1 Intangiriro
Kugeza ubu, ibikoresho nyamukuru bikoreshwa muguteguraselile etherni ipamba, kandi umusaruro wacyo uragabanuka, kandi igiciro nacyo kizamuka;
Byongeye kandi, imiti ikoreshwa cyane nka aside ya chloroacetike (uburozi bukabije) na okiside ya Ethylene (kanseri) nayo yangiza umubiri wumuntu nibidukikije. Igitabo
Muri iki gice, pine selulose ifite isuku igereranije irenga 90% yakuwe mu gice cya kabiri ikoreshwa nkibikoresho fatizo, naho sodium chloroacetate na 2-chloroethanol ikoreshwa nkibisimburwa.
Gukoresha aside irike cyane ya chloroacetike nka etherifying agent, anioniccarboxymethyl selulose (CMC), hydroxyethyl selulose itari ionic yarateguwe.
Cellulose (HEC) hamwe na hydroxyethyl carboxymethyl selulose (HECMC) ether eshatu za selile. ikintu kimwe
Ubuhanga bwo gutegura ether eshatu za selile zashyizwe mubikorwa hakoreshejwe ubushakashatsi nubushakashatsi bwa orthogonal, kandi ethes ya selile ya selile yaranzwe na FT-IR, XRD, H-NMR, nibindi.
Shingiro rya selulose etherification
Ihame rya selulose etherification irashobora kugabanywamo ibice bibiri. Igice cya mbere ni inzira ya alkalisation, ni ukuvuga, mugihe cya alkalisation reaction ya selile,
Ikwirakwijwe neza mu gisubizo cya NaOH, pine selulose irabyimba cyane bitewe no gukanika imashini, hamwe no kwaguka kwamazi
Umubare munini wa molekile ntoya ya NaOH yinjiye imbere muri selile ya pinusi, hanyuma ikorana nitsinda rya hydroxyl kumpeta yikigo cyubaka glucose,
Bibyara alkali selile, ikigo gikora cya etherification reaction.
Igice cya kabiri ni inzira ya etherification, ni ukuvuga, reaction hagati yikigo gikora na sodium chloroacetate cyangwa 2-chloroethanol mubihe bya alkaline, bikavamo
Muri icyo gihe, agent ya etherifying sodium chloroacetate na 2-chloroethanol nayo izatanga amazi runaka mugihe cya alkaline.
Imyitwarire yo kuruhande yiyemeje kubyara sodium glycolate na Ethylene glycol.
2 Kwibanda kuri alkali decrystallisation ya pine selile
Ubwa mbere, tegura ubunini bwumuti wa NaOH hamwe namazi ya deionion. Hanyuma, ku bushyuhe runaka, 2g ya fibre fibre
Vitamine ishonga mubunini runaka bwumuti wa NaOH, ikabikwa mugihe runaka, hanyuma ikayungurura kugirango ikoreshwe.
Ibikoresho by'icyitegererezo
Uburebure bwa pH
Ubwoko bw'abakusanya burigihe ubushyuhe bushyushya magnetiki stirrer
Ifuru yumisha
Impirimbanyi ya elegitoroniki
Kuzenguruka ubwoko bwamazi menshi-pompe vacuum
Fourier Guhindura Infrared Spectrometer
X-ray itandukanya
Nuclear Magnetic Resonance Spectrometer
Hangzhou Aolilong Instrument Co., Ltd.
Hangzhou Huichuang Ibikoresho Byuma Co, Ltd.
Shanghai Jinghong Ibikoresho Byubushakashatsi Co, Ltd.
METTLER TOLEDO Ibikoresho (Shanghai) Co, Ltd.
Hangzhou David Science and Education Instrument Co., Ltd.
Abanyamerika Thermo Fisher Co., Ltd.
Isosiyete y'Abanyamerika ya Thermoelectric Ubusuwisi ARL
Isosiyete yo mu Busuwisi BRUKER
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Gutegura CMC
Gukoresha ibiti bya pinusi alkali selulose yateguwe na alkali decrystallisation yibikoresho nkibikoresho fatizo, ukoresheje Ethanol nkumuti kandi ugakoresha sodium chloroacetate nka etherification
CMC hamwe na DS yo hejuru yateguwe hongerwaho alkali kabiri na etherifying agent kabiri. Ongeramo 2g y'ibiti bya pinusi alkali selulose muri flask y'amajosi ane, hanyuma ongeramo ingano runaka ya solide ya Ethanol, hanyuma ubireke neza kuri 30min
hafi, kugirango alkali selulose itatanye rwose. Noneho ongeramo umubare runaka wa alkali agent na sodium chloroacetate kugirango ukore mugihe runaka mubushyuhe runaka bwa etherification
Nyuma yigihe, kongeramo kabiri ya alkaline agent na sodium chloroacetate ikurikirwa na etherification mugihe runaka. Nyuma yuko reaction irangiye, humura hanyuma ukonje, hanyuma
Kutabogama hamwe na aside ikwiye ya glacial acetike, hanyuma kuyungurura, gukaraba no gukama.
Gutegura HEC
Gukoresha ibiti bya pinusi alkali selulose yabanjirijwe hamwe na alkali decrystallisation yibikoresho nkibikoresho fatizo, Ethanol nkibishishwa na 2-chloroethanol nka etherification
HEC hamwe na MS yo hejuru yateguwe hongerwaho alkali kabiri na etherifying agent kabiri. Ongeramo 2g y'ibiti bya pinusi alkali selulose mumashanyarazi ane yizosi, hanyuma wongereho ingano ya 90% (agace k'ubunini) Ethanol, koga
Kangura mugihe runaka kugirango ukwirakwize rwose, hanyuma wongereho urugero rwa alkali, hanyuma ushushe buhoro, ongeramo ingano ya 2-
Chloroethanol, yatewe ubushyuhe buri gihe mugihe runaka, hanyuma ikongeramo hydroxide ya sodium isigaye na 2-chloroethanol kugirango ikomeze etherifike mugihe runaka. kuvura
Nyuma yo kubyitwaramo birangiye, shyira hamwe na aside irike ya glacial acide, hanyuma ushungure ukoresheje akayunguruzo k'ikirahure (G3), gukaraba, no kuma.
Gutegura HEMCC
Gukoresha HEC yateguwe muri 3.2.3.4 nkibikoresho fatizo, Ethanol nkigikoresho cyo kubyitwaramo, na sodium chloroacetate nkibikoresho bya etherifingi kugirango witegure
HECMC. Inzira yihariye ni: fata umubare runaka wa HEC, uyishyire muri 100 mL flask yamajosi ane, hanyuma wongere umubare munini wubunini
90% Ethanol, koresha imashini mugihe runaka kugirango itatanye neza, ongeramo urugero rwa alkali nyuma yo gushyushya, hanyuma wongereho buhoro
Sodium chloroacetate, etherification kubushyuhe burigihe burangira nyuma yigihe runaka. Nyuma yo kubyitwaramo birangiye, uyihindure hamwe na acide glacial acetike kugirango uyitesha agaciro, hanyuma ukoreshe akayunguruzo k'ikirahure (G3)
Nyuma yo kuyungurura, gukaraba no gukama.
Isuku rya selile
Muburyo bwo gutegura selile ya selulose, bimwe mubicuruzwa bikunze gukorwa, cyane cyane umunyu wa organic sodium sodium chloride nibindi bimwe
umwanda. Mu rwego rwo kuzamura ubwiza bwa selile ya selile, kweza byoroshye byakozwe kuri selile yabonetse. kuko bari mumazi
Hariho uburyo butandukanye bwo gukemura, bityo igeragezwa rikoresha igice kinini cya etanol hydrated kugirango isukure ethers eshatu zateguwe.
impinduka.
Shira selulose ether sample yateguwe hamwe nubwiza runaka muri beaker, ongeramo umubare munini wa 80% Ethanol yashushe kugeza kuri 60 ℃ ~ 65 and, hanyuma ukomeze gukanika imashini kuri 60 ℃ ~ 65 ℃ kumashanyarazi ahoraho ashyushya magnetiki stirrer kuri 10 ℃. min. Fata ndengakamere kugirango wumuke
Muri beaker isukuye, koresha nitrate ya silver kugirango urebe niba ioni ya chloride. Niba hari imvura yera, iyungurure unyuze mu kirahure hanyuma ufate igikomeye
Subiramo intambwe zabanjirije igice cyumubiri, kugeza igihe filtrate nyuma yo kongeramo igitonyanga 1 cyumuti wa AgNO3 idafite imvura yera, ni ukuvuga kweza no gukaraba birangiye.
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muri (cyane cyane gukuraho reaction kubicuruzwa NaCl). Nyuma yo kuyungurura, kuyumisha, gukonjesha ubushyuhe bwicyumba no gupima.
misa, g.
Uburyo bwo Kugerageza no Kuranga Uburyo bwa Cellulose Ethers
Kugena Impamyabumenyi yo Gusimbuza (DS) na Molar Impamyabumenyi yo Gusimbuza (MS)
Kumenya DS: Icya mbere, ipima 0,2 g (neza na 0.1 mg) ya selile ya selile yanduye kandi yumye, uyishongeshe
80mL y'amazi yatoboye, akangurirwa mu bwogero bwamazi buri gihe kuri 30 ℃ ~ 40 ℃ kuri 10min. Noneho uhindure hamwe na acide sulfurike cyangwa igisubizo cya NaOH
pH yumuti kugeza pH yumuti ari 8. Noneho muri beaker ifite ibikoresho bya electrode ya pH, koresha igisubizo gisanzwe cya acide sulfurike
Kugirango utange titre, mubihe bitera imbaraga, reba metero ya pH usoma mugihe utanga titre, mugihe pH agaciro k'igisubizo ihinduwe kuri 3.74,
Umutwe urangiye. Reba ingano ya acide sulfurike isanzwe ikoreshwa muriki gihe.
Igisekuru:
Igiteranyo cyimibare yo hejuru ya proton hamwe nitsinda rya hydroxyethyl
Ikigereranyo cyumubare wa proton yo hejuru; I7 ni misa yitsinda rya methylene kumatsinda ya hydroxyethyl
Ubukomezi bwa proton resonance peak; ni ubukana bwa proton resonance impinga ya matsinda 5 ya methine nitsinda rimwe rya methylene kumurongo wa glucose selile
Sum.
Uburyo bwikizamini bwasobanuwe kubizamini bya infragre biranga ibizamini bitatu bya selile ya CMC, HEC na HEECMC
Amategeko
3.2.4.3 Ikizamini cya XRD
X-ray Itandukaniro Isesengura Ikiranga Ikizamini cya Cellulose Ethers CMC, HEC na HEECMC
uburyo bw'ikizamini bwasobanuwe.
3.2.4.4 Ikizamini cya H-NMR
H NMR yerekanwe ya HEC yapimwe na Avance400 H NMR yerekanwe na BRUKER.
Ukoresheje dimethyl sulfoxide ya deuterated nka solvent, igisubizo cyageragejwe na hydrogen hydrogène NMR spectroscopy. Inshuro yikizamini yari 75.5MHz.
Igishyushye, igisubizo ni 0.5mL.
3.3 Ibisubizo n'isesengura
3.3.1 Gukwirakwiza uburyo bwo gutegura CMC
Ukoresheje pine selulose yakuwe mu gice cya kabiri nkibikoresho fatizo, no gukoresha sodium chloroacetate nka agent ya etherifying, hakoreshejwe uburyo bwo kugerageza ibintu bimwe,
Gahunda yo gutegura CMC yarakozwe neza, kandi impinduka zambere zigeragezwa zashyizweho nkuko bigaragara mu mbonerahamwe 3.3. Ibikurikira nuburyo bwo gutegura HEC
Mubuhanzi, isesengura ryibintu bitandukanye.
Imbonerahamwe 3.3 Indangagaciro Zibanze
Ikintu Agaciro kambere
Kwirinda ubushyuhe bukabije / ℃ 40
Kwitegura mbere yo kugabanya igihe / h 1
Ikigereranyo gikomeye-kigereranyo / (g / mL) 1:25
Kwitegura mbere yo kwibanda /% 40
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Icyiciro cya mbere etherification ubushyuhe / ℃ 45
Icyiciro cya mbere etherification igihe / h 1
Icyiciro cya kabiri etherification ubushyuhe / ℃ 70
Icyiciro cya kabiri etherification igihe / h 1
Igipimo fatizo murwego rwa etherification / g 2
Umubare wibikoresho bya etherifingi murwego rwa etherification / g 4.3
Ikigereranyo gikomeye-cyamazi / (g / mL) 1:15
3.3.1.1 Ingaruka zimpamvu zitandukanye kurwego rwo gusimbuza CMC murwego rwo kwitegura alkalisation
1. Ingaruka yubushyuhe bwa alkalisation yo kurwego rwo gusimbuza CMC
Kugirango dusuzume ingaruka zubushyuhe bwa alkalisiyonike kurwego rwo gusimbuza CMC wabonye, mugihe cyo gukosora ibindi bintu nkibiciro byambere,
Mubihe, ingaruka zubushyuhe bwa alkalisiyonike kurwego rwo gusimbuza CMC ziraganirwaho, kandi ibisubizo byerekanwe mubishusho.
Kwirinda ubushyuhe bukabije / ℃
Ingaruka zo kwitegura ubushyuhe bugabanya ubushyuhe bwa CMC
Birashobora kugaragara ko urwego rwo gusimbuza CMC rwiyongera hamwe no kwiyongera kwubushyuhe bwa alkalisation, naho ubushyuhe bwa alkalisation ni 30 ° C.
Impamyabumenyi zavuzwe haruguru zo gusimburwa zigabanuka hamwe n'ubushyuhe bwiyongera. Ni ukubera ko ubushyuhe bwa alkalizing buri hasi cyane, kandi molekile ntizikora kandi ntishobora
Gusenya neza agace ka kristaline ya selile, bigatuma bigora umukozi wa etherifyinga kwinjira imbere muri selile mu cyiciro cya etherification, kandi urwego rwo kubyitwaramo ruri hejuru.
hasi, bivamo urwego rwo hasi rwo gusimbuza ibicuruzwa. Nyamara, ubushyuhe bwa alkalisation ntibukwiye kuba hejuru cyane. Nkuko ubushyuhe bwiyongera, munsi yubushyuhe bwo hejuru na alkali ikomeye,
Cellulose ikunda kwangirika kwa okiside, kandi urwego rwo gusimbuza ibicuruzwa CMC rugabanuka.
2. Ingaruka zo kwitegura alkalinisation kurwego rwo gusimbuza CMC
Mugihe hashyizweho ubushyuhe bwa alkalisation yubushyuhe ni 30 ° C nibindi bintu nindangagaciro zambere, ingaruka zigihe cyo kwangirika kwa CMC ziraganirwaho.
Ingaruka zo gusimburwa. Impamyabumenyi yo gusimburwa
Kwitegura mbere yo kugabanya igihe / h
Ingaruka zo kwitegura alkalinisation igihe kuriCMCimpamyabumenyi
Igicucu ubwacyo kirihuta cyane, ariko igisubizo cya alkali gikenera igihe cyo gukwirakwiza muri fibre.
Birashobora kugaragara ko mugihe alkalisation ari 0.5-1.5h, urwego rwo gusimbuza ibicuruzwa rwiyongera hamwe no kwiyongera kwigihe.
Urwego rwo gusimbuza ibicuruzwa rwabonye nirwo rwinshi mugihe igihe cyari 1.5h, naho urwego rwo gusimburwa rwaragabanutse no kwiyongera kwigihe nyuma ya 1.5h. Ibi birashoboka
Bishobora kuba kubera ko mugitangira alkalisation, hamwe no kongera igihe cya alkalisation, kwinjira kwa alkali kuri selile birahagije, kuburyo fibre
Imiterere yibanze iraruhutse, yongera ibikorwa bya etherifying hamwe nuburyo bukora
Igihe cyo kohereza: Apr-26-2024