Focus on Cellulose ethers

Cellulose Ether akan Resin Epoxy

Cellulose ether a kan Epoxy Resin

Ana amfani da auduga mai sharar gida da sawdust azaman albarkatun ƙasa, kuma ana sanya su cikin alkalicellulose etherƙarƙashin aikin 18% alkali da jerin abubuwan ƙari. Sa'an nan amfani da epoxy guduro don grafting, da molar rabo na epoxy guduro da alkali fiber ne 0.5: 1.0, da dauki zazzabi ne 100.°C, lokacin amsawa shine 5.0h, adadin mai kara kuzari shine 1%, kuma ƙimar etherification shine 32%. The samu epoxy cellulose ether aka blended da 0.6mol Cel-Ep da 0.4mol CAB don hada wani sabon shafi samfurin tare da mai kyau yi. An tabbatar da tsarin samfurin tare da IR.

Mabuɗin kalmomi:ether cellulose; hadawa; CAB; shafi Properties

 

Cellulose ether shi ne na halitta polymer, wanda aka kafa ta condensation naβ- glucose. Cellulose yana da babban digiri na polymerization, kyakkyawan matsayi na daidaitawa, da kuma kyakkyawan kwanciyar hankali na sinadarai. Ana iya samun shi ta hanyar sinadarai na maganin cellulose (esterification ko etherification). Jerin abubuwan da aka samo asali na cellulose, waɗannan samfuran ana amfani da su sosai a cikin robobi, akwatunan abincin rana mai lalacewa, manyan kayan kwalliyar mota, sassan auto, tawada bugu, adhesives, da sauransu. ci gaba da fadadawa, a hankali yana samar da tsarin masana'antar fiber. Wannan batu shi ne a yi amfani da sawdust ko auduga da aka sharar da za a sanya ruwa cikin gajeriyar zaruruwa ta hanyar lemun tsami, sa'an nan kuma a daka su da sinadarai da kuma gyara su don samar da wani sabon nau'in suturar da ba a ba da rahoto a cikin takardar ba.

 

1. Gwaji

1.1 Reagents da kayan aiki

Sharar gida auduga (wanke da bushe), NaOH, 1,4-butanediol, methanol, thiourea, urea, epoxy guduro, acetic anhydride, butyric acid, trichloroethane, formic acid, glioxal, toluene, CAB, da dai sauransu (Tsarki ne CP sa). . Magna-IR 550 infrared spectrometer da Kamfanin Nicolet na Amurka ya samar an yi amfani da shi don shirya samfuran ta hanyar shafan tetrahydrofuran. Tu-4 viscometer, FVXD3-1 nau'in yawan zafin jiki mai sarrafa kansa mai sarrafa wutar lantarki, wanda Weihai Xiangwei Chemical Machinery Factory ya samar; juyi viscometer NDJ-7, Z-10MP5 nau'in, samar da Shanghai Tianping Instrument Factory; Ana auna nauyin kwayoyin ta hanyar Ubbelohde danko; Shirye-shiryen da gwaji na fim ɗin fenti za a yi su bisa ga ma'auni na GB-79 na kasa.

1.2 Ka'idar amsawa

1.3 Haɗin kai

Kira na epoxy cellulose: Add 100g na yankakken auduga fiber zuwa akai-akai zafin jiki mai sarrafa kai lantarki stirring reactor, ƙara oxidant da amsa na minti 10, sa'an nan kuma ƙara barasa da alkali don yin lye tare da maida hankali na 18%. Ƙara accelerators A, B, da dai sauransu don ciki. Amsa a wani zafin jiki a karkashin injin don awanni 12, tace, bushe da auna 50g na cellulose alkalized, ƙara gauraye da sauran ƙarfi don yin slurry, ƙara mai kara kuzari da resin epoxy tare da takamaiman nauyin kwayoyin, zafi har zuwa 90 ~ 110domin etherification dauki 4.0 ~ 6.0h har sai da reactants ne miscible. Add formic acid don neutralize da cire wuce haddi alkali, raba da ruwa bayani da sauran ƙarfi, wanke da 80ruwan zafi don cire gishirin sodium, kuma bushe don amfani daga baya. An auna danko na ciki tare da ma'aunin sikometer na Ubbelohde kuma an ƙididdige matsakaicin ma'aunin ƙwayar ƙwayar cuta bisa ga adabi.

An shirya acetate butyl cellulose bisa ga hanyar wallafe-wallafe, auna nauyin 57.2g na auduga mai ladabi, ƙara 55g na acetic anhydride, 79g na butyric acid, 9.5g na magnesium acetate, 5.1g na sulfuric acid, yi amfani da butyl acetate a matsayin sauran ƙarfi, kuma amsa a wani zafin jiki har sai ya cancanta, neutralized ta ƙara sodium acetate, precipitated, tacewa, wanke, tacewa, da bushe don amfani daga baya. Ɗauki Cel-Ep, ƙara adadin CAB da ya dace da ƙayyadaddun gauraye mai gauraye, zafi sama da motsawa don 0.5h don samar da ruwa mai kauri na uniform, kuma shirye-shiryen fim ɗin da gwajin aiki ya bi hanyar GB-79.

Ƙaddamar da mataki na esterification na cellulose acetate: na farko narke acetate cellulose a dimethyl sulfoxide, ƙara wani metered adadin alkali bayani ga zafi da kuma hydrolyzes, da kuma titrate da hydrolyzed bayani tare da NaOH misali bayani don lissafin jimlar yawan amfani da alkali. Ƙayyade abun ciki na ruwa: Sanya samfurin a cikin tanda a 100 ~ 105°C don bushewa na 0.2h, auna kuma lissafta sha ruwan bayan sanyaya. Ƙayyade shayarwar alkali: auna samfurin ƙididdiga, narkar da shi a cikin ruwan zafi, ƙara alamar methyl violet, sa'an nan kuma titrate tare da 0.05mol/L H2SO4. Ƙaddamar da digiri na fadada: Auna samfurin 50g, murkushe shi kuma saka shi a cikin bututu mai digiri, karanta ƙarar bayan girgizar lantarki, kuma kwatanta shi tare da ƙarar foda na cellulose mara kyau don ƙididdige darajar fadada.

 

2. Sakamako da tattaunawa

2.1 Alakar dake tsakanin maida hankali na alkali da matakin kumburin cellulose

Halin da ake yi na cellulose tare da wani nau'i na maganin NaOH zai iya lalata tsarin crystallization na cellulose na yau da kullum kuma ya sa cellulose ya kumbura. Kuma daban-daban degendations faruwa a lye, rage mataki na polymerization. Gwaje-gwaje sun nuna cewa matakin kumburin cellulose da adadin alkali dauri ko adsorption yana ƙaruwa tare da maida hankali na alkali. Matsayin hydrolysis yana ƙaruwa tare da ƙara yawan zafin jiki. Lokacin da ƙaddamarwar alkali ya kai 20%, matakin hydrolysis shine 6.8% a t = 100.°C; Matsayin hydrolysis shine 14% a t = 135°C. A lokaci guda, gwajin ya nuna cewa lokacin da alkali ya fi 30%, matakin hydrolysis na sarkar cellulose yana raguwa sosai. Lokacin da alkali maida hankali ya kai 18%, da adsorption iya aiki da kumburi digiri na ruwa ne matsakaicin, maida hankali ya ci gaba da karuwa, ya ragu sosai zuwa wani tudu, sa'an nan kuma canje-canje a hankali. A lokaci guda, wannan canjin yana da matukar kula da tasirin zafin jiki. Ƙarƙashin ƙwayar alkali guda ɗaya, lokacin da zafin jiki ya yi ƙasa (<20°C), matakin kumburi na cellulose yana da girma, kuma adadin adsorption na ruwa yana da girma; a high zafin jiki, kumburi mataki da ruwa adsorption adadin suna da muhimmanci. rage.

Filayen alkali da ke da abun ciki na ruwa daban-daban da abun ciki na alkali an ƙaddara su ta hanyar nazarin rarrabuwar kawuna na X-ray bisa ga adabi. A cikin aiki na ainihi, ana amfani da 18% ~ 20% lye don sarrafa wani zafin jiki don ƙara yawan kumburin cellulose. Gwaje-gwaje sun nuna cewa cellulose da aka amsa ta hanyar dumama don 6 ~ 12h na iya narkar da su a cikin kaushi na polar. Bisa ga wannan gaskiyar, marubucin yana tunanin cewa solubility na cellulose yana taka muhimmiyar rawa a cikin digiri na lalata haɗin gwiwar hydrogen tsakanin kwayoyin cellulose a cikin ɓangaren crystalline, wanda ya biyo baya matakin lalata haɗin gwiwar hydrogen na ƙungiyoyin glucose na intramolecular C3-C2. Mafi girman matakin lalata haɗin gwiwar hydrogen, mafi girman matakin kumburin fiber alkali, kuma haɗin hydrogen ya lalace gaba ɗaya, kuma hydrolyzate na ƙarshe shine abu mai narkewa da ruwa.

2.2 Tasirin Accelerator

Ƙara barasa mai zafi mai zafi yayin alkalization na cellulose zai iya ƙara yawan zafin jiki, da kuma ƙara ƙaramin adadin furotin kamar ƙananan barasa da thiourea (ko urea) na iya haɓaka shiga da kumburin cellulose. Yayin da yawan barasa ya karu, shayarwar alkali na cellulose yana ƙaruwa, kuma akwai canjin canji kwatsam lokacin da maida hankali ya kasance 20%, wanda zai iya zama cewa barasa na monofunctional ya shiga cikin kwayoyin cellulose don samar da haɗin hydrogen tare da cellulose, yana hana cellulose. Kwayoyin Halitta Haɗin hydrogen tsakanin sarƙoƙi da sarƙoƙi na ƙwayoyin cuta suna ƙara ƙimar rashin ƙarfi, ƙara yanayin ƙasa, da haɓaka adadin adadin alkali. Duk da haka, a ƙarƙashin yanayi guda, ƙwayar alkali na kwakwalwan itace yana da ƙasa, kuma lanƙwasa yana canzawa a cikin yanayi mai canzawa. Yana iya kasancewa yana da alaƙa da ƙananan abun ciki na cellulose a cikin guntun itace, wanda ya ƙunshi babban adadin lignin, wanda ke hana shigar da barasa, kuma yana da kyakkyawan juriya na ruwa da juriya na alkali.

2.3 Etherification

Ƙara 1% B mai kara kuzari, sarrafa yanayin zafi daban-daban, da aiwatar da gyaran etherification tare da resin epoxy da fiber alkali. Ayyukan amsawar etherification yayi ƙasa a 80°C. Yawan grafting na Cel shine kawai 28%, kuma aikin etherification ya kusan ninka sau biyu a 110°C. Idan aka yi la'akari da yanayin amsawa kamar sauran ƙarfi, yawan zafin jiki shine 100°C, kuma lokacin amsawa shine 2.5h, kuma ƙimar grafting na Cel na iya kaiwa 41%. Bugu da ƙari, a farkon mataki na etherification dauki (<1.0h), saboda da iri-iri dauki tsakanin alkali cellulose da epoxy guduro, da grafting kudi ne low. Tare da karuwa da digiri na etherification Cel, a hankali ya juya zuwa wani abu mai kama da juna, don haka aikin ya karu sosai, kuma ƙimar grafting ya karu.

2.4 Dangantaka tsakanin Cel grafting rate da solubility

Gwaje-gwaje sun nuna cewa bayan grafting epoxy guduro tare da alkali cellulose, na jiki Properties kamar samfurin danko, adhesion, ruwa juriya, da thermal kwanciyar hankali za a iya muhimmanci inganta. Gwajin solubility Samfurin tare da ƙimar Cel grafting <40% ana iya narkar da shi a cikin ƙananan barasa-ester, resin alkyd, guduro acid polyacrylic, acrylic pimaric acid da sauran resins. Cel-Ep guduro yana da tabbataccen sakamako mai narkewa.

Haɗe tare da gwajin fim ɗin shafa, haɗuwa tare da ƙimar grafting na 32% ~ 42% gabaɗaya suna da daidaituwa mafi kyau, kuma haɗuwa tare da ƙimar grafting na <30% suna da rashin daidaituwa da ƙarancin haske na fim ɗin shafi; da grafting kudi ne mafi girma fiye da 42%, da tafasasshen ruwa juriya, barasa juriya, da iyakacin duniya sauran ƙarfi ƙarfi juriya na shafi fim an rage. Don inganta daidaituwar kayan aiki da aikin sutura, marubucin ya ƙara CAB bisa ga dabarar da ke cikin Teburin 1 don ƙara daidaitawa da gyaggyarawa don haɓaka kasancewar Cel-Ep da CAB. Cakudar ta samar da tsarin tsarin kamanni. Ƙaƙƙarfan ƙaƙƙarfan ƙayyadaddun ƙayyadaddun gaurayawan yakan zama bakin ciki sosai kuma yana ƙoƙarin kasancewa cikin yanayin nano-cells.

2.5 Dangantaka tsakanin Cel-Ep/CAB hadewar rabo da kaddarorin jiki

Yin amfani da Cel-Ep don haɗawa tare da CAB, sakamakon gwajin gwaji ya nuna cewa acetate cellulose na iya inganta ingantaccen kayan shafa na kayan, musamman ma saurin bushewa. Sashin tsabta na Cel-Ep yana da wuyar bushewa a dakin da zafin jiki. Bayan ƙara CAB, kayan biyu suna da ingantaccen aikin aiki.

2.6 Gano bakan FTIR

 

3. Kammalawa

(1) Auduga cellulose zai iya kumbura a 80°C tare da> 18% maida hankali alkali da jerin additives, ƙara yawan zafin jiki, tsawaita lokacin amsawa, ƙara yawan kumburi da lalacewa har sai an cika shi da ruwa.

(2) Etherification dauki, Cel-Ep molar abinci rabo ne 2, da dauki zazzabi ne 100°C, lokacin shine 5h, adadin mai kara kuzari shine 1%, kuma ƙimar etherification na iya kaiwa 32% ~ 42%.

(3) Haɗin gyare-gyare, lokacin da rabon molar na Cel-Ep: CAB = 3: 2, aikin samfurin da aka haɗa yana da kyau, amma Cel-Ep mai tsabta ba za a iya amfani da shi azaman sutura ba, kawai a matsayin m.


Lokacin aikawa: Janairu-16-2023
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