Kaphatikizidwe ndi Makhalidwe a Butane Sulfonate Cellulose Ether Water Reducer

Microcrystalline mapadi (MCC) ndi digiri yotsimikizika ya polymerization akalandira asidi hydrolysis wa mapadi thonje zamkati ntchito ngati zopangira. Pansi pa kutsegula kwa sodium hydroxide, idachitidwa ndi 1,4-butane sultone (BS) kuti ipeze A cellulose butyl sulfonate (SBC) yochepetsera madzi yokhala ndi kusungunuka kwamadzi bwino idapangidwa. Kapangidwe kazinthu kamene kamadziwika ndi ma infrared spectroscopy (FT-IR), nyukiliya maginito resonance spectroscopy (NMR), sikani ma electron microscopy (SEM), X-ray diffraction (XRD) ndi njira zina zowunikira, ndi digiri ya polymerization, chiŵerengero cha zinthu zopangira, ndi machitidwe a MCC adafufuzidwa. Zotsatira za zinthu zopangira zinthu monga kutentha, nthawi yochitirapo kanthu, ndi mtundu wa zoyimitsira pakuchita kuchepetsa madzi kwa chinthucho. Zotsatira zimasonyeza kuti: pamene digiri ya polymerization ya MCC yaiwisi ndi 45, chiwerengero cha misala cha reactants ndi: AGU (ma cellulose glucoside unit): n (NaOH): n (BS) = 1.0: 2.1: 2.2, The suspending agent ndi isopropanol, nthawi yotsegula ya chipinda chopangira, ndi nthawi yopangira kutentha kwa 2 ndi 2. 5 h. Kutentha kukakhala 80 ° C, mankhwala omwe apezeka amakhala ndi digiri yapamwamba kwambiri yamagulu a butanesulfonic acid, ndipo mankhwalawa amakhala ndi ntchito yabwino kwambiri yochepetsera madzi.

Mawu ofunikira:cellulose; cellulose butylsulfonate; kuchepetsa madzi; madzi kuchepetsa ntchito

1,Mawu Oyamba

Concrete superplasticizer ndi imodzi mwazinthu zofunika kwambiri za konkriti yamakono. Ndi ndendende chifukwa cha maonekedwe a madzi kuchepetsa wothandizira kuti mkulu workability, zabwino durability ngakhale mkulu mphamvu konkire akhoza kutsimikiziridwa. Zomwe zimagwiritsidwa ntchito kwambiri pakalipano zochepetsera madzi ogwiritsira ntchito kwambiri makamaka zikuphatikizapo magulu otsatirawa: naphthalene-based water reducer (SNF), sulfonated melamine resin-based water-reducer (SMF), sulfamate-based water-reducer (ASP), kusinthidwa Lignosulfate superplasticizer (ML), ndi polycarboxylate yogwira ntchito superplasticizer (PC), yomwe ikugwiritsidwa ntchito panopa. Kuwunika kaphatikizidwe ka zochepetsera madzi, ambiri am'mbuyomu ochepetsera madzi a condensate amagwiritsa ntchito formaldehyde yokhala ndi fungo lamphamvu ngati zinthu zopangira polycondensation reaction, ndipo njira ya sulfonation nthawi zambiri imachitika ndi dzimbiri lotentha la sulfuric acid kapena acid sulfuric acid. Izi zidzabweretsa zotsatirapo zoipa kwa ogwira ntchito ndi malo ozungulira, komanso zidzatulutsa zotsalira zambiri za zinyalala ndi madzi otayira, zomwe sizingagwirizane ndi chitukuko chokhazikika; komabe, ngakhale ochepetsera madzi a polycarboxylate ali ndi ubwino wa kutaya pang'ono kwa konkire pakapita nthawi, mlingo wochepa, kuyenda bwino Kuli ndi ubwino wa kachulukidwe kakang'ono ndipo palibe zinthu zoopsa monga formaldehyde, koma n'zovuta kulimbikitsa ku China chifukwa cha mtengo wapamwamba. Kuchokera pakuwunika kwa gwero la zopangira zopangira, sikovuta kupeza kuti ambiri omwe atchulidwa pamwambawa ochepetsera madzi amapangidwa pogwiritsa ntchito mafuta a petrochemical / ndi-products, pamene mafuta a petroleum, monga gwero losasinthika, akusowa kwambiri ndipo mtengo wake ukukwera nthawi zonse. Chifukwa chake, momwe mungagwiritsire ntchito zotsika mtengo komanso zochuluka zachilengedwe zongowonjezwdwa ngati zida zopangira zida zatsopano zopangira konkriti zapamwamba zakhala gawo lofunikira pakufufuza kwa superplasticizers konkire.

Selulosi ndi liniya macromolecule opangidwa ndi kulumikiza ambiri D-glucopyranose ndi β-(1-4) glycosidic zomangira. Pali magulu atatu a hydroxyl pa mphete iliyonse ya glucopyranosyl. Thandizo loyenera likhoza kupeza reactivity inayake. Mu pepala, mapadi thonje zamkati ntchito monga zopangira koyamba, ndipo pambuyo asidi hydrolysis kupeza mapadi microcrystalline ndi digiri yoyenera ya polymerization, izo adamulowetsa ndi sodium hydroxide ndi anachita ndi 1,4-butane sultone kukonzekera butyl sulfonate Acid mapadi efa superplasticizer, ndi chikoka zinthu zinakambirana.

2. Yesani

2.1 Zopangira

Celulosi thonje zamkati, polymerization digiri 576, Xinjiang Aoyang Technology Co., Ltd.; 1,4-butane sultone (BS), kalasi ya mafakitale, yopangidwa ndi Shanghai Jiachen Chemical Co., Ltd.; 52.5R wamba Portland simenti, Urumqi Zoperekedwa ndi fakitale simenti; China ISO muyezo mchenga, opangidwa 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 ndizoyera, zomwe zimagulitsidwa.

2.2 Njira yoyesera

Yesani kuchuluka kwa thonje zamkati ndikugaya bwino, ndikuyiyika mu botolo la khosi lachitatu, onjezerani chigawo china cha dilute hydrochloric acid, kusonkhezera kutentha ndi hydrolyze kwa nthawi inayake, kuzizira mpaka kutentha, fyuluta, kusamba ndi madzi mpaka kusalowerera ndale, ndi vacuum youma pa 50 ° C kuti mupeze. mu botolo la khosi la khosi atatu, ikani ndi suspending 10 nthawi 10 kuchuluka kwake, onjezerani madzi ena a sodium hydroxide amadzimadzi, yambitsani ndikuyambitsa kutentha kwa firiji kwa nthawi inayake, onjezerani chiwerengero cha 1,4-butane sultone (BS), kutentha mpaka kutentha, kutengera kutentha kwa nthawi zonse, kuzizira, kutentha kwa kutentha, kuzizira ndi kutentha. kusefera. Muzimutsuka ndi madzi ndi methanol kwa nthawi 3, ndi fyuluta ndi kuyamwa kupeza chomaliza, ndicho cellulose butylsulfonate water reducer (SBC).

2.3 Kusanthula kwazinthu ndi mawonekedwe

2.3.1 Kutsimikiza kwa zinthu za sulfure zomwe zili ndi sulfure ndikuwerengera kuchuluka kwa m'malo

FLASHEA-PE2400 elemental analyzer idagwiritsidwa ntchito kusanthula zinthu zowuma pa cellulose butyl sulfonate water reducer product kuti mudziwe za sulfure.

2.3.2 Kutsimikiza kwa madzi a matope

Kuyesedwa molingana ndi 6.5 mu GB8076-2008. Ndiko kuti, kuyeza choyamba madzi / simenti / muyezo mchenga osakaniza pa NLD-3 simenti matope fluidity tester pamene kukula m'mimba mwake ndi (180 ± 2) mm. simenti, kuyeza benchmark madzi kumwa ndi 230g), ndiyeno kuwonjezera wochepetsera madzi amene kulemera kwake ndi 1% ya misa simenti kumadzi, malinga simenti / madzi kuchepetsa wothandizila / muyezo madzi / muyezo mchenga = 450g/4.5g/230 g/ Chiŵerengero cha 1350 g amaikidwa mu matope osakaniza a JJ-5 ndi chipwirikiti chosakaniza ndi matope osakaniza. pa matope fluidity tester amayezedwa, umene ndi kuyeza matope fluidity.

2.3.3 Makhalidwe Azinthu

Chitsanzocho chinali chodziwika ndi FT-IR pogwiritsa ntchito mtundu wa EQUINOX 55 wa Fourier kusintha spectrometer ya infuraredi ya Bruker Company; The H NMR sipekitiramu wa chitsanzo anali yodziwika ndi INOVA ZAB-HS pulawo superconducting nyukiliya maginito resonance chida cha Varian Company; Mapangidwe a mankhwalawo adawonedwa pansi pa maikulosikopu; Kusanthula kwa XRD kunachitika pachitsanzochi pogwiritsa ntchito X-ray diffractometer ya MAC Company M18XHF22-SRA.

3. Zotsatira ndi zokambirana

3.1 Zotsatira za Makhalidwe

3.1.1 zotsatira za mawonekedwe a FT-IR

Kusanthula kwa infrared kunachitika pa cellulose ya microcrystalline yokhala ndi digiri ya polymerization Dp = 45 ndi mankhwala SBC opangidwa kuchokera kuzinthu izi. Popeza nsonga zamayamwidwe za SC ndi SH ndizofooka kwambiri, siziyenera kuzindikirika, pomwe S=O ili ndi chiwopsezo champhamvu chakuya. Choncho, ngati pali gulu la sulfonic acid mu dongosolo la maselo likhoza kutsimikiziridwa ndi kutsimikizira kukhalapo kwa nsonga ya S = O. Mwachiwonekere, mu mawonekedwe a cellulose, pali chiwongolero champhamvu choyamwa pa chiwerengero cha 3344 cm-1, chomwe chimatchedwa hydroxyl yotambasula kugwedezeka pachimake mu cellulose; nsonga yamphamvu yoyamwa pamafunde a 2923 cm-1 ndi nsonga yotambasula ya methylene (-CH2). Kugwedezeka pachimake; mndandanda wamagulu opangidwa ndi 1031, 1051, 1114, ndi 1165cm-1 amawonetsa nsonga ya mayamwidwe a hydroxyl kutambasula kugwedezeka komanso nsonga ya mayamwidwe a ether bond (COC) kugwedezeka; nambala yoweyula 1646cm-1 imawonetsa haidrojeni yopangidwa ndi hydroxyl ndi madzi aulere Chimake chomangira chomangira; gulu la 1432 ~ 1318cm-1 likuwonetsa kukhalapo kwa ma cellulose makristalo. Mu IR spectrum ya SBC, mphamvu ya gulu 1432 ~ 1318cm-1 imafooka; pamene mphamvu ya nsonga ya mayamwidwe pa 1653 cm-1 ikuwonjezeka, kusonyeza kuti mphamvu yopanga ma hydrogen bonds imalimbikitsidwa; 1040. Kutengera kusanthula pamwambapa, zitha kuwoneka kuti pambuyo pa etherification ya cellulose, pali magulu a sulfonic acid mu unyolo wake wama cell.

3.1.2 H NMR zotsatira za mawonekedwe

H NMR sipekitiramu ya cellulose butyl sulfonate imatha kuwoneka: mkati mwa γ = 1.74 ~ 2.92 ndi hydrogen proton chemical shift ya cyclobutyl, ndipo mkati mwa γ=3.33 ~ 4.52 ndi cellulose anhydroglucose unit Kusintha kwa mankhwala a oxygen proton mu γ = 4.52 ~ 4.52 ~ 6 mankhwala ogwirizana ndi yllulf acid mu gulu la yllfonic protoni mpweya, ndipo palibe pachimake pa γ=6~7, kusonyeza kuti mankhwala si Mapulotoni ena alipo.

3.1.3 Zotsatira za SEM

Kuwona kwa SEM kwa cellulose thonje zamkati, cellulose ya microcrystalline ndi cellulose butylsulfonate. Pofufuza zotsatira za kusanthula kwa SEM za zamkati za thonje, microcrystalline cellulose ndi mankhwala a cellulose butanesulfonate (SBC), apeza kuti cellulose ya microcrystalline yomwe imapezeka pambuyo pa hydrolysis ndi HCL imatha kusintha kwambiri mapangidwe a cellulose fibers. The fibrous dongosolo anawonongedwa, ndi zabwino agglomerated mapadi particles analandira. SBC yomwe idapezedwa pochitanso ndi BS inalibe mawonekedwe a ulusi ndipo idasinthidwa kukhala mawonekedwe aamorphous, omwe anali opindulitsa pakusungunuka kwake m'madzi.

3.1.4 Zotsatira za XRD

Kuwala kwa cellulose ndi zotumphukira zake kumatanthawuza kuchuluka kwa dera la crystalline lomwe limapangidwa ndi kapangidwe ka cellulose chonse. Pamene mapadi ndi zotumphukira zake akukumana ndi mankhwala anachita, zomangira haidrojeni mu molekyulu ndi pakati mamolekyu awonongedwa, ndi crystalline dera adzakhala amorphous dera, potero kuchepetsa crystallinity. Choncho, kusintha crystallinity pamaso ndi pambuyo anachita ndi muyeso wa mapadi Mmodzi mwa mfundo kutenga nawo mbali poyankha kapena ayi. Kusanthula kwa XRD kunachitika pa cellulose ya microcrystalline ndi cellulose butanesulfonate. Zitha kuwoneka poyerekezera kuti pambuyo pa etherification, crystallinity imasintha kwambiri, ndipo mankhwalawo asinthidwa kukhala mawonekedwe a amorphous, kotero kuti akhoza kusungunuka m'madzi.

3.2 Zotsatira za kuchuluka kwa ma polymerization azinthu zopangira pakuchepetsa madzi azinthu

Madzi amadzimadzi amadzimadzi amawonetsa mwachindunji ntchito yochepetsera madzi a mankhwalawa, ndipo sulfure yomwe imakhalapo ndi imodzi mwa zinthu zofunika kwambiri zomwe zimakhudza madzi a matope. The fluidity ya matope amayesa kuchepetsa madzi ntchito ya mankhwala.

Pambuyo kusintha zinthu hydrolysis anachita kukonzekera MCC ndi madigiri osiyana polymerization, malinga ndi pamwamba njira, kusankha kaphatikizidwe ndondomeko kukonzekera SBC mankhwala, kuyeza okhutira sulfure kuwerengera mankhwala m'malo digiri, ndi kuwonjezera mankhwala SBC kwa madzi / simenti / muyezo mchenga kusakaniza dongosolo Kuyeza fluidity wa matope.

Zitha kuwoneka kuchokera ku zotsatira zoyesera kuti mkati mwa kafukufuku wofufuza, pamene digiri ya polymerization ya microcrystalline cellulose yaiwisi yaiwisi imakhala yochuluka, sulfure (yolowa m'malo digiri) ya mankhwala ndi fluidity ya matope ndi otsika. Izi ndichifukwa chakuti: kulemera kwa maselo azinthu zopangira ndizochepa, zomwe zimathandiza kuti yunifolomu isakanike zopangira ndi kulowetsedwa kwa etherification wothandizira, potero kupititsa patsogolo mlingo wa etherification wa mankhwala. Komabe, mankhwala kuchepetsa mlingo wa madzi sauka molunjika ndi kuchepa kwa mlingo wa polymerization wa zipangizo. Zotsatira zoyesera zimasonyeza kuti matope amadzimadzi a matope a simenti osakaniza osakaniza ndi SBC okonzedwa pogwiritsa ntchito cellulose ya microcrystalline ndi digiri ya polymerization Dp<96 (mamolekyu kulemera<15552) ndi wamkulu kuposa 180 mm (omwe ndi aakulu kuposa opanda madzi ochepetsera). benchmark fluidity), kusonyeza kuti SBC ikhoza kukonzedwa pogwiritsa ntchito cellulose yokhala ndi mamolekyulu olemera osakwana 15552, ndipo mulingo wina wochepetsera madzi ukhoza kupezeka; SBC zakonzedwa pogwiritsa ntchito mapadi microcrystalline ndi digiri ya polymerization wa 45 (maselo kulemera: 7290), ndipo anawonjezera kusakaniza konkire , kuyeza fluidity wa matope ndi yaikulu, kotero amaona kuti mapadi ndi digiri ya polymerization pafupifupi 45 ndi abwino kwambiri pokonzekera SBC; pamene mlingo wa polymerization wa zipangizo ndi wamkulu kuposa 45, ndi fluidity ya matope pang'onopang'ono amachepetsa, kutanthauza kuti madzi kuchepetsa mlingo amachepetsa. Ichi ndi chifukwa pamene kulemera kwa maselo kuli kwakukulu, kumbali imodzi, kukhuthala kwa dongosolo losakaniza kudzawonjezeka, kufalikira kwa simenti kudzawonongeka, ndipo kubalalitsidwa mu konkire kudzachedwa, zomwe zidzakhudza kubalalitsidwa; Komano, pamene maselo kulemera ndi lalikulu, The macromolecules wa superplasticizer ali mwachisawawa koyilo conformation, amene ndi zovuta adsorb padziko particles simenti. Koma pamene mlingo wa polymerization wa zopangira ndi zosakwana 45, ngakhale zili sulfure (m'malo digiri) mankhwala ndi lalikulu, fluidity wa matope osakaniza akuyambanso kuchepa, koma kuchepa ndi kochepa kwambiri. Chifukwa chake ndi chakuti pamene kulemera kwa maselo ochepetsera madzi kumakhala kochepa, ngakhale kuti kufalikira kwa maselo ndikosavuta komanso kumakhala konyowa bwino, kuthamanga kwa molekyulu kumakhala kwakukulu kuposa molekyulu, ndi unyolo woyendetsa madzi ndi waufupi kwambiri, ndipo kukangana pakati pa tinthu tating'onoting'ono ndi kwakukulu, komwe kumawononga konkriti. Kubalalitsa kwake sikuli bwino ngati kochepetsera madzi komwe kumakhala ndi kulemera kwakukulu kwa maselo. Choncho, ndikofunika kwambiri kulamulira bwino kulemera kwa maselo a nkhope ya nkhumba (gawo la cellulose) kuti likhale ndi ntchito yochepetsera madzi.

3.3 Zotsatira za zomwe zimachitika pakugwiritsa ntchito kuchepetsa madzi kwa mankhwalawa

Amapezeka kudzera mu zoyesera kuti kuwonjezera pa digiri ya polymerization ya MCC, chiŵerengero cha reactants, kutentha anachita, kutsegula kwa zipangizo, nthawi kaphatikizidwe mankhwala, ndi mtundu wa suspending wothandizira zonse zimakhudza madzi kuchepetsa ntchito ya mankhwala.

3.3.1 Reactant ratio

(1) Mlingo wa BS

Pansi pa zomwe zimatsimikiziridwa ndi magawo ena azinthu (mlingo wa polymerization wa MCC ndi 45, n(MCC):n(NaOH) = 1:2.1, woyimitsa ndi isopropanol, nthawi yotsegulira ya cellulose pa kutentha kwa firiji ndi 2h, kutentha kwa kaphatikizidwe ndi 80°C, ndi kaphatikizidwe ka nthawi ya 5h) 1,4-butane sultone (BS) pa mlingo wolowa m'malo mwa magulu a butanesulfonic acid a mankhwala ndi fluidity ya matope.

Zitha kuwoneka kuti kuchuluka kwa BS kukuwonjezeka, kuchuluka kwa kulowetsedwa kwa magulu a butanesulfonic acid ndi fluidity ya matope kumawonjezeka kwambiri. Pamene chiŵerengero cha BS ku MCC chikufika pa 2.2: 1, madzi a DS ndi matope amafika pamtunda. mtengo, amaonedwa kuti ntchito yochepetsera madzi ndiyo yabwino kwambiri panthawiyi. Mtengo wa BS unapitilira kuwonjezeka, ndipo kuchuluka kwa kulowetsedwa m'malo ndi madzi amtondo kunayamba kuchepa. Izi ndichifukwa choti BS ikachulukira, BS imachita ndi NaOH kupanga HO-(CH2)4SO3Na. Chifukwa chake, pepalali limasankha chiŵerengero choyenera cha BS ku MCC monga 2.2:1.

(2) Mlingo wa NaOH

Pansi pa zomwe zimatsimikiziridwa ndi magawo ena a ndondomeko (mlingo wa polymerization wa MCC ndi 45, n (BS): n (MCC) = 2.2: 1. Woyimitsa ndi isopropanol, nthawi yotsegula ya cellulose pa kutentha kwa firiji ndi 2h, kutentha kwa kaphatikizidwe ndi 80 ° C, ndi kaphatikizidwe nthawi 5h), kufufuza kuchuluka kwa sodium hydroxide pa mlingo wa hydroxide Magulu a butanesulfonic acid muzogulitsa ndi fluidity ya matope.

Zitha kuwoneka kuti, ndi kuwonjezeka kwa kuchepetsa kuchepetsa, mlingo wa kulowetsedwa kwa SBC ukuwonjezeka mofulumira, ndipo umayamba kuchepa pambuyo pofika pamtengo wapamwamba kwambiri. Izi zili choncho chifukwa, pamene NaOH okhutira ndi mkulu, pali zambiri zapansi ufulu m'dongosolo, ndi mwayi wa zochita za mbali kumawonjezeka, kuchititsa owonjezera etherification agents (BS) nawo mbali zochita, potero kuchepetsa mlingo wa m'malo magulu asidi sulfonic mu mankhwala. Pa kutentha kwakukulu, kukhalapo kwa NaOH yochuluka kudzasokonezanso cellulose, ndipo ntchito yochepetsera madzi ya mankhwalawa idzakhudzidwa pamlingo wochepa wa polymerization. Malingana ndi zotsatira zoyesera, pamene chiŵerengero cha molar cha NaOH ku MCC chili pafupi ndi 2.1, mlingo wolowa m'malo ndi waukulu kwambiri, kotero pepala ili limatsimikizira kuti chiŵerengero cha molar cha NaOH ku MCC ndi 2.1: 1.0.

3.3.2 Mmene kutentha kumachitira pa ntchito yochepetsera madzi

Pansi pa zinthu anatsimikiza ndi magawo ena ndondomeko (mlingo wa polymerization wa MCC ndi 45, n(MCC):n(NaOH):n(BS) =1:2.1:2.2, kuyimitsidwa wothandizira ndi isopropanol, ndi kutsegula nthawi ya mapadi kutentha firiji ndi 2h. Time 5h), chikoka cha kaphatikizidwe kaphatikizidwe kutentha kwa asidi m'malo mankhwala anali m'malo mlingo wa kutentha kwa asidi synthesis. kufufuzidwa.

Zitha kuwoneka kuti momwe kutentha kumachulukira, digiri ya sulfonic acid substitution DS ya SBC imawonjezeka pang'onopang'ono, koma pamene kutentha kumadutsa 80 ° C, DS imasonyeza kutsika. The etherification anachita pakati 1,4-butane sultone ndi mapadi ndi endothermic anachita, ndi kuonjezera kutentha anachita ndi opindulitsa zimene anachita pakati etherifying wothandizila ndi mapadi hydroxyl gulu, koma ndi kuwonjezeka kutentha, zotsatira za NaOH ndi mapadi pang'onopang'ono kumawonjezeka. Zimakhala zamphamvu, zomwe zimapangitsa kuti cellulose iwonongeke ndikugwa, zomwe zimapangitsa kuchepa kwa maselo olemera a cellulose komanso kupanga mashuga ang'onoang'ono. Zochita za mamolekyu ang'onoang'ono okhala ndi etherifying agents ndizosavuta, ndipo zowonjezera zowonjezera zidzadyedwa, zomwe zimakhudza kuchuluka kwa m'malo mwa mankhwala. Chifukwa chake, lingaliro ili likuwona kuti kutentha koyenera kwambiri kwa etherification ya BS ndi mapadi ndi 80 ℃.

3.3.3 Zotsatira za nthawi yakuchitapo kanthu pakuchepetsa madzi

The nthawi lagawidwa mu chipinda kutentha kutsegula kwa zipangizo ndi zonse kutentha kaphatikizidwe nthawi ya mankhwala.

(1) Room kutentha kutsegula nthawi ya zipangizo

Pansi pamwambapa mulingo woyenera kwambiri ndondomeko (MCC digiri ya polymerization ndi 45, n(MCC):n(NaOH):n(BS)=1:2.1:2.2, kuyimitsidwa wothandizira ndi isopropanol, kaphatikizidwe anachita kutentha ndi 80°C, mankhwala Constant kutentha kaphatikizidwe nthawi 5h), fufuzani chikoka cha kutentha kwa gulu la asidi activation gulu la substitution acid.

Zitha kuwoneka kuti kuchuluka kwa m'malo mwa gulu la butanesulfonic acid la mankhwala SBC kumawonjezeka poyamba ndiyeno kumachepa ndi kutalika kwa nthawi yotsegula. Chifukwa chowunikira chikhoza kukhala kuti pakuwonjezeka kwa nthawi ya NaOH, kuwonongeka kwa cellulose kumakhala koopsa. Chepetsani kulemera kwa cellulose kuti mupange shuga wocheperako. Zochita za mamolekyu ang'onoang'ono okhala ndi etherifying agents ndizosavuta, ndipo zowonjezera zowonjezera zidzadyedwa, zomwe zimakhudza kuchuluka kwa m'malo mwa mankhwala. Choncho, pepalali amaona kuti chipinda kutentha kutsegula nthawi ya zipangizo ndi 2h.

(2) Nthawi yopangira zinthu

Pansi pamikhalidwe yabwino kwambiri pamwambapa, zotsatira za nthawi yotsegulira kutentha kwa firiji pamlingo wolowa m'malo mwa gulu la butanesulfonic acid. Zitha kuwoneka kuti pakutalikitsa kwa nthawi yochitira, kuchuluka kwa kulowetsedwa kumawonjezeka, koma nthawi yoyankha ikafika 5h, DS imawonetsa kutsika. Izi zikugwirizana ndi maziko aulere omwe amapezeka mu etherification reaction ya cellulose. Pa kutentha kwambiri, kutalika kwa nthawi ya zomwe zimachitika kumabweretsa kuwonjezeka kwa mlingo wa alkali hydrolysis wa mapadi, kufupikitsa unyolo wa cellulose, kuchepa kwa kulemera kwa mankhwala, ndi kuwonjezeka kwa zomwe zimachitika, zomwe zimabweretsa m'malo. digiri imachepa. Pakuyesa uku, nthawi yoyenera kaphatikizidwe ndi 5h.

3.3.4 Zotsatira za mtundu wa woyimitsira pakugwiritsa ntchito kuchepetsa madzi kwa mankhwala

Pansi mulingo woyenera kwambiri ndondomeko zinthu (MCC polymerization digiri ndi 45, n(MCC):n(NaOH):n(BS)=1:2.1:2.2, nthawi kutsegula kwa zipangizo pa firiji kutentha ndi 2h, nthawi zonse kutentha kaphatikizidwe nthawi ya mankhwala ndi 5h, ndi kaphatikizidwe anachita kutentha 80 ℃), motero, kusankha isolpanoltanol, ethanol, ethanol, ndi 2h. acetate ndi petroleum ether ngati zoyimitsa, ndikukambirana momwe zimakhudzira kuchepetsa madzi kwa mankhwalawo.

Mwachiwonekere, isopropanol, n-butanol ndi ethyl acetate zonse zitha kugwiritsidwa ntchito ngati kuyimitsira munjira iyi ya etherification. Udindo wa suspending wothandizira, kuwonjezera kumwaza reactants, akhoza kulamulira anachita kutentha. Malo otentha a isopropanol ndi 82.3 ° C, kotero isopropanol imagwiritsidwa ntchito ngati choyimitsa, kutentha kwa dongosololi kungathe kuyendetsedwa pafupi ndi momwe kutentha kumayendera, ndipo mlingo wa m'malo mwa magulu a butanesulfonic acid mu mankhwala ndi fluidity ya matope ndipamwamba kwambiri; pamene kuwira mfundo ya Mowa ndi mkulu kwambiri Low, zimene kutentha si kukumana zofunika, mlingo wa m'malo mwa butanesulfonic asidi magulu mankhwala ndi fluidity wa matope ndi otsika; petroleum ether akhoza kutenga nawo mbali pakuchita, kotero palibe mankhwala omwazika omwe angapezeke.

4 Mapeto

(1) Kugwiritsa ntchito thonje zamkati ngati zopangira zoyambira,cellcrystalline cellulose (MCC)ndi digiri yoyenera ya polymerization anakonzedwa, adamulowetsa ndi NaOH, ndipo anachita ndi 1,4-butane sultone kukonzekera madzi sungunuka butylsulfonic asidi Cellulose ether, ndiko kuti, mapadi ofotokoza madzi reducer. Mapangidwe a mankhwalawo adadziwika, ndipo adapeza kuti pambuyo pa etherification ya cellulose, panali magulu a sulfonic acid pa unyolo wa maselo, omwe adasandulika kukhala amorphous, ndipo mankhwala ochepetsera madzi anali ndi kusungunuka kwamadzi;

(2) Kupyolera mu zoyesera, zimapezeka kuti pamene digiri ya polymerization ya cellulose ya microcrystalline ndi 45, ntchito yochepetsera madzi ya mankhwala omwe adalandira ndi yabwino kwambiri; pansi pa chikhalidwe chakuti digiri ya polymerization ya zopangira imatsimikiziridwa, chiŵerengero cha reactants ndi n(MCC):n(NaOH):n(BS)=1:2.1:2.2, nthawi yotsegula ya zipangizo pa kutentha kwa chipinda ndi 2h, kutentha kwa kaphatikizidwe ka mankhwala ndi 80 °C, ndi nthawi ya kaphatikizidwe ndi 5h. Kuchita kwamadzi ndikwabwino.