00838nas a2200193 4500008004100000245010600041210006900147260000800216300001200224490000700236520013000243100002100373700002100394700002600415700002600441700002100467700002900488856012700517 2009 eng d00aContinuous hydroxyalkylation of p-Cresol to 2,2 `-methylenebis(4-Methylphenol) in a fixed bed reactor0 aContinuous hydroxyalkylation of pCresol to 22 methylenebis4Methy cOCT a782-7870 v423 a

{Catalytic activity of various solid acid catalysts is evaluated for the continuous hydroxyalkylation of p-cresol to [

1 aGarade, Ajit, C.1 aHengne, Amol, M.1 aDeshpande, Tushar, N.1 aShaligram, Sayali, V.1 aShirai, Masayuki1 aRode, Chandrashekhar, V. uhttps://library.ncl.res.in/content/continuous-hydroxyalkylation-p-cresol-22-methylenebis4-methylphenol-fixed-bed-reactor-001646nas a2200277 4500008004100000022001400041245008400055210006900139260005700208300001200265490000800277520071600285653000601001653001801007653002401025653001301049653002901062100002101091700002101112700002501133700002801158700002301186700002101209700002901230856010901259 2010 eng d a1011-372X00aCu:Al Nano catalyst for selective hydrogenolysis of glycerol to 1,2-propanediol0 aCuAl Nano catalyst for selective hydrogenolysis of glycerol to 1 a233 SPRING ST, NEW YORK, NY 10013 USAbSPRINGERcMAR a141-1470 v1353 a

Non-chromium Cu:Al nano catalyst prepared by simultaneous co-precipitation and digestion method without any template or stabilizer, showed three times higher activity than the bulk Cu-Cr catalyst for hydrogenolysis of glycerol in both isopropanol and water solvents, with the selectivity to 1,2-Propanediol (1,2-PDO) as high as 91% at 493 K and H(2) pressure of 7 MPa in 5 h. XRD pattern showed the presence of Cu(+) species in the activated Cu: Al nano catalyst. Although Cu(+) is catalytically inactive in glycerol hydrogenolysis reaction, the presence of Cu(+) helps to stabilize the particle size in a narrow range of 7-11 nm by inhibiting the sintering of copper particles under reaction conditions.

10a110a2-Propanediol10aCu:Al nano catalyst10aGlycerol10aSelective hydrogenolysis1 aMane, Rasika, B.1 aHengne, Amol, M.1 aGhalwadkar, Ajay, A.1 aVijayanand, Subramanian1 aMohite, Pravin, H.1 aPotdar, Hari, S.1 aRode, Chandrashekhar, V. uhttps://library.ncl.res.in/content/cual-nano-catalyst-selective-hydrogenolysis-glycerol-12-propanediol-001723nas a2200205 4500008004100000022001400041245011500055210006900170260007100239300001400310490000700324520091700331100002801248700002501276700001701301700002101318700002301339700002501362856013001387 2010 eng d a1083-616000aSelective hydrogenolysis of glycerol to 1,2-propanediol: comparison of batch and continuous process operations0 aSelective hydrogenolysis of glycerol to 12propanediol comparison a1155 16TH ST, NW, WASHINGTON, DC 20036 USAbAMER CHEMICAL SOCcNOV a1393-14000 v143 a

The screening of copper chromite catalysts with various promoters such as Al, Zn, and Ba for glycerol hydrogenolysis to 1,2-propanediol (1,2-PDO) in a batch reaction showed that Cu-Cr (Ba) catalyst gave the highest conversion of 34% and selectivity of 84% to 1,2-PDO. In a continuous operation (23 g catalyst bed) the same catalyst showed higher conversion of glycerol and selectivity for 1,2-PDO of 65% and > 90%, respectively, with an on-stream activity of similar to 800 h. Better performance in a continuous operation could be due to the in situ activation of the catalyst, suppression of glycerol cracking to ethylene glycol, as well as excessive hydrogenation of 1,2-PDO to 2-propanol due to lower contact time of 1.3 h as compared to that in a batch operation (5 h). Effects of various process parameters on conversion and selectivity also have been compared for batch and continuous operations.

1 aRode, Chandrashekhar, V1 aGhalwadkar, Ajay, A.1 aMane, R., B.1 aHengne, Amol, M.1 aJadkar, Sachin, T.1 aBiradar, Narayan, S. uhttps://library.ncl.res.in/content/selective-hydrogenolysis-glycerol-12-propanediol-comparison-batch-and-continuous-process-001769nas a2200265 4500008004100000022001400041245008200055210006900137260007300206300001200279490000800291520089000299653000601189653002301195653001101218653001601229653002801245653002001273100001701293700002501310700002101335700002401356700001701380856010601397 2011 eng d a0920-586100aRole of promoters in copper chromite catalysts for hydrogenolysis of glycerol0 aRole of promoters in copper chromite catalysts for hydrogenolysi aPO BOX 211, 1000 AE AMSTERDAM, NETHERLANDSbELSEVIER SCIENCE BVcAPR a447-4500 v1643 a

Various copper chromite catalysts with and without promoters were prepared by simultaneous co-precipitation and digestion technique and the role of promoters (Al, Ba and Zn) was investigated for hydrogenolysis of glycerol to 1,2-propylene glycol (1,2-PG) in both batch and continuous operations. Among various promoters studied, copper chromite catalyst with Ba as a promoter showed the highest activity and selectivity of 85% to 1,2-PG. This catalyst was found to be active for more than 800 h in a continuous operation also. Ammonia TPD results showed that barium promoted copper chromite catalyst had the highest acidity which facilitates the dehydration of glycerol to acetol which is the first step in hydrogenolysis of glycerol to 1,2-PG. The effect of barium content and variation in the promoters combination was also studied. (C) 2010 Elsevier B.V. All rights reserved.

10a110a2-Propylene glycol10aAcetol10aAmmonia TPD10aGlycerol hydrogenolysis10aSurface acidity1 aMane, R., B.1 aGhalwadkar, Ajay, A.1 aHengne, Amol, M.1 aSuryawanshi, Y., R.1 aRode, C., V. uhttps://library.ncl.res.in/content/role-promoters-copper-chromite-catalysts-hydrogenolysis-glycerol-001883nas a2200157 4500008004100000022001400041245011800055210006900173260011000242300001400352490000700366520117100373100002101544700002901565856013101594 2012 eng d a1463-926200aCu-ZrO2 nanocomposite catalyst for selective hydrogenation of levulinic acid and its ester to gamma-valerolactone0 aCuZrO2 nanocomposite catalyst for selective hydrogenation of lev aTHOMAS GRAHAM HOUSE, SCIENCE PARK, MILTON RD, CAMBRIDGE CB4 0WF, CAMBS, ENGLANDbROYAL SOC CHEMISTRYcFEB a1064-10720 v143 a

Several copper based catalysts were prepared, characterized and evaluated for the hydrogenation of levulinic acid and its methyl ester. Among these, nanocomposites of Cu-ZrO2 and Cu-Al2O3 quantitatively catalyzed the hydrogenation of levulinic acid and its methyl ester to give 90-100% selectivity to gamma-valerolactone in methanol and water respectively. Both the Cu-ZrO2 and Cu-Al2O3 nanocomposites were prepared by the co-precipitation method using mixed precursors under controlled conditions. XRD results showed that the main active phase of the reduced Cu-ZrO2 catalyst was metallic copper and particle size was found to be of 10-14 nm by HRTEM. The active metal leaching was at a maximum for the Cu-Al2O3 catalyst in a water medium due to the formation of a copper-carboxylate complex that was blue in colour. Surprisingly, copper leaching was completely suppressed in the case of the Cu-ZrO2 catalyst in methanol in spite of the substrate loading was increased from 5 to 20% w/w. The excellent recyclability of the Cu-ZrO2 catalyst with complete LA conversion and > 90% GVL selectivity makes it a sustainable process having a commercial potential.

1 aHengne, Amol, M.1 aRode, Chandrashekhar, V. uhttps://library.ncl.res.in/content/cu-zro2-nanocomposite-catalyst-selective-hydrogenation-levulinic-acid-and-its-ester-gamma-001674nas a2200253 4500008004100000022001400041245012900055210006900184260005700253300001200310490000800322520076900330653001301099653001701112653002401129653001201153653001801165653002201183653000801205100002101213700002501234700002901259856013201288 2012 eng d a1011-372X00aSurface species of supported ruthenium catalysts in selective hydrogenation of levulinic esters for bio-refinery application0 aSurface species of supported ruthenium catalysts in selective hy a233 SPRING ST, NEW YORK, NY 10013 USAbSPRINGERcJUN a779-7870 v1423 a

Several supported noble metal catalysts were screened for the hydrogenation of methyl levulinate to gamma-valerolactone (GVL). Among these catalysts 5 % Ru/C showed the highest conversion of 95 % of methyl levulinate with 91 % selectivity to GVL. A detailed characterization was carried out using TPR, XRD, XPS and BET techniques. XPS studies revealed that higher extent of Ru-0 species in case of carbon supported Ru was responsible for its higher hydrogenation activity as compared to Ru on other supports. Effect of process parameters such as temperature, H-2 pressure, catalyst and substrate concentration and metal loading on methyl LA conversion and selectivity to GVL also has been studied. 5 % Ru/C catalyst was found to be stable up to five reuses.

10a5 % Ru/C10aBiofeedstock10agamma-Valerolactone10aH-2-TPR10aHydrogenation10aMethyl levulinate10aXPS1 aHengne, Amol, M.1 aBiradar, Narayan, S.1 aRode, Chandrashekhar, V. uhttps://library.ncl.res.in/content/surface-species-supported-ruthenium-catalysts-selective-hydrogenation-levulinic-esters-bio-002149nas a2200169 4500008004100000022001400041245016200055210006900217260011000286300001400396490000700410520136000417100002101777700002201798700002901820856013001849 2013 eng d a1463-926200aSingle pot conversion of furfuryl alcohol to levulinic esters and gamma-valerolactone in the presence of sulfonic acid functionalized ILs and metal catalysts0 aSingle pot conversion of furfuryl alcohol to levulinic esters an aTHOMAS GRAHAM HOUSE, SCIENCE PARK, MILTON RD, CAMBRIDGE CB4 0WF, CAMBS, ENGLANDbROYAL SOC CHEMISTRYcJUL a2540-25470 v153 a

Ionic liquids functionalized with acidic anions, HSO4, ClSO3H, PTSA, TFA (MIm), HSO4 and TFA (NMP) were found to efficiently (99% conversion) catalyze the alcoholysis of furfuryl alcohol (FAL) in the presence of methanol, ethanol, n-butanol and isopropyl alcohol (IPA) to the corresponding levulinic acid esters under mild temperature (90-130 degrees C) conditions. The extended alkyl chain length of [MIm] using 1,4-butane sultone enhanced the Bronsted acidity of [BMIm-SH][HSO4] catalyst resulting into the highest selectivity of >95% to Me-LA. An increase in both temperature and catalyst concentration increased the furfuryl alcohol conversion and selectivity to levulinate esters. In contrast, an increase in the substrate concentration from 5 to 15% caused a decrease in Me-LA selectivity due to accumulation of intermediate ethers of furfuryl alcohol. Using a combination of [BMIm-SH][HSO4] and 5% Ru/C catalyst, direct conversion of FAL to gamma-valerolactone (GVL) is shown for the first time. A complete conversion of FAL with the highest selectivity of 68% to GVL could be achieved under optimum conditions while higher Ru loading enhanced the GVL selectivity to 94% in the hydrogenation step of this tandem approach. Our catalyst system could be efficiently recycled five times retaining the original activity and selectivity levels.

1 aHengne, Amol, M.1 aKamble, Sumit, B.1 aRode, Chandrashekhar, V. uhttps://library.ncl.res.in/content/single-pot-conversion-furfuryl-alcohol-levulinic-esters-and-gamma-valerolactone-presence-001810nas a2200265 4500008004100000022001400041245009000055210006900145260007100214300001200285490000600297520089200303653002301195653001801218653001101236653001801247653001001265100002501275700002101300700002501321700002801346700002501374700002901399856011601428 2014 eng d a2168-048500aSingle-pot formation of THFAL via catalytic hydrogenation of FFR over Pd/MFI catalyst0 aSinglepot formation of THFAL via catalytic hydrogenation of FFR  a1155 16TH ST, NW, WASHINGTON, DC 20036 USAbAMER CHEMICAL SOCcFEB a272-2810 v23 a

Furfural (FFR) was selectively hydrogenated in a single pot to tetrahydrofurfuryl alcohol (THFAL) over a Si MFI molecular sieve supported Pd catalyst. Studies on catalyst screening revealed that both the metal function and the support were critical for directing the selectivity to the ringhydrogenated product, THFAL. The structural feature of MFI as shown by XRD was completely retained in the used sample of the 3% Pd/MFI catalyst confirming its stability under reaction conditions. XRD, along with SEM characterization of the used samples, established retention of morphology of the structured silicate, suggesting a strong interaction between hexagonal porous silicate and Pd particles. The complete conversion of FFR with an enhanced selectivity of 95% to THFAL could be achieved by recycling the crude of the first hydrogenation experiment over the same 3% Pd/MFI catalyst.

10aBiomass conversion10aHydrogenation10aPd/MFI10aRecyclability10aTHFAL1 aBiradar, Narayan, S.1 aHengne, Amol, M.1 aBirajdar, Shobha, N.1 aNiphadkar, Prashant, S.1 aJoshi, Praphulla, N.1 aRode, Chandrashekhar, V. uhttps://library.ncl.res.in/content/single-pot-formation-thfal-catalytic-hydrogenation-ffr-over-pdmfi-catalyst-001248nas a2200181 4500008004100000022001400041245012800055210006900183260011000252300001400362490000600376520045600382100002100838700002500859700002500884700002900909856012800938 2014 eng d a2046-206900aSurface synergism of an Ag-Ni/ZrO2 nanocomposite for the catalytic transfer hydrogenation of bio-derived platform molecules0 aSurface synergism of an AgNiZrO2 nanocomposite for the catalytic aTHOMAS GRAHAM HOUSE, SCIENCE PARK, MILTON RD, CAMBRIDGE CB4 0WF, CAMBS, ENGLANDbROYAL SOC CHEMISTRYcFEB a9730-97360 v43 a

Levulinic acid was completely and selectively converted to GVL, in the presence of formic acid over an Ag-Ni/ZrO2 catalyst. The synergism between Ag and Ni in transfer hydrogenation eliminates the need for external hydrogen, making the process safer. The magnetic nature of the catalyst offers easy recovery for efficient recycling. This approach is standardized for the hydrogenation of several C-3-C-6 platform molecules in an aqueous medium.

1 aHengne, Amol, M.1 aMalawadkar, Atul, V.1 aBiradar, Narayan, S.1 aRode, Chandrashekhar, V. uhttps://library.ncl.res.in/content/surface-synergism-ag-nizro2-nanocomposite-catalytic-transfer-hydrogenation-bio-derived-002367nas a2200181 4500008004100000245010700041210006900148260000800217300001600225490000700241520169400248100002201942700002101964700002501985700002902010700002402039856012202063 2016 eng d00aReductive cyclization of levulinic acid to gamma-valerolactone over non-noble bimetallic nanocomposite0 aReductive cyclization of levulinic acid to gammavalerolactone ov cDEC a13032-130390 v553 aBimetallic nanoparticles have diverse applications in catalytic processes owing to the differences in individual properties that contribute to their increased catalytic activity. To further improve the efficiency, they are dispersed in an inert support that enhances the catalytic activity toward organic transformations. In this study, we report simple, facile, and cost-effective chemical route for the fabrication of nanocomposites with Fe-Ni bimetallic nanoparticles supported on montmorillonite (MMT) possessing variation in the Fe and Ni content. These composites are characterized with X-ray diffraction, transmission electron microscopy surface area, and NH3-TPD. Fe Ni bimetallic nanoparticles are well-dispersed within MMT structure having particle sizes of about 30-40 nm. Among various compositions of Fe-Ni/MMT catalysts, composite with 25% Fe and 25% Ni exhibits >99% LA conversion with 98% selectivity to GVL within 1 h. IPA is found to be better solvent for levulinic acid (LA) to gamma-valerolactone (GVL) conversion, while substantial leaching of iron takes place when water is used as a solvent. It is observed that bimetallic sites are responsible for reduction of LA, while strong acidic sites of MMT are favoring subsequent cyclization to GVL. XPS analysis of fresh and reused Fe-Ni/MMT composites suggest that the catalyst surface does not undergo any chemical change during successive cycles, and the catalytic activity is retained up to six cycles. The plausible mechanism for LA to GVL conversion involves reductive cyclization processes through formation of levulinate ester that undergoes lactonization due to synergism in bimetallic nanoparticles and MMT clay.1 aKadu, Brijesh, S.1 aHengne, Amol, M.1 aBiradar, Narayan, S.1 aRode, Chandrashekhar, V.1 aChikate, Rajeev, C. uhttps://library.ncl.res.in/content/reductive-cyclization-levulinic-acid-gamma-valerolactone-over-non-noble-bimetallic01446nas a2200253 4500008004100000022001400041245009400055210006900149260005700218300001400275490000800289520056900297653001000866653001300876653002100889653001700910653002700927100002500954700002100979700001901000700001801019700002901037856012601066 2016 eng d a1011-372X00aSingle pot transfer hydrogenation and aldolization of furfural over metal oxide catalysts0 aSingle pot transfer hydrogenation and aldolization of furfural o a233 SPRING ST, NEW YORK, NY 10013 USAbSPRINGERcAUG a1611-16190 v1463 a

One pot catalytic transfer hydrogenation (CTH) of furfural to furfuryl alcohol (FAL) by using hydrogen producing alcohols and simultaneous aldolization of carbonyl compounds produced during CTH, with furfural was achieved over non-noble metal oxides with bifunctional sites. Basic sites of MgO responsible for abstraction of proton showed complete conversion of furfural to give FAL and C8 monomer in a ratio of 3:1, respectively, the later altered to 1:1 by incorporating Al into MgO. Catalyst stability was established by its four cycles study. [GRAPHICS]

10aAldol10afurfural10aFurfuryl alcohol10aMetal oxides10atransfer hydrogenation1 aBiradar, Narayan, S.1 aHengne, Amol, M.1 aSakate, S., S.1 aSwami, R., K.1 aRode, Chandrashekhar, V. uhttps://library.ncl.res.in/content/single-pot-transfer-hydrogenation-and-aldolization-furfural-over-metal-oxide-catalysts02168nas a2200193 4500008004100000022001400041245011200055210006900167260011000236300001600346490000600362520135400368100002101722700002201743700002501765700002401790700002901814856013101843 2016 eng d a2046-206900aTransfer hydrogenation of biomass-derived levulinic acid to gamma-valerolactone over supported Ni catalysts0 aTransfer hydrogenation of biomassderived levulinic acid to gamma aTHOMAS GRAHAM HOUSE, SCIENCE PARK, MILTON RD, CAMBRIDGE CB4 0WF, CAMBS, ENGLANDbROYAL SOC CHEMISTRYcJUN a59753-597610 v63 a

A sustainable process of catalytic transfer hydrogenation (CTH) of levulinic acid (LA) to gamma-valerolactone (GVL) was investigated over Ni on various supports (Al2O3, ZnO, MMT and SiO2) in the presence of isopropanol (IPA) as the H-donor. Among these, the montmorillonite (MMT) supported Ni catalyst showed almost complete LA conversion (>99%) and selectivity (>99%) to GVL within 1 h. XRD and XPS results showed that the concentration of the metallic species significantly enhanced (two to four times) in the recovered sample as compared to the freshly prepared Ni/MMT. This was due to the in situ reduction of Ni2+ species present on the catalyst surface, through liberated H-2 under the reaction conditions. The strong acid strength of MMT, evidenced by NH3-TPD and py-IR, facilitated the esterification of LA as well as cyclization to GVL. The conversion-selectivity pattern was found to decrease in the IPA-water mixture while, it remained unchanged in the IPA-acetone mixture. Our catalyst could be efficiently recycled up to five times with consistent CTH activity and selectivity to GVL. The plausible mechanism of LA to GVL conversion involves the formation of a levulinate ester with IPA that favours its simultaneous hydrogenation and cyclization in a spontaneous manner to give GVL and regenerating IPA for sustainability.

1 aHengne, Amol, M.1 aKadu, Brijesh, S.1 aBiradar, Narayan, S.1 aChikate, Rajeev, C.1 aRode, Chandrashekhar, V. uhttps://library.ncl.res.in/content/transfer-hydrogenation-biomass-derived-levulinic-acid-gamma-valerolactone-over-supported-ni01900nas a2200181 4500008004100000245010800041210006900149260000800218300001400226490000700240520123300247100002101480700002101501700001601522700002401538700002901562856012701591 2018 eng d00aSingle pot selective hydrogenation of furfural to 2-methylfuran over carbon supported iridium catalysts0 aSingle pot selective hydrogenation of furfural to 2methylfuran o cMAY a2027-20370 v203 aVarious iridium supported carbon catalysts were prepared and screened for the direct hydrogenation of furfural (FFR) to 2-methyl furan (2-MF). Amongst these, 5% Ir/C showed excellent results with complete FFR conversion and highest selectivity of 95% to 2-MF at a very low H-2 pressure of 100 psig. Metallic (Ir degrees) and oxide (IrO2) phases of Ir catalyzed the first step hydrogenation involving FFR to FAL and subsequent hydrogenation to 2-MF, respectively. This was confirmed by XPS analysis and some control experiments. At a low temperature of 140 degrees C, almost equal selectivities of FAL (42%) and 2-MF (43%) were observed, while the higher temperature (220 degrees C) favored selective hydrodeoxygenation. At optimized temperature, 2-MF was formed selectively while higher pressure and higher catalyst loading favored ring hydrogenation of furfural rather than side chain hydrogenation. With the combination of several control experimental results and detailed catalyst characterization, a plausible reaction pathway has been proposed for the selective formation of 2-MF. The selectivity to various other products in FFR hydrogenation can be manipulated by tailoring the reaction conditions over the same catalyst.1 aDate, Nandan, S.1 aHengne, Amol, M.1 aHuang, K-W.1 aChikate, Rajeev, C.1 aRode, Chandrashekhar, V. uhttps://library.ncl.res.in/content/single-pot-selective-hydrogenation-furfural-2-methylfuran-over-carbon-supported-iridium01927nas a2200217 4500008004100000022001400041245011600055210006900171260000800240300001600248490000700264520115800271100002101429700002101450700002101471700001801492700002301510700002501533700001901558856013201577 2019 eng d a0888-588500aPreparation and activity of copper-gallium nanocomposite catalysts for carbon dioxide hydrogenation to methanol0 aPreparation and activity of coppergallium nanocomposite catalyst cNOV a21331-213400 v583 a

Copper (Cu) nanocomposite catalysts with gallium (Ga) and aluminum (Al) were prepared using the simultaneous coprecipitation digestion method. The catalysts were characterized by N-2 adsorption, N2O titration, XRD (X-ray diffraction), H-2-TPR (H-2 temperature-programmed reduction), XPS (X-ray photoelectron spectroscopy), and CO2-TPD (CO2 temperature-programmed desorption) techniques, and CO2 hydrogenation to methanol synthesis was performed. The use of Ga in Cu catalysts enhanced the weak basic sites more than the Cu catalysts with Al. With the CuGa nanocomposite formation, the catalyst showed a sequential reduction of CuO, for example, Cu+2 to Cu+ to Cu-0, and the Cu surface area was also high in comparison with CuAl. These findings confirmed that both the Cu surface area and CuO reducibility in the catalyst helped to boost the conversion of CO2, whereas selectivity to methanol was associated with the basicity of the catalyst. CuAl catalysts showed very poor selectivity to methanol despite CO formation, which could be due to the weak interaction of the CuAl nanocomposite catalysts compared to the CuGa nanocomposite catalysts.

1 aHengne, Amol, M.1 aYuan, Ding, Jier1 aDate, Nandan, S.1 aSaih, Youssef1 aKamble, Sanjay, P.1 aRode, Chandrashekhar1 aHuang, Kuo-Wei uhttps://library.ncl.res.in/content/preparation-and-activity-copper-gallium-nanocomposite-catalysts-carbon-dioxide-hydrogenation02423nas a2200253 4500008004100000022001400041245011300055210006900168260000900237300001400246490000600260520155200266653002801818653002401846653001301870653001801883653002301901100002101924700002101945700001901966700002401985700002902009856013102038 2020 eng d a2365-654900aOne pot hydrogenation of furfural to 2-methyl tetrahydrofuran over supported mono- and Bi-metallic catalysts0 aOne pot hydrogenation of furfural to 2methyl tetrahydrofuran ove cAUG  a9590-96000 v53 a

2-Methyltetrahydrofuran is a valuable commercial product that can be obtained by direct hydrogenation of furfural. In the present study, among several carbon supported bimetallic Ir-Ni catalysts with different loadings screened, 4% Ir-4% Ni/C catalyst showed excellent activity in terms of direct conversion (99%) to 2-MeTHF with a maximum selectivity of similar to 74% at 220 degrees C and 750 psig, suppressing the formation of side chain as well as ring opening products. The catalytic activity was found to be mainly affected by catalyst preparation methods, metal loadings, surface composition, temperature, pressure and catalyst loading. HR-TEM and STEM revealed well dispersed Ir-Ni NPs having the particle sizes in the range of 2 to 5 nm. Different phases of Ir i. e. Ir degrees and IrO(2)as well as oxygen vacancies were found to be responsible for hydrogenation of furfural to 2-methyl furan while, Ni degrees and NiO were responsible for further hydrogenation to 2-MeTHF. The synergic effect between Ir and Ni was established through XPS, H-2-TPR analysis. With the help of some control experiments, the plausible reaction pathway was also proposed. The catalyst prepared by co-impregnation method found more effective than prepared by sequential addition method. At lower Ni loadings of 1% and 2%, low temperature of 160 degrees C as well as at low H(2)pressure of 250 psig, mixture of furfuryl alcohol and 2-methyl furan were formed selectively. Catalyst could be successfully reused up to 3 times without leaching of metals.

10a2-Methyltetrahydrofuran10aBimetallic catalyst10afurfural10aHydrogenation10aOER type mechanism1 aDate, Nandan, S.1 aHengne, Amol, M.1 aHuang, K., -W.1 aChikate, Rajeev, C.1 aRode, Chandrashekhar, V. uhttps://library.ncl.res.in/content/one-pot-hydrogenation-furfural-2-methyl-tetrahydrofuran-over-supported-mono-and-bi-metallic