Synthesis hamwe nibiranga Butane Sulfonate Cellulose Ether Amazi Kugabanya

Microcrystalline selulose (MCC) ifite urugero rwihariye rwa polymerisiyumu yabonetse na aside hydrolysis ya selile ya pamba ya selulose yakoreshejwe nkibikoresho fatizo. Nyuma yo gukora hydroxide ya sodium, yakiriwe na 1,4-butane sultone (BS) kugirango ibone amazi ya selilose butyl sulfonate (SBC) igabanya amazi meza kandi meza. Imiterere y'ibicuruzwa yaranzwe na infragre spekitroscopi (FT-IR), magnetic magnetic resonance spectroscopy (NMR), scanning electron microscopie (SEM), X-ray itandukanya (XRD) nubundi buryo bwo gusesengura, hamwe nimpamyabumenyi ya polymerisiyasi, igipimo cyibikoresho fatizo, hakozwe iperereza kuri reaction ya MCC. Ingaruka zuburyo bwimikorere nkubushyuhe, igihe cyo kubyitwaramo, nubwoko bwo guhagarika ibikorwa kumikorere igabanya amazi yibicuruzwa. Ibisubizo byerekana ko: iyo urwego rwa polymerisation yibikoresho fatizo MCC ari 45, igipimo rusange cyibisubizo ni: AGU (selile selile glucoside): n (NaOH): n (BS) = 1.0: 2.1: 2.2, The guhagarika agent ni isopropanol, igihe cyo gukora ibikoresho bibisi mubushyuhe bwicyumba ni 2 h, naho igihe cyo guhuza ibicuruzwa ni 5 h. Iyo ubushyuhe ari 80 ° C, ibicuruzwa byabonetse bifite urwego rwo hejuru rwo gusimbuza amatsinda ya aside ya butanesulfonike, kandi ibicuruzwa bifite imikorere myiza yo kugabanya amazi.

Amagambo y'ingenzi:selile; selilose butylsulfonate; umukozi ugabanya amazi; kugabanya amazi

1、Intangiriro

Beto superplasticizer ni kimwe mubintu byingirakamaro bya beto igezweho. Nubusanzwe kuberako isura igabanya amazi niyo ishobora gukora cyane, kuramba neza ndetse nimbaraga nyinshi za beto. Kugeza ubu ikoreshwa cyane mu kugabanya amazi meza cyane harimo ibyiciro bikurikira: kugabanya amazi ashingiye kuri naphthalene (SNF), kugabanya amazi ya sulfatique ya melamine-kugabanya amazi (SMF), kugabanya amazi ya sulfamate (ASP), byahinduwe na Lignosulfonate superplasticizer ( ML), hamwe na polycarboxylate superplasticizer (PC), ubu ikaba ikorerwa ubushakashatsi cyane. Gusesengura uburyo bwo kugabanya amazi agabanya amazi, ibyinshi mubisanzwe bigabanya amazi ya kondensate yabanjirije gukoresha fordehide ifite impumuro nziza nkibikoresho fatizo bya polycondensation, kandi inzira ya sulfonasiyo ikorwa hamwe na acide sulfurike yangiza cyane cyangwa acide sulfurike. Ibi byanze bikunze bizatera ingaruka mbi kubakozi no kubidukikije, kandi bizanatanga umusaruro mwinshi wibisigazwa byimyanda n’amazi y’imyanda, bidafasha iterambere rirambye; icyakora, nubwo kugabanya amazi ya polycarboxylate bifite ibyiza byo gutakaza bike bya beto mugihe, dosiye nkeya, gutembera neza Ifite ibyiza byubucucike bwinshi kandi nta bintu bifite uburozi nka formaldehyde, ariko biragoye kuyiteza imbere mubushinwa kubera hejuru igiciro. Duhereye ku isesengura ry’inkomoko y’ibikoresho fatizo, ntabwo bigoye kubona ko ibyinshi mu bigabanya amazi yavuzwe haruguru bihuzwa hashingiwe ku bicuruzwa bikomoka kuri peteroli / ibikomoka ku bicuruzwa, mu gihe peteroli, nk’umutungo udashobora kuvugururwa, igenda iba mike kandi igiciro cyacyo gihora kizamuka. Kubwibyo, uburyo bwo gukoresha umutungo uhendutse kandi mwinshi ushobora kuvugururwa nkibikoresho fatizo kugirango utezimbere imikorere mishya yo hejuru cyane ya superplasticizers yabaye icyerekezo cyingenzi cyubushakashatsi kuri superplasticizers.

Cellulose ni umurongo wa macromolecule ugizwe no guhuza D-glucopyranose nyinshi na β- (1-4) glycosidic. Hano hari amatsinda atatu ya hydroxyl kuri buri mpeta ya glucopyranosyl. Kuvura neza birashobora kubona reaction runaka. Muri iyi nyandiko, ipamba ya selulose yakoreshejwe nkibikoresho byambere bibanza, hanyuma nyuma ya hydrolysis ya aside kugirango ibone microcrystalline selulose ifite urugero rwiza rwa polymerisation, yakoreshejwe na sodium hydroxide hanyuma ikorana na 1,4-butane sultone kugirango itegure Acide butyl sulfonate Acide selulose ether superplasticizer, hamwe nibintu bigira ingaruka kuri buri reaction byaganiriweho.

2. Ubushakashatsi

2.1 Ibikoresho bibisi

Cellulose ipamba, impamyabumenyi ya polymerisation 576, Sinayi Aoyang Technology Co., Ltd.; 1,4-butane sultone (BS), urwego rwinganda, rwakozwe na Shanghai Jiachen Chemical Co., Ltd.; 52.5R sima isanzwe ya Portland, Urumqi Itangwa nuruganda rwa sima; Ubushinwa ISO umusenyi usanzwe, wakozwe na Xiamen Ace Ou Standard Sand Co., Ltd.; hydroxide ya sodium, aside hydrochloric, isopropanol, methanol ya anhydrous, etil acetate, n-butanol, peteroli ether, nibindi, byose birasesenguwe neza, biraboneka mubucuruzi.

2.2 Uburyo bw'igerageza

Gupima urugero runaka rw'ipamba hanyuma ukasya neza, ubishyire mu icupa ry'amajosi atatu, ongeramo urugero runaka rwa acide hydrochloric acide, ushyire hejuru kugirango ushushe na hydrolyze mugihe runaka, bikonje kugeza ubushyuhe bwicyumba, kuyungurura, oza n'amazi kugeza utabogamye, na vacuum yumye kuri 50 ° C kugirango ubone Nyuma yo kugira ibikoresho fatizo bya microcrystalline selulose hamwe na dogere zitandukanye za polymerisime, bapima urugero rwabo rwa polymerisation ukurikije ibitabo, ubishyire mumacupa ya reaction yijosi atatu, ubihagarike hamwe umukozi uhagarika inshuro 10 ubwinshi bwayo, ongeramo umubare munini wa sodium hydroxide yumuti wamazi ukurura, Kangura hanyuma ukore mubushyuhe bwicyumba mugihe runaka, ongeramo umubare wabazwe wa 1,4-butane sultone (BS), shyushya ku bushyuhe bwa reaction, reba ubushyuhe burigihe mugihe runaka, gukonjesha ibicuruzwa kubushyuhe bwicyumba, hanyuma ubone ibicuruzwa biva mukuyungurura. Kwoza amazi na methanol inshuro 3, hanyuma uyungurure unywe kugirango ubone ibicuruzwa byanyuma, aribyo kugabanya amazi ya selilose butylsulfonate (SBC).

2.3 Isesengura ryibicuruzwa nibiranga

2.3.1 Kumenyekanisha ibicuruzwa bya sulfuru no kubara urwego rwo gusimburwa

Isesengura ryibanze rya FLASHEA-PE2400 ryakoreshejwe mugukora isesengura ryibanze ku bicuruzwa byumye bya selile yumye butyl sulfonate igabanya amazi kugirango hamenyekane ibirimo sulfure.

2.3.2 Kumenya amazi ya minisiteri

Gupimwa ukurikije 6.5 muri GB8076-2008. Nukuvuga, banza upime amazi / sima / imvange yumucanga usanzwe kuri NLD-3 sima ya minisiteri yipimisha mugihe diameter yo kwaguka ari (180 ± 2) mm. sima, ibipimo by'amazi byapimwe ni 230g), hanyuma wongereho umukozi ugabanya amazi ufite ubwinshi bwa 1% ya sima kumazi, nkuko bitangazwa na sima / kugabanya amazi / amazi asanzwe / umucanga usanzwe = 450g / 4.5g / 230 g / Ikigereranyo cya 1350 g gishyirwa muvangavanga rya sima ya JJ-5 ya sima hanyuma ikabyutsa kimwe, hanyuma hapimwa diameter yagutse ya minisiteri ku kizamini cya minisiteri y’amazi, ikaba ari yo yapimye amazi ya minisiteri.

2.3.3 Ibiranga ibicuruzwa

Icyitegererezo cyaranzwe na FT-IR ukoresheje ubwoko bwa EQUINOX 55 bwa Fourier transform infrared spectrometer ya Bruker Company; icyerekezo cya H NMR cyicyitegererezo cyaranzwe na INOVA ZAB-HS isuka irenze urugero igikoresho cya magnetiki resonance igikoresho cya sosiyete ya Varian; Imiterere y'ibicuruzwa yagaragaye munsi ya microscope; Isesengura rya XRD ryakozwe ku cyitegererezo hakoreshejwe X-ray diffractometer ya MAC Company M18XHF22-SRA.

3. Ibisubizo n'ibiganiro

3.1 Ibisubizo biranga

3.1.1 Ibisubizo biranga FT-IR

Isesengura ridafite ishingiro ryakozwe ku bikoresho fatizo bya microcrystalline selulose hamwe na dogere ya polymerisation Dp = 45 nibicuruzwa SBC ikomatanya bivuye muri ibi bikoresho. Kubera ko impinga zo kwinjiza za SC na SH zifite intege nke cyane, ntabwo zikwiriye kumenyekana, mugihe S = O ifite impinga ikomeye yo kwinjiza. Kubwibyo, niba hari itsinda rya acide sulfonique mumiterere ya molekile irashobora kugenwa no kwemeza ko impinga ya S = O. Ikigaragara ni uko muri selire ya selile, hari impinga ikomeye yo kwinjirira kumuraba wa cm 3344 cm-1, ibyo bikaba biterwa na hydroxyl irambuye hejuru yinyeganyeza muri selile; imbaraga zo kwinjirira cyane kumuraba wa cm 2923 cm-1 nigitambambuga kirambuye cya methylene (-CH2). Impinga yo kunyeganyega; urukurikirane rw'imigwi igizwe na 1031, 1051, 1114, na 1165cm-1 yerekana impinga yo kwinjiza hydroxyl irambuye ihindagurika hamwe nimpinga yo kwinjirira ya ether bond (COC) yunamye; umuraba numero 1646cm-1 yerekana hydrogène ikorwa na hydroxyl namazi yubusa Impinga yo kwinjiza ingwate; itsinda rya 1432 ~ 1318cm-1 ryerekana kubaho kwa selile ya selile. Muri IR spektr ya SBC, ubukana bwitsinda 1432 ~ 1318cm-1 bugabanuka; mugihe ubukana bwimpinga yo kwinjiza kuri 1653 cm-1 bwiyongera, byerekana ko ubushobozi bwo gukora imigozi ya hydrogène bukomera; 1040, 605cm-1 igaragara nkimpinga zikomeye za Absorption, kandi izi ebyiri ntizigaragara mumurongo wa infragre ya selile ya selile, iyambere niyo iranga kwinjirira impinga ya S = O, naho iyanyuma niyo mpanvu yibiranga ya SO. Ukurikije isesengura ryavuzwe haruguru, birashobora kugaragara ko nyuma ya etherification reaction ya selile, hariho amatsinda ya acide sulfonique mumurongo wa molekile.

3.1.2 H NMR ibisubizo biranga

H NMR ya selile ya selilose butyl sulfonate irashobora kugaragara: muri γ = 1.74 ~ 2.92 ni hydrogène proton ihinduranya imiti ya cyclobutyl, naho muri γ = 3.33 ~ 4.52 ni selile ya anhydroglucose ya selile ya chimique ya proton ya ogisijeni muri γ = 4.52 ~ 6 ni ihinduka ryimiti ya methylene proton mumatsinda ya acide ya butylsulfonique ihujwe na ogisijeni, kandi nta mpinga iri kuri γ = 6 ~ 7, byerekana ko ibicuruzwa atari Izindi proton zibaho.

3.1.3 ibisubizo biranga SEM

SEM kwitegereza selulose ipamba, microcrystalline selulose nibicuruzwa bya selile butylsulfonate. Iyo usesenguye ibyavuye mu isesengura rya SEM ya pamba ya selile, microcrystalline selulose hamwe nibicuruzwa selulose butanesulfonate (SBC), usanga selile microcrystalline yabonetse nyuma ya hydrolysis hamwe na HCL ishobora guhindura cyane imiterere ya fibre selile. Imiterere ya fibrous yarasenyutse, haboneka uduce twiza twa selile. SBC yabonetse mugukomeza kwitwara hamwe na BS ntabwo yari ifite fibrous structure kandi ahanini yahinduwe muburyo bwa amorphous, byagize akamaro ko kuyasesa mumazi.

3.1.4 Ibisubizo biranga XRD

Crystallinite ya selile n'ibiyikomokaho bivuga ijanisha ryakarere ka kristalline kagizwe nuburyo bwa selile ya selile muri rusange. Iyo selile n'ibiyikomokaho byatewe na chimique, imigozi ya hydrogène muri molekile no hagati ya molekile irasenywa, kandi akarere ka kristaline kazahinduka akarere ka amorphous, bityo bikagabanya kristu. Kubwibyo, impinduka muri kristu mbere na nyuma yo kubyitwaramo ni igipimo cya selulose Kimwe mubisabwa kugira uruhare mugusubiza cyangwa kutabikora. Isesengura XRD ryakozwe kuri microcrystalline selulose hamwe nibicuruzwa bya selile butanesulfonate. Birashobora kugaragara ugereranije ko nyuma ya etherification, kristu ihinduka cyane, kandi ibicuruzwa byahindutse rwose muburyo bwa amorphous, kuburyo bishobora gushonga mumazi.

3.2 Ingaruka yurwego rwa polymerisation yibikoresho fatizo kumikorere igabanya amazi yibicuruzwa

Amazi ya minisiteri yerekana mu buryo butaziguye imikorere igabanya amazi ku bicuruzwa, kandi ibirimo sulfure biri mu bicuruzwa ni kimwe mu bintu byingenzi bigira ingaruka ku mazi ya minisiteri. Amazi ya minisiteri apima imikorere igabanya amazi yibicuruzwa.

Nyuma yo guhindura imiterere ya hydrolysis kugirango utegure MCC hamwe nimpamyabumenyi zitandukanye za polymerisation, ukurikije uburyo bwavuzwe haruguru, hitamo uburyo bumwe bwoguhindura kugirango utegure ibicuruzwa bya SBC, upime ibirimo sulfure kugirango ubare impamyabumenyi yo gusimbuza ibicuruzwa, hanyuma wongere ibicuruzwa bya SBC mumazi. / sima / sisitemu isanzwe ivanga umucanga Gupima amazi ya minisiteri.

Birashobora kugaragara mubisubizo byubushakashatsi ko mubushakashatsi bwakozwe, mugihe urwego rwa polymerisation ya microcrystalline selulose yibikoresho fatizo ari byinshi, ibirimo sulfure (impamyabumenyi yo gusimbuza) ibicuruzwa nibitemba bya minisiteri biri hasi. Ibi ni ukubera ko: uburemere bwa molekuline yibikoresho fatizo ni bito, bifasha kuvanga kimwe ibikoresho fatizo no kwinjira kwa agent ya etherification, bityo bikazamura urwego rwa etherifike yibicuruzwa. Nyamara, igipimo cyo kugabanya amazi ntigishobora kuzamuka kumurongo ugororotse hamwe no kugabanuka kurwego rwa polymerisation yibikoresho fatizo. Ibisubizo byubushakashatsi byerekana ko amazi ya minisiteri yimvange ya sima ivanze na SBC yateguwe ukoresheje microcrystalline selulose ifite urugero rwa polymerisation Dp <96 (uburemere bwa molekile <15552) irenze mm 180 (iruta iyo idafite kugabanya amazi) . ibipimo ngenderwaho), byerekana ko SBC ishobora gutegurwa ukoresheje selile ifite uburemere bwa molekile iri munsi ya 15552, kandi igipimo cyo kugabanya amazi gishobora kuboneka; SBC itegurwa no gukoresha microcrystalline selulose ifite urwego rwa polymerisation ya 45 (uburemere bwa molekile: 7290), hanyuma ikongerwaho kuvangwa na beto, amazi yapimye ya minisiteri nini cyane, bityo bikaba bifatwa ko selile ifite urwego rwa polymerizasi ya 45 ni byiza cyane mugutegura SBC; iyo urugero rwa polymerisation yibikoresho bibisi rurenze 45, amazi ya minisiteri agabanuka buhoro buhoro, bivuze ko igipimo cyo kugabanya amazi kigabanuka. Ibi ni ukubera ko iyo uburemere bwa molekile ari bunini, kuruhande rumwe, ububobere bwa sisitemu ivanze biziyongera, uburinganire bwa sima buzagenda bwangirika, kandi gutatanya muri beto bizatinda, bizagira ingaruka ku ngaruka zo gutatanya; kurundi ruhande, iyo uburemere bwa molekile ari bunini, macromolecules ya superplasticizer iri muburyo bwa coil ihinduka, bikaba bigoye cyane adsorb hejuru yubutaka bwa sima. Ariko iyo urugero rwa polymerisation yibikoresho bibisi ruri munsi ya 45, nubwo ibirimo sulfure (impamyabumenyi yo gusimbuza) ibicuruzwa ari binini cyane, amazi yimvange ya minisiteri nayo atangira kugabanuka, ariko kugabanuka ni nto cyane. Impamvu nuko iyo uburemere bwa molekuline bwibintu bigabanya amazi ari bito, nubwo ikwirakwizwa rya molekile ryoroshye kandi rikaba rifite amazi meza, umuvuduko wa adsorption ya molekile uba munini ugereranije na molekile, kandi urunigi rwo gutwara amazi ruba rugufi cyane, no guterana hagati yibi bice ni binini, byangiza kuri beto. Ingaruka zo gukwirakwiza ntabwo ari nziza nkizigabanya amazi nuburemere bunini bwa molekile. Niyo mpamvu, ni ngombwa cyane kugenzura neza uburemere bwa molekuline yisura yingurube (agace ka selile) kugirango tunoze imikorere igabanya amazi.

3.3 Ingaruka yimiterere yimikorere kumikorere igabanya amazi yibicuruzwa

Byagaragaye binyuze mubushakashatsi bwerekana ko usibye urwego rwa polymerisation ya MCC, igipimo cyibisubizo, ubushyuhe bwibisubizo, gukora ibikoresho fatizo, igihe cyo guhuza ibicuruzwa, nubwoko bwo guhagarika ibintu byose bigira ingaruka kumikorere igabanya amazi yibicuruzwa.

3.3.1 Ikigereranyo gifatika

(1) Igipimo cya BS

Mugihe ibintu byagenwe nibindi bipimo (urugero rwa polymerisation ya MCC ni 45, n (MCC): n (NaOH) = 1: 2.1, umukozi uhagarika ni isopropanol, igihe cyo gukora selile mu bushyuhe bwicyumba ni 2h, ubushyuhe bwa synthesis ni 80 ° C, hamwe na synthesis time 5h), kugirango hakorwe iperereza ku ngaruka ziterwa na agent ya etherification 1,4-butane sultone (BS) kurwego rwo gusimbuza amatsinda ya acide ya butanesulfonike yibicuruzwa nibisukari. minisiteri.

Birashobora kugaragara ko uko ingano ya BS yiyongera, urugero rwo gusimbuza amatsinda ya aside ya butanesulfonike hamwe n’amazi ya minisiteri yiyongera cyane. Iyo igipimo cya BS na MCC kigeze kuri 2.2: 1, amazi ya DS na minisiteri bigera kuri byinshi. agaciro, bifatwa ko imikorere igabanya amazi aribyiza muriki gihe. Agaciro BS yakomeje kwiyongera, kandi urwego rwo gusimbuza hamwe n’amazi ya minisiteri byatangiye kugabanuka. Ni ukubera ko iyo BS ikabije, BS izakorana na NaOH kubyara HO- (CH2) 4SO3Na. Kubwibyo, iyi mpapuro ihitamo igipimo cyiza cya BS na MCC nka 2.2: 1.

(2) Igipimo cya NaOH

Mubihe byagenwe nibindi bipimo (urugero rwa polymerisation ya MCC ni 45, n (BS): n (MCC) = 2.2: 1. Umukozi uhagarika ni isopropanol, igihe cyo gukora selile mu bushyuhe bwicyumba ni 2h, ubushyuhe bwa synthesis ni 80 ° C, hamwe nigihe cyo guhuza 5h), kugirango hakorwe iperereza ku ngaruka ziterwa na hydroxide ya sodium ku rwego rwo gusimbuza amatsinda ya aside ya butanesulfonike mu bicuruzwa no gutembera kwa minisiteri.

Birashobora kugaragara ko, hamwe no kwiyongera kwamafaranga yagabanutse, urwego rwo gusimbuza SBC rwiyongera vuba, kandi rutangira kugabanuka nyuma yo kugera ku giciro cyo hejuru. Ibi ni ukubera ko, iyo ibiri muri NaOH ari byinshi, hariho sisitemu nyinshi zubusa muri sisitemu, kandi amahirwe yo kwitwara kuruhande ariyongera, bigatuma abakozi benshi ba etherification (BS) bagira uruhare mubitekerezo, bityo bikagabanya urwego rwo gusimbuza sulfonike amatsinda ya aside mubicuruzwa. Ku bushyuhe bwo hejuru, kuba NaOH irenze urugero nabyo bizatesha agaciro selile, kandi imikorere igabanya amazi yibicuruzwa izagira ingaruka kurwego rwo hasi rwa polymerisation. Ukurikije ibyavuye mu bushakashatsi, iyo igipimo cy’imisemburo ya NaOH na MCC kigera kuri 2.1, urwego rwo gusimbuza ni rwo runini, iyi mpapuro rero igena ko igipimo cy’imitsi ya NaOH na MCC ari 2.1: 1.0.

3.3.2 Ingaruka yubushyuhe bwa reaction kumikorere igabanya amazi

Mubihe byagenwe nibindi bipimo (urwego rwa polymerisation ya MCC ni 45, n (MCC): n (NaOH): n (BS) = 1: 2.1: 2.2, umukozi uhagarika ni isopropanol, nigihe cyo gukora cyo selile mubushyuhe bwicyumba ni 2h. Igihe cya 5h), ubushakashatsi bwakozwe nubushyuhe bwa synthesis reaction kurwego rwo gusimbuza amatsinda ya acide ya butanesulfonike mubicuruzwa.

Birashobora kugaragara ko uko ubushyuhe bwa reaction bwiyongera, impamyabumenyi ya sulfonike ya DS ya SBC yiyongera buhoro buhoro, ariko iyo ubushyuhe bwa reaction burenze 80 ° C, DS yerekana inzira yo kumanuka. Imyitwarire ya etherification hagati ya 1,4-butane sultone na selile ni reaction ya endothermic reaction, kandi kongera ubushyuhe bwa reaction ni ingirakamaro kumyitwarire hagati ya etherifying agent na selile hydroxyl, ariko hamwe no kwiyongera kwubushyuhe, ingaruka za NaOH na selile ziyongera buhoro buhoro . Irakomera, itera selile yangirika ikagwa, bikavamo kugabanuka kwuburemere bwa molekuline ya selile no kubyara isukari ntoya. Imyitwarire ya molekile ntoya hamwe nibikoresho bya etherifing biroroshye byoroshye, kandi nibindi byinshi bizakoreshwa, bigira ingaruka kurwego rwo gusimbuza ibicuruzwa. Kubwibyo, iyi nsanganyamatsiko ireba ko ubushyuhe bukwiye bwa reaction ya etherification ya BS na selile ni 80 ℃.

3.3.3 Ingaruka yigihe cyo kwitwara kubikorwa byo kugabanya amazi

Igihe cyo kubyitwaramo kigabanijwemo ubushyuhe bwicyumba cyo gukora ibikoresho bibisi hamwe nigihe cyo guhuza ubushyuhe burigihe bwibicuruzwa.

(1) Igihe cyo gukora ubushyuhe bwicyumba igihe cyibikoresho fatizo

Muburyo bwiza bwavuzwe haruguru (MCC urwego rwa polymerisation ni 45, n (MCC): n (NaOH): n (BS) = 1: 2.1: 2.2, guhagarika agent ni isopropanol, ubushyuhe bwa synthesis ni 80 ° C, ibicuruzwa Guhorana ubushyuhe burigihe 5h), shakisha ingaruka zigihe cyo gukora ubushyuhe bwicyumba kurwego rwo gusimbuza ibicuruzwa itsinda rya acide butanesulfonic.

Birashobora kugaragara ko urwego rwo gusimbuza aside aside ya butanesulfonike yibicuruzwa SBC yiyongera mbere hanyuma bikagabanuka hamwe no kongera igihe cyo gukora. Impamvu yo gusesengura irashobora kuba nuko hamwe no kwiyongera kwa NaOH igihe cyibikorwa, kwangirika kwa selile birakomeye. Kugabanya uburemere bwa molekuline ya selile kugirango ubyare isukari nto. Imyitwarire ya molekile ntoya hamwe nibikoresho bya etherifing biroroshye byoroshye, kandi nibindi byinshi bizakoreshwa, bigira ingaruka kurwego rwo gusimbuza ibicuruzwa. Kubwibyo, iyi mpapuro yerekana ko icyumba cyo gukora ubushyuhe bwicyumba cyibikoresho fatizo ari 2h.

(2) Igihe cyo guhuza ibicuruzwa

Muburyo bwiza bwo gukora neza hejuru, hasuzumwe ingaruka zigihe cyo gukora mubushyuhe bwicyumba kurwego rwo gusimbuza ibicuruzwa bya butanesulfonic acide. Birashobora kugaragara ko hamwe nigihe kirekire cyigihe cyo kubyitwaramo, urwego rwo gusimburwa rwambere rwiyongera, ariko iyo igihe cyo kwitwara kigeze 5h, DS yerekana inzira yo kumanuka. Ibi bifitanye isano nubusa bwibanze muri etherification reaction ya selile. Ku bushyuhe bwinshi, igihe kinini cyibisubizo biganisha ku kwiyongera kurwego rwa alkali hydrolysis ya selile, kugabanuka k'urunigi rwa selile, kugabanuka k'uburemere bwa molekile y'ibicuruzwa, no kwiyongera k'uruhande, bikavamo kwiyongera. gusimburwa. impamyabumenyi iragabanuka. Muri ubu bushakashatsi, igihe cyiza cyo guhuza ni 5h.

3.3.4 Ingaruka zubwoko bwihagarikwa kumikorere igabanya amazi yibicuruzwa

Muburyo bwiza bwo gukora (impamyabumenyi ya MCC ni 45, n (MCC): n (NaOH): n (BS) = 1: 2.1: 2.2, igihe cyo gukora ibikoresho fatizo mubushyuhe bwicyumba ni 2h, igihe cyo guhuza ubushyuhe burigihe y'ibicuruzwa ni 5h, hamwe na synthesis reaction yubushyuhe bwa 80 ℃), buri kimwe hitamo isopropanol, Ethanol, n-butanol, Ethyl acetate na peteroli ether nkibikoresho bihagarika, hanyuma baganire ku ngaruka zabyo ku mikorere igabanya amazi y’ibicuruzwa.

Biragaragara, isopropanol, n-butanol na Ethyl acetate byose birashobora gukoreshwa nkumukozi uhagarika iyi reaction ya etherification. Uruhare rwumukozi uhagarika, usibye gukwirakwiza reaction, rushobora kugenzura ubushyuhe bwimikorere. Ingingo yo gutekesha isopropanol ni 82.3 ° C, bityo isopropanol ikoreshwa nkumukozi uhagarika, ubushyuhe bwa sisitemu burashobora kugenzurwa hafi yubushyuhe bwiza, hamwe nurwego rwo gusimbuza amatsinda ya acide ya butanesulfonike mubicuruzwa no gutembera neza minisiteri ni ndende; mugihe aho gutekera Ethanol ari hejuru cyane Hasi, ubushyuhe bwa reaction ntibujuje ibisabwa, urugero rwo gusimbuza amatsinda ya aside ya butanesulfonike mubicuruzwa kandi amazi ya minisiteri ni make; peteroli ether irashobora kugira uruhare mubitekerezo, kuburyo nta bicuruzwa bitatanye bishobora kuboneka.

4 Umwanzuro

(1) Gukoresha ipamba nkibikoresho byambere bibisi,microcrystalline selulose (MCC)hamwe nurwego rukwiye rwa polymerisation yarateguwe, ikorwa na NaOH, hanyuma ikorana na 1,4-butane sultone kugirango itegure amazi ya elegitoronike ya butylsulfonic acide Cellulose ether, ni ukuvuga kugabanya amazi ya selile. Imiterere y'ibicuruzwa yaranzwe, kandi byagaragaye ko nyuma ya etherification ya selile, hari amatsinda ya acide sulfonique kumurongo wa molekile yayo, yari yarahindutse muburyo bwa amorphous, kandi ibicuruzwa bigabanya amazi byari bifite amazi meza;

. hashingiwe ko igipimo cya polymerisation yibikoresho fatizo cyagenwe, igipimo cyibisubizo ni n (MCC): n (NaOH): n (BS) = 1: 2.1: 2.2, igihe cyo gutangiza ibikoresho fatizo mubushyuhe bwicyumba ni 2h, ibicuruzwa bya synthesis ubushyuhe ni 80 ° C, naho igihe cyo guhuza ni 5h. Imikorere y'amazi nibyiza.