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11 stream can represent a potential loss of entrainer, Which can be compensated for by the introduction of additional entrainertotheprocess. In one embodiment, feed stream 430 further comprises ethanol. As described herein above, the feed stream 430 is distilledinthe?rstdistillationcolumn 650 toprovidethe?rst bottoms stream 410, Which comprises the extractant and Waterandissubstantiallyfreeofbutanol,entrainer,andetha nol, and the ?rstvaporous overhead stream 300, Which com prises Water, butanol, entrainer, ethanol, and any non-con densable gas present inthe feed. The ?rstbottoms stream 410 can include from about 3 to about 15 Weight percent Water, less than about 0.01 Weight percent butanol, less than about 0.01Weightpercentethanol,andlessthanabout0.01Weight percent entrainer. Feed stream 430 comprising butanol and ethanol is introduced into column 650 at a feed point above thestrippingsection. When the feed comprises butanol and ethanol, the vapor ous overhead stream 300 from the ?rst distillationcolumn can include10toabout40Weightpercentbutanol,about1to20 about10Weightpercentethanol,about10toabout50Weight percent Water, and about 5 to about 30 Weight percent entrainer. The composition of stream 300 Will depend on the composition of the feed stream, the operating conditions of the?rstcolumn(forexampletemperatureandpressure),and 25 theamount ofentrainercirculatingintheprocess.When more entrainer is used in the process than about the minimal amount su?icient to provide phase separation of the ?rst mixed condensate under the selected operating conditions, theamountofentrainerinstream300isproportionately30 increased, and the Weight percentages of butanol, ethanol, and Water are proportionately decreased. Condensation of stream 300 produces the ?rst mixed condensate stream 350, Which should comprise su?icient entrainer to provide phase separationoftheorganicandtheaqueousphases.Theliquid 35 organicphasecomprisesbutanol,entrainer,ethanol,and optionally the extractant. The liquid organic phase can con tain less than about 80 Weight percent, or from about 40 to about70Weightpercent,entrainer.Theliquidaqueousphase issubstantiallyfreeofentrainerandcomprisesWater,40 butanol, and ethanol. The liquid aqueous phase can contain lessthanabout0.1Weightpercententrainer. As disclosedhereinabove,the?rstportionoftheorganic phase leaving the decanter, stream 500, is distilled in the seconddistillationcolumn950toprovidethesecondbottoms 45 stream 600 and the second vaporous overhead stream 210. When thefeedstream430 comprisesbutanolandethanol,the second bottoms stream 600 also comprises butanol and etha nol. In general, operating conditions for the ?rst and second columnscanbeselectedtomaintainaboutthesameratio(on 50 a mass basis) of ethanol to butanol in stream 600 as in feed stream 430. Stream 600 may contain from about 70 Weight percent to about 99 Weight percent butanol and from about 1 Weight percent to about 30 Weight percent ethanol. Stream 600mayalsocontainsmallquantitiesofextractantand55 entrainer. The vaporous overhead stream 210 can contain from about 1 Weight percent to about 10 Weight percent butanol, from about 1 Weight percent to about 10 Weight percentethanol,andfromabout70Weightpercenttoabout90 Weightpercententrainer. The entrainer can be introduced to any appropriate point or points in the portion of the process through Which the entrainer circulates. Appropriate process streams or vessels to Whichtheentrainer(orastreamcomprisingtheentrainer)can be added include the feed stream 430, the ?rst vaporous 65 overhead stream 300, the ?rst mixed condensate stream 350, thesecondcondensatestream250,theportionoftheorganic 12 phase 500 Which is introduced into the second column, the vaporous overhead stream 210 from the second distillation column,the?rstdistillationcolumn650,thedecanter700,the upper section of the second distillation column 950, and combinations thereof. ShoWn in FIG. 1 is addition of the entrainerasstream120tothedecanter700.When thestream toWhichtheentrainerisintroducedisvaporous,theentrainer is preferably preheated and added as a vaporous stream. Additionoftheentrainertotheprocesscanbeperformedin a continuous manner or in a discontinuous manner, so long as the amount of entrainer in the ?rst mixed condensate, and/or in the combination of the ?rst mixed condensate stream and the second condensate stream, is suf?cient to provide phase separation of the organic and the aqueous phases under the operatingconditionsoftheprocess.An amountofentrainerin excessofthatrequiredforphaseseparationcanbeusedbutas this can lead to increased volumes of the process streams comprisingtheentrainer,increasedenergyconsumption,pro portionallylargerlossofentrainerfromtheprocess,and increased operating cost, the use of signi?cantly excess entrainerintheprocessistypicallynotdesirable.Useofabout theminimalamountofentrainerWhichissuf?cienttoprovide phase separation under the selected operating conditions is preferred.Typically,make-upentrainerisaddedtothepro cess to compensate for the entrainer losses Which can be incurred When vaporous streams exit the process. Thepresentprocessesforseparatingorrecoveringbutanol provide butanol knoWn to have an energy content similar to thatofgasolineandWhichcanbeblendedWithanyfossilfuel. Butanol is favored as a fuel or fuel additive as ityields only CO2 andlitleorno SOXorNOXWhen burnedinthestandard internalcombustionengine.Additionally,butanolislesscor rosive than ethanol, the most preferred fuel additive to date. In addition to its utility as a biofuel or fuel additive, the butanolrecoveredaccordingtothepresentprocesseshasthe potentialofimpactinghydrogendistributionproblemsinthe emergingfuelcellindustry.Fuelcellstodayareplaguedby safety concerns associated With hydrogen transport and dis tribution.Butanolcanbeeasilyreformedforitshydrogen contentandcanbedistributedthroughexistinggasstationsin the purity required for either fuel cells or vehicles. Further more, the present processes recover butanol obtained from plantderivedcarbonsources,avoidingthenegativeenviron mentalimpactassociatedWithstandardpetrochemicalpro cesses for butanol production. One advantage of the present processes for separation or recoveryofbutanolisthatbyreturningaportionoftheaque ousphasefromthedecantertothe?rstcolumn,thetempera tureinthe?rstcolumniskeptrelativelyloW,forexample beloW about 1400 C. under any conditions, and in the case of operation at atmospheric pressure, closer to 100° C. LoWer temperaturesavoidorreducefoulingoftheheatexchangers associated With the column, as can occur When the extractant inthebottomsstreamdegrades,forexamplethroughreac tionsWithorcatalyZedbyfermentationbyproductscontained inthe bottoms stream. LoWer column temperatures also make the recovery process more economical. An additionaladvantageisthatthe?rstbottomsstream comprisingtheextractantissubstantiallyfreeofthebutanol product,Whichcontributestohighyieldintherecoverypro cess.Beingsubstantiallyfreeofbutanolalsoenablesoptional recycling of the ?rst bottoms stream to the fermentative pro cess. It also simpli?es its disposition, should it not be recycled. Another advantage of the present invention is that it pro vides a more ef?cient process due to the increased relative US 8,563,788B2 60PDF Image | RECOVERY OF BUTANOL
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