I-Cellulose Ether ku-Epoxy Resin

Imfucuza ikotini kanye ne-sawdust isetshenziswa njengezinto ezingavuthiwe, futhi i-hydrolyzed ibe yi-alkalii-cellulose etherngaphansi kwesenzo se-alkali engu-18% kanye nochungechunge lwezithako. Bese usebenzisa i-epoxy resin ukuxhunyelelwa, isilinganiso se-molar ye-epoxy resin ne-alkali fiber ngu-0.5:1.0, izinga lokushisa lokuphendula liyi-100.°C, isikhathi sokuphendula ngu-5.0h, umthamo we-catalyst ngu-1%, futhi izinga lokuxhunyelelwa kwe-etherification lingama-32%. I-epoxy cellulose ether etholiwe ihlanganiswe ne-0.6mol Cel-Ep kanye ne-0.4mol CAB ukuze kuhlanganiswe umkhiqizo omusha wokumboza ngokusebenza kahle. Isakhiwo somkhiqizo siqinisekiswe nge-IR.

Amagama angukhiye:i-cellulose ether; ukuhlanganisa; I-CAB; enamathela izakhiwo

I-Cellulose ether iyi-polymer yemvelo, eyakhiwe ukufingqa kweβ- ushukela. I-Cellulose inezinga eliphezulu le-polymerization, izinga elihle lokuma, kanye nokuzinza okuhle kwamakhemikhali. Ingatholwa ngokwelapha i-cellulose ngamakhemikhali (i-esterification noma i-etherification). Uchungechunge lwezinto eziphuma ku-cellulose, le mikhiqizo isetshenziswa kakhulu kumapulasitiki, amabhokisi esidlo sasemini angaboli, okokugcotshwa kwezimoto okusezingeni eliphezulu, izingxenye zezimoto, oyinki bokuphrinta, izinto zokunamathisela, njll. ikhula njalo, kancane kancane yakha uhlelo lwemboni yefiber. Lesi sihloko esokusebenzisa i-sawdust noma udoti kakotini ukuze ugaywe ngamanzi abe imicu emifushane nge-lye, bese ixhunyelelwa ngamakhemikhali bese ilungiswa ukuze kwakhiwe uhlobo olusha lokumboza olungazange lubikwe kudokhumenti.

1. Isivivinyo

1.1 Ama-reagents nezinsimbi

Imfucumfucu kakotini (igeziwe yomiswa), i-NaOH, 1,4-butanediol, i-methanol, i-thiourea, i-urea, i-epoxy resin, i-acetic anhydride, i-butyric acid, i-trichloroethane, i-formic acid, i-glyoxal, i-toluene, i-CAB, njll. (Ubumsulwa yibanga le-CP) . I-Magna-IR 550 infrared spectrometer ekhiqizwe yi-Nicolet Company yase-United States yasetshenziswa ukulungisa amasampula nge-solvent tetrahydrofuran coating. I-viscometer ye-Tu-4, i-FVXD3-1 uhlobo lokushisa oluqhubekayo oluzilawulayo lukagesi olushukumisayo lokusabela, olukhiqizwa yi-Weihai Xiangwei Chemical Machinery Factory; I-viscometer ejikelezayo i-NDJ-7, uhlobo lwe-Z-10MP5, ekhiqizwe i-Shanghai Tianping Instrument Factory; isisindo samangqamuzana silinganiswa nge-viscosity ye-Ubbelohde; Ukulungiswa nokuhlolwa kwefilimu kapende kuzokwenziwa ngokwezinga likazwelonke le-GB-79.

1.2 Umgomo wokusabela

1.3 Ukuhlanganisa

Ukwenziwa kwe-epoxy cellulose: Engeza u-100g wefayibha kakotini osikiwe endaweni eqhubekayo yokushisa kagesi eshukumisayo, engeza i-oxidant bese usabele imizuzu engu-10, bese ufaka utshwala ne-alkali ukuze wenze i-lye ene-concentration engu-18%. Engeza ama-accelerator A, B, njll. ukuze ukhulelwe. Phendula ezingeni lokushisa elithile ngaphansi kwe-vacuum amahora angu-12, hlunga, womile futhi ukale u-50g we-alkalize cellulose, engeza i-solvent exubile ukwenza udaka, engeza i-catalyst ne-epoxy resin enesisindo esithile se-molecule, ukushisa kufika ku-90~110.℃ngokusabela kwe-etherification 4.0~ 6.0h kuze kube yilapho ama-reactants exubana. Faka i-formic acid ukuze unciphise futhi ususe i-alkali eyeqile, uhlukanise isixazululo esimanzi kanye ne-solvent, geza nge-80℃amanzi ashisayo ukususa usawoti we-sodium, futhi wome ukuze usetshenziswe kamuva. I-viscosity yangaphakathi yalinganiswa nge-viscometer ye-Ubbelohde futhi isisindo se-viscosity-avareji ye-molecular yabalwa ngokuvumelana nezincwadi.

I-acetate butyl cellulose ilungiswa ngokwendlela yezincwadi, kala u-57.2g kakotini ocolisisiwe, engeza u-55g we-acetic anhydride, u-79g we-butyric acid, u-9.5g we-magnesium acetate, u-5.1g we-sulfuric acid, sebenzisa i-butyl acetate njenge-solvent, futhi usabele lapho izinga lokushisa elithile kuze kube yilapho lifaneleka, lincishisiwe ngokwengeza i-sodium acetate, imvula, ihlungiwe, igezwe, ihlungiwe, futhi yomiswe ukuze isetshenziswe kamuva. Thatha i-Cel-Ep, engeza inani elifanele le-CAB nesincibilikisthi esithile esixubile, shisa futhi ugovuze amahora angu-0.5 ukuze wenze uketshezi oluwugqinsi olufana nolunye, futhi ukulungiselelwa kwefilimu yokumboza nokuhlola ukusebenza kulandele indlela ye-GB-79.

Ukunqunywa kwezinga le-esterification ye-cellulose acetate: qala ngokuncibilikisa i-cellulose acetate ku-dimethyl sulfoxide, engeza inani elilinganisiwe lesisombululo se-alkali ekushiseni nasekufakweni kwe-hydrolyze, bese ucindezela isixazululo se-hydrolyzed ngesisombululo esijwayelekile se-NaOH ukuze ubale ukusetshenziswa kwe-alkali okuphelele. Ukunqunywa kokuqukethwe kwamanzi: Faka isampula kuhhavini ku-100~105°C ukuze wome u-0.2h, kala futhi ubale ukumuncwa kwamanzi ngemva kokupholisa. Ukunqunywa kokumuncwa kwe-alkali: kala isampula yobuningi, yincibilikise emanzini ashisayo, engeza inkomba ye-methyl violet, bese u-titrate nge-0.05mol/L H2SO4. Ukunqunywa kwedigri yokwandisa: Kala isampula engu-50g, uyichoboze bese uyifaka eshubhuni elineziqu, funda ivolumu ngemva kokudlidliza kukagesi, bese uyiqhathanisa nevolumu yempushana ye-cellulose engafakwanga ukuze ubale idigri yokwandisa.

2. Imiphumela kanye nengxoxo

2.1 Ubudlelwano phakathi kokugxila kwe-alkali kanye nedigri yokuvuvukala kwe-cellulose

Ukusabela kwe-cellulose nge-concentration ethile yesisombululo se-NaOH kungabhubhisa i-crystallization evamile futhi ehlelekile ye-cellulose futhi yenze i-cellulose ikhukhumale. Futhi ukuwohloka okuhlukahlukene kwenzeka ku-lye, kunciphisa izinga le-polymerization. Ukuhlola kubonisa ukuthi izinga lokuvuvukala kwe-cellulose kanye nenani lokubophezela kwe-alkali noma i-adsorption liyakhuphuka ngokugxila kwe-alkali. Izinga le-hydrolysis liyakhula ngokunyuka kwezinga lokushisa. Lapho ukuhlushwa kwe-alkali kufinyelela ku-20%, izinga le-hydrolysis lingu-6.8% ku-t=100°C; izinga le-hydrolysis liyi-14% ku-t=135°C. Ngesikhathi esifanayo, ukuhlola kubonisa ukuthi uma i-alkali ingaphezu kuka-30%, izinga le-hydrolysis ye-cellulose chain scission liyancipha kakhulu. Lapho ukuhlushwa kwe-alkali kufinyelela ku-18%, umthamo wokukhangisa kanye nezinga lokuvuvukala lamanzi liphezulu, ukugxila kuyaqhubeka nokwanda, kwehle kakhulu ethafeni, bese kushintsha kancane kancane. Ngesikhathi esifanayo, lolu shintsho luzwela kakhulu ethonyeni lokushisa. Ngaphansi kokugxilwa kwe-alkali okufanayo, lapho izinga lokushisa liphansi (<20°C), izinga lokuvuvukala kwe-cellulose likhulu, futhi inani le-adsorption lamanzi likhulu; ekushiseni okuphezulu, idigri yokuvuvukala kanye nenani le-adsorption yamanzi libalulekile. nciphisa.

Imicu ye-alkali enokuqukethwe kwamanzi okuhlukile nokuqukethwe kwe-alkali kwanqunywa indlela yokuhlaziya i-X-ray diffraction ngokusho kwezincwadi. Ekusebenzeni kwangempela, i-lye engu-18% ~ 20% isetshenziselwa ukulawula izinga lokushisa elithile lokusabela ukukhulisa izinga lokuvuvukala kwe-cellulose. Ukuhlola kubonisa ukuthi i-cellulose esabela ngokushisisa i-6~12h ingancibilika kuzincibilikisi ze-polar. Ngokusekelwe kuleli qiniso, umbhali ucabanga ukuthi ukuncibilika kwe-cellulose kudlala indima ebalulekile ngezinga lokubhujiswa kwe-hydrogen bond phakathi kwama-molecule e-cellulose engxenyeni ye-crystalline, okulandelwa izinga lokubhujiswa kwe-hydrogen bond yamaqembu e-intramolecular glucose C3-C2. Uma izinga lokubhujiswa kwebhondi ye-hydrogen likhulu, izinga lokuvuvuka kwe-alkali fibre, futhi isibopho se-hydrogen sibhujiswa ngokuphelele, futhi i-hydrolyzate yokugcina iyinto encibilikayo emanzini.

2.2 Umthelela we-Accelerator

Ukwengeza utshwala obushisa kakhulu ngesikhathi sokwenziwa kwe-cellulose alkalization kungakhuphula izinga lokushisa lokusabela, futhi ukwengeza inani elincane le-propellant njengotshwala obuphansi kanye ne-thiourea (noma i-urea) kungakhuthaza kakhulu ukungena nokuvuvukala kwe-cellulose. Njengoba ukugcwala kotshwala kuyanda, ukumuncwa kwe-alkali kwe-cellulose kuyanda, futhi kuba khona ushintsho kungazelelwe lapho ukugxiliswa kwe-alcoho kungu-20%, okungenzeka kube ukuthi utshwala obusebenzayo bungena kuma-molecule e-cellulose ukuze kwakheke izibopho ze-hydrogen ne-cellulose, ukuvimbela i-cellulose. ama-molecule Amabhondi e-hydrogen phakathi kwamaketanga namaketanga amangqamuzana akhuphula izinga lokuphazamiseka, andise indawo engaphezulu, futhi andise inani le-alkali adsorption. Kodwa-ke, ngaphansi kwezimo ezifanayo, ukumuncwa kwe-alkali kwamachips ezinkuni kuphansi, futhi ijika liyashintsha esimweni esishintshashintshayo. Kungase kuhlotshaniswe nokuqukethwe okuphansi kwe-cellulose kuma-chips ezinkuni, aqukethe inani elikhulu le-lignin, elivimbela ukungena kotshwala, futhi linokumelana okuhle kwamanzi nokumelana ne-alkali.

2.3 I-Etherification

Engeza i-1% B catalyst, lawula amazinga okushisa okusabela ahlukene, futhi wenze ukuguqulwa kwe-etherification nge-epoxy resin ne-alkali fiber. Umsebenzi wokusabela kwe-etherification uphansi ku-80°C. Izinga lokuxhunyelelwa kwe-Cel lingama-28% kuphela, futhi umsebenzi wokufaka i-etherification ucishe uphindwe kabili ku-110.°C. Uma ucabangela izimo zokusabela njenge-solvent, izinga lokushisa lokusabela liyi-100°C, futhi isikhathi sokuphendula singu-2.5h, futhi izinga lokuxhunyelelwa likaCel lingafinyelela ku-41%. Ukwengeza, esigabeni sokuqala sokusabela kwe-etherification (<1.0h), ngenxa yokusabela okungafani phakathi kwe-alkali cellulose ne-epoxy resin, izinga lokuxhunyelelwa liphansi. Ngokukhula kwe-Cel etherification degree, kancane kancane iphenduka i-homogeneous reaction, ngakho ukusabela Umsebenzi wanda kakhulu, futhi izinga lokuxhunyelelwa landa.

2.4 Ubudlelwano phakathi kwesilinganiso sokuxhunyelelwa kwe-Cel kanye nokuncibilika

Ukuhlola kubonise ukuthi ngemva kokuxhunyelelwa i-epoxy resin ne-alkali cellulose, izici ezibonakalayo ezifana ne-viscosity yomkhiqizo, ukunamathela, ukumelana kwamanzi, nokuzinza kokushisa kungathuthukiswa kakhulu. Ukuhlolwa kokuncibilika Umkhiqizo onesilinganiso sokuxhunyelelwa kwe-Cel u-<40% ungancibilika ku-alcohol-ester ephansi, i-alkyd resin, i-polyacrylic acid resin, i-acrylic pimaric acid nezinye izinhlaka. I-Cel-Ep resin inomphumela osobala wokuxazululela.

Kuhlanganiswe nokuhlolwa kwefilimu yokugqoka, izingxube ezinezinga lokuxhunyelelwa lika-32% ~ 42% ngokuvamile zinokuhambisana okungcono, futhi izingxube ezinezinga lokuxhunyelelwa elingu-<30% zinokuhambisana okungalungile kanye nokucwebezela okuphansi kwefilimu yokuhlanganisa; izinga lokuxhunyelelwa lingaphezu kwama-42%, ukumelana namanzi abilayo, ukumelana notshwala, kanye nokumelana ne-polar organic solvent yefilimu yokumboza kuyancishiswa. Ukuze kuthuthukiswe ukuhambisana kwezinto kanye nokusebenza kokumboza, umbhali wengeze i-CAB ngokuvumelana nefomula ekuThebula 1 ukuze kuqhutshekwe kuncibilikiswe futhi kulungiswe ukuze kuthuthukiswe ukuba khona ndawonye kwe-Cel-Ep ne-CAB. Ingxube yakha uhlelo lwe-homogeneous cishe. Ugqinsi lwesixhumi esibonakalayo senhlanganisela sithanda ukuba mncane kakhulu futhi sizame ukuba sesimweni sama-nano-cell.

2.5 Ubudlelwano phakathi kukaCel-Isilinganiso se-Ep/CAB sokuxuba kanye nezakhiwo ezibonakalayo

Isebenzisa i-Cel-Ep ukuze ixubane ne-CAB, imiphumela yokuhlolwa kokumboza ikhombisa ukuthi i-cellulose acetate ingathuthukisa kakhulu izakhiwo zokumboza zezinto, ikakhulukazi isivinini sokumisa. Ingxenye emsulwa ye-Cel-Ep inzima ukuyomisa ekamelweni lokushisa. Ngemuva kokwengeza i-CAB, lezi zinto ezimbili zinokuhambisana okusobala kokusebenza.

2.6 Ukutholwa kwe-spectrum ye-FTIR

3. Isiphetho

(1) I-cotton cellulose ingavuvukala ku-80°I-C ene->18% ye-alkali egxilile kanye nochungechunge lwezithasiselo, yandisa izinga lokushisa lokusabela, yandise isikhathi sokusabela, yandise izinga lokuvuvukala nokuwohloka kuze kube yilapho i-hydrolyzed ngokuphelele.

(2) Ukusabela kwe-Etherification, i-Cel-Ep molar feed ratio ingu-2, izinga lokushisa lokusabela liyi-100°C, isikhathi singu-5h, umthamo we-catalyst ngu-1%, futhi izinga lokuxhunyelelwa kwe-etherification lingafinyelela ku-32% ~ 42%.

(3) Ukuguqulwa kokuxutshwa, lapho isilinganiso se-molar se-Cel-Ep:CAB=3:2, ukusebenza komkhiqizo ohlanganisiwe kuhle, kodwa i-Cel-Ep ehlanzekile ayikwazi ukusetshenziswa njenge-coating, kuphela njenge-adhesive.