Cellulose Ether ka Epoxy Resin

Litsila tsa k'hothone le sawdust li sebelisoa e le lisebelisoa tse tala, 'me li entsoe ka hydrolyzed hore e be alkalicellulose ethertlas'a ketso ea 18% ea alkali le letoto la li-additives. Ebe u sebelisa epoxy resin bakeng sa grafting, molar ratio ea epoxy resin le alkali fiber ke 0.5:1.0, mocheso oa karabelo ke 100.°C, nako ea ho arabela ke 5.0h, tekanyo ea catalyst ke 1%, 'me sekhahla sa etherification grafting ke 32%. Epoxy cellulose ether e fumanoeng e kopantsoe le 0.6mol Cel-Ep le 0.4mol CAB ho kopanya sehlahisoa se secha sa ho roala se nang le ts'ebetso e ntle. Sebopeho sa sehlahisoa se tiisitsoe ka IR.

Mantsoe a bohlokoa:cellulose ether; tlhaho; TEKESI; thepa ea ho roala

Cellulose ether ke polima ea tlhaho, e entsoeng ka condensation eaβ- tsoekere. Cellulose e na le tekanyo e phahameng ea polymerization, tekanyo e ntle ea ho sheba, le botsitso bo botle ba lik'hemik'hale. E ka fumanoa ka ho phekola cellulose ka lik'hemik'hale (esterification kapa etherification). Letoto la li-cellulose derivatives, lihlahisoa tsena li sebelisoa haholo ka polasetiki, mabokoseng a lijo tsa motšeare a senyehileng, liphahlo tsa likoloi tse phahameng, likarolo tsa koloi, li-inks tsa khatiso, likhomaretsi, joalo-joalo ho atoloha kamehla, butle-butle ho theha tsamaiso ea indasteri ea fiber. Sehlooho sena ke ho sebelisa sawdust kapa litšila tsa k'hothone ho hydrolyzed hore e be likhoele tse khutšoane ka li-lye, ebe e hlomathisoa ka lik'hemik'hale le ho fetoloa ho theha mofuta o mocha oa ho roala o so kang o tlalehoa tokomaneng.

1. Teko

1.1 Lisebelisoa le lisebelisoa

K'hothone e litšila (e hlatsoitsoeng le e omisitsoeng), NaOH, 1,4-butanediol, methanol, thiourea, urea, epoxy resin, acetic anhydride, butyric acid, trichloroethane, formic acid, glyoxal, toluene, CAB, joalo-joalo (Bohloeki ke CP grade) . Magna-IR 550 infrared spectrometer e hlahisoang ke Nicolet Company ea United States e ile ea sebelisoa ho lokisa lisampole ka ho roala ha solvent tetrahydrofuran. Tu-4 viscometer, FVXD3-1 mofuta o sa khaotseng mocheso intša laola motlakase susumetsang itšoara joang ketlele, e hlahisoang ke Weihai Xiangwei Chemical Machinery Factory; rotational viscometer NDJ-7, mofuta oa Z-10MP5, e hlahisoang ke Shanghai Tianping Instrument Factory; boima ba limolek'hule bo lekantsoe ka Viscosity ea Ubbelohde; Tokiso le tlhahlobo ea filimi ea pente e tla etsoa ho latela maemo a naha a GB-79.

1.2 Molao-motheo oa ho itšoara

1.3 Tšimoloho

Synthesis ea epoxy cellulose: Eketsa 100g ea fiber e khaotsoeng ea k'hothone ho mocheso o sa khaotseng oa motlakase o laolang motlakase, eketsa oxidant 'me u arabe ka metsotso e 10, ebe u eketsa joala le alkali ho etsa lye e nang le motsoako oa 18%. Kenya li-accelerator A, B, joalo-joalo bakeng sa ho ima. Etsa ka mocheso o itseng tlas'a vacuum bakeng sa lihora tse 12, sefa, se omme 'me se be boima ba 50g ea selulose ea alkali, eketsa motsoako o motsoako ho etsa slurry, eketsa catalyst le epoxy resin ka boima bo itseng ba molek'hule, mocheso ho fihlela ho 90 ~ 110.℃bakeng sa karabelo ea etherification 4.0~ 6.0h ho fihlela li-reactants li sa kopane. Eketsa formic acid ho fokotsa le ho tlosa alkali e feteletseng, arola tharollo ea metsi le solvent, hlatsoa ka 80.℃metsi a chesang ho tlosa letsoai la sodium, le ho omisa bakeng sa tšebeliso ea hamorao. The intrinsic viscosity e ne e lekanyetsoa ka viscometer ea Ubbelohde le viscosity-average ea boima ba molek'hule e ne e baloa ho latela lingoliloeng.

Acetate butyl cellulose e lokiselitsoe ho latela mokhoa oa lingoliloeng, boima ba 57.2g ea k'hothone e hloekisitsoeng, eketsa 55g ea acetic anhydride, 79g ea butyric acid, 9.5g ea magnesium acetate, 5.1g ea sulfuric acid, sebelisa butyl acetate e le solvent, 'me u arabe mocheso o itseng ho fihlela o tšoaneleha, o fokotsehile ka ho eketsa sodium acetate, e kolobisitsoeng, e tlhotliloeng, e hlatsuoa, e tlhotliloeng, 'me e omisitsoe hore e sebelisoe hamorao. Nka Cel-Ep, eketsa palo e loketseng ea CAB le solvent e khethehileng e tsoakiloeng, futhumatsa 'me u hlohlelletse bakeng sa 0.5h ho etsa mokelikeli o teteaneng o lekanang,' me tlhahlobo ea filimi ea ho roala le tlhahlobo ea ts'ebetso e latela mokhoa oa GB-79.

Boikemisetso ba tekanyo ea esterification ea cellulose acetate: pele qhala cellulose acetate ka dimethyl sulfoxide, eketsa tekanyo ea metered ea alkali tharollo mocheso le hydrolyze, 'me titrate tharollo ea hydrolyzed ka tharollo e tloaelehileng ea NaOH ho bala kakaretso ea tšebeliso ea alkali. Boikemisetso ba litaba tsa metsi: Beha sampole ka ontong ka likhato tse 100 ~ 105°C ho omella bakeng sa 0.2h, lekanya le ho bala ho monya metsi ka mor'a ho pholile. Boikemisetso ba ho monya alkali: lekanya sampole ea bongata, e qhibilile metsing a chesang, eketsa methyl violet indicator, ebe o titrate ka 0.05mol/L H2SO4. Boikemisetso ba tekanyo ea katoloso: Beha sampuli ea 50g, e silakanye 'me u e kenye ka har'a tube e phethiloeng, bala molumo ka mor'a ho sisinyeha ha motlakase,' me u e bapise le palo ea phofo ea cellulose e sa lekaneng ho bala tekanyo ea ho atolosa.

2. Liphetho le lipuisano

2.1 Kamano pakeng tsa mahloriso a alkali le tekanyo ea ho ruruha ha cellulose

Karabelo ea selulose e nang le motsoako o itseng oa tharollo ea NaOH e ka senya kristale e tloaelehileng le e hlophisehileng ea selulose mme ea etsa hore selulose e ruruhe. 'Me ho senyeha ho fapaneng ho etsahala ka lye, ho fokotsa tekanyo ea polymerization. Liteko li bonts'a hore tekanyo ea ho ruruha ha selulose le palo ea alkali e tlamang kapa adsorption e eketseha ka bongata ba alkali. Tekanyo ea hydrolysis e eketseha ka ho eketseha ha mocheso. Ha motsoako oa alkali o fihla ho 20%, tekanyo ea hydrolysis ke 6.8% ho t = 100.°C; tekanyo ea hydrolysis ke 14% ho t = 135°C. Ka nako e ts'oanang, teko e bontša hore ha alkali e feta 30%, tekanyo ea hydrolysis ea cellulose chain scission e fokotsehile haholo. Ha mahloriso a alkali a fihla ho 18%, matla a adsorption le tekanyo ea ho ruruha ea metsi ke eona e phahameng ka ho fetisisa, mahloriso a tsoela pele ho eketseha, a theoha haholo ho ea sehlabeng, ebe o fetoha butle-butle. Ka nako e ts'oanang, phetoho ena e tsotella haholo tšusumetso ea mocheso. Tlas'a khatello e tšoanang ea alkali, ha mocheso o le tlase (<20°C), tekanyo ea ho ruruha ea selulose e kholo, 'me palo ea adsorption ea metsi e kholo; ka mocheso o phahameng, tekanyo ea ho ruruha le palo ea adsorption ea metsi e bohlokoa. fokotsa.

Likhoele tsa alkali tse nang le metsi a fapaneng le litaba tsa alkali li ile tsa khethoa ke mokhoa oa tlhahlobo ea X-ray diffraction ho latela lingoliloeng. Ts'ebetsong ea 'nete, 18% ~ 20% lye e sebelisoa ho laola mocheso o itseng oa karabelo ho eketsa tekanyo ea ho ruruha ea selulose. Liteko li bonts'a hore selulose e ileng ea arabela ka ho futhumatsa bakeng sa 6 ~ 12h e ka qhibiliha ka har'a li-solvents tsa polar. Ho itšetlehile ka 'nete ena, mongoli o nahana hore ho qhibiliha ha selulose ho phetha karolo ea bohlokoa ka tekanyo ea ho timetsoa ha hydrogen bond pakeng tsa limolek'hule tsa cellulose karolong ea crystalline, e lateloa ke tekanyo ea ho timetsoa ha hydrogen bond ea lihlopha tsa intramolecular glucose C3-C2. Ha tekanyo e kholo ea ho timetsoa ha hydrogen bond, tekanyo e kholo ea ho ruruha ha fiber ea alkali, 'me tlamo ea hydrogen e senyeha ka ho feletseng,' me hydrolyzate ea ho qetela ke ntho e qhibilihang ka metsing.

2.2 Phello ea Accelerator

Ho eketsa joala bo belang haholo nakong ea alkalization ea cellulose ho ka eketsa mocheso oa karabelo, 'me ho eketsa tekanyo e nyane ea propellant joalo ka joala bo tlase le thiourea (kapa urea) ho ka khothaletsa ho kenella le ho ruruha ha selulose haholo. Ha mokelikeli oa joala o ntse o eketseha, ho kenngoa ha alkali ea selulose ho eketseha, 'me ho na le phetoho ea tšohanyetso ha mahloriso a le 20%, e ka' nang ea e-ba hore joala bo sa sebetseng bo kenella ka har'a limolek'hule tsa cellulose ho theha likamano tsa hydrogen le cellulose, ho thibela selulose. Limolek'hule Maqhama a haedrojene pakeng tsa liketane le liketane tsa limolek'hule li eketsa tekanyo ea pherekano, li eketsa sebaka se ka holimo, 'me li eketsa bongata ba alkali adsorption. Leha ho le joalo, tlas'a maemo a tšoanang, ho monya ha alkali ea mapolanka a lehong ho tlaase, 'me lekhalo le fetoha boemong bo feto-fetohang. E ka 'na ea amana le litaba tse tlaase tsa selulose ka lithapo tsa lehong, tse nang le palo e kholo ea lignin, e sitisang ho kenella ha joala,' me e na le ho hanyetsa metsi hantle le ho hanyetsa alkali.

2.3 Etherification

Eketsa 1% B catalyst, laola mocheso o fapaneng oa karabelo, 'me u etse phetoho ea etherification ka epoxy resin le alkali fiber. Ts'ebetso ea etherification e tlase ho 80°C. Sekhahla sa ho hlomathiseletsoa ha Cel ke 28% feela, 'me mosebetsi oa etherification o batla o imena habeli ho 110.°C. Ha re nahana ka maemo a karabelo joalo ka solvent, mocheso oa karabelo ke 100°C, 'me nako ea karabelo ke 2.5h,' me sekhahla sa ho hlomathiseletsoa sa Cel se ka fihla ho 41%. Ho phaella moo, mothating oa pele oa karabelo ea etherification (<1.0h), ka lebaka la karabelo e fapaneng pakeng tsa alkali cellulose le epoxy resin, sekhahla sa ho hlomathisetsoa se tlaase. Ka keketseho ea tekanyo ea Cel etherification, butle-butle e fetoha karabelo e ts'oanang, kahoo karabelo Ts'ebetso e ile ea eketseha haholo, 'me sekhahla sa grafting se ile sa eketseha.

2.4 Kamano pakeng tsa sekhahla sa ho hlomathiseletsoa ha Cel le ho qhibiliha

Liteko li bontšitse hore ka mor'a ho hlomathisetsa epoxy resin le alkali cellulose, thepa ea 'mele e kang viscosity ea sehlahisoa, ho khomarela, ho hanyetsa metsi, le botsitso ba mocheso li ka ntlafatsoa haholo. Teko ea Solubility Sehlahisoa se nang le tekanyo ea Cel grafting <40% se ka qhibiliha ka ester e tlaase ea joala-ester, alkyd resin, polyacrylic acid resin, acrylic pimaric acid le li-resin tse ling. Cel-Ep resin e na le phello e hlakileng ea ho solubilizing.

E kopantsoe le teko ea filimi ea ho roala, ho kopanya ka sekhahla sa 32% ~ 42% ka kakaretso ho na le ho lumellana ho molemo, 'me metsoako e nang le tekanyo ea grafting ea <30% e na le ho se lumellane ho fokolang le khanya e tlaase ea filimi ea ho roala; sekhahla sa ho hlomathiseletsoa se phahame ho feta 42%, ho hanyetsa metsi a belang, ho hanyetsa joala, le khanyetso ea polar organic solvent ea filimi ea ho roala e fokotsehile. E le ho ntlafatsa ho lumellana ha thepa le ts'ebetso ea ho roala, mongoli o kentse CAB ho ea ka foromo e Lethathamong la 1 ho tsoela pele ho qhibiliha le ho fetola ho khothalletsa ho ba teng ha Cel-Ep le CAB. Motsoako o etsa mokhoa o batlang o tšoana. Sebopeho sa sebopeho sa sebopeho sa motsoako se atisa ho ba tšesaane haholo 'me se leka ho ba boemong ba nano-cells.

2.5 Kamano pakeng tsa Cel-Ep/CAB motsoako oa karolelano le thepa ea 'mele

U sebelisa Cel-Ep ho kopanya le CAB, liphetho tsa liteko tsa ho roala li bontša hore cellulose acetate e ka ntlafatsa haholo thepa ea ho roala thepa, haholo lebelo la ho omisa. Karolo e hloekileng ea Cel-Ep e thata ho omisa mocheso oa kamore. Kamora ho kenyelletsa CAB, lisebelisoa tse peli li na le tlatsetso e hlakileng ea ts'ebetso.

2.6 FTIR spectrum lemoha

3. Qetello

(1) Cotton cellulose e ka ruruha ho 80°C ka> 18% e tsepamisitse maikutlo a alkali le letoto la li-additives, eketsa mocheso oa karabelo, lelefatsa nako ea ho itšoara, eketsa tekanyo ea ho ruruha le ho senyeha ho fihlela e le hydrolyzed ka ho feletseng.

(2) Etherification reaction, the Cel-Ep molar feed ratio ke 2, mocheso oa karabelo ke 100°C, nako ke 5h, tekanyo ea catalyst ke 1%, 'me sekhahla sa etherification grafting se ka fihla ho 32% ~ 42%.

(3) Phetoho ea ho kopanya, ha tekanyo ea molar ea Cel-Ep: CAB = 3: 2, ts'ebetso ea sehlahisoa se entsoeng e le ntle, empa Cel-Ep e hloekileng e ke ke ea sebelisoa e le ho roala, feela e le sekhomaretsi.