1 Gabatarwa
A halin yanzu, babban kayan da ake amfani da shi wajen shiryawacellulose etherauduga ce, kuma fitar da ita tana raguwa, kuma farashin ma yana ƙaruwa;
Bugu da ƙari, sinadaran etherifying da ake amfani da su akai-akai kamar chloroacetic acid (mai guba sosai) da ethylene oxide (mai cutar kansa) suma suna da illa ga jikin ɗan adam da muhalli.
A cikin wannan babi, ana amfani da sinadarin pine cellulose mai tsaftar fiye da kashi 90% da aka cire a babi na biyu a matsayin kayan aiki, kuma ana amfani da sodium chloroacetate da 2-chloroethanol a matsayin madadinsu.
Amfani da sinadarin chloroacetic acid mai guba sosai a matsayin maganin etherifying, anioniccellulose carboxymethyl (CMC), an shirya cellulose na non-ionic hydroxyethyl.
Cellulose (HEC) da gaurayen hydroxyethyl carboxymethyl cellulose (HECMC) ƙwayoyin cellulose guda uku.
An inganta dabarun shirya ethers cellulose guda uku ta hanyar gwaje-gwaje da gwaje-gwajen orthogonal, kuma an siffanta ethers na cellulose da aka haɗa ta hanyar FT-IR, XRD, H-NMR, da sauransu.
Tushen Tasirin Cellulose
Za a iya raba ƙa'idar etherification ta cellulose zuwa sassa biyu. Kashi na farko shine tsarin alkalization, wato, yayin amsawar alkalization na cellulose,
An warwatse a cikin ruwan NaOH daidai gwargwado, pine cellulose yana kumbura sosai a ƙarƙashin aikin motsa jiki na injiniya, da kuma faɗaɗa ruwa.
Yawan ƙananan ƙwayoyin NaOH sun shiga cikin cikin pine cellulose, kuma sun yi aiki da ƙungiyoyin hydroxyl akan zoben sashin tsarin glucose,
Yana samar da sinadarin alkali cellulose, cibiyar aiki ta hanyar amsawar etherification.
Kashi na biyu shine tsarin etherification, wato, amsawar da ke tsakanin cibiyar aiki da sodium chloroacetate ko 2-chloroethanol a ƙarƙashin yanayin alkaline, wanda ke haifar da
A lokaci guda, sinadarin sodium chloroacetate da 2-chloroethanol suma za su samar da wani matakin ruwa a ƙarƙashin yanayin alkaline.
Ana warware halayen da ke haifar da hakan don samar da sodium glycolate da ethylene glycol, bi da bi.
2 Maganin cire sinadarin alkali mai ƙarfi kafin a fara amfani da shi na pine cellulose
Da farko, a shirya wani adadin ruwan NaOH da aka narkar da shi. Sannan, a wani zafin jiki, 2g na zare na pine
Ana narkar da sinadarin bitamin a cikin wani adadin ruwan NaOH, a juya na tsawon lokaci, sannan a tace shi don amfani.
Mai ƙera Samfurin Kayan Aiki
Daidaiton Ma'aunin pH
Nau'in mai tarawa mai ɗumama zafin jiki mai ɗumama maganadisu
Murhun busar da injin injin
Ma'aunin lantarki
Na'urar famfo mai amfani da ruwa mai amfani da yawa
Na'urar auna hasken infrared ta Fourier Transform
Na'urar auna hasken X-ray diffractometer
Na'urar auna siginar maganadisu ta nukiliya (Nuclear Magnetic Resonance Spectrometer)
Kamfanin Aolilong Instrument Co., Ltd.
Kamfanin Kayan Aikin Hangzhou Huichuang, Ltd.
Kamfanin Kayan Gwaji na Shanghai Jinghong, Ltd.
Kamfanin METTLER TOLEDO Instruments (Shanghai) Co., Ltd.
Kamfanin Kayan Aikin Kimiyya da Ilimi na Hangzhou David, Ltd.
Kamfanin Thermo Fisher na Amurka, Ltd.
Kamfanin ARL na Amurka Thermoelectric Switzerland
Kamfanin BRUKER na Switzerland
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Shiri na CMCs
Amfani da cellulose na itacen Pine alkali wanda aka riga aka yi masa magani ta hanyar rage yawan alkali a matsayin kayan aiki, amfani da ethanol a matsayin mai narkewa da kuma amfani da sodium chloroacetate a matsayin etherification
An shirya CMC mai DS mafi girma ta hanyar ƙara alkali sau biyu da kuma maganin etherifying sau biyu. Sai a zuba 2g na pine wood alkali cellulose a cikin kwalbar mai wuya huɗu, sannan a zuba wani adadin ethanol mai narkewa, sannan a gauraya sosai na tsawon minti 30.
game da, don haka cellulose na alkali ya warwatse gaba ɗaya. Sannan ƙara wani adadin maganin alkali da sodium chloroacetate don amsawa na ɗan lokaci a wani zafin jiki na etherification.
Bayan lokaci, sai a sake ƙara sinadarin alkaline da sodium chloroacetate a karo na biyu, sannan a sake fitar da sinadarin etherification na wani lokaci. Bayan an gama shan maganin, sai a huce sannan a huce, sannan a sake zuba sinadarin a cikin ruwan.
Sai a tace shi da sinadarin glacial acetic acid, sannan a tace, a wanke sannan a busar da shi.
Shiri na HECs
Amfani da maganin alkali na itacen Pine da aka riga aka yi wa magani da shi tare da rage yawan alkali a matsayin kayan aiki, ethanol a matsayin mai narkewa da kuma 2-chloroethanol a matsayin etherification.
An shirya HEC mai babban MS ta hanyar ƙara alkali sau biyu da kuma maganin etherifying sau biyu. Sai a zuba 2g na pine wood alkali cellulose a cikin kwalba mai wuya huɗu, sannan a ƙara wani adadin ethanol na 90% (ƙaramar girma) a gauraya.
Sai a gauraya na ɗan lokaci domin ya warwatse gaba ɗaya, sannan a ƙara wani adadin alkali, sannan a hankali a yi zafi, a ƙara wani adadin na 2-
Chloroethanol, an tace shi a yanayin zafi mai ɗorewa na tsawon lokaci, sannan aka ƙara sauran sodium hydroxide da 2-chloroethanol don ci gaba da etherification na tsawon lokaci.
Bayan an gama aikin, a tace da wani adadin glacial acetic acid, sannan a ƙarshe a tace da gilashin tacewa (G3), a wanke, sannan a busar da shi.
Shiri na HEMCC
Amfani da HEC da aka shirya a cikin 3.2.3.4 a matsayin kayan aiki, ethanol a matsayin hanyar amsawa, da sodium chloroacetate a matsayin wakilin etherifying don shiryawa
HECMC. Tsarin da aka tsara shi ne: a ɗauki wani adadin HEC, a saka shi a cikin kwalba mai wuya huɗu mai nauyin 100 mL, sannan a ƙara wani adadin adadin
ethanol kashi 90%, a juya shi ta hanyar injina na tsawon lokaci don ya wargaje gaba ɗaya, a ƙara wani adadin alkali bayan an dumama shi, sannan a hankali a zuba a ciki.
Sodium chloroacetate, etherification a yanayin zafi mai ɗorewa yana ƙarewa bayan wani lokaci. Bayan an kammala amsawar, a rage shi da glacial acetic acid don rage shi, sannan a yi amfani da matatar gilashi (G3)
Bayan tacewa, wankewa da busarwa.
Tsarkakewar ƙwayoyin cellulose
A cikin tsarin shirya cellulose ether, ana samar da wasu samfuran da suka lalace, galibi gishirin da ba shi da sinadarai, sodium chloride da sauran su.
ƙazanta. Domin inganta ingancin cellulose ether, an yi tsaftacewa mai sauƙi akan cellulose ether da aka samu. Domin suna cikin ruwa
Akwai nau'ikan narkewa daban-daban, don haka gwajin yana amfani da wani ƙaramin juzu'i na ethanol mai ruwa don tsarkake ƙwayoyin cellulose guda uku da aka shirya.
canji.
Sanya samfurin cellulose ether da aka shirya da wani inganci a cikin kwalba, ƙara wani adadin ethanol 80% wanda aka riga aka kunna shi zuwa 60 ℃ ~ 65 ℃, sannan a ci gaba da juyawar injin a 60 ℃ ~ 65 ℃ a kan na'urar motsa jiki mai dumama zafin jiki na tsawon minti 10. A kai ruwan da ke cikin kwalbar ya bushe.
A cikin kwalba mai tsabta, yi amfani da silver nitrate don duba ions na chloride. Idan akwai farin ruwa, a tace shi ta hanyar matatar gilashi sannan a ɗauki daskararrun.
Maimaita matakan da suka gabata ga sashin jiki, har sai tacewa bayan ƙara digo 1 na maganin AgNO3 ba shi da wani farin ruwa, wato, tsarkakewa da wankewa sun kammala.
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a cikin (galibi don cire NaCl ɗin da ke ɗauke da martanin). Bayan tacewa, busarwa, sanyaya zuwa zafin ɗaki da kuma aunawa.
taro, g.
Gwaji da Hanyoyin Haɓaka Cellulose Ethers
Tabbatar da Digirin Sauyawa (DS) da Digirin Sauyawa (MS)
Ƙayyade DS: Da farko, auna 0.2 g (daidai zuwa 0.1 mg) na samfurin ether na cellulose da aka tsarkake da busasshe, sannan a narkar da shi a cikin
80mL na ruwan da aka tace, a juya a cikin ruwan wanka mai zafi akai-akai a zafin 30℃ ~ 40℃ na tsawon minti 10. Sannan a daidaita da maganin sulfuric acid ko maganin NaOH.
pH na maganin har sai pH na maganin ya kai 8. Sannan a cikin beaker da aka sanya masa na'urar auna pH, yi amfani da maganin sulfuric acid na yau da kullun.
Don yin titration, a ƙarƙashin yanayin juyawa, lura da karatun mita pH yayin titration, lokacin da aka daidaita ƙimar pH na maganin zuwa 3.74,
Titration ɗin ya ƙare. Lura da yawan maganin sulfuric acid da aka yi amfani da shi a wannan lokacin.
Tsarawa:
Jimlar lambobin proton na sama da rukunin hydroxyethyl
Rabon adadin protons na sama; I7 shine nauyin ƙungiyar methylene akan rukunin hydroxyethyl
Ƙarfin kololuwar amsawar proton; shine ƙarfin kololuwar amsawar proton na ƙungiyoyin methine guda 5 da kuma rukunin methylene guda ɗaya akan na'urar glucose ta cellulose
Jimilla.
Hanyoyin gwaji da aka bayyana don gwajin halayen infrared na ƙwayoyin cellulose guda uku CMC, HEC da HEECMC
Dokar
3.2.4.3 Gwajin XRD
Gwajin Halayyar Nazarin Rarraba X-ray na Cellulose Ethers guda uku CMC, HEC da HEECMC
hanyar gwajin da aka bayyana.
3.2.4.4 Gwajin H-NMR
An auna na'urar auna H NMR na HEC ta amfani da na'urar auna Avance400 H NMR da BRUKER ya samar.
An yi amfani da deuterated dimethyl sulfoxide a matsayin mai narkewa, an gwada maganin ta hanyar amfani da ruwa hydrogen NMR spectroscopy. Mitar gwajin ita ce 75.5MHz.
Dumi, maganin shine 0.5 ml.
3.3 Sakamako da Bincike
3.3.1 Inganta tsarin shirye-shiryen CMC
An yi amfani da sinadarin Pine cellulose da aka cire a babi na biyu a matsayin kayan aiki na asali, sannan aka yi amfani da sodium chloroacetate a matsayin sinadarin etherifying, an yi amfani da hanyar gwajin abu ɗaya,
An inganta tsarin shirye-shiryen CMC, kuma an saita ma'aunin farko na gwajin kamar yadda aka nuna a cikin Tebur 3.3. Ga tsarin shirye-shiryen HEC.
A fannin fasaha, nazarin abubuwa daban-daban.
Tebur 3.3 Ƙimar Ma'aunin Farko
Ƙimar farko
Zafin alkaline kafin magani/℃ 40
Lokacin da ake amfani da alkaline kafin a fara magani/h 1
Rabon ruwa mai ƙarfi kafin magani/(g/mL) 1:25
Yawan sinadarin lye kafin a fara magani/% 40
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Mataki na farko zafin etherification / ℃ 45
Lokacin etherification na mataki na farko/h 1
Zafin etherification na mataki na biyu/℃ 70
Lokacin etherification na mataki na biyu/h 1
Matsakaicin sashi a matakin etherification/g 2
Adadin wakilin etherifying a matakin etherification/g 4.3
Rabon ruwa mai ƙarfi/(g/mL) 1:15
3.3.1.1 Tasirin abubuwa daban-daban akan matakin maye gurbin CMC a matakin alkali kafin magani
1. Tasirin zafin alkali kafin a fara magani akan matakin maye gurbin CMC
Domin a yi la'akari da tasirin zafin alkali kafin a fara magani kan matakin maye gurbin CMC da aka samu, idan aka gyara wasu abubuwa a matsayin ƙimar farko,
A ƙarƙashin yanayin, an tattauna tasirin zafin alkali kafin magani akan matakin maye gurbin CMC, kuma an nuna sakamakon a cikin Hoto.
Zafin alkaline kafin magani/℃
Tasirin zafin jiki na alkali kafin magani akan matakin maye gurbin CMC
Ana iya ganin cewa matakin maye gurbin CMC yana ƙaruwa tare da ƙaruwar zafin alkali kafin a fara magani, kuma zafin alkali shine 30 °C.
Matakan maye gurbin da ke sama suna raguwa tare da ƙaruwar zafin jiki. Wannan saboda zafin alkaline ya yi ƙasa sosai, kuma ƙwayoyin ba sa aiki sosai kuma ba sa iya yin hakan
Yana lalata yankin lu'ulu'u na cellulose yadda ya kamata, wanda hakan ke sa ya zama da wahala ga wakilin etherifying ya shiga cikin cellulose a matakin etherification, kuma matakin amsawar yana da girma sosai.
ƙasa, wanda ke haifar da ƙarancin matakin maye gurbin samfur. Duk da haka, zafin alkali bai kamata ya yi yawa ba. Yayin da zafin jiki ke ƙaruwa, a ƙarƙashin tasirin zafi mai yawa da alkaline mai ƙarfi,
Cellulose yana da saurin lalacewa ta hanyar iskar oxygen, kuma matakin maye gurbin samfurin CMC yana raguwa.
2. Tasirin lokacin da aka yi amfani da alkaline kafin a fara magani akan digirin maye gurbin CMC
A ƙarƙashin yanayin cewa zafin alkali kafin magani shine 30 °C da sauran dalilai sune ƙimar farko, an tattauna tasirin lokacin alkali kafin magani akan CMC.
Tasirin maye gurbin. Matakin maye gurbin
Lokacin allurar kafin magani/h
Tasirin lokacin da aka fara amfani da alkaline kafin a fara magani akanCMCdigirin maye gurbin
Tsarin bulking ɗin kansa yana da sauri, amma maganin alkali yana buƙatar wani lokacin yaɗuwa a cikin zare.
Ana iya ganin cewa lokacin da lokacin alkali ya kasance awanni 0.5-1.5, matakin maye gurbin samfurin yana ƙaruwa tare da ƙaruwar lokacin alkali.
Matsayin maye gurbin samfurin da aka samu ya fi girma lokacin da lokacin ya kasance awanni 1.5, kuma matakin maye gurbin ya ragu tare da ƙaruwar lokaci bayan awanni 1.5. Wannan zai iya faruwa.
Yana iya zama saboda a farkon alkali, tare da tsawaita lokacin alkali, shigar alkali zuwa cellulose ya fi isa, don haka zare
Tsarin farko ya fi annashuwa, yana ƙara sinadarin etherifying da kuma hanyar aiki
Lokacin Saƙo: Afrilu-26-2024