1 Okwu mmalite
Ugbu a, isi akụrụngwa eji na nkwadebe nkecellulose etherbụ owu, na mmepụta ya na-agbada, ọnụ ahịa na-arị elu;
Ọzọkwa, ihe etherifying ndị a na-ejikarị eme ihe dị ka chloroacetic acid (nke na-egbu egbu) na ethylene oxide (carcinogenic) na-emerụkwa ahụ mmadụ na gburugburu ebe obibi. Akwụkwọ
N'isiakwụkwọ a, a na-eji pine cellulose nwere ihe dị ọcha karịa 90% ewepụtara n'isi nke abụọ dị ka ihe eji eme ihe, a na-ejikwa sodium chloroacetate na 2-chloroethanol dochie ya.
Iji chloroacetic acid na-egbu egbu dị ka onye na-eme ka etherifying, anioniccarboxymethyl cellulose (CMC), A kwadebere cellulose na-abụghị ionic hydroxyethyl.
Cellulose (HEC) na ngwakọta hydroxyethyl carboxymethyl cellulose (HECMC) atọ cellulose ethers. otu ihe
Emebere usoro nkwadebe nke ether cellulose atọ kachasị mma site na nnwale na nnwale orthogonal, na ethers cellulose synthesized bụ nke e ji mara FT-IR, XRD, H-NMR, wdg.
Ihe ndị bụ isi nke etherification cellulose
Enwere ike kewaa ụkpụrụ nke etherification cellulose n'ime akụkụ abụọ. Akụkụ nke mbụ bụ usoro alkalization, ya bụ, n'oge mmeghachi omume alkalization nke cellulose.
Na-agbasasịkwa na ngwọta NaOH, pine cellulose na-aza nke ọma n'okpuru ọrụ nke mkpagharị igwe, yana mgbasawanye nke mmiri.
Ọnụ ọgụgụ dị ukwuu nke obere ụmụ irighiri NaOH batara n'ime ime cellulose pine, wee meghachi omume na otu hydroxyl na mgbanaka nke akụkụ glucose,
Na-emepụta cellulose alkali, etiti na-arụ ọrụ nke mmeghachi omume etherification.
Akụkụ nke abụọ bụ usoro etherification, ya bụ, mmeghachi omume n'etiti etiti na-arụ ọrụ na sodium chloroacetate ma ọ bụ 2-chloroethanol n'okpuru ọnọdụ alkaline, na-akpata ya.
N'otu oge ahụ, onye na-ahụ maka etherifying sodium chloroacetate na 2-chlorethanol ga-emepụtakwa mmiri ụfọdụ n'okpuru ọnọdụ alkaline.
A na-ekpebi mmeghachi omume akụkụ iji mepụta sodium glycolate na ethylene glycol, n'otu n'otu.
2 Mwepụta alkali decrystallisation pretreatment nke pine cellulose
Nke mbụ, dozie ụfọdụ ntinye nke ngwọta NaOH na mmiri deionized. Mgbe ahụ, na okpomọkụ ụfọdụ, 2g nke eriri pine
A na-agbaze vitamin ahụ n'otu olu nke ngwọta NaOH, kpalie ruo oge ụfọdụ, wee kpochaa maka ojiji.
Onye nrụpụta Model akụrụngwa
Igwe pH ziri ezi
Ọchịkọta ụdị mgbe niile okpomọkụ kpo oku magnetik stirrer
Igwe ọkụ na-ehicha ọkụ
Eletrọnịkị itule
Na-ekesa mmiri ụdị multi-nzube agụụ mgbapụta
Fourier Transform Infrared Spectrometer
X-ray diffractometer
Spectrometer magnetik resonance nke nuklia
Ụgwọ nke ụlọ ọrụ Hangzhou Aolilong Instrument Co., Ltd.
Ụgwọ nke ụlọ ọrụ Hangzhou Huichuang Instrument Equipment Co., Ltd.
Ụgwọ nke ụlọ ọrụ Shanghai Jinghong Experimental Equipment Co., Ltd.
METTLER TOLEDO Instruments (Shanghai) Co., Ltd.
Hangzhou David Science and Education Instrument Co., Ltd.
Ụgwọ nke ụlọ ọrụ American Thermo Fisher Co., Ltd.
Ụlọ ọrụ American Thermoelectric Switzerland ARL Company
Ụlọ ọrụ Switzerland BRUER
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Nkwadebe nke CMC
Iji osisi pine alkali cellulose pretreated site na itinye uche alkali decrystallization dị ka akụrụngwa, na-eji ethanol dị ka ihe mgbaze na iji sodium chloroacetate dị ka etherification.
A kwadebere CMC nwere DS dị elu site n'ịgbakwunye alkali ugboro abụọ na onye ọrụ etherifying ugboro abụọ. Tinye 2g nke osisi pine alkali cellulose n'ime flask nwere olu anọ, wee tinye otu olu nke ethanol ihe mgbaze, ma kpalie nke ọma maka 30min.
banyere, nke mere na cellulose alkali na-agbasasị n'ụzọ zuru ezu. Mgbe ahụ, tinye ego ụfọdụ nke onye na-ahụ maka alkali na sodium chloroacetate iji meghachi omume maka oge ụfọdụ n'otu oge okpomọkụ.
Ka oge na-aga, mgbakwunye nke abụọ nke onye na-ahụ maka alkaline na sodium chloroacetate na-esote etherification ruo oge ụfọdụ. Mgbe mmeghachi omume ahụ gwụsịrị, dị jụụ ma daa jụụ, mgbe ahụ
Wepụ ya na oke glacial acetic acid kwesịrị ekwesị, wee mee nzacha mmiri, sachaa ma kpọọ nkụ.
Nkwadebe nke HEC
Iji osisi pine alkali cellulose pretreated na ndọpụ alkali decrystallization dị ka akụrụngwa, ethanol dị ka ihe mgbaze na 2-chloroethanol dị ka etherification.
A kwadebere HEC nwere MS dị elu site n'ịgbakwunye alkali ugboro abụọ na onye ọrụ etherifying ugboro abụọ. Tinye 2g nke osisi pine alkali cellulose n'ime flask nwere olu anọ, tinyekwa otu olu nke 90% (ụda olu) ethanol, kpalie.
Kpoo oge ka ị gbasasịa n'ụzọ zuru ezu, wee gbakwunye obere alkali, ma jiri nwayọọ nwayọọ kpoo ọkụ, tinye otu olu nke 2-
Chloroethanol, na-ekpochapụ na okpomọkụ na-adịgide adịgide ruo oge ụfọdụ, wee gbakwunye sodium hydroxide na 2-chloroethanol fọdụrụnụ ka ọ gaa n'ihu na-etherification ruo oge ụfọdụ. na-emeso
Mgbe emechara mmeghachi omume ahụ, were ntakịrị glacial acetic acid wepụ ya, n'ikpeazụ were nzacha iko (G3), sachaa, kpochaa.
Nkwadebe nke HEMCC
Iji HEC kwadebere na 3.2.3.4 dị ka akụrụngwa, ethanol dị ka mmeghachi omume mmeghachi omume, na sodium chloroacetate dị ka onye na-emepụta ihe iji kwadebe.
HECMC. Usoro a kapịrị ọnụ bụ: were ụfọdụ HEC, tinye ya na 100 ml nke olu olu anọ, wee gbakwunye obere olu.
90% ethanol, na-emegharị ahụ nke ọma ruo oge ụfọdụ iji mee ka ọ gbasaa kpamkpam, tinye obere alkali mgbe kpochara, wee jiri nwayọọ nwayọọ tinye.
Sodium chloroacetate, etherification na okpomọkụ na-adịgide adịgide na-agwụ mgbe oge ụfọdụ gasịrị. Mgbe emechara mmeghachi omume ahụ, wepụ ya na glacial acetic acid iji kpochapụ ya, wee jiri nzacha iko (G3)
Mgbe nzacha mmiri ara, ịsacha na ihicha.
Ịdị ọcha nke cellulose ethers
N'ime usoro nkwadebe nke cellulose ether, a na-emepụtakarị ụfọdụ ngwaahịa, karịsịa nnu inorganic sodium chloride na ụfọdụ ndị ọzọ.
adịghị ọcha. Iji mee ka mma cellulose ether dịkwuo mma, a na-eme ka ọ dị ọcha dị mfe na ether cellulose nwetara. n'ihi na ha nọ na mmiri
Enwere solubility dị iche iche, ya mere nnwale ahụ na-eji akụkụ ụfọdụ nke ethanol hydrated mee ka ether cellulose atọ a kwadebere dị ọcha.
gbanwee.
Debe ihe nlele cellulose ether nke a kwadebere nke ọma na beaker, gbakwunye ụfọdụ 80% ethanol nke etinyere ya na 60 ℃ ~ 65 ℃, ma nọgide na-emegharị igwe na 60 ℃ ~ 65 ℃ na okpomọkụ na-ekpo ọkụ mgbe niile. maka 10 ℃. min. Were supernatant kpoo nkụ
Na beaker dị ọcha, jiri nitrate ọlaọcha chọpụta ion chloride. Ọ bụrụ na enwere mkpọda ọcha, kpochaa ya site na nzacha iko wee buru ihe siri ike
Tinyegharịa usoro ndị gara aga maka akụkụ ahụ ahụ, ruo mgbe nzacha ahụ gbakwunyere 1 dobe nke ngwọta AgNO3 enweghị ntụpọ ọcha, ya bụ, a na-emecha ọcha na ịsacha.
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n'ime (tumadi iji wepu mmeghachi omume sitere na ngwaahịa NaCl). Mgbe imi filtration, ihicha, jụrụ ka ụlọ okpomọkụ na-atụ.
okwu, g.
Uzo nnwale na njirimara maka cellulose ethers
Mkpebi nke ogo nnọchi anya (DS) na Molar Degree of nnọchi (MS)
Mkpebi nke DS: Nke mbụ, tụọ 0.2 g (nke ziri ezi na 0.1 mg) nke ihe nlele ether cellulose dị ọcha na nke a mịrị amị, gbarie ya.
80ml nke distilled mmiri, kpaliri na a mgbe nile okpomọkụ mmiri saa na 30 ℃ ~ 40 ℃ 10min. Wee dozie ya na ngwọta sulfuric acid ma ọ bụ ngwọta NaOH
pH nke ngwọta ruo mgbe pH nke ngwọta bụ 8. Mgbe ahụ na beaker nke nwere pH mita electrode, jiri ngwọta ọkọlọtọ nke sulfuric acid.
Iji titrate, n'okpuru ọnọdụ mkpali, lelee pH mita ọgụgụ mgbe titrating, mgbe pH uru nke ngwọta na-gbanwere na 3.74,
Titration agwụ. Rịba ama olu ọkọlọtọ ọkọlọtọ sulfuric acid ejiri n'oge a.
Ọgbọ:
Nchikota nke ọnụọgụ proton nke elu na otu hydroxyethyl
Ọnụ ọgụgụ nke protons dị elu; I7 bụ oke nke otu methylene na otu hydroxyethyl
Ike nke proton resonance kacha elu; bụ ike nke proton resonance ọnụ ọgụgụ nke 5 methine otu na otu methylene otu na cellulose glucose unit.
Nchikota.
Ụzọ ule akọwara maka nyocha njirimara infrared nke cellulose ethers CMC, HEC na HEECMC.
Iwu
3.2.4.3 XRD ule
Nnwale njirimara njirimara X-ray Diffraction nke Cellulose Ethers CMC, HEC na HEECMC
usoro ule a kọwara.
3.2.4.4 Nnwale nke H-NMR
A tụrụ spectrometer H NMR nke HEC site na Avance400 H NMR spectrometer nke BRUKER mepụtara.
N'iji deuterated dimethyl sulfoxide dị ka ihe mgbaze, a nwalere ngwọta ya site na mmiri mmiri hydrogen NMR spectroscopy. Ugboro ule bụ 75.5MHz.
Na-ekpo ọkụ, ihe ngwọta bụ 0.5 ml.
3.3 Nsonaazụ na nyocha
3.3.1 Kachasị mma nke usoro nkwadebe CMC
N'iji cellulose pine nke ewepụtara na isi nke abụọ dị ka akụrụngwa, na iji sodium chloroacetate dị ka onye na-emepụta ihe, a nakweere usoro nnwale nke otu ihe.
A kwadoro usoro nkwadebe nke CMC, na mgbanwe ndị mbụ nke nnwale ahụ ka edobere dị ka egosiri na Tebụl 3.3. Ihe na-esonụ bụ usoro nkwadebe HEC
Na nkà, nyocha nke ihe dị iche iche.
Tebụl 3.3 Ụkpụrụ Mmasị Mbụ
Ihe kpatara uru mbido
Pretreatment alkalizing okpomọkụ/℃ 40
Oge ntụ ntụ ntụ ntụ 1
Pretreatment siri ike-mmiri ruru/(g/mL) 1:25
Mgbochi lye itinye uche/% 40
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Nke mbụ ogbo etherification okpomọkụ/℃ 45
Oge etherification nke ọkwa mbụ/h 1
Nkeji nke abụọ etherification okpomọkụ/℃ 70
Oge etherification ogbo nke abụọ/h 1
Usoro usoro onunu ogwu na ogbo etherification/g 2
Ọnụ ego nke ihe na-eme ka etherification na ọkwa etherification/g 4.3
Oke mmiri mmiri siri ike nke etherified/(g/ml) 1:15
3.3.1.1 Mmetụta nke ihe dị iche iche na CMC nnọchi ogo na pretreatment alkalization ogbo.
1. Mmetụta nke pretreatment alkalization okpomọkụ na nnọchi ogo nke CMC
Iji tụlee mmetụta nke pretreatment alkalization okpomọkụ na ogo nke nnọchi na CMC nwetara, n'ihe banyere idozi ihe ndị ọzọ dị ka mbụ ụkpụrụ.
N'okpuru ọnọdụ ahụ, a na-atụle mmetụta nke pretreatment alkalization okpomọkụ na CMC nnọchi ogo, na-arụpụta na-egosi na fig.
Pretreatment alkalizing okpomọkụ/℃
Mmetụta pretreatment alkalizing okpomọkụ na CMC nnọchi ogo
Enwere ike ịhụ na ogo nke nnọchi nke CMC na-abawanye na mmụba nke pretreatment alkalization okpomọkụ, na alkalization okpomọkụ bụ 30 Celsius C.
Ogo ngbanwe dị n'elu na-ebelata na okpomọkụ na-abawanye. Nke a bụ n'ihi na okpomọkụ alkalizing dị oke ala, na ụmụ irighiri ihe ndị ahụ adịchaghị arụ ọrụ na enweghị ike
Mebie kristal kristal nke cellulose nke ọma, nke na-eme ka o sie ike maka onye na-ahụ maka etherifying ịbanye n'ime cellulose na ọkwa etherification, na ogo mmeghachi omume dị elu.
dị ala, na-ebute obere ngbanwe nke ngwaahịa. Otú ọ dị, okpomọkụ alkalization ekwesịghị ịdị elu. Ka okpomọkụ na-abawanye, n'okpuru ọrụ nke okpomọkụ dị elu na alkali siri ike,
Cellulose na-adịkarị mfe imebi oxidative, na ogo ngbanwe nke ngwaahịa CMC na-ebelata.
2. Mmetụta nke pretreatment alkalinization oge na CMC nnọchi ogo
N'okpuru ọnọdụ na pretreatment alkalization okpomọkụ bụ 30 Celsius C na ihe ndị ọzọ bụ ụkpụrụ mbụ, mmetụta nke pretreatment alkalization oge na CMC na-atụle.
Mmetụta nke nnọchi. Ogo nke nnọchi
Mgbochi ọgwụgwọ alkalizing oge/h
Mmetụta nke pretreatment alkalinization oge naCMCnnochi anya ogo
Usoro bulking n'onwe ya dị ngwa ngwa, mana ngwọta alkali chọrọ oge mgbasa ozi na eriri.
Enwere ike ịhụ na mgbe oge alkalization bụ 0.5-1.5h, ogo ngbanwe nke ngwaahịa na-abawanye na oge alkalisation na-abawanye.
Ogo nke ngbanwe nke ngwaahịa a nwetara bụ nke kachasị elu mgbe oge ahụ bụ 1.5h, na ogo ngbanwe na-ebelata na mmụba nke oge mgbe 1.5h gasịrị. Nke a nwere ike
O nwere ike ịbụ n'ihi na na mmalite nke alkalization, na ogologo oge nke alkalization, ntinye nke alkali na cellulose zuru oke, nke mere na eriri ahụ.
Ihe owuwu kachasị dị jụụ karị, na-amụba onye na-ahụ maka etherifying na onye na-arụ ọrụ
Oge nzipu: Eprel-26-2024