1 Hoolauna
I kēia manawa, ʻo ka mea maka nui i hoʻohana ʻia i ka hoʻomākaukau ʻana ocellulose eterahe pulupulu, a ke emi nei ka hua, a ke pii pu nei ke kumukuai;
Eia kekahi, ʻoi aku ka pōʻino o nā mea etherifying e like me ka chloroacetic acid (nui loa) a me ka ethylene oxide (carcinogenic) i ke kino kanaka a me ke kaiapuni. Buke
Ma kēia mokuna, hoʻohana ʻia ka pine cellulose me ka maʻemaʻe pili ma mua o 90% i unuhi ʻia ma ka mokuna ʻelua e like me ka mea maka, a ua hoʻohana ʻia ka sodium chloroacetate a me 2-chloroethanol i mea pani.
Ke hoʻohana nei i ka waika chloroacetic ʻona loa ma ke ʻano he etherifying agent, anioniccarboxymethyl cellulose (CMC), ua hoʻomākaukau ʻia ka hydroxyethyl cellulose non-ionic.
Cellulose (HEC) a hui pū me ka hydroxyethyl carboxymethyl cellulose (HECMC) ʻekolu cellulose ethers. kumu hoʻokahi
ʻO nā ʻenehana hoʻomākaukau o ʻekolu cellulose ethers i hoʻopaʻa ʻia e nā hoʻokolohua a me nā hoʻokolohua orthogonal, a ua ʻike ʻia nā cellulose ethers synthesized e FT-IR, XRD, H-NMR, etc.
Nā kumu o ka cellulose etherification
Hiki ke hoʻokaʻawale ʻia ke kumu o ka cellulose etherification i ʻelua ʻāpana. ʻO ka hapa mua ke kaʻina hana alkalization, ʻo ia hoʻi, i ka wā o ka hoʻololi ʻana o ka cellulose,
Hoʻopuehu ʻia i loko o ka hopena NaOH, pehu nui ka pine cellulose ma lalo o ka hana o ka hoʻoulu ʻana i ka mīkini, a me ka hoʻonui ʻana o ka wai.
ʻO ka nui o nā molekole liʻiliʻi o NaOH i komo i loko o ka loko o ka pine cellulose, a hoʻopili ʻia me nā pūʻulu hydroxyl ma ke apo o ka ʻāpana hana glucose,
Hoʻopuka i ka cellulose alkali, ke kikowaena ikaika o ka hopena etherification.
ʻO ka ʻāpana ʻelua ka hana etherification, ʻo ia hoʻi, ka hopena ma waena o ke kikowaena ikaika a me ka sodium chloroacetate a i ʻole 2-chloroethanol ma lalo o nā kūlana alkaline, e hopena i
I ka manawa like, e hoʻopuka pū ka mea etherifying sodium chloroacetate a me 2-chloroethanol i kahi pae wai ma lalo o nā kūlana alkaline.
Hoʻoholo ʻia nā hopena ʻaoʻao e hana i ka sodium glycolate a me ka ethylene glycol, kēlā me kēia.
2 Hoʻomaʻamaʻa mua ʻana i ka alkali decrystallization o ka pine cellulose
ʻO ka mua, e hoʻomākaukau i kahi ʻano o ka hopena NaOH me ka wai deionized. A laila, ma kahi mahana, 2g o ka fiber pine
Hoʻoheheʻe ʻia ka huaora i loko o kahi leo o ka hopena NaOH, hoʻoulu ʻia no kekahi manawa, a laila kānana no ka hoʻohana ʻana.
Mea Hana Hoʻohālike Mea Hana
Meka pH pololei
Mea hōʻiliʻili ʻano hoʻonā wela mau
ʻO ka umu hoʻomaloʻo maloʻo
Kaulike uila
ʻO ka ʻano wai kaʻapuni ʻana i nā ʻano ʻano pauma maʻemaʻe
Fourier Transform Infrared Spectrometer
X-ray diffractometer
Nuclear Magnetic Resonance Spectrometer
Hangzhou Aolilong Instrument Co., Ltd.
ʻO Hangzhou Huichuang Mea Hana Mea Hana Co., Ltd.
ʻO Shanghai Jinghong Experimental Equipment Co., Ltd.
METTLER TOLEDO Mea Hana (Shanghai) Co., Ltd.
Hangzhou David Science and Education Instrument Co., Ltd.
ʻO American Thermo Fisher Co., Ltd.
ʻAmelika Hui Pū ʻIa Thermoelectric Switzerland ARL
Hui Swiss BRUKER
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Hoʻomākaukau i nā CMC
Ke hoʻohana nei i ka lāʻau pine lāʻau alkali cellulose i hoʻomaʻamaʻa mua ʻia e ka concentrated alkali decrystallization ma ke ʻano he mea maka, me ka hoʻohana ʻana i ka ethanol ma ke ʻano he solvent a me ka hoʻohana ʻana i ka sodium chloroacetate e like me ka etherification.
Ua hoʻomākaukau ʻia ʻo CMC me ka DS kiʻekiʻe ma ka hoʻohui ʻana i ka alkali i ʻelua a me ʻelua etherifying agent. E hoʻohui i 2g o ka lāʻau paina alkali cellulose i loko o ka ipu ʻāʻī ʻehā, a laila e hoʻohui i kahi leo o ka ethanol solvent, a hoʻoulu maikaʻi no 30min.
e pili ana, i hoʻopuehu loa ʻia ka cellulose alkali. A laila e hoʻohui i kahi nui o ka mea hana alkali a me ka sodium chloroacetate e hana ai no kahi manawa i kahi mahana etherification.
Ma hope o ka manawa, hoʻohui ʻia ka lua o ka alkaline agent a me ka sodium chloroacetate i ukali ʻia e ka etherification no kekahi manawa. Ma hope o ka pau ʻana o ka hopena, e hoʻomaha a hoʻomaha, a laila
Neutralize me ka nui kūpono o ka glacial acetic acid, a laila hoʻoheheʻe kānana, holoi a maloʻo.
Hoʻomākaukau i nā HEC
Ke hoʻohana nei i ka lāʻau paina alkali cellulose i hoʻomaʻamaʻa mua ʻia me ka decrystallization alkali koʻikoʻi ma ke ʻano he mea maka, ethanol ma ke ʻano he mea hoʻoheheʻe a me 2-chloroethanol ma ke ʻano he etherification.
Ua hoʻomākaukau ʻia ka HEC me MS kiʻekiʻe ma ka hoʻohui ʻana i ka alkali i ʻelua a me ʻelua etherifying agent. E hoʻohui i 2g o ka lāʻau paina alkali cellulose i loko o kahi hue ʻāʻī ʻehā, a hoʻohui i kahi leo o 90% (nui ka hapa) ethanol, hoʻoulu.
E hoʻoulu i kahi manawa e hoʻopuehu piha, a laila e hoʻohui i kahi nui o ka alkali, a me ka wela mālie, e hoʻohui i kahi leo o 2-
ʻO Chloroethanol, etherified ma ka wela mau no kekahi manawa, a laila hoʻohui i ke koena sodium hydroxide a me 2-chloroethanol e hoʻomau i ka etherification no kekahi manawa. mālama
Ma hope o ka pau ʻana o ka hopena, e hoʻokaʻawale me kahi nui o ka waika acetic glacial, a hope e kānana me kahi kānana aniani (G3), holoi, a maloʻo.
Ka hoomakaukau ana o HEMCC
Ke hoʻohana nei i ka HEC i hoʻomākaukau ʻia ma 3.2.3.4 ma ke ʻano he mea maka, ethanol ma ke ʻano o ka hopena, a me ka sodium chloroacetate ma ke ʻano he etherifying agent e hoʻomākaukau ai.
HECMC. ʻO ke kaʻina hana kikoʻī: e lawe i kahi nui o ka HEC, e hoʻokomo i loko o kahi pahu 100 mL ʻehā ʻāʻī, a laila hoʻohui i kahi nui o ka leo.
90% ethanol, hoʻoulu me ka mechanically no kahi manawa e hoʻopuehu piha ai, hoʻohui i kahi nui o ka alkali ma hope o ka hoʻomehana ʻana, a hoʻohui mālie.
ʻO ka sodium chloroacetate, hoʻopau ka etherification i ka mahana mau ma hope o kahi manawa. Ma hope o ka pau ʻana o ka hopena, e hoʻokaʻawale iā ia me ka glacial acetic acid e hoʻopau ai, a laila e hoʻohana i kahi kānana aniani (G3)
Ma hope o ka kānana ʻana, holoi a hoʻomaloʻo.
Hoʻomaʻemaʻe i ka cellulose ethers
I ka hoʻomākaukau ʻana o ka cellulose ether, ua hana pinepine ʻia kekahi mau huahana, ʻo ia hoʻi ka paʻakai paʻakai paʻakai inorganic a me nā mea ʻē aʻe.
haumia. I mea e hoʻomaikaʻi ai i ka maikaʻi o ka cellulose ether, ua hoʻomaʻemaʻe maʻalahi i ka cellulose ether i loaʻa. no ka mea, aia lākou i loko o ka wai
He ʻokoʻa ka solubility, no laila, hoʻohana ka hoʻokolohua i kekahi hakina leo o ka ethanol hydrated e hoʻomaʻemaʻe i nā etera cellulose ʻekolu i hoʻomākaukau ʻia.
hoololi.
E kau i ka laʻana cellulose ether i hoʻomākaukau ʻia me kekahi ʻano maikaʻi i loko o ka beaker, e hoʻohui i kahi nui o 80% ethanol i hoʻomoʻa mua ʻia i 60 ℃ ~ 65 ℃, a mālama i ka hoʻoulu ʻana i ka mechanical ma 60 ℃ ~ 65 ℃ ma kahi wela wela mau. no ka 10 ℃. min. E lawe i ka supernatant e maloʻo
I loko o ka ipu wai maʻemaʻe, e hoʻohana i ka nitrate kālā e nānā i nā ion chloride. Inā loaʻa kahi ʻeke keʻokeʻo, kānana iā ia ma kahi kānana aniani a lawe i ka paʻa
E hana hou i nā ʻanuʻu mua no ka ʻāpana kino, a hiki i ka filtrate ma hope o ka hoʻohui ʻana i 1 kulu o ka solution AgNO3 ʻaʻohe eha keʻokeʻo, ʻo ia hoʻi, pau ka hoʻomaʻemaʻe a me ka holoi ʻana.
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i loko (no ka wehe ʻana i ka hopena o ka huahana NaCl). Ma hope o ka kānana suction, hoʻomaloʻo, hoʻomaloʻo i ka lumi wela a me ke kaupaona ʻana.
nuipaʻa, g.
Nā ʻano hoʻāʻo a me ke ʻano no ka Cellulose Ethers
Ka Hoʻoholo ʻana o ka Degree of Substitution (DS) a me Molar Degree of Substitution (MS)
Ka Hoʻoholo ʻana o DS: ʻO ka mua, e kaupaona i ka 0.2 g (pololei i ka 0.1 mg) o ka laʻana cellulose ether i hoʻomaʻemaʻe ʻia a maloʻo, e hoʻoheheʻe i loko.
80mL o ka wai distilled, hoʻoulu ʻia i loko o kahi ʻauʻau wai wela mau ma 30 ℃ ~ 40 ℃ no 10min. A laila e hoʻoponopono me ka ʻakika sulfuric solution a i ʻole ka hopena NaOH
pH o ka hoʻonā a hiki i ka pH o ka hopena he 8. A laila i loko o ka beaker i hoʻolako ʻia me kahi electrode mika pH, e hoʻohana i kahi hopena maʻamau o ka sulfuric acid.
No ka titrate, ma lalo o ka hoʻoulu ʻana, e nānā i ka heluhelu ʻana i ka mika pH i ka wā e titrating, ke hoʻoponopono ʻia ka waiwai pH o ka hopena i 3.74,
Pau ka titration. E hoʻomaopopo i ka nui o ka sulfuric acid solution maʻamau i hoʻohana ʻia i kēia manawa.
Hanau:
ʻO ka huina o nā helu proton luna a me ka hui hydroxyethyl
ʻO ka lakio o ka helu o nā protons luna; ʻO I7 ka nuipaʻa o ka hui methylene ma ka hui hydroxyethyl
Ka ikaika o ka proton resonance peak; ʻO ia ka ikaika o ka piko o ka resonance proton o 5 mau pūʻulu methine a me hoʻokahi pūʻulu methylene ma ka pūʻulu glucose cellulose.
Sum.
ʻO nā ʻano hoʻāʻo i wehewehe ʻia no ka hoʻāʻo ʻana o ka infrared characterization o nā cellulose ethers ʻekolu CMC, HEC a me HEECMC
Kānāwai
3.2.4.3 XRD hoao
X-ray Diffraction Analysis Characterization Test of Three Cellulose Ethers CMC, HEC a me HEECMC
ke ano hoao i hoakakaia.
3.2.4.4 Hoao ana o H-NMR
Ua ana ʻia ka H NMR spectrometer o HEC e Avance400 H NMR spectrometer i hana ʻia e BRUKER.
Me ka hoʻohana ʻana i ka dimethyl sulfoxide deuterated e like me ka solvent, ua hoʻāʻo ʻia ka hopena e ka wai hydrogen NMR spectroscopy. ʻO 75.5MHz ka alapine hoʻokolohua.
Mehana, ʻo ka hopena he 0.5mL.
3.3 Nā hualoaʻa a me ka nānā ʻana
3.3.1 Optimization o ka CMC kaʻina hoʻomākaukau
Ke hoʻohana nei i ka pine cellulose i unuhi ʻia ma ka mokuna ʻelua e like me ka mea maka, a me ka hoʻohana ʻana i ka sodium chloroacetate ma ke ʻano he etherifying agent, ua lawe ʻia ke ʻano o ka hoʻokolohua hoʻokahi kumu.
Ua hoʻonohonoho pono ʻia ke kaʻina hana hoʻomākaukau o CMC, a ua hoʻonohonoho ʻia nā mea hoʻololi mua o ka hoʻokolohua e like me ka hōʻike ʻana ma ka Papa 3.3. Eia ka papa hana hoʻomākaukau HEC
Ma ke kiʻi, ke kālailai ʻana i nā kumu like ʻole.
Papa 3.3 Kumu Waiwai
Kumu waiwai kumu
ʻO ka mahana alkalizing ka hoʻomaʻamaʻa mua ʻana/℃ 40
Ka manawa alkalizing o ka hoʻomaʻamaʻa mua ʻana/h 1
Ka lākiō paʻa-wai/(g/mL) 1:25
ʻO ka hoʻomaʻamaʻa mua ʻana i ka lye ʻike/% 40
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ʻO ka pae mua etherification wela / ℃ 45
Ka manawa etherification pae mua/h 1
Ka lua o ka etherification wela wela/℃ 70
ʻElua manawa etherification manawa/h 1
ʻO ke ʻano kumu i ka pae etherification/g 2
Ka nui o ka lāʻau etherifying i ka wā etherification/g 4.3
Lakiō paʻa-wai etherified/(g/mL) 1:15
3.3.1.1 Ka hopena o nā mea like ʻole ma ke kēkelē hoʻololi CMC i ka pae hoʻomaʻamaʻa mua.
1. Ka hopena o ka pretreatment alkalization wela ma ke degere pani o CMC
I mea e noʻonoʻo ai i ka hopena o ka pretreatment alkalization wela ma ke degere o ka hoʻololi ʻana i ka CMC i loaʻa, i ka hihia o ka hoʻoponopono ʻana i nā kumu ʻē aʻe e like me nā kumu waiwai mua,
Ma lalo o nā kūlana, kūkākūkā ʻia ka hopena o ka pretreatment alkalization ma luna o ke degere hoʻololi CMC, a hōʻike ʻia nā hopena ma Fig.
Hoʻomaʻamaʻa mua i ka mahana alkalizing/℃
Ka hopena o ka mahana alkalizing pretreatment ma ke degere pani pani CMC
Hiki ke ʻike ʻia ka piʻi ʻana o ke kiʻekiʻe o ka hoʻololi ʻana o CMC me ka piʻi ʻana o ka mahana alkalization pretreatment, a ʻo ka mahana alkalization he 30 °C.
ʻO nā degere o ka hoʻololi i luna e emi iho me ka piʻi ʻana o ka mahana. ʻO kēia ke kumu no ka haʻahaʻa loa o ka mahana alkalizing, a ʻaʻole hiki i nā molekole ke hana
Hoʻopau maikaʻi i ka wahi crystalline o cellulose, kahi mea paʻakikī i ka mea etherifying e komo i loko o ka cellulose i ka pae etherification, a ʻoi aku ka kiʻekiʻe o ka hopena.
haʻahaʻa, e hopena i kahi haʻahaʻa haʻahaʻa o ka hoʻololi huahana. Eia naʻe, ʻaʻole pono ke kiʻekiʻe loa ka mahana alkaliization. Ke piʻi aʻe ka mahana, ma lalo o ka hana o ka wela kiʻekiʻe a me ka alkali ikaika,
Pilikia ka Cellulose i ka degradation oxidative, a ke emi nei ka degere o ka hoʻololi ʻana o ka huahana CMC.
2. Ka hopena o ka manawa alkalinization pretreatment ma ke degere pani CMC
Ma lalo o ke kūlana he 30 °C ka mahana o ka alkalization pretreatment a ʻo nā kumu ʻē aʻe nā kumu waiwai mua, ua kūkākūkā ʻia ka hopena o ka manawa alkalization pretreatment ma CMC.
Ka hopena o ke pani. Degere o ka pani
Ka manawa alkalizing hoʻomaʻamaʻa mua
Ka hopena o ka manawa alkalinization pretreatment maCMCdegere pani
ʻO ke kaʻina hana bulking ponoʻī he wikiwiki, akā pono ka hopena alkali i kahi manawa diffusion i ka fiber.
Hiki ke ʻike ʻia inā he 0.5-1.5h ka manawa alkalization, piʻi ka degere pani o ka huahana me ka piʻi ʻana o ka manawa alkalization.
ʻO ke kiʻekiʻe o ka hoʻololi o ka huahana i loaʻa ke kiʻekiʻe loa i ka manawa he 1.5h ka manawa, a ua emi ke degere o ka hoʻololi ʻana me ka hoʻonui ʻana o ka manawa ma hope o 1.5h. Hiki kēia
Ma muli paha o ka hoʻomaka ʻana o ka alkalization, me ka hoʻolōʻihi ʻana o ka manawa alkaliization, ʻoi aku ka lawa o ka infiltration o ka alkali i cellulose, no laila ka fiber.
ʻOi aku ka ʻoluʻolu o ka hoʻolālā prime, e hoʻonui ana i ka etherifying agent a me ka mea hana
Ka manawa hoʻouna: Apr-26-2024