1 Nhanganyaya
Parizvino, zvinhu zvikuru zvinoshandiswa pakugadziraether ye cellulosedonje, uye kubuda kwaro kuri kudzikira, uye mutengo uri kukwirawo;
Uyezve, zvinhu zvinopisa muviri zvinoshandiswa zvakanyanya zvakaita sechloroacetic acid (ine chepfu yakanyanya) uye ethylene oxide (inokonzera carcinogenic) zvinokuvadzawo muviri wemunhu nenharaunda.
Muchitsauko chino, pine cellulose ine kuchena kweinopfuura 90% yakatorwa muchitsauko chechipiri inoshandiswa sechinhu chisina kugadzirwa, uye sodium chloroacetate ne2-chloroethanol zvinoshandiswa sezvinhu zvinotsiva.
Kushandisa chloroacetic acid ine chepfu yakawanda semushonga we etherifying, anioniccarboxymethyl cellulose (CMC), non-ionic hydroxyethyl cellulose yakagadzirwa.
Cellulose (HEC) uye mixed hydroxyethyl carboxymethyl cellulose (HECMC) ine ether nhatu dze cellulose. single factor
Matekiniki ekugadzirira ether nhatu dze cellulose akagadziriswa kuburikidza nekuyedza uye kuyedza kwe orthogonal, uye ether dze cellulose dzakagadzirwa dzakaratidzwa neFT-IR, XRD, H-NMR, nezvimwewo.
Nheyo dzekushandiswa kwe etherification ye cellulose
Nheyo ye etherification ye cellulose inogona kukamurwa kuita zvikamu zviviri. Chikamu chekutanga inzira ye alkalization, ndiko kuti, panguva ye alkalization ye cellulose,
Kana yakapararira zvakaenzana muNaOH solution, pine cellulose inokura zvine simba pasi pechiito chekukurunga kwemuchina, uye nekuwedzera kwemvura.
Mamorekuru madiki eNaOH akawanda akapinda mukati mepine cellulose, uye akaita zvakafanana nemapoka ehydroxyl ari pamhete ye glucose structural unit,
Inogadzira alkali cellulose, iyo inonyanya kushanda pakuita kuti etherification iite.
Chikamu chechipiri inzira ye etherification, ndiko kuti, maitiro ari pakati penzvimbo inoshanda ne sodium chloroacetate kana 2-chloroethanol pasi pemamiriro e alkaline, zvichikonzera
Panguva imwe chete, chinhu chinodziisa mvura chinonzi sodium chloroacetate uye 2-chloroethanol zvinogadzirawo mvura yakati wandei pasi pemamiriro ealkaline.
Matambudziko acho anokonzerwa nekugadzira sodium glycolate uye ethylene glycol, zvichiteerana.
2 Kurapa pine cellulose nealkali yakasanganiswa
Kutanga, gadzirai huwandu hwakati hweNaOH solution nemvura yakabviswa ion. Zvadaro, patembiricha yakati, 2g yepine fiber
Vhitamini inonyungudutswa mune imwe vhoriyamu yeNaOH solution, yokurunga kwenguva yakati, yozosefa kuti ishandiswe.
Mugadziri weModhi yeZvishandiso
Meter yepH chaiyo
Muunganidzi wemhando yekupisa tembiricha inogara ichidziya magnetic stirrer
Ovheni yekuomesa yemuchina wekuchenesa
Kuenzanisa kwemagetsi
Pombi ye vacuum inotenderera yemhando yemvura ine zvinangwa zvakawanda
Spectrometer yeFourier Transform Infrared
Diffractometer yeX-ray
Spektrometa yeMagineti yeNyukireya
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 yeAmerica Co., Ltd.
Kambani yeAmerican Thermoelectric Switzerland ARL
Kambani yeSwitzerland BRUKER
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Kugadzirira kweCMCs
Kushandisa alkali cellulose yemapuranga emupaini yakagadziriswa nekubvisa makristali emuchadenga sechinhu chisina kugadzirwa, kushandisa ethanol se solvent uye kushandisa sodium chloroacetate se etherification
CMC ine DS yakakwirira yakagadzirwa nekuwedzera alkali kaviri uye chinhu chinosimbisa muviri kaviri. Wedzera 2g ye alkali cellulose yemuti wepine muflask ine mitsipa mina, wobva wawedzera ethanol solvent yakati wandei, wobva wasanganisa zvakanaka kwemaminitsi makumi matatu.
pamusoro, kuitira kuti alkali cellulose ipararire zvizere. Wobva wawedzera huwandu hwakati hwealkali agent uye sodium chloroacetate kuti iite chimwe chinhu kwenguva yakati pane imwe tembiricha ye etherification.
Mushure menguva, kuwedzera kwechipiri alkaline agent uye sodium chloroacetate kunozoteverwa ne etherification kwenguva yakati. Kana reaction yapera, tonhodza wozotonhodza, wobva wawedzera
Shandisa glacial acetic acid yakakwana, wozoipukuta woipukuta woiomesa.
Kugadzirira maHEC
Kushandisa pine wood alkali cellulose yakagadziriswa ne concentrated alkali decrystallization se raw material, ethanol se solvent uye 2-chloroethanol se etherification
HEC ine MS yakakwirira yakagadzirwa nekuwedzera alkali kaviri uye chinhu chinosimbisa muviri kaviri. Wedzera 2g yealkali cellulose yemuti wepine muflask ine mitsipa mina, wobva wawedzera huwandu hwakati hwe90% (chikamu chevhoriyamu) ethanol, sanganisa.
Kurunga kwenguva yakati kuti ipararire zvizere, wobva wawedzera huwandu hwakati hwealkali, wobva wapisa zvishoma nezvishoma, wowedzera huwandu hwakati hwe2-
Chloroethanol, yakapiswa nemhepo patembiricha isingachinji kwenguva yakati, uye yakawedzerwa sodium hydroxide yasara ne2-chloroethanol kuti irambe ichipiswa kwenguva yakati.
Kana zvapera, bvisa glacial acetic acid, wozopedzisira waisa girazi (G3), wogeza, wozoomesa.
Kugadzirira kweHEMCC
Kushandisa HEC yakagadzirwa mu3.2.3.4 sezvinhu zvakabikwa, ethanol senzira yekubatsira, uye sodium chloroacetate senzira yekusimbisa muviri kuti ugadzirire
HECMC. Maitiro chaiwo ndeekuti: tora huwandu hwakati hweHEC, uhuise mubhodhoro rine 100 mL rine mitsipa mina, wobva wawedzera huwandu hwakati hwehuwandu.
90% ethanol, kurungai kwenguva yakati kuti ipararire zvizere, wedzerai huwandu hwakati hwealkali mushure mekudziya, uye wedzerai zvishoma nezvishoma
Sodium chloroacetate, etherification pakupisa kwakafanana inopera mushure menguva yakati. Mushure mekunge reaction yapera, ibvise ne glacial acetic acid kuti ibvise, wobva washandisa glass filter (G3).
Mushure mekusveta, kusuka nekuomesa.
Kucheneswa kwe ethers dze cellulose
Mukugadzirira cellulose ether, zvimwe zvigadzirwa zvinowanzogadzirwa, kunyanya inorganic salt sodium chloride nezvimwe.
tsvina. Kuti pave nekuvandudzwa kwemhando ye cellulose ether, kucheneswa kuri nyore kwakaitwa pa cellulose ether yakawanikwa. nekuti iri mumvura.
Kune kunyungudika kwakasiyana, saka kuyedza uku kunoshandisa chikamu chakati chehuwandu hweethanol yakanyungudutswa kuchenesa ma ether matatu e cellulose akagadzirwa.
shanduko.
Isa sample ye cellulose ether yakagadzirwa nehunhu hwakati mubeaker, wedzera huwandu hwakati hwe 80% ethanol yakapiswa kusvika 60 ℃ ~ 65 ℃, uye chengetedza kusanganisa kwemuchina pa60 ℃ ~ 65 ℃ pane stirrer inodziya magnetic stirrer kwenguva inodziya kwe10 ℃. maminetsi. Isa supernatant kuti iome.
Mubhokisi rakachena, shandisa silver nitrate kuti utarise ma chloride ions. Kana paine white precipitate, isefa negirazi filter wotora solid
Dzokorora matanho apfuura echikamu chemuviri, kusvika filtrate mushure mekuwedzera donhwe rimwe remushonga weAgNO3 isisina precipitate chena, kureva kuti, kuchenesa nekusuka zvapera.
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mu (kunyanya kubvisa NaCl inobuda muchinhu ichocho). Mushure mekusveta, kuomesa, kutonhodza kusvika patembiricha yemumba uye kuyerwa.
huremu, g.
Nzira dzeKuyedza uye dzeKuratidza Maonero eCellulose Ethers
Kugadzwa kweDhigirii rekutsiva (DS) uye Dhigirii rekutsiva reMolar (MS)
Kuongororwa kweDS: Kutanga, yera 0.2 g (yakarurama kusvika 0.1 mg) yemuenzaniso we cellulose ether wakacheneswa uye wakaomeswa, woinyungudutsa mu
80mL yemvura yakasanganiswa, yakasanganiswa mumvura inodziya nguva dzose pa30℃ ~40℃ kwemaminitsi gumi. Wobva wagadzirisa ne sulfuric acid solution kana NaOH solution
pH yemushonga kusvika pH yemushonga yava 8. Zvadaro mubeaker ine pH meter electrode, shandisai sulfuric acid yakajairwa.
Kuti utarise titration, kana uchikurunga, tarisa pH meter uchiverenga titration, kana pH yemushonga yagadziriswa kusvika pa3.74,
Titration inopera. Cherechedza huwandu hwe sulfuric acid standard solution inoshandiswa panguva ino.
Chizvarwa:
Huwandu hwenhamba dzeproton dzepamusoro neboka rehydroxyethyl
Chiyero chehuwandu hwemapurotoni ekumusoro; I7 huremu hweboka remethylene riri muboka rehydroxyethyl
Kusimba kweproton resonance peak; ndiko kusimba kweproton resonance peak yemapoka mashanu emethine uye boka rimwe remethylene payuniti yeglucose yecellulose
Huwandu.
Nzira dzekuyedza dzakatsanangurwa pakuyedzwa kwehunhu hweinfrared hwematatu e-cellulose ethers CMC, HEC uye HEECMC
Mutemo
3.2.4.3 Bvunzo reXRD
Kuongororwa kweX-ray Diffraction Analysis Characterization Test yeThree Cellulose Ethers CMC, HEC uye HEECMC
nzira yekuyedza yakatsanangurwa.
3.2.4.4 Kuedzwa kweH-NMR
H NMR spectrometer yeHEC yakayerwa neAvance400 H NMR spectrometer yakagadzirwa neBRUKER.
Uchishandisa deuterated dimethyl sulfoxide se solvent, mhinduro iyi yakaedzwa ne liquid hydrogen NMR spectroscopy. Kuongororwa kwacho kwaive 75.5MHz.
Inodziya, mhinduro yacho ndeye 0.5mL.
3.3 Mhedzisiro uye Ongororo
3.3.1 Kugadzirisa maitiro ekugadzirira CMC
Kushandisa pine cellulose yakatorwa muchitsauko chechipiri sezvinhu zvakagadziriswa, uye kushandisa sodium chloroacetate semushonga we etherifying, nzira yekuedza kwechinhu chimwe chete yakagamuchirwa,
Maitiro ekugadzirira CMC akagadziriswa, uye mavari ekutanga ekuyedza akaiswa sezvakaratidzwa muTafura 3.3. Inotevera ndiyo maitiro ekugadzirira HEC
Muunyanzvi, kuongorora zvinhu zvakasiyana-siyana.
Tafura 3.3 Maonero Ekutanga Ezvinhu
Kukosha kwekutanga kweFactor
Kurapa tembiricha yekudziya kwemvura isati yatanga/℃ 40
Nguva yekurapa isati yasvika ye alkalizing/h 1
Kurapa usati watanga kushandisa solid-liquid ratio/(g/mL) 1:25
Kuwanda kweLye usati warapwa/% 40
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Tembiricha yekutanga ye etherification padanho rekutanga/℃ 45
Nguva ye etherification yedanho rekutanga/h 1
Tembiricha ye etherification yedanho rechipiri/℃ 70
Nguva ye etherification yedanho rechipiri/h 1
Chiyero chekutanga muchikamu che etherification/g 2
Huwandu hwechinhu chinobatidza muviri muchikamu che etherification/g 4.3
Chiyero chemvura yakasimba-yakasimba (etherified solid-liquid ratio/(g/mL) 1:15
3.3.1.1 Kukanganiswa kwezvinhu zvakasiyana-siyana padanho rekutsiva CMC muchikamu chealkaliization yekurapa usati watanga
1. Mhedzisiro yekupisa kwealkaliization ye pretreatment padanho rekutsiva reCMC
Kuti tifunge nezvemhedzisiro yekupisa kwealkaliization isati yatanga kurapwa padanho rekutsiva muCMC yakawanikwa, kana paine zvimwe zvinhu sezviyero zvekutanga,
Pasi pemamiriro ezvinhu aya, mhedzisiro yekupisa kwealkaliization yekurapa isati yatanga inokurukurwa padanho rekutsiva CMC, uye mhedzisiro yacho inoratidzwa muFig.
Kurapa tembiricha yekudziya/℃ isati yatanga
Mhedzisiro yekupisa kwealkalizing tembiricha padanho rekutsiva CMC
Zvinogona kuonekwa kuti mwero wekutsiva CMC unowedzera nekuwedzera kwekushisa kwealkalization yekurapa, uye tembiricha yealkalization iri 30 °C.
Madhigirii ekutsiva ari pamusoro apa anoderera nekupisa kuri kuwedzera. Izvi zvinokonzerwa nekuti tembiricha yealkalizing yakaderera zvakanyanya, uye mamorekuru haashande zvakanyanya uye haakwanise
Kuparadza nzvimbo yekristaro ye cellulose zvinobudirira, izvo zvinoita kuti zviomere kuti chinhu chinopisa chipinde mukati me cellulose panguva ye etherification, uye huwandu hwe reaction hwakakwira.
yakaderera, zvichikonzera mwero wakaderera wekutsiva chigadzirwa. Zvisinei, tembiricha yealkali haifanirwe kunge yakanyanya kukwira. Sezvo tembiricha ichiwedzera, pasi pekushanda kwekupisa kwakanyanya uye alkali yakasimba,
Cellulose inokurumidza kuora kwe oxidative, uye mwero wekutsiva chigadzirwa cheCMC unoderera.
2. Kupesvedzera kwenguva yekurapa alkalineization padanho rekutsiva reCMC
Kana tembiricha yekugadziriswa kwealkali isati yatanga kurapwa iri 30 °C uye zvimwe zvinhu zviri izvo zvinoonekwa pakutanga, mhedzisiro yenguva yekugadziriswa kwealkali isati yatanga kurapwa paCMC inokurukurwa.
Mhedzisiro yekutsiva. Dhigirii rekutsiva
Nguva yekurapa isati yasvika yekuyeresa
Mhedzisiro yenguva yekurapa alkalineization isati yatangaCMCdhigirii rekutsiva
Maitiro ekuwedzera zvinhu zvesimbi pachawo anokurumidza, asi mhinduro yealkali inoda nguva yakati yekupararira mufiber.
Zvinogona kuonekwa kuti kana nguva ye alkalizing iri 0.5-1.5h, mwero wekutsiva kwechigadzirwa unowedzera nekuwedzera kwenguva ye alkalizing.
Mwero wekutsiva chigadzirwa wakawanikwa waive wepamusoro-soro panguva yaive 1.5a, uye mwero wekutsiva wakaderera nekuwedzera kwenguva mushure me1.5a. Izvi zvinogona
Zvingangodaro nekuti pakutanga kwe alkaliization, nekurebeswa kwenguva ye alkaliization, kupinda kwe alkali mu cellulose kwakakwana, saka fiber
Chimiro chikuru chakasununguka, zvichiwedzera chinhu chinopa simba uye chinhu chinoshanda.
Nguva yekutumira: Kubvumbi-26-2024