1 Hordhac
Waqtigan xaadirka ah, walxaha ugu muhiimsan ee loo isticmaalo diyaarintacellulose etherwaa cudbi, wax soo saarkiisuna hoos ayuu u dhacayaa, qiimuhuna sidoo kale wuu kor u kacayaa;
Intaa waxaa dheer, wakiilada etherifying-ka ee sida chloroacetic acid (sumowga aadka u badan) iyo ethylene oxide (kansarka keena) ayaa sidoo kale aad u waxyeello badan u leh jirka aadanaha iyo deegaanka.
Cutubkan, cellulose-ka geedka loo yaqaan 'pine cellulose' oo leh nadiifnimo qaraabo ah oo ka badan 90% laga soo saaray cutubka labaad ayaa loo isticmaalaa sidii walxaha ceeriin ah, sodium chloroacetate iyo 2-chloroethanol-na waxaa loo isticmaalaa beddel ahaan.
Isticmaalka aashitada chloroacetic-ga aadka u sunta ah sida wakiilka etherifying, anioniccellulose-ka carboxymethyl (CMC), cellulose-ka aan ionic ahayn ee hydroxyethyl ayaa la diyaariyey.
Cellulose (HEC) iyo isku-dhafka hydroxyethyl carboxymethyl cellulose (HECMC) saddex ether cellulose ah. hal arrin
Farsamooyinka diyaarinta ee saddex ether cellulose ah waxaa lagu habeeyay tijaabooyin iyo tijaabooyin orthogonal ah, ethers-ka cellulose ee la sameeyayna waxaa lagu gartaa FT-IR, XRD, H-NMR, iwm.
Aasaaska etherification-ka cellulose
Mabda'a etherification-ka cellulose waxaa loo qaybin karaa laba qaybood. Qaybta koowaad waa habka alkalization-ka, taas oo ah, inta lagu jiro falgalka alkalization-ka ee cellulose-ka,
Iyadoo si siman loogu kala firdhiyey xalka NaOH, cellulose-ka geedku si xoog leh ayuu u bararaa iyadoo la adeegsanayo walaaqidda farsamada, iyo ballaarinta biyaha.
Tiro badan oo ah molecules yaryar oo NaOH ah ayaa galay gudaha cellulose-ka geedka pine, waxayna la falgaleen kooxaha hydroxyl ee ku yaal giraanta cutubka qaab-dhismeedka gulukooska,
Waxay soo saartaa cellulose alkali ah, oo ah xarunta firfircoon ee falgalka etherification.
Qaybta labaad waa habka etherification-ka, taas oo ah, falcelinta u dhaxaysa xarunta firfircoon iyo sodium chloroacetate ama 2-chloroethanol xaaladaha alkaline, taasoo keenta
Isla mar ahaantaana, wakiilka etherifying sodium chloroacetate iyo 2-chloroethanol ayaa sidoo kale soo saari doona heer gaar ah oo biyo ah xaaladaha alkaline.
Falcelinta dhinaca waxaa lagu xalliyaa inay soo saaraan sodium glycolate iyo ethylene glycol, siday u kala horreeyaan.
2 Daaweynta ka hor inta aan la isticmaalin alkali decrystallization ee cellulose-ka geedka pine
Marka hore, diyaari xoogaa dareere ah oo NaOH ah oo leh biyo la dhalaaliyay. Kadib, heerkul gaar ah, 2g oo ah faybar geed ah.
Fiitamiinka waxaa lagu milmaa mug gaar ah oo ah xalka NaOH, waxaana la walaaqaa muddo, ka dibna waxaa la sifeeyaa si loo isticmaalo.
Soo-saaraha Moodeelka Qalabka
Mitirka pH ee Saxda ah
Nooca ururiyaha kuleyliyaha heerkulka joogtada ah ee walaaqaha magnetic
Foornada qalajinta faakuumka
Hadhaaga elektaroonigga ah
Nooca biyaha wareegaya ee bamka faakuumka ee ujeedo badan leh
Spectrometer-ka Fourier Transform Infrared Spectrometer-ka
Cabbiraha kala-soocidda raajada X-ray
Qalabka Cabbiraadaha Resonance Magnetic-ga Nukliyeerka
Shirkadda Aolilong Instrument Co., Ltd.
Shirkadda Qalabka Qalabka ee Hangzhou Huichuang, Ltd.
Shirkadda Qalabka Tijaabada ee Shanghai Jinghong, Ltd.
Shirkadda METTLER TOLEDO Instruments (Shanghai) Co., Ltd.
Shirkadda Qalabka Sayniska iyo Waxbarashada ee Hangzhou David, Ltd.
Shirkadda American Thermo Fisher Co., Ltd.
Shirkadda ARL ee Mareykanka ee Thermoelectric Switzerland
Shirkadda Swiss-ka ah ee BRUKER
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Diyaarinta CMC-yada
Isticmaalka cellulose alkali alkali oo alwaax geed ah oo hore loogu daaweeyay decrystallization alkali ah oo xoog leh sida walxo cayriin ah, isticmaalka ethanol sida dareeraha iyo isticmaalka sodium chloroacetate sida etherification
CMC oo leh DS sare ayaa la diyaariyey iyadoo lagu daray alkali laba jeer iyo wakiilka etherifying laba jeer. Ku dar 2g oo ah cellulose alkali alwaax geed ah weelka afar-qoorta leh, ka dibna ku dar mug gaar ah oo dareere ethanol ah, oo si fiican u walaaq 30 daqiiqo.
ku saabsan, si cellulose-ka alkaligu si buuxda u kala firdho. Kadib ku dar xaddi cayiman oo ah wakiilka alkali iyo sodium chloroacetate si aad uga falceliso muddo ah heerkulka etherification gaar ah.
Waqti ka dib, ku dar labaad oo ah wakiilka alkaline iyo sodium chloroacetate ka dibna ku dar etherification muddo ah. Ka dib marka falgalku dhammaado, qabooji oo qabooji, ka dibna
Ku dhex milmi xaddi ku habboon oo ah aashitada glacial acetic acid, ka dibna nuug shaandhada, dhaq oo qalaji.
Diyaarinta HEC-yada
Isticmaalka cellulose alkali alkali oo alwaax geed ah oo hore loogu daaweeyay iyadoo la isticmaalayo alkali disintegralization oo xoog leh sida walxo cayriin ah, ethanol oo ah dareere iyo 2-chloroethanol oo ah etherification
HEC oo leh MS sare waxaa la diyaariyey iyadoo lagu daray alkali laba jeer iyo walax etherifying ah laba jeer. Ku dar 2g oo ah cellulose alkali alwaax geed ah weel afar-qoor leh, oo ku dar mug gaar ah oo ah ethanol 90% (jajab mugga) ah, walaaq.
Walaaq muddo si aad si buuxda u kala firdhiso, ka dibna ku dar xaddi gaar ah oo alkali ah, oo si tartiib tartiib ah u kululee, ku dar mug gaar ah oo ah 2-
Chloroethanol, oo lagu ether gareeyay heerkul joogto ah muddo ah, ka dibna lagu daray soodhiyam hydroxide oo haray iyo 2-chloroethanol si ay u sii wadaan etherification muddo ah.
Ka dib marka falgalka la dhammeeyo, ku dhex milmi xaddi cayiman oo ah aashitada glacial acetic, ugu dambayntiina ku shaandhee shaandho galaas ah (G3), dhaq, oo qalaji.
Diyaarinta HEMCC
Iyadoo la adeegsanayo HEC oo lagu diyaariyey 3.2.3.4 sida walxaha ceeriin ah, ethanol oo ah habka falcelinta, iyo sodium chloroacetate oo ah wakiilka etherifying si loo diyaariyo
HECMC. Habka gaarka ah waa: qaado xaddi cayiman oo HEC ah, ku rid dhalo afar-qoorta ah oo 100 mL ah, ka dibna ku dar xaddi cayiman oo mug ah
90% ethanol, si farsamo ahaan u walaaq muddo ah si uu si buuxda u kala firdho, ku dar xaddi gaar ah oo alkali ah ka dib marka la kululeeyo, oo si tartiib tartiib ah ugu dar.
Sodium chloroacetate, etherification-ka heerkulka joogtada ah wuxuu ku dhammaadaa muddo ka dib. Ka dib marka falgalka la dhammeeyo, ku dhex milmi glacial acetic acid si aad u dhexdhexaadiso, ka dibna isticmaal shaandho galaas ah (G3)
Ka dib shaandhaynta nuugista, dhaqidda iyo qallajinta.
Nadiifinta ether-ka cellulose
Habka diyaarinta ether-ka cellulose, qaar ka mid ah waxyaabaha ka soo baxa ayaa badanaa la soo saaraa, gaar ahaan milixda aan dabiiciga ahayn ee sodium chloride iyo qaar kale oo ka mid ah.
wasakhda. Si loo hagaajiyo tayada ether-ka cellulose, si fudud ayaa loo nadiifiyay ether-ka cellulose ee la helay. sababtoo ah waxay ku jiraan biyo.
Waxaa jira milmi kala duwan, sidaa darteed tijaabadu waxay isticmaashaa qayb mug gaar ah oo ethanol ah si loo nadiifiyo saddexda ether ee cellulose ee la diyaariyey.
isbeddel.
Ku rid muunadda ether-ka cellulose-ka ee lagu diyaariyey tayo gaar ah weel, ku dar xaddi go'an oo ah ethanol 80% oo la kululeeyay ilaa 60 ℃ ~ 65 ℃, oo ku hay walaaqidda farsamada heerkul joogto ah 60 ℃ ~ 65 ℃ walaaqaha birlabta kululaynta heerkulka joogtada ah muddo 10 ℃ ah. Ka saar subagga si uu u qalalo.
Weel nadiif ah ku rid, isticmaal nitrate qalin ah si aad u hubiso ion-yada koloriinta. Haddii ay jirto daadasho cad, ku shaandhee shaandho galaas ah oo qaado adag.
Ku celi tallaabooyinkii hore ee qaybta jirka, ilaa shaandhaynta ka dib marka lagu daro 1 dhibic oo ah xalka AgNO3 aysan lahayn wax cad oo soo daadanaya, taas oo ah, nadiifinta iyo dhaqiddu way dhammaadaan.
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ku dhex mil (inta badan si looga saaro NaCl-ka falcelinta ee ka soo baxa wax soo saarka). Ka dib shaandhaynta, qalajinta, qaboojinta heerkulka qolka iyo miisaanka.
cuf, g.
Hababka Tijaabada iyo Astaamaha ee Cellulose Ethers
Go'aaminta Heerka Beddelka (DS) iyo Heerka Beddelka Molar (MS)
Go'aaminta DS: Marka hore, miisaan 0.2 g (sax ah ilaa 0.1 mg) oo ah muunadda ether-ka cellulose ee la safeeyey iyo kuwa la qalajiyey, ku milmi
80mL oo biyo la sifeeyay ah, oo lagu walaaqo biyo kulul oo heerkul joogto ah leh 30℃ ~ 40℃ muddo 10 daqiiqo ah. Kadibna ku hagaaji xalka sulfuric acid ama xalka NaOH.
pH-ga xalka ilaa pH-ga xalka uu noqdo 8. Kadibna weel ku qalabaysan elektroodh cabbira pH ah, isticmaal xal caadi ah oo ah aashitada sulfuric.
Si aad u titrate gareyso, xaaladaha walaaqaya, fiiri akhrinta mitirka pH inta titrate gareyso, marka qiimaha pH ee xalka loo hagaajiyo 3.74,
Titration-ku wuu dhammaanayaa. Fiiro gaar ah u yeelo mugga xalka caadiga ah ee sulfuric acid ee la isticmaalo waqtigan.
Jiilka:
Wadarta tirooyinka proton-ka sare iyo kooxda hydroxyethyl
Saamiga tirada protons-ka sare; I7 waa cufka kooxda methylene ee kooxda hydroxyethyl
Xoogga sare ee falcelinta proton; waa xoojinta ugu sarreysa ee falcelinta proton ee 5 kooxood oo methine ah iyo hal koox oo methylene ah oo ku taal cutubka gulukooska cellulose
Wadarta.
Hababka tijaabada ah ee lagu sharraxay tijaabada astaamaha infrared-ka ee saddexda ether cellulose CMC, HEC iyo HEECMC
Sharciga
3.2.4.3 Tijaabada XRD
Tijaabada Astaamaha Falanqaynta Kala-baxa X-ray ee Saddex Cellulose Ethers CMC, HEC iyo HEECMC
habka tijaabada ee lagu sharraxay.
3.2.4.4 Tijaabada H-NMR
Qalabka cabbira H NMR ee HEC waxaa lagu cabbiray qalabka cabbira Avance400 H NMR ee uu soo saaray BRUKER.
Iyadoo la isticmaalayo dimethyl sulfoxide oo ah dareere, xalka waxaa lagu tijaabiyay dareere hydrogen NMR spectroscopy. Inta jeer ee tijaabada la qaaday waxay ahayd 75.5MHz.
Diiran, xalka waa 0.5 ml.
3.3 Natiijooyinka iyo Falanqayn
3.3.1 Hagaajinta habka diyaarinta CMC
Iyadoo la adeegsanayo cellulose-ka geedka loo yaqaan 'pine cellulose' ee laga soo saaray cutubka labaad sidii walxo ceeriin ah, iyo iyadoo la isticmaalayo sodium chloroacetate oo ah wakiilka etherifying, habka tijaabada hal-cutub ayaa la qaatay,
Habka diyaarinta ee CMC waa la hagaajiyay, doorsoomayaasha bilowga ah ee tijaabadana waxaa loo dejiyay sida ku cad Shaxda 3.3. Kuwa soo socda waa habka diyaarinta HEC.
Farshaxanka, falanqaynta arrimo kala duwan.
Shaxda 3.3 Qiimaha Qodobka Hore
Qiimaha bilowga ah ee qodobka
Heerkulka alkaliinta kahor daaweynta/℃ 40
Waqtiga alkaliinta kahor daaweynta/saacaddii 1
Saamiga dareeraha adag ee ka horreeya daaweynta/(g/mL) 1:25
Isugeynta dareeraha ka hor daaweynta/% 40
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Heerkulka etherification-ka heerka koowaad / ℃ 45
Waqtiga etherification-ka marxaladda koowaad/saacaddii 1aad
Heerkulka etherification-ka heerka labaad/℃ 70
Waqtiga etherification-ka marxaladda labaad/saacaddii 1aad
Qiyaasta salka ah ee marxaladda etherification/g 2
Cadadka wakiilka etherifying ee marxaladda etherification/g 4.3
Saamiga adag iyo dareeraha la etherified/(g/mL) 1:15
3.3.1.1 Saamaynta arrimo kala duwan oo ku saabsan heerka beddelka CMC ee marxaladda alkaliyeynta kahor daaweynta
1. Saamaynta heerkulka alkaliyeynta kahor daaweynta heerka beddelka CMC
Si loo tixgeliyo saameynta heerkulka alkalization-ka kahor daaweynta uu ku leeyahay heerka beddelka ee CMC-ga la helay, marka la eego hagaajinta arrimo kale sida qiimayaasha bilowga ah,
Xaaladaha hoos yimaada, saameynta heerkulka alkaliyeynta ka hor daaweynta ee heerka beddelka CMC ayaa laga wada hadlay, natiijooyinkana waxaa lagu muujiyay Jaantuska.
Heerkulka alkaliinta kahor daaweynta / ℃
Saamaynta heerkulka alkaliinta kahor daaweynta ee heerka beddelka CMC
Waxaa la arki karaa in heerka beddelka CMC uu kordho marka heerkulka alkaliin-ka kahor daaweynta la kordhiyo, heerkulka alkaliin-kana uu yahay 30 °C.
Heerarka beddelka ee kor ku xusan ayaa hoos u dhaca marka heerkulku sii kordho. Tani waxay sabab u tahay heerkulka alkaliinta oo aad u hooseeya, molecules-kuna way yar yihiin oo ma awoodaan inay
Si wax ku ool ah u burburi aagga kristalinta ee cellulose, taas oo adkeyneysa in wakiilka etherifying uu galo gudaha cellulose marxaladda etherification, heerka falcelintuna waa mid aad u sarreeya.
hooseeya, taasoo keenta heer hoose oo beddelka badeecada ah. Si kastaba ha ahaatee, heerkulka alkaliyeynta waa inaanu aad u sarreyn. Marka heerkulku kordho, iyadoo heerkulku uu shaqeynayo heerkul sare iyo alkali xooggan,
Cellulose waxay u nugul tahay burburka oksaydhka, heerka beddelka CMC-na wuu yaraadaa.
2. Saamaynta waqtiga alkaliinization-ka kahor daaweynta ee heerka beddelka CMC
Marka heerkulka alkaliyeynta kahor daaweynta uu yahay 30 °C iyo arrimo kale ayaa ah qiimayaasha bilowga ah, saameynta waqtiga alkaliyeynta kahor daaweynta ee CMC ayaa laga wada hadlayaa.
Saamaynta beddelka. Heerka beddelka
Waqtiga alkaliinta kahor daaweynta/saacaddii
Saamaynta waqtiga alkaliin-ka kahor daaweyntaCMCshahaadada beddelka ah
Habka isku-darka laftiisu waa mid degdeg ah, laakiin xalka alkali wuxuu u baahan yahay waqti faafin gaar ah oo ku jira faybarka.
Waxaa la arki karaa marka waqtiga alkaliin-ku uu yahay 0.5-1.5 saacadood, heerka beddelka badeecaddu wuu kordhaa marka uu sii kordho waqtiga alkaliin-ku.
Heerka beddelka badeecada la helay wuxuu ahaa kii ugu sarreeyay markii waqtigu ahaa 1.5 saacadood, heerka beddelkana wuu yaraadaa marka uu kordho waqtiga 1.5 saacadood ka dib. Tani waxay awood u yeelan kartaa
Waxaa laga yaabaa inay sabab u tahay bilowga alkaliyeynta, iyadoo la dheereynayo waqtiga alkaliyeynta, gelinta alkali ee cellulose ayaa ku filan, sidaa darteed faybarku wuxuu
Qaab-dhismeedka ugu muhiimsan ayaa aad u dabacsan, isagoo kordhinaya wakiilka etherifying iyo habka firfircoon.
Waqtiga boostada: Abriil-26-2024