1 Isingeniso
Njengamanje, izinto eziphambili ezingavuthiwe ezisetshenziselwa ukulungisaI-Cellulose Etherkukhona ukotini, futhi ukuphuma kwalo kuyancipha, futhi intengo iyavuka;
Ngaphezu kwalokho, ama-ejenti asetshenziswa kakhulu asetshenziswa njenge-chlororocetic acid (ubuthi obunobuthi obunobuthi) ne-ethylene oxide (carcinogenic) futhi kuyingozi emzimbeni womuntu kanye nemvelo. Ibhuku
Kulesi sahluko, i-pine cellulose enobumsulwa obuhlobene bangaphezulu kwama-90% esahlukweni sesibili kusetshenziswa njengento eluhlaza, kanye ne-sodium chloropetate kanye ne-2-chloroethanol kanye ne-2-chloroethanol zisetshenziswa njengezigatshaneni.
Kusetshenziswa i-chlororopetic acid enobuthi kakhulu njenge-ejenti etherati, i-anionicI-Carboxymethyl Cellulose (CMC)Kwalungiswa i-Heldroxyyethyyls engekho e-Ionoxyyethyl.
I-Cellulose (HEC) ne-Hydroxyyethyl carboxyllyl celtulose (HECMC) ezintathu ze-cellulose. isici esisodwa
Amasu okulungiselela ama-cellulose afers alungiselelwe izivivinyo kanye nokuhlolwa kwe-orthogonal, kanye nezimpikiswano zokwenziwa kwe-cellulose zazibonakaliswa yi-FT-IR, XRD, H-NMR, njll.
Okuyisisekelo se-cellulose etherification
Umgomo we-cellulose ukuhanjiswa uhlukaniswe izingxenye ezimbili. Ingxenye yokuqala inqubo ye-alkalization, okungukuthi, ngesikhathi sokusabela kwe-alkalization ye-cellulose,
Ahlakazeke ngokulinganayo kusixazululo se-nao, uPine Cellulose wavuvukala ngobudlova ngaphansi kwesenzo sokuvuselelwa kwemishini, nangokunwetshwa kwamanzi
Inani elikhulu lama-molecule amancane ama-Naoh angena ngaphakathi kwephalulamu yepayipi, futhi aphendule ngamaqembu e-hydroxyl endabeni ye-glucose yesakhiwo,
Khiqiza i-Alkali Cellulose, isikhungo esisebenzayo sokuphendula okuthe xaxa.
Ingxenye yesibili inqubo yokuthezeka, okungukuthi, ukusabela phakathi kwesikhungo esisebenzayo kanye ne-sodium chloropetate noma 2-chloroethanol ngaphansi kwezimo ze-alkali, okuholela
Ngasikhathi sinye, i-ejenti yokuphelisa i-agent sodium chloropetate kanye no-2-chlorothanol nayo izokhiqiza izinga elithile lamanzi ngaphansi kwezimo ze-alkali.
Ukusabela eceleni kuxazululwa ukukhiqiza i-sodium glycolate ne-ethylene glycol, ngokulandelana.
2 ukugxila kwe-alkali edidekisa ukwenziwa kwe-pine cellulose
Okokuqala, lungiselela ukugxila okuthile kwesisombululo se-nao ngamanzi ama-deionized. Ngemuva kwalokho, emazingeni okushisa athile, 2g we-pine fiber
Amavithamini ancibilikisiwe ngevolumu ethile yesixazululo sikaNaoh, avuselelwa isikhathi esithile, bese ehlunga ukuthi isetshenziswe.
Umkhiqizi Wamamodeli Wensimbi
I-PRITION PH Imitha
I-Collector Throad Temperature Heathring Magnetic Stillrer
I-vacuum yomisa kuhhavini
Ibhalansi ye-elekthronikhi
Ukujikeleza kwamanzi okujikeleza amanzi ahlukahlukene
I-Fourier Transform Infrared Spectrometer
I-X-RAY IGRRACTOmeter
I-Nuclear Magnetic Resonance Spectrometer
I-Hangzhou Aolilong Ithuluzi Wezentengiso Co, Ltd.
I-Hangzhou Huichuang Izinsiza Zensimbi Co, Ltd.
Shanghai Jinghong Experimental Equipment Co, Ltd.
I-Mettler Toledo Amathuluzi (Shanghai) Co, Ltd.
I-Hangzhou Daving Science ne-Education Mounty Co, Ltd.
I-American Thermo Fisher Co, Ltd.
Inkampani yase-American Thermoelectric Switzelectric Switzelland
I-Swiss Company Bruker
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Ukulungiselela ama-CMC
Usebenzisa i-Pine Wood Alkali Cellulose Phezu kokumiswa okuhlanganisiwe kwe-Alkali Decrystallization njenge-ethanol njenge-solvent kanye nokusebenzisa i-sodium chlororoate njengokuthezeka
I-CMC ene-DS ephakeme yalungiswa ngokungeza i-Alkali kabili kanye ne-ejenti ethembisa kabili. Faka i-2G ye-Pine Wood Alkali Cellule ku-Flask entamo ezine, bese wengeza umthamo othile we-ethanol solvent, bese uvusa kahle ama-30min
mayelana, ukuze i-Alkali Cellulose ihlakazeke ngokuphelele. Ngemuva kwalokho engeza inani elithile le-Agent ye-Alkali ne-sodium chlororetate ukuze usabele isikhathi esithile sokushisa okuthile kokuthezeka
Ngemuva kwesikhathi, ukungezwa kwesibili kwe-alkaline ejenti kanye ne-sodium chloropetate elandelwa ukusheshisa isikhathi esithile. Ngemuva kokuthi ukusabela sekuphelile, kupholile phansi futhi kupholile phansi, khona-ke
Hlanganisa nenani elifanele le-glacial acetic acid, bese uchofoza isihlungi, ugeze futhi womile.
Ukulungiselela ama-HEC
Usebenzisa uPine Wood Alkali Cellulose Pred Hiellowed nge-Alkali Decrystallization njengezinto ezibonakalayo ezifuywayo, i-ethanol njenge-solvent ne-2-chloroethanol njenge-etherification
I-HEC ene-MS ephakeme yalungiswa ngokungeza i-Alkali kabili kanye ne-ejenti ethembisa kabili. Engeza i-Pine Wood Wood Alkali Celluleli ku-Flask entamo ezine, bese wengeza umthamo othile wama-90% (Ingxenye yevolumu) ethanol, ivuse
Govuza isikhathi sokusakaza ngokugcwele, bese ufaka inani elithile le-alkali, futhi ufudumele kancane kancane, engeza umqulu othile we-2-
I-Chloroethanol, i-etherifish emazingeni okushisa ahlala njalo, bese wengeza i-sodium hydroxide esele esele kanye ne-2-chloroethanol ukuze uqhubeke nokuthelwa kwesikhathi esithile. phatha
Ngemuva kokuthi ukusabela sekuqediwe, hlangothi ngenani elithile le-glacial acetic acid, bese ekugcineni uhlunga ngesihlungi sengilazi (G3), geza, bese womile.
Ukulungiselela i-hemcc
Usebenzisa i-HEC elungiselelwe ngo-3.2.3.4 njengento eluhlaza, i-ethanol njenge-reaction medium, kanye ne-sodium chloropetate njenge-ejenti yokuphelelisa ukulungiselela
I-HECMC. Inqubo ethile yilena: Thatha inani elithile le-hec, likubeke eflethini elinentamo elingama-100 ml, bese wengeza inani elithile levolumu
I-90% ethanol, nge-mechanicage ivusa isikhathi esithile ukuyenza ihlakazeke ngokuphelele, engeza inani elithile le-alkali ngemuva kokushisa, futhi lingeze kancane
I-Sodium Chlororoetate, ukusheshisa ekushiseni okuhlala njalo kuphele isikhathi esithile. Ngemuva kokuthi ukusabela sekuqediwe, kungathathi hlangothi nge-glacial acetic acid ukuze uyisebenzise, bese usebenzisa isihlungi sengilazi (G3)
Ngemuva kokumunca ukungcola, ukugeza nokukomisa.
Ukuhlanzwa kwe-Cellulose Afers
Ehlelweni lokulungiselela le-cellulose ether, eminye imikhiqizo ethile ivame ukukhiqizwa, ikakhulukazi i-inorganic usawoti chlorium chloride nabanye
ukungcola. Ukuze uthuthukise ikhwalithi ye-cellulose ether, ukuhlanzwa okulula kwenziwa ku-ether etholwe ku-cellulose. ngoba zisemanzini
Kukhona i-soubity ehlukile, ngakho-ke ukuhlolwa kusebenzisa ingxenye ethile yevolumu ye-ethanol egcwele ukuhlanza ama-relueles tallulose.
shintsha.
Beka isampula ye-cellulose err elungiselelwe ngekhwalithi ethile ku-beaker, engeza inani elithile le-80% ethanol elisuke labuyiselwa ku-60 ℃ ~ 65 ~ 65 ~ 65 ~ 65 ~ 65 ~ 65 ~ 65 ~ 65 ~ 65 ~ 65 ~ 65 ~ 60 ngo-10 ℃. imiz. Thatha i-supernatant ukuze wome
Ku-beaker ehlanzekile, sebenzisa i-nitrate yesiliva ukuze uhlole i-chloride ion. Uma kukhona i-verapitate emhlophe, hlunga ngokusebenzisa isihlungi sengilazi bese uthatha okuqinile
Phinda izinyathelo zangaphambilini zengxenye yomzimba, kuze kube yilapho i-filtrate ngemuva kokungeza i-1 yehlayo ye-Agno3 isixazululo esimhlophe, okungukuthi, ukuwa okuhlanzwa nokugeza kuqediwe.
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ku (ikakhulukazi ukususa ukusabela kwe-nacl yomkhiqizo). Ngemuva kokutholwa kwe-filtration, ukomisa, ukupholisa kokushisa kwegumbi nokukala.
isisindo, g.
Izindlela Zokuhlola Nezimpawu Zama-Cellulose Afers
Ukunqunywa kwezinga lokufaka esikhundleni (DS) kanye ne-molar degree yokufaka esikhundleni (MS)
Ukunqunywa kwe-DS: Okokuqala, kunesisindo esingu-0.2 g (kunembile ku-0,1 mg) wesampula ye-ether ye-ether ye-cellulose ehlanziwe, uyikhiphe ngaphakathi
I-80ML yamanzi anciphile, ivuselelwa ekugezeni kwamanzi okushisa njalo ku-30 ℃ ~ 40 ~ 40 ℃ nge-10min. Bese ulungisa nge-Sulfuric Acid Solution noma i-Naoh Solution
ph kwesixazululo kuze kube yilapho i-pH yesisombululo ineminyaka engu-8. Ngemuva kwalokho e-beaker efakwe i-eclector ye-Ph metle, sebenzisa isixazululo esijwayelekile se-sulfuric acid
Ukuthambeka, ngaphansi kwemibandela evuthayo, gcina ukufundwa kwemitha ye-Ph ngenkathi kuthathwa khona, lapho inani le-PH lekhambi liyalungiswa ku-3.74,
Ukuphakanyiswa kuyaphela. Qaphela umthamo wesisombululo esijwayelekile se-sulfuric acid esetshenziswe ngalesi sikhathi.
Isizukulwane:
Isamba sezinombolo ezingenhla ze-proton neqembu le-hydroxyethyl
Isilinganiso senombolo yamaprotoni aphezulu; I-I7 inqwaba yeqembu le-methylene eqenjini le-hydroxyethyl
Ubukhulu be-protoon resonance peak; ubukhulu be-proton resonance peak yamaqembu ama-5 we-methrine neqembu elilodwa le-methylene e-cellulose glucose unit
Isamba.
Izindlela zokuhlola ezichazwe ekuhlolweni kokuhlolo okwenziwa yi-cellulose Talers CMC, i-HEC kanye ne-HeECMC
Umthetho
3.2.4.3 Ukuhlolwa kwe-XD
I-X-RAY Ukuhlaziywa kokuhlaziywa kokuhlolwa kokuphakanyiswa kwama-celluLose Tathers CMC, i-HEC ne-HeECMC
indlela yokuhlola echaziwe.
3.2.4.4 Ukuhlolwa kwe-H-NMR
I-H NMR Spectrometer ye-HEC yakalwa nge-Avance400 h NMR Spectrometer ekhiqizwe nguBruker.
Usebenzisa i-Dimethyl Suutatedl Sulfoxide njenge-solvent, isixazululo sahlolwa yi-Spectroscopy ye-Liquid Hydrogen NMR. Imvamisa yokuhlola yayingu-75.5mhz.
Kufudumele, ikhambi lingu-0.5ml.
3.3 Imiphumela nokuhlaziywa
3.3.1 Ukusebenza kwenqubo yokulungiselela i-CMC
Kusetshenziswa i-Pine Cellulose ekhishwe esahlukweni sesibili njengento eluhlaza, futhi isebenzisa i-sodium chloropetate njenge-ejenti etheriving, indlela yokuhlolwa kwesici esisodwa,
Inqubo yokulungiselela ye-CMC yenziwa kahle, futhi okuguquguqukayo kokuqala kokuhlolwa kwathathwa njengoba kukhonjisiwe kuThebula 3.3. Okulandelayo inqubo yokulungiselela ye-HEC
Kwezobuciko, ukuhlaziywa kwezinto ezahlukahlukene.
Ithebula 3.3 Amanani Omqala Factor
Inani lokuqala
Ukwehla kokushisa okushisa / ℃ 40
Ukuhlekisa Ukuvumelanisa isikhathi / h 1
Isilinganiso esimanzi esiqinile / (G / ML) 1:25
Ukuhlukumezeka kwe-Pertyment Orne /% 40
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Isiteji sokuqala sokushisa / ℃ 45
Isikhathi sokuqala sokuthezeka / h 1
Isigaba sesibili sokushisa / ℃ 70
Isikhathi sesigaba sesibili / h 1
Umthamo wesisekelo esigabeni sokusheshisa / g 2
Inani le-ejenti etheratiset in etherification Stage / G 4.3
I-etherified soliquid ratio / (G / ML) 1:15
3.3.1.1 Ithonya lezinto ezahlukahlukene ku-CMC Ukufakwa esikhundleni se-CMC esiteji sokuhlekisa i-Alkalization
1. Umphumela wokushisa kokuphumula kokushisa kokushisa esikhundleni se-CMC
Ukuze ubheke umphumela wokushisa okuzenzakalelayo kwamazinga okushisa afinyelela esikhundleni sokufakwa esikhundleni se-CMC etholakele, esimweni sokulungisa ezinye izinto njengamanani okuqala,
Ngaphansi kwemibandela, umphumela wokushisa kwe-alkalization lokushisa ku-CMC Ukufakwa esikhundleni se-CMC kuyaxoxwa, futhi imiphumela ikhonjiswa ku-Fig.
Ukwehlisa izinga lokushisa / ℃
Umphumela Wokuhlehlisa Ukushisa Ukushisa kokufakwa esikhundleni se-CMC
Kungabonakala ukuthi izinga lokufaka esikhundleni se-CMC likhuphuka ngokunyuka kokushisa kwe-alkalization yokuphumula, kanti izinga lokushisa le-alkalization lingu-30 ° C.
Amazinga angenhla wokuncipha kokuncipha ngokushisa okwandayo. Lokhu kungenxa yokuthi izinga lokushisa le-alkalizing liphansi kakhulu, futhi ama-molecule awasebenzi kahle futhi awakwazi
Ukubhubhisa ngempumelelo indawo ye-crystalline ye-cellulose, okwenza kube nzima nge-ejenti etherishini yokungena ngaphakathi kwe-cellulose esiteji sokuthethelwa, futhi izinga lokuphendula liphezulu.
ephansi, okuholela ngezinga eliphansi lokufakwa esikhundleni komkhiqizo. Kodwa-ke, izinga lokushisa le-alkalization akufanele liphezulu kakhulu. Njengoba izinga lokushisa likhuphuka, ngaphansi kwesenzo sokushisa okuphezulu kanye ne-alkali eqinile,
I-cellulose ithambekele ekuwohlokeni kwe-oxidative, futhi izinga lokufaka esikhundleni somkhiqizo i-CMC liyancipha.
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Ngaphansi kwesimo sokushisa kwe-alkalization ye-alkalization uneminyaka engama-30 ° C kanti ezinye izinto zingamanani okuqala, umphumela wesikhathi sokuhlekisa ngesikhathi ku-CMC.
Umphumela wokufaka esikhundleni. Degree of inzuzo
Ukwehla kwe-alkaling isikhathi / h
Umphumela wesikhathi sokuhlekisa i-alkalishinization onCmUkufakwa esikhundleni
Inqubo enobuningi ngokwayo ishesha kakhulu, kepha isixazululo se-alkali sidinga isikhathi esithile sokuphazamiseka ku-fiber.
Kungabonakala ukuthi lapho isikhathi se-alkaliation singu-0.5-1.5h, isilinganiso sokufakwa komkhiqizo sikhuphuka ngokwanda kwesikhathi se-alkalization.
Izinga lokufaka esikhundleni somkhiqizo esitholwe laliphezulu kakhulu lapho isikhathi se-1.5h, futhi izinga lokufaka esikhundleni sehle ngokwanda kwesikhathi ngemuva kwe-1.5h. Lokhu kungakwenza
Kungaba yingoba ekuqaleni kwe-alkalization, ngokunwebeka kwesikhathi sokuhlangana, ukungena kwe-Alkali ku-cellulose kwanele ngokwenele, ukuze i-fiber
Isakhiwo esiyinhloko sivuseleleke ngokwengeziwe, sandisa i-ejenti etherishini kanye ne-medium esebenzayo
Isikhathi sePosi: Apr-26-2024