1 Okwu Mmalite
Ugbu a, ihe eji eme ihe bụ isi eji eme nkwadebe nkecellulose etherbụ owu, mmepụta ya na-ebelatakwa, ọnụ ahịa ya na-arịkwa elu;
Ọzọkwa, ihe ndị a na-ejikarị eme ka ihe dị ka chloroacetic acid (nke na-egbu egbu nke ukwuu) na ethylene oxide (nke na-akpata ọrịa kansa) na-emerụkwa ahụ mmadụ na gburugburu ebe obibi ahụ nke ọma.
N'isiakwụkwọ a, a na-eji pine cellulose nke nwere ịdị ọcha karịa 90% nke ewepụtara n'isiakwụkwọ nke abụọ dị ka ihe e ji arụ ọrụ, a na-ejikwa sodium chloroacetate na 2-chloroethanol dị ka ihe nnọchi anya.
Iji chloroacetic acid dị oke egbu egbu dị ka ihe na-eme ka ikuku dị ọcha, anioniccellulose carboxymethyl (CMC), e mepụtara cellulose na-abụghị ionic hydroxyethyl.
Cellulose (HEC) na hydroxyethyl carboxymethyl cellulose (HECMC) ngwakọta nke cellulose ether atọ.
E jiri nnwale na nnwale orthogonal mee ka usoro nkwadebe nke cellulose ether atọ ka mma, e jikwa FT-IR, XRD, H-NMR, wdg mara cellulose ethers ndị a haziri ahazi.
Isi ihe dị mkpa maka etherification nke cellulose
Enwere ike kewaa ụkpụrụ nke cellulose etherification ụzọ abụọ. Akụkụ mbụ bụ usoro alkalization, ya bụ, n'oge mmeghachi omume alkalization nke cellulose,
N'ịbụ nke a gbasasịrị n'otu n'otu na mmiri NaOH, pine cellulose na-aza nke ọma n'okpuru mkpali igwe, yana mmụba nke mmiri.
Nnukwu obere molekul NaOH banyere n'ime pine cellulose, wee meghachi omume na otu hydroxyl dị na mgbanaka nke ngalaba nhazi glucose,
Na-emepụta alkali cellulose, ebe etiti ọrụ nke mmeghachi omume etherification.
Akụkụ nke abụọ bụ usoro etherification, ya bụ, mmeghachi omume dị n'etiti etiti na-arụ ọrụ na sodium chloroacetate ma ọ bụ 2-chloroethanol n'okpuru ọnọdụ alkaline, na-ebute
N'otu oge ahụ, ihe na-emepụta ihe na-eme ka mmiri dị n'ime ya dị ka sodium chloroacetate na 2-chloroethanol ga-emepụtakwa mmiri ụfọdụ n'okpuru ọnọdụ alkaline.
A na-edozi mmeghachi omume ndị dị n'akụkụ iji mepụta sodium glycolate na ethylene glycol, n'otu n'otu.
2 Ọgwụgwọ tupu ọgwụgwọ pine cellulose nke alkali a na-etinye n'ime ihe
Mbụ, kwadebe otu njupụta nke mmiri NaOH na mmiri e tinyere ion. Mgbe ahụ, n'ọnọdụ okpomọkụ ụfọdụ, 2g nke eriri pain
A na-agbaze vitamin ahụ n'ime obere ihe ngwọta NaOH, na-akpali ya ruo oge ụfọdụ, wee tee ya ka o wee jiri ya.
Onye Mmepụta Ihe Nlereanya Ngwa Ngwa
Mita pH nke ziri ezi
Ụdị nchịkọta okpomọkụ na-agbanwe agbanwe na-ekpo ọkụ magnetik stirrer
Oven nkụ igwe nchacha ikuku
Nhazi eletrọniki
Mmiri na-agbagharị agbagharị ụdị mmiri dị iche iche
Igwe nlele infrared Fourier Transform
Ihe nlele X-ray diffractometer
Igwe ihe nlele resonance magnetik nuklia
Hangzhou Aolilong Instrument Co., Ltd.
Ụlọ ọrụ ngwa ngwa nke Hangzhou Huichuang, Ltd.
Ụlọ ọrụ akụrụngwa nnwale nke Shanghai Jinghong, Ltd.
Ụlọ ọrụ METTLER TOLEDO Instruments (Shanghai) Co., Ltd.
Ụlọ ọrụ Sayensị na Mmụta nke Hangzhou David., Ltd.
Ụlọ ọrụ American Thermo Fisher Co., Ltd.
Ụlọ ọrụ ARL nke America Thermoelectric Switzerland
Ụlọ ọrụ Switzerland bụ BRUKER
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Nkwadebe nke CMCs
Iji mkpụrụ osisi pine alkali cellulose agwọ ọrịa site na iji alkali decrystallization dị ka ihe eji arụ ọrụ, jiri ethanol mee ihe dị ka ihe mgbaze ma jiri sodium chloroacetate mee ihe dị ka etherification.
A kwadebere CMC nwere DS dị elu site na itinye alkali ugboro abụọ na ihe na-eme ka ihe dị ọkụ ugboro abụọ. Tinye 2g nke pine wood alkali cellulose n'ime karama olu anọ, wee tinye obere olu nke ihe mgbaze ethanol, wee gwakọta nke ọma ruo nkeji iri atọ.
gbasara, ka alkali cellulose wee gbasaa kpamkpam. Mgbe ahụ tinye obere ihe nnọchite anya alkali na sodium chloroacetate iji meghachi omume ruo oge ụfọdụ na okpomọkụ etherification ụfọdụ.
Mgbe oge ụfọdụ gasịrị, a na-agbakwunye ihe na-eme ka alkaline na sodium chloroacetate nke abụọ wee tinye ya na etherification ruo oge ụfọdụ. Mgbe mmeghachi omume ahụ gasịrị, jụọ oyi ma jụọ oyi, wee tinye ya na mmiri.
Jiri glacial acetic acid kwesịrị ekwesị mee ka ọ dị n'otu, wee jiri nzacha mmiri mee ya, saa ya ma kpọọ ya nkụ.
Nkwadebe nke HECs
Iji osisi pine alkali cellulose eme ihe tupu oge eruo, a na-eji alkali decrystallization eme ihe dị ka ihe e ji arụ ọrụ, ethanol dị ka ihe mgbaze na 2-chloroethanol dị ka etherification.
A kwadebere HEC nwere MS dị elu site na itinye alkali ugboro abụọ na ihe na-eme ka ihe dị ọkụ ugboro abụọ. Tinye 2g nke pine wood alkali cellulose n'ime karama olu anọ, ma tinye obere olu nke 90% (nkezi olu) ethanol, gwakọta ya.
Gwakọta ruo oge ụfọdụ ka o gbasaa nke ọma, wee tinye ụfọdụ alkali, wee jiri nwayọ kpoo ọkụ, tinye obere olu nke 2-
Chloroethanol, nke a na-eme ka ọ dị ọkụ mgbe niile ruo oge ụfọdụ, wee tinye sodium hydroxide na 2-chloroethanol fọdụrụnụ iji nọgide na-eme ka ọ dị ọkụ ruo oge ụfọdụ.
Mgbe mmeghachi omume ahụ mechara, jiri obere glacial acetic acid mee ka ọ dị nro, wee mechaa jiri ihe nzacha iko (G3) hichaa ya, saa ya, ma kpọọ nkụ.
Nkwadebe nke HEMCC
Iji HEC nke e kwadebere na 3.2.3.4 dị ka ihe eji arụ ọrụ, ethanol dị ka ihe na-eme ka mmeghachi omume dị, na sodium chloroacetate dị ka ihe na-eme ka etherifying dị njikere.
HECMC. Usoro a kapịrị ọnụ bụ: were obere HEC, tinye ya n'ime karama olu anọ nke 100 mL, wee tinye obere olu nke
90% ethanol, a na-agwakọta ya n'ime igwe ruo oge ụfọdụ ka ọ gbasaa kpamkpam, tinye obere alkali mgbe ọ kpochara ọkụ, wee jiri nwayọ tinye ya.
Sodium chloroacetate, etherification na okpomọkụ na-adịgide adịgide na-akwụsị mgbe oge ụfọdụ gasịrị. Mgbe emechara mmeghachi omume ahụ, wepụ ya na glacial acetic acid iji mee ka ọ ghara ịdị irè, wee jiri ihe nzacha iko (G3)
Mgbe a sachara mmiri, saa ya ma kpọọ ya nkụ.
Ịsachapụ nke cellulose ethers
N'ime usoro nkwadebe nke cellulose ether, a na-emepụta ụfọdụ ihe ndị ọzọ, ọkachasị nnu inorganic sodium chloride na ụfọdụ ihe ndị ọzọ.
ihe ndị na-adịghị ọcha. Iji mee ka mma nke cellulose ether dịkwuo mma, e mere nhicha dị mfe na cellulose ether e nwetara. N'ihi na ha dị na mmiri.
E nwere ike ịgbaze dị iche iche, yabụ nnwale ahụ na-eji obere olu nke ethanol mmiri mmiri mee ka ether cellulose atọ a kwadebere dị ọcha.
mgbanwe.
Debe ihe nlele cellulose ether nke e ji ihe dị iche mee n'ime beaker, tinye obere ego nke ethanol 80% nke e tinyere ọkụ ruo 60 ℃ ~ 65 ℃, ma nọgide na-akpali ya na igwe na okpomọkụ 60 ℃ ~ 65 ℃ na ihe na-akpali ya na magnetik nke na-ekpo ọkụ ruo mgbe ọ dị ihe dị ka nkeji 10. Mee ka ihe na-ekpo ọkụ kpọọ nkụ.
N'ime ite dị ọcha, jiri silver nitrate lelee ion chloride. Ọ bụrụ na e nwere ihe na-eme ka ọ dị ọcha, hichaa ya site na nzacha iko wee were ihe siri ike ahụ.
Megharịa usoro ndị gara aga maka akụkụ ahụ, ruo mgbe nzacha ahụ mgbe etinyere otu ntapụ nke ngwọta AgNO3 enweghị ihe na-akpalite ọcha, ya bụ, nhicha na ịsacha ahụ agwụchaala.
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n'ime (karịsịa iji wepụ mmeghachi omume NaCl site na ngwaahịa ahụ). Mgbe a mịrị amịchara ya, kpọọ nkụ, jụọ ya ka ọ dị jụụ ruo okpomọkụ ụlọ ma tụọ ya.
oke, g.
Usoro Ule na Nkọwapụta maka Cellulose Ethers
Mkpebi nke ogo nnọchi (DS) na ogo nnọchi (MS)
Mkpebi nke DS: Nke mbụ, tụọ 0.2 g (nke ziri ezi ruo 0.1 mg) nke ihe nlele ether cellulose dị ọcha ma kpọọ nkụ, gbazee ya na
80mL nke mmiri a gwakọtara agwakọta, gwakọta ya na mmiri ịsa ahụ mgbe niile na okpomọkụ 30℃ ~ 40℃ maka nkeji 10. Mgbe ahụ, jiri mmiri sulfuric acid ma ọ bụ mmiri NaOH dozie ya.
pH nke ngwọta ahụ ruo mgbe pH nke ngwọta ahụ dị 8. Mgbe ahụ, n'ime beaker nke nwere electrode mita pH, jiri ngwọta ọkọlọtọ nke sulfuric acid.
Iji titration, n'ọnọdụ na-akpali akpali, lelee ọgụgụ pH mita mgbe ị na- titration, mgbe agbanwere uru pH nke ngwọta ahụ ka ọ bụrụ 3.74,
Ntụnye ahụ kwụsịrị. Rịba ama olu nke ihe ngwọta ọkọlọtọ sulfuric acid ejiri mee ihe n'oge a.
Ọgbọ:
Ngụkọta nke nọmba proton dị elu na otu hydroxyethyl
Oke nke ọnụọgụ proton dị n'elu; I7 bụ oke nke otu methylene dị na otu hydroxyethyl
Oke ike nke proton resonance; bụ ike nke oke proton resonance nke otu methine ise na otu methylene na nkeji glucose cellulose
Nchịkọta.
Usoro nnwale akọwara maka nnwale njirimara infrared nke cellulose ethers atọ CMC, HEC na HEECMC
Iwu
3.2.4.3 Nnwale XRD
Nnyocha Nkọwa nke X-ray Diffraction Ule njirimara nke Cellulose Ethers atọ CMC, HEC na HEECMC
usoro nnwale akọwara.
3.2.4.4 Nnwale nke H-NMR
E jiri Avance400 H NMR spectrometer nke BRUKER mepụtara tụọ spectrometer H NMR nke HEC.
Site na iji deuterated dimethyl sulfoxide dị ka ihe mgbaze, a nwalere ngwọta ahụ site na iji mmiri hydrogen NMR spectroscopy. Ugboro ule ahụ bụ 75.5MHz.
Ọkụ, ihe ngwọta ahụ bụ 0.5 ml.
3.3 Nsonaazụ na Nyocha
3.3.1 Nhazi nke usoro nkwadebe CMC
Site n'iji pine cellulose ewepụtara n'isi nke abụọ dị ka ihe e ji arụ ọrụ, ma jiri sodium chloroacetate dị ka ihe na-eme ka etherifying mee ihe, a nabatara usoro nnwale otu ihe,
E mere ka usoro nkwadebe nke CMC ka mma, e dokwara mgbanwe mbụ nke nnwale ahụ dịka egosiri na Tebụl 3.3. Ihe ndị a bụ usoro nkwadebe HEC.
N'ihe osise, nyocha nke ihe dị iche iche.
Tebụl 3.3 Ụkpụrụ Ihe Mmalite
Ihe Mgbakwunye Uru mbụ
Okpomọkụ alkali tupu ọgwụgwọ / ℃ 40
Oge nhazi alkali tupu ọgwụgwọ/h 1
Oke mmiri siri ike na mmiri tupu ọgwụgwọ/(g/mL) 1:25
Ọnụọgụ lye tupu a gwọọ ya/% 40
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Ogbo mbụ okpomọkụ etherification / ℃ 45
Oge nhazi nke ọkwa mbụ/h 1
Okpomọkụ etherification nke ogbo nke abụọ/℃ 70
Oge nhazi nke abụọ/h 1
Ọnụọgụ isi dị na ogbo etherification/g 2
Ọnụọgụ ihe na-eme ka etherifying dị n'ọkwa etherification/g 4.3
Oke mmiri siri ike/(g/mL) 1:15
3.3.1.1 Mmetụta nke ihe dị iche iche na ogo nnọchi CMC na ọkwa alkali tupu ọgwụgwọ
1. Mmetụta nke okpomọkụ alkalization tupu ọgwụgwọ na ọkwa nnọchi nke CMC
Iji tụlee mmetụta nke okpomọkụ alkalization tupu ọgwụgwọ na ogo nnọchi na CMC enwetara, ma ọ bụrụ na edozi ihe ndị ọzọ dị ka ụkpụrụ mbụ,
N'okpuru ọnọdụ ndị a, a na-atụle mmetụta nke okpomọkụ alkalization tupu ọgwụgwọ na ọkwa nnọchi CMC, a na-egosikwa nsonaazụ ya na Fig.
Okpomọkụ alkali tupu ọgwụgwọ / ℃
Mmetụta nke okpomọkụ alkali tupu ọgwụgwọ na ogo nnọchi CMC
A pụrụ ịhụ na ọkwa nke nnọchi nke CMC na-abawanye ka okpomọkụ nke alkalization tupu ọgwụgwọ na-abawanye, okpomọkụ alkalization na-erukwa 30 Celsius.
Ogo nnọchi anya dị n'elu na-ebelata ka okpomọkụ na-arị elu. Nke a bụ n'ihi na okpomọkụ nke alkali dị oke ala, molekul anaghịkwa arụ ọrụ nke ọma ma enweghị ike ime ya
Bibie akụkụ kristal nke cellulose nke ọma, nke na-eme ka o siere onye na-emepụta ihe ike ịbanye n'ime cellulose n'oge etherification, ogo mmeghachi omume dịkwa elu.
dị ala, nke na-eme ka obere ọkwa nke nnọchi ngwaahịa dị ala. Agbanyeghị, okpomọkụ nke alkali ekwesịghị ịdị oke elu. Ka okpomọkụ na-abawanye, n'okpuru ọrụ nke oke okpomọkụ na alkali siri ike,
Cellulose na-enwe ike imebi oxidative, ọkwa nke nnọchi nke ngwaahịa CMC na-ebelatakwa.
2. Mmetụta nke oge alkalining tupu ọgwụgwọ na ogo nnọchi CMC
N'ọnọdụ na okpomọkụ nke alkalization tupu ọgwụgwọ bụ 30 Celsius na ihe ndị ọzọ bụ ụkpụrụ mbụ, a na-atụle mmetụta nke oge alkalization tupu ọgwụgwọ na CMC.
Mmetụta nke nnọchi. Ogo nke nnọchi
Oge nhazi alkali tupu ọgwụgwọ/h
Mmetụta nke oge alkaliination tupu ọgwụgwọ naCMCogo nnọchi
Usoro ibuli ihe n'onwe ya na-adị ngwa ngwa, mana ngwọta alkali chọrọ oge mgbasa ozi ụfọdụ na eriri ahụ.
A pụrụ ịhụ na mgbe oge alkalizi bụ awa 0.5-1.5, ọkwa nnọchi nke ngwaahịa ahụ na-abawanye ka oge alkalizizi na-abawanye.
Ogo nnọchi nke ngwaahịa e nwetara bụ nke kachasị elu mgbe oge ahụ bụ awa 1.5, ogo nnọchi ahụ belatakwara ka oge na-aga mgbe awa 1.5 gachara. Nke a nwere ike ime ka nke a ghara ịdị irè.
O nwere ike ịbụ n'ihi na na mmalite nke alkali, ka oge alkali na-agbatị, ntinye nke alkali na cellulose zuru oke, nke mere na eriri ahụ
Ọdịdị praịm ahụ na-eme ka ahụ dị jụụ karị, na-eme ka ihe na-eme ka etherifying na ihe na-arụ ọrụ dịkwuo elu
Oge ozi: Eprel-26-2024