Halaye da Halayen Butane Sulfonate Cellulose Ether Mai Rage Ruwa

Microcrystalline cellulose (MCC) tare da takamaiman digiri na polymerization samu ta acid hydrolysis na cellulose auduga ɓangaren litattafan almara aka yi amfani da albarkatun kasa. Ƙarƙashin kunna sodium hydroxide, an mayar da shi tare da 1,4-butane sultone (BS) don samun A cellulose butyl sulfonate (SBC) mai rage ruwa tare da ingantaccen ruwa mai narkewa. Tsarin samfurin ya kasance ta hanyar infrared spectroscopy (FT-IR), Nukiliya Magnetic Resonance spectroscopy (NMR), scanning electron microscopy (SEM), X-ray diffraction (XRD) da sauran hanyoyin nazari, da kuma polymerization digiri, albarkatun kasa rabo. kuma an bincika martanin MCC. Tasirin yanayin tsari na roba kamar zazzabi, lokacin amsawa, da nau'in wakili mai dakatarwa akan aikin rage ruwa na samfurin. Sakamakon ya nuna cewa: lokacin da digiri na polymerization na albarkatun kasa MCC ya kasance 45, yawan adadin masu amsawa shine: AGU (cellulose glucoside unit): n (NaOH): n (BS) = 1.0: 2.1: 2.2, The wakili mai dakatarwa shine isopropanol, lokacin kunna kayan albarkatun ƙasa a cikin zafin jiki shine 2 h, kuma lokacin kiran samfurin shine 5 h. Lokacin da zafin jiki ya kai 80 ° C, samfurin da aka samu yana da mafi girman matakin maye gurbin rukunin butanesulfonic acid, kuma samfurin yana da mafi kyawun aikin rage ruwa.

Mabuɗin kalmomi:cellulose; butylsulfonate cellulose; wakili mai rage ruwa; rage aikin ruwa

1,Gabatarwa

Concrete superplasticizer yana daya daga cikin abubuwan da ake bukata na simintin zamani. Daidai ne saboda bayyanar wakili na rage ruwa cewa za a iya tabbatar da babban aikin aiki, ƙarfin aiki mai kyau har ma da ƙarfin siminti. Masu rage ruwa mai inganci da ake amfani da su a halin yanzu sun haɗa da nau'ikan masu zuwa: naphthalene-based water reducer (SNF), sulfonated melamine resin-based water-reducer (SMF), sulfamate-based water-reducer (ASP), modified Lignosulfonate superplasticizer (SNF). ML), da polycarboxylate superplasticizer (PC), wanda a halin yanzu ana bincike sosai. Yin nazarin tsarin haɗin gwiwar masu rage ruwa, yawancin masu rage ruwa na gargajiya na gargajiya na baya suna amfani da formaldehyde tare da ƙaƙƙarfan ƙamshi mai ƙaƙƙarfan ƙamshi azaman albarkatun ƙasa don amsawar polycondensation, kuma ana aiwatar da tsarin sulfonation gabaɗaya tare da sulfuric acid mai lalata sosai ko tattara sulfuric acid. Wannan ba makawa zai haifar da illa ga ma'aikata da muhallin da ke kewaye da shi, sannan kuma zai haifar da tarin sharar gida da sharar ruwa, wadanda ba su da amfani ga ci gaba mai dorewa; duk da haka, kodayake masu rage ruwa na polycarboxylate suna da fa'idodi na ƙananan asarar siminti a kan lokaci, ƙananan sashi, mai kyau ya kwarara Yana da fa'ida daga babban yawa kuma babu abubuwa masu guba irin su formaldehyde, amma yana da wuya a inganta shi a kasar Sin saboda girman girma. farashin. Daga nazarin tushen albarkatun kasa, ba shi da wahala a gano cewa yawancin masu rage ruwa da aka ambata a sama an haɗa su bisa ga samfurori / samfurori na man fetur, yayin da man fetur, a matsayin albarkatun da ba za a iya sabuntawa ba, yana ƙara ƙaranci kuma farashinsa yana karuwa akai-akai. Saboda haka, yadda za a yi amfani da arha da ɗimbin albarkatu masu sabuntawa na halitta azaman albarkatun ƙasa don haɓaka sabbin manyan ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun ƙwararrun masana'anta.

Cellulose shine macromolecule na layi wanda aka kafa ta hanyar haɗa yawancin D-glucopyranose tare da β- (1-4) glycosidic bonds. Akwai ƙungiyoyin hydroxyl guda uku akan kowane zoben glucopyranosyl. Maganin da ya dace zai iya samun wani abin da zai sake aiki. A cikin wannan takarda, an yi amfani da ɓangaren litattafan almara na cellulose a matsayin kayan aiki na farko, kuma bayan acid hydrolysis don samun microcrystalline cellulose tare da digiri mai dacewa na polymerization, an kunna shi ta hanyar sodium hydroxide kuma ya amsa tare da 1,4-butane sultone don shirya butyl sulfonate Acid. cellulose ether superplasticizer, kuma an tattauna abubuwan da suka shafi kowane hali.

2. Gwaji

2.1 Kayan danye

Cellulose auduga ɓangaren litattafan almara, polymerization digiri 576, Xinjiang Aoyang Technology Co., Ltd .; 1,4-butane sultone (BS), masana'antu sa, samar da Shanghai Jiachen Chemical Co., Ltd .; 52.5R talakawa Portland siminti, Urumqi Samar da ta siminti factory; Sin ISO misali yashi, samar da Xiamen Ace Ou Standard Sand Co., Ltd.; sodium hydroxide, hydrochloric acid, isopropanol, methanol anhydrous, ethyl acetate, n-butanol, petroleum ether, da dai sauransu, duk tsarkakku ne na nazari, ana kasuwanci.

2.2 Hanyar gwaji

Sai a auna gwangwanin auduga kadan a nika shi da kyau, sai a zuba a cikin kwalbar wuya uku, sai a zuba wani sinadarin dilute hydrochloric acid, a jujjuya shi zuwa ruwa na wani lokaci, a sanyaye zuwa dakin, tace. wanke da ruwa har sai tsaka tsaki, da kuma bushe bushe a 50 ° C don samun Bayan samun microcrystalline cellulose albarkatun kasa tare da daban-daban digiri na polymerization, auna su digiri na polymerization bisa ga wallafe-wallafen, sanya shi a cikin wani uku-wuyansa dauki kwalban, dakatar da shi tare da. wakili mai dakatarwa 10 sau da yawa, ƙara wani adadin sodium hydroxide aqueous bayani a ƙarƙashin motsawa, Dama kuma kunna a dakin da zafin jiki na wani lokaci, ƙara adadin ƙididdiga na 1,4-butane sultone (BS), zafi sama. zuwa yanayin zafin jiki, amsa a akai-akai zazzabi na wani ɗan lokaci, sanyaya samfurin zuwa zafin daki, da samun ɗanyen samfurin ta tsotsa tacewa. A wanke da ruwa da methanol har sau 3, sannan a tace tare da tsotsa don samun samfurin ƙarshe, wato cellulose butylsulfonate water reducer (SBC).

2.3 Binciken samfur da halayyar

2.3.1 Ƙaddamar da abun ciki na sulfur samfurin da lissafin digiri na maye gurbin

An yi amfani da FLASHEA-PE2400 na'urar nazari na farko don gudanar da bincike na farko akan busashen samfurin butyl sulfonate na rage ruwa don tantance abun cikin sulfur.

2.3.2 Ƙaddamar da ruwa na turmi

An auna bisa ga 6.5 a cikin GB8076-2008. Wato da farko a auna cakuda ruwan/ciminti/misali yashi akan ma'aunin siminti turmi NLD-3 lokacin da diamita na fadada (180±2) mm. siminti, ma'aunin ruwan da aka auna shine 230g), sannan a ƙara wani wakili mai rage ruwa wanda adadinsa shine 1% na yawan siminti a cikin ruwa, bisa ga siminti / ruwa rage wakili / daidaitaccen ruwa / daidaitaccen yashi = 450g/4.5g/ 230 g/ Ana sanya rabon 1350 g a cikin mahaɗar siminti na siminti JJ-5 kuma an motsa shi daidai, kuma ana auna girman diamita na turmi akan ma'aunin ruwa na turmi, wanda shine ma'aunin ruwan turmi da aka auna.

2.3.3 Halayen Samfur

An kwatanta samfurin ta hanyar FT-IR ta amfani da nau'in EQUINOX 55 na Fourier transform infrared spectrometer na Kamfanin Bruker; da H NMR bakan na samfurin da aka halin da INOVA ZAB-HS garma superconducting nukiliya Magnetic rawa kayan aiki na Varian Company; An lura da yanayin halittar samfurin a ƙarƙashin wani microscope; An gudanar da bincike na XRD akan samfurin ta amfani da diffractometer X-ray na Kamfanin MAC M18XHF22-SRA.

3. Sakamako da tattaunawa

3.1 Sakamakon Halaye

3.1.1 Sakamakon halayyar FT-IR

An gudanar da bincike na infrared akan albarkatun microcrystalline cellulose tare da digiri na polymerization Dp = 45 da samfurin SBC da aka haɗa daga wannan kayan. Tun da kololuwar sha na SC da SH suna da rauni sosai, ba su dace da ganewa ba, yayin da S=O yana da kololuwar sha. Sabili da haka, ko akwai ƙungiyar sulfonic acid a cikin tsarin kwayoyin halitta za a iya ƙayyade ta hanyar tabbatar da kasancewar S = O kololuwa. A bayyane yake, a cikin bakan cellulose, akwai ƙaƙƙarfan ƙyalli mai ƙarfi a lamba ta 3344 cm-1, wanda aka danganta ga kololuwar girgizar girgizar hydroxyl a cikin cellulose; Ƙarfin shayarwa mai ƙarfi a lambar igiyar ruwa na 2923 cm-1 shine miƙewar rawar jiki na methylene (-CH2). Kololuwar girgiza; jerin makada da suka hada da 1031, 1051, 1114, da 1165cm-1 suna nuna kololuwar shanyewar girgizar girgizar hydroxyl da kololuwar shayarwar ether bond (COC) lankwasawa; lambar igiyar ruwa mai lamba 1646cm-1 tana nuna hydrogen da aka kafa ta hydroxyl da ruwa kyauta Ƙwararrun ɗaukar haɗin gwiwa; band na 1432 ~ 1318cm-1 yana nuna wanzuwar tsarin crystal cellulose. A cikin nau'in IR na SBC, ƙarfin ƙarfin 1432 ~ 1318cm-1 yana raunana; yayin da ƙarfin ƙwayar ƙwayar cuta a 1653 cm-1 yana ƙaruwa, yana nuna cewa ikon samar da haɗin gwiwar hydrogen yana ƙarfafa; 1040, 605cm-1 ya bayyana mafi ƙarfi Absorption kololuwa, kuma waɗannan biyun ba su bayyana a cikin infrared bakan na cellulose, tsohon shi ne halayyar sha kololuwar S = O bond, kuma na karshen shi ne halayyar sha kololuwa na SO bond. Dangane da binciken da aka yi a sama, ana iya ganin cewa bayan amsawar etherification na cellulose, akwai ƙungiyoyin sulfonic acid a cikin sarkar kwayoyin halitta.

3.1.2 H sakamakon halayyar NMR

Ana iya ganin bakan H NMR na cellulose butyl sulfonate: a cikin γ = 1.74 ~ 2.92 shine canjin sinadarai na hydrogen proton na cyclobutyl, kuma a cikin γ=3.33 ~ 4.52 shine sashin cellulose anhydroglucose Matsakaicin sinadarai na proton oxygen a cikin γ=4.52 ~ 6 shine canjin sinadarai na methylene proton a cikin rukunin butylsulfonic acid da aka haɗa da oxygen, kuma babu kololuwa a γ=6 ~ 7, yana nuna cewa samfurin ba sauran protons ba ne.

3.1.3 Sakamakon halayyar SEM

SEM lura na cellulose auduga ɓangaren litattafan almara, microcrystalline cellulose da samfurin cellulose butylsulfonate. Ta hanyar nazarin sakamakon binciken SEM na ɓangaren litattafan almara na auduga cellulose, microcrystalline cellulose da samfurin cellulose butanesulfonate (SBC), an gano cewa microcrystalline cellulose da aka samu bayan hydrolysis tare da HCL na iya canza tsarin filaye na cellulose. An lalata tsarin fibrous, kuma an sami ɓangarorin cellulose mai kyau agglomerated. SBC da aka samu ta hanyar ƙara mayar da martani tare da BS ba shi da tsarin fibrous kuma a zahiri ya rikiɗe zuwa tsarin amorphous, wanda ke da fa'ida ga rushewar ruwa.

3.1.4 Sakamakon siffanta XRD

Kristalinity na cellulose da abubuwan da suka samo asali yana nufin adadin yankin crystalline da aka kafa ta tsarin sashin cellulose a gaba ɗaya. Lokacin da cellulose da abubuwan da suka samo asali suka shiga wani nau'i na sinadarai, haɗin gwiwar hydrogen da ke cikin kwayoyin halitta da tsakanin kwayoyin halitta sun lalace, kuma yankin crystalline zai zama yanki na amorphous, wanda zai rage crystallinity. Saboda haka, canji a cikin crystallinity kafin da kuma bayan amsa shine ma'auni na cellulose Ɗaya daga cikin ma'auni don shiga cikin amsa ko a'a. An yi nazarin XRD akan microcrystalline cellulose da cellulose butanesulfonate. Ana iya gani ta hanyar kwatanta cewa bayan etherification, crystallinity ya canza asali, kuma samfurin ya canza gaba daya zuwa tsarin amorphous, don haka za'a iya narkar da shi cikin ruwa.

3.2 Tasirin digiri na polymerization na albarkatun kasa akan aikin rage ruwa na samfurin

Ruwan turmi kai tsaye yana nuna aikin rage ruwa na samfurin, kuma abun cikin sulfur na samfurin yana ɗaya daga cikin mahimman abubuwan da ke shafar ruwa na turmi. Ruwan turmi yana auna aikin rage ruwa na samfurin.

Bayan canza yanayin amsawar hydrolysis don shirya MCC tare da digiri daban-daban na polymerization, bisa ga hanyar da ke sama, zaɓi wani takamaiman tsari don shirya samfuran SBC, auna abun ciki na sulfur don ƙididdige matakin maye gurbin samfurin, sannan ƙara samfuran SBC a cikin ruwa. /ciment/daidaitaccen tsarin hadawa yashi Auna yawan ruwan turmi.

Ana iya gani daga sakamakon gwaje-gwajen cewa a cikin kewayon bincike, lokacin da digiri na polymerization na microcrystalline cellulose albarkatun kasa yana da girma, abun ciki na sulfur (masanin digiri) na samfurin da kuma ruwa na turmi yana da ƙasa. Wannan shi ne saboda: nauyin kwayoyin halitta na albarkatun kasa yana da ƙananan, wanda ya dace da haɗuwa da kayan aiki na kayan aiki da kuma shigar da wakili na etherification, don haka inganta matakin etherification na samfurin. Koyaya, ƙimar rage ruwa samfurin baya tashi a madaidaiciyar layi tare da raguwar matakin polymerization na albarkatun ƙasa. Sakamakon gwaji ya nuna cewa ruwan turmi na siminti turmi cakuda gauraye da SBC shirya ta amfani da microcrystalline cellulose tare da wani digiri na polymerization Dp <96 (nauyin kwayoyin <15552) ya fi 180 mm (wanda ya fi girma fiye da haka ba tare da rage ruwa ba) . ruwa mai ma'ana), yana nuna cewa ana iya shirya SBC ta amfani da cellulose tare da nauyin kwayoyin da bai wuce 15552 ba, kuma ana iya samun wani adadin rage ruwa; An shirya SBC ta hanyar amfani da microcrystalline cellulose tare da digiri na polymerization na 45 (nauyin kwayoyin halitta: 7290), kuma an kara da shi zuwa gaurayar kankare , ma'auni mai mahimmanci na turmi shine mafi girma, don haka ana la'akari da cewa cellulose tare da digiri na polymerization. na kusan 45 ya fi dacewa da shirye-shiryen SBC; lokacin da adadin polymerization na albarkatun kasa ya fi 45, yawan ruwa na turmi ya ragu a hankali, wanda ke nufin cewa rage yawan ruwa yana raguwa. Wannan shi ne saboda lokacin da nauyin kwayoyin halitta ya yi girma, a gefe guda, danko na tsarin cakuda zai karu, daidaitattun rarrabuwar simintin zai lalace, kuma tarwatsawa a cikin kankare zai yi jinkirin, wanda zai shafi tasirin watsawa; a daya bangaren kuma, lokacin da nauyin kwayoyin halitta ya yi girma, Macromolecules na superplasticizer suna cikin wani bazuwar coil conformation, wanda ke da wuyar haɗuwa a saman sassan siminti. Amma lokacin da matakin polymerization na albarkatun kasa ya kasance ƙasa da 45, kodayake abun ciki na sulfur (masanin digiri) na samfurin yana da girma sosai, haɓakar cakudawar turmi shima ya fara raguwa, amma raguwar ya ragu sosai. Dalili kuwa shi ne, a lokacin da nauyin kwayoyin halitta na wakili na rage ruwa ya yi kadan, duk da cewa yaduwar kwayoyin halitta yana da sauƙi kuma yana da ruwa mai kyau, saurin adsorption na kwayoyin ya fi girma fiye da na kwayoyin, kuma tsarin jigilar ruwa yana da gajeren lokaci. kuma juzu'in da ke tsakanin barbashi yana da girma, wanda ke da illa ga siminti. Tasirin watsawa ba shi da kyau kamar na mai rage ruwa tare da mafi girman nauyin kwayoyin halitta. Sabili da haka, yana da matukar mahimmanci don sarrafa nauyin kwayoyin halitta na fuskar alade (yankin cellulose) don inganta aikin mai rage ruwa.

3.3 Tasirin yanayin amsawa akan aikin rage ruwa na samfurin

An samo shi ta hanyar gwaje-gwajen cewa ban da matakin polymerization na MCC, rabon masu amsawa, zafin jiki na amsawa, kunna albarkatun ƙasa, lokacin haɗin samfur, da nau'in wakili mai dakatarwa duk suna shafar aikin rage ruwa na samfurin.

3.3.1 Rarraba Reactant

(1) Matsakaicin BS

A karkashin sharuɗɗan da aka ƙayyade ta wasu sigogi na tsari (digiri na polymerization na MCC shine 45, n (MCC): n (NaOH) = 1: 2.1, wakili mai dakatarwa shine isopropanol, lokacin kunnawa na cellulose a dakin da zafin jiki shine 2h, da Yawan zafin jiki na kira shine 80 ° C, da lokacin kira 5h), don bincika tasirin adadin etherification 1,4-butane sultone (BS) akan matakin maye gurbin butanesulfonic acid kungiyoyin na samfurin da kuma ruwa na turmi.

Ana iya ganin cewa yayin da adadin BS ya karu, matakin maye gurbin kungiyoyin butanesulfonic acid da kuma yawan ruwa na turmi yana ƙaruwa sosai. Lokacin da rabon BS zuwa MCC ya kai 2.2:1, yawan ruwa na DS da turmi ya kai matsakaicin. darajar, ana la'akari da cewa aikin rage ruwa shine mafi kyau a wannan lokacin. Ƙimar BS ta ci gaba da ƙaruwa, kuma duka biyun matakin maye gurbin da ruwa na turmi ya fara raguwa. Wannan saboda lokacin da BS ya wuce kima, BS zai amsa tare da NaOH don samar da HO-(CH2)4SO3Na. Saboda haka, wannan takarda ta zaɓi mafi kyawun rabon kayan abu na BS zuwa MCC azaman 2.2: 1.

(2) Yawan adadin NaOH

A karkashin sharuɗɗan da aka ƙayyade ta wasu sigogi na tsari (matsakaicin polymerization na MCC shine 45, n (BS): n (MCC) = 2.2: 1. Wakilin dakatarwa shine isopropanol, lokacin kunnawa na cellulose a dakin da zafin jiki shine 2h, da zafin jiki na kira shine 80 ° C, da lokacin kira 5h), don bincika tasirin adadin sodium hydroxide akan matakin maye gurbin rukunin butanesulfonic acid a cikin samfurin da kuma ruwa na turmi.

Ana iya ganin cewa, tare da karuwar adadin raguwa, matakin maye gurbin SBC yana ƙaruwa da sauri, kuma ya fara raguwa bayan ya kai matsayi mafi girma. Wannan saboda, lokacin da abun ciki na NaOH ya yi girma, akwai sansanonin kyauta da yawa a cikin tsarin, kuma yuwuwar halayen halayen haɓaka yana ƙaruwa, yana haifar da ƙarin etherification wakilai (BS) suna shiga cikin halayen gefe, don haka rage matakin maye gurbin sulfonic. kungiyoyin acid a cikin samfurin. A yanayin zafi mafi girma, kasancewar NaOH mai yawa kuma zai lalata cellulose, kuma aikin rage ruwa na samfurin zai shafi a ƙananan digiri na polymerization. Dangane da sakamakon gwaji, lokacin da rabon molar NaOH zuwa MCC ya kai kusan 2.1, matakin maye gurbin shine mafi girma, don haka wannan takarda ta ƙayyade cewa ƙimar molar NaOH zuwa MCC shine 2.1: 1.0.

3.3.2 Tasirin zafin jiki na amsawa akan aikin rage ruwa na samfur

A karkashin sharuɗɗan da aka ƙaddara ta wasu sigogi na tsari (matakin polymerization na MCC shine 45, n (MCC): n (NaOH): n (BS) = 1: 2.1: 2.2, wakili mai dakatarwa shine isopropanol, da lokacin kunnawa. cellulose a dakin da zafin jiki shine 2h Time 5h), an bincika tasirin yanayin zafin jiki akan matakin maye gurbin butanesulfonic acid a cikin samfurin.

Ana iya ganin cewa yayin da yawan zafin jiki ya karu, matakin maye gurbin sulfonic acid DS na SBC yana ƙaruwa sannu a hankali, amma lokacin da zafin jiki ya wuce 80 ° C, DS yana nuna yanayin ƙasa. Halin etherification tsakanin 1,4-butane sultone da cellulose wani abu ne na endothermic, kuma ƙara yawan zafin jiki yana da amfani ga amsawa tsakanin etherifying wakili da cellulose hydroxyl kungiyar, amma tare da karuwar yawan zafin jiki, sakamakon NaOH da cellulose a hankali yana ƙaruwa. . Ya zama mai ƙarfi, yana sa cellulose ya ragu kuma ya fadi, yana haifar da raguwa a cikin nauyin kwayoyin halitta na cellulose da kuma samar da ƙananan sukari na kwayoyin halitta. Halin irin waɗannan ƙananan ƙwayoyin cuta tare da etherifying wakilai yana da sauƙin sauƙi, kuma za a cinye ƙarin etherifying wakilai, yana tasiri matakin maye gurbin samfurin. Saboda haka, wannan labarin yayi la'akari da cewa mafi dace dauki zafin jiki ga etherification dauki na BS da cellulose ne 80 ℃.

3.3.3 Tasirin lokacin amsawa akan aikin rage ruwa na samfur

Lokacin amsawa ya kasu kashi cikin dakin zafin jiki kunna kayan albarkatun kasa da yawan zafin jiki na lokaci na samfurori.

(1) Lokacin kunna zafin ɗaki na albarkatun ƙasa

A ƙarƙashin yanayin mafi kyawun tsari na sama (digiri na MCC na polymerization shine 45, n (MCC): n (NaOH): n (BS) = 1: 2.1: 2.2, wakili mai dakatarwa shine isopropanol, yanayin halayen kira shine 80 ° C, samfurin. Yawan zafin jiki na tsawon lokaci 5h), bincika tasirin lokacin kunna zafin daki akan matakin maye gurbin samfurin butanesulfonic acid.

Ana iya ganin cewa matakin maye gurbin ƙungiyar butanesulfonic acid na samfurin SBC yana ƙaruwa da farko sannan kuma yana raguwa tare da tsawaita lokacin kunnawa. Dalilin bincike na iya zama cewa tare da karuwar lokacin aikin NaOH, lalatawar cellulose yana da tsanani. Rage nauyin kwayoyin halitta na cellulose don samar da ƙananan sukarin kwayoyin halitta. Halin irin waɗannan ƙananan ƙwayoyin cuta tare da etherifying wakilai yana da sauƙin sauƙi, kuma za a cinye ƙarin etherifying wakilai, yana tasiri matakin maye gurbin samfurin. Sabili da haka, wannan takarda yayi la'akari da cewa lokacin kunna yawan zafin jiki na kayan aiki shine 2h.

(2) Lokacin haɗin samfur

A ƙarƙashin ingantattun yanayin tsari na sama, an bincika tasirin lokacin kunnawa a cikin ɗaki akan matakin maye gurbin ƙungiyar butanesulfonic acid. Ana iya ganin cewa tare da tsawaita lokacin amsawa, matakin canji na farko yana ƙaruwa, amma lokacin da lokacin amsa ya kai 5h, DS yana nuna yanayin ƙasa. Wannan yana da alaƙa da tushe na kyauta da ke cikin etherification dauki na cellulose. A mafi girma yanayin zafi, da tsawaita lokacin dauki take kaiwa zuwa wani karuwa a cikin digiri na alkali hydrolysis na cellulose, a takaice daga cikin cellulose kwayoyin sarkar, da rage a cikin kwayoyin nauyi na samfurin, da kuma karuwa a gefe halayen, sakamakon a sakamakon. canji. digiri yana raguwa. A cikin wannan gwaji, madaidaicin lokacin haɗawa shine 5h.

3.3.4 Tasirin nau'in wakili na dakatarwa akan aikin rage ruwa na samfurin

A ƙarƙashin mafi kyawun yanayin tsari (digiri na MCC polymerization shine 45, n (MCC): n (NaOH): n (BS) = 1: 2.1: 2.2, lokacin kunna kayan albarkatun ƙasa a cikin zafin jiki shine 2h, lokacin haɗuwa da zafin jiki akai-akai. na kayayyakin ne 5h, da kuma kira zafin jiki dauki 80 ℃), bi da bi zaži isopropanol, ethanol, n-butanol, ethyl acetate da man fetur ether a matsayin dakatar jamiái, da kuma tattauna su tasiri a kan ruwa-rage aikin samfurin.

Babu shakka, isopropanol, n-butanol da ethyl acetate za a iya amfani da su azaman wakili mai dakatarwa a cikin wannan amsawar etherification. Matsayin wakili mai dakatarwa, ban da tarwatsa masu amsawa, na iya sarrafa yanayin zafin jiki. Matsayin tafasa na isopropanol shine 82.3 ° C, don haka ana amfani da isopropanol azaman wakili mai dakatarwa, za'a iya sarrafa zafin jiki na tsarin kusa da mafi kyawun zafin jiki, da matakin maye gurbin rukunin butanesulfonic acid a cikin samfurin da kuma yawan ruwa. turmi yana da inganci; yayin da ma'aunin tafasar ethanol ya yi yawa Low, yawan zafin jiki bai dace da buƙatun ba, matakin maye gurbin rukunin butanesulfonic acid a cikin samfurin da ƙarancin turmi sun yi ƙasa; ether petroleum na iya shiga cikin abin da ya faru, don haka ba za a iya samun samfurin da aka tarwatsa ba.

4 Kammalawa

(1) Yin amfani da ɓangaren litattafan almara a matsayin kayan asali na farko,microcrystalline cellulose (MCC)tare da matakin da ya dace na polymerization an shirya shi, wanda NaOH ya kunna, kuma ya amsa tare da 1,4-butane sultone don shirya butylsulfonic acid cellulose ether mai narkewa mai ruwa, wato, mai rage ruwa na cellulose. An kwatanta tsarin samfurin, kuma an gano cewa bayan amsawar etherification na cellulose, akwai ƙungiyoyin sulfonic acid a kan sarkar kwayoyin halitta, wanda ya rikide zuwa tsarin amorphous, kuma samfurin mai rage ruwa yana da ruwa mai kyau;

(2) Ta hanyar gwaje-gwaje, an gano cewa lokacin da digiri na polymerization na microcrystalline cellulose shine 45, aikin rage ruwa na samfurin da aka samu shine mafi kyau; A karkashin yanayin da aka ƙaddara matakin polymerization na albarkatun ƙasa, rabon masu amsawa shine n (MCC): n (NaOH): n ( BS) = 1: 2.1: 2.2, lokacin kunna kayan albarkatun ƙasa a cikin zafin jiki shine. 2h, samfurin samfurin zafin jiki shine 80 ° C, kuma lokacin kira shine 5h. Ayyukan ruwa yana da kyau.