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US 2012/0132538 A1 May 31,2012 -continued [0036] Theone-stageprocessofproducingbutanolfrom carbondioxideandWatermay yieldadditionalorganicprod ucts, including formic acid and acetic acid, Which Were observedbygaschromatography(GC)andnuclearmagnetic resonance (NMR) With greater relative yields than butanol. Products other than butanol in the product mixture (e.g., formic acid, acetic acid, methanol, ethanol, acetone, and/or propanol) may be reaction intermediates. For instance, becausethereactiontoproducebutanolrequiresatransferof 24electronsandprotons,butanolproductionmay belikelyto be kinetically limited relative to reaction intermediates that requirefeWerelectronandprotontransfers.Forgreaterselec tivity, yield, and reaction rates, the tWo-stage process for producing butanol from carbon dioxide and Water may be employed. The tWo-stage process includes tWo cells With the folloWingreactions: Cell1; 2002+H2O—>OCHCHO+11/202 (E0=-1.44vat25°0.) Cell2; 2(OCHCHO)+3H2O—>C4H9OH+ (E0=—1.76vat25°c.) 302 [0037] Thereactionineachofcell1andcell2requiressix electrons per glyoxal molecule (OCHCHO). Although the total energy requirement for the tWo-stage process may be higherthantheone-stageprocessforproducingbutanolfrom carbon dioxide and Water, much higher selectivity and fara daic yield (current e?iciency) may be provided via the tWo stage process. For instance, experiments Were conducted Whereinagreaterthan25% faradaicyieldforglyoxalWith greater than 90% selectivity Were possible. Moreover, gly oxal Was converted to 2-butanol in the second cell With greaterthan99% selectivity. [0038] ReferringtoFIG.2,ablockdiagramofasystem200 is shoWn in accordance With a speci?c embodiment of the present invention. System 200 may be utiliZed for the tWo stageprocessfortheproductionofbutanolfromcarbondiox ideandWater.The system(orapparatus)200 generallycom prises a ?rst cell 202, a ?rst extractor 204, a second cell 206, and a second extractor 208. The ?rst cell 202 and the second cell 206 may each utiliZe the divided cell structure as dis closed With reference to cell 102 of FIG. 1. [0039] The?rstcell202isgenerallyoperationaltoreduce carbon dioxide into a glyoxal rich mixture. In a particular implementation,the?rstcell202incorporatesinthecathode compartmentatype430stainlesssteelcathode,a60mM concentrationofimidaZolecatalyst,anda0.5M KCl electro lyte. The cathode compartment may be pH adjusted to betWeenapproximately5andapproximately8byusing,for example,sodiumhydroxide(NaOH)orpotassiumhydroxide (KOH). Carbondioxidemay bebubbledthroughthecathode compartment, Where the cathode potential may be approxi mately —lV vs. SCE (saturated calomel electrode). Pyrrole and other chemicals that react to convert aldehydes to imines oracetalsmay beaddedtothecatholyteofthe?rstcell202to drive the kinetics of the reaction in the cell toWard greater glyoxalproduction.Asolidsorbentmayservethesamerole andalsosimultaneouslyextractglyoxalforuseinthesecond cell206.Theanolyteinthe?rstcell202may consistofWater With an electrolyte to permit Water oxidation at the anode. Water may be added to the anode compartment as itis con sumed for the process. Glyoxal may be extracted from the productmixtureofthe?rstcell202Withthe?rstextractor204 Which may incorporate any combination of derivitiZation, liquid-liquid extraction, and/or solid sorbents. While FIG. 2 depictsthe?rstextractor204separatedfromthe?rstcell202, itmay be appreciated that various extraction processes and instrumentation may be part of, implemented With, and/or coupled to the ?rst cell 202 in order to extract a particular product(e.g.,glyoxal)oftheproductmixture. [0040] Glyoxalformationinthecathodecompartmentof the ?rst cell 202 may be aided through various combinations of cathode materials, catalysts, and cell conditions. For instance, the cathode material may include indium, tin, molybdenum, 316 stainless stel, nickel 625, nickel 600, nickel-chromium, elgiloy (cobalt-nickel-chromium), and copper-nickel. Iron, stel, cobalt, chromium, and alloys thereofmay alsobeutiliZedascathodematerialinthecathode compartmentofthe?rstcell202.Catalystsinthe?rstcell202 maybeincludepyridine,quinoline,1-methylimidaZole,4,4' bipyridine,andotherheterocyclestoconvertcarbondioxide toglyoxalundertheappropriateconditions.Suchconditions may include loWer pHs and differing electrolytes. The com binationofcathode,catalyst,andcellconditionssu?icientfor the reaction in the cathode compartment of the ?rst cell 202 may be disclosedinUs. patentapplicationSer.No. 12/846, 221,entitled“ReducingCarbonDioxidetoProducts,”Which isherebyincorporatedbyreference. [0041] Theproductmixtureofthe?rstcell202mayinclude one or more tWo-carbon intermediates including glyoxal, oxalic acid, glyoxylic acid, glycolic acid, acetic acid, and acetaldehyde. One ormore ofthecomponents oftheproduct mixturemay beutiliZedasanintermediateinthetWo-stage process(i.e.,may beusedasaninputtothesecondcell206). Glyoxalmay includebene?cialcharacteristicsforuseasthe intermediate,including,butnotlimitedto,beingnon-corro sive,beingstableinWater,andrequiringsixelectronsforits formationfromcarbondioxideandWater.Generally,the?rst extractor 204 is su?icient to provide a component-rich por tion 210 as an input to the second cell 206, and a component lean portion 212 (e.g., catholyte rich portion) that may be utiliZed for additional reactions in the ?rst cell 202. [0042] Inthesecondcell206,atWo-carbonintermediate, such as glyoxal, may be converted to 2-butanol via electro hydrodimeriZation, as disclosed in Us. patent application Ser.No. 12/846,011,“HeterocycleCatalyZedElectrochemi calProcess,”Whichisherebyincorporatedbyreference.Ina particularimplementation,aqueousglyoxalisintroducedasa reactant to the second cell 206 With concentrations of up to approximately40%.Thecatholyteinthesecondcell206may include Water and KCl, or other suitable electrolyte. The cathode compartment in the second cell 206 may include a catalyst,includingaheterocycliccatalyst,suchas4,4'bipri dine. HoWever, in some instances, no catalyst or no hetero cycliccatalystisprovidedinthecathodecompartmentinthe second cell 206, Whereby the cathode itself facilitates the tWo-carbon intermediate to butanol reaction. The anolyte in theanodecompartmentofthesecondcell206may include Water With an electrolyte su?icient for Water oxidation at the anode. [0043] Thesecondcell206mayincludeabutanolrich output 214 as a product of the second cell reactions. ThePDF Image | ELECTROCHEMICAL PRODUCTION OF BUTANOL FROM CO2 and H2O
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