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5,412,958 34 cleaning ?uid is shown schematically in FIG. 1. The 20° C. and 100° C. or from about 3500 psi to about 5000 systemgenerallycomprisesthreevessels,thecleaning psiattemperaturesbetweenabout20°C.and37°C. vessel10,preferablyarotatabledrum,thegasvaporizer vessel 11, and the storage vessel 12, all of which are interconnected. The cleaning vessel, where soiled sub strates (e.g. clothing) are received and placed into contactwiththecleaning?uidisalsoreferredtoasan autoclave. As will be described further below, much of the CO2 cleaning ?uid isrecycled in this system. Where fabricsarebeingcleaned,onepreferablyworks within a temperature range between about 20° C. to about 100° C. In addition, ithas been found within this rangethatprocesseswhichraisethetemperatureprior to decompression reduce the damage to polymeric parts. Suitable compounds as the ?rst fluid are either liquid or are ina supercritical statewithin the temperature and pressure hatched area illustrated by FIG. 3. The partic ularlypreferred?rst?uidinpracticingthisinventionis CO2 isoftenstoredand/ortransportedinrefrigerated tanks at approximately 300 psi and — 18° C. In charging theinventivesystemwithCO2, pump 21isadaptedto drawlowpressureliquidCO2throughline92thatis carbondioxideduetoitsreadyavailabilityandenviron connected to a refrigerated tank (not shown) through mental safety. The critical temperature of carbon diox make-upheater42whichraisesthetemperatureofthe 5 ideis31°C.andthedense(orcompressed)gasphase C02. The heater preferably has ?nned coils through which ambient air ?ows and employs resistive electric heating.Pump 21isadirectdrive,single-pistonpump. Liquid CO2 is then stored in the storage vessel 12 at approximately915psiand25°C.Thestoragevesselis20 employedasthe?rst?uidbythemselvesorinmixture. preferablymade ofstainlesssteel.As shown inFIG. 1, conventional temperature gauges (each depicted as an encircled “T”), pressure gauges (each depicted as an encircled“P”),liquidCO2levelmeters(eachdepicted nol,benzene,toluene,p-xylene,chlorotri?uorometh as an encircled “L”), and a ?owmeter (depicted as an 25 ane, trichloro?uoromethane, per?uoropropane, chlo encircled“F”)areemployedinthesystem.Inaddition, conventional valves are used. In operation, after placing soiled substrate into the cleaningvessel,thecleaningvesselisthenchargedwith gaseousCO2(fromthestoragevessel)toanintermedi 30 sourceofhydrogenperoxideandanorganicbleach 'ate pressure of approximately 200-300 psi to prevent activatortherefor,asisdescribedincopendingapplica extreme thermal shock to the chamber. The gaseous tion Ser. No. 754,809, ?led Sep. 4, 1991, inventors CO2istransferredintothecleaningvesselthroughlines Mitchelletal.,ofcommonassignmentherewith.For 82 and 84. Thereafter, liquid CO2 ispumped into the example, the source of hydrogen peroxide can be se cleaningvesselfromthestoragevesselthroughlines80, lectedfromhydrogenperoxideoraninorganicperox 91, 81, and 82 by pump 20 which preferably has dual pistons with either direct or hydraulic/electric drive. The pump raises the pressure of the liquid CO; to ap proximately 900 to 1500 psi. Subcooler 30 lowers the temperatureoftheCO2by2°to3°belowtheboiling40 particularlymineraloilorpetrolatum),asdescribedin point to prevent pump cavitation. The temperature of the CO2 can be adjusted by heating/cooling coils 95 locatedinsidethecleaningvessel.Beforeorduringthe cleaningcycle,cleaningadditivesmaybeaddedintothe cleaningvesselbypump23throughlines82and83.45 tion,fabricsareinitiallypretreatedbeforebeingcon Moreover, pump 23 through lines82 and 83 can alsobe used to deliver a compressed gas into the cleaning ves sel as described below. tacted with the ?rst ?uid. Pretreatment may be per formed at about ambient pressure and temperature, or at elevated temperature. For example, pretreatment can include contacting a fabric to be cleaned with one or Practice of the invention requires contact of a sub strate having a contaminant with the ?rst, substantially 50 more of water, a surfactant, an organic solvent, and non-polar ?uid that is in a liquid or in a supercritical state. With reference to FIG. 3, when using CO2 as the ?rst ?uid, its temperature can range broadly from slightly below about 20° C. to slightly above about 100° C.asindicatedonthehorizontalaxisandthepressure55 actuallybeimpeded. can range from about 1000 psi to about 5000 psi as shown on the vertical axis. However, within this broad range of temperature and pressure, it has been discov ered that there is a zone (represented by the hatched area of the left, or on the convex side, of the curve) 60 then a step after the ?rst ?uid cleaning is preferable where surface blistering to components such as buttons can be reduced, whereas practice outside of the zone tends to lead to button damage that can be quite severe. As is seen by the hatched region of FIG. 3, preferred conditions are between about 900 psi to 2000 psi at 65 involved an extraction type of process where clean, temperaturesbetweenabout20°C.toabout45°C.,with more preferred conditions being pressure from about 900 psi to about 1500 psi at temperatures between about dense gas ispumped into a chamber containing the substrate while “dirty” dense gas is drained. This type of continuous extraction restricts the ability to quickly above the critical temperature and near (or above) the critical pressure is often referred to as a “supercritical fluid.”Otherdensi?edgasesknownfortheirsupercriti cal properties, as well as carbon dioxide, may also be Thesegasesincludemethane,ethane,propane,ammoni um-butane, n-pentane, n-hexane, cyclohexane, n-hep tane,ethylene,propylene,methanol,ethanol,isopropa rodifluoromethane, sulfur hexa?uoride, and nitrous oxide. Although the ?rst ?uid itself is substantially non polar, it may include other components, such as a ide and the organic bleach activator can be a carbonyl ester such as alkanoyloxybenzene. Further, the ?rst ?uid may include a cleaning adjunct such as another liquid (e.g., alkanes, alcohols, aldehydes, and the like, Ser. No. 715,299, ?led Jun. 14, 1991, now US. Pat. No. 5,279,6l5, inventor Mitchell et al., of common assign ment herewith. Inapreferredmode ofpracticingthepresentinven other active cleaning materials such as enzymes. Sur prisingly, ifthese pretreating components are added to the bulk solution of densi?ed carbon dioxide (rather than as a pretreatment), the stain removal process can Since water is not very soluble in carbon dioxide, it can adhere to the substrate being cleaned in a dense carbon dioxide atmosphere, and impede the cleaning process. Thus, when a pretreating step includes water, where the cleaning ?uid is contacted with a hygro scopic ?uid, such as glycerol, to eliminate water other wise absorbed onto fabric. Prior art cleaning with carbon dioxide has typicallyPDF Image | LIQUID SUPERCRITICAL CARBON DIOXIDE DRY CLEANING SYSTEM
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