Cellulose Ether oo ku jira Epoxy Resin

Cudbiga qashinka ah iyo balka waxaa loo isticmaalaa sida alaabta ceeriin, waxaana lagu shubaa alkaliether cellulosehoos ficilka 18% alkali iyo taxane ah oo lagu daro. Kadib isticmaal xabagta epoxy si aad u tallaalto, saamiga molar ee xabka epoxy iyo fiber alkali waa 0.5: 1.0, heerkulka falcelinta waa 100°C, waqtiga falcelinta waa 5.0h, qiyaasta kicinta waa 1%, iyo heerka grafting etherification waa 32%. Eter-ka epoxy cellulose ee la helay waxaa lagu dhex daray 0.6mol Cel-Ep iyo 0.4mol CAB si loo soo saaro badeecad cusub oo daahan leh oo leh waxqabad wanaagsan. Qaab dhismeedka badeecada waxaa lagu xaqiijiyay IR.

Erayada muhiimka ah:ether cellulose; isku-duubnida; CAB; guryaha daahan

Cellulose ether waa polymer-dabiiciga ah, kaas oo lagu sameeyay uumiβ-glucose. Cellulose waxay leedahay heerar sare oo polymerization, darajo wanaagsan oo jihayn, iyo xasilooni kiimikaad oo wanaagsan. Waxaa lagu heli karaa iyadoo kiimikaad lagu daweeyo cellulose (esterification ama etherification). Taxane ka mid ah derivatives cellulose, alaabta kuwan waxaa si weyn loo isticmaalaa in balaastiig, sanduuqyada qadada biodegradable, daahan baabuurta-dhamaadka sare, qaybo auto, daabacaadda khad, koollada, iwm. Waqtigan xaadirka ah, noocyo cusub oo cellulose wax laga beddelay ayaa si joogto ah u soo baxaya, iyo beeraha codsiga waa si joogto ah u balaadhinta, si tartiib tartiib ah u sameysa nidaamka warshadaha fiber. Mawduucan waa in la isticmaalo balka ama suufka wasakhda ah si loogu shubo fiilooyinka gaaban by lye, ka dibna si kiimiko ah lagu tallaalo oo la beddelo si loo sameeyo nooc cusub oo dahaar ah oo aan lagu soo sheegin dukumeentiga.

1. Tijaabi

1.1 Reagents iyo qalabka

Cudbiga qashinka ah (la dhaqay oo la qalajiyey), NaOH, 1,4-butanediol, methanol, thiourea, urea, resin epoxy, acetic anhydride, butyric acid, trichloroethane, formic acid, glioxal, toluene, CAB, iwm. (Nadiiftu waa darajada CP) . Magna-IR 550 spectrometer infrared spectrometer oo ay soo saartay Shirkadda Nicolet ee Maraykanka ayaa loo isticmaalay in lagu diyaariyo muunada iyada oo daahan tetrahydrofuran dareere ah. Viscometer Tu-4, FVXD3-1 nooca heerkulka joogtada ah ee is-xakamaynta kiriyaha falcelinta kicinta korontada, oo ay soo saartay Weihai Xiangwei Kiimikada Warshada; viscometer wareeg ah NDJ-7, nooca Z-10MP5, oo ay soo saartay Shanghai Tianping Instrument Factory; Miisaanka molecular waxaa lagu qiyaasaa Ubbelohde viscosity; Diyaarinta iyo tijaabinta filimka rinjiga waa in lagu fuliyaa si waafaqsan heerka qaranka GB-79.

1.2 Mabda'a falcelinta

1.3 Qalabaynta

Synthesis of epoxy cellulose: Ku dar 100g oo fiber cudbi ah oo la jarjaray si joogto ah heerkulka is-xakamaynta kicinta koronto, ku dar oksaydhiyaha oo ka falcelisa 10 daqiiqo, ka dibna ku dar aalkolo iyo alkali si aad u samayso lye leh fiirsashada 18%. Ku dar dar-dariyeyaasha A, B, iwm. si uur u yeesho. Ka fal celi heerkul cayiman oo faaruq ah 12 saacadood, shaandhr, qallaji oo miisaan 50g oo cellulose alkalized ah, ku dar dareere isku dhafan si aad u samayso slurry, ku dar kicinta iyo resin epoxy leh miisaan gaar ah, kuleyl ilaa 90 ~ 110℃Dareen-celinta etherification 4.0 ~ 6.0h ilaa fal-celinta fal-celintu ay tahay mid aan caqli-gal ahayn. Ku dar aashitada formic si aad u baabi'iso oo aad uga saarto alkali dheeraadka ah, kala saar xalka aqueous iyo dareeraha, ku dhaq 80℃biyo kulul si ay u soo saaraan cusbada sodium, oo ay u engegaan isticmaalka dambe. Mawduucyada gudaha waxaa lagu cabbiray viskometer-ka Ubbelohde iyo celceliska mawduuca-koobka unugyada waxaa loo xisaabiyay si waafaqsan suugaanta.

Acetate butyl cellulose waxaa loo diyaariyaa sida waafaqsan habka suugaanta, miisaankeedu yahay 57.2g oo suuf la safeeyey, ku dar 55g oo ah acetic anhydride, 79g of butyric acid, 9.5g of magnesium acetate, 5.1g of sulfuric acid, isticmaal butyl acetate sida dareere ah, oo ka falcelisa heerkul gaar ah ilaa laga gaadhayo , dhexdhexaadin lagu darayo sodium acetate, degdegay, la sifeeyay, la dhaqay, la sifeeyay, oo la qalajiyey si hadhow loo isticmaalo. Qaado Cel-Ep, ku dar qadarka saxda ah ee CAB iyo dareere isku dhafan oo gaar ah, kuleyli oo walaaq ilaa 0.5h si aad u sameysid dareere dhumuc weyn leh, diyaarinta filimka daahan iyo tijaabada waxqabadka waxay raacdaa habka GB-79.

Go'aaminta heerka esterification of acetate cellulose: marka hore milmaan cellulose acetate in dimethyl sulfoxide, ku dar qadar mitir ah xal alkali si ay u kululeeyo iyo hydrolyzed, iyo titrate xal hydrolyzed leh xal heerka NaOH si loo xisaabiyo wadarta isticmaalka alkali. Go'aaminta waxa ku jira biyaha: Ku rid saamiga foornada 100-105°C si aad u qallajiso 0.2h, miisaan oo xisaabi nuugista biyaha ka dib qaboojinta. Go'aaminta nuugista alkali: miisaan muunad qiyaas ah, ku mil biyo kulul, ku dar tilmaame violet methyl, ka dibna titrate 0.05mol/L H2SO4. Go'aaminta shahaadada ballaarinta: Miisaan 50g muunad, burburi oo geli tuubo qalin-jabinaysa, akhri mugga ka dib gariir koronto, oo barbar dhig mugga budada cellulose-ka aan alkalinka ahayn si aad u xisaabiso shahaadada ballaarinta.

2. Natiijooyinka iyo doodaha

2.1 Xiriirka ka dhexeeya feejignaanta alkali iyo heerka bararka cellulose

Dareen-celinta cellulose oo leh qayb gaar ah oo xal NaOH ah waxay burburin kartaa crystallization joogto ah iyo nidaamsan ee cellulose waxayna ka dhigi kartaa cellulose barar. Iyo hoos u dhacyo kala duwan ayaa ku dhaca lye, yaraynta heerka polymerization. Tijaabooyinku waxay muujinayaan in heerka bararka cellulose-ka iyo xaddiga alkali-ku-xidhka ama xayeysiinta ay kordhiso xoojinta alkali. Heerka hydrolysis wuxuu kordhiyaa kororka heerkulka. Marka fiirsashada alkaligu gaadho 20%, heerka hydrolysis waa 6.8% at t=100°C; heerka hydrolysis waa 14% at t=135°C. Isla mar ahaantaana, tijaabadu waxay muujinaysaa in marka alkali uu ka badan yahay 30%, heerka hydrolysis ee maqaarka silsiladda cellulose ayaa si weyn hoos ugu dhacay. Marka fiirsashada alkaligu gaadho 18%, awoodda adsorption iyo heerka bararka biyaha ayaa ah ugu badnaan, fiirsashada ayaa sii socota inay kordhiso, si aad ah ayey hoos ugu dhacdaa taagga, ka dibna si tartiib ah ayey isu beddeshaa. Isla mar ahaantaana, isbeddelkani wuxuu aad ugu nugul yahay saameynta heerkulka. Marka la eego isla feejignaanta alkali, marka heerkulku hooseeyo (<20°C), heerka bararka cellulose waa weyn yahay, iyo qadarka adsorption ee biyaha waa weyn; Heerkulka sare, heerka bararka iyo qadarka biyaha ayaa ah mid muhiim ah. dhimo.

Fiilooyinka alkali leh ee ka kooban biyo kala duwan iyo alkaliyada waxaa lagu go'aamiyay habka falanqaynta raajada sida waafaqsan suugaanta. Hawlgalka dhabta ah, 18% ~ 20% lye ayaa loo isticmaalaa si loo xakameeyo heerkulka falcelinta qaarkood si loo kordhiyo heerka bararka cellulose. Tijaabooyinku waxay muujinayaan in cellulose ay ka falcelisay kuleyliyaha 6 ~ 12h lagu kala diri karo dareerayaasha polar. Iyada oo ku saleysan xaqiiqadan, qoraagu wuxuu qabaa in milanka cellulose uu door muhiim ah ka ciyaaro heerka burburka bond hydrogen ee u dhexeeya molecules cellulose ee qaybta crystalline, oo ay ku xigto heerka burburinta bond hydrogen ee kooxaha gulukooska intramolecular C3-C2. Heerarka weyn ee burburka dammaanadda hydrogen-ka, waxaa sii badanaya heerka bararka fiber-ka alkali, iyo bond bond-ka si buuxda ayaa loo burburiyay, iyo hydrolyzate ugu dambeeya waa walax biyo-milmi leh.

2.2 Saamaynta dardar-geliyaha

Ku darida khamriga-karka sare leh inta lagu jiro alkalization cellulose waxay kordhin kartaa heerkulka falcelinta, iyo ku darida xaddi yar oo kicinta ah sida khamriga hoose iyo thiourea (ama HOL) waxay si weyn kor ugu qaadi kartaa dhexgalka iyo bararka cellulose. Marka qiyaasta alkoholku korodho, nuugista alkali ee cellulose ayaa kordheysa, waxaana jira isbeddel degdeg ah marka diiradda la saaro 20%, taas oo noqon karta in khamriga monofunctional uu galo unugyada cellulose si ay u sameeyaan bond bonds leh cellulose, ka hortagga cellulose molecules Xidhiidhada hydrogen ee u dhexeeya silsiladaha iyo silsiladaha molecular waxay kordhiyaan heerka khalkhalka, waxay kordhiyaan aagga dusha sare, waxayna kordhiyaan qadarka adsorption alkali. Si kastaba ha ahaatee, isla shuruudo isku mid ah, nuugista alkali ee jajabyada alwaaxdu waa hooseeyaa, iyo qalooca ayaa isbeddelaya xaalad isbeddelaysa. Waxaa laga yaabaa inay la xiriirto maadada yar ee cellulose ee jajabyada alwaax, taas oo ka kooban qadar badan oo lignin ah, taas oo caqabad ku ah dhexgalka khamriga, oo leh caabbinta biyaha iyo caabbinta alkali.

2.3 Etherification

Ku dar 1% B kicinta, xakamee heerkulka falcelinta ee kala duwan, oo samee wax ka beddelka etherification leh resin epoxy iyo fiber alkali. Dhaqdhaqaaqa falcelinta etherification ayaa ku yar 80°C. Heerka tallaalka ee Cel waa 28% oo keliya, iyo hawsha etherification ayaa ku dhow labanlaabantay 110°C. Iyadoo la tixgelinayo xaaladaha falcelinta sida dareeraha, heerkulka falcelintu waa 100°C, iyo waqtiga falcelinta waa 2.5h, iyo heerka grafting ee Cel wuxuu gaari karaa 41%. Intaa waxaa dheer, marxaladda bilowga ah ee falcelinta etherification (<1.0h), sababtoo ah falcelinta kala duwan ee u dhexeeya alkali cellulose iyo epoxy resin, heerka tallaalka ayaa hooseeya. Kordhinta darajada etherification Cel, waxay si tartiib tartiib ah isu beddeshaa falcelin isku mid ah, markaa falcelinta Dhaqdhaqaaqa ayaa si xoog leh u kordhay, heerka tallaalka ayaa kordhay.

2.4 Xiriirka ka dhexeeya heerka tallaalka Celinta iyo milanka

Tijaabooyinku waxay muujiyeen in ka dib markii lagu tallaalo resin epoxy leh cellulose alkali, sifooyinka jireed sida viscosity sheyga, adhesion, caabbinta biyaha, iyo xasiloonida kulaylka ayaa si weyn loo hagaajin karaa. Tijaabada milanka Alaabta leh heerka tallaalka Cel-celiska <40% waxa lagu milmi karaa alkohol-ester-ka hoose, resin alkyd, resin polyacrylic acid, acrylic pimaric acid iyo resins kale. Xabagta Cel-Ep waxay leedahay saamayn milmiyeed cad.

Isku-darka tijaabada filimka dahaarka, isku-darka leh heerka grafting ee 32% ~ 42% guud ahaan waxay leeyihiin iswaafajin wanaagsan, iyo isku-darka heerka tallaalka <30% waxay leeyihiin iswaafajin liidata iyo dhaldhalaalka hooseeya ee filimka daahan; heerka grafting ayaa ka sarreeya 42%, caabbinta biyaha karkaraya, caabbinta khamriga, iyo caabbinta dareeraha organic polar ee filimka daahan waa la dhimay. Si loo wanaajiyo iswaafajinta walxaha iyo waxqabadka daahan, qoraagu wuxuu ku daray CAB sida ku cad qaacidada shaxda 1 si loo sii milmo oo wax looga beddelo si kor loogu qaado wada-noolaanshaha Cel-Ep iyo CAB. Isku darku wuxuu sameeyaa hannaan isku mid ah oo qiyaas ah. Dhumucda isku dhafka ka kooban ee isku darka waxay u egtahay mid aad u dhuuban oo isku day inaad ku jirto xaalada nano-unugyada.

2.5 Xiriirka ka dhexeeya Cel-Saamiga isku dhafka Ep/CAB iyo sifooyinka jireed

Isticmaalka Cel-Ep si loogu daro CAB, natiijooyinka tijaabada daahan ayaa muujinaya in acetate cellulose ay si weyn u wanaajin karto sifooyinka daahan ee walxaha, gaar ahaan xawaaraha qalajinta. Qaybta saafiga ah ee Cel-Ep way adagtahay in lagu qalajiyo heerkulka qolka. Ka dib marka lagu daro CAB, labada walxood waxay leeyihiin dhammaystir waxqabad oo muuqda.

2.6 FTIR ogaanshaha spectrum

3. Gabagabo

(1) Cudbi cellulose wuxuu barari karaa 80°C leh> 18% alkali uruursan iyo taxane ah oo lagu daro, kordhiya heerkulka falcelinta, kordhiso waqtiga falcelinta, kordhiso heerka bararka iyo nabaad-guurka ilaa ay si buuxda u biyo-saarto.

(2) Falcelinta Etherification, saamiga quudinta molarka ee Cel-Ep waa 2, heerkulka falcelinta waa 100°C, waqtigu waa 5h, qiyaasta kicinta waa 1%, iyo heerka tallaalka etherification wuxuu gaari karaa 32% ~ 42%.

(3) Wax ka beddelka isku-dhafka, marka saamiga molarka ee Cel-Ep: CAB = 3: 2, waxqabadka badeecada la isku daray ayaa wanaagsan, laakiin Cel-Ep saafi ah looma isticmaali karo dahaar ahaan, kaliya sida koolo.