Al2O3 catalyst are ascribed to the synergistic effect of Ni and Mo2N, the most uniform Ni dispersion and the excellent coke resistance ability. Ni, as an auxiliary, is conductive to the cleavage of H–H bonds, while Mo2N are beneficial to the cleavage of C–O bonds. In addition, the metal-support interaction would affect the deoxygenation pathway of jatropha oil. This research proposes an efficient strategy for enhancing the hydrodeoxygenation performance of Mo2N catalysts for the jatropha oil conversion.

Calcination temperature induced structural change of red mud and its enhanced catalytic performance for hydrocarbon-based biofuels production

Red mud (RM) is a strongly solid waste from alumina production, and the disposal of RM leads to series of environmental problems such as alkalization of occupied land and pollution of nearby water systems. Using RM as catalyst or carrier is one of the important methods for the comprehensive utilization of RM. Herein, the application of Ni supported RM (Ni/RM) for the efficient hydrodeoxygenation (HDO) of waste oils to produce hydrocarbon-based biofuels is reported. The structural properties of Ni/RM catalysts were investigated. The catalytic performance for HDO of palmitic acid as the model compound was evaluated. The results showed that RM calcinated at low temperature (400–600 °C) has a larger specific surface area and well dispersion of Ni, while the high calcination temperature (700 °C ~ 900 °C) results in sintering of metal oxides and lower dispersion of Ni. Ni/RM-500 shows the largest specific surface area of 77 m2/g. The conversion of palmitic acid over Ni/RM-500 is 100% at 250 °C, and alkanes are the only products at 300 °C. The reaction path of HDO and DCO/DCO2 is related to reaction temperature. The Ni/RM-500 shows the feasibility to different feedstocks. Finally, the catalytic performance of Ni/RM-500 was tested for 135 h, and the main reason causing the deactivation of Ni/RM-500 was revealed.

Upgrading pyrolysis oil by catalytic hydrodeoxygenation reaction in supercritical ethanol with different hydrogen sources

The effects of hydrogen sources (hydrogen gas as an ex-situ hydrogen source and formic acid as an in-situ hydrogen source) on upgrading of pyrolysis oil by hydrodeoxygenation (HDO) in supercritical ethanol were comparatively investigated in this study for the first time. Effects of catalysts (5%Ru/C and 10%Ni-6%Mo-5%W/Al2O3), time and temperature on the product yields and quality of upgraded oil were investigated comparatively with different hydrogen sources. An interesting result was obtained, demonstrating that the in-situ hydrogen (formic acid) showed better HDO performance at mild temperatures (260, 300 ℃), while the HDO of pyrolysis oil with ex-situ hydrogen (H2 gas) at higher temperatures (325 or 350 ℃) with respects to degree of deoxygenation and the quality of the produced upgraded oils. HDO of the woody derived pyrolysis oil with total acid number (TAN) of 136.0 mgKOH/g at 350 ℃ for 2 h over Ru/C catalyst with formic acid or hydrogen gas resulted in 74% and 85% degree of de-oxygenation, respectively, producing high quality upgraded oils with TAN of 35.3 mgKOH/g and 50.1 mgKOH/g and HHV of 39.5 MJ/kg and 43.0 MJ/kg, respectively.

A highly dispersed Ni3P/HZSM-5 catalyst for hydrodeoxygenation of phenolic compounds to cycloalkanes

A highly dispersed Ni3P/HZSM-5 catalyst was prepared by deposition-precipitation of Ni species followed by electroless plating and thermal treatment, and characterized by means of XRD, ICP, N2 physical adsorption, TEM, XPS, NH3-TPD, and CO chemisorption. Electroless plating reaction takes place in an aqueous solution under mild conditions, facilitating the high dispersion of the formed Ni3P particles. XRD measurements illustrated the lamellar nickel phyllosilicate was produced at the first step of deposition-precipitation, amorphous Ni-P was formed in the subsequent electroless plating, and highly dispersed Ni3P crystallites were generated in thermal treatment. TEM observation demonstrated that the average particle size of Ni3P crystallites in the prepared Ni3P/HZSM-5 catalyst was 4.3 nm. Bifunctional Ni3P/HZSM-5 was investigated in hydrodeoxygenation (HDO) of phenolic compounds, including phenol, m-cresol, and guaiacol. Ni3P/HZSM-5 exhibited high catalytic performance in HDO with enhanced hydrogenation and dehydration pathway.