(12)
UnitedStatesPatent
Wadaetai.
1111111111111111111111111111111111111111111111111111111111111111111
US006261748Bl
(10)
PatentNo.:
(45)
DateofPatent:
US6,261,748Bl
Jui.17,2001
(54)RECOVERINGMETHODOFSUPPORTANDUSEFULINGREDIENTFROMIMAGEFORMINGMATERIAL(75)Inventors:YasunoriWada;KiyoshiGoto,bothofHino
(lP)
(73)Assignee:KonicaCorporation
(lP)
(*)
Notice:Subjecttoanydisclaimer,thetermofthispatentisextendedoradjustedunder35U.S.c.154(b)by0days.(21)Appl.No.:09/585,017(22)(30)Filed:Jun.1,2000ForeignApplicationPriorityData
Jun.2,1999(JP)11-155279
(51)Int.CI?G03C5/395(52)U.S.CI.430/398;210/634(58)FieldofSearch430/398;210/634(56)ReferencesCitedU.S.PATENTDOCUMENTS
3,652,4663/1972Hitteletal.521/463,873,3143/1975Wooetal.75/7133,982,932
*
9/1976Korosi430/3985,288,728
*
2/1994Spearsetal.430/398
FOREIGNPATENTDOCUMENTS
193455244270971/1970(DE).2/1996(DE).
OTHERPUBLICATIONSEuropeanSearchReportEP00304666.
*
citedbyexaminer
PrimaryExaminer---Roa
Van
Le
(74)Attorney,Agent,orFirm-lordan
B.Bierman;Bierman,MuserlianandLucas(57)ABSTRACTAmethodforrecoveringaresinsupportfromanimageformingmaterialcomprisingaresinsupporthavingthereonanimageforminglayerisdisclosed,inwhichtheimageformingmaterialisimmersedintoadipolaraproticsolventoranalkalinealcoholandtheimageforminglayerisdissolvedwithstirringunderheat.9Claims,NoDrawings
US6,261,748B1
1
RECOVERINGMETHODOFSUPPORTANDUSEFULINGREDIENTFROMIMAGEFORMINGMATERIALFIELDOFTHEINVENTIONThepresentinventionrelatestoamethodforseparatinganimageforminglayerfromanimageformingmaterialandrecoveringaresinsupportorusefulingredientscontainedintheimageforminglayer.BACKGROUNDOFTHEINVENTIONAfteremployingasilverhalidelightsensitivephoto-graphicmaterialsasanimageformingmaterial,silvercoveragethereofhasbeenconductedinsuchawaythatthe
15
photographicmaterialisallowedtobedippedinanaqueousalkalisolutionandstirredwithheatingtoseparateconsti-tutionalmaterialsfromthephotographicmaterial,andtherebysilverisrecoveredfromtheconstitutionalcompo-nents.Recently,however,imageformingmaterialshave
20
undergonemanychangesandnewtypeofimageformingmaterialshavebeenintroduced,inwhichthecomponentsarenoteasilyremovable,suchas"DryView"availablefromImationCorp.,"DryStar"3000availablefromAgfa-GavaertAGor"Helios"availablefromSterlingCorp.
25
Inconventionalsilverhalidephotographicmaterials,gelatinhasmainlybeenemployedasbinder,whichisreadilysolubleinanaqueousalkalisolution.However,thebinder(s)usedinsuchnewproductsasdescribedabove,whicharenotmainlycomposedofgelatin,cannotbedissolvedbycon-
30
ventionalmeans.Asanothermeansforrecoveringsilverfromausedsilverhalidephotographicmaterialisknownamethodinwhichthephotographicmaterialissubjectedtocombustionandsilverisrecoveredfromtheresidue.However,thismethod,inwhichthesupportisalsoburned,
35
isnotdesirableintermsofrecentenvironmentalprotectionmeasures.Inviewoftheforegoingstatus,thereisdesiredamethodforrecoveringthesupportorotherusefulconstituentmate-rialfromnewimageformingmaterialssubstitutablefor
40
conventionalsilverhalidephotographicmaterialsandamethodofreusethereof.Whenimageformingmaterialsaretreatedinasolventtodissolveatleastapartofthesolidconstituentmaterialsonthesupporttoseparateitfromthesupport,consumptionof
45
thelargeamountofrequiredsolventisnotpreferredintermsoftheenvironmentandcost.Further,minimalsolventorwaterispreferredinrecoveryofusefulingredientsfromthesolution.Asameanstherefor,itispreferredtorecoverthesolventbydistillationandtocondensetheimageforming
50
components.However,increasingtheconcentrationrateresultsinanincreaseinviscosity,makingitshandlingmoredifficult.SUMMARYOFTHEINVENTION
It
isanobjectofthepresentinventiontoprovideamethodforefficientlyrecoveringusefulmaterialssuchasaresinsupportorotherusefulingredientsintheimageforminglayerofnewtypeimageformingmaterialshavingalayer
60
insolubleinanaqueousalkali.Theaboveobjectoftheinventioncanbeaccomplishedbythefollowingconstitution:1.Amethodforrecoveringaresinsupportfromanimageformingmaterialcomprisingaresinsupporthaving
65
thereonanimageforminglayer,themethodcomprisingthestepsof:
2
5
(a)immersingtheimageformingmaterialintoadipolaraproticsolventoranalkalinealcohol,and(b)dissolvingtheimageforminglayerwithstirringunderheattoformanimageforminglayersolution;2.Themethoddescribedin1.above,whereinthedipolaraproticsolventisselectedfromthegroupconsistingofdimethylsulfoxide,dimethylformamideanddimethylacetoamide;3.Themethoddescribedin2.,whereinthemethodfurthercomprises:(c)separatingtheimageforminglayersolutionfromtheresinsupport,and(d)recoveringthedipolaraproticsolventoralkalinealcoholfromtheimageforminglayersolution;4.Themethoddescribedin1.,whereintheresinsupportispolyethyleneterephthalateorcellulosetriacetate.5.Themethoddescribedin1.,whereininstep(b),ultrasonicisemployedtopromotedissolution;6.Themethoddescribedin1.,whereininstep(a),aftertheimageformingmaterialiscuttoasizeof0.1cmxO.1emto10cmx10ern,theimageformingmate-rialimmersedintothedipolaraproticsolventoralka-linealcohol;7.Themethoddescribedin3.,whereininstep(c),afterseparatingtheimageforminglayersolutionfromtheresinsupport,theresinsupportiswashedwithwatertorecoverthesupport;8.Themethoddescribedinanyof1.through7.,whereintheresinsupportwhichhasbeenrecoveredfromtheimageformingmaterialaccordingtothemethodasdescribedinanyof1.through7.isreusedasasupportofanimageformingmaterial;9.Themethoddescribedin1.,whereinthemethodfurthercomprises:(e)recoveringausefulingredientfromtheimageforminglayersolution;10.Themethoddescribed
III
9.,whereintheusefulingredientissilver;11.Themethoddescribedin9.,whereininstep(e),theimageforminglayersolutionissubjectedtocombus-tiontorecovertheusefulingredient;12.Themethoddescribedin1.,whereinthemethodfurthercomprises:(c1)separatingtheimageforminglayersolutionfromtheresinsupport,and(e1)addingaprecipitatingagenttotheimageforminglayersolutiontorecoverausefulingredientthere-from;13.Amethodforrecoveringaresinsupportfromanimageformingmaterialcomprisingaresinsupporthavingthereonasparinglywater-solublelayer,whereintheimageformingmaterialfurthercomprisesawater-solublelayer,whichisprovidedbetweentheresinsupportandthesparinglywater-solublelayer;14.Themethoddescribedin13.,whereinthewater-solublelayerisadjacenttotheresinsupport;15.Themethoddescribedin13.,whereinalayercon-tainingausefulingredientisprovidedbetweentheresinsupportandthesparinglywater-solublelayer;thewater-solublelayerbeingthelayercontainingausefulingredient,orbeingalayerprovidedbetweentheresinsupportandthelayercontainingausefulingredient;16.Themethoddescribedin15.,whereinthemethodcomprising:
10
55
3
US
6,261,748
B1
4
(a)immersingtheimageformingmaterialintowater,(b)dissolvingthewater-solublelayertoformawater-solublelayersolution,(c)separatingalayerincludingtheresinsupportfromamixtureincludingthesparinglywater-solublelayer
5
andthewater-solublelayersolution,and(d)recoveringausefulingredientfromthemixtureincludingthesparinglywater-solublelayerandthewater-solublelayersolution;17.Amethodforrecoveringaresinsupportfromanimageformingmaterialcomprisingaresinsupporthavingthereonasparinglywater-solublelayer,whereintheimageformingmaterialfurthercomprisesalayer(II),whichissolubleinanaqueousalkalinesolutionoranaqueousacidsolutionandprovidedbetweentheresinsupportandthesparinglywater-solublelayer;18.Themethoddescribedin17.,whereinthelayer(II)isadjacenttotheresinsupport;19.Themethoddescribedin17.,whereinalayercon-tainingausefulingredientisprovidedbetweentheresinsupportandthesparinglywater-solublelayer,thelayer(II)beingthelayercontainingausefulingredientorbeingalayerprovidedbetweentheresinsupportandthelayercontainingausefulingredient;and20.Themethoddescribedin19.,whereinthemethodcomprising:(a)immersingtheimageformingmaterialintoanaqueousalkalinesolutionoranaqueousacidsolution,
30
(b)dissolvingthelayer(II)toformanaqueouslayer(II)solution,(c)separatingalayerincludingtheresinsupportfromamixtureincludingthesparinglywater-solublelayerandthelayer(II)solution,and
35
(d)recoveringausefulingredientfromthemixturecomprisingthesparinglywater-solublelayerandthelayer(II)solution.DETAILEDDESCRIPTIONOFIREINVENTIONAsaresultoftheinventor'sexplorationofmethodsforrecoveringusefulingredientscontainedinnewtypesofimageformingmaterials,itwasfoundthattheuseofhydrophilicorganicsolvents,i.e.,adipolaraproticsolvent,specificallysuchasdimethylsulfoxide,dimethylformamideordimethylacetoamide,ortheuseoflow-pricedalkalinealcoholswasadvantageous,therebyenablingrecoveryorreuseofusefulingredientsfromimageformingmaterialswhicharenotmainlycomposedofgelatin,suchas"DryView"availablefromImationCorp.,"DryStar"3000avail-ablefromAgfa-GavaertAGor"Helios"availablefromSterlingCorp.Herein,thedipolaraproticsolventreferstoapolarsolventcomprisedofpolarmoleculesandhavingnoprotichydro-
55
gen.Thepresentinventioncanbeappliednotonlytoaspecifictypeofimageformingmaterialsbutalsotoanyonewhichcontainsausefulingredientinanimageformingmaterialorhasareusablesupport.Animageformingmaterialusableintheinventioncomprisesaresinsupporthavingthereonatleastoneimageforminglayer.Exemplaryexamplesthereofincludeimageformingmaterials,whichcomprisearesinsupportsuchaspolyethyleneterephthalate,polyethylenenaphthalate,cellulosetriacetateorsyndiotacticpolystyrene,providedonthesupportwithaphotothermographicrecord-inglayer(suchas"DrySilver"),athermalrecordinglayerorathermaltransferlayer.Abinderusedintheselayersisnotgelatinbutisoftenawater-insolublebinder,suchaspolyvinylbutyral,celluloseacetatetypepolymers,orpoly-vinylalcohol.Suchimageformingmaterialsinclude,forexample,DrySilver-typephotothermographicmaterials,ink-jetsystemimagereceivingmaterials,ablation-typeimageformingmaterials,thermalrecordingmaterialsandthermaltransfermaterials.Specifically,DrySilver-typematerials,whichcontainsilvercomponentsareimportantin
10
termsofrecoveryofnaturalresources.Theimageformingmaterialusedintheinventionmaybetreatedassuchbutcomponentlayerssometimesarenotsufficientlydissolvedoutduetooverlappingofimageform-ingmaterials.Suchcasesarenotpreferred,oftenleadingto
15
loweringtherecoveryefficiencyofusefulingredientsordeterioratedqualityofasupport.Installationofabaffleplateinadissolvingtank,selectionofstirringbladesorspeed-upofstirringcanresultinimprovementstosomeextentbutisusuallynotsufficient.
It
wasprovedthatdissolutionofthe
20
imageforminglayerofanimageformingmaterialwasmarkedlyimprovedbycuttingtheimageformingmaterialtoagivensmallsize.Thus,itispreferredtocutitfromasizeof0.1cmxO.1emto10cmxlOern,morepreferably0.1cmxO.1emto2cmx2ern,andstillmorepreferably0.1
25
cmxO.1to1cmx1ern.Furthertheuseofultrasonicagitationenablesnotonlycompletedissolving-outbutalsoshortensthetimefortheprocess.Incaseswhenusingadipolaraproticsolventsuchasdimethylsulfoxide,dimethylformamideordimethylacetoamide,thedissolvingtemperatureis20to180
0
c.,
preferably40to150
0
c.,
andmorepreferably60to120
0
C.Theboilingpointofdimethylsulfoxide,dimethylforma-mideanddimethylacetoamideis179
0
c.,
153
0
C.and165
0
c.,
respectively,sothatrefluxextraction(orSoxhletextraction)ispreferablyemployed.Further,asameansforenhancingtheextractionefficiencyortheextractionrateispreferablyemployedultrasonic.Afterdissolvingwithdimethylsulfoxide,dimethylformamide,dimethylacetoamideoralkalinealcoholto
40
removetheimageforminglayer,itispreferredtowashtheresinsupportwithwater.Theuseofthewater-solublesolventsdescribedabovecausesnoseparationofwaterandthesolvent,makingwashingeasier.Theuseofwatersome-timescausesprecipitationofasparinglywater-soluble
45
ingredientfromthesolutionattachedtothesupport.Insuchacase,afterseparatingtheprecipitate,thesupportisagainwashedwithasolvent,therebyleadingtomarkedenhance-mentinwashingefficiency,ascomparedtothecasewithoutwashingwithwater.Therecoveredsupportissuperiorin
50
purity,causingnodeteriorationintransparency,ascomparedtotheuseofothersolvents.Althoughthedipolaraproticsolventssuchasdimethylsulfoxide,dimethylformamideordimethylacetoamidewasprovedtobesuperiorinseparationofanimageforminglayerfromanimageformingmaterialcomparedtocom-monlyusedsolvents,suchadipolaraproticsolventisrelativelyhigh-priced.
It
wasfurtherfoundthattheuseofanalcoholaddedwithanalkaliexhibitedsuperiorseparationefficiency.Alkalinealcoholisanalcoholinwhichanalkali
60
suchascausticpotash(orpotassiumhydroxide),causticsoda(orsodiumhydroxide),sodiummethoxideorsodiumethoxideisdissolvedpreferablyinanamountof1to30%,andmorepreferably20to30%,andwhichmaycontainasmallamountofwater.Examplesoftheusablealcohol
65
includeloweralcoholssuchasmethanol,ethanolandiso-propanol.Thealkalinealcoholscanbeemployedasasolventinamannersimilartotheaproticsolventssuchas
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