LT6311B - Metal/graphene catalyst preparation method - Google Patents
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Išradimas priskiriamas cheminiams procesams, būtent efektyvių Pt/grafeno katalizatorių gavimo būdui ir gali būti naudojamas įvairiose pramonės srityse, tokiose, kaip cheminių junginių sintezėje, kenksmingų medžiagų išmetimo dujų nukenksminime, alternatyvių energijos šaltinių, t. y. šarminių polimerinių membranų kuro elementų gamyboje, vandenilio dujų gavime.The invention relates to chemical processes, in particular to the preparation of efficient Pt / graphene catalysts, and can be used in a variety of industrial applications such as chemical synthesis, decontamination of harmful exhaust gases, alternative energy sources, e.g. y. in the production of alkaline polymeric membrane fuel cells, in the production of hydrogen gas.
Yra žinomi katalizatoriai, į kurių sudėtį įeina platina (Pt) ir auksas (Au). Nors taurieji metalai Pt ir Au plačiai taikomi kaip elektrokatalizatoriai natrio borhidrido, metanolio ar etanolio oksidacijos reakcijoms, tačiau jų panaudojimas praktiniams tikslams nėra perspektyvus dėl jų brangumo. Siekiant sumažinti naudojamo tauraus metalo kiekį katalizatoriuje, tuo pačiu nesumažinant, o net padidinant jo aktyvumą, buvo pradėti tyrinėti Pt lydiniai su pereinamaisiais metalais - Ni, Co, Cu, Fe (A. Tegou, S. Papadimitriou, I. Mintsouli, S. Armyanov, E. Valova, G. Kokkinidis, S. Sotiropoulos, Rotating disc electrode studies of borohydride oxidation at Pt and bimetallic Pt—Ni and Pt-Co electrodes. Catal. Today 170 (2011) 126-133), (L. Yi, L. Liu, X. Liu, X. VVang, W. Yi, P. He, X. Wang, Carbon-supported Pt-Co nanoparticles as anode catalyst for direct borohydride-hydrogen peroxide fuel cell: Electrocatalysis and fuel cell performance. Int. J. Hydrogen Energy 37 (2012) 12650-12658), (L. Yi, Y. Song, X. Liu, X. VVang, G. Zou, P. He, W. Yi. High activity of Au-Cu/C electrocatalyst as anodic catalyst for direct borohydride-hydrogen peroxide fuel cell. Int. J. Hydrogen Energy 36 (2011) 15775-15782).There are known catalysts containing platinum (Pt) and gold (Au). Although the precious metals Pt and Au are widely used as electrocatalysts for the oxidation reactions of sodium borohydride, methanol or ethanol, their practical use is not viable due to their high cost. In order to reduce the amount of precious metal used in the catalyst, while not reducing or even increasing its activity, investigations were carried out on Pt alloys with transition metals - Ni, Co, Cu, Fe (A. Tegou, S. Papadimitriou, I. Mintsouli, S. Armyanov). , E. Valova, G. Kokkinidis, S. Sotiropoulos, Rotating Disc Electrode Studies on Borohydride Oxidation at Pt and Bimetallic Pt-Ni and Pt-Co Electrodes. Catal. Today 170 (2011) 126-133), (L. Yi, L. Liu, X. Liu, X. Wang, W. Yi, P. He, X. Wang, Carbon-supported Pt-Co nanoparticles as an anode catalyst for direct borohydride-hydrogen peroxide fuel cell: Electrocatalysis and fuel cell performance Int. J. Hydrogen Energy 37 (2012) 12650-12658), (L. Yi, Y. Song, X. Liu, X. Wang, G. Zou, P. He, W. Yi. High activity of Au-Cu / C electrocatalyst as an anodic catalyst for direct borohydride-hydrogen peroxide fuel cell. Int. J. Hydrogen Energy 36 (2011) 15775-15782).
Šio tipo bimetalinių katalizatorių gavimui naudojami įvairūs būdai; organinės sintezės (X. Zhang, K.-Y. Tsang, K.-Y. Chan, Electrocatalytic properties of supported platinum-cobalt nanoparticles with uniform and controlled composition. J. Electroanal. Chem. 573 (2004) 1-9), cheminės redukcijos, reduktoriumi naudojant natrio borhidridą (J. R. C. Salgado, E. Antolini, E. R. Gonzalez, Preparation of Pt-Co/C electrocatalysis by reduction with borohydride in acid and alkaline media: the effect on the performance of the catalyst. J. Power Sources 138 (2004) 56-60; Z. Liu, C. Yu, I. A. Rusakova,There are various methods for obtaining this type of bimetallic catalysts; organic synthesis (X. Zhang, K.-Y. Tsang, K.-Y. Chan, Electrocatalytic properties of supported platinum-cobalt nanoparticles with uniform and controlled composition. J. Electroanal. Chem. 573 (2004) 1-9), chemical reduction using sodium borohydride as a reducing agent (JRC Salgado, E. Antolini, ER Gonzalez, Preparation of Pt-Co / C Electrocatalysis by Reduction with Borohydride in Acid and Alkaline Media: J. Power Sources 138 (2004) 56-60; Z. Liu, C. Yu, IA Rusakova,
D. Huang, P. Strasser, Synthesis of Pt3Co Alloy Nanocatalyst via reverse micelle for oxygen reduction reaction in PEMFCs. Top. Catal. 49 (2008) 241-250), impregnavimo (P. Mania, R. Srivastava, P. Strasser, Dealloyed binary PtlVh (M = Cu, Co, Ni) and ternary PtNiaM (M = Cu, Co, Fe, Cr) electrocatalysts for the oxygen reduction reaction: Performance in polymer electrolyte membrane fuel cells. J. Power Sources 196 (2011) 666-673), cheminiais (žiūr. JAV patentus 6,262,129 B1, 6,783,569 B2, 8,110,021 B2, 2011/0118111 A1, 6,967,183 B2).D. Huang, P. Strasser, Synthesis of Pt3Co Alloy Nanocatalyst via Reverse Micelle for Oxygen Reduction Reaction in PEMFCs. Top. Catal. 49 (2008) 241-250), impregnation (P. Mania, R. Srivastava, P. Strasser, Dealloyed binary PtlVh (M = Cu, Co, Ni) and ternary PtNiaM (M = Cu, Co, Fe, Cr) electrocatalysts for the oxygen reduction reaction: Performance in polymer electrolyte membrane fuel cells. J. Power Sources 196 (2011) 666-673), chemical (see U.S. Patents 6,262,129 B1, 6,783,569 B2, 8,110,021 B2, 2011/0118111 A1, 6,967,183 B2). .
Nors Pt yra vienas iš aktyviausių dehidrinimo katalizatorių organinių junginių elektrooksidacijos reakcijose, bet dėl jos brangumo naudojimas tampa nerentabilus ir neperspektyvus. Todėl keliami tikslai - sumažinti naudojamo tauraus metalo kiekį katalizatoriuje, tuo pačiu padidinant jo aktyvumą. Pastaruoju metu naudojama perspektyvi medžiaga - grafenas, pasižymintis labai dideliu aktyviu paviršiaus plotu (2600 m2g~1), ypatingomis fizikocheminėmis savybėmis, elektroniniu laidumu bei stabilumu.Although Pt is one of the most active dehydrogenation catalysts in electrooxidation reactions of organic compounds, its high cost makes its use unprofitable and unprofitable. Therefore, the goal is to reduce the amount of precious metal used in the catalyst while increasing its activity. A promising material recently used is graphene, which has a very high active surface area (2600 m 2 g ~ 1 ), special physicochemical properties, electronic conductivity and stability.
Artimiausias siūlomam būdui yra Pt/grafeno katalizatoriaus gavimo būdas, kur mišinį iš 0,1 g grafeno miltelių, 0,04 ml 0,036 M FhPtCIe, 19 ml etilenglikolio (99 %), maišo ultragarsu 2 vai. ir apdoroja 170°C temperatūroje mikrobangų reaktoriuje. Gautą mišinį filtruoja, praplauna acetonu, distiliuotu vandeniu ir džiovina vakuuminėje krosnyje 80 °C 2 vai. (M. Semaško, L. Tamašauskaitė-Tamašiūnaitė „Pt/TiC>2-GRAFENO NANOKOMPOZITŲ SINTEZĖ, CHARAKTERIZAVIMAS IR TAIKYMAS METANOLIO KURO ELEMENTUOSE“, Studentų moksliniai tyrimai 2012/2013). Tokiu būdu gauna Pt/grafeno nanokompozitus, kuriuose nusodintos Pt nanodalelės yra 4-7 nm dydžio.The closest to the proposed process is the Pt / graphene catalyst method, whereby a mixture of 0.1 g of graphene powder, 0.04 mL of 0.036 M FhPtCle, 19 mL of ethylene glycol (99%) is sonicated for 2 hours. and processes at 170 ° C in a microwave reactor. The resulting mixture was filtered, washed with acetone, distilled water and dried in a vacuum oven at 80 ° C for 2 hours. (M. Semaško, L. Tamašauskaitė-Tamašiūnaitė “SYNTHESIS, CHARACTERIZATION AND APPLICATION OF Pt / TiC> 2-GRAPHENAN NANO-COMPOSITES IN METHANOL FUEL ELEMENTS”, Student Research 2012/2013). In this way, Pt / graphene nanocomposites are obtained in which the deposited Pt nanoparticles have a size of 4-7 nm.
Nors gautas katalizatorius ir pasižymi geru kataliziniu aktyvumu, tačiau Pt dalelės ant katalizatoriaus išliko didesnio nei norima dydžio.Although the resulting catalyst exhibits good catalytic activity, the Pt particles on the catalyst remain larger than the desired size.
Išradimo tikslas - katalizatorių, pasižyminčių pagerintu elektrokataliziniu aktyvumu su mažesnėmis Pt dalelėmis, gavimo būdas.SUMMARY OF THE INVENTION An object of the present invention is to provide catalysts having improved electrocatalytic activity with smaller Pt particles.
Tikslas pasiekiamas tuo, kad pagal šį išradimą pasiūlytame katalizatoriaus gavimo būde, kur mišinį iš 0,05-0,5 m.% grafeno miltelių,It is an object of the present invention to provide, in a process for the preparation of a catalyst according to the present invention, wherein a mixture of 0.05-0.5% by weight of graphene powder,
0,02-0,1 m.% HhPtCle,0.02-0.1% HhPtCl,
0,039 iki 0,231 m.% Co(ll) druskos0.039 to 0.231% by weight of Co (II) salt
0,04 - 0,633 m. % NaOH0.04 - 0.633 m. % NaOH
99,9 - 99,0 m.% etilenglikolio, maišo ultragarsu 0,5-2 h, mikrobangų reaktoriuje apdoroja 140 - 200 °C temperatūroje 10-30 min, naudojant 300 - 850 W mikrobangų galingumą, maišo 100 - 500 aps/min, suformuoja Pt/grafeno katalizatorių, esant Pt:Co moliniams santykiams, lygiems 1:3,1:10,1:30 ir 1:50, ir kur gautame Pt/grafeno katalizatoriuje nusodintos Pt nanodalelės yra 1-3 nm dydžio.99.9 - 99.0 wt% ethylene glycol, ultrasonically stirred for 0.5-2 h, processed in a microwave reactor at 140 - 200 ° C for 10-30 min using 300 - 850 W microwave power, stirred at 100 - 500 rpm , forms a Pt / graphene catalyst at a Pt: Co molar ratio of 1: 3.1: 10.1: 30 and 1:50, and wherein the resulting Pt / graphene catalyst precipitates Pt nanoparticles in the range of 1-3 nm.
įvedimas pereinamųjų metalų (Ni, Co, Cu) į Pt/grafeno katalizatorių pagerina gautų bimetalinių Pt-Ni, Pt/Co ir Pt/Cu katalizatorių aktyvumą metanolio, natrio borhidrido ir deguonies redukcijos reakcijoms lyginant su grynos Pt elektrodu ir su Pt/grafeno nanokompozitais.introduction of transition metals (Ni, Co, Cu) into Pt / graphene catalysts improves the activity of the resulting bimetallic Pt-Ni, Pt / Co and Pt / Cu catalysts for the reduction reactions of methanol, sodium borohydride and oxygen as compared to pure Pt electrode and Pt / graphene nanocomposites .
Pt lydinių su pereinamaisiais metalais didesnį katalizinį aktyvumą sąlygoja PtM lydinių susidarymas bei Pt elektroninės struktūros pasikeitimas dėl pereinamojo metalo buvimo, Pt-Pt atstumo ir d-elektronų tankio platinoje.The higher catalytic activity of Pt alloys with transition metals is due to the formation of PtM alloys and the change in Pt electronic structure due to the presence of transition metal, Pt-Pt distance and d-electron density in platinum.
Šiuo atveju siūlomas Co pridėjimas į Pt/grafeno katalizatorių padidina gauto PtCo/grafeno katalizatoriaus elektrokatalizinį aktyvumą, lyginant su Pt/grafeno katalizatoriumi ir yra žymiu mastu pigesnis, nes vietoj dalies Pt yra naudojamas Co.In this case, the proposed addition of Co to the Pt / graphene catalyst increases the electrocatalytic activity of the resulting PtCo / graphene catalyst as compared to the Pt / graphene catalyst and is significantly less expensive, since Co is used instead of a portion of Pt.
PAVYZDYS:EXAMPLE:
Reakcijos mišinį iš 0,1 g grafeno miltelių, 0,25 ml 0,096 M HkPtCle, 0.6 ml 0,4 M C0CI2, 0,2-3,2 ml 1 M NaOH ir 18 ml etilenglikolio maišo ultragarsu 1 h. Po to įdeda į mikrobangų reaktorių ir apdoroja 170 °C temperatūroje 30 min, naudojant 700 W mikrobangų galingumą ir 300 aps/min maišymą. Susintetintą platinos-kobalto-grafeno katalizatorių filtruoja, praplauna acetonu, po to distiliuotu vandeniu ir džiovina vakuuminėje krosnyje 80 °C temperatūroje 2 valandas.Reaction mixture of 0.1 g of graphene powder, 0.25 mL of 0.096 M HkPtCle, 0.6 mL of 0.4 M CO 2 Cl 2, 0.2-3.2 mL of 1 M NaOH and 18 mL of ethylene glycol was sonicated for 1 h. It is then placed in a microwave reactor and treated at 170 ° C for 30 min using 700 W microwave power and 300 rpm stirring. The synthesized platinum-cobalt-graphene catalyst is filtered, washed with acetone, then distilled water, and dried in a vacuum oven at 80 ° C for 2 hours.
Tokiu būdu gautas platinos-kobalto-grafeno katalizatorius yra miltelių pavidalo. Keičiant C0CI2 ir NaOH koncentracijas pradinių medžiagų mišinyje, suformuoja platinos-kobalto-grafeno nanokompozitus, esant Pt:Co moliniams santykiams 1:3, 1:10, 1:30 ir 1:50, o nusodintos Pt nanodalelės yra 1-3 nm dydžio.The platinum-cobalt-graphene catalyst thus obtained is in powder form. By varying the concentrations of C0CI2 and NaOH in the mixture of starting materials, platinum-cobalt-graphene nanocomposites are formed at Pt: Co molar ratios of 1: 3, 1:10, 1:30 and 1:50, and the deposited Pt nanoparticles are in the range of 1-3 nm.
Išmatuotos natrio borhidrido oksidacijos srovės tankio vertės ant PtCo/grafenas katalizatoriaus, kai Pt:Co molinis santykis yra 1:44, yra apie 24 kartus didesnės nei jos yra ant Pt/grafenas katalizatoriaus. PtCo/grafenas katalizatoriaus aktyvumą įvairių medžiagų (natrio borhidrido, etanolio ir kt.) oksidacijos reakcijoms apsprendžia PtCo/grafenas katalizatoriaus sudėtis, t.y. Pt:Co molinis santykis. Pvz., didžiausiu elektrokataliziniu aktyvumu natrio borhidrido oksidacijos reakcijai pasižymi PtCo/grafenas katalizatorius, kai Pt:Co molinis santykis yra 1:44, lyginant su katalizatoriais, esant Pt:Co moliniams santykiams 1:7 ir 1:22, kai, tuo tarpu, didžiausiu elektrokataliziniu aktyvumu etanolio oksidacijai šarminėje terpėje pasižymi PtCo/grafenas katalizatorius, esant Pt:Co moliniam santykiui 1:7, lyginant su katalizatoriais, kai Pt:Co molinis santykis yra 1:1 ir 1:44.The measured sodium borohydride oxidation current density values on the PtCo / graphene catalyst at a Pt: Co molar ratio of 1:44 are about 24 times higher than those on the Pt / graphene catalyst. The activity of the PtCo / graphene catalyst for the oxidation reactions of various materials (sodium borohydride, ethanol, etc.) is determined by the composition of the PtCo / graphene catalyst, i.e. Pt: Co molar ratio. For example, the highest electrocatalytic activity for the sodium borohydride oxidation reaction is characterized by a PtCo / graphene catalyst at a Pt: Co molar ratio of 1:44, compared to catalysts at a Pt: Co molar ratio of 1: 7 and 1:22, whereas, the highest electrocatalytic activity for the oxidation of ethanol in alkaline medium is characterized by a PtCo / graphene catalyst at a Pt: Co molar ratio of 1: 7 compared to catalysts with a Pt: Co molar ratio of 1: 1 and 1:44.
Paprastai mažesnio dydžio Pt dalelės pasižymi didesniu kataliziniu aktyvumu, todėl 1-3 nm dydžio Pt nanodalelių nusodinimas yra viena iš sąlygų, taip pat padidinančių PtCo katalizatoriaus aktyvumą (žr. lentelę).Usually, smaller Pt particles exhibit higher catalytic activity, so precipitation of Pt nanoparticles of 1-3 nm size is one of the conditions that also increase the activity of the PtCo catalyst (see Table).
LentelėTable
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Citations (5)
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US6262129B1 (en) | 1998-07-31 | 2001-07-17 | International Business Machines Corporation | Method for producing nanoparticles of transition metals |
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US20110118111A1 (en) | 2009-11-18 | 2011-05-19 | Hyundai Motor Company | PREPARATION METHOD FOR PtCo NANOCUBE CATALYST |
US8110021B2 (en) | 2008-07-28 | 2012-02-07 | Honda Motor Co., Ltd. | Synthesis of PtCo nanoparticles |
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Patent Citations (5)
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US6262129B1 (en) | 1998-07-31 | 2001-07-17 | International Business Machines Corporation | Method for producing nanoparticles of transition metals |
US6967183B2 (en) | 1998-08-27 | 2005-11-22 | Cabot Corporation | Electrocatalyst powders, methods for producing powders and devices fabricated from same |
US6783569B2 (en) | 2001-08-16 | 2004-08-31 | Korea Advanced Institute Of Science And Technology | Method for synthesis of core-shell type and solid solution alloy type metallic nanoparticles via transmetalation reactions and applications of same |
US8110021B2 (en) | 2008-07-28 | 2012-02-07 | Honda Motor Co., Ltd. | Synthesis of PtCo nanoparticles |
US20110118111A1 (en) | 2009-11-18 | 2011-05-19 | Hyundai Motor Company | PREPARATION METHOD FOR PtCo NANOCUBE CATALYST |
Non-Patent Citations (5)
Title |
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A. TEGOU ET AL.: "Rotating disc electrode studies of borohydride oxidation at Pt and bimetallic Pt-Ni and Pt-Co electrodes", CATAL. TODAY, 2011, pages 126 - 133 |
J. R. C. SALGADO ET AL.: "Preparation of Pt-Co/C electrocatalysts by reduction with borohydride in acid and alkaline media", J. POWER SOURCES, 2004, pages 56 - 60, XP004618337, DOI: doi:10.1016/j.jpowsour.2004.06.011 |
L. YI ET AL.: "Carbon-supported Pt-Co nanoparticles as anode catalyst for direct borohydride-hydrogen peroxide fuel cell", INT. J. HYDROGEN ENERGY, 2012, pages 12650 - 12658 |
L. YI ET AL.: "High activity of Au-Cu/C electrocatalyst as anodic catalyst for direct borohydride-hydrogen peroxide fuel cell", INT. J. HYDROGEN ENERGY, 2011, pages 15775 - 15782, XP028320673, DOI: doi:10.1016/j.ijhydene.2011.09.019 |
X. ZHANG ET AL.: "Electrocatalytic properties of supported platinum-cobalt nanoparticles with uniform and controlled composition", J. ELECTROANAL. CHEM., 2004, pages 1 - 9, XP004607070, DOI: doi:10.1016/j.jelechem.2004.06.023 |
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