Indlela yokuhlaziya yezakhiwo ze-physicochemical ze-cellulose ether
Umthombo, isakhiwo, izakhiwo kanye nokusetshenziswa kwe-cellulose ether kwethulwa. Ngenxa yokuhlolwa kwenkomba yempahla ye-physicochemical yezinga lemboni ye-cellulose ether, indlela ecwengisisiwe noma ethuthukisiwe yabekwa phambili, futhi ukuba nokwenzeka kwayo kwahlaziywa ngokuhlolwa.
Amagama angukhiye:i-cellulose ether; Izakhiwo zomzimba namakhemikhali; Indlela yokuhlaziya; Uphenyo lokuhlola
I-Cellulose iyinhlanganisela ye-polymer yemvelo eningi kakhulu emhlabeni. Uchungechunge lwama-derivatives lungatholwa ngokuguqulwa kwamakhemikhali e-cellulose. I-Cellulose ether iwumkhiqizo we-cellulose ngemuva kwe-alkalization, i-etherification, ukugeza, ukuhlanzwa, ukugaya, ukomisa nezinye izinyathelo. Izinto zokusetshenziswa eziyinhloko ze-cellulose ether ukotini, i-kapok, uqalo, izinkuni, njll., phakathi kwazo okuqukethwe kwe-cellulose ukotini kuphakeme kakhulu, kuze kufike ku-90 ~ 95%, kuyindlela eluhlaza efanelekile yokukhiqiza i-cellulose ether, futhi i-China izwe elikhulu lokukhiqiza ukotini, elibuye likhuthaze ukuthuthukiswa kwemboni ye-cellulose ether yaseShayina ngezinga elithile. Njengamanje, ukukhiqizwa, ukucubungula kanye nokusetshenziswa kwe-fiber ether kuhola umhlaba.
I-cellulose ether ekudleni, emithini, kwezimonyo, ezintweni zokwakha, ephepheni nakwezinye izimboni kunezinhlobonhlobo zezicelo. Inezici zokuncibilika, i-viscosity, ukuzinza, ukungabi nobuthi kanye ne-biocompatibility. Izinga lokuhlola i-cellulose ether JCT 2190-2013, okuhlanganisa ukubukeka kahle kwe-cellulose ether, izinga lokuncipha kwesisindo elomile, umlotha wesulfate, i-viscosity, inani le-pH, ukudluliswa kwemali nezinye izinkomba ezibonakalayo namakhemikhali. Nokho, lapho i-cellulose ether isetshenziswa ezimbonini ezihlukene, ngaphezu kokuhlaziywa ngokomzimba namakhemikhali, umphumela wokusetshenziswa kwe-cellulose ether kulesi simiso ungase uhlolwe ngokwengeziwe. Isibonelo, ukugcinwa kwamanzi embonini yezokwakha, ukwakhiwa kodaka, njll.; Ukunamathela embonini ye-Adhesives, ukuhamba, njll.; Ukuhamba kwansuku zonke kwemboni yamakhemikhali, ukunamathela, njll. Izici ezingokomzimba nezamakhemikhali ze-cellulose ether zinquma ububanzi bokusebenza kwayo. Ukuhlaziywa ngokomzimba namakhemikhali kwe-cellulose ether kubalulekile ekukhiqizeni, ekucubunguleni noma ekusetshenzisweni. Ngokusekelwe ku-JCT 2190-2013, leli phepha liphakamisa izikimu ezintathu zokucwenga noma zokuthuthukisa zokuhlaziywa kwezakhiwo ze-physicochemical ze-cellulose ether, futhi liqinisekisa ukuthi kungenzeka yini ngokuhlola.
1. Izinga lokulahlekelwa isisindo elomile
Ukomisa izinga lokulahlekelwa kwesisindo kuyinkomba eyisisekelo kakhulu ye-cellulose ether, ebizwa nangokuthi okuqukethwe komswakama, okuhlobene nezingxenye zayo ezisebenzayo, impilo yeshalofu nokunye. Indlela yokuhlola ejwayelekile yindlela yesisindo sehhavini: Cishe amasampula angu-5g akalwa afakwa ebhodleleni lokukala elinokujula okungeqile ku-5mm. Isigqoko sebhodlela sasibekwe phansi kuhhavini, noma isivalo sebhodlela sasivulwa uhhafu futhi somiswe ku-105 ° C ±2 ° C amahora angu-2. Khona-ke i-cap yebhodlela ikhishwa futhi ipholiswe ekamelweni lokushisa ekamelweni elomile, likalwe, bese yomiswa kuhhavini imizuzu engu-30.
Kuthatha amahora angu-2 ~ 3 ukuthola umswakama wesampula ngale ndlela, futhi okuqukethwe komswakama kuhlobene nezinye izinkomba kanye nokulungiswa kwesixazululo. Izinkomba eziningi zingenziwa kuphela ngemva kokuqedwa kokuhlolwa kokuqukethwe komswakama. Ngakho-ke, le ndlela ayifanele ukusetshenziswa okungokoqobo ezimweni eziningi. Isibonelo, ulayini wokukhiqiza wezinye izimboni ze-cellulose ether udinga ukubona okuqukethwe kwamanzi ngokushesha okukhulu, ngakho-ke zingase zisebenzise ezinye izindlela ukuthola okuqukethwe kwamanzi, njengemitha yomswakama osheshayo.
Ngokwendlela evamile yokuthola umswakama wokuqukethwe, ngokuya ngesipiliyoni esisebenzayo sokuhlola sangaphambilini, ngokuvamile kuyadingeka ukomisa isampula ukuze libe nesisindo esingaguquki kokuthi 105℃, 2.5h.
Imiphumela yokuhlola yokuqukethwe kwe-cellulose ether ehlukile komswakamo ngaphansi kwezimo ezihlukene zokuhlola. Kungabonakala ukuthi imiphumela yokuhlola engu-135℃ no-0.5 h iseduze kakhulu naleyo yendlela evamile engu-105℃ no-2.5h, futhi ukuchezuka kwemiphumela yemitha yomswakama osheshayo kukhulu uma kuqhathaniswa. Ngemva kokuphuma kwemiphumela yokuhlola, izimo ezimbili zokutholwa ze-135℃, 0.5 h kanye ne-105℃, 2.5 h yendlela evamile zaqhubeka zibhekwa isikhathi eside, futhi imiphumela yayingakahluka kakhulu. Ngakho-ke, indlela yokuhlola engu-135℃ no-0.5 h ingenzeka, futhi isikhathi sokuhlola okuqukethwe komswakama singafinyezwa cishe ngamahora ama-2.
2. Umlotha we-sulfate
I-Sulfate ash cellulose ether iyinkomba ebalulekile, ehlobene ngokuqondile nokwakheka kwayo okusebenzayo, ubumsulwa nokunye. Indlela yokuhlola ejwayelekile: Sula isampula ku-105℃±2℃ ukuze ugcinwe, kala cishe u-2 g wesampula ku-crucible eshiswe isisindo esiqondile nesingapheli, beka i-crucible epuleti lokushisisa noma esithandweni sikagesi bese ushisa kancane kuze kube isampula. i-carbonized ngokuphelele. Ngemuva kokupholisa i-crucible, i-2 ml ye-sulfuric acid egxilile yengezwa, futhi insalela imanziswe futhi ishise kancane kuze kuvele intuthu emhlophe. I-crucible ifakwa esithandweni se-Muffle futhi ishiswe ku-750 ° C ± 50 ° C ihora elingu-1. Ngemuva kokushisa, i-crucible ikhishwa futhi ipholiswe ekamelweni lokushisa ekamelweni elomile futhi likalwe.
Kungabonakala ukuthi indlela evamile isebenzisa inani elikhulu le-sulfuric acid egxilile ekushiseni. Ngemuva kokushisa, inani elikhulu lentuthu ye-sulfuric acid egxilile. Noma ngabe isetshenziswa ku-fume hood, izoba nomthelela omkhulu endaweni ezungezile ngaphakathi nangaphandle kwelabhorethri. Kuleli phepha, ama-cellulose ether ahlukene asetshenziselwa ukubona umlotha ngokuhambisana nendlela evamile ngaphandle kokwengeza i-sulfuric acid egxilile, futhi imiphumela yokuhlolwa iqhathaniswa nendlela evamile evamile.
Kungabonakala ukuthi kunegebe elithile emiphumeleni yokutholwa yalezi zindlela ezimbili. Ngokusekelwe kule datha yoqobo, iphepha libala ukuphindaphinda kwegebe kokubili ebangeni elilinganiselwe lika-1.35 ~ 1.39. Okusho ukuthi, uma umphumela wokuhlola wendlela ngaphandle kwe-sulfuric acid uphindaphindwa nge-coefficient ye-1.35 ~ 1.39, umphumela wokuhlolwa komlotha nge-sulfuric acid ungatholakala cishe. Ngemva kokukhishwa kwemiphumela yokuhlola, izimo ezimbili zokutholwa zaqhathaniswa isikhathi eside, futhi imiphumela yahlala cishe kule coefficient. Kubonisa ukuthi le ndlela ingasetshenziswa ukuhlola i-cellulose ether ash ehlanzekile. Uma kunezidingo ezikhethekile zomuntu ngamunye, indlela ejwayelekile kufanele isetshenziswe. Njengoba i-ether ye-cellulose eyinkimbinkimbi yengeza izinto ezihlukahlukene, ngeke kuxoxwe ngakho lapha. Ekulawuleni ikhwalithi ye-cellulose ether, ukusebenzisa indlela yokuhlola umlotha ngaphandle kwe-sulfuric acid egxilile kunganciphisa ukungcola ngaphakathi nangaphandle kwelabhorethri, kunciphise isikhathi sokuhlola, ukusetshenziswa kwe-reagent futhi kunciphise izingozi zengozi ezingaba khona ezibangelwa inqubo yokuhlola.
3, isampula yesampula yokuhlolwa kokuqukethwe kweqembu le-cellulose ether
Okuqukethwe kweqembu kungenye yezinkomba ezibaluleke kakhulu ze-cellulose ether, enquma ngokuqondile izakhiwo zamakhemikhali ze-cellulose ether. Ukuhlolwa kokuqukethwe kweqembu kubhekisela ku-ether ye-cellulose ngaphansi kwesenzo se-catalyst, ukushisisa nokuqhekeka ku-reactor evaliwe, bese kuba ukukhishwa komkhiqizo nomjovo ku-chromatograph yegesi ukuze kuhlaziywe ubuningi. Inqubo yokushisa yokuqhekeka kokuqukethwe kweqembu ibizwa ngokuthi ukwelashwa kwangaphambili kuleli phepha. Indlela ejwayelekile yokwelapha yangaphambi kokwelashwa yilena: kala isampula eyomisiwe engu-65mg, engeza i-adipic acid engu-35mg ebhodleleni lokusabela, donsa uketshezi lwangaphakathi olujwayelekile elingu-3.0ml kanye no-2.0ml we-hydroiodic acid, phonsa ebhodleleni lokuphendula, ikhava ngokuqinile futhi ukale. Nyakazisa ibhodlela lokusabela ngesandla iminyaka engu-30, faka ibhodlela lokuphendula ku-thermostat yensimbi ku-150℃±2℃ i-20min, ulikhiphe bese ulinyakazisa ama-30S, bese ulishisa imizuzu engu-40. Ngemuva kokupholisa ekamelweni lokushisa, ukuncipha kwesisindo kuyadingeka ukuthi kungabi ngaphezu kwe-10mg. Uma kungenjalo, isisombululo sesampula sidinga ukulungiswa futhi.
Indlela evamile yokushisa isetshenziswa ekuphenduleni kokushisa kwe-thermostat yensimbi, ekusetshenzisweni kwangempela, umehluko wokushisa womugqa ngamunye wokugeza kwensimbi mkhulu, imiphumela ayiphindaphindeki kahle kakhulu, futhi ngenxa yokuthi ukusabela kokuqhekeka kokushisa kubi kakhulu, ngokuvamile ngenxa yokuthi ukusabela ibhodlela cap akuyona ukuvuza esiqinile futhi igesi ukuvuza, kukhona ingozi ethile. Kuleli phepha, ngokuhlolwa nokubheka isikhathi eside, indlela yokwelapha kusengaphambili ishintshelwa ku: kusetshenziswa ibhodlela lengilazi lokuphendula, elinepulaki yerabha ye-butyl ngokuqinile, kanye netheyiphu ye-polypropylene engashisi isongwe isixhumi esibonakalayo, bese ifaka ibhodlela lokusabela kusilinda esincane esikhethekile. , ikhava ngokuqinile, ekugcineni ifakwe kuhhavini lokushisa. Ibhodlela lokusabela ngale ndlela ngeke livuze uketshezi noma umoya, futhi liphephile futhi kulula ukusebenza lapho i-reagent inyakaziswa kahle ngesikhathi sokusabela. Ukusetshenziswa kokuqhuma kukagesi okomisa i-oven ukushisisa kungenza isampula ngalinye lishise ngokulinganayo, umphumela uwukuphindaphinda okuhle.
4. Isifinyezo
Imiphumela yokuhlola ibonisa ukuthi izindlela ezithuthukisiwe zokuthola i-cellulose ether okukhulunywe ngayo kuleli phepha zingenzeka. Ukusebenzisa izimo kuleli phepha ukuhlola izinga lokulahlekelwa kwesisindo okomisa kungathuthukisa ukusebenza kahle futhi kunciphise isikhathi sokuhlola. Ukusebenzisa akukho sulfuric acid test omlilo umlotha, kunganciphisa ukungcola labhorethri; Indlela kahhavini esetshenziswe kuleli phepha njengendlela yokwelashwa kwangaphambili yokuhlolwa kokuqukethwe kweqembu le-cellulose ether ingenza ukwelapha kwangaphambili kusebenze kahle futhi kuphephe.
Isikhathi sokuthumela: Feb-14-2023