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US 6,960,242B2 78 refrigerant from a condenser, such as nitrogen or another disposable refrigerant, can be used as a purge for regenera tion of the dirty adsorption bed at loW pressures. The purged impurities from the adsorption bed, such as the co-solvent, can be recovered separately, ifdesired. The puri?ed CO2 stream 90 is dried to remove residual Water vapor, such as by being passed through a tWo bed desiccant dryer 95. The puri?ed stream can supplement or replace the ?rst stage purity CO2 stream 11 from the bulk supplybytheactionofvalves92and12.Thepuri?edCO2 vapor passes through ?lters 13 and 14 as described above, and is cooled in the condenser 18 to a temperature such that the CO2 is entirely condensed and returned to the loW pressure accumulation vessel 30. EXAMPLE A semiconductorWaferisprocessedusingamixtureof supercritical CO2 and 10% organic co-solvent. Residue removed from the Wafer precipitates out as the pressure of the gas isreduced from about 300 bar (30 MPa) to about 25 to about 30 bar (2.5 to 3 MPa). The temperature of the gas atthisstage isbetWeen about 30° to about 60° C. This CO2 gas(containing5% byWeightorganicco-solvent)iscooled to temperatures betWeen about —10° C. and —5° C. A vapor-liquid phase system is formed Where a majority of the organic co-solvents and other impurities are present in the liquidphase.Thevaporphasecontainsabout300—1000ppm oforganicco-solventmaterial.Theliquidphaseisseparated by gravity in a settling chamber, and the vapor phase is transported to an adsorbent bed containing an organic polar 30 separating the tWo phase mixture into a process liquid, containing co-solvent ifpresent, and a process vapor phasestream; collectingtheprocessliquid; ?ltering the process vapor phase stream to remove par ticulates and optionally residual co-solvent; passing the ?ltered process vapor stream through an adsorber to remove trace impurities to form a puri?ed molecule-selective adsorbent. Activated alumina is suitable forthisseparation. Additional adsorbents, such as activated carbons and molecular sieves, may also be present to adsorb any other trace organic impurities. The clean CO2, recovered at about 20barpressure(2MPa) isthencooledtoabout—20° C.and lique?ed. The lique?ed CO2 product is returned to the CO2 accumulator tank. About 90% of the CO2 is recovered by this process. The additional 10% requirement can be obtained from the bulk CO2 supply as described above. 35 carbon dioxide vapor stream; and, dryingthepuri?edcarbondioxidevaporstreamtoremove residual Water vapor. 2. The process of claim 1 further comprising: optionallysupplementingthedried,puri?edcarbondiox 40 ide vapor stream With a distilled carbon dioxide vapor stream to form a feed carbon dioxide vapor stream; ?ltering the feed carbon dioxide vapor stream to remove condensable vapors and particulates; and, cooling the ?ltered feed carbon dioxide stream to form an intermediate carbon dioxide liquid stream. 3. The process of claim 2 further comprising: ?ltering the intermediate carbon dioxide liquid stream; and pressuriZing the intermediate carbon dioxide liquid stream. 4. The process of claim 3 further comprising forming a supercritical?uidfromthepressuriZedcarbondioxideliquid streamanddeliveringthesupercritical?uidtotheextraction 55 procedure. 5. The process of claim 1 Wherein the adsorber is a The present apparatus and process are advantageous over prior systems because they provide for the removal of trace contaminants Without a major change in operation procedure,bychangingadsorbentsascomparedtorequiring distillation of CO2/so-solvent (such as ethanol) mixtures. 45 The provide for cyclic operation, i.e., they do not require continuous feed for operation. Further, they provide a more economical design and operation, due to the absence of unnecessary accessory equipment such as boilers and con densers. The entire process may be controlled by a programmable controller, and records data from the process can be sent to a computer Which can be used to retrieve the data remotely. The apparatus and process may include a fully automated microprocessorcontrollerWhichcontinuouslymonitorssys temoperationprovidingfaultdetection,pressurecontroland valve sequencing, ensuring puri?er reliability, While mini miZing operator involvement. plurality of adsorber beds, further comprising isolating at least one adsorber bed and ?ushing the isolated adsorber bed With vaporiZed refrigerant from at least one condenser. 6.A processforcarbondioxidesupercriticalextraction and recovery comprising: distilling a feed stream comprising carbon dioxide vapor off of a liquid carbon dioxide supply; ?ltering the feed carbon dioxide vapor stream to remove condensable vapors and particulates; cooling the ?ltered feed carbon dioxide stream to form an intermediate carbon dioxide liquid stream; By Way of example and not limitation, level sensor 53, pressure sensor 54, and temperature sensors can provide 60 information for the controller, in order to provide instruc tions to How control valves 12, 24, 25, 34, and 92, or safety relief valves 55 and 56. Isolation bypass valves 69 and 76 may be controlled automatically or manually. The valves in the apparatus may be actuated pneumatically, by pulling a 65 tap off of the CO2 vapor conduit such as at valve 93, to supply gas for valve actuation. The apparatus may include system alarms to detect poten tial haZards, such as temperature or pressure excursions, to ensure system integrity.Alarm and Warning conditions may be indicated at the operator interface and may be accompa nied by an alarm beeper. It Will be understood that the embodiment(s) described herein is/are merely exemplary and that a person skilled in the artmay make many variations and modi?cations Without departingfromthespiritandscopeoftheinvention.Allsuch 10 modi?cations and variations are intended to be included Within the scope of the invention as described herein. It should be understood that any embodiments described above are not only in the alternative, but can be combined. We claim: 15 1. A carbon dioxide recovery process for supercritical extractioncomprising: providing a process stream from a supercritical extraction procedure Wherein the process stream includes pres suriZed carbon dioxide, extraction process Waste and optionally at least one co-solvent; reducing the pressure of the process stream beloW critical pressure; venting loW pressure carbon dioxide vapor to exhaust; 25 cooling the process stream to form a tWo phase mixture;PDF Image | CO2 RECOVERY PROCESS FOR SUPERCRITICAL EXTRACTION
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