Noj cov kab mob cellulose ua raw cov ntaub ntawv, synthesize 2-hydroxy-3-sulfate propyate cellulose ether. Lub infrared spectrometer soj ntsuam cov qauv khoom. Cov txheej txheem zoo tshaj plaws rau kev sib txuas ntawm cov kab mob hauv paus cellulose ether. Cov txiaj ntsig tau pom tias qhov kev sib pauv muaj peev xwm ntawm 2-hydroxy-3-sulfonic acid-based propyate bacterial ether synthesized nyob rau hauv kev ua kom zoo dua yog 0.481mmol / g.
Ntsiab lus: kab mob cellulose; 2-hydroxyl-3-sulfonic acid-based gornemine cellulose ether; pauv peev xwm
Microbial synthetic bacterial cellulose zoo ib yam li cog cellulose hauv tshuaj muaj pes tsawg leeg thiab cov qauv molecular. Nws yog ib tug ncaj polysaccharide txuas los ntawm D-pyrarot qabzib nrogβ-1,4-glycoside bonds. Piv nrog cov nroj tsuag cellulose, cov kab mob cellulose muaj cov yam ntxwv zoo dua. Nws yog ib qho ultra-micro fiber net tsim los ntawm ultra-micro fibers. Nws muaj nyob rau hauv daim ntawv ntawm cellulose ntshiab thiab muaj ntau yam tshwj xeeb functions. Cov yam ntxwv ntawm cov khoom siv acoustic thiab cov roj mining tau siv dav.
2-hydroxyl-3-sulfonate cellular cellulose ether yog ib qho tseem ceeb ntawm cellulose derivative uas tuaj yeem ua los ntawm cov ntaub ntawv nqus dej siab. Nws kuj tseem siv tau los ua cov khoom purity rau adsorption ntawm cov hlau hnyav ions thiab cov protein ua cation. Feng Qingqin, Jie Zhefeng thiab lwm yam cellulose siv nyob rau hauv nplej plhaub pob kws straw los npaj 2-hydroxyl-3-sulfate cellulose ether muaj zog acid cationic exchanges. Kab lus no siv cov kab mob cellulose ua raw cov ntaub ntawv, synthesizing 2-hydroxyl-3-sulfonic acid-based bacterial cellulose ether, thiab siv cov kev sim orthogonal los kawm txog nws cov khoom siv hluavtaws zoo tshaj plaws thiab 2-hydroxyl-3-sulfa-sulfa sulfa npaj nyob rau hauv cov xwm txheej no. Lub peev xwm sib pauv ntawm cov kua qaub-based gornemine cellulose ether muab theoretical hauv paus rau kev siv tiag tiag ntawm cov khoom.
1. Kev sim ib feem
1.1 Reagents thiab ntsuas
Cov kab mob cellulose (tus kheej tsim), sodium hydroxide, sodium carbonate, sodium bisulfite, dioxane, epichlorohydrin, acetone, ethanol, sodium carbonate, cov saum toj no reagents yog ntawm analytical qib.
Incubator / ziab lub thawv (Shanghai-Heng Technology Co., Ltd.); GQF-1 dav hlau zeb (Powder Center, Nanjing University of Science thiab Technology); Fourier infrared spectrometer (Lub teb chaws Yelemees); Agilent AAS-3510 atomic absorption spectrophotometer
1.2 Kev npaj ntawm 2-hydroxy-3-sulfopropyl kab mob cellulose ether
1.2.1 Synthesis of cross-linked bacterial cellulose
Ntxiv 10g ntawm cov kab mob cellulose hmoov, 60mL ntawm epichlorohydrin thiab 125mL ntawm 2mol.·L-1 NaOH tov rau hauv lub khob peb-caj dab nruab nrog lub reflux condenser thiab stirrer, cua sov rau reflux rau 1h, lim, thiab hla-ntxuav nrog acetone thiab dej mus rau nruab nrab cov khoom, thiab qhuav nyob rau hauv lub tshuab nqus tsev ntawm 60.°C kom tau cov kab mob sib kis kab mob cellulose.
1.2.2 Synthesis ntawm sodium 3-chloro-2 hydroxypropanesulfonate
Qhov hnyav 104.0gNaHSO3 thiab yaj hauv 200mLH2O, thiab cia nws saturated nrog SO2 roj. Kub mus txog 70-90°C nrog nplawm, ces ntxiv 160mL epichlorohydrin nrog ib tug xa me nyuam rov funnel, thiab react ntawm 85°C rau 4h. Cov khoom siv tshuaj tiv thaiv tau txias kom qis dua 5°C kom crystallize cov khoom, ces suction lim, ntxuav, thiab qhuav kom tau ib tug daj ntseg daj crude khoom. Cov khoom lag luam crude tau recrystallized nrog 1: 1 ethanol kom tau txais cov muaju dawb.
1.2.3 Synthesis ntawm 2-hydroxy-3-sulfopropyl kab mob cellulose ether
Ntxiv 2 g ntawm cov kab mob sib txuas ntawm cov kab mob cellulose, ib qho nyiaj ntawm 3-chloro-2-hydroxypropanesulfonate, 0.7 g ntawm sodium carbonate, thiab 70 mL ntawm dioxane aqueous tov rau hauv peb-caj dab ntim nrog lub reflux condenser thiab stirrer, nitrogen Nyob rau hauv kev tiv thaiv, tswj ib tug tej yam kub thiab do kom react rau ib lub sij hawm ntawm lub sij hawm, lim, ntxuav nrog acetone thiab dej nyob rau hauv lem mus rau nruab nrab, thiab nqus-qhuav ntawm 60.°C kom tau lub teeb daj.
1.3 Kev txheeb xyuas cov khoom siv
FT-IR xeem: khoom KBr ntsiav tshuaj, xeem ntau yam: 500cm-1～4000cm-1.
1.4 Kev txiav txim siab ntawm kev sib pauv peev
Siv 1-2g ntawm 2-hydroxy-3-sulfopropyl kab mob cellulose ether, ntxiv cov dej distilled kom haum, ces ncuav rau hauv kem pauv nrog nplawm, yaug nrog qhov tsim nyog ntawm cov dej distilled, thiab tom qab ntawd siv li 100mL 5% Hydrochloric acid yaug, tswj tus nqi ntws ntawm 3mL ib feeb. Tom qab ntawd ntxuav nrog dej distilled kom txog thaum nws tsis pom acidity thaum kuaj los ntawm methyl txiv kab ntxwv, ces elute nrog txog 60mL ntawm sodium chloride nrog ib tug concentration ntawm 1mol L-1, tswj tus nqi ntws ntawm txog 3mL / min, thiab sau cov effluent nrog ib tug Erlenmeyer khob. Tom qab ntawd ntxuav lub kem nrog 50-80mL dej distilled. Cov tshuaj sib sau tau titrated nrog 0.1mol·L-1 sodium hydroxide standard tov siv phenolphthalein ua qhov taw qhia, thiab cov naj npawb ntawm milliliters ntawm sodium hydroxide noj yog VNaOH.
2. Cov txiaj ntsig thiab kev sib tham
2.1 Cov yam ntxwv ntawm cov kab mob sib txuas ntawm cov kab mob cellulose
Vim qhov kev taw qhia tshiab C—H, cov kab mob sib txuas ntawm cov cellulose yog 2922.98cm-1. Lub zog vibration ntawm C—H ntawm lub nplhaib qab zib yog txhim kho, thiab cov yam ntxwv nqus siab siab ntawm cov pab pawg hydroxyl ntawm 1161.76cm-1 thiab 1061.58cm-1 ntawm cov kab spectral a yog tsis muaj zog, uas yog cov yam ntxwv ntawm qhov nqus ntawm pawg hydroxyl hauv cellulose. Ntawm 3433.2cm-1, qhov kev nqus nqus siab ncov ntawm pawg hydroxyl cuam tshuam tseem muaj, tab sis cov txheeb ze siv tau txo qis, qhia tias pawg hydroxyl ntawm lub nplhaib glucoside tsis tau hloov tag nrho.
2.2 Tus yam ntxwv ntawm tus yam ntxwv ntawm sodium 3-chloro-2-hydroxypropanesulfonate
ib 3525～3481cm-1 yog qhov ncab kev co ntawm koom haum hydroxyl O—H daim ntawv cog lus, 2930.96cm-1 yog asymmetric stretching vibration ntawm C—H, 2852.69cm yog symmetrical stretching vibration ntawm C—H, 1227.3cm-1, 1054. 95cm-1 yog stretching vibration ntawm S = O, 810.1cm-1 yog stretching vibration ntawm COS, thiab 727.4cm-1 yog stretching vibration ntawm C—Cl, qhia tias cov khoom lag luam yog tsim.
2.3 Cov yam ntxwv ntawm 2-hydroxy-3-sulfopropyl kab mob cellulose ether
3431cm-1 yog OH stretching vibration ncov, 2917cm-1 yog saturated CH stretching vibration ncov, 1656cm-1 yog CC stretching vibration ncov, 1212 ~ 1020cm-1 yog -SO2-antisymmetric thiab symmetric stretching vibration, - 658cm SO daim ntawv cog lus stretching vibration.
2.4 Optimization ntawm synthesis tej yam kev mob rau 2-hydroxy-3-sulfopropyl kab mob cellulose ether
Hauv kev sim, kev sib pauv tau siv los ntsuas qhov zoo ntawm 2-hydroxy-3-sulfopropyl kab mob cellulose ether. Tus nqi ntawm 3-chloro-2 hydroxypropanesulfonate sodium ntxiv rau hauv cov tshuaj tiv thaiv, qhov concentration ntawm dioxane aqueous tov, lub sij hawm cov tshuaj tiv thaiv thiab qhov kub thiab txias tau ua plaub yam thiab peb theem ntawm orthogonal thwmsim los soj ntsuam cov nyhuv ntawm txhua yam ntawm cov kab mob cellulose xanthate. . Kev cuam tshuam ntawm ester zog.
Orthogonal thwmsim qhia tau hais tias qhov zoo tshaj plaws ua ke ntawm 4 yam yog A2B1C3D. 1 Range tsom xam qhia tau hais tias qhov ntsuas kub ntawm cov tshuaj tiv thaiv muaj qhov cuam tshuam loj tshaj plaws ntawm kev ua haujlwm adsorption ntawm 2-hydroxy-3-sulfopropyl cellulose ether, thiab qhov ntau yog 1. 914, ua raws li cov concentration ntawm lub sij hawm, dioxane, thiab pub mis ntawm 3. chloro-2 hydroxypropanesulfonate sodium. Lub peev xwm pauv ntawm 2-hydroxy-3-sulfopropyl kab mob cellulose ether npaj nyob rau hauv cov kev kho kom zoo yog 0.481mmol / g, uas yog siab dua li SE-type cellulose muaj zog acid cation txauv ntoo qhia hauv phau ntawv.
3. Cov lus xaus
Los ntawm kev hloov kho cov kab mob cellulose, 2-hydroxy-3-sulfonic acid propyl bacterial cellulose ether tau ua ke, thiab nws cov qauv yog tus yam ntxwv thiab nws cov peev xwm pauv tau raug ntsuas. Cov lus xaus hauv qab no tau kos: 1) 2-hydroxy-3 - Cov txheej txheem zoo tshaj plaws rau kev sib txuas ntawm sulfopropyl kab mob cellulose ether yog: 2g cross-linked bacterial cellulose, 3.5g 3-chloro-2-hydroxypropanesulfonate sodium, 0.7g sodium carbonate thiab 7OmI30% dioxane Aqueous tov, cov tshuaj tiv thaiv ntawm 70°C nyob rau hauv kev tiv thaiv nitrogen rau 1h, 2-hydroxy-3-sulfonic acid propyl kab mob cellulose ether npaj nyob rau hauv cov xwm txheej no muaj peev xwm pauv ntau dua; 2) 2-hydroxy-3-sulfonic acid pawg Lub peev xwm pauv ntawm propyl kab mob cellulose ether yog siab dua li ntawm SE hom cellulose muaj zog acid cation txauv resin qhia hauv phau ntawv qhia.
Post lub sij hawm: Mar-06-2023