1 Selelekela
Hona jwale, thepa e tala e ka sehloohong e sebediswang ho lokisengether ea seluloseke k'hothone, 'me tlhahiso ea eona ea theoha, 'me theko le eona ea nyoloha;
Ho feta moo, lintho tse atisang ho sebelisoa tse kang chloroacetic acid (e chefo haholo) le ethylene oxide (e bakang kankere) le tsona li kotsi haholo 'meleng oa motho le tikolohong.
Khaolong ena, cellulose ea phaene e nang le bohloeki bo fetang 90% bo ntšitsoeng khaolong ea bobeli e sebelisoa e le thepa e tala, 'me sodium chloroacetate le 2-chloroethanol li sebelisoa e le lintho tse nkelang sebaka.
Ho sebelisa chloroacetic acid e chefo haholo e le moemeli oa ho etherifying, anionicselulose ea carboxymethyl (CMC), ho ile ha lokiswa selulose ya hydroxyethyl e seng ionic.
Cellulose (HEC) le hydroxyethyl carboxymethyl cellulose e tsoakiloeng (HECMC) li-ether tse tharo tsa cellulose. ntlha e le 'ngoe
Mekhoa ea ho lokisa li-ether tse tharo tsa cellulose e ntlafalitsoe ka liteko le liteko tsa orthogonal, 'me li-ether tsa cellulose tse entsoeng ka maiketsetso li ne li khetholloa ka FT-IR, XRD, H-NMR, jj.
Metheo ea etherification ea cellulose
Molao-motheo oa etherification ea cellulose o ka aroloa likarolo tse peli. Karolo ea pele ke ts'ebetso ea alkalization, ke hore, nakong ea karabelo ea alkalization ea cellulose,
Ha e qhalakantsoe ka ho lekana ka tharollong ea NaOH, cellulose ea phaene e ruruha ka matla tlas'a ts'ebetso ea ho hlohlelletsa ka mechine, le ka katoloso ea metsi
Palo e kholo ea limolek'hule tse nyane tsa NaOH li ile tsa kenella ka hare ho cellulose ea phaene, 'me tsa arabela le lihlopha tsa hydroxyl selikalikoeng sa yuniti ea sebopeho sa tsoekere,
E hlahisa alkali cellulose, setsi se sebetsang sa karabelo ea etherification.
Karolo ea bobeli ke ts'ebetso ea etherification, ke hore, karabelo pakeng tsa setsi se sebetsang le sodium chloroacetate kapa 2-chloroethanol tlas'a maemo a alkaline, e leng se fellang ka
Ka nako e ts'oanang, sesebelisoa sa ho futhumatsa sa sodium chloroacetate le 2-chloroethanol le tsona li tla hlahisa tekanyo e itseng ea metsi tlas'a maemo a alkaline.
Likarabelo tse ka thoko li rarolloa ho hlahisa sodium glycolate le ethylene glycol, ka ho latellana.
2 Phekolo ea pele ea cellulose ea phaene e nang le alkali e tebileng
Taba ea pele, lokisa motsoako o itseng oa tharollo ea NaOH ka metsi a hloekisitsoeng. Ebe, mochesong o itseng, 2g ea faeba ea phaene
Vithamine e qhibiliha ka bongata bo itseng ba tharollo ea NaOH, e hlohlelletsoa ka nako e itseng, ebe e sefshoa bakeng sa tšebeliso.
Moetsi oa Mohlala oa Lisebelisoa
Methara ea pH e nepahetseng
Moqokeleli oa mofuta oa kamehla oa mocheso o futhumatsang motlakase o tsosang takatso
Onto ea ho omisa ka vacuum
Tekanyo ea elektroniki
Pompo ea vacuum e potolohang ea mofuta oa metsi a mangata
Spectrometer ea Infrared ea Phetoho ea Fourier
Sesupa-tsela sa X-ray
Spektrometara ea Resonance ea Magnetic ea Nyutlelie
Hangzhou Aolilong Instrument Co., Ltd.
Hangzhou Huichuang Lisebelisoa tsa Lisebelisoa Co., Ltd.
Shanghai Jinghong Lisebelisoa tsa Teko Co., Ltd.
Mettler TOLEDO Instruments (Shanghai) Co., Ltd.
Hangzhou David Saense le Thuto ea Lisebelisoa tsa Sesebelisoa. Co., Ltd.
Thermo Fisher ea Amerika Co., Ltd.
Khamphani ea American Thermoelectric Switzerland ARL
Khamphani ea Switzerland ea BRUKER
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Tokisetso ea CMCs
Ho sebelisa alkali cellulose ea lehong la phaene e phekotsoeng esale pele ka ho tlosa likristale tse matla tsa alkali e le thepa e tala, ho sebelisoa ethanol e le solvent le ho sebelisa sodium chloroacetate e le etherification
CMC e nang le DS e phahameng e lokisitsoe ka ho eketsa alkali habeli le moemeli oa ho etherifying habeli. Kenya 2g ea alkali cellulose ea patsi ea phaene ka har'a flask e nang le melala e mene, ebe u eketsa bophahamo bo itseng ba ethanol solvent, 'me u hlohlelletse hantle metsotso e 30.
hoo e ka bang, e le hore alkali cellulose e hasane ka botlalo. Ebe o eketsa tekanyo e itseng ea alkali agent le sodium chloroacetate ho arabela ka nako e itseng mochesong o itseng oa etherification.
Kamora nako, ho eketsoa ha alkaline agent le sodium chloroacetate ka lekhetlo la bobeli ho lateloe ke etherification ka nako e itseng. Kamora hore karabelo e fele, e pholise 'me u pholise, ebe
Hlatsoa ka tekanyo e loketseng ea glacial acetic acid, ebe u sefa, u hlatsoe ebe u omisa.
Tokisetso ea HECs
Ho sebelisa alkali cellulose ea patsi ea phaene e phekotsoeng esale pele ka decrystallization e matla ea alkali e le thepa e tala, ethanol e le solvent le 2-chloroethanol e le etherification
HEC e nang le MS e phahameng e lokisitsoe ka ho eketsa alkali habeli le moemeli oa ho etherifying habeli. Kenya 2g ea alkali cellulose ea patsi ea phaene ka har'a flask e nang le melala e mene, 'me u kenye molumo o itseng oa 90% (karolo ea bophahamo), u hlohlelletse.
Hlohlelletsa nako e itseng ho hasana ka botlalo, ebe o eketsa alkali e itseng, ebe o futhumatsa butle-butle, eketsa bophahamo bo itseng ba 2-
Chloroethanol, e qhibilihisoa mochesong o sa fetoheng ka nako e itseng, ebe e eketsa sodium hydroxide e setseng le 2-chloroethanol ho tswela pele ho qhibilihisa mocheso ka nako e itseng.
Kamora hore karabelo e phetheloe, e ntlafatse ka tekanyo e itseng ea glacial acetic acid, 'me qetellong u e hloekise ka khalase ea sefe (G3), u e hlatsoe, 'me u e omise.
Tokisetso ea HEMCC
Ho sebelisa HEC e lokisitsoeng ho 3.2.3.4 e le thepa e tala, ethanol e le mokhoa oa karabelo, le sodium chloroacetate e le moemeli oa ho futhumatsa ho lokisa
HECMC. Ts'ebetso e tobileng ke ena: nka HEC e itseng, u e kenye ka har'a botlolo e nang le melala e mene ea 100 mL, ebe u eketsa bophahamo bo itseng.
90% ea ethanol, hlohlelletsa ka mechine nako e itseng ho e qhalanya ka botlalo, eketsa alkali e itseng ka mor'a ho futhumatsa, 'me u e kenye butle-butle.
Sodium chloroacetate, etherification mochesong o sa fetoheng e fela ka mor'a nako e itseng. Kamora hore karabelo e phetheloe, e ntlafatse ka glacial acetic acid ho e ntlafatsa, ebe o sebelisa sefe sa khalase (G3).
Kamora ho sefa, ho hlatsoa le ho omisa.
Ho hlwekisa di-ether tsa selulose
Ts'ebetsong ea ho lokisa ether ea cellulose, lihlahisoa tse ling tse tsoang ho eona hangata li hlahisoa, haholo-holo letsoai le sa tloaelehang la sodium chloride le tse ling.
litšila. E le ho ntlafatsa boleng ba ether ea cellulose, ho ile ha etsoa tlhoekiso e bonolo holim'a ether ea cellulose e fumanoeng. hobane li ka metsing
Ho na le ho qhibiliha ho fapaneng, kahoo teko e sebedisa karolo e itseng ya volume ya ethanol e nang le metsi ho hlwekisa di-ether tse tharo tsa cellulose tse lokisitsweng.
phetoho.
Beha sampole ea ether ea cellulose e lokisitsoeng ka boleng bo itseng ka beaker, eketsa tekanyo e itseng ea 80% ethanol e seng e chesitsoe ho fihlela ho 60 ℃ ~ 65 ℃, 'me u boloke ho hlohlelletsa ka mechine ho 60 ℃ ~ 65 ℃ holim'a stirrer ea makenete e futhumatsang mocheso o sa fetoheng bakeng sa 10 ℃. Metsotso. Nka supernatant ho omisa.
Ka beaker e hloekileng, sebelisa silver nitrate ho hlahloba li-ion tsa chloride. Haeba ho na le letheba le lesoeu, le sefe ka sefe ea khalase ebe u nka se tiileng
Pheta mehato e fetileng bakeng sa karolo ea 'mele, ho fihlela sefaha ka mor'a ho eketsa lerotholi le le leng la tharollo ea AgNO3 se se na matheba a masoeu, ke hore, tlhoekiso le ho hlatsoa li phethiloe.
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ka hare (haholo-holo ho tlosa karabelo e tsoang ho NaCl). Kamora ho sefa, ho omisa, ho phodisa mochesong wa kamore le ho bekha.
boima, g.
Mekhoa ea Teko le Tlhahlobo ea Litšobotsi bakeng sa Li-Ether tsa Cellulose
Ho Fumana Tekanyo ea Tekanyo ea Phetolo (DS) le Tekanyo ea Molar ea Phetolo (MS)
Ho fumana DS: Taba ea pele, bekha 0.2 g (e nepahetseng ho isa ho 0.1 mg) ea sampole ea ether ea cellulose e hloekisitsoeng le e omisitsoeng, ebe u e qhala ka har'a
80mL ea metsi a hloekisitsoeng, a hlohlelletsoe ka bateng ea metsi e futhumetseng e sa fetoheng ho 30℃ ~ 40℃ metsotso e 10. Ebe u lokisa ka tharollo ea sulfuric acid kapa tharollo ea NaOH
pH ea tharollo ho fihlela pH ea tharollo e le 8. Ebe ka beaker e nang le electrode ea pH meter, sebelisa tharollo e tloaelehileng ea sulfuric acid
Ho lekanya ka titration, tlasa maemo a ho hlohlelletsa, shebella ho bala ha pH meter ha o ntse o lekanya ka titration, ha boleng ba pH ba tharollo bo fetoloa ho 3.74,
Titration e fela. Hlokomela bophahamo ba tharollo e tloaelehileng ea sulfuric acid e sebelisoang nakong ena.
Moloko:
Kakaretso ea linomoro tsa proton tse holimo le sehlopha sa hydroxyethyl
Karolelano ea palo ea liprothone tse ka holimo; I7 ke boima ba sehlopha sa methylene sehlopheng sa hydroxyethyl
Matla a tlhoro ea resonance ea proton; ke matla a tlhoro ea resonance ea proton ea lihlopha tse 5 tsa methine le sehlopha se le seng sa methylene holim'a yuniti ea glucose ea cellulose
Kakaretso.
Mekhoa ea teko e hlalositsoeng bakeng sa teko ea tlhaloso ea infrared ea li-ether tse tharo tsa cellulose CMC, HEC le HEECMC
Molao
3.2.4.3 Teko ea XRD
Teko ea ho Hlalosa Litšobotsi tsa Tlhahlobo ea Phapang ea X-ray ea Li-Ether tse Tharo tsa Cellulose CMC, HEC le HEECMC
mokhoa oa teko o hlalositsoeng.
3.2.4.4 Teko ea H-NMR
Spektrometara ea H NMR ea HEC e lekantsoe ka spectrometara ea Avance400 H NMR e hlahisitsoeng ke BRUKER.
Ka ho sebelisa deuterated dimethyl sulfoxide e le solvent, tharollo e ile ea lekoa ka liquid hydrogen NMR spectroscopy. Maqhubu a teko e ne e le 75.5MHz.
Mofuthu, tharollo ke 0.5mL.
3.3 Liphetho le Tlhahlobo
3.3.1 Ntlafatso ea ts'ebetso ea ho lokisa CMC
Ka ho sebedisa cellulose ya phaene e ntshitsweng kgaolong ya bobedi e le thepa e tala, le ka ho sebedisa sodium chloroacetate e le moemedi wa ho tjhesa, mokgwa wa teko ya ntlha e le nngwe o ile wa amohelwa,
Ts'ebetso ea ho lokisa CMC e ntlafalitsoe, 'me liphetoho tsa pele tsa teko li behiloe joalo ka ha ho bontšitsoe ho Tafole ea 3.3. Se latelang ke ts'ebetso ea ho lokisa HEC
Ho tsa bonono, tlhahlobo ea lintlha tse fapaneng.
Tafole 3.3 Boleng ba Ntlha ea Pele
Boleng ba qalong ba ntlha
Mocheso oa alkalizing oa pele ho kalafo/℃ 40
Nako ea ho lokisa alkali pele ho kalafo/h 1
Karolelano ea metsi a tiileng pele ho kalafo/(g/mL) 1:25
Khakanyo ea lye pele ho kalafo/% 40
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Mocheso oa etherification oa mohato oa pele/℃ 45
Nako ea ho kenya etherification ea mohato oa pele/h 1
Mocheso oa etherification oa mohato oa bobeli/℃ 70
Nako ea ho kenya etherification ea mohato oa bobeli/h 1
Tekanyo ea motheo mohatong oa etherification/g 2
Palo ea moemeli ea etherifying mohatong oa etherification/g 4.3
Karolelano ea metsi a tiileng a nang le etherified/(g/mL) 1:15
3.3.1.1 Tšusumetso ea lintlha tse fapaneng tekanyong ea phetolo ea CMC mohatong oa alkalization ea pele ho kalafo
1. Phello ea mocheso oa alkalization oa pele ho kalafo holim'a tekanyo ea phetolo ea CMC
E le ho nahana ka phello ea mocheso oa alkalization oa pele ho kalafo tekanyong ea ho nkeloa sebaka ho CMC e fumanoeng, tabeng ea ho lokisa lintlha tse ling e le litekanyetso tsa pele,
Tlas'a maemo ana, phello ea mocheso oa alkalization oa pele ho kalafo ho tekanyo ea phetoho ea CMC ea tšohloa, 'me liphetho li bontšitsoe ho Setšoantšo.
Mocheso oa alkalizing oa pele ho kalafo/℃
Phello ea mocheso oa alkalizing oa pele ho kalafo ho tekanyo ea phetolo ea CMC
Ho ka bonoa hore tekanyo ea ho nkeloa sebaka ha CMC e eketseha ka keketseho ea mocheso oa alkalization ea pele ho kalafo, 'me mocheso oa alkalization ke 30 °C.
Dikhato tse ka hodimo tsa ho nkela sebaka di a fokotseha ha mocheso o ntse o eketseha. Lebaka ke hobane mocheso wa alkalizing o tlase haholo, mme dimolek'hule ha di sebetse hantle mme ha di kgone ho
Senya sebaka sa kristale sa cellulose ka katleho, e leng se etsang hore ho be thata hore moemeli ea futhumatsang a kene kahare ho cellulose mohatong oa etherification, 'me tekanyo ea karabelo e phahame haholo.
e tlase, e leng se fellang ka tekanyo e tlase ea ho nkeloa sebaka ha sehlahisoa. Leha ho le joalo, mocheso oa alkali ha oa lokela ho ba holimo haholo. Ha mocheso o ntse o eketseha, tlas'a tšusumetso ea mocheso o phahameng le alkali e matla,
Cellulose e sekametse ho senyeha ha oxidative, 'me tekanyo ea ho nkeloa sebaka ha sehlahisoa sa CMC ea fokotseha.
2. Tšusumetso ea nako ea alkaline pele ho kalafo tekanyong ea phetolo ea CMC
Tlas'a boemo ba hore mocheso oa alkalization ea pele ho kalafo ke 30 °C 'me lintlha tse ling ke boleng ba pele, phello ea nako ea alkalization ea pele ho phekolo ho CMC e tšohloa.
Phello ea ho nkela sebaka. Tekanyo ea ho nkela sebaka
Nako ea ho lokisa alkali pele ho kalafo/h
Phello ea nako ea alkaline pele ho kalafo e qalaCMCtekanyo ea ho nkela sebaka
Ts'ebetso ea ho bokellana ka boeona e potlakile haholo, empa tharollo ea alkali e hloka nako e itseng ea ho hasana ka har'a fiber.
Ho ka bonoa hore ha nako ea alkalization e le lihora tse 0.5-1.5, tekanyo ea ho nkeloa sebaka ha sehlahisoa e eketseha ka keketseho ea nako ea alkalization.
Tekanyo ea ho nkeloa sebaka ha sehlahisoa e fumanoeng e ne e le e phahameng ka ho fetisisa ha nako e ne e le 1.5h, 'me tekanyo ea ho nkeloa sebaka e ile ea fokotseha ha nako e ntse e eketseha ka mor'a 1.5h. Sena se ka
E ka ’na eaba ke hobane qalong ea alkalization, ka nako ea alkalization e ntseng e eketseha, ho kenella ha alkali ho cellulose ho lekane, hoo fiber e leng teng.
Sebopeho sa mantlha se phutholohile haholoanyane, se eketsa ntho e futhumatsang le sebaka se sebetsang.
Nako ea poso: Mmesa-26-2024