1 Intangiriro
Muri iki gihe, ibikoresho by'ingenzi bikoreshwa mu guteguraeteri ya seluloseni ipamba, kandi umusaruro wayo urimo kugabanuka, kandi igiciro nacyo kirimo kuzamuka;
Byongeye kandi, ibintu bikunze gukoreshwa nka aside chloroacetic (ifite uburozi bwinshi) na ethylene oxide (itera kanseri) na byo byangiza umubiri w'umuntu n'ibidukikije.
Muri iki gice, selulose ya pinusi ifite ubuziranenge burenze 90% ivanywe mu gice cya kabiri ikoreshwa nk'ibikoresho fatizo, naho sodium chloroacetate na 2-chloroethanol bikoreshwa nk'ibisimbura.
Gukoresha aside chloroacetic irimo uburozi bwinshi nk'ikintu gitanga uburozi, anionicselulose ya karboksimetili (CMC), hateguwe selulose idafite ionic hydroxyethyl cellulose.
Selulose (HEC) na selulose ivanze ya hydroxyethyl carboxymethyl (HECMC) ether eshatu za selulose. factor imwe
Uburyo bwo gutegura eteri eshatu za selulosi bwanogejwe binyuze mu bushakashatsi n'igerageza rya orthogonal, kandi eteri za selulosi zakozwe zaranzwe na FT-IR, XRD, H-NMR, nibindi.
Ibintu by'ibanze byo gukoresha etherification ya cellulose
Ihame rya etherification ya cellulose rishobora kugabanywamo ibice bibiri. Igice cya mbere ni inzira ya alkalize, ni ukuvuga, mu gihe cy'ihinduka rya alkalize rya cellulose,
Iyo ikwirakwijwe mu buryo butangana mu gisubizo cya NaOH, selulose ya pinusi irabyimba cyane bitewe n'ibikorwa byo gukangura ibyuma, kandi amazi akagenda akura.
Ingano nini ya NaOH yinjiye mu gice cy’imbere cya selulose ya pinusi, maze ikora hamwe n’amatsinda ya hydroxyl ku ruziga rw’imiterere ya glucose,
Ikora selulose ya alkali, ikigo gikora mu gukora etherification.
Igice cya kabiri ni inzira yo gukwirakwiza ether, ni ukuvuga, uburyo hagati y’aho ikigo gikora na sodium chloroacetate cyangwa 2-chloroethanol mu gihe cy’imiterere ya alkaline, bigatuma
Muri icyo gihe, ikintu gitera ubushyuhe cya sodium chloroacetate na 2-chloroethanol nabyo bizakora amazi mu gihe cy’amazi afite alkaline.
Ingaruka mbi ziboneka mu gukora sodium glycolate na ethylene glycol.
2 Gutegura mbere yo gukoresha selulose ya pinusi hakoreshejwe alkali nyinshi
Ubwa mbere, tegura urugero runaka rwa NaOH ukoresheje amazi yakuwemo iyoni. Hanyuma, ku bushyuhe runaka, 2g ya fibre ya pinusi
Vitamine ishongeshwa mu gipimo runaka cya NaOH, ikavungagurwa igihe runaka, hanyuma ikayungururwa kugira ngo ikoreshwe.
Uruganda rw'Icyitegererezo cy'Ibikoresho
Igipimo cya pH cy'ubuziranenge
Igikoresho gishyushya ubushyuhe buhoraho gikoresha ikoranabuhanga rya magnetic stirrer
Ifuru yumisha icyuma gikoresha umwuka
Ingano y'ikoranabuhanga
Pompe y'amazi azunguruka ifite imikorere myinshi
Spektrometero ya Fourier Transform Infrared
Igipimo cy'urumuri rw'amabara ya X-ray
Spektrometero y'ihumure rya magnetic resonance
Hangzhou Aolilong Instrument Co., Ltd.
Hangzhou Huichuang Instrument Equipment Co., Ltd.
Shanghai Jinghong Experimental Equipment Co., Ltd.
Mettler TOLEDO Instruments (Shanghai) Co., Ltd.
Hangzhou David Science and Education Instrument Co., Ltd.
Thermo Fisher Co., Ltd y'Abanyamerika
Isosiyete y'Abanyamerika ishinzwe ikoranabuhanga rya Thermoelectric mu Busuwisi (ARL)
Ikigo cy'Ubusuwisi cyitwa BRUKER
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Gutegura CMCs
Gukoresha alkali cellulose yo mu giti cya pinusi yavuwe mbere hakoreshejwe alkali decrystallization nk'ibikoresho fatizo, gukoresha ethanol nk'umusemburo na sodium chloroacetate nk'umusemburo wa etherification
CMC ifite DS nyinshi yateguwe hakoreshejwe alkali kabiri n'umuti utanga etherifying kabiri. Shyira garama 2 za cellulose ya alkali yo mu giti cya pinusi mu icupa rifite ijosi enye, hanyuma ushyiremo ingano runaka ya ethanol solvent, hanyuma uvange neza mu minota 30.
hafi, kugira ngo selulose ya alkali ikwirakwizwe neza. Hanyuma ongeramo ingano runaka ya alkali na sodium chloroacetate kugira ngo bikore mu gihe runaka ku bushyuhe runaka bwa etherification.
Nyuma y'igihe, hongerwamo kabiri alkaline agent na sodium chloroacetate hanyuma hagakurikiraho etherification mu gihe runaka. Nyuma y'uko reaction irangiye, komeza ukonje hanyuma ukonje, hanyuma
Shyiramo aside acetic y'ibara ry'umukara uhagije, hanyuma uyungurure, woge hanyuma wumishe.
Gutegura HECs
Gukoresha selulosi ya alkali yo mu giti cya pinusi yavuwe mbere hakoreshejwe decrystallization ya alkali ikomeye nk'ibikoresho fatizo, ethanol nk'umusemburo na 2-chloroethanol nk'umusemburo wa etherification
HEC ifite MS iri hejuru yateguwe hakoreshejwe alkali kabiri n'umusemburo wo gushyushya kabiri. Shyira garama 2 za cellulose ya alkali yo mu giti cya pinusi mu icupa rifite ijosi rinini, hanyuma wongeremo ingano runaka ya 90% (igice cy'ingano) ya ethanol, uvange.
Kangura igihe runaka kugira ngo ushire neza, hanyuma wongereho urugero runaka rwa alkali, hanyuma ushyushye buhoro buhoro, wongereho urugero runaka rwa 2-
Chloroethanol, yahinduwe ishyushye ku bushyuhe budahinduka mu gihe runaka, hanyuma yongeramo sodium hydroxide isigaye na 2-chloroethanol kugira ngo ikomeze gushyushya mu gihe runaka.
Nyuma y’uko igikorwa kirangiye, shyiramo ingano runaka ya aside asetiki y’urubura, hanyuma uyungurure ukoresheje akayunguruzo k’ikirahure (G3), oza, hanyuma wumishe.
Itegurwa rya HEMCC
Gukoresha HEC yateguwe muri 3.2.3.4 nk'ibikoresho fatizo, ethanol nk'uburyo bwo gusubiza, na sodium chloroacetate nk'ikintu gitanga ubushyuhe mu gutegura
HECMC. Uburyo bwihariye ni ubu: gufata ingano runaka ya HEC, uyishyire mu icupa rifite imililitiro 100, hanyuma wongeremo ingano runaka y'ingano
90% ya etanoli, uvange mu buryo bw'ikoranabuhanga mu gihe runaka kugira ngo ikwirakwizwe neza, ongeramo ingano runaka ya alkali nyuma yo gushyushya, hanyuma ushyiremo buhoro buhoro
Sodium chloroacetate, etherification ku bushyuhe budahinduka irangira nyuma y'igihe runaka. Nyuma y'uko reaction irangiye, shyiramo aside glacial acetic kugira ngo uyikuremo, hanyuma ukoreshe akayunguruzo k'ikirahure (G3)
Nyuma yo kuyungurura, gukaraba no kumisha.
Gutunganya eteri za selulose
Mu gutegura eteri ya selulosi, hari ibintu bimwe na bimwe bikunze gukorwa, cyane cyane umunyu utari uw’umwimerere wa sodium chloride n’ibindi
imyanda. Kugira ngo hongerwe ubwiza bwa eteri ya selulosi, hakozwe isuku yoroshye kuri eteri ya selulosi yabonetse. kuko iri mu mazi
Hari uburyo butandukanye bwo gushonga, bityo igerageza rikoresha igice runaka cya ethanol yuzuye amazi kugira ngo risukure eteri eshatu za selulosi zateguwe.
impinduka.
Shyira icyitegererezo cya eteri ya selulosi yateguwe ifite ubuziranenge runaka mu gikombe, ongeramo ingano runaka ya ethanol ya 80% yashyushye kugeza kuri 60 ℃ ~ 65 ℃, kandi ukomeze gukangura hakoreshejwe ikoranabuhanga kuri 60 ℃ ~ 65 ℃ ku gikoresho gishyushya magnetic stirrer mu gihe cy'iminota 10 ℃. Fata supernatant kugira ngo yumuke.
Mu gikombe gisukuye, koresha nitrati y'ifeza kugira ngo urebe niba hari iyoni za chloride. Niba hari akantu k'umweru gahari, kayungurure unyuze mu kayunguruzo k'ikirahure hanyuma ufate ikintu gikomeye
Subiramo intambwe zabanje ku gice cy'umubiri, kugeza igihe akayunguruzo nyuma yo kongeramo igitonyanga 1 cy'umuti wa AgNO3 kadafite amazi yera, ni ukuvuga ko gusukura no gukaraba birangiye.
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mu (cyane cyane kugira ngo ukureho NaCl ikomoka ku bimera). Nyuma yo gukurura, kumisha, gukonjesha kugeza ku bushyuhe bw'icyumba no gupima.
uburemere, g.
Uburyo bwo gupima no kugaragaza imiterere ya eteri za selulosi
Kugena Impamyabumenyi yo Gusimbuza (DS) n'Impamyabumenyi yo Gusimbuza (MS)
Kumenya DS: Ubwa mbere, pima 0.2 g (kuri 0.1 mg) y'icyitegererezo cya cellulose ether cyasukuwe kandi cyumye, hanyuma ugishongeshe mu
80ml z'amazi yaciwe, ubyuke mu bwogero bw'amazi buri ku bushyuhe buhoraho kuri 30℃ ~ 40℃ mu gihe cy'iminota 10. Hanyuma ushyireho umuti wa aside sulfurike cyangwa umuti wa NaOH
pH y'umuti kugeza igihe pH y'umuti igeze kuri 8. Hanyuma mu gikoresho gifite electrode ya pH, koresha umuti usanzwe wa aside sulfuriki
Kugira ngo umenye neza, mu gihe cyo gukangura, reba igipimo cya pH mu gihe upima, iyo agaciro ka pH k'umuti kahinduwe kagera kuri 3.74,
Ingano y'umuti usanzwe wa aside sulfuriki irarangira. Reba ingano y'umuti usanzwe wa aside sulfuriki ukoreshwa muri iki gihe.
Inkomoko:
Igiteranyo cy'imibare ya protoni yo hejuru n'itsinda rya hydroxyethyl
Igipimo cy'umubare wa protoni zo hejuru; I7 ni uburemere bw'itsinda rya methylene riri mu itsinda rya hydroxyethyl
Ubukana bw'agace ka proton resonance; ni ubukana bw'agace ka proton resonance k'amatsinda 5 ya methine n'itsinda rimwe rya methylene ku gice cya glucose ya cellulose
Igiteranyo.
Uburyo bwo gupima bwasobanuwe mu gupima imiterere ya infrared ya ether eshatu za cellulose CMC, HEC na HEECMC
Amategeko
3.2.4.3 Ikizamini cya XRD
Isuzuma ry'imiterere y'isesengura rya X-ray rya Ether eshatu za Cellulose CMC, HEC na HEECMC
uburyo bwo gupima bwasobanuwe.
3.2.4.4 Isuzuma rya H-NMR
Spektrometero ya H NMR ya HEC yapimwe na spectrometero ya Avance400 H NMR yakozwe na BRUKER.
Hakoreshejwe dimethyl sulfoxide ya deuterated nk'umusemburo, umuti wapimwe hakoreshejwe spectroscopy y'amazi ya hydrogen NMR. Ingano y'igerageza yari 75.5MHz.
Ubushyuhe, umuti ni 0.5mL.
3.3 Ibisubizo n'isesengura
3.3.1 Kunoza gahunda yo gutegura CMC
Hakoreshejwe selulose ya pinusi yakuwe mu gice cya kabiri nk'ibikoresho fatizo, no gukoresha sodium chloroacetate nk'ikintu gitanga ubushyuhe, uburyo bwo gukora igerageza rya single factor bwakoreshejwe,
Uburyo bwo gutegura CMC bwaranogejwe, kandi ibipimo bya mbere by'igerageza byashyizweho nk'uko bigaragara mu mbonerahamwe ya 3.3. Ibi bikurikira ni uburyo bwo gutegura HEC
Mu buhanzi, isesengura ry'ibintu bitandukanye.
Imbonerahamwe 3.3 Ingano y'Ibintu Bibanza
Agaciro k'ibanze k'ikintu
Ubushyuhe bwo gusukura mbere yo kuvura alkalizing/℃ 40
Igihe cyo kuvura mbere yo gukoresha alkalizing/h 1
Igipimo cy'amazi akomeye mbere yo kuyavura/(g/mL) 1:25
Igipimo cya lye mbere yo kuvurwa/% 40
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Ubushyuhe bwa etherification bw'icyiciro cya mbere / ℃ 45
Igihe cyo gupima ether mu cyiciro cya mbere/isaha 1
Ubushyuhe bwa etherification yo mu cyiciro cya kabiri / ℃ 70
Igihe cyo gupima ether mu cyiciro cya kabiri / isaha 1
Igipimo cy'ibanze mu cyiciro cya etherification / g 2
Ingano y'ibikoresho bitanga ubushyuhe mu cyiciro cya etherification / g 4.3
Igipimo cy'amazi akomeye n'afite etherized/(g/mL) 1:15
3.3.1.1 Ingaruka z'ibintu bitandukanye ku gipimo cyo gusimbuza CMC mu cyiciro cyo gusimbuza alkali mbere yo kuvurwa
1. Ingaruka z'ubushyuhe bwa alkalizing mbere yo kuvurwa ku gipimo cyo gusimbuza CMC
Kugira ngo harebwe ingaruka z'ubushyuhe bwa alkalisation mbere yo kuvurwa ku rugero rwo gusimbuza muri CMC yabonetse, mu gihe hashyirwaho ibindi bintu nk'agaciro k'ibanze,
Muri ibi bihe, ingaruka z'ubushyuhe bwa alkalizing mbere yo kuvurwa ku gipimo cyo gusimbuza CMC ziraganirwaho, kandi ibisubizo bigaragazwa ku ishusho.
Ubushyuhe bwo gusukura bwa alkalizing mbere yo kuvurwa/℃
Ingaruka z'ubushyuhe bwa alkalizing mbere yo kuvurwa ku gipimo cyo gusimbuza CMC
Bigaragara ko urugero rwo gusimbuza CMC rwiyongera uko ubushyuhe bwa alkalizasiyo buzamuka mbere yo kuvurwa, kandi ubushyuhe bwa alkalizasiyo bukaba 30 °C.
Ibipimo byavuzwe haruguru byo gusimbuza bigabanuka uko ubushyuhe bwiyongera. Ibi biterwa nuko ubushyuhe bwa alkalizing buba buri hasi cyane, kandi molekile ntizikora cyane kandi ntizishobora
Senya neza agace ka kristu ka cellulose, bigatuma bigora igikoresho gitanga ubushyuhe kwinjira imbere muri cellulose mu cyiciro cya etherification, kandi urwego rw'imyitwarire rugaragara cyane.
hasi, bigatuma habaho igipimo gito cyo gusimbuza ibicuruzwa. Ariko, ubushyuhe bwa alkali ntibugomba kuba buri hejuru cyane. Uko ubushyuhe bwiyongera, bitewe n'ubushyuhe bwinshi n'alkali ikomeye,
Selulosi ikunze kwangirika mu buryo bwa oxidative, kandi urwego rwo gusimbuza CMC rugabanuka.
2. Ingaruka z'igihe cyo gushyira alkali mu bikorwa mbere yo kuvurwa ku gipimo cyo gusimbuza CMC
Mu gihe ubushyuhe bwa alkalize yo mu gihe cyo kuvurwa ari 30 °C n'ibindi bintu ari byo bipimo by'ibanze, ingaruka z'igihe cyo kuvurwa kuri CMC ziraganirwaho.
Ingaruka zo gusimbuza. Ingano yo gusimbuza
Igihe cyo kuvura mbere yo gukoresha alkali/isaha
Ingaruka zo gukoresha alkalis mbere yo kuvurwa ku giheCMCimpamyabumenyi yo gusimbuza
Uburyo bwo gukusanya ubwabwo bwihuta cyane, ariko umuti wa alkali ukeneye igihe runaka cyo gukwirakwira muri fibre.
Bigaragara ko iyo igihe cyo gusimbuza amazi ari amasaha 0.5-1.5, igipimo cyo gusimbuza amazi kiriyongera uko igihe cyo gusimbuza amazi cyiyongera.
Igipimo cyo gusimbuza ibicuruzwa cyabonetse cyari cyo hejuru cyane iyo igihe cyari isaha 1.5, kandi igipimo cyo gusimbuza cyaragabanutse uko igihe cyo kwiyongera nyuma y'isaha 1.5. Ibi bishobora
Bishobora kuba biterwa nuko mu ntangiriro yo kongera igihe cyo kongera kwiyongera kwa alkali, kwinjira kwa alkali muri selulose biba bihagije, ku buryo fibre
Imiterere y'ibanze irushaho koroherwa, bigatuma umwuka urushaho gushyuha n'uburyo bwo gukora ibintu
Igihe cyo kohereza: 26 Mata 2024