Synthesis uye Hunhu hweButane Sulfonate Cellulose Ether Mvura Reducer

Microcrystalline cellulose (MCC) ine dhigirii chaiyo yepolymerization yakawanikwa neacid hydrolysis ye cellulose donje pulp yakashandiswa seyakagadzirwa. Pasi pekushandiswa kwe sodium hydroxide, yakaitwa ne 1,4-butane sultone (BS) kuti iwane A cellulose butyl sulfonate (SBC) inoderedza mvura ine yakanaka solubility yemvura yakagadzirwa. Chimiro chechigadzirwa chairatidzwa ne infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy (NMR), scanning electron microscopy (SEM), X-ray diffraction (XRD) nedzimwe nzira dzekuongorora, uye dhigirii repolymerization, raw material ratio, uye maitiro eMCC zvakaongororwa. Mhedzisiro yemamiriro ekugadzira maitiro senge tembiricha, nguva yekuita, uye mhando yekumisa mumiriri pakuita kwekudzikisa mvura kwechigadzirwa. Mhedzisiro yacho inoratidza kuti: kana dhigirii repolymerization yeMCC raw raw iri makumi mana neshanu, chiyero chehuwandu hwema reactants ndeichi: AGU (cellulose glucoside unit): n (NaOH): n (BS) = 1.0: 2.1: 2.2, Iyo yekumisa mumiriri is isopropanol, iyo activation yenguva yenguva yechigadzirwa cheiyo 2. 5 h. Kana tembiricha iri 80 ° C, chigadzirwa chakawanikwa chine dhigirii yepamusoro yekutsiviwa kwemapoka ebutanesulfonic acid, uye chigadzirwa chine yakanyanya kunaka yekudzikisa mvura.

Mazwi akakosha:cellulose; cellulose butylsulfonate; mvura inoderedza mumiririri; mvura kuderedza kushanda

1,Nhanganyaya

Concrete superplasticizer ndechimwe chezvinhu zvakakosha zvekongiri yemazuva ano. Izvo chaizvo nekuda kwekuonekwa kwemvura inodzikisa agent iyo yakanyanya kushanda, yakanaka kusimba uye kunyange yakakwirira simba rekongiri inogona kuvimbiswa. Ikozvino inoshandiswa zvakanyanya-inoderedza mvura inoderedza kunyanya inosanganisira zvinotevera: naphthalene-based water reducer (SNF), sulfonated melamine resin-based water-reducer (SMF), sulfamate-based water-reducer (ASP), yakagadziridzwa Lignosulfonate superplasticizer (ML), uye polycarboxylate inoshingaira superplasticizer (PC), iyo ikozvino inotsvakurudza. Kuongorora maitiro ekugadzira ezvidzikisiri zvemvura, mazhinji ekare ekare echinyakare condensate anoderedza mvura anoshandisa formaldehyde ine yakasimba pungent hwema seyakabikwa yepolycondensation reaction, uye iyo sulfonation process inowanzoitwa ine corrosive fuming sulfuric acid kana concentrated sulfuric acid. Izvi zvinozokonzera mhedzisiro yakaipa kune vashandi uye nharaunda yakapoteredza, uye ichaitawo huwandu hukuru hwemarara emarara uye tsvina yemvura, iyo isingakodzeri kubudirira kwakasimba; zvisinei, kunyange zvazvo polycarboxylate water reducers vane zvakanakira kurasikirwa kuduku kwekongiri nekufamba kwenguva, dhigirii yakaderera, kuyerera kwakanaka Iine zvakanakira kukwirira kwepamusoro uye pasina zvinhu zvine chepfu zvakadai se formaldehyde, asi zvakaoma kuikurudzira muChina nekuda kwemutengo wepamusoro. Kubva pakuongorora kunobva zvinhu zvakasvibirira, hazvisi zvakaoma kuwana kuti vazhinji vevadziviriri vemvura vataurwa pamusoro apa vanogadzirwa zvichienderana nepetrochemical products / by-products, nepo petroleum, sechinhu chisingagadziriswi, chiri kuwedzera kushayikwa uye mutengo wayo unoramba uchikwira. Naizvozvo, mashandisiro ekushandisa zvakachipa uye akawanda echisikigo anogona kudzokororwa zviwanikwa semidziyo mitsva yekugadzira nyowani yepamusoro-inoshanda kongiri superplasticizers yave yakakosha yekutsvagisa nzira yekongiri superplasticizers.

Cellulose is linear macromolecule inoumbwa nekubatanidza D-glucopyranose yakawanda ne β-(1-4) glycosidic bonds. Kune matatu mapoka emahydroxyl pane yega yega glucopyranosyl ring. Kurapa kwakakodzera kunogona kuwana imwe reactivity. Mupepa iri, cellulose donje pulp yakashandiswa seyekutanga mbishi, uye mushure measidhi hydrolysis kuti iwane microcrystalline cellulose ine dhigirii yakakodzera yepolymerization, yakagadziriswa nesodium hydroxide uye yakaitwa ne 1,4-butane sultone kugadzira butyl sulfonate Acid cellulose ether superplasticizer, uye izvo zvinopesvedzera zvega rega zvakakurukurwa.

2. Kuedza

2.1 Raw zvinhu

Cellulose donje pulp, polymerization dhigirii 576, Xinjiang Aoyang Technology Co., Ltd.; 1,4-butane sultone (BS), giredhi yeindasitiri, yakagadzirwa neShanghai Jiachen Chemical Co., Ltd.; 52.5R yakajairwa Portland simende, Urumqi Inopihwa nefekitori simende; China ISO yakajairika jecha, yakagadzirwa na Xiamen Ace Ou Standard Sand Co., Ltd.; sodium hydroxide, hydrochloric acid, isopropanol, anhydrous methanol, ethyl acetate, n-butanol, petroleum ether, nezvimwewo, zvose zvakachena, zvinotengeswa.

2.2 Nzira yekuedza

Yeresa imwe chiyero chedonje pulp woikuya zvakanaka, woiisa mubhodhoro remitsipa mitatu, wedzera imwe musanganiswa we dilute hydrochloric acid, kurudzira kupisa uye hydrolyze kweimwe nguva yenguva, inotonhorera kusvika kukamuri tembiricha, sefa, geza nemvura kusvika isina kwayakarerekera, uye vacuum yakaoma pa50 ° C kuti uwane Mushure mekuva ne microcrystalline cellulose yezvinyorwa zvepolymer dhigirii, isa madhigirii epolymer ezvinyorwa zvakasiyana-siyana maererano nepolymer degree. mubhodhoro rine mitsipa mitatu rekuita, rimise nemushonga unomisa kagumi pakukura kwayo, wedzera imwe sodium hydroxide aqueous solution pasi pekubvongodza, Svidza uye shandisa pamhepo tembiricha kweimwe nguva yenguva, wedzera huwandu hwakaverengerwa hwe1,4-butane sultone (BS), kupisa kusvika kune tembiricha yekuita, tora pane inogara nguva tembiricha, kutonhora kwechigadzirwa, kutonhora kweimwe nguva chigadzirwa. kusefa. Shamba nemvura uye methanol ka3, uye sefa nekusveta kuti uwane chigadzirwa chekupedzisira, chinonzi cellulose butylsulfonate water reducer (SBC).

2.3 Kuongororwa kwechigadzirwa uye maitiro

2.3.1 Kutemerwa kwechigadzirwa sarufa zvirimo uye kuverenga kwedhigirii rekutsiva

Iyo FLASHEA-PE2400 elemental analyzer yakashandiswa kuita ongororo yekutanga pane yakaomeswa cellulose butyl sulfonate mvura inoderedza chigadzirwa kuona iyo sulfur yemukati.

2.3.2 Kuona kuyerera kwedhaka

Yakayerwa zvinoenderana ne6.5 muGB8076-2008. Ndiko kuti, tanga kuyera mvura / simende / yakajairwa jecha musanganiswa paNLD-3 simende dhaka fluidity tester kana dhayamita yekuwedzera iri (180±2) mm. simende, iyo yakayerwa chiyero chekushandiswa kwemvura i230g), wobva wawedzera mvura yekudzikisa iyo ine huremu huri 1% yehuremu hwesimende kumvura, zvichienderana nesamende / mvura yekudzikisa ajenti / standard mvura / standard jecha = 450g / 4.5g / 230 g / Chiyero che1350 g chinoiswa muJJ-5 dhayamita yakasanganiswa uye dhayamita dhayamita. pa mortar fluidity tester inopimwa, inova inopimwa yemotar fluidity.

2.3.3 Chigadzirwa Chimiro

Sample yairatidzwa neFT-IR ichishandisa EQUINOX 55 mhando yeFourier inoshandura infrared spectrometer yeBruker Company; iyo H NMR spectrum yemuenzaniso yakaratidzwa neINOVA ZAB-HS gejo superconducting nuclear magnetic resonance instrument yeVarian Company; The morphology yechigadzirwa yakaonekwa pasi pe microscope; Ongororo yeXRD yakaitwa pasample nekushandisa X-ray diffractometer yeMAC Company M18XHF22-SRA.

3. Migumisiro uye nhaurirano

3.1 Maitiro ehunhu

3.1.1 FT-IR maitiro ekuita

Ongororo ye infrared yakaitwa pane yakabikwa microcrystalline cellulose ine dhigirii repolymerization Dp = 45 uye chigadzirwa SBC chakagadzirwa kubva kune iyi mbishi. Sezvo nhongonya dzeSC neSH dzisina kusimba, hadzina kukodzera kuzivikanwa, nepo S=O ine peak yakasimba yekunyura. Naizvozvo, kana paine sulfonic acid boka muchimiro chemolecular inogona kutsanangurwa nekusimbisa kuvepo kweiyo S = O peak. Zviripachena, mune cellulose spectrum, kune yakasimba kunyura peak pane wave nhamba ye 3344 cm-1, iyo inofungidzirwa kune iyo hydroxyl inotambanudza vibration peak mu cellulose; iyo yakanyanya kunyura peak pane wave nhamba ye2923 cm-1 ndiyo inotambanudzira vibration peak yemethylene (-CH2). Vibration peak; nhevedzano yemabhendi anoumbwa ne1031, 1051, 1114, uye 1165cm-1 anoratidza kunyudzwa kwepamusoro pehydroxyl inotambanudza vibration uye iyo yekunyudza peak ye ether bond (COC) bending vibration; iyo wave nhamba 1646cm-1 inoratidza iyo haidrojeni yakaumbwa nehydroxyl uye yemahara mvura Iyo bond absorption peak; iyo bhendi ye1432 ~ 1318cm-1 inoratidza kuvepo kweiyo cellulose crystal chimiro. Mune IR spectrum yeSBC, kusimba kwebhendi 1432 ~ 1318cm-1 kunopera simba; nepo kusimba kwekunyura kwepamusoro pa 1653 cm-1 kunowedzera, zvichiratidza kuti kukwanisa kugadzira hydrogen bonds kunosimbiswa; 1040. Kubva pane ongororo iri pamusoro, zvinogona kuonekwa kuti mushure mekuita kwe etherification ye cellulose, kune mapoka e sulfonic acid mumaketani ayo e-molecular.

3.1.2 H NMR maitiro ehunhu

Iyo H NMR spectrum ye cellulose butyl sulfonate inogona kuonekwa: mukati me γ = 1.74 ~ 2.92 ndiyo hydrogen proton kemikari kuchinja kwe cyclobutyl, uye mukati me γ=3.33 ~ 4.52 ndiyo cellulose anhydroglucose unit Kuchinja kwekemikari yeoxygen proton mu γ=4.52 ~ 6 yekemikari yeprotoni ye methylsu toni ye methylsu to 6 asi ikemikari yakabatana oxygen, uye hapana peak pa γ=6~7, zvichiratidza kuti chigadzirwa hachisi Mamwe maproton aripo.

3.1.3 SEM maitiro ehunhu

SEM yekucherechedza cellulose donje pulp, microcrystalline cellulose uye chigadzirwa cellulose butylsulfonate. Nekuongorora iyo SEM yekuongorora mhedzisiro ye cellulose donje pulp, microcrystalline cellulose uye chigadzirwa cellulose butanesulfonate (SBC), zvinoonekwa kuti iyo microcrystalline cellulose inowanikwa mushure me hydrolysis neHCL inogona kushandura zvakanyanya chimiro che cellulose fiber. Iyo fibrous chimiro chakaparadzwa, uye yakanaka agglomerated cellulose particles yakawanikwa. Iyo SBC yakawanikwa nekuwedzera kuita neBS yakanga isina chimiro chefibrous uye yakashandurwa kuita chimiro cheamorphous, icho chaibatsira pakuparara kwayo mumvura.

3.1.4 XRD maitiro emhedzisiro

Iyo crystallinity ye cellulose uye zvinobva mairi inoreva chikamu cheiyo crystalline dunhu rakaumbwa ne cellulose unit chimiro mune yese. Kana cellulose nezvinobuda pairi kuita kemikari kuita, zvisungo zvehydrogen mumorekuru uye pakati pemamorekuru zvinoparadzwa, uye nharaunda yecrystalline ichava dunhu reamorphous, nekudaro ichidzikisa kuchena. Nokudaro, shanduko yekristallinity isati yasvika uye mushure mekuita chiyero che cellulose Imwe yemaitiro ekutora chikamu mumhinduro kana kwete. XRD ongororo yakaitwa pamicrocrystalline cellulose uye chigadzirwa cellulose butanesulfonate. Inogona kuonekwa nekuenzanisa kuti mushure me etherification, crystallinity inoshanduka zvakanyanya, uye chigadzirwa chacho chakashandurwa zvachose kuva chimiro cheamorphous, kuitira kuti chigone kunyungudutswa mumvura.

3.2 Mhedzisiro yedhigirii repolymerization yezvigadzirwa pamvura inoderedza kuita kwechigadzirwa.

Iyo fluidity yedhaka inoratidzira zvakananga kushanda kwemvura-kuderedza kwechigadzirwa, uye sulfuri yezvinyorwa zvechigadzirwa ndechimwe chezvinhu zvakakosha zvinokanganisa kusvibiswa kwedhaka. Iyo fluidity yevhu inoyera kudzikisa mvura kwechigadzirwa.

Mushure mekushandura mamiriro ekuita kwehydrolysis kugadzirira MCC ine madhigirii akasiyana epolymerization, zvinoenderana nenzira iri pamusoro, sarudza imwe nzira yekugadzira kugadzirira zvigadzirwa zveSBC, kuyera sarufa yemukati kuverenga dhigirii rekutsiva chigadzirwa, uye wedzera zvigadzirwa zveSBC kumvura / simende / yakajairwa jecha musanganiswa system Yera kuyerera kwedhaka.

Inogona kuonekwa kubva mumigumisiro yekuedza iyo mukati mekutsvaga kwekutsvaga, apo dhigirii yepolymerization ye microcrystalline cellulose raw material yakakwira, sulfur content (inotsiva dhigirii) yechigadzirwa uye fluidity yedhaka yakaderera. Izvi zvinodaro nekuti: huremu hwemamorekuru hweiyo mbishi idiki, iyo inobatsira kune yunifomu kusanganiswa kwezvinhu zvakasvibiswa Uye kupinda kweiyo etherification agent, nekudaro inovandudza dhigirii reetherification yechigadzirwa. Nekudaro, mwero wekudzikisa mvura yechigadzirwa hausimuke mumutsara wakatwasuka nekudzikira kwedhigirii repolymerization yezvigadzirwa. Migumisiro yekuedza inoratidza kuti dhaka remvura yemusanganiswa wesamende yakasanganiswa neSBC yakagadzirirwa nekushandisa microcrystalline cellulose ine dhigirii yepolymerization Dp <96 (molecular weight<15552) yakakura kudarika 180 mm (iyo yakakura kudarika iyo isina mvura inoderedza). benchmark fluidity), zvichiratidza kuti SBC inogona kugadzirwa nekushandisa cellulose ine huremu hwemamorekuru isingasviki 15552, uye imwe chiyero chekudzikisa mvura inogona kuwanikwa; SBC inogadzirirwa nekushandisa microcrystalline cellulose ine dhigirii yepolymerization ye45 (molecular uremu: 7290), uye yakawedzerwa kune musanganiswa wekrete , iyo yakayerwa fluidity yedhaka ndiyo yakakura, saka inofungidzirwa kuti cellulose ine chidimbu chepolymerization inenge 45 inonyanya kukodzera kugadzirira kweSBC; apo dhigirii yepolymerization yezvinhu zvakasvibirira yakakura kudarika 45, kunyunguduka kwevhu kunoderera zvishoma nezvishoma, izvo zvinoreva kuti mvura inoderedza chiyero inoderera. Izvi zvinodaro nekuti kana huremu hwemamorekuru hwakakura, kune rumwe rutivi, viscosity yemusanganiswa system ichawedzera, kupararira kufanana kwesimende kuchave kwakaderera, uye kupararira mukongiri kunononoka, izvo zvinokanganisa kupararira mhedzisiro; nerumwe rutivi, kana huremu hwemamorekuru hwakakura, Iwo macromolecules e superplasticizer ari mune isina kujairika coil conformation, iyo inonetsa kushambadza pamusoro pemasimende esimende. Asi kana dhigirii yepolymerization yezvigadzirwa zvisingasviki makumi mana nemashanu, kunyange zvazvo sulfur yemukati (inotsiva dhigirii) yechigadzirwa yakakura, mvura yemusanganiswa wedhaka inotanga kuderera, asi kuderera kuduku zvikuru. Chikonzero ndechekuti kana huremu hwemamorekuru emushonga wekudzikisa mvura hudiki, kunyangwe kupararira kwema molecular kuri nyore uye kuine kunyorova kwakanaka, kukurumidza kweadsorption kwemorekuru kwakakura kupfuura iyo yemamorekuru, uye cheni yekufambisa yemvura ipfupi, uye kupokana pakati pezvimedu zvakakura, izvo zvinokuvadza kongiri. The dispersion effect haina kunaka seyeyekuderedza mvura ine hombe mamolecular huremu. Naizvozvo, zvakakosha kudzora nemazvo huremu hwema molecular yenguruve face (cellulose segment) kuvandudza mashandiro emvura inoderedza.

3.3 Mhedzisiro yemamiriro ekuita pane mvura-kudzikisa kuita kwechigadzirwa

Inowanikwa kuburikidza nekuyedza kuti mukuwedzera kune dhigirii repolymerization yeMCC, chiyero chezvinoita, tembiricha yekuita, activation yezvakagadzirwa, chigadzirwa synthesis nguva, uye mhando yekumisa mumiriri zvese zvinokanganisa kuita-kudzikisa mvura kwechigadzirwa.

3.3.1 Reactant ratio

(1) Chiyero cheBS

Pasi pemamiriro akatemerwa nemamwe maparamendi ehurongwa (dhigirii repolymerization yeMCC 45, n(MCC):n(NaOH) = 1:2.1, iyo inomisa mumiriri is isopropanol, iyo activation nguva ye cellulose pamhepo tembiricha ndeye 2h, tembiricha yekubatanidza i80 ° C, uye iyo synthesis nguva yekuongorora mhedzisiro ye5h). 1,4-butane sultone (BS) pachiyero chekutsiviwa kwebutanesulfonic acid mapoka echigadzirwa uye fluidity yedhaka.

Zvinogona kuonekwa kuti sezvo huwandu hweBS hunowedzera, dhigirii yekutsiviwa kweboka rebutanesulfonic acid uye fluidity yedhaka inowedzera zvakanyanya. Kana chiyero cheBS kune MCC chasvika 2.2: 1, iyo fluidity yeDS uye dhaka inosvika pakakwirira. kukosha, inofungidzirwa kuti mvura-inoderedza kushanda ndiyo yakanakisisa panguva ino. Kukosha kweBS kwakaramba kuchiwedzera, uye zvose dhigirii yekutsiviwa uye fluidity yevhu yakatanga kuderera. Izvi zvinodaro nekuti kana BS yakawandisa, BS ichaita neNaOH kugadzira HO-(CH2)4SO3Na. Naizvozvo, bepa rino rinosarudza yakaringana zvinhu reshiyo yeBS kune MCC se2.2:1.

(2) Chiyero cheNaOH

Pasi pemamiriro ezvinhu akatemerwa nemamwe maitiro ekugadzirisa (dhigirii yepolymerization yeMCC ndeye 45, n (BS): n (MCC) = 2.2: 1. Mushonga unomira ndeye isopropanol, nguva yekushanda ye cellulose pakushambidzika kwekamuri ndeye 2h, kupisa kwekugadzirisa ndeye 80 ° C, uye synthesis nguva ye5h), kuongorora chiyero che sodium dhigirii ye hydroxide. butanesulfonic acid mapoka mune chigadzirwa uye fluidity yedhaka.

Zvinogona kuonekwa kuti, nekuwedzera kwehuwandu hwekuderedza, dhigirii yekutsiviwa kweSBC inowedzera nokukurumidza, uye inotanga kuderera mushure mokusvika pamutengo wepamusoro. Izvi zvinodaro nekuti, kana iyo NaOH yemukati yakakwira, kune yakawandisa mabhesi emahara muhurongwa, uye mukana wekuita kwedivi kunowedzera, zvichikonzera kuti mamwe etherification agents (BS) atore chikamu mukuita kwedivi, nekudaro kuderedza dhigirii rekutsiva sulfonic acid mapoka muchigadzirwa. Pakupisa kwepamusoro, kuvapo kweNaOH yakawandisa kuchaderedzawo cellulose, uye mvura inoderedza kushanda kwechigadzirwa ichakanganiswa pachidimbu chepolymerization. Maererano nemigumisiro yekuedza, kana chiyero chemolar cheNaOH kuMCC chinenge 2.1, dhigirii yekutsiva ndiyo yakakura, saka bepa rino rinotarisa kuti molar ratio yeNaOH kuMCC i2.1: 1.0.

3.3.2 Mhedzisiro yetembiricha yekuita pane chigadzirwa chinoderedza kuita kwemvura

Pasi pemamiriro ezvinhu akatemerwa nemamwe maitiro ekugadzirisa (dhigirii yepolymerization yeMCC ndeye 45, n (MCC): n (NaOH): n (BS) = 1: 2.1: 2.2, iyo inomisa mhepo inonzi isopropanol, uye nguva yekushanda ye cellulose pakushambidzika kwekamuri ndeye 2h. Nguva 5h), pesvedzero yeadhidhi yeadhidhi yeadhidhi yeadhidhiyo yaiva substitution yeasidhi inopindirana kuferefetwa.

Zvinogona kuonekwa kuti sezvo tembiricha yekuita ichiwedzera, sulfonic acid inotsiva dhigirii DS yeSBC zvishoma nezvishoma inowedzera, asi kana tembiricha yekupindura ikadarika 80 °C, DS inoratidza kudzikira. Iyo etherification reaction pakati pe 1,4-butane sultone uye cellulose ndeye endothermic reaction, uye kuwedzera kwekuita tembiricha kunobatsira kuita pakati peetherifying agent uye cellulose hydroxyl boka, asi nekuwedzera kwekushisa, mhedzisiro yeNaOH uye cellulose inowedzera zvishoma nezvishoma. Inova yakasimba, zvichiita kuti cellulose ideredze uye iwire pasi, zvichiita kuti kuderera kwema molecular weight ye cellulose uye kuberekwa kwemashuga maduku. Kuita kwemamorekuru madiki akadaro ane etherifying agents ari nyore, uye mamwe etherifying agents anozopedzwa, zvichikanganisa dhigirii yekutsiviwa kwechigadzirwa. Naizvozvo, thesis iyi inofunga kuti yakanyanya kufanira kuita tembiricha ye etherification reaction yeBS uye cellulose i80 ℃.

3.3.3 Mhedzisiro yenguva yekuita pane chigadzirwa chekudzikisa mvura

Iyo nguva yekuita yakakamurwa kuita tembiricha yekamuri activation yezvinhu zvakabikwa uye inogara tembiricha synthesis nguva yezvigadzirwa.

(1) Room tembiricha activation nguva yezvinhu mbishi

Pasi pemamiriro epamusoro epamusoro maitiro (MCC dhigirii yepolymerization ndeye 45, n(MCC):n(NaOH):n(BS)=1:2.1:2.2, suspending agent is isopropanol, synthesis reaction tembiricha i80°C, chigadzirwa Constant tembiricha synthesis nguva 5h), ongorora pesvedzero yekamuri yekupisa yeasidhi yeboka asidhigirii

Zvinogona kuonekwa kuti dhigirii yekutsiviwa kweboka rebutanesulfonic acid yechigadzirwa SBC inowedzera kutanga uye inoderera nekuwedzera kwenguva yekushanda. Chikonzero chekuongorora chingave chokuti nekuwedzera kweNaOH nguva yekuita, kuora kwe cellulose kwakakomba. Deredza huremu hwemamorekuru ecellulose kuti ugadzire mashuga madiki. Kuita kwemamorekuru madiki akadaro ane etherifying agents ari nyore, uye mamwe etherifying agents anozopedzwa, zvichikanganisa dhigirii yekutsiviwa kwechigadzirwa. Naizvozvo, pepa iri rinoona kuti tembiricha yekamuri activation nguva yezvinhu zvakabikwa ndeye 2h.

(2) Chigadzirwa synthesis nguva

Pasi pemamiriro epamusoro pemaitiro ari pamusoro, mhedzisiro ye activation nguva pakudziya kwekamuri pachiyero chekutsiviwa kwechigadzirwa butanesulfonic acid boka yakaongororwa. Zvinogona kuonekwa kuti nekuwedzera kwenguva yekuita, dhigirii yekutsiva inotanga kuwedzera, asi kana nguva yekuita inosvika 5h, DS inoratidza kuderera. Izvi zvine chekuita neyemahara base iripo mune etherification reaction ye cellulose. Pakupisa kwepamusoro, kurebesa kwenguva yekuita kunounza kuwedzera kwechiyero che alkali hydrolysis ye cellulose, kupfupika kwe cellulose molecular chain, kuderera kwehuremu hwechigadzirwa, uye kuwedzera kwemaitiro epadivi, zvichikonzera kutsiviwa. dhigirii inodzikira. Muchiyedzo ichi, yakanakira synthesis nguva ndeye 5h.

3.3.4 Mhedzisiro yerudzi rweanomisa basa pakudzikisa mvura kwechigadzirwa.

Under the optimal process conditions (MCC polymerization degree is 45, n(MCC):n(NaOH):n(BS)=1:2.1:2.2, activation time ye mbishi pamhepo tembiricha ndeye 2h, inogara tembiricha synthesis nguva yezvigadzirwa i5h, uye synthesis reaction tembiricha 80 ℃), zvichiteerana, n-pronoltanoltanoltano, zvichiteerana acetate nepetroleum ether semaajenti ekumisa, uye kurukura nezvesimba razvo pakudzikisa mvura kwechigadzirwa.

Zviripachena, isopropanol, n-butanol uye ethyl acetate zvese zvinogona kushandiswa seanomisa mumiriri mune iyi etherification reaction. Basa remumiriri wekumisa, kunze kwekuparadzira mareactants, anogona kudzora tembiricha yekuita. Iyo yekubikira ye isopropanol ndeye 82.3 ° C, saka isopropanol inoshandiswa sechinhu chinomisa, kutonhora kwegadziriro inogona kudzorwa pedyo nepamusoro pekushisa kwekushisa, uye dhigirii yekutsiviwa kweboka rebutanesulfonic acid mune chigadzirwa uye fluidity yevhu inenge yakakwirira; nepo iyo yekubikira ye ethanol yakanyanya Kudzika, iyo inodziya tembiricha haina kusangana nezvinodiwa, dhigirii rekutsinhanisa mapoka ebutanesulfonic acid mune chigadzirwa uye fluidity yedhaka yakaderera; petroleum ether inogona kutora chikamu mukuita, saka hapana chigadzirwa chakaparadzirwa chinogona kuwanikwa.

4 Mhedziso

(1) Kushandisa donje pulp seyekutanga mbishi,microcrystalline cellulose (MCC)ine dhigirii yakakodzera yepolymerization yakagadzirwa, yakashandiswa neNaOH, uye yakaitwa ne 1,4-butane sultone kugadzira mvura-inonyungudika butylsulfonic acid Cellulose ether, kureva, cellulose-based water reducer. Kurongeka kwechigadzirwa chacho kwakaratidzwa, uye zvakaonekwa kuti mushure mekuita kwe etherification ye cellulose, pakanga pane mapoka e-sulfonic acid pacheni yaro ye molecular, iyo yakanga yashandura kuita amorphous structure, uye mvura inoderedza chigadzirwa yakanga ine mvura yakanaka yekunyungudika;

(2) Kuburikidza nemiedzo, inowanikwa kuti kana dhigirii yepolymerization ye microcrystalline cellulose iri 45, mvura inoderedza kushanda kwechigadzirwa chakawanikwa ndiyo yakanakisisa; pasi pemamiriro ekuti dhigirii yepolymerization yezvinhu zvakasvibiswa inotarwa, chiyero chezvinoita n(MCC):n(NaOH):n(BS)=1:2.1:2.2, nguva yekushandiswa kwezvinhu zvakasvibirira pane tembiricha yekamuri ndeye 2h, tembiricha yekugadzirwa kwechigadzirwa i80 ° C, uye nguva yekubatanidza i5h. Kuita kwemvura ndiko kwakaringana.