Focus on Cellulose ethers

2-hydroxyl-3-sulfonic acid glycopyl bacterioprocycin fibin ether synthesis

Ukuthatha i-cellulose yebhaktheriya njengezinto zokusetshenziswa, hlanganisa i-2-hydroxy-3-sulfate propyate cellulose ether. I-spectrometer ye-infrared ihlaziya ukwakheka komkhiqizo. Izimo zenqubo ezingcono kakhulu zokuhlanganiswa kwe-base bacterial cellulose ether. Imiphumela yabonisa ukuthi umthamo wokushintshana we-2-hydroxy-3-sulfonic acid-based propyate ether yebhaktheriya ehlanganiswe ngaphansi kwezimo zokuthuthukisa yayingu-0.481mmol / g.

Amagama angukhiye: i-cellulose yebhaktheriya; I-2-hydroxyl-3-sulfonic acid-based gornemine cellulose ether; umthamo wokushintshana

 

I-microbial synthetic bacterial cellulose ifana ne-cellulose yezitshalo ekwakhiweni kwamakhemikhali kanye nesakhiwo samangqamuzana. I-polysaccharide eqondile exhunywe nge-D-pyrarot glucoseβ-1, 4-glycoside bond. Uma kuqhathaniswa ne-cellulose yezitshalo, i-cellulose yebhaktheriya inesici esingcono. Kuyi-ultra-micro fiber net eyakhiwe imicu yama-ultra-micro. Ikhona ngesimo se-cellulose ehlanzekile futhi inemisebenzi eminingi eyingqayizivele. Izici zemishini ye-acoustic kanye nezimayini zikawoyela zisetshenziswe kakhulu.

I-2-hydroxyl-3-sulfonate cellulose ether iyingxenye ebalulekile ye-cellulose engenziwa ngezinto zokumunca amanzi aphezulu. Ingasetshenziswa futhi njengokuhlanzeka okuqinile kokukhangisa kwama-ion ensimbi esindayo namaprotheni njenge-cation. I-Feng Qingqin, i-Jie Zhefeng kanye nenye i-cellulose esetshenziswa kutshani bombila wegobolondo lerayisi ukuze kulungiswe i-2-hydroxyl-3-sulfate cellulose ether ukuhwebelana okuqinile kwe-asidi ye-cationic. Lesi sihloko sisebenzisa i-cellulose yebhaktheriya njengezinto zokusetshenziswa, ihlanganisa i-2-hydroxyl-3-sulfonic acid-based bacterial cellulose ether, futhi isebenzisa ukuhlolwa kwe-orthogonal ukutadisha izimo zayo ezingcono kakhulu zokwenziwa kanye ne-2-hydroxyl-3-sulfa-sulfa sulfa elungiselelwe ngaphansi kwalesi simo. Umthamo wokushintshana we-asidi-based gornemine cellulose ether uhlinzeka ngesisekelo sethiyori sokusetshenziswa kwangempela kwento.

 

1. Ingxenye yokuhlola

1.1 Ama-reagents nezinsimbi

I-cellulose yebhaktheriya (ezenzele yona), i-sodium hydroxide, i-sodium carbonate, i-sodium bisulfite, i-dioxane, i-epichlorohydrin, i-acetone, i-ethanol, i-sodium carbonate, ama-reagents angenhla asezingeni lokuhlaziya.

I-incubator/ibhokisi lokomisa (i-Shanghai-Heng Technology Co., Ltd.); I-GQF-1 jet mill (Powder Center, Nanjing University of Science and Technology); I-Fourier infrared spectrometer (eJalimane); I-Agilent AAS-3510 i-spectrophotometer yokumuncwa kwe-athomu.

1.2 Ukulungiswa kwe-2-hydroxy-3-sulfopropyl bacterial cellulose ether

1.2.1 Ukuhlanganiswa kwe-cellulose yebhaktheriya exhumene

Faka u-10g we-bacterial cellulose powder, 60mL we-epichlorohydrin kanye no-125mL we-2mol·Isixazululo se-L-1 NaOH sibe yiflask enezintamo ezintathu efakwe i-reflux condenser kanye ne-stirrer, ukushisa kuya ku-reflux ye-1h, isihlungi, nokugeza okuphambene ne-acetone namanzi kuya ezindaweni eziphakathi, futhi zomiswe ngaphansi kwe-vacuum ku-60.°C ukuthola i-cellulose yebhaktheriya exhumene.

1.2.2 Ukuhlanganiswa kwe-sodium 3-chloro-2 hydroxypropanesulfonate

Kala u-104.0gNaHSO3 bese uyincibilikisa ku-200mLH2O, futhi uyivumele igcwaliswe ngegesi ye-SO2. Shisisa kufika ku-70-90°C ngokushukumisa, bese wengeza i-epichlorohydrin engu-160mL ngefaneli yokuwisa, bese usabele ku-85.°C ngo 4h. Umkhiqizo wokusabela upholiswe waba ngaphansi kuka-5°C ukwenza umkhiqizo ube yikristalu, bese ukumuncwa kuyahlungwa, kugezwe, futhi komiswe ukuze kutholwe umkhiqizo ongahluziwe ophuzi ngokuphaphathekile. Umkhiqizo ongahluziwe waphinde wahlanganiswa nge-ethanol engu-1:1 ukuze uthole amakristalu amhlophe.

1.2.3 Ukuhlanganiswa kwe-2-hydroxy-3-sulfopropyl bacterial cellulose ether

Faka u-2 g we-cellulose yebhaktheriya exhumene nesiphambano, inani elithile le-3-chloro-2-hydroxypropanesulfonate, 0.7 g we-sodium carbonate, kanye no-70 mL wesisombululo samanzi se-dioxane eflaskini enezintamo ezintathu efakwe i-reflux condenser kanye ne-stirrer, I-nitrogen Ngaphansi kokuvikelwa, lawula izinga lokushisa elithile futhi ushukumise ukuze usabele isikhathi esithile, hlunga, geza nge-acetone namanzi ngokushintshashintsha kokungathathi hlangothi, futhi usule-vacuum-dry ngo-60.°C ukuze uthole okuqinile okuphuzi okukhanyayo.

1.3 Ukuhlaziywa kwesakhiwo somkhiqizo

Ukuhlolwa kwe-FT-IR: ithebhulethi ye-KBR eqinile, ibanga lokuhlola: 500cm-14000cm-1.

1.4 Ukunqunywa kwamandla okushintshanisa

Thatha u-1-2g we-2-hydroxy-3-sulfopropyl bacterial cellulose ether, engeza inani elifanele lamanzi acwecwe ukuze ucwiliswe, bese uwathela kukholomu yokushintshanisa ngokugqugquzela, hlambulula ngamanzi acwebile afanelekile, bese usebenzisa cishe u-100mL 5% I-Hydrochloric acid hlambulula, lawula izinga lokugeleza lika-3mL ngomzuzu. Bese ugeza ngamanzi acwecwe kuze kube yilapho engabonisi i-acidity uma ihlolwa i-methyl orange, bese u-elute cishe ngo-60mL we-sodium chloride ene-concentration ye-1mol L-1, ulawule izinga lokugeleza cishe ku-3mL/min, bese uqoqa ukungcola nge- I-Erlenmeyer flask. Bese ugeza ikholomu ngamanzi angama-50-80mL acwecwe. Isixazululo esiqoqiwe sifakwe ku-0.1mol·Isixazululo esijwayelekile se-L-1 sodium hydroxide sisebenzisa i-phenolphthalein njengenkomba, kanye nenani lamamililitha e-sodium hydroxide esetshenzisiwe laliyi-VNaOH.

 

2. Imiphumela kanye nengxoxo

2.1 Ukubonakaliswa kwesakhiwo se-cellulose yebhaktheriya exhumene

Ngenxa yokwethulwa kwe-C-H, i-cellulose yebhaktheriya exhunywe ngokuphambana ingu-2922.98cm-1. Ukudlidliza okunwebekayo kwe-C-U-H eringini kashukela uyathuthukiswa, futhi izici zokumunca eziyisici zamaqembu e-hydroxyl ku-1161.76cm-1 kanye no-1061.58cm-1 womugqa we-spectral a ziba buthaka, okuyiziqongo zokumunca eziyisici zamaqembu e-hydroxyl ku-cellulose. Ku-3433.2cm-1, inani eliphakeme lokumuncwa lokudlidliza leqembu le-hydroxyl elihlobene lisekhona, kodwa ukuqina okuhlobene kuyehla, okubonisa ukuthi iqembu le-hydroxyl eringini ye-glucoside alikashintshwa ngokuphelele.

2.2 Ukubonakaliswa kwesakhiwo se-sodium 3-chloro-2-hydroxypropanesulfonate

3525I-3481cm-1 ukudlidliza okunwebekayo kwenhlangano i-hydroxyl O-I-H bond, 2930.96cm-1 iwukudlidliza okwelula kwe-asymmetric kwe-C-H, 2852.69cm ukudlidliza okulinganayo kwe-C-H, 1227.3cm-1, 1054. 95cm-1 ukudlidliza okunwebekayo kwe-S=O, 810.1cm-1 ukudlidliza okunwebekayo kwe-COS, futhi 727.4cm-1 ukudlidliza okunwebekayo kwe-C-Cl, okubonisa ukuthi umkhiqizo okuhlosiwe wakhiwe.

2.3 Ukubonakaliswa kwesakhiwo se-2-hydroxy-3-sulfopropyl bacterial cellulose ether

I-3431cm-1 iyisiqongo sokudlidliza se-OH esinwebekayo, i-2917cm-1 iyisiqongo sokudlidliza se-CH esigcwele esinwebekayo, i-1656cm-1 iyisiqongo sokudlidliza esinwebekayo se-CC, 1212 ~ 1020cm-1 is -SO2-antisymmetric kanye ne-symmetric stretching vibration yi-65cm-1 ukudlidliza okunwebeka kwe-SO bond.

2.4 Ukwenziwa ngcono kwezimo zokuhlanganisa ze-2-hydroxy-3-sulfopropyl bacterial cellulose ether

Ocwaningweni, umthamo wokushintshana wasetshenziswa ukuhlola ikhwalithi ye-2-hydroxy-3-sulfopropyl bacterial cellulose ether. Inani le-3-chloro-2 hydroxypropanesulfonate sodium engezwe ekuphenduleni, ukuhlangana kwesixazululo esinamanzi se-dioxane, isikhathi sokuphendula kanye nezinga lokushisa lenze izici ezine namazinga amathathu okuhlolwa kwe-orthogonal ukuhlaziya umphumela wesici ngasinye kubhaktheriya cellulose xanthate. . Umthelela wezakhiwo ze-ester.

Ukuhlolwa kwe-Orthogonal kubonisa ukuthi inhlanganisela efanele yezinto ezingu-4 i-A2B1C3D. 1 Uhlaziyo lwebanga lubonisa ukuthi izinga lokushisa lokusabela linethonya elikhulu ekusebenzeni kwe-adsorption ye-2-hydroxy-3-sulfopropyl cellulose ether, futhi ububanzi bungu-1. 914, kulandelwa ukuhlangana kwesikhathi, i-dioxane, nenani lokuphakelayo elingu-3 -Chloro-2 hydroxypropanesulfonate sodium. Umthamo wokushintshana we-2-hydroxy-3-sulfopropyl bacterial cellulose ether elungiswe ngaphansi kwezimo ezithuthukisiwe wawungu-0.481mmol/g, owawuphezulu kunalowo we-SE-type cellulose izihlahla zokushintshanisa i-asidi eqinile ebikwe kubhukwana.

 

3. Isiphetho

Ngokushintsha i-cellulose yebhaktheriya, i-2-hydroxy-3-sulfonic acid propyl bacterial cellulose ether yahlanganiswa, futhi isakhiwo sayo sabonakala futhi amandla ayo okushintshana alinganiswa. Iziphetho ezilandelayo zafinyelelwa: 1) 2-hydroxy-3 – Izimo ezilungile zenqubo yokuhlanganiswa kwe-sulfopropyl bacterial cellulose ether yilezi: 2g i-cellulose yebhaktheriya exhumene nesiphambano, 3.5g 3-chloro-2-hydroxypropanesulfonate sodium, 0.7g sodium carbonate kanye ne-7OmI30% isixazululo se-dioxane Aqueous, ukusabela ku-70°C ngaphansi kokuvikelwa kwe-nitrogen ye-1h, i-2-hydroxy-3-sulfonic acid propyl bacterial cellulose ether elungiselelwe ngaphansi kwalesi simo inamandla okushintshaniswa okuphezulu; 2) Iqembu le-2-hydroxy-3-sulfonic acid Amandla okushintshana e-propyl bacterial cellulose ether aphakeme kunalawo ohlobo lwe-SE olufana ne-cellulose i-acid cation exchange resin ebikwe encwadini yesandla.


Isikhathi sokuthumela: Mar-06-2023
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