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US 6,960,242B2 12 CO2 RECOVERY PROCESS FOR SUPERCRITICAL EXTRACTION CROSS-REFERENCE TO RELATED APPLICATIONS This application claims priority from Provisional Patent Application No. 60/415,655 ?led Oct. 2, 2002, Which is incorporated herein by reference. FIELD OF THE INVENTION The present invention relates to a process and apparatus for recovering carbon dioxide used for supercritical extrac tion in an industrial process, such as semiconductor Wafer cleaning. ?ltering the process vapor phase stream to remove par ticulatesandoptionallyresidualco-solvent; passing the ?ltered process vapor stream through an adsorber to remove trace impurities to form a puri?ed carbon dioxide vapor stream; and, drying the puri?ed carbon dioxide vapor stream to remove residual Water vapor. The process may further comprise optionally supplement ing the dried, puri?ed carbon dioxide vapor stream With a 10 distilled carbon dioxide vapor stream to form a feed carbon dioxidevaporstream;?lteringthefeedcarbondioxidevapor stream to remove condensable vapors and particulates; and cooling the ?ltered feed carbon dioxide stream to form an intermediate carbon dioxide liquid stream. 15 BACKGROUND Theprocessmay stilfurthercomprise?lteringtheinter mediate carbon dioxide liquid stream; and pressuriZing the intermediate carbon dioxide liquid stream. A supercritical ?uid may be formed from the pressuriZed carbon dioxide Supercritical mixtures of high purity CO2 and organic co-solvents, such as ethanol, are used in the production of semiconductorWafers.Thisincludespost-etchcleaning,20 liquidstreamanddeliveredtotheextractionprocedure. residue removal, and metal and dielectric deposition. For a commercial process, CO2 ?oWs are large and CO2 needs to be recycled after each Wafer production step. CO2 recycle for semiconductor requirements can only be done if the co-solvents and dissolved impurities can be substantially 25 removed from the recycle stream. For a large-scale chemical production system, the amounts of CO2/co-solvent Waste generated are signi?cant. To make the process more economical, CO2 can be recycled, as long as the co-solvent (and other impurities) can be 30 separated from the CO2. To accomplish this, the prior art discloses the use of distillation columns, Where the CO2 and the co-solvents are separated. This system Will Work as long as there are only tWo major components in the system, namely CO2 and the co-solvent. If trace amounts of other 35 components are present, this process has to be substantially altered With additional equipment, design changes and added expense. Stil,theseparationofallmeasurable traces is not alWays possible With knoWn systems. In one embodiment, Wherein the adsorber is a plurality of adsorber beds, the process may further comprise isolating at least one adsorber bed and ?ushing the isolated adsorber bed With vaporiZed refrigerant from at least one condenser. In another embodiment, a process for carbon dioxide supercritical extraction and recovery is provided compris ing: 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; ?ltering the intermediate carbon dioxide liquid stream; pressuriZing the intermediate carbon dioxide liquid stream; forming a supercritical ?uid from the pressuriZed carbon dioxide liquid stream and delivering the supercritical ?uid Previousprocessesforrecoveryofcarbondioxidefor40 andoptionallyaco-solventforasupercriticalextraction reuse in industrial processes such as semiconductor Wafer manufacturing require the use of accessory equipment such as boilers and condensers for distilling and condensing the solvent Waste stream, together With signi?cant energy requirements. US. Pat.No.4,349,415disclosesaprocessforseparating organic liquid solutes from their solvent mixtures, Wherein the extractant can be carbon dioxide used in the supercritical state. SUMMARY A carbon dioxide recovery process for supercritical extractionisprovidedcomprising: providingaprocessstreamfromasupercriticalextraction procedure Wherein the process stream includes pressuriZed 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; cooling the process stream to form a tWo phase mixture; separating the tWo phase mixture into a process liquid, containingco-solventifpresent,andaprocessvaporphase stream; 45 55 procedure; obtaining a process stream from the supercritical extrac tion procedure Wherein the process stream includes pressur iZed 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; cooling the process stream to form a tWo phase mixture; separating the tWo phase mixture into a process liquid, containing co-solvent ifpresent, and a process vapor phase stream; 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 collecting the process liquid; dioxide from a supercritical extraction process producing a carbon dioxide vapor stream; 60 dryingthepuri?edcarbondioxidevaporstreamtoremove residual Water vapor; and, optionallysupplementingthedried,puri?edcarbondiox ide vapor stream With additional distilled carbon dioxide 65 vapor. An apparatus is provided for the recovery of carbonPDF Image | CO2 RECOVERY PROCESS FOR SUPERCRITICAL EXTRACTION
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