SiO2 supported Au Ni bimetallic catalyst for the selective hydrogenation of acetylene

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1 Chinese Journal of Catalysis 38 (217) 催化学报 217 年第 38 卷第 8 期 available at journal homepage: Article SiO2 supported Au Ni bimetallic catalyst for the selective hydrogenation of acetylene Mengqian Chai a,b, Xiaoyan Liu a, *, Lin Li a, Guangxian Pei a,b, Yujing Ren a,b, Yang Su a, Hongkui Cheng c, Aiqin Wang a, Tao Zhang a a State Key Laboratory of Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 11623, Liaoning, China b University of Chinese Academy of Sciences, Beijing 149, China c Chia Tai Energy Materials (Dalian) Co., Ltd., Dalian 11621, Liaoning, China A R T I C L E I N F O A B S T R A C T Article history: Received 14 April 217 Accepted 6 June 217 Published 5 August 217 Keywords: Gold Nickel Bimetallic catalyst Synergistic effect Acetylene hydrogenation Supported Au catalysts have been reported to exhibit high ethylene selectivity in the hydrogenation of acetylene, but the conversion is relatively low. Adding a second metal to Au has proven to be a promising approach to enhance its catalytic performance in acetylene hydrogenation. In this work, SiO2 supported Au Ni bimetallic catalysts were synthesized and investigated in the selective hydrogenation of acetylene. The Au Ni bimetallic catalysts exhibited much higher catalytic performance than that of the corresponding monometallic Au or Ni catalysts. By tuning the reduction temperature and/or Ni loading, we obtained an Au Ni/SiO2 catalyst with optimal performance. The results of transmission electron microscopy imaging revealed that the Au Ni bimetallic particles were highly dispersed on the SiO2 support. Meanwhile, analysis of the bimetallic catalyst by energy dispersive X ray spectroscopy, high resolution transmission electron microscopy, and in situ diffuse reflectance infrared Fourier transform spectroscopy demonstrated the formation of Au Ni alloy, which contributed to the synergistic effect between Au and Ni in the hydrogenation of acetylene. 217, Dalian Institute of Chemical Physics, Chinese Academy of Sciences. Published by Elsevier B.V. All rights reserved. 1. Introduction The ethylene used in the production of polymers is obtained by the cracking of naphtha and typically contains on the order of 1% acetylene [1]. The presence of acetylene is poisonous to the catalyst in ethylene polymerization [2,3]. The selective hydrogenation of acetylene to ethylene is the most widely used method by industry to remove acetylene from ethylene feed gas [4]. Thus, catalysts for selective hydrogenation of acetylene should have both high activity for acetylene conversion and high selectivity for ethylene [5,6]. Pd based catalysts are typically used to eliminate the traces of acetylene from ethylene [7 1]. However, they show poor selectivity for ethylene because the over hydrogenation of acetylene and ethylene leads to production of oligomers ( green oil ) and wastes ethylene in the feed gas [2,3,11]. Since the pioneering work of Haruta et al. [12] in 1987, supported Au nanoparticles have been found to exhibit prom * Corresponding author. Tel: ; Fax: ; E mail: This work was supported by the National Natural Science Foundation of China ( , , , , ), Youth Innovation Promotion Association of the Chinese Academy of Sciences (214163), the National Key Projects for Fundamental Research and Development of China (216YFA2281), the Strategic Priority Research Program of the Chinese Academy of Sciences (XDB1721), and the Department of Science and Technology of Liaoning Province ( ). DOI: 1.116/S (17) Chin. J. Catal., Vol. 38, No. 8, August 217

2 Mengqian Chai et al. / Chinese Journal of Catalysis 38 (217) ising catalytic performance in a variety of reactions, including the water gas shift reaction [13], selective oxidation of alcohols [14], and selective hydrogenation of nitroarenes [15,16]. Au catalysts have proven to be highly selective in the hydrogenation of acetylene to ethylene; however, the conversion of acetylene is very low [17 2]. One of the most promising approaches to improve the conversion of acetylene over Au catalysts is to synthesize Au based bimetallic catalysts; for example, Au Pd [21], Au Fe [22], Au Ag [23], and Au Cu [24]. Among these catalysts, the Au Pd bimetallic system is the most popular. The catalytic conversion of acetylene can be efficiently improved by the addition of Pd compared with that of the monometallic Au catalyst. Au Pd core shell nanoparticles have been constructed by various methods to tune the selectivity for ethylene in acetylene hydrogenation [25,26]. However, it has been proved that the contiguous Pd can lead to the over hydrogenation of acetylene and/or ethylene [27]. In our previous work [28], we tried to isolate Pd atoms in Au Pd bimetallic catalysts by synthesizing Au Pd alloy via a two step method by tuning the ratio of Pd to Au. The alloyed Pd single atom catalyst showed both high conversion and selectivity in acetylene hydrogenation with excess ethylene. We proposed that the alloyed Pd single atoms drove the conversion of acetylene, while Au played an important role in preventing the over hydrogenation of acetylene. Ni is from the same group as Pd in the periodic table. Supported Ni catalysts are important in hydrogenation reactions [29,3]. Thus, adding Ni to Au might improve its catalytic performance in hydrogenation reactions. Although Ni does not form alloys with Au as easily as Pd does, Au Ni bimetallic catalysts have been reported to show synergistic effects in various reactions, such as the hydrogenolysis of benzylic alcohols [31], the water gas shift reaction [32], CO oxidation [32], chemoselective hydrogenation of nitroarenes [15], ethanol conversion into linear primary alcohols [33], and selective hydrogenation of 1,3 butadiene [34]. In this work, we synthesize a series of Au Ni bimetallic nanoparticles supported on silica (SiO2) with different atomic ratios of Ni to Au to investigate their synergistic effect in acetylene hydrogenation. The catalytic performance of the Au Ni bimetallic catalysts in acetylene hydrogenation is investigated. The energy dispersive X ray spectroscopy (EDS), high resolution transmission electron microscopy (HRTEM), and in situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) are used to characterize the interaction between Au and Ni in the bimetallic catalysts. This work could provide new insights into the intrinsic origin of the high catalytic performance of Au Ni bimetallic catalysts and guide the design of new catalysts for hydrogenation reactions. 2. Experimental 2.1. Catalyst preparation We prepared the catalysts by a two step method previously developed by our group [15]. In this method, commercial SiO2 (Qingdao Ocean Chemical Plant, ABET = 463 m 2 /g) was first functionalized with 3 aminopropyltriethoxysilane (APTES; Acros Organics, 99%) by heating under reflux in alcohol at 8 C for 24 h. After suction filtration, washing with ethanol, and drying at 6 C for 1 d, APTES functionalized SiO2 was obtained (denoted as SiO2 APTES). In the first step, SiO2 APTES (1. g) was dispersed in HAuCl4 solution (2 ml, 2. gau/l) and stirred for 3 min. After being filtered and washed with deionized water, the recovered solid was dispersed in deionized water (1 ml) and then NaBH4 solution (1 ml,.2 mol/l) was added dropwise to reduce Au 3+. After stirring for 15 min, suction filtration, and washing with deionized water, the Au loaded SiO2 support was obtained. In the second step, the Au loaded SiO2 support was dispersed in Ni(NO3)2 solution (1 ml) with a certain concentration and stirred for 3 min. Then, tert butylamine borane solution (1 ml,.1 mol/l) was added dropwise to reduce Ni 2+ under continuous stirring for 3 min. After suction filtration, washing with deionized water, drying at 6 C for 1 d, and calcination at 5 C for 3 h, the AuNix/SiO2 catalysts were obtained (x refers to the atomic ratio of Ni to Au). According to the corresponding step of the above method, monometallic Au/SiO2 and Ni.5/SiO2 (Ni.5/SiO2 has the same Ni loading as AuNi.5/SiO2) catalysts were prepared after being calcined at 5 C for 3 h. The catalysts (e.g., AuNi1/SiO2) reduced at a certain temperature (e.g., 45 C) under H2/He flow are denoted by the suffix H2 temperature (e.g., AuNi1/SiO2 H2 45) Reaction tests The performance of the as prepared catalysts in the selective hydrogenation of acetylene was tested using a fixed bed reactor. All the gases used in the reaction were controlled by mass flow controllers. Before the reaction, catalyst (3 mg) was loaded into the reactor and reduced in an H2/He (2 ml/min; volume ratio of 4:1; H2: UHP, %; He: UHP, %) gas stream at a certain temperature for 7 min. After cooling to room temperature in He (2 ml/min), feed gas consisting of C2H2/H2/He (3 ml/min; volume ratio of 1:2:79) stabilized at room temperature for more than 5 min was introduced into the reactor. As the temperature was increased from 1 to 3 C at a heating rate of 8 C/min, the catalyst s activity was tested every 4 C and each reaction temperature was kept constant for 25 min before being increased to the next temperature. The analysis of the outlet gas components was performed by an online gas chromatograph (GC; Agilent Technologies 689N) equipped with a flame ionization detector (FID). In this study, the C2 products detected by GC/FID were only C2H4 and C2H6. Therefore, the acetylene conversion and ethylene selectivity were calculated as follows: Conversion = [ C2H2(feed) C2H2]/C2H2(feed) 1% (1) Selectivity = C2H4/[C2H2(feed) C2H2] 1% (2) 2.3. Characterization The metal loading of the as prepared catalysts was measured by an inductively coupled plasma atomic emission spectrometer (ICP AES; Thermo IRIS Intrepid II XSP, Thermo Elec

3 134 Mengqian Chai et al. / Chinese Journal of Catalysis 38 (217) tron Co.). X ray diffraction (XRD) patterns were obtained on an X ray diffractometer (PW34/6, X pert Pro Super, PANalytical) equipped with a Cu Kα radiation source (λ = nm) operating at 4 kv and 4 ma. The data were collected in continuous mode in the 2θ range from 1 to 8 with a scan rate of 1 /min. Transmission electron microscopy (TEM), HRTEM, and EDS measurements were conducted with an electron microscope (JEM 21F, JEOL) operating at 2 kv. In situ DRIFTS data were recorded by an infrared spectrometer (Vertex 7, Bruker) with a mercury cadmium telluride detector and operated at room temperature and atmospheric pressure. The spectra were obtained by collecting 64 scans with 4 cm 1 resolution. Before CO adsorption, each as prepared sample was loaded into the DRIFTS cell (HC 5, Pike technologies) and reduced in an H2/He gas stream (2 ml/min; volume ratio of 4:1) at 45 C for 3 min, followed by purging with pure He (2 ml/min) for 1 min and then cooling to room temperature. After a background spectrum was collected for the sample, a CO/He gas stream (2 ml/min; volume ratio of 1:99) was introduced into the DRIFTS cell for about 3 min, followed by purging with pure He (2 ml/min) for 3 min. Spectra were collected during this process. 3. Results and discussion 3.1. Catalytic performance in the selective hydrogenation of acetylene Effect of reduction temperature on catalytic performance The reduction pretreatment of the catalyst could influence the states of Au and Ni and thus the interaction between them. To investigate whether a synergistic effect exists between Au and Ni, we first measured the catalytic performance of AuNi1/SiO2 reduced at different temperatures. The acetylene conversion and ethylene selectivity at reaction temperatures from 1 to 3 C are given in Fig. 1. With increasing reduction temperature of the catalyst, its activity in acetylene hydrogenation rises considerably (Fig. 1(a)). Meanwhile, the selectivity for ethylene slightly improved as the reduction temperature rose from 3 to 45 C and then declined dramatically when the reduction temperature exceeded 45 C (Fig. 1(b)). For the catalyst reduced at 55 C, the conversion of acetylene was 1% over the whole reaction temperature range but its highest selectivity was only 18%. The marked change of the catalytic performance of AuNi1/SiO2 with reduction temperature may be attributed to the reduction temperature influencing the interaction between Au and Ni in the catalyst. With increasing reduction temperature, more Au Ni alloy will form, which might promote acetylene conversion. Therefore, the activities of the catalysts are correlated with their content of Au Ni alloy Effect of Ni:Au atomic ratio on catalytic performance In addition to the reduction temperature, the loading of Ni is another factor that strongly affects the composition of the Au Ni alloy nanoparticles. Therefore, the effect of the Ni:Au atomic ratio on catalytic performance was studied. According to Fig. 1, we found that 45 C was the optimal reduction temperature for relatively high acetylene conversion and the highest ethylene selectivity. Therefore, we reduced all the catalysts with different Ni:Au atomic ratios at 45 C. The acetylene conversion and ethylene selectivity of AuNix/SiO2 H2 45 with different Ni:Au atomic ratios are given in Fig. 2. The monometallic Au/SiO2 H2 45 catalyst exhibited the highest selectivity for ethylene (~9%) over the whole reaction temperature range, while its conversion of acetylene increased with temperature and the highest conversion was only ~3%. For Ni.5/SiO2 H2 45, which had similar Ni loading to that of AuNi.5/SiO2 H2 45, almost no acetylene was converted until 22 C and the highest conversion was 5% with selectivity below 4%. The addition of Ni to the monometallic Au catalyst greatly improved its catalytic performance. The conversion of acetylene by each AuNix/SiO2 H2 45 catalyst was higher than Conversion (%) (a) o C 6 4 o C o C 4 45 o C 475 o C 3 5 o C 2 55 o C Selectivity (%) 1 (b) o C 4 o C 425 o C 45 o C 475 o C 5 o C 55 o C Fig. 1. Acetylene conversion (a) and ethylene selectivity (b) as a function of reaction temperature over AuNi1/SiO2 catalysts reduced at 3, 4, 425, 45, 475, 5, and 55 C, respectively.

4 Mengqian Chai et al. / Chinese Journal of Catalysis 38 (217) Conversion (%) (a) AuNi 1 AuNi.5 AuNi.25 AuNi.125 Au Ni Selectivity (%) 1 (b) AuNi 1 AuNi.5 AuNi.25 AuNi.125 Au Ni Fig. 2. Acetylene conversion (a) and ethylene selectivity (b) as a function of reaction temperature over the AuNi1/SiO2 H2 45, AuNi.5/SiO2 H2 45, AuNi.25/SiO2 H2 45, AuNi.125/SiO2 H2 45, Au/SiO2 H2 45, and Ni.5/SiO2 H2 45 catalysts. the sum of the conversions by the Au/SiO2 H2 45 and Ni.5/SiO2 H2 45 catalysts. As the Ni:Au atomic ratio increased from.125 to.5, there was an obvious improvement of catalytic activity. The catalyst with a Ni:Au atomic ratio of.5 exhibited the highest acetylene conversion and ethylene selectivity of the catalysts. When the Ni:Au atomic ratio was increased to 1, the catalyst displayed similar catalytic performance to that of AuNi.5/SiO2 H2 45. Compared with those reported in the literature for monometallic Au catalysts [18,19,28,35], the activities of the optimized Au Ni bimetallic catalysts were higher. The ethylene selectivity of the bimetallic catalysts was lower compared with that of Au catalysts and higher compared with those of monometallic Pd and Ni catalysts [2,3,11,36,37]. These results imply that the enhancement of activity caused by adding Ni can be ascribed to a synergistic effect between Au and Ni in the hydrogenation of acetylene Characterization results We determined the actual metal loadings of all the as prepared catalysts by ICP AES; the results are shown in Table 1. The actual loadings of Ni and Au were close to the theoretical values. By using tert butylamine borane as the reduction agent, Ni can be successfully loaded into the bimetallic catalysts. The actual atomic ratios of Ni to Au were slightly higher Table 1 Metal loadings and atomic ratios of different AuNix/SiO2 catalysts. Catalyst Nominal loading (wt%) Actual loading (wt%) Au Ni Au Ni Actual Ni:Au atomic ratio AuNi1/SiO AuNi.5/SiO AuNi.25/SiO AuNi.125/SiO Au/SiO Ni.5/SiO than the corresponding nominal values Particle sizes of the AuNix/SiO2 H2 45 catalysts The XRD patterns of AuNix/SiO2 (x =,.25,.5, 1) and Ni.5/SiO2 after reduction at 45 C are depicted in Fig. 3. All the AuNix/SiO2 H2 45 catalysts displayed four broad peaks at 2θ = 38.2, 44.4, 64.6, and 77.5, which corresponded to the reflections of the (111), (2), (22), and (311) lattice planes of metallic Au, respectively. The broad peaks indicate the small size of the AuNix/SiO2 H2 45 catalyst particles. According to the Scherrer equation, the estimated average particle size of Au/SiO2 is about 2.7 nm. With increasing Ni loading, the peaks of Au remained broad, and there was no marked variation of particle size. The estimated average crystallite sizes of Au in the Intensity (a.u.) (111) Ni.5 AuNi 1 AuNi.5 AuNi / ( ) Au Au (JCPDS: ) (2) (22) (311) (111) Ni (JCPDS: ) (2) (22) Fig. 3. XRD patterns of the AuNix/SiO2 H2 45 (x =,.25,.5, and 1) and Ni.5/SiO2 H2 45 catalysts.

5 1342 Mengqian Chai et al. / Chinese Journal of Catalysis 38 (217) Au/SiO2 H2 45, AuNi.25/SiO2 H2 45, AuNi.5/SiO2 H2 45, and AuNi1/SiO2 H2 45 catalysts are 2.7, 2.8, 2.7, and 3. nm, respectively. Meanwhile, there was no obvious peak of metallic Ni observed from the XRD patterns of the AuNix/SiO2 H2 45 and Ni.5/SiO2 H2 45 catalysts. The absence of a Ni phase in the XRD patterns suggests that Ni is highly dispersed in the catalysts or the content of Ni is below the detection limit. We also did not identify any peaks consistent with the Au Ni alloy phase. This result implies that the content of Au Ni alloy was too low to be detected by XRD or no Au Ni alloy formed. The detailed particle size distribution of AuNix/SiO2 H2 45 (x =,.25,.5, 1) was further characterized by TEM, as illustrated in Fig. 4. The metal particles in all catalysts were uniformly dispersed on the support. No very big particles were observed in arbitrarily selected regions of each catalyst. We calculated the average particle sizes of all the catalysts by arbitrarily selecting more than 2 particles from different areas. The histograms in Fig. 4 reveal that the average particle sizes of Au, AuNi.25, AuNi.5, and AuNi1 are 2.8, 2.9, 3.1, and 3.1 nm, respectively, which is in agreement with the XRD results. The (a) (b) (c) (d) (e) nm nm nm nm nm Fig. 4. TEM images and corresponding histograms of particle size distribution of the Au/SiO2 H2 45 (a), AuNi.25/SiO2 H2 45 (b), AuNi.5/SiO2 H2 45 (c), and AuNi1/SiO2 H2 45 (d) catalysts; (e) HAADF STEM image and corresponding histograms of particle size distribution of the Ni.5/SiO2 H2 45 catalyst. Ni.5/SiO2 H2 45 catalyst was difficult to characterize clearly by TEM, so a high angle annular dark field scanning transmission electron microscope (HAADF STEM) image of this sample was captured (Fig. 4(e)). As shown in Fig. 4(e), the Ni species were highly dispersed on the silica support in Ni.5/SiO2 H2 45, with a particle size of 2.4 nm Formation of Au Ni alloy To observe the composition of the metal nanoparticles in the AuNix/SiO2 H2 45 catalysts, EDS was used to characterize the individual particles in the AuNi.25/SiO2 H2 45 and AuNi.5/SiO2 H2 45 catalysts. As shown in Fig. 5(a) and (b), from the HAADF STEM images, several randomly selected individual particles were analyzed by EDS. The results revealed that the particles of the two catalysts contained both Au and Ni, although their chemical composition was different. The metal particles containing both Au and Ni suggest the formation of Au Ni alloy was possible under the catalyst preparation conditions. To further understand the geometric structure of the Au Ni bimetallic particles, we used HRTEM to characterize the lattice fringes of individual particles of the AuNi.25/SiO2 H2 45 and AuNi.5/SiO2 H2 45 catalysts. Both catalysts consisted of metal particles with a lattice spacing between those of Au(111) (.235 nm) and Ni(111) (.22 nm), as shown in Fig. 5(c) and (d). Therefore, the Au Ni bimetallic catalysts contained Au Ni alloy. Although it is not easy for bulk Au and Ni to form an alloy, Labat et al. [38] reported that the segregation of Au to the surface results in the interfacial mixing of Au and Ni to decrease the elastic stress of Ni during its growth process in core shell nanocrystals. Recently, Tsuji and colleagues [39] investigated the epitaxial growth of Ni shells on polyhedral Au cores. When the particle size decreased to the nanometer level, (a) (c) nm Ni:Au (b) (d) nm Ni:Au Fig. 5. (a, b) EDS analysis of individual particles and (c, d) HRTEM images of the AuNi.25/SiO2 H2 45 (a, c) and AuNi.5/SiO2 H2 45 (b, d).

6 Mengqian Chai et al. / Chinese Journal of Catalysis 38 (217) the formation of Au Ni alloy became possible. Zhou et al. [4] synthesized Au Ni alloy in oleylamine solution using trioctylphosphine and butyllithium as protecting and reducing agents, respectively. Meanwhile, Liuʼs group developed a general two step method to synthesize Au Cu [41], Au Ag [23] and Au Pd [42,43] alloy nanoparticles dispersed on SiO2 and/or alumina supports using NaBH4 as the reducing agent. Soon after, Wei et al. [15] proved that NaBH4 was not appropriate for the formation of Au Ni alloy nanoparticles. However, when tert butylamine borane was used as the reducing agent, highly dispersed Au Ni alloy nanoparticles were successfully synthesized on an SiO2 support. Their extended X ray absorption fine structure results demonstrated that a substantial fraction of Ni was alloyed with Au in their AuNi3/SiO2 catalyst. In this work, all of the AuNix/SiO2 bimetallic catalysts were prepared by the same two step method and tert butylamine borane was used as a relatively weak reducing agent for Ni 2+ in the second step. Based on the noble metal induced reduction (NMIR) mechanism [44], Au particles will be able to induce the preferential deposition of Ni on their surfaces. This allows Au and Ni to interact intimately and thus, Au Ni alloy could form on the AuNix/SiO2 H2 45 catalysts, as indicated by the EDS and HRTEM results. To obtain information about the interaction between Au and Ni on the surface of the catalysts, we employed in situ DRIFTS using CO as the probe molecule to study the surface properties of the AuNix/SiO2 H2 45 (x =,.25,.5, 1) and Ni.5/SiO2 H2 45 catalysts. The variation of in situ DRIFTS results for the catalysts in CO atmosphere is shown in Fig. 6. As illustrated in Fig. 6(a), a strong absorption band at 2113 cm 1 originating from CO appeared for the Au/SiO2 H2 45 sample, which was ascribed to CO adsorbed on metallic Au [45,46]. The in situ DRIFTS plot for the Ni.5/SiO2 H2 45 catalyst (Fig. 6(b)) contained only bands from gas phase CO; thus, no CO absorbed on the monometallic Ni catalyst. The reason for this may be that there were too few metallic Ni particles existing in the monometallic Ni catalyst to be detected. The DRIFTS results for the AuNix/SiO2 H2 45 catalysts in Fig. 6(c) (e) contain strong absorption bands at 2113 cm 1 from CO accompanied with a weak band at 263 cm 1, which can be assigned to CO adsorbed on metallic Au and metallic Ni [45 47]. With the increasing Ni content, the intensity of the absorption band at 263 cm 1 increased. For the AuNix/SiO2 H2 45 catalysts, the appearance of the an absorption band consistent with CO on a metallic Ni surface means that the Au nanoparticles induced the reduction of Ni through the NMIR. This phenomenon further confirms that there was an intimate interaction between Au and Ni in the bimetallic nanoparticles. (a) Au (b) Ni s 15 s 3 s 45 s 6 s 75 s 15 s 15 s 3 s 15 s 3 s 45 s 6 s 75 s 15 s 21 s (c) AuNi.25 (d) AuNi.5 (e) AuNi s 15 s 3 s 45 s 6 s 75 s 15 s 27 s 3 s 15 s 3 s 45 s 6 s 75 s 15 s 27 s 3 s 15 s 3 s 45 s 6 s 75 s 15 s 27 s Fig. 6. In situ DRIFTS results for the Au/SiO2 H2 45 (a), Ni.5/SiO2 H2 45 (b), AuNi.25/SiO2 H2 45 (c), AuNi.5/SiO2 H2 45 (d), and AuNi1/SiO2 H2 45 (e) catalysts in CO atmosphere.

7 1344 Mengqian Chai et al. / Chinese Journal of Catalysis 38 (217) These results are in good agreement with those of EDS (Fig. 5(a) and (b)) and HRTEM (Fig. 5(c) and (d)). Nikolaev et al. [48] found that their Au NiO/Al2O3 catalyst contained Au δ+ because of the electron transfer from the electron rich Au particles to the electron deficient NiO. However, no positively charged Au was detected in our work, indicating that there was no obvious electron transfer between Au and Ni Origin of the synergistic effect between Au and Ni in the bimetallic catalysts The DRIFTS analysis of Au/SiO2 H2 45 in Fig. 6(a) revealed that there was only metallic Au in this catalyst. Thus, the activity of Au/SiO2 H2 45 in acetylene hydrogenation (Fig. 2(a)) can be attributed to the metallic Au, as reported in the literature [49,5]. The DRIFTS results for the AuNix/SiO2 H2 45 catalysts in Fig. 6(c) (e) show that Au exists in its metallic state accompanied with metallic Ni. Yang et al. [4] proposed that acetylene adsorbed strongly on Ni, which leads to its low activity in acetylene hydrogenation, while the doping a Ni catalyst with Au can weaken the acetylene adsorption and give rise to increased activity. Thus, the separated Ni plays an important role in catalyzing acetylene hydrogenation [51]. The HRTEM results in Fig. 5(c) and (d) demonstrated that the Au Ni bimetallic nanoparticles contained Au Ni alloy. Therefore, we presume that the formation of Au Ni alloy converts the continuous Ni into separated Ni particles and weakens the acetylene adsorption on Ni. Thus, the separated metallic Ni gives rise to the activity of the Au Ni bimetallic catalysts in acetylene hydrogenation. Meanwhile, the ethylene selectivity of the Au Ni bimetallic catalysts was much higher than that of the monometallic Ni catalyst. According to the density functional theory calculations of Yang et al. [4], the adsorption energies of ethylene on Ni(111) and Au/Ni(111) surfaces are.58 and.27 ev, respectively. The adsorption of ethylene on Ni was weakened by Au, making it easier to desorb, which will contribute to the improved ethylene selectivity in acetylene hydrogenation upon addition of Ni to Au. Thus, the Au in the Au Ni bimetallic catalysts might play an important role in promoting the selectivity for ethylene. Therefore, the synergistic effect between Au and Ni in the bimetallic catalysts in hydrogenation of acetylene can be ascribed to the formation of Au Ni alloy. 4. Conclusions We synthesized silica supported Au Ni bimetallic catalysts with different Ni:Au ratios and studied the synergistic effect between Au and Ni in the selective hydrogenation of acetylene. The Au Ni bimetallic catalysts exhibited higher acetylene conversion than the corresponding monometallic Au and Ni catalysts. The results of HRTEM, EDS and in situ DRIFTS measurements revealed the formation of Au Ni alloy. The dilution of Ni by Au contributed to not only the enhancement of acetylene conversion but also ethylene selectivity. These results provide a reference for the design of gold based bimetallic catalysts for selective hydrogenation reactions. References [1] B. M. Collins, US Patent , [2] A. Borodzinski, G. C. Bond, Catal. Rev. Sci. Eng., 26, 48, [3] A. Borodzinski, G. C. Bond, Catal. Rev. Sci. Eng., 28, 5, [4] B. Yang, R. Burch, C. Hardacre, G. Headdock, P. Hu, ACS Catal., 212, 2, [5] A. Borodzinski, A. Cybulski, Appl. Catal. A, 2, 198, [6] J. Osswald, K. Kovnir, M. Armbruster, R. Giedigkeit, R. E. Jentoft, U. Wild, Y. Grin, R. Schlogl, J. Catal., 28, 258, [7] T. V. Choudhary, C. Sivadinarayana, A. K. Datye, D. Kumar, D. W. Goodman, Catal. Lett., 23, 86, 1 8. [8] Y. H. Park, G. L. Price, Ind. Eng. Chem. Res., 1992, 31, [9] J. Panpranot, K. Kontapakdee, P. Praserthdam, J. Phys. Chem. B, 26, 11, [1] I. Y. Ahn, H. L. Ji, S. S. Kum, S. H. Moon, Catal. Today, 27, 123, [11] Q. W. Zhang, J. Li, X. X. Liu, Q. M. Zhu, Appl. Catal. A, 2, 197, [12] M. Haruta, T. Kobayashi, H. Sano, N. Yamada, Chem. Lett., 1987, [13] Q. Fu, H. Saltsburg, M. Flytzani Stephanopoulos, Science, 23, 31, [14] C. Della Pina, E. Falletta, M. Rossi, Chem. Soc. Rev., 212, 41, Graphical Abstract Chin. J. Catal., 217, 38: doi: 1.116/S (17) SiO2 supported Au Ni bimetallic catalyst for the selective C 2H 2 + H 2 C 2H 4 hydrogenation of acetylene 1 1 Ni/Au Meng Qian Chai, Xiao Yan Liu *, Lin Li, Guang Xian Pei, Yujing Ren, Yang Su, Hongkui Cheng, Aiqin Wang, Tao Zhang Dalian Institute of Chemical Physics, Chinese Academy of Sciences; University of Chinese Academy of Sciences; Chia Tai Energy Materials (Dalian) Co., Ltd Gold and nickel exhibited a strong synergistic effect in the hydrogenation of acetylene, which was ascribed to the formation of gold nickel alloy. Conversion (%) AuNi.5 /SiO 2 〇 Au/SiO 2 Ni.5 /SiO 2 Ni/Au Selectivity (%) 25 nm nm 2 nm

8 Mengqian Chai et al. / Chinese Journal of Catalysis 38 (217) [15] H. S. Wei, X. F. Wei, X. Yang, G. Z. Yin, A. Q. Wang, X. Y. Liu, Y. Q. Huang, T. Zhang, Chin. J. Catal., 215, 36, [16] Y. Tan, X. Y. Liu, L. L. Zhang, A. Q. Wang, L. Li, X. L. Pan, S. Miao, M. Haruta, H. S. Wei, H. Wang, F. J. Wang, X. D. Wang, T. Zhang, Angew. Chem. Int. Ed., 217, 56, [17] C. Aprile, A. Corma, M. E. Domine, H. Garcia, C. Mitchell, J. Catal., 29, 264, [18] A. C. Gluhoi, J. W. Bakker, B. E. Nieuwenhuys, Catal. Today, 21, 154, [19] X. Y. Liu, C. Y. Mou, S. Lee, Y. N. Li, J. Secrest, B. W. L. Jang, J. Catal., 212, 285, [2] X. L. Yan, J. H. Bao, C. Yuan, J. Wheeler, W. Y. Lin, R. F. Li, B. W. L. Jang, J. Catal., 216, 344, [21] A. Sarkany, A. Horvath, A. Beck, Appl. Catal. A, 22, 229, [22] A. Sarkany, Z. Schay, K. Frey, E. Szeles, I. Sajo, Appl. Catal. A, 21, 38, [23] X. Y. Liu, Y. N. Li, J. W. Lee, C. Y. Hong, C. Y. Mou, B. W. Jang, Appl. Catal. A, 212, 439, [24] J. W. Lee, X. Y. Liu, C. Y. Mou, J. Chin. Chem. Soc., 213, 6, [25] A. Sarkany, O. Geszti, G. Safran, Appl. Catal. A, 28, 35, [26] A. J. McCue, R. T. Baker, J. A. Anderson, Faraday Discuss., 216, 188, [27] G. Kyriakou, M. B. Boucher, A. D. Jewell, E. A. Lewis, T. J. Lawton, A. E. Baber, H. L. Tierney, M. Flytzani Stephanopoulos, E. H. Sykes, Science, 212, 335, [28] G. X. Pei, X. Y. Liu, A. Q. Wang, L. Li, Y. Q. Huang, T. Zhang, J. W. Lee, B. W. L. Jang, C. Y. Mou, New J. Chem., 214, 38, [29] S. Hwang, J. Lee, U. G. Hong, J. C. Jung, J. H. Baik, D. J. Koh, H. Lim, I. K. Song, J. Nanosci. Nanotechnol., 212, 12, [3] H. Ozay, Sci. Adv. Mater., 213, 5, [31] H. Nishikawa, D. Kawamoto, Y. Yamamoto, T. Ishida, H. Ohashi, T. Akita, T. Honma, H. Oji, Y. Kobayashi, A. Hamasaki, T. Yokoyama, M. Tokunaga, J. Catal., 213, 37, [32] S. A. Nikolaev, E. V. Golubina, L. M. Kustov, A. L. Tarasov, O. P. Tkachenko, Kinet. Catal., 214, 55, [33] A. V. Chistyakov, P. A. Zharova, M. V. Tsodikov, S. A. Nikolaev, I. N. Krotova, D. I. Ezzhelenko, Kinet. Catal., 216, 57, [34] A. Aguilar Tapia, L. Delannoy, C. Louis, C. W. Han, V. Ortalan, R. Zanella, J. Catal., 216, 344, [35] Y. Azizi, C. Petit, V. Pitchon, J. Catal., 28, 256, [36] G. X. Pei, X. Y. Liu, A. Q. Wang, A. F. Lee, M. A. Isaacs, L. Li, X. L. Pan, X. F. Yang, X. D. Wang, Z. J. Tai, K. Wilson, T. Zhang, ACS Catal., 215, 5, [37] G. X. Pei, X. Y. Liu, X. F. Yang, L. L. Zhang, A. Q. Wang, L. Li, H. Wang, X. D. Wang, T. Zhang, ACS Catal., 217, 7, [38] S. Labat, F. Bocquet, B. Gilles, O. Thomas, Scripta Mater., 24, 5, [39] M. Tsuji, D. Yamaguchi, M. Matsunaga, K. Ikedo, Cryst. Growth Des., 211, 11, [4] S. H. Zhou, Z. Ma, H. F. Yin, Z. L. Wu, B. Eichhorn, S. H. Overbury, S. Dai, J. Phys. Chem. C, 29, 113, [41] X. Y. Liu, A. Q. Wang, X. D. Wang, C. Y. Mou, T. Zhang, Chem. Commun., 28, [42] X. Wei, X. F. Yang, A. Q. Wang, L. Li, X. Y. Liu, T. Zhang, C. Y. Mou, J. Li, J. Phys. Chem. C, 212, 116, [43] A. Q. Wang, X. Y. Liu, C. Y. Mou, T. Zhang, J. Catal., 213, 38, [44] D. S. Wang,Y. D. Li, J. Am. Chem. Soc., 21, 132, [45] X. Y. Liu, M. H. Liu, Y. C. Luo, C. Y. Mou, S. D. Lin, H. K. Cheng, J. M. Chen, J. F. Lee, T. S. Lin, J. Am. Chem. Soc., 212, 134, [46] M. Mihaylov, H. Knoezinger, K. Hadjiivanov, B. C. Gates, Chem. Ing. Tech., 27, 79, [47] K. I. Hadjiivanov, G. N. Vayssilov, Adv. Catal., 22, 47, [48] S. A. Nikolaev, D. A. Pichugina, D. F. Mukhamedzyanova, Gold Bull., 212, 45, [49] X. Y. Liu, C. Y. Mou, S. Lee, Y. N. Li, J. Secrest, B. W. L. Jang, J. Catal., 212, 285, [5] M. Boronat, P. Concepción, A. Corma, J. Phys. Chem. C, 29, 113, [51] J. H. Xu, Y. Q. Huang, X. F. Yang, L. He, H. R. Zhou, Q. Q. Lin, T. Zhang, H. R. Geng, J. Nanosci. Nanotechnol., 214, 14, SiO 2 负载的 Au-Ni 双金属催化剂在乙炔选择加氢反应中的应用 柴梦倩 a,b, 刘晓艳 a,*, 李林 a, 裴广贤 a,b, 任煜京 a,b, 苏杨 a, 程鸿魁 c, 王爱琴 a a, 张涛 a 中国科学院大连化学物理研究所催化基础国家重点实验室, 辽宁大连 b 中国科学院大学, 北京 149 c 正大能源材料 ( 大连 ) 股份有限公司, 辽宁大连 摘要 : 负载型 Au 催化剂在乙炔选择加氢反应中表现出很高的乙烯选择性, 但其转化率相对较低. 通过添加第二种金属如 Pd, Fe, Ag 和 Cu 等, 制备双金属催化剂是提高其在加氢反应中催化活性的一种非常有效的手段. 其中 Au-Pd 双金属催化剂是最受关注的体系之一, Pd 的加入可以非常显著地提高其催化乙炔选择加氢反应的活性. 据文献报道, 与 Pd 同一主族的 Ni 也具有较好的加氢活性. 尽管与 Pd 相比, Ni 很难与 Au 形成合金, 但目前已有 Au-Ni 双金属催化剂在多种反应中表现出协同效应的报道, 如水气变换 CO 氧化以及芳香硝基化合物选择加氢等. 因此, 向 Au 催化剂中添加 Ni 也可能提高催化剂在乙炔选择加氢反应中的催化活性. 因此, 我们采用两步法制备了一系列 SiO 2 负载的具有不同 Ni:Au 原子比的 Au-Ni 双金属催化剂, 并将其用于乙炔选择加氢反应, 发现 Au-Ni 双金属催化剂在该反应中表现出了显著的协同效应, 其活性明显优于相应单金属催化剂的活性. 尽管其乙烯选择性略低于单金属 Au 催化剂, 但明显高于单金属 Ni 催化剂. 通过调节还原温度和 / 或 Ni:Au 的比例, 对催化剂的性能进行了优化. 结果显示, 当 Ni:Au =.5 时, 催化剂表现出最优的综合性能, 即兼具较高的乙炔转化率和乙烯选择性. 为了研究 Au-Ni 双金属催化剂中金属纳米粒子的结构 组成以及 Au-Ni 之间的相互作用, 我们对催化剂进行了 X 射线衍射 (XRD) 高分辨透射电镜(HRTEM) 能量散射谱(EDS) 以及原位红外光谱 (DRIFTS) 表征. XRD 和 TEM 结果显示, 催化剂

9 1346 Mengqian Chai et al. / Chinese Journal of Catalysis 38 (217) 中的 Au-Ni 双金属纳米粒子都具有高分散和粒径均匀的特点. 通过 EDS 分析, 发现在 Au-Ni 双金属催化剂中的单个金属纳 米粒子同时含有 Au 和 Ni 两种元素, 尽管每个纳米粒子中 Ni:Au 的比例有差异. HRTEM 结果发现, Au-Ni 双金属纳米粒子的 晶格间距介于 Au(111) 和 Ni(111) 的晶面间距之间, 说明在 Au-Ni 双金属催化剂中有 Au-Ni 合金形成. 原位 DRIFTS 结果显示, 在 Au-Ni 双金属催化剂中, Au 的存在促进了 Ni 的还原, 说明 Au 与 Ni 之间存在紧密的相互作用. 综上可见, Au 和 Ni 在乙炔选 择加氢反应中所表现出的协同效应主要归功于 Au-Ni 合金的形成, 其中金属态 Ni 起主要的活性作用, 而 Au 的存在则提高了 催化剂的乙烯选择性. 关键词 : 金 ; 镍 ; 双金属催化剂 ; 协同效应 ; 乙炔加氢 收稿日期 : 接受日期 : 出版日期 : * 通讯联系人. 电话 : (411) ; 传真 : (411) ; 电子信箱 : 基金来源 : 国家自然科学基金 ( , , , , ); 中国科学院青年促进会 (214163); 国家重点研发计划 纳米科技 重点专项 (216YFA2281); 中国科学院战略性先导科技专项 (XDB1721); 辽宁省科技厅 ( ). 本文的英文电子版由 Elsevier 出版社在 ScienceDirect 上出版 (

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