Gbigba cellulose kokoro-arun bi awọn ohun elo aise, synthesize 2-hydroxy-3-sulfate propyate cellulose ether.spectrometer infurarẹẹdi ṣe itupalẹ ilana ọja naa.Awọn ipo ilana ti o dara julọ fun iṣelọpọ ti cellulose ether bakteria ipilẹ.Awọn abajade fihan pe agbara paṣipaarọ ti 2-hydroxy-3-sulfonic acid-orisun propyate kokoro ether ti a ṣepọ labẹ awọn ipo iṣapeye jẹ 0.481mmol / g.
Awọn ọrọ-ọrọ: cellulose kokoro arun;2-hydroxyl-3-sulfonic acid-orisun gornemine cellulose ether;agbara paṣipaarọ
Makirobia sintetiki kokoro arun cellulose jẹ iru si ọgbin cellulose ni kemikali tiwqn ati molikula be.O jẹ polysaccharide taara ti o ni asopọ nipasẹ D-pyrarot glukosi pẹluβ-1, 4-glycoside ìde.Ti a bawe pẹlu cellulose ọgbin, cellulose kokoro-arun ni abuda to dara julọ.O ti wa ni ohun ultra-micro okun net kq ultra-micro awọn okun.O wa ni irisi cellulose mimọ ati pe o ni ọpọlọpọ awọn iṣẹ alailẹgbẹ.Awọn abala ti ohun elo akositiki ati iwakusa epo ti ni lilo pupọ.
2-hydroxyl-3-sulfonate cellular cellulose ether jẹ itọsẹ cellulose pataki ti o le ṣe awọn ohun elo gbigba omi ti o ga.O tun le ṣee lo bi mimọ to lagbara fun adsorption ti awọn ions irin eru ati amuaradagba bi cation.Feng Qingqin, Jie Zhefeng ati awọn miiran cellulose lo ninu iresi ikarahun oka koriko lati mura 2-hydroxyl-3-sulfate cellulose ether lagbara acid cationic pasipaaro.Nkan yii nlo cellulose kokoro-arun bi awọn ohun elo aise, synthesizing 2-hydroxyl-3-sulfonic acid-based bacterial cellulose ether, ati lilo awọn adanwo orthogonal lati ṣe iwadi awọn ipo sintetiki ti o dara julọ ati 2-hydroxyl-3-sulfa-sulfa sulfa ti a pese sile labẹ ipo yii.Agbara paṣipaarọ ti acid-orisun gornemine cellulose ether pese ipilẹ ilana fun ohun elo gangan ti ohun elo naa.
1. Apakan idanwo
1.1 Reagents ati ohun elo
cellulose kokoro arun (ti ara ẹni), iṣuu soda hydroxide, soda kaboneti, sodium bisulfite, dioxane, epichlorohydrin, acetone, ethanol, soda carbonate, awọn reagents loke jẹ ti ipele analitikali.
Incubator / apoti gbigbe (Shanghai-Heng Technology Co., Ltd.);GQF-1 jet ọlọ (Ile-iṣẹ Powder, Nanjing University of Science and Technology);spectrometer infurarẹẹdi Fourier (Germany);Agilent AAS-3510 atomiki gbigba spectrophotometer.
1.2 Igbaradi ti 2-hydroxy-3-sulfopropyl bacterial cellulose ether
1.2.1 Agbekale ti cellulose kokoro arun ti o ni asopọ agbelebu
Fi 10g ti kokoro cellulose lulú, 60ml ti epichlorohydrin ati 125mL ti 2mol·Ojutu L-1 NaOH sinu ọpọn ọrùn mẹta ti o ni ipese pẹlu condenser reflux ati aruwo, ooru si reflux fun 1h, àlẹmọ, ati fifọ agbelebu pẹlu acetone ati omi si awọn ohun-ini alabọde, ati ki o gbẹ labẹ igbale ni 60°C lati gba cellulose kokoro arun ti o ni asopọ agbelebu.
1.2.2 Iṣagbepọ ti iṣuu soda 3-chloro-2 hydroxypropanesulfonate
Ṣe iwọn 104.0gNaHSO3 ki o tu ni 200mLH2O, ki o jẹ ki o kun fun gaasi SO2.Ooru soke si 70-90°C pẹlu gbigbe, lẹhinna ṣafikun 160mL epichlorohydrin pẹlu eefin sisọ silẹ, ki o fesi ni 85°C fun wakati 4.Ọja ifaseyin ti tutu si isalẹ 5°C lati ṣaja ọja naa, lẹhinna a ṣe iyọda, fo, ati gbigbe lati gba ọja robi ofeefee kan.A ṣe atunṣe ọja robi pẹlu 1: 1 ethanol lati gba awọn kirisita funfun.
1.2.3 Akopọ ti 2-hydroxy-3-sulfopropyl kokoro arun cellulose ether
Fi 2 g ti cellulose kokoro ti o ni asopọ agbelebu, iye kan ti 3-chloro-2-hydroxypropanesulfonate, 0.7 g ti sodium carbonate, ati 70 milimita ti ojutu olomi dioxane sinu ọpọn ọrùn mẹta ti o ni ipese pẹlu condenser reflux ati aruwo, nitrogen Labẹ aabo, ṣakoso iwọn otutu kan ki o ru lati fesi fun akoko kan, àlẹmọ, wẹ pẹlu acetone ati omi ni iyipada si didoju, ati igbale-gbẹ ni 60°C lati gba ina ofeefee ri to.
1.3 Ọja igbekale igbekale
Idanwo FT-IR: tabulẹti KBr ti o lagbara, iwọn idanwo: 500cm-1～4000cm-1.
1.4 Ipinnu ti agbara paṣipaarọ
Mu 1-2g ti 2-hydroxy-3-sulfopropyl bakteria cellulose ether, fi iye ti o yẹ fun omi ti a ti sọ distilled lati rọ, lẹhinna tú u sinu iwe-paṣipaarọ pẹlu gbigbọn, fi omi ṣan pẹlu iye ti o yẹ ti omi ti a fi omi ṣan, lẹhinna lo nipa 100mL 5% Hydrochloric acid fi omi ṣan, ṣakoso iwọn sisan ti 3mL fun iṣẹju kan.Lẹhinna wẹ pẹlu omi distilled titi ti ko fi han acidity nigba idanwo nipasẹ osan methyl, lẹhinna elute pẹlu iwọn 60mL ti iṣuu soda kiloraidi pẹlu ifọkansi ti 1mol L-1, ṣakoso iwọn sisan ni bii 3mL/min, ati gba itujade pẹlu ẹya Erlenmeyer fila.Lẹhinna wẹ ọwọn naa pẹlu omi distilled 50-80mL.Ojutu ti a gba ni titrated pẹlu 0.1mol·Ojutu boṣewa L-1 sodium hydroxide ni lilo phenolphthalein gẹgẹbi itọkasi, ati nọmba awọn milimita ti iṣuu soda hydroxide jẹ VNaOH.
2. Awọn esi ati ijiroro
2.1 Iṣalaye igbekale ti cellulose kokoro-arun ti o ni asopọ agbelebu
Nitori iṣafihan tuntun C-H, cellulose kokoro arun ti o ni asopọ agbelebu jẹ 2922.98cm-1.Gbigbọn nina ti C-H lori iwọn suga ti ni ilọsiwaju, ati awọn giga gbigba abuda ti awọn ẹgbẹ hydroxyl ni 1161.76cm-1 ati 1061.58cm-1 ti laini iwoye a ti ni irẹwẹsi, eyiti o jẹ awọn giga gbigba abuda ti awọn ẹgbẹ hydroxyl ni cellulose.Ni 3433.2cm-1, giga gbigba gbigbọn ti ẹgbẹ hydroxyl ti o ni nkan ṣe tun wa, ṣugbọn kikankikan ojulumo dinku, ti o fihan pe ẹgbẹ hydroxyl lori iwọn glucoside ko ti rọpo patapata.
2.2 Iṣalaye igbekale ti iṣuu soda 3-chloro-2-hydroxypropanesulfonate
3525～3481cm-1 jẹ gbigbọn nina ti ẹgbẹ hydroxyl O-H bond, 2930.96cm-1 jẹ gbigbọn nina asymmetric ti C-H, 2852.69cm jẹ gbigbọn nina asami-ara ti C-H, 1227.3cm-1, 1054. 95cm-1 jẹ gbigbọn gbigbọn ti S=O, 810.1cm-1 jẹ gbigbọn gbigbọn ti COS, ati 727.4cm-1 jẹ gbigbọn gbigbọn ti C.-Cl, o nfihan pe ọja ibi-afẹde ti ṣẹda.
2.3 Iṣalaye igbekale ti 2-hydroxy-3-sulfopropyl bacterial cellulose ether
3431cm-1 jẹ tente gbigbọn gbigbọn OH, 2917cm-1 jẹ tente gbigbọn gbigbọn CH ti o kun, 1656cm-1 jẹ tente gbigbọn gbigbọn CC, 1212 ~ 1020cm-1 jẹ -SO2-antisymmetric ati imunra gbigbọn, 658cm-1 awọn SO mnu nínàá gbigbọn.
2.4 Imudara awọn ipo iṣelọpọ fun 2-hydroxy-3-sulfopropyl ether cellulose bacterial
Ninu idanwo naa, a lo agbara paṣipaarọ lati ṣe idanwo didara 2-hydroxy-3-sulfopropyl ether bacterial cellulose.Awọn iye ti 3-chloro-2 hydroxypropanesulfonate soda ti a fi kun ninu ifura, ifọkansi ti ojutu olomi dioxane, akoko ifarabalẹ ati iwọn otutu ti ṣe awọn ifosiwewe mẹrin ati awọn ipele mẹta ti awọn idanwo orthogonal lati ṣe itupalẹ ipa ti ifosiwewe kọọkan lori cellulose xanthate kokoro-arun. .Ipa ti awọn ohun-ini ester.
Awọn adanwo Orthogonal fihan pe apapọ ti o dara julọ ti awọn ifosiwewe 4 jẹ A2B1C3D.1 Itupalẹ ibiti o fihan pe iwọn otutu ifasẹyin ni ipa ti o tobi julọ lori iṣẹ adsorption ti 2-hydroxy-3-sulfopropyl cellulose ether, ati ibiti o wa ni 1. 914, ti o tẹle pẹlu ifọkansi ti akoko, dioxane, ati iye ifunni ti 3. -chloro-2 hydroxypropanesulfonate iṣuu soda.Agbara paṣipaarọ ti 2-hydroxy-3-sulfopropyl bacterial cellulose ether ti a pese sile labẹ awọn ipo iṣapeye jẹ 0.481mmol/g, eyiti o ga ju ti iru SE-type cellulose lagbara acid cation awọn igi paṣipaarọ ti a royin ninu itọnisọna.
3. Ipari
Nipa iyipada cellulose kokoro-arun, 2-hydroxy-3-sulfonic acid propyl bakteria cellulose ether ti wa ni iṣelọpọ, ati pe a ṣe afihan ọna rẹ ati pe a ṣe iwọn agbara paṣipaarọ rẹ.Awọn ipinnu wọnyi ni a ṣe: 1) 2-hydroxy-3 - Awọn ilana ilana ti o dara julọ fun iṣelọpọ ti sulforopyl bakteria cellulose ether jẹ: 2g cellulose kokoro ti o ni asopọ agbelebu, 3.5g 3-chloro-2-hydroxypropanesulfonate sodium, 0.7g sodium carbonate carbonate. ati 7OmI30% dioxane Aqueous ojutu, esi ni 70°C labẹ aabo nitrogen fun 1h, 2-hydroxy-3-sulfonic acid propyl bacterial cellulose ether ti a pese sile labẹ ipo yii ni agbara paṣipaarọ ti o ga julọ;2) 2-hydroxy-3-sulfonic acid Ẹgbẹ Agbara paṣipaarọ ti propyl bakteria cellulose ether jẹ ti o ga ju ti iru SE iru cellulose lagbara acid cation resini paṣipaarọ royin ninu awọn gede.
Akoko ifiweranṣẹ: Mar-06-2023