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Ukwandiswa kwe-shale kwiindawo zokugcina amanzi ezidala iingxaki ezinkulu, nto leyo ekhokelela ekungazinzini kwe-wellbore. Ngenxa yezizathu zokusingqongileyo, ukusetyenziswa kolwelo lokumba olusekelwe emanzini olune-shale inhibitors eyongezelelweyo kukhethwa kune-oyile-based drilling fluid. Ii-Ionic liquids (ILs) zitsale ingqalelo enkulu njenge-shale inhibitors ngenxa yeempawu zazo eziguquguqukayo kunye neempawu ezinamandla ze-electrostatic. Nangona kunjalo, ii-ionic liquids (ILs) ezisekelwe kwi-imidazolyl, ezisetyenziswa kakhulu kwi-drilling fluids, ziye zabonakala zinobuthi, aziboli kwaye zibiza kakhulu. Ii-Deep eutectic solvents (DES) zithathwa njengenye indlela engabizi kakhulu kwaye engenabuthi kakhulu kunee-ionic liquids, kodwa zisasilela ekuzinzeni kwendalo okufunekayo. Inkqubela phambili yakutshanje kweli candelo ikhokelele ekungenisweni kwe-deep eutectic solvents yendalo (NADES), eyaziwa ngokuba nobuhlobo bokwenyani nokusingqongileyo. Olu phononongo luphande ii-NADES, eziqulethe i-citric acid (njenge-hydrogen bond acceptor) kunye ne-glycerol (njengomnikeli we-hydrogen bond) njengezongezo zolwelo lokumba. Ulwelo lokugrumba olusekelwe kwi-NADES lwenziwe ngokuhambelana ne-API 13B-1 kwaye ukusebenza kwalo kuthelekiswa nolwelo lokugrumba olusekelwe kwi-potassium chloride, ulwelo lwe-ionic olusekelwe kwi-imidazolium, kunye nolwelo lokugrumba olusekelwe kwi-choline chloride:urea-DES. Iipropati ze-physicochemical ze-NADES ezizimeleyo zichazwe ngokweenkcukacha. Iipropati ze-rheological, ukulahleka kolwelo, kunye neepropati zokuthintela i-shale yolwelo lokugrumba zivavanyiwe ngexesha lophando, kwaye kwaboniswa ukuba kwi-concentration ye-3% NADESs, umlinganiselo woxinzelelo lwe-yield/plastic viscosity (YP/PV) wonyusiwe, ubukhulu be-mud cake buncitshisiwe ngama-26%, kwaye umthamo we-filtrate wehlisiwe ngama-30.1%. Okuphawulekayo kukuba, i-NADES ifumene izinga lokuthintela ukwanda elimangalisayo lama-49.14% kwaye yandisa imveliso ye-shale ngama-86.36%. Ezi ziphumo zibangelwa kubuchule be-NADES bokutshintsha umsebenzi womphezulu, amandla e-zeta, kunye nomgama phakathi kwe-clays, ezixoxwa kweli phepha ukuqonda iindlela ezisisiseko. Olu lwelo lokugrumba oluzinzileyo kulindeleke ukuba lutshintshe ishishini lokugrumba ngokubonelela ngenye indlela engenabungozi, engabizi kakhulu, nesebenza kakhulu endaweni yezithinteli zokugrumba ze-shale zemveli, nto leyo evula indlela yeendlela zokugrumba ezinobuhlobo nokusingqongileyo.
I-Shale lilitye elinokuguquguquka elisebenza njengomthombo kunye nomthombo wee-hydrocarbons, kwaye ulwakhiwo lwayo olunemingxuma1 lubonelela ngamathuba okuvelisa kunye nokugcina ezi zixhobo zixabisekileyo. Nangona kunjalo, i-shale ityebile kwiiminerali zodongwe ezifana ne-montmorillonite, i-smectite, i-kaolinite kunye ne-illite, ezenza ukuba idumbe xa ivezwa emanzini, nto leyo ekhokelela ekungazinzini kwe-wellbore ngexesha lemisebenzi yokugrumba2,3. Ezi ngxaki zinokukhokelela kwixesha elingasebenziyo (i-NPT) kunye neengxaki ezininzi zokusebenza kubandakanya imibhobho ebambekileyo, ukulahleka kokujikeleza kodaka, ukudilika kwe-wellbore kunye nokungcola kweebhithi, okwandisa ixesha lokubuyisela kunye neendleko. Ngokwesiko, ii-oil-based drilling fluids (OBDF) bezilukhetho olukhethwayo kwi-shale formations ngenxa yokukwazi kwazo ukumelana nokwanda kwe-shale4. Nangona kunjalo, ukusetyenziswa kwee-oil-based drilling fluids kubandakanya iindleko eziphezulu kunye nemingcipheko yokusingqongileyo. Ii-synthetic-based drilling fluids (SBDF) ziye zathathwa njengenye indlela, kodwa ukufaneleka kwazo kumaqondo obushushu aphezulu akwanelisi. Ulwelo lokubhola olusekelwe emanzini (i-WBDF) lusisombululo esinomtsalane kuba lukhuselekile, lunobuhlobo nokusingqongileyo, kwaye lunexabiso eliphantsi kune-OBDF5. Ii-shale inhibitors ezahlukeneyo zisetyenzisiwe ukuphucula amandla okuthintela i-shale ye-WBDF, kubandakanya ii-inhibitors zendabuko ezifana ne-potassium chloride, ilayimu, i-silicate, kunye ne-polymer. Nangona kunjalo, ezi zithinteli zinemida malunga nokusebenza kakuhle kunye nempembelelo yokusingqongileyo, ngakumbi ngenxa yoxinzelelo oluphezulu lwe-K+ kwii-inhibitors ze-potassium chloride kunye novakalelo lwe-pH lwee-silicates. 6 Abaphandi bahlolisise amathuba okusebenzisa ii-ionic liquids njengezongezo zolwelo lokubhola ukuphucula i-rheology yolwelo lokubhola kunye nokuthintela ukudumba kwe-shale kunye nokwakheka kwe-hydrate. Nangona kunjalo, ezi zi-ionic liquids, ngakumbi ezo ziqulethe ii-imidazolyl cations, ngokubanzi ziyingozi, zibiza kakhulu, aziboli, kwaye zifuna iinkqubo zokulungiselela ezinzima. Ukusombulula ezi ngxaki, abantu baqala ukukhangela enye indlela engabizi kakhulu nenobuhlobo nokusingqongileyo, eyakhokelela ekuveleni kwe-deep eutectic solvents (DES). I-DES ngumxube we-eutectic owenziwe ngumnikeli we-hydrogen bond (HBD) kunye ne-hydrogen bond acceptor (HBA) kwi-molar ratio kunye nobushushu obuthile. Le mixube ye-eutectic ineendawo zokunyibilika eziphantsi kunezakhi zayo, ngokuyintloko ngenxa yokudilika kwetshaja okubangelwa ziibhondi ze-hydrogen. Izinto ezininzi, kubandakanya amandla e-lattice, utshintsho lwe-entropy, kunye nokusebenzisana phakathi kwee-anions kunye ne-HBD, zidlala indima ephambili ekunciphiseni i-melting point ye-DES.
Kwizifundo zangaphambili, izongezo ezahlukeneyo zongezwa kulwelo lokubhola olusekelwe emanzini ukusombulula ingxaki yokwandiswa kweshale. Umzekelo, u-Ofei nabanye bongeze i-1-butyl-3-methylimidazolium chloride (BMIM-Cl), eyanciphisa kakhulu ubukhulu bekhekhe lodaka (ukuya kuthi ga kwi-50%) kwaye yehlisa ixabiso le-YP/PV nge-11 kumaqondo obushushu ahlukeneyo. U-Huang nabanye basebenzise ulwelo lwe-ionic (ngokukodwa, i-1-hexyl-3-methylimidazolium bromide kunye ne-1,2-bis(3-hexylimidazol-1-yl)ethane bromide) ngokudibeneyo namaqhekeza e-Na-Bt kwaye yanciphisa kakhulu ukudumba kweshale nge-86.43% kunye ne-94.17%, ngokulandelelana12. Ukongeza, uYang nabanye. basebenzise i-1-vinyl-3-dodecylimidazolium bromide kunye ne-1-vinyl-3-tetradecylimidazolium bromide ukunciphisa ukudumba kwe-shale nge-16.91% kunye ne-5.81%, ngokulandelelana. 13 UYang nabanye basebenzise ne-1-vinyl-3-ethylimidazolium bromide kwaye banciphisa ukwanda kwe-shale nge-31.62% ngelixa begcina ukubuyiselwa kwe-shale kwi-40.60%. 14 Ukongeza, uLuo nabanye basebenzise i-1-octyl-3-methylimidazolium tetrafluoroborate ukunciphisa ukudumba kwe-shale nge-80%. 15, 16 UDai nabanye basebenzise ii-ionic liquid copolymers ukuthintela i-shale kwaye bafumana ukunyuka kwe-18% ekubuyiseleni okuthe ngqo xa kuthelekiswa ne-amine inhibitors. 17
Ii-ionic liquids ngokwazo zineengxaki ezithile, nto leyo eyabangela ukuba izazinzulu zifune ezinye iindlela ezinobuhlobo nokusingqongileyo endaweni yee-ionic liquids, kwaye ngaloo ndlela kwazalwa i-DES. UHanjia wayengowokuqala ukusebenzisa i-deep eutectic solvents (DES) equka i-vinyl chloride propionic acid (1:1), i-vinyl chloride 3-phenylpropionic acid (1:2), kunye ne-3-mercaptopropionic acid + itaconic acid + vinyl chloride (1:1:2), eyathintela ukudumba kwe-bentonite ngama-68%, 58%, kunye nama-58%, ngokulandelelana. Kwisilingo sasimahla, uMH Rasul wasebenzisa umlinganiselo we-2:1 we-glycerol kunye ne-potassium carbonate (DES) kwaye wanciphisa kakhulu ukudumba kweesampuli ze-shale ngama-87%19,20. UMa wasebenzisa i-urea:vinyl chloride ukunciphisa kakhulu ukwanda kwe-shale ngama-67%.21 URasul et al. Udibaniso lwe-DES kunye ne-polymer lwasetyenziswa njenge-dual-action shale inhibitor, eyafumana isiphumo esihle kakhulu sokuthintela i-shale22.
Nangona i-deep eutectic solvents (DES) ngokubanzi ithathwa njengenye indlela eluhlaza kune-ionic liquids, ikwaqulathe izinto ezinokuba yityhefu ezifana ne-ammonium salts, nto leyo eyenza ukuba i-eco-friendly yazo ithandabuzeke. Le ngxaki ikhokelele ekuphuhlisweni kwe-natural deep eutectic solvents (NADES). Zisahlulwa njenge-DES, kodwa zenziwe ngezinto zendalo kunye neetyuwa, kubandakanya i-potassium chloride (KCl), i-calcium chloride (CaCl2), i-Epsom salts (MgSO4.7H2O), kunye nezinye. Iintlanganisela ezininzi ezinokubakho ze-DES kunye ne-NADES zivula umda obanzi wophando kule ndawo kwaye kulindeleke ukuba zifumane izicelo kwiindawo ezahlukeneyo. Abaphandi abaninzi baye baphuhlisa ngempumelelo iindibaniselwano ezintsha ze-DES eziye zabonakala zisebenza kwiindlela ezahlukeneyo zokusebenza. Umzekelo, uNaser et al. 2013 wenza i-potassium carbonate-based DES kwaye wafunda iipropati zayo ze-thermophysical, ezathi kamva zafumana izicelo kwiindawo zokuthintela i-hydrate, izongezo zolwelo lokubhola, i-deignification, kunye ne-nanofibrillation. 23 UJordy Kim kunye nabanye abasebenzi baphuhlise i-NADES esekelwe kwi-ascorbic acid baza bavavanya iipropati zayo ze-antioxidant kwizicelo ezahlukeneyo. 24 UChrister nabanye baphuhlise i-NADES esekelwe kwi-citric acid baza bafumanisa amandla ayo njengomncedi weemveliso ze-collagen. 25 ULiu Yi kunye nabanye abasebenzi bashwankathele ukusetyenziswa kwe-NADES njenge-excipient kunye ne-chromatography media kuphononongo olupheleleyo, ngelixa uMisan nabanye baxoxe ngokusetyenziswa ngempumelelo kwe-NADES kwicandelo lokutya kwezolimo. Kubalulekile ukuba abaphandi bolwelo lokumba baqale ukunaka ukusebenza kwe-NADES kwizicelo zabo. kutshanje. Ngo-2023, uRasul nabanye basebenzise indibaniselwano eyahlukeneyo ye-deep eutectic solvents yendalo esekelwe kwi-ascorbic acid26, i-calcium chloride27, i-potassium chloride28 kunye ne-Epsom salt29 kwaye bafezekisa ukuthintela kwe-shale okumangalisayo kunye nokubuyiselwa kwe-shale. Olu phononongo lolunye lwezifundo zokuqala zokwazisa i-NADES (ingakumbi i-citric acid kunye ne-glycerol-based formulation) njenge-shale inhibitor enobuhlobo nokusingqongileyo kwaye isebenzayo kulwelo lokubhola olusekelwe emanzini, olune-stability entle kakhulu yokusingqongileyo, amandla okuthintela i-shale aphuculweyo kunye nokusebenza ngcono kolwelo xa kuthelekiswa nezithinteli zemveli ezifana ne-KCl, ulwelo lwe-ionic olusekelwe kwi-imidazolyl kunye ne-DES yendabuko.
Olu phononongo luza kubandakanya ukulungiswa kwangaphakathi kwe-NADES esekwe kwi-citric acid (CA) kulandele ukuchazwa okuneenkcukacha kwe-physicochemical kunye nokusetyenziswa kwayo njengesongezelelo solwelo lokubhola ukuvavanya iimpawu zolwelo lokubhola kunye nokukwazi kwalo ukuthintela ukudumba. Kolu phononongo, i-CA iya kusebenza njengesamkeli se-hydrogen bond ngelixa i-glycerol (Gly) iya kusebenza njengomnikeli we-hydrogen bond okhethiweyo ngokusekelwe kwiikhrayitheriya zokuhlola ze-MH zokwakheka/ukukhethwa kwe-NADES kwizifundo zokuthintela i-shale30. I-Fourier transform infrared spectroscopy (FTIR), i-X-ray diffraction (XRD) kunye nokulinganisa kwe-zeta potential (ZP) kuya kucacisa ukusebenzisana kwe-NADES-clay kunye nendlela esekwe ngayo ukuthintela ukudumba kodongwe. Ukongeza, olu phononongo luza kuthelekisa ulwelo lokubhola olusekwe kwi-CA NADES kunye ne-DES32 ngokusekelwe kwi-1-ethyl-3-methylimidazolium chloride [EMIM]Cl7,12,14,17,31, KCl kunye ne-choline chloride:urea (1:2) ukuphanda ukusebenza kwazo ekuthinteleni i-shale kunye nokuphucula ukusebenza kolwelo lokubhola.
I-asidi ye-citric (i-monohydrate), i-glycerol (99 USP), kunye ne-urea zithengwe kwi-EvaChem, eKuala Lumpur, eMalaysia. I-Choline chloride (>98%), [EMIM]Cl 98%, kunye ne-potassium chloride zithengwe kwi-Sigma Aldrich, eMalaysia. Ulwakhiwo lweekhemikhali lwazo zonke iikhemikhali luboniswe kuMfanekiso 1. Umzobo oluhlaza uthelekisa iikhemikhali eziphambili ezisetyenzisiweyo kolu phononongo: i-imidazolyl ionic liquid, i-choline chloride (DES), i-citric acid, i-glycerol, i-potassium chloride, kunye ne-NADES (i-citric acid kunye ne-glycerol). Itheyibhile yobungani bendalo yeekhemikhali ezisetyenzisiweyo kolu phononongo iboniswe kwiTheyibhile 1. Kwitheyibhile, ikhemikhali nganye ilinganiswe ngokusekelwe kwityhefu, ukubola kwezinto eziphilayo, iindleko, kunye nokuzinza kokusingqongileyo.
Izakhiwo zeekhemikhali zezinto ezisetyenzisiweyo kolu phononongo: (a) i-citric acid, (b) [EMIM]Cl, (c) i-choline chloride, kunye (d) ne-glycerol.
Abanikeli be-hydrogen bond (HBD) kunye nabamkeli be-hydrogen bond (HBA) abafanelekileyo kuphuhliso lwe-CA (natural deep eutectic solvent) esekelwe kwi-NADES bakhethwe ngononophelo ngokwemigaqo yokukhetha ye-MH 30, eyenzelwe uphuhliso lwe-NADES njenge-shale inhibitors ezisebenzayo. Ngokwale miqathango, izinto ezinenani elikhulu labanikeli be-hydrogen bond kunye nabamkeli kunye namaqela asebenzayo e-polar zithathwa njengezifanelekileyo kuphuhliso lwe-NADES.
Ukongeza, i-ionic liquid [EMIM]Cl kunye ne-choline chloride:urea deep eutectic solvent (DES) zikhethwe ukuze zithelekiswe kolu phononongo kuba zisetyenziswa kakhulu njengezongezo zolwelo lokubhola33,34,35,36. Ukongeza, i-potassium chloride (KCl) ithelekiswe kuba sisithinteli esiqhelekileyo.
I-asidi ye-citric kunye ne-glycerol zixutywe ngokwemilinganiselo eyahlukeneyo ye-molar ukuze kufunyanwe imixube ye-eutectic. Ukuhlolwa okubonakalayo kubonise ukuba umxube we-eutectic wawululwelo olufanayo, olucacileyo olungena-turbidity, nto leyo ebonisa ukuba umniki-mali we-hydrogen bond (HBD) kunye nommkeli we-hydrogen bond (HBA) zixutywe ngempumelelo kolu lwakhiwo lwe-eutectic. Uvavanyo lokuqala lwenziwe ukujonga indlela yokuziphatha exhomekeke kubushushu benkqubo yokuxuba i-HBD kunye ne-HBA. Ngokweencwadi ezikhoyo, umlinganiselo wemixube ye-eutectic uvavanywe kumaqondo obushushu amathathu athile ngaphezulu kwe-50 °C, 70 °C kunye ne-100 °C, nto leyo ebonisa ukuba ubushushu be-eutectic buhlala buphakathi kwe-50–80 °C. Ibhalansi yedijithali ye-Mettler isetyenzisiwe ukulinganisa ngokuchanekileyo izinto ze-HBD kunye ne-HBA, kwaye ipleyiti eshushu ye-Thermo Fisher isetyenzisiwe ukufudumeza nokuvuselela i-HBD kunye ne-HBA kwi-100 rpm phantsi kweemeko ezilawulwayo.
Iimpawu ze-thermophysical ze-deep eutectic solvent yethu (DES) eyenziweyo, kuquka uxinano, uxinzelelo lomphezulu, i-refractive index, kunye ne-viscosity, zilinganiswe ngokuchanekileyo kuluhlu lobushushu oluqala kwi-289.15 ukuya kwi-333.15 K. Kufuneka kuqatshelwe ukuba olu luhlu lobushushu lukhethwe ikakhulu ngenxa yokunqongophala kwezixhobo ezikhoyo. Uhlalutyo olupheleleyo luquke uphando olunzulu lweepropati ezahlukeneyo ze-thermophysical zale fomyula ye-NADES, olutyhila indlela eziziphatha ngayo kuluhlu lobushushu. Ukugxila kolu luhlu lobushushu oluthile kubonelela ngengqiqo kwiipropati ze-NADES ezibaluleke kakhulu kwizicelo ezininzi.
Uxinzelelo lomphezulu we-NADES olulungisiweyo lulinganiswe ukusuka kwi-289.15 ukuya kwi-333.15 K kusetyenziswa imitha yoxinzelelo lwe-interfacial (IFT700). Amathontsi e-NADES enziwa kwigumbi elizaliswe ngumthamo omkhulu wolwelo kusetyenziswa inaliti ye-capillary phantsi kweemeko ezithile zobushushu kunye noxinzelelo. Iinkqubo zemifanekiso zanamhlanje zizisa iiparameter ezifanelekileyo zejometri ukubala uxinzelelo lwe-interfacial kusetyenziswa i-Laplace equation.
I-ATAGO refractometer isetyenzisiwe ukumisela i-refractive index ye-NADES esandul’ ukulungiswa kuluhlu lobushushu oluyi-289.15 ukuya kwi-333.15 K. Esi sixhobo sisebenzisa imodyuli yobushushu ukulawula ubushushu ukuqikelela inqanaba lokurhawuzelelwa kokukhanya, kususa imfuneko yokuhlamba amanzi ngobushushu obungaguqukiyo. Umphezulu weprism we-refractometer kufuneka ucocwe kwaye isisombululo sesampulu kufuneka sisasazwe ngokulinganayo phezu kwawo. Linganisa ngesisombululo esiqhelekileyo esaziwayo, uze ufunde i-refractive index kwisikrini.
Ubungakanani be-NADES obulungisiweyo bulinganiswe kubushushu obuphakathi kwama-289.15 ukuya kuma-333.15 K kusetyenziswa i-Brookfield rotational viscometer (uhlobo lwe-cryogenic) ngesantya se-shear se-30 rpm kunye nobukhulu be-spindle obuyi-6. I-viscometer ilinganisa ubuninzi be-viscometer ngokumisela i-torque efunekayo ukuze kujikeleziswe i-spindle ngesantya esingaguqukiyo kwisampuli yolwelo. Emva kokuba isampuli ibekwe kwiscreen phantsi kwe-spindle kwaye iqiniswe, i-viscometer ibonisa ubuninzi be-viscometer kwi-centipoise (cP), inika ulwazi oluxabisekileyo malunga neempawu ze-rheological zolwelo.
Imitha yoxinano oluphathwayo i-DMA 35 Basic isetyenzisiwe ukufumanisa uxinano lwe-natural deep eutectic solvent (NDEES) esandul’ ukulungiswa kubushushu obuyi-289.15–333.15 K. Ekubeni isixhobo singenaso isifudumezi esakhelwe ngaphakathi, kufuneka sifudunyezwe kubushushu obuchaziweyo (± 2 °C) ngaphambi kokusebenzisa imitha yoxinano lwe-NADES. Tsala ubuncinane i-2 ml yesampulu ngetyhubhu, kwaye uxinano luya kuboniswa kwangoko kwiscreen. Kubalulekile ukuqaphela ukuba ngenxa yokungabikho kwesifudumezi esakhelwe ngaphakathi, iziphumo zokulinganisa zinempazamo ye-± 2 °C.
Ukuvavanya i-pH ye-NADES esandula ukulungiswa kuluhlu lobushushu oluyi-289.15–333.15 K, sisebenzise imitha ye-pH ye-Kenis benchtop. Ekubeni kungekho sixhobo sokufudumeza esakhelwe ngaphakathi, i-NADES yaqala yafudunyezwa ukuya kubushushu obufunekayo (±2 °C) kusetyenziswa i-hotplate yaze yalinganiswa ngokuthe ngqo ngemitha ye-pH. Gcwalisa ngokupheleleyo i-pH meter probe kwi-NADES kwaye urekhode ixabiso lokugqibela emva kokuba ukufundwa kuzinzile.
Uhlalutyo lwe-thermogravimetric (TGA) lusetyenzisiwe ukuvavanya uzinzo lobushushu lwe-natural deep eutectic solvents (NADES). Iisampulu zahlalutywa ngexesha lokufudumeza. Kusetyenziswa ibhalansi echanekileyo kakhulu kunye nokujonga ngononophelo inkqubo yokufudumeza, kwaveliswa isicwangciso sokulahleka kobunzima xa kuthelekiswa nobushushu. I-NADES yafudunyezwa ukusuka kwi-0 ukuya kwi-500 °C ngesantya se-1 °C ngomzuzu.
Ukuqala inkqubo, isampuli ye-NADES kufuneka ixutywe kakuhle, ihlanganiswe ngokulinganayo, kwaye kususwe umswakama womphezulu. Isampuli elungisiweyo ibekwa kwi-cuvette ye-TGA, edla ngokwenziwa ngezinto ezingangeniyo ezifana ne-aluminium. Ukuqinisekisa iziphumo ezichanekileyo, izixhobo ze-TGA ziyalinganiswa kusetyenziswa izixhobo zokubhekisa, ngokuqhelekileyo imigangatho yobunzima. Nje ukuba ilinganiswe, uvavanyo lwe-TGA luqala kwaye isampuli ifudunyezwa ngendlela elawulwayo, ngokuqhelekileyo ngesantya esingaguqukiyo. Ukubeka iliso rhoqo kubudlelwane phakathi kobunzima besampuli kunye nobushushu yinxalenye ebalulekileyo yovavanyo. Izixhobo ze-TGA ziqokelela idatha kubushushu, ubunzima, kunye nezinye iiparameter ezifana nokuhamba kwegesi okanye ubushushu besampuli. Nje ukuba uvavanyo lwe-TGA lugqityiwe, idatha eqokelelweyo iyahlalutywa ukuze kuchongwe utshintsho kubunzima besampuli njengomsebenzi wobushushu. Olu lwazi lubalulekile ekumiseleni uluhlu lobushushu oluhambelana notshintsho lomzimba kunye neekhemikhali kwisampuli, kubandakanya iinkqubo ezifana nokunyibilika, ukufuma, i-oxidation, okanye ukubola.
Ulwelo lokugrumba olusekelwe emanzini lwenziwe ngononophelo ngokwemigangatho ye-API 13B-1, kwaye ulwakhiwo lwalo oluthile ludweliswe kwiTheyibhile 2 ukuze kubhekiselwe kulo. I-Citric acid kunye ne-glycerol (99 USP) zithengwe kwiSigma Aldrich, eMalaysia ukuze kulungiswe i-natural deep eutectic solvent (NADES). Ukongeza, i-conventional shale inhibitor potassium chloride (KCl) nayo ithengwe kwiSigma Aldrich, eMalaysia. I-1-ethyl, i-3-methylimidazolium chloride ([EMIM]Cl) enobumsulwa obungaphezulu kwe-98% ikhethiwe ngenxa yempembelelo yayo ebalulekileyo ekuphuculeni i-rheology yolwelo lokugrumba kunye nokuthintela i-shale, eyaqinisekiswa kwizifundo zangaphambili. Zombini i-KCl kunye ne-([EMIM]Cl) ziya kusetyenziswa kuhlalutyo lokuthelekisa ukuvavanya ukusebenza kokuthintela i-shale kwe-NADES.
Abaphandi abaninzi bakhetha ukusebenzisa ii-bentonite flakes ukuze bafunde ukudumba kwe-shale kuba i-bentonite ineqela elifanayo "le-montmorillonite" elibangela ukudumba kwe-shale. Ukufumana iisampulu zoqobo ze-shale core kunzima kuba inkqubo yokubopha iyawuphazamisa umphezulu we-shale, nto leyo ebangela iisampulu ezingezizo ngokupheleleyo ze-shale kodwa zihlala ziqulathe umxube wesanti kunye neengqimba ze-limestone. Ukongeza, iisampulu ze-shale zihlala zingenazo amaqela e-montmorillonite abangela ukudumba kwe-shale kwaye ke ngoko azifanelekanga kwiimvavanyo zokuthintela ukudumba.
Kolu phononongo, sisebenzise amasuntswana e-bentonite aphinde akhiwa anobubanzi obumalunga ne-2.54 cm. Amasuntswana enziwe ngokucinezela i-11.5 grams ye-sodium bentonite powder kwi-hydraulic press kwi-1600 psi. Ubukhulu bamasuntswana bulinganiswe ngokuchanekileyo ngaphambi kokuba bubekwe kwi-linear dilatometer (LD). Amasuntswana emva koko antywiliselwa kwiisampulu zolwelo lokubhola, kuquka iisampulu zesiseko kunye neesampulu ezifakwe izithinteli ezisetyenziselwa ukuthintela ukudumba kwe-shale. Utshintsho kubukhulu be-granule emva koko lwajongwa ngononophelo kusetyenziswa i-LD, kunye nemilinganiselo erekhodwe kwizithuba zemizuzwana engama-60 kangangeeyure ezingama-24.
I-X-ray diffraction ibonise ukuba ukwakheka kwe-bentonite, ingakumbi i-47% ye-montmorillonite component, yinto ebalulekileyo ekuqondeni iimpawu zayo zejoloji. Phakathi kwe-montmorillonite component ye-bentonite, i-montmorillonite yeyona nxalenye iphambili, ebalelwa kwi-88.6% yezakhi zizonke. Okwangoku, i-quartz ibalelwa kwi-29%, i-illite ibe yi-7%, kunye ne-carbonate ibe yi-9%. Inxalenye encinci (malunga ne-3.2%) ngumxube we-illite kunye ne-montmorillonite. Ukongeza, iqulethe izinto ezincinci ezifana ne-Fe2O3 (4.7%), i-silver aluminosilicate (1.2%), i-muscovite (4%), kunye ne-phosphate (2.3%). Ukongeza, kukho inani elincinci le-Na2O (1.83%) kunye ne-iron silicate (2.17%), nto leyo eyenza kube lula ukuqonda ngokupheleleyo izinto eziyinxalenye ye-bentonite kunye nobungakanani bazo.
Eli candelo libanzi lophando lichaza iipropati ze-rheological kunye ne-filtration zeesampulu zolwelo lokubhola ezilungiselelwe kusetyenziswa i-natural deep eutectic solvent (NADES) kwaye zisetyenziswa njenge-drilling fluid additive kwii-concentrations ezahlukeneyo (1%, 3% kunye ne-5%). Iisampulu ze-slurry ezisekelwe kwi-NADES emva koko zathelekiswa zaza zahlalutywa ngeesampulu ze-slurry eziquka i-potassium chloride (KCl), i-CC:urea DES (i-choline chloride deep eutectic solvent:urea) kunye ne-ionic liquids. Inani leeparameter eziphambili zigutyungelwe kolu phononongo kubandakanya ukufundwa kwe-viscosity okufunyenwe kusetyenziswa i-FANN viscometer ngaphambi nasemva kokuvezwa kwiimeko zokwaluphala kwi-100°C kunye ne-150°C. Ukulinganiswa kuthathwe ngesantya sokujikeleza esahlukileyo (3 rpm, 6 rpm, 300 rpm kunye ne-600 rpm) okuvumela uhlalutyo olupheleleyo lokuziphatha kolwelo lokubhola. Idatha efunyenweyo ingasetyenziselwa ukumisela iipropati eziphambili ezifana ne-yield point (YP) kunye ne-plastic viscosity (PV), ezibonelela ngengqiqo yokusebenza kolwelo phantsi kweemeko ezahlukeneyo. Uvavanyo lokuhluza olunoxinzelelo oluphezulu (HPHT) kwi-400 psi kunye ne-150°C (amaqondo obushushu aqhelekileyo kwimithombo yobushushu obuphezulu) lumisela ukusebenza kokuhluza (ubukhulu bekhekhe kunye nomthamo wokuhluza).
Eli candelo lisebenzisa izixhobo zanamhlanje, iGrace HPHT Linear Dilatometer (M4600), ukuvavanya ngokupheleleyo iipropati zokuthintela ukudumba kwe-shale kwi-fluids zethu zokubhola ezisekelwe emanzini. I-LSM ngumatshini wanamhlanje oqulathe izinto ezimbini: i-plate compactor kunye ne-linear dilatometer (imodeli: M4600). Iiplate zeBentonite zalungiselelwa uhlalutyo kusetyenziswa iGrace Core/Plate Compactor. I-LSM emva koko inika idatha yokudumba kwangoko kwezi plate, ivumela uvavanyo olupheleleyo lweepropati zokuthintela ukudumba kwe-shale. Uvavanyo lokwandiswa kwe-Shale lwenziwe phantsi kweemeko ezingqongileyo, oko kukuthi, ama-25°C kunye ne-1 psia.
Uvavanyo lokuzinza kwe-shale lubandakanya uvavanyo oluphambili oludla ngokubizwa ngokuba luvavanyo lokubuyisela i-shale, uvavanyo lwe-shale dip okanye uvavanyo lokusasazwa kwe-shale. Ukuqala olu vavanyo, iziqwenga ze-shale zahlulwe kwisikrini se-BSS #6 zize zibekwe kwisikrini se-#10. Iziqwenga emva koko zinikwa itanki yokubamba apho zixutywa khona nolwelo olusisiseko kunye nodaka lokubhola olune-NADES (Natural Deep Eutectic Solvent). Inyathelo elilandelayo kukubeka umxube kwi-oven ukuze kuqhutyekwe nenkqubo yokuqengqeleka eshushu kakhulu, ukuqinisekisa ukuba iziqwenga kunye nodaka zixutywe kakuhle. Emva kweeyure ezili-16, iziqwenga zisuswa kwi-pulp ngokuvumela i-shale ukuba ibole, nto leyo ekhokelela ekunciphiseni ubunzima beziqwenga. Uvavanyo lokubuyisela i-shale lwenziwe emva kokuba iziqwenga ze-shale zibanjwe kudaka lokubhola kwi-150°C kunye ne-1000 psi. intshi kwiiyure ezingama-24.
Ukuze silinganise ukubuyiselwa kodaka lwe-shale, saluhluza ngesikrini esicolekileyo (i-40 mesh), saza saluhlamba kakuhle ngamanzi, saza ekugqibeleni salomisa kwi-oven. Le nkqubo inzima isivumela ukuba siqikelele udaka olufunyenweyo xa kuthelekiswa nobunzima bokuqala, ekugqibeleni sibala ipesenti yodaka lwe-shale olufunyenwe ngempumelelo. Umthombo weesampuli ze-shale uvela kwiSithili saseNiah, kwiSithili saseMiri, eSarawak, eMalaysia. Ngaphambi kovavanyo lokusasazwa nokubuyiselwa, iisampuli ze-shale zenziwa uhlalutyo olupheleleyo lwe-X-ray diffraction (XRD) ukuze kulinganiswe ukwakheka kwazo kodongwe kwaye kuqinisekiswe ukuba zifanelekile na ukuvavanywa. Ukwakheka kweeminerali zodongwe kwisampuli kulandelayo: illite 18%, kaolinite 31%, chlorite 22%, vermiculite 10%, kunye ne-mica 19%.
Uxinzelelo lomphezulu yinto ephambili elawula ukungena kweendawo zamanzi kwii-shale micropores ngesenzo se-capillary, esiza kufundwa ngokweenkcukacha kweli candelo. Eli phepha lihlola indima yoxinzelelo lomphezulu kwipropati edibeneyo yolwelo lokubhola, ligxininisa impembelelo yalo ebalulekileyo kwinkqubo yokubhola, ingakumbi uthintelo lwe-shale. Sisebenzise i-interfacial tensiometer (IFT700) ukulinganisa ngokuchanekileyo uxinzelelo lomphezulu weesampuli zolwelo lokubhola, sityhila inkalo ebalulekileyo yokuziphatha kolwelo kwimeko yothintelo lwe-shale.
Eli candelo lixoxa ngokweenkcukacha ngesithuba se-d-layer, esikumgama ophakathi kwe-aluminosilicate layers kunye ne-aluminosilicate layer enye kwi-clays. Uhlalutyo lugubungele iisampulu zodaka olumanzi oluqulethe i-1%, 3% kunye ne-5% CA NADES, kunye ne-3% KCl, 3% [EMIM]Cl kunye ne-3% CC:urea based DES ukuze kuthelekiswe. I-benchtop X-ray diffractometer (D2 Phaser) yanamhlanje esebenza kwi-40 mA kunye ne-45 kV ene-Cu-Kα radiation (λ = 1.54059 Å) idlale indima ebalulekileyo ekurekhodeni iincopho ze-X-ray diffraction zeesampulu ze-Na-Bt ezimanzi nezomileyo. Ukusetyenziswa kwe-Bragg equation kwenza kube lula ukumisela ngokuchanekileyo isithuba se-d-layer, ngaloo ndlela kubonelela ngolwazi oluxabisekileyo malunga nokuziphatha kodongwe.
Eli candelo lisebenzisa isixhobo esiphambili seMalvern Zetasizer Nano ZSP ukulinganisa ngokuchanekileyo amandla e-zeta. Olu vavanyo lubonelele ngolwazi oluxabisekileyo malunga neempawu zetshaja zeesampuli zodaka oluxutyiweyo oluqulethe i-1%, 3%, kunye ne-5% CA NADES, kunye ne-3% KCl, 3% [EMIM]Cl, kunye ne-3% CC:urea-based DES yohlalutyo oluthelekisayo. Ezi ziphumo zinegalelo ekuqondeni kwethu ukuzinza kweekhompawundi ze-colloidal kunye nokusebenzisana kwazo kwiilwelo.
Iisampulu zodongwe zihlolwe ngaphambi nasemva kokuvezwa kwi-natural deep eutectic solvent (NADES) kusetyenziswa i-Zeiss Supra 55 VP field emission scanning electron microscope (FESEM) exhotyiswe nge-energy dispersive X-ray (EDX). Isisombululo somfanekiso yayiyi-500 nm kwaye amandla e-electron beam yayiyi-30 kV kunye ne-50 kV. I-FESEM ibonelela ngembonakalo ephezulu yesimo somphezulu kunye neempawu zesakhiwo seesampulu zodongwe. Injongo yolu phononongo yayikukufumana ulwazi malunga nempembelelo ye-NADES kwiisampulu zodongwe ngokuthelekisa imifanekiso efunyenwe ngaphambi nasemva kokuvezwa.
Kolu phononongo, iteknoloji ye-field emission scanning electron microscopy (FESEM) isetyenzisiwe ukuphanda impembelelo ye-NADES kwiisampuli zodongwe kwinqanaba le-microscope. Injongo yolu phononongo kukucacisa ukusetyenziswa okunokwenzeka kwe-NADES kunye nempembelelo yayo kwimo yodongwe kunye nobukhulu obuphakathi bee-particle, nto leyo eya kubonelela ngolwazi oluxabisekileyo kuphando kweli candelo.
Kolu phononongo, imivalo yeempazamo isetyenzisiwe ukuchaza ngokubonakalayo umahluko kunye nokungaqiniseki kwempazamo yepesenti ephakathi (i-AMPE) kwiimeko zovavanyo. Endaweni yokuceba ixabiso le-AMPE ngalinye (ekubeni ukuceba ixabiso le-AMPE kunokufihla imikhwa kwaye kugqithise umahluko omncinci), sibala imivalo yeempazamo sisebenzisa umthetho we-5%. Le ndlela iqinisekisa ukuba ibha nganye yeempazamo imele ixesha apho ixesha lokuzithemba le-95% kunye ne-100% yamaxabiso e-AMPE kulindeleke ukuba liwe, ngaloo ndlela kubonelela ngesishwankathelo esicacileyo nesifutshane sokusasazwa kwedatha kwimeko nganye yovavanyo. Ukusebenzisa imivalo yeempazamo ngokusekelwe kumthetho we-5% ngaloo ndlela kuphucula ukutolikwa kunye nokuthembeka kwemiboniso yemizobo kwaye kunceda ukubonelela ngokuqonda okuneenkcukacha ngakumbi kweziphumo kunye neziphumo zazo.
Ekuqulunqweni kwezinto zemvelo ezinzulu ze-eutectic solvents (NADES), iiparameter ezininzi ezibalulekileyo zifundwe ngononophelo ngexesha lenkqubo yokulungiselela ngaphakathi endlwini. Ezi zinto zibalulekileyo ziquka ubushushu, umlinganiselo we-molar, kunye nesantya sokuxuba. Uvavanyo lwethu lubonisa ukuba xa i-HBA (i-citric acid) kunye ne-HBD (glycerol) zixutywe kwi-molar ratio ye-1:4 kwi-50°C, umxube we-eutectic wenziwa. Uphawu olwahlukileyo lomxube we-eutectic kukubonakala kwawo okucacileyo, okufanayo, kunye nokungabikho kwe-sediment. Ngoko ke, eli nyathelo libalulekileyo ligxininisa ukubaluleka komlinganiselo we-molar, ubushushu, kunye nesantya sokuxuba, phakathi kwazo umlinganiselo we-molar wawuyeyona nto inefuthe ekulungiseleleni i-DES kunye ne-NADES, njengoko kubonisiwe kuMfanekiso 2.
Isalathisi sokuchasana (n) sichaza umlinganiselo wesantya sokukhanya kwi-vacuum kwisantya sokukhanya kwi-medium yesibini, exineneyo. Isalathisi sokuchasana sinomdla kakhulu kwi-natural deep eutectic solvents (NADES) xa kujongwa ukusetyenziswa kwe-optically sensitive njenge-biosensors. Isalathisi sokuchasana se-NADES esifundwe kwi-25 °C yayiyi-1.452, esezantsi ngokumangalisayo kuneye-glycerol.
Kubalulekile ukuqaphela ukuba i-refractive index ye-NADES iyancipha ngobushushu, kwaye le ndlela ingachazwa ngokuchanekileyo ngefomula (1) kunye noMfanekiso 3, apho i-absolute mean percentage error (AMPE) ifikelela kwi-0%. Le ndlela yokuziphatha exhomekeke kubushushu ichazwa kukwehla kwe-viscosity kunye noxinano kubushushu obuphezulu, okubangela ukuba ukukhanya kuhambe kwi-medium ngesantya esiphezulu, okubangela ixabiso eliphantsi le-refractive index (n). Ezi ziphumo zibonelela ngengqiqo ebalulekileyo malunga nokusetyenziswa kwe-NADES kwi-optical sensing, zigqamisa amandla azo kwizicelo ze-biosensor.
Uxinzelelo lomphezulu, olubonisa ukuthambekela komphezulu wolwelo ekunciphiseni indawo yawo, lubaluleke kakhulu ekuvavanyeni ukufaneleka kwe-natural deep eutectic solvents (NADES) kwizicelo ezisekelwe kuxinzelelo lwe-capillary. Uphononongo loxinzelelo lomphezulu kuluhlu lobushushu oluyi-25–60 °C lubonelela ngolwazi oluxabisekileyo. Kwi-25 °C, uxinzelelo lomphezulu lwe-NADES olusekelwe kwi-citric acid yayiyi-55.42 mN/m, ephantsi kakhulu kunaleyo yamanzi kunye ne-glycerol. Umfanekiso 4 ubonisa ukuba uxinzelelo lomphezulu luyehla kakhulu xa ubushushu busanda. Le nto ingachazwa ngokwanda kwamandla e-molecular kinetic kunye nokwehla okulandelayo kwamandla anomtsalane phakathi kweemolekyuli.
Ukwehla okuthe ngqo koxinzelelo lomphezulu olubonwe kwi-NADES efundwayo kunokubonakaliswa kakuhle yi-equation (2), ebonisa ubudlelwane obusisiseko bezibalo kuluhlu lobushushu obuyi-25–60 °C. Igrafu ekuMfanekiso 4 ibonisa ngokucacileyo utyekelo loxinzelelo lomphezulu kunye nobushushu obunempazamo yepesenti ephakathi (i-AMPE) eyi-1.4%, elinganisa ukuchaneka kwamaxabiso oxinzelelo lomphezulu axeliweyo. Ezi ziphumo zinempembelelo ebalulekileyo ekuqondeni ukuziphatha kwe-NADES kunye nokusetyenziswa kwayo okunokwenzeka.
Ukuqonda i-density dynamics ye-natural deep eutectic solvents (NADES) kubalulekile ukuze kube lula ukuyisebenzisa kwizifundo ezininzi zesayensi. Uxinano lwe-citric acid-based NADES kwi-25°C yi-1.361 g/cm3, ephezulu kunoxinano lwe-parent glycerol. Lo mahluko ungachazwa ngokongezwa kwe-hydrogen bond acceptor (citric acid) kwi-glycerol.
Ukuthatha i-NADES esekelwe kwi-citrate njengomzekelo, uxinano lwayo luyehla luye kwi-1.19 g/cm3 kwi-60°C. Ukwanda kwamandla e-kinetic xa kushushu kubangela ukuba iimolekyuli ze-NADES zisasazeke, nto leyo ebangela ukuba zihlale kwivolumu enkulu, nto leyo ebangela ukwehla koxinano. Ukwehla okubonwayo koxinano kubonisa ulwalamano oluthile oluhambelanayo nokunyuka kobushushu, olunokubonakaliswa ngokufanelekileyo ngefomula (3). Umfanekiso 5 ubonisa ngokucacileyo ezi mpawu zotshintsho loxinano lwe-NADES ngempazamo yepesenti echanekileyo (AMPE) ye-1.12%, ebonelela ngomlinganiselo wobungakanani bokuchaneka kwamaxabiso oxinano axeliweyo.
Ukuqina ngamandla anomtsalane phakathi kweengqimba ezahlukeneyo zolwelo oluhambayo kwaye ludlala indima ephambili ekuqondeni ukusebenza kwe-natural deep eutectic solvents (NADES) kwizicelo ezahlukeneyo. Kwi-25 °C, i-viscosity ye-NADES yayiyi-951 cP, ephezulu kuneye-glycerol.
Ukwehla okubonwayo kwe-viscosity kunye nobushushu obukhulayo kuchazwa kakhulu kubuthathaka kwamandla akhangayo phakathi kweemolekyuli. Le nto ibangela ukwehla kwe-viscosity yolwelo, umkhwa oboniswe ngokucacileyo kuMfanekiso 6 kwaye ulinganiswe yi-Equation (4). Okuphawulekayo kukuba, kwi-60°C, i-viscosity yehla iye kwi-898 cP kunye ne-avareji yepesenti ye-avareji (AMPE) ye-1.4%. Ukuqonda okuneenkcukacha kwe-viscosity ngokuchasene nokuxhomekeka kobushushu kwi-NADES kubaluleke kakhulu ekusebenziseni kwayo okusebenzayo.
I-pH yesisombululo, echongwa yi-logarithm engalunganga yoxinzelelo lwe-hydrogen ion, ibalulekile, ngakumbi kwizicelo ezinobuzaza be-pH ezifana nokwenziwa kwe-DNA, ngoko ke i-pH ye-NADES kufuneka ifundwe ngononophelo ngaphambi kokuba isetyenziswe. Ukuthatha i-NADES esekelwe kwi-citric acid njengomzekelo, i-pH ene-asidi ecacileyo ye-1.91 inokubonwa, nto leyo eyahluke kakhulu kwi-pH engathathi cala ye-glycerol.
Okunomdla kukuba, i-pH ye-natural citric acid dehydrogenase soluble solvent (NADES) ibonise ukwehla okungaqhelekanga kunye nokunyuka kwamaqondo obushushu. Le nto ibangelwa kukwanda kokungcangcazela kweemolekyuli okuphazamisa ibhalansi ye-H+ kwisisombululo, okukhokelela ekwakhiweni kwee-ions ze-[H]+ kwaye, ngokuphindaphindiweyo, utshintsho kwixabiso le-pH. Ngelixa i-pH yendalo ye-citric acid isusela kwi-3 ukuya kwi-5, ubukho be-hydrogen ene-acid kwi-glycerol buyinciphisa ngakumbi i-pH ukuya kwi-1.91.
Ukuziphatha kwe-pH ye-NADES esekelwe kwi-citrate kuluhlu lobushushu obuyi-25–60 °C kunokumelwa ngokufanelekileyo yi-equation (5), enika intetho yemathematika yethrendi ye-pH ebonweyo. Umfanekiso 7 ubonisa ngokucacileyo olu lwalamano lunomdla, ugxininisa impembelelo yobushushu kwi-pH ye-NADES, exelwe ukuba yi-1.4% ye-AMPE.
Uhlalutyo lwe-thermogravimetric (TGA) lwe-natural citric acid deep eutectic solvent (NADES) lwenziwe ngokucwangcisiweyo kumanqanaba obushushu ukusuka kubushushu begumbi ukuya kwi-500 °C. Njengoko kunokubonwa kwiMifanekiso 8a kunye no-b, ukulahleka kokuqala kobunzima ukuya kwi-100 °C kwakubangelwa kakhulu ngamanzi afunxwayo kunye namanzi adibene ne-citric acid kunye ne-glycerol ecocekileyo. Ukugcinwa okukhulu kobunzima obumalunga ne-88% kwabonwa ukuya kuthi ga kwi-180 °C, okwakubangelwa ikakhulu kukubola kwe-citric acid kwi-aconitic acid kunye nokwakheka okulandelayo kwe-methylmaleic anhydride (III) xa kufudunyezwa ngakumbi (Umfanekiso 8 b). Ngaphezulu kwe-180 °C, ukubonakala okucacileyo kwe-acrolein (acrylaldehyde) kwi-glycerol nako kunokubonwa, njengoko kuboniswe kwiMifanekiso 8b37.
Uhlalutyo lwe-thermogravimetric (TGA) ye-glycerol lubonise inkqubo yokulahleka kobunzima obunezigaba ezibini. Inqanaba lokuqala (180 ukuya kwi-220 °C) libandakanya ukwakheka kwe-acrolein, kulandele ukulahleka okukhulu kobunzima kumaqondo obushushu aphezulu ukusuka kwi-230 ukuya kwi-300 °C (Umfanekiso 8a). Njengoko ubushushu busanda, i-acetaldehyde, i-carbon dioxide, i-methane, kunye ne-hydrogen zenziwa ngokulandelelana. Okuphawulekayo kukuba, yi-28% kuphela yobunzima egcinwe kwi-300 °C, nto leyo ebonisa ukuba iipropati zangaphakathi ze-NADES 8(a)38,39 zinokuba neziphene.
Ukuze kufunyanwe ulwazi malunga nokwakheka kweebhondi ezintsha zeekhemikhali, ukumiswa okusandul’ ukulungiswa kwe-natural deep eutectic solvents (NADES) kuhlalutywe yi-Fourier transform infrared spectroscopy (FTIR). Uhlalutyo lwenziwe ngokuthelekisa i-spectrum ye-NADES suspension kunye ne-spectra ye-citric acid ecocekileyo (CA) kunye ne-glycerol (Gly). I-CA spectrum ibonise iincopho ezicacileyo kwi-1752 1/cm kunye ne-1673 1/cm, ezimele ukungcangcazela okunwebekayo kwebhondi ye-C=O kwaye zikwaphawu lwe-CA. Ukongeza, utshintsho olukhulu kwi-OH bending vibration kwi-1360 1/cm lubonwe kummandla weminwe, njengoko kubonisiwe kuMfanekiso 9.
Ngokufanayo, kwimeko ye-glycerol, utshintsho lwe-OH stretching kunye ne-bending vibrations lufunyenwe kwiinombolo zamaza ze-3291 1/cm kunye ne-1414 1/cm, ngokulandelelana. Ngoku, ngokuhlalutya i-spectrum ye-NADES elungisiweyo, kufunyenwe utshintsho olukhulu kwi-spectrum. Njengoko kubonisiwe kuMfanekiso 7, ukungcangcazela kokungcangcazela kwe-C=O bond kutshintshe ukusuka kwi-1752 1/cm ukuya kwi-1720 1/cm kunye nokungcangcazela kokungcangcazela kwe--OH bond ye-glycerol kutshintshe ukusuka kwi-1414 1/cm ukuya kwi-1359 1/cm. Olu tshintsho kwiinombolo zamaza lubonisa utshintsho kwi-electronegativity, olubonisa ukwakheka kweebhondi ezintsha zeekhemikhali kwisakhiwo se-NADES.