Kupanga ndi Kufotokozera kwa Butane Sulfonate Cellulose Ether Water Reducer

Microcrystalline cellulose (MCC) yokhala ndi mulingo wotsimikizika wa polymerization wopezeka ndi acid hydrolysis ya cellulose thonje pulp idagwiritsidwa ntchito ngati zopangira. Pogwiritsa ntchito sodium hydroxide, idasinthidwa ndi 1,4-butane sultone (BS) kuti ipeze A cellulose butyl sulfonate (SBC) water reducer yokhala ndi madzi osungunuka bwino idapangidwa. Kapangidwe ka mankhwalawo kanadziwika ndi infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy (NMR), scanning electron microscopy (SEM), X-ray diffraction (XRD) ndi njira zina zowunikira, ndipo digiri ya polymerization, raw material ratio, ndi reaction ya MCC zidafufuzidwa. Zotsatira za mikhalidwe yopangira zinthu monga kutentha, nthawi yochitira, ndi mtundu wa suspension agent pa magwiridwe antchito a mankhwala ochepetsa madzi. Zotsatira zake zikusonyeza kuti: pamene mlingo wa polymerization wa MCC wa zopangira uli 45, chiŵerengero cha kulemera kwa reactants ndi: AGU (cellulose glucoside unit): n (NaOH): n (BS) = 1.0: 2.1: 2.2, Chothandizira choyimitsa ndi isopropanol, nthawi yoyatsira ya zopangira kutentha kwa chipinda ndi maola awiri, ndipo nthawi yopangira mankhwala ndi maola 5. Pamene kutentha kuli 80°C, mankhwala omwe apezeka amakhala ndi mlingo wapamwamba kwambiri wosinthira magulu a butanesulfonic acid, ndipo mankhwalawa ali ndi magwiridwe antchito abwino kwambiri ochepetsa madzi.

Mawu ofunikira:cellulose; cellulose butylsulfonate; chochepetsera madzi; ntchito yochepetsa madzi

1、Chiyambi

Konkriti superplasticizer ndi chimodzi mwa zinthu zofunika kwambiri pa konkriti yamakono. Chifukwa cha mawonekedwe a chochepetsera madzi, kugwira ntchito bwino, kulimba bwino, komanso mphamvu zambiri za konkriti zitha kutsimikizika. Zinthu zochepetsera madzi zomwe zimagwiritsidwa ntchito kwambiri pano zimaphatikizapo magulu otsatirawa: naphthalene-based water reducer (SNF), sulfonated melamine resin-based water-reducer (SMF), sulfamate-based water-reducer (ASP), modified Lignosulfonate superplasticizer (ML), ndi polycarboxylate superplasticizer (PC), zomwe zikufufuzidwa kwambiri pakadali pano. Pofufuza momwe zinthu zochepetsera madzi zimagwirira ntchito, zinthu zambiri zakale zochepetsera madzi a condensate zimagwiritsa ntchito formaldehyde yokhala ndi fungo lamphamvu ngati zinthu zopangira polycondensation reaction, ndipo njira ya sulfonation nthawi zambiri imachitika ndi sulfuric acid yowononga kwambiri kapena sulfuric acid yokhazikika. Izi zingayambitse zotsatira zoyipa kwa ogwira ntchito ndi chilengedwe chozungulira, komanso zimapanganso zinyalala zambiri ndi madzi otayira, zomwe sizingathandize pakukula kokhazikika; Komabe, ngakhale kuti zochepetsera madzi za polycarboxylate zili ndi ubwino wochepa wa kutayika kwa konkriti pakapita nthawi, mlingo wochepa, kuyenda bwino. Ili ndi ubwino wochepa kwambiri komanso yopanda zinthu zoopsa monga formaldehyde, koma n'zovuta kuilimbikitsa ku China chifukwa cha mtengo wake wokwera. Kuchokera ku kusanthula kwa gwero la zipangizo zopangira, sizovuta kupeza kuti zinthu zambiri zochepetsera madzi zomwe zatchulidwa pamwambapa zimapangidwa kutengera zinthu za petrochemical/zopangidwa ndi petrochemical, pomwe mafuta, monga chuma chosabwezeretsedwanso, akuchepa kwambiri ndipo mtengo wake ukukwera nthawi zonse. Chifukwa chake, momwe mungagwiritsire ntchito zinthu zachilengedwe zotsika mtengo komanso zambiri zobwezerezedwanso ngati zopangira popanga zinthu zatsopano zopangira konkriti zapamwamba kwambiri kwakhala njira yofunika kwambiri yofufuzira ma superplasticizer a konkriti.

Cellulose ndi macromolecule yolunjika yomwe imapangidwa polumikiza ma D-glucopyranose ambiri ndi ma β-(1-4) glycosidic bonds. Pali magulu atatu a hydroxyl pa mphete iliyonse ya glucopyranosyl. Kuchiza koyenera kungapangitse kuti pakhale reactivity inayake. Mu pepalali, cellulose thonje pulp idagwiritsidwa ntchito ngati zinthu zoyambira zopangira, ndipo pambuyo pa acid hydrolysis kuti ipeze microcrystalline cellulose yokhala ndi digiri yoyenera ya polymerization, idayambitsidwa ndi sodium hydroxide ndipo idachitidwa ndi 1,4-butane sultone kuti ikonzekere butyl sulfonate Acid cellulose ether superplasticizer, ndipo zinthu zomwe zimakhudza reaction iliyonse zidakambidwa.

2. Kuyesera

2.1 Zipangizo zopangira

Cellulose thonje la pulp, digiri ya polymerization 576, Xinjiang Aoyang Technology Co., Ltd.; 1,4-butane sultone (BS), mtundu wa mafakitale, wopangidwa ndi Shanghai Jiachen Chemical Co., Ltd.; 52.5R wamba simenti ya Portland, Urumqi Yoperekedwa ndi fakitale ya simenti; China ISO standard mchenga, wopangidwa ndi Xiamen Ace Ou Standard Sand Co., Ltd.; sodium hydroxide, hydrochloric acid, isopropanol, anhydrous methanol, ethyl acetate, n-butanol, petroleum ether, ndi zina zotero, zonse ndi zoyera, zimapezeka m'masitolo.

2.2 Njira yoyesera

Yesani kuchuluka kwa thonje la thonje ndikulipera bwino, liikeni mu botolo la khosi zitatu, onjezerani kuchuluka kwa hydrochloric acid wosungunuka, sakanizani kuti litenthe ndikuwonjezera hydrolyze kwa nthawi inayake, lizireni kutentha kwa chipinda, sefani, sambitsani ndi madzi mpaka litakhala lopanda mpweya, ndikuumitsa pa vacuum pa 50°C kuti mupeze. Mukamaliza kugwiritsa ntchito zinthu zopangira cellulose za microcrystalline zokhala ndi madigiri osiyanasiyana a polymerization, yesani kuchuluka kwa polymerization malinga ndi zomwe zalembedwa, liikeni mu botolo la reaction la khosi zitatu, liyimitseni ndi suspension agent kuwirikiza ka 10 kulemera kwake, onjezerani kuchuluka kwa sodium hydroxide aqueous solution pansi pa kusakaniza. Sakanizani ndikuyambitsa kutentha kwa chipinda kwa nthawi inayake, onjezerani kuchuluka kwa 1,4-butane sultone (BS) komwe kwawerengedwa, tenthetsani mpaka kutentha kwa reaction, chitani kutentha kosasintha kwa nthawi inayake, ziziritsani mankhwalawa kutentha kwa chipinda, ndikupeza chinthu chosaphikidwa pogwiritsa ntchito suction filtration. Tsukani ndi madzi ndi methanol kwa nthawi zitatu, ndikusefa ndi suction kuti mupeze chinthu chomaliza, chomwe ndi cellulose butylsulfonate water reducer (SBC).

2.3 Kusanthula ndi kufotokoza za malonda

2.3.1 Kudziwa kuchuluka kwa sulfure mu chinthucho ndi kuwerengera kuchuluka kwa cholowa m'malo mwake

Choyezera zinthu cha FLASHEA-PE2400 chinagwiritsidwa ntchito poyesa zinthu za sulfure zouma pogwiritsa ntchito cellulose butyl sulfonate water reducer kuti adziwe kuchuluka kwa sulfure.

2.3.2 Kudziwa kusinthasintha kwa matope

Kuyezedwa molingana ndi 6.5 mu GB8076-2008. Ndiye kuti, choyamba yesani madzi/simenti/mchenga wokhazikika pa choyezera madzi cha simenti cha NLD-3 pamene kukula kwake kuli (180±2)mm. simenti, kuchuluka kwa madzi komwe kumayesedwa ndi 230g), kenako onjezerani choyezera madzi chomwe kulemera kwake ndi 1% ya kulemera kwa simenti kumadzi, malinga ndi simenti/choyezera madzi/mchenga wokhazikika=450g/4.5g/230 g/ Chiŵerengero cha 1350 g chimayikidwa mu chosakanizira cha simenti cha JJ-5 ndikusakanizidwa mofanana, ndipo kukula kwa kukula kwa simenti pa choyezera madzi cha simenti kumayesedwa, komwe ndi kuchuluka kwa madzi komwe kumayesedwa.

2.3.3 Kufotokozera Zinthu

Chitsanzocho chinadziwika ndi FT-IR pogwiritsa ntchito EQUINOX 55 type Fourier transform infrared spectrometer ya Bruker Company; H NMR spectrum ya chitsanzocho inadziwika ndi INOVA ZAB-HS plow superconducting nuclear magnetic resonance instrument ya Varian Company; Kapangidwe ka chinthucho kanawonedwa pansi pa maikulosikopu; XRD analysis idachitika pa chitsanzocho pogwiritsa ntchito X-ray diffractometer ya MAC Company M18XHF22-SRA.

3. Zotsatira ndi zokambirana

3.1 Zotsatira za makhalidwe

3.1.1 Zotsatira za FT-IR

Kusanthula kwa infrared kunachitika pa cellulose ya microcrystalline yokhala ndi digiri ya polymerization Dp=45 ndi chinthu chomwe SBC idapanga kuchokera kuzinthu zopangirazi. Popeza nsonga za kuyamwa za SC ndi SH ndizofooka kwambiri, sizoyenera kuzindikirika, pomwe S=O ili ndi nsonga yamphamvu ya kuyamwa. Chifukwa chake, ngati pali gulu la sulfonic acid mu kapangidwe ka mamolekyulu zitha kudziwika potsimikizira kukhalapo kwa nsonga ya S=O. Mwachiwonekere, mu selulosi, pali nsonga yamphamvu ya kuyamwa pa nambala ya mafunde ya 3344 cm-1, yomwe imayambitsidwa ndi nsonga ya hydroxyl stretching vibration mu cellulose; nsonga yamphamvu ya kuyamwa pa nambala ya mafunde ya 2923 cm-1 ndi nsonga ya methylene (-CH2). Nsonga ya kugwedezeka; mndandanda wa magulu opangidwa ndi 1031, 1051, 1114, ndi 1165cm-1 amawonetsa nsonga ya kuyamwa ya kugwedezeka kwa hydroxyl stretching ndi nsonga ya absorption ya ether bond (COC) bending vibration; Nambala ya mafunde 1646cm-1 imasonyeza haidrojeni yopangidwa ndi hydroxyl ndi madzi omasuka. Chimake cha bond absorption; gulu la 1432 ~ 1318cm-1 limasonyeza kukhalapo kwa kapangidwe ka cellulose crystal. Mu IR spectrum ya SBC, mphamvu ya gulu la 1432 ~ 1318cm-1 imafooka; pomwe mphamvu ya chimake cha absorption pa 1653 cm-1 imawonjezeka, zomwe zikusonyeza kuti mphamvu yopangira ma hydrogen bonds imalimbikitsidwa; 1040, 605cm-1 imawoneka ngati peaks yolimba ya Absorption, ndipo ziwirizi sizikuwonetsedwa mu infrared spectrum ya cellulose, yoyamba ndi chimake cha absorption cha S=O bond, ndipo yomaliza ndi chimake cha absorption cha bond ya SO. Kutengera ndi kusanthula pamwambapa, zitha kuwoneka kuti pambuyo pa etherification reaction ya cellulose, pali magulu a sulfonic acid mu unyolo wake wa molekyulu.

3.1.2 Zotsatira za mafotokozedwe a H NMR

Mtundu wa H NMR wa cellulose butyl sulfonate ukhoza kuwoneka: mkati mwa γ=1.74~2.92 pali kusintha kwa hydrogen proton chemical kwa cyclobutyl, ndipo mkati mwa γ=3.33~4.52 pali cellulose anhydroglucose unit Kusintha kwa chemical kwa oxygen proton mu γ=4.52~6 ndi kusintha kwa chemical kwa methylene proton mu gulu la butylsulfonic acid lolumikizidwa ndi oxygen, ndipo palibe pachimake pa γ=6~7, zomwe zikusonyeza kuti mankhwalawa si Ma proton ena alipo.

3.1.3 Zotsatira za SEM

Kuwona kwa SEM kwa pulp ya thonje ya cellulose, microcrystalline cellulose ndi butylsulfonate ya cellulose. Pofufuza zotsatira za kusanthula kwa SEM kwa pulp ya thonje ya cellulose, microcrystalline cellulose ndi cellulose butanesulfonate ya product (SBC), zapezeka kuti microcrystalline cellulose yomwe idapezeka pambuyo pa hydrolysis ndi HCL ingasinthe kwambiri kapangidwe ka ulusi wa cellulose. Kapangidwe ka ulusi kanawonongeka, ndipo tinthu tating'onoting'ono ta cellulose tomwe tinasonkhana tinapezeka. SBC yomwe idapezeka pochitapo kanthu ndi BS sinali ndi kapangidwe ka ulusi ndipo kwenikweni idasanduka kapangidwe ka amorphous, komwe kanali kothandiza pakusungunuka kwake m'madzi.

3.1.4 Zotsatira za XRD

Kuchuluka kwa kristalo wa cellulose ndi zotumphukira zake kumatanthauza kuchuluka kwa dera la kristalo lomwe limapangidwa ndi kapangidwe ka cellulose unit yonse. Pamene cellulose ndi zotumphukira zake zimachitika ndi mankhwala, ma hydrogen bonds mu molekyulu ndi pakati pa mamolekyu amawonongeka, ndipo dera la kristalo lidzakhala dera lopanda mawonekedwe, motero limachepetsa kuchuluka kwa kristalo. Chifukwa chake, kusintha kwa kristalo musanayambe komanso pambuyo pa yankho ndi muyeso wa cellulose Chimodzi mwazofunikira kuti mutenge nawo mbali mu yankho kapena ayi. Kusanthula kwa XRD kunachitika pa microcrystalline cellulose ndi cellulose butanesulfonate yopangidwa. Zitha kuwoneka poyerekeza kuti pambuyo pa etherification, kristalo imasintha kwambiri, ndipo chinthucho chasandulika kwathunthu kukhala kapangidwe kopanda mawonekedwe, kotero kuti chikhoza kusungunuka m'madzi.

3.2 Zotsatira za kuchuluka kwa polymerization ya zinthu zopangira pa ntchito yochepetsa madzi ya chinthucho

Kuyenda kwa matope kumasonyeza mwachindunji momwe mankhwalawo amachepetsera madzi, ndipo kuchuluka kwa sulfure m'matopewo ndi chimodzi mwazinthu zofunika kwambiri zomwe zimakhudza kuyenda kwa matopewo. Kuyenda kwa matopewo kumayesa momwe mankhwalawo amachepetsera madzi.

Pambuyo posintha momwe hydrolysis reaction imagwirira ntchito kuti ikonze MCC yokhala ndi madigiri osiyanasiyana a polymerization, malinga ndi njira yomwe ili pamwambapa, sankhani njira inayake yopangira zinthu za SBC, yesani kuchuluka kwa sulfure kuti muwerengere digiri yosinthira zinthu, ndikuwonjezera zinthu za SBC ku madzi/simenti/dongosolo losakaniza mchenga wamba. Yesani kusinthasintha kwa matope.

Kuchokera ku zotsatira za kafukufuku, zikuwoneka kuti mkati mwa kafukufuku, pamene digiri ya polymerization ya microcrystalline cellulose raw material ili pamwamba, kuchuluka kwa sulfure (digiri yosinthira) ya chinthucho ndi kutsika kwa matope kumakhala kochepa. Izi zili choncho chifukwa: kulemera kwa mamolekyulu a zinthuzo ndi kochepa, zomwe zimathandiza kuti zinthuzo zisakanikirane bwino komanso kulowa kwa etherification agent, motero zimapangitsa kuti etherification ya chinthucho ikule bwino. Komabe, kuchuluka kwa madzi a chinthucho sikukwera molunjika ndi kuchepa kwa mlingo wa polymerization wa zinthuzo. Zotsatira za kafukufukuyu zikuwonetsa kuti kutsika kwa matope a simenti osakaniza ndi SBC okonzedwa pogwiritsa ntchito microcrystalline cellulose yokhala ndi digiri ya polymerization Dp<96 (kulemera kwa mamolekyulu<15552) ndi kwakukulu kuposa 180 mm (komwe kuli kwakukulu kuposa popanda wochepetsera madzi). kuchuluka kwa madzi, zomwe zikusonyeza kuti SBC ikhoza kukonzedwa pogwiritsa ntchito cellulose yokhala ndi kulemera kwa mamolekyulu kosakwana 15552, ndipo kuchuluka kwa madzi komwe kungapezeke kungapezeke; SBC imakonzedwa pogwiritsa ntchito microcrystalline cellulose yokhala ndi digiri ya polymerization ya 45 (kulemera kwa mamolekyulu: 7290), ndipo ikawonjezeredwa ku konkriti, kusinthasintha kwa matope komwe kumayesedwa ndi kwakukulu kwambiri, kotero zimaganiziridwa kuti cellulose yokhala ndi digiri ya polymerization ya pafupifupi 45 ndiyo yoyenera kwambiri pokonzekera SBC; pamene digiri ya polymerization ya zipangizo zopangira ili yoposa 45, kusinthasintha kwa matope kumachepa pang'onopang'ono, zomwe zikutanthauza kuti kuchepa kwa madzi kumachepa. Izi zili choncho chifukwa pamene kulemera kwa mamolekyulu kuli kwakukulu, mbali imodzi, kukhuthala kwa dongosolo losakaniza kudzawonjezeka, kufanana kwa simenti kudzachepa, ndipo kufalikira kwa konkriti kudzakhala pang'onopang'ono, zomwe zidzakhudza kufalikira; kumbali ina, pamene kulemera kwa mamolekyulu kuli kwakukulu, ma macromolecule a superplasticizer ali mu mawonekedwe a coil osasinthika, omwe ndi ovuta kuwameza pamwamba pa tinthu ta simenti. Koma pamene mlingo wa polymerization wa zopangira uli wochepera 45, ngakhale kuti kuchuluka kwa sulfure (digiri yosinthira) ya chinthucho kuli kwakukulu, kusinthasintha kwa chisakanizo cha matope kumayambanso kuchepa, koma kuchepa kumakhala kochepa kwambiri. Chifukwa chake n'chakuti pamene kulemera kwa molekyulu ya chinthu chochepetsera madzi kuli kochepa, ngakhale kufalikira kwa molekyulu kumakhala kosavuta komanso konyowa bwino, kufulumira kwa mamolekyulu kumakhala kwakukulu kuposa kwa molekyulu, ndipo unyolo woyendera madzi ndi waufupi kwambiri, ndipo kukangana pakati pa tinthu tating'onoting'ono ndi kwakukulu, komwe kumakhala kovulaza konkriti. Kufalikira sikwabwino ngati kwa chochepetsera madzi chokhala ndi kulemera kwakukulu kwa molekyulu. Chifukwa chake, ndikofunikira kwambiri kuwongolera bwino kulemera kwa molekyulu ya nkhope ya nkhumba (segment cellulose) kuti muwongolere magwiridwe antchito a chochepetsera madzi.

3.3 Zotsatira za momwe zinthu zimachitikira pa ntchito yochepetsa madzi ya chinthucho

Kudzera mu zoyeserera, zapezeka kuti kuwonjezera pa kuchuluka kwa polymerization ya MCC, chiŵerengero cha ma reactants, kutentha kwa reaction, kuyatsa kwa zinthu zopangira, nthawi yopangira zinthu, ndi mtundu wa chinthu choyimitsa zonse zimakhudza magwiridwe antchito a chinthucho ochepetsa madzi.

3.3.1 Chiŵerengero cha Reactant

(1) Mlingo wa BS

Pansi pa mikhalidwe yomwe yatsimikiziridwa ndi magawo ena a njira (mlingo wa polymerization wa MCC ndi 45, n(MCC):n(NaOH)=1:2.1, wothandizira woyimitsa ndi isopropanol, nthawi yoyambitsa cellulose kutentha kwa chipinda ndi 2h, kutentha kwa kapangidwe ndi 80°C, ndi nthawi yopangira 5h), kuti tifufuze momwe kuchuluka kwa wothandizira etherification 1,4-butane sultone (BS) kumakhudzira kuchuluka kwa magulu a butanesulfonic acid a chinthucho komanso kuchuluka kwa matope.

Zikuoneka kuti pamene kuchuluka kwa BS kukuwonjezeka, kuchuluka kwa magulu a butanesulfonic acid m'malo mwake komanso kuchuluka kwa matope kumawonjezeka kwambiri. Pamene chiŵerengero cha BS ku MCC chikufika pa 2.2:1, kuchuluka kwa DS ndi matope kumafika pamlingo wapamwamba kwambiri, zimaganiziridwa kuti mphamvu yochepetsera madzi ndiyo yabwino kwambiri panthawiyi. Mtengo wa BS unapitirira kukwera, ndipo kuchuluka kwa kusintha ndi kuchuluka kwa matope kunayamba kuchepa. Izi zili choncho chifukwa BS ikapitirira, BS idzachitapo kanthu ndi NaOH kuti ipange HO-(CH2)4SO3Na. Chifukwa chake, pepalali limasankha chiŵerengero chabwino kwambiri cha BS ku MCC monga 2.2:1.

(2) Mlingo wa NaOH

Pansi pa mikhalidwe yomwe yatsimikiziridwa ndi magawo ena a njira (mlingo wa polymerization wa MCC ndi 45, n(BS):n(MCC)=2.2:1. Chogwirizira ndi isopropanol, nthawi yoyambitsa cellulose kutentha kwa chipinda ndi 2h, kutentha kwa kapangidwe ndi 80°C, ndi nthawi yopangira ndi 5h), kuti tifufuze momwe kuchuluka kwa sodium hydroxide kumakhudzira kuchuluka kwa magulu a butanesulfonic acid m'malo mwake komanso kuchuluka kwa matope.

Zikuoneka kuti, ndi kuwonjezeka kwa kuchuluka kwa kuchepetsa, mlingo wa kusintha kwa SBC umawonjezeka mofulumira, ndipo umayamba kuchepa utafika pamtengo wapamwamba kwambiri. Izi zili choncho chifukwa, pamene kuchuluka kwa NaOH kuli kwakukulu, pali ma free bases ambiri mu dongosolo, ndipo mwayi wa zochitika zina umawonjezeka, zomwe zimapangitsa kuti othandizira ambiri a etherification (BS) azichita nawo zochitika zina, motero kuchepetsa mlingo wa kusintha kwa magulu a sulfonic acid mu chinthucho. Pa kutentha kwakukulu, kukhalapo kwa NaOH yochulukirapo kudzawononganso cellulose, ndipo magwiridwe antchito ochepetsa madzi a chinthucho adzakhudzidwa ndi mlingo wochepa wa polymerization. Malinga ndi zotsatira za kuyesera, pamene chiŵerengero cha molar cha NaOH ku MCC chili pafupifupi 2.1, mlingo wa kusintha ndiye waukulu kwambiri, kotero pepalali limatsimikizira kuti chiŵerengero cha molar cha NaOH ku MCC ndi 2.1:1.0.

3.3.2 Zotsatira za kutentha kwa zinthu zomwe zimakhudzidwa ndi kutentha kwa madzi zomwe zimachititsa kuti zinthu zichepetse mphamvu ya madzi

Pansi pa mikhalidwe yomwe yatsimikiziridwa ndi magawo ena a njira (mlingo wa polymerization wa MCC ndi 45, n(MCC):n(NaOH):n(BS)=1:2.1:2.2, chinthu choyimitsa ndi isopropanol, ndipo nthawi yoyambitsa cellulose kutentha kwa chipinda ndi 2h. Nthawi 5h), mphamvu ya kutentha kwa kaphatikizidwe pamlingo wosinthira magulu a butanesulfonic acid mu chinthucho idafufuzidwa.

Zikuoneka kuti pamene kutentha kwa reaction kumawonjezeka, digiri ya sulfonic acid substitution DS ya SBC imawonjezeka pang'onopang'ono, koma kutentha kwa reaction kukapitirira 80 °C, DS imasonyeza kutsika. Kuyankha kwa etherification pakati pa 1,4-butane sultone ndi cellulose ndi endothermic reaction, ndipo kuwonjezera kutentha kwa reaction kumapindulitsa pa reaction pakati pa etherifying agent ndi cellulose hydroxyl group, koma ndi kuwonjezeka kwa kutentha, zotsatira za NaOH ndi cellulose zimawonjezeka pang'onopang'ono. Zimakhala zolimba, zomwe zimapangitsa kuti cellulose iwonongeke ndikugwa, zomwe zimapangitsa kuti kulemera kwa molekyulu ya cellulose kuchepe komanso kupanga shuga ang'onoang'ono a molekyulu. Kuyankha kwa mamolekyu ang'onoang'ono otere okhala ndi etherifying agents ndikosavuta, ndipo etherifying agents ambiri adzagwiritsidwa ntchito, zomwe zimakhudza kuchuluka kwa kusintha kwa mankhwalawo. Chifukwa chake, nkhaniyi ikuwona kuti kutentha koyenera kwambiri kwa reaction pa etherification reaction ya BS ndi cellulose ndi 80℃.

3.3.3 Zotsatira za nthawi yochitira zinthu pa ntchito yochepetsa madzi a chinthucho

Nthawi yochitira zinthu imagawidwa m'magulu awiri: kutentha kwa chipinda, nthawi yopangira zinthu zopangidwira kutentha kwa chipinda, ndi nthawi yopangira zinthu zopangidwira kutentha kwa nthawi zonse.

(1) Nthawi yoyatsira kutentha kwa chipinda cha zipangizo zopangira

Pansi pa mikhalidwe yabwino kwambiri ya ndondomekoyi (mlingo wa MCC wa polymerization ndi 45, n(MCC):n(NaOH):n(BS)=1:2.1:2.2, chinthu choyimitsa ndi isopropanol, kutentha kwa kaphatikizidwe ndi 80°C, nthawi yopangira kutentha kwa chinthucho ndi 5h), fufuzani momwe nthawi yoyatsira kutentha kwa chipinda imakhudzira kuchuluka kwa kusintha kwa gulu la butanesulfonic acid.

Zikuoneka kuti kuchuluka kwa gulu la butanesulfonic acid la SBC kumawonjezeka kaye kenako kumachepa ndi nthawi yogwira ntchito. Chifukwa chowunikira chingakhale chakuti ndi kuchuluka kwa nthawi yogwira ntchito ya NaOH, kuwonongeka kwa cellulose kumakhala kwakukulu. Chepetsani kulemera kwa maselo a cellulose kuti mupange shuga wang'onoang'ono wa mamolekyulu. Kuchita kwa mamolekyu ang'onoang'ono otere ndi zinthu zotenthetsera ndikosavuta, ndipo zinthu zambiri zotenthetsera zidzagwiritsidwa ntchito, zomwe zimakhudza kuchuluka kwa kusintha kwa chinthucho. Chifukwa chake, pepalali likuwona kuti nthawi yogwiritsira ntchito kutentha kwa chipinda cha zinthu zopangira ndi maola awiri.

(2) Nthawi yopangira zinthu

Pansi pa mikhalidwe yabwino kwambiri ya ndondomekoyi, zotsatira za nthawi yoyambitsa kutentha kwa chipinda pa mlingo wosinthira gulu la butanesulfonic acid la chinthucho zinafufuzidwa. Zikuoneka kuti ndi nthawi yotalikitsa nthawi yochitapo kanthu, mlingo wosinthira umawonjezeka koyamba, koma nthawi yochitapo kanthu ikafika maola 5, DS imasonyeza kutsika. Izi zikugwirizana ndi maziko aulere omwe alipo mu etherification reaction ya cellulose. Pa kutentha kwakukulu, kutalikitsa nthawi yochitapo kanthu kumabweretsa kuwonjezeka kwa alkali hydrolysis ya cellulose, kufupikitsa kwa cellulose molecular chain, kuchepa kwa kulemera kwa molecular ya chinthucho, ndi kuwonjezeka kwa zochitika zina, zomwe zimapangitsa kuti digiri yosinthira ichepe. Mu kuyesera uku, nthawi yoyenera yopangira ndi maola 5.

3.3.4 Zotsatira za mtundu wa chinthu chopachikira pa ntchito yochepetsa madzi ya chinthucho

Pansi pa mikhalidwe yabwino kwambiri ya ndondomeko (MCC polymerization degree ndi 45, n(MCC):n(NaOH):n(BS)=1:2.1:2.2, nthawi yoyatsira zinthu zopangira kutentha kwa chipinda ndi 2h, nthawi yokhazikika yopangira zinthu ndi 5h, ndipo kutentha kwa kapangidwe kake ndi 80 ℃), motsatana sankhani isopropanol, ethanol, n-butanol, ethyl acetate ndi petroleum ether ngati zinthu zoyimitsa, ndikukambirana za momwe zimakhudzira magwiridwe antchito a chinthucho kuchepetsa madzi.

Mwachionekere, isopropanol, n-butanol ndi ethyl acetate zonse zingagwiritsidwe ntchito ngati choimitsa mu etherification reaction iyi. Ntchito ya choimitsa, kuwonjezera pa kufalitsa ma reactants, imatha kuwongolera kutentha kwa reaction. Malo otentha a isopropanol ndi 82.3°C, kotero isopropanol imagwiritsidwa ntchito ngati choimitsa, kutentha kwa dongosolo kumatha kulamulidwa pafupi ndi kutentha koyenera kwa reaction, ndipo mlingo wa kusintha magulu a butanesulfonic acid mu chinthucho ndi madzimadzi a matope ndi okwera; pomwe kutentha kwa ethanol kuli kokwera kwambiri. Kotsika, kutentha kwa reaction sikukwaniritsa zofunikira, mlingo wa kusintha magulu a butanesulfonic acid mu chinthucho ndi madzimadzi a matope ndi otsika; petroleum ether ikhoza kutenga nawo mbali mu reaction, kotero palibe mankhwala omwazikana omwe angapezeke.

4 Mapeto

(1) Kugwiritsa ntchito thonje ngati zinthu zoyambira zopangira,cellulose ya microcrystalline (MCC)Ndi digiri yoyenera ya polymerization idakonzedwa, idayambitsidwa ndi NaOH, ndipo idasinthidwa ndi 1,4-butane sultone kuti ipange butylsulfonic acid yosungunuka m'madzi. Cellulose ether, kutanthauza, chochepetsera madzi chochokera ku cellulose. Kapangidwe ka mankhwalawa kanadziwika, ndipo zidapezeka kuti pambuyo pa etherification reaction ya cellulose, panali magulu a sulfonic acid pa unyolo wake wa molekyulu, womwe unasanduka kapangidwe ka amorphous, ndipo chochepetsera madzi chinali ndi kusungunuka kwabwino kwa madzi;

(2) Kudzera mu zoyeserera, zapezeka kuti pamene mlingo wa polymerization wa microcrystalline cellulose uli 45, magwiridwe antchito ochepetsa madzi a chinthu chomwe chapezeka ndi abwino kwambiri; malinga ndi momwe mlingo wa polymerization wa zinthu zopangira watsimikizidwira, chiŵerengero cha reactants ndi n(MCC):n(NaOH):n(BS)=1:2.1:2.2, nthawi yoyatsira zinthu zopangira kutentha kwa chipinda ndi 2h, kutentha kwa kapangidwe ka chinthu ndi 80°C, ndipo nthawi yopangira ndi 5h. Magwiridwe antchito a madzi ndi abwino kwambiri.