Cellulose ether na Epoxy resin

A na-eji owu na-ekpofu ahịhịa na sawdust mee ihe dị ka akụrụngwa, ma na-agbanye mmiri n'ime alkalicellulose ethern'okpuru omume nke 18% alkali na usoro nke mgbakwunye. Mgbe ahụ, jiri epoxy resin maka grafting, molar ruru nke epoxy resin na alkali eriri bụ 0.5: 1.0, mmeghachi omume okpomọkụ bụ 100.°C, oge mmeghachi omume bụ 5.0h, usoro ọgwụgwọ na-akpali akpali bụ 1%, na ọnụego etherification grafting bụ 32%. A na-ejikọta ether epoxy cellulose nke enwetara na 0.6mol Cel-Ep na 0.4mol CAB iji mepụta ngwaahịa mkpuchi ọhụrụ na arụmọrụ dị mma. Eji IR kwadoro nhazi ngwaahịa a.

Isi okwu:cellulose ether; njikọ; CAB; Njirimara mkpuchi

Cellulose ether bụ eke polima, nke a kpụrụ site condensation nkeβ- glucose. Cellulose nwere ọkwa dị elu nke polymerization, ọkwa dị mma nke nghazi, yana ezigbo nkwụsi ike nke kemịkal. Enwere ike nweta ya site na ọgwụgwọ cellulose (esterification ma ọ bụ etherification). A usoro nke cellulose mmepụta, ndị a na ngwaahịa na-ọtụtụ ebe na-eji plastik, biodegradable nri ehihie igbe, elu-ọgwụgwụ akpakanamde mkpuchi, akpaaka akụkụ, obibi akwụkwọ inks, adhesives, wdg Ugbu a, ọhụrụ gbanwetụrụ cellulose iche na-mgbe niile apụta, na ngwa ubi bụ. na-agbasawanye mgbe niile, jiri nwayọọ nwayọọ na-etolite usoro ụlọ ọrụ fiber. Isiokwu a bụ iji sawdust ma ọ bụ owu na-ekpofu ahịhịa ka a ga-eji lye mee ka mmiri mee ka ọ bụrụ obere eriri, wee nyadokwa kemịkalụ ma gbanwee iji mepụta ụdị mkpuchi ọhụrụ nke a na-edebeghị na akwụkwọ ahụ.

1. Nnwale

1.1 Reagents na ngwa

Owu efu (asachara na akpọnwụ), NaOH, 1,4-butanediol, methanol, thiourea, urea, resin epoxy, acetic anhydride, butyric acid, trichloroethane, formic acid, glioxal, toluene, CAB, wdg (Ọcha bụ ọkwa CP) . A na-eji spectrometer Magna-IR 550 infrared infrared mepụtara site na ụlọ ọrụ Nicolet nke United States iji kwadebe ihe nlele ahụ site na mkpuchi tetrahydrofuran mgbaze. Tu-4 viscometer, FVXD3-1 ụdị mgbe niile okpomọkụ onwe-achịkwa eletriki edemede mmeghachi omume kettle, nke Weihai Xiangwei Chemical Machinery Factory mepụtara; viscometer rotational NDJ-7, ụdị Z-10MP5, nke Shanghai Tianping Instrument Factory mepụtara; A na-atụle ịdị arọ molekụla site na Ubbelohde viscosity; A ga-eme nkwadebe na nyocha nke ihe nkiri agba dị ka ọkọlọtọ mba GB-79 si dị.

1.2 Ụkpụrụ mmeghachi omume

1.3 Nkwekọrịta

Synthesis nke epoxy cellulose: Tinye 100g nke chopped owu eriri na a mgbe nile okpomọkụ onwe-achịkwa electric edemede reactor, tinye oxidant na-emeghachi omume maka 10 nkeji, mgbe ahụ tinye mmanya na alkali na-eme ka a lye na ịta nke 18%. Tinye ngwa ngwa A, B, wdg maka impregnation. Meghachi omume na ụfọdụ okpomọkụ n'okpuru agụụ maka awa 12, nyo, kpoo ma tụọ 50g nke cellulose alkalized, gbakwunye ihe mgbaze gwakọtara iji mee slurry, tinye ihe na-akpali akpali na resin epoxy na arọ molekụla kpọmkwem, kpoo ruo 90 ~ 110.℃maka etherification mmeghachi omume 4.0 ~ 6.0h ruo mgbe reactants bụ miscible. Tinye formic acid iji wepụ ma wepụ alkali dị ukwuu, kewaa ngwọta mmiri na ihe mgbaze, saa ya na 80.℃mmiri ọkụ iji wepụ sodium nnu, na nkụ maka ojiji ọzọ. Ejiri viscometer Ubbelohde tụọ viscosity dị n'ime ma gbakọọ nkezi ịdị arọ nke viscosity dị ka akwụkwọ si dị.

A na-akwadebe acetate butyl cellulose dị ka usoro akwụkwọ si dị, tụọ 57.2g nke owu a nụchara anụcha, tinye 55g acetic anhydride, 79g nke butyric acid, 9.5g nke magnesium acetate, 5.1g nke sulfuric acid, jiri butyl acetate dị ka ihe mgbaze, ma meghachi omume na a ụfọdụ okpomọkụ ruo mgbe ruru eru , neutralized site n'ịgbakwụnye sodium acetate, precipitated, filter, sachara, filter, na akpọnwụ maka emechaa. Were Cel-Ep, gbakwunye ego CAB kwesịrị ekwesị na ihe mgbaze agwakọta ọnụ, kpoo ọkụ ma kpalie maka 0.5h iji mee otu mmiri mmiri siri ike, na nkwadebe ihe nkiri mkpuchi na ule arụmọrụ na-agbaso usoro GB-79.

Mkpebi nke ogo esterification nke cellulose acetate: mbụ igbari cellulose acetate na dimethyl sulfoxide, tinye a metered ego nke alkali ngwọta okpomọkụ na hydrolyzes, na titrate hydrolyzed ngwọta na NaOH ọkọlọtọ ngwọta gbakọọ ngụkọta oriri nke alkali. Mkpebi nke ọdịnaya mmiri: Tinye ihe nlele na oven na 100 ~ 105°C ka akpọọ nkụ maka 0.2h, tụọ ma gbakọọ nnabata mmiri mgbe ọ jụrụ. Mkpebi nke absorption alkali: tụọ ihe atụ nke ọnụọgụ, gbazee ya na mmiri ọkụ, gbakwunye ihe ngosi methyl violet, wee titrate na 0.05mol/L H2SO4. Mkpebi nke ogo mgbasawanye: tụọ 50g sample, gwepịa ya ma tinye ya n'ime tube gụsịrị akwụkwọ, gụọ olu ahụ mgbe ụda eletrik gasịrị, ma jiri ya tụnyere olu nke cellulose ntụ ntụ na-enweghị alkalined iji gbakọọ ogo mgbasawanye.

2. Nsonaazụ na mkparịta ụka

2.1 Mmekọrịta dị n'etiti ịta alkali na ogo ọzịza cellulose

Mmeghachi omume nke cellulose na ụfọdụ ntinye nke ngwọta NaOH nwere ike ibibi kristal na cellulose mgbe niile ma mee ka cellulose zaa. Na mmebi dị iche iche na-eme na lye, na-ebelata ogo nke polymerization. Nnwale na-egosi na ogo ọzịza nke cellulose na ọnụọgụ alkali na-ejikọta ma ọ bụ mgbasa ozi na-abawanye na ntinye nke alkali. Ogo nke hydrolysis na-abawanye na mmụba nke okpomọkụ. Mgbe ntinye alkali ruru 20%, ogo hydrolysis bụ 6.8% na t = 100.°C; ogo nke hydrolysis bụ 14% na t = 135°C. N'otu oge ahụ, nnwale na-egosi na mgbe alkali bụ ihe karịrị 30%, ogo nke hydrolysis nke cellulose yinye scission na-budata belata. Mgbe ịta alkali ruru 18%, ikike mgbasa ozi na ọzịza nke mmiri bụ nke kachasị, itinye uche na-aga n'ihu na-abawanye, na-adaba nke ọma na mbara ala, wee na-agbanwe nwayọ. N'otu oge ahụ, mgbanwe a na-enwe mmetụta nke ọma na mmetụta nke okpomọkụ. N'okpuru otu ntinye alkali, mgbe okpomọkụ dị ala (<20°C), ogo ọzịza nke cellulose dị ukwuu, na ọnụọgụ mgbasa ozi buru ibu; na oke okpomọkụ, ogo ọzịza na ọnụọgụ mgbasa mmiri dị oke mkpa. belata.

A na-ekpebi eriri alkali nwere mmiri dị iche iche yana ọdịnaya alkali site na usoro nyocha ihe gbasara X-ray dị ka akwụkwọ si dị. Na arụ ọrụ n'ezie, a na-eji 18% ~ 20% lye chịkwaa ụfọdụ mmeghachi omume okpomọkụ iji mee ka ọzịza nke cellulose dịkwuo elu. Nlele na-egosi na cellulose meghachi omume site kpo oku maka 6 ~ 12h nwere ike igbari na pola solvents. Dabere na eziokwu a, onye edemede ahụ na-eche na solubility nke cellulose na-arụ ọrụ dị mkpa n'ókè nke mbibi nke njikọ hydrogen n'etiti mkpụrụ ndụ cellulose na akụkụ crystalline, na-esote ogo nke hydrogen bond mbibi nke intramolecular glucose otu C3-C2. Ọnụ ọgụgụ dị ukwuu nke mbibi nke njikọ hydrogen, ka mmụba nke eriri alkali na-abawanye, na njikọ hydrogen na-ebibi kpamkpam, na hydrolyzate ikpeazụ bụ ihe na-edozi mmiri.

2.2 Mmetụta nke ngwa ngwa

Ịgbakwunye mmanya na-esi ísì dị elu n'oge cellulose alkalization nwere ike ime ka mmeghachi omume ahụ dịkwuo elu, na ịtinye obere ihe na-emepụta ihe dị ka obere mmanya na thiourea (ma ọ bụ urea) nwere ike ịkwalite ntinye na ọzịza nke cellulose. Ka ịta mmanya na-aba n'anya na-abawanye, nnabata alkali nke cellulose na-abawanye, na enwere mgbanwe mgbanwe mberede mgbe ịta ahụ dị 20%, nke nwere ike ịbụ na mmanya monofunctional na-abanye n'ime mkpụrụ ndụ cellulose iji mepụta njikọ hydrogen na cellulose, na-egbochi cellulose. molecules Njikọ hydrogen n'etiti agbụ na ụdọ molekụla na-abawanye ogo nke ọgba aghara, na-abawanye ebe elu, ma na-abawanye ọnụọgụ alkali adsorption. Otú ọ dị, n'okpuru otu ọnọdụ ahụ, absorption alkali nke ibe osisi dị ala, na ntụgharị na-agbanwe na ọnọdụ na-agbanwe agbanwe. Ọ nwere ike jikọta ya na obere ọdịnaya nke cellulose na ibe osisi, nke nwere nnukwu lignin, nke na-egbochi ntinye nke mmanya na-aba n'anya, ma nwee ezigbo mmiri na-eguzogide na alkali.

2.3 Etherification

Tinye 1% B na-akpali akpali, jikwaa ọnọdụ mmeghachi omume dị iche iche, wee jiri resin epoxy na alkali mee mgbanwe etherification. Ọrụ mmeghachi omume etherification dị ala na 80°C. Ọnụọgụ grafting nke Cel bụ naanị 28%, yana ọrụ etherification fọrọ nke nta ka ọ bụrụ okpukpu abụọ na 110.°C. N'ịtụle ọnọdụ mmeghachi omume dị ka ihe mgbaze, mmeghachi omume okpomọkụ bụ 100°C, na oge mmeghachi omume bụ 2.5h, na ọnụ ọgụgụ grafting nke Cel nwere ike iru 41%. Tụkwasị na nke ahụ, na mmalite nke mmeghachi omume etherification (<1.0h), n'ihi mmeghachi omume dị iche iche n'etiti alkali cellulose na epoxy resin, ọnụ ọgụgụ grafting dị ala. Site na mmụba nke Cel etherification ogo, ọ na-eji nwayọọ nwayọọ na-aghọ mmeghachi omume homogeneous, ya mere mmeghachi omume ahụ na-abawanye nke ọma, na ọnụ ọgụgụ grafting mụbara.

2.4 Mmekọrịta dị n'etiti Cel grafting ọnụego na solubility

Nlele egosiwo na mgbe grafting epoxy resin na alkali cellulose, a na-ahụ anya Njirimara dị ka ngwaahịa viscosity, adhesion, mmiri na-eguzogide, na thermal kwụsie ike nke ukwuu. Nnwale solubility Ngwaahịa nwere ọnụ ọgụgụ Cel grafting <40% nwere ike igbari na obere mmanya ester, resin alkyd, polyacrylic acid resin, acrylic pimaric acid na resin ndị ọzọ. Cel-Ep resin nwere mmetụta solubilizing doro anya.

Ejikọtara ya na nyocha ihe nkiri mkpuchi mkpuchi, ngwakọta na ọnụ ọgụgụ grafting nke 32% ~ 42% n'ozuzu nwere ndakọrịta ka mma, na ngwakọta na ọnụ ọgụgụ grafting nke <30% enweghị ndakọrịta na-adịghị mma na obere gloss nke ihe nkiri mkpuchi; ọnụ ọgụgụ grafting dị elu karịa 42%, nkwụsị mmiri na-esi ísì ụtọ, nkwụsị mmanya na-egbu egbu na polar organic mgbaze ihe nkiri na-ebelata. Iji meziwanye ihe ndakọrịta ihe na arụmọrụ mkpuchi, onye edemede ahụ gbakwunyere CAB dịka usoro dị na Tebụl 1 iji nwetakwuo solubilize na gbanwee iji kwalite ịdị n'otu nke Cel-Ep na CAB. Ngwakọta ahụ na-etolite usoro ihe jikọrọ ọnụ. Ọkpụrụkpụ interface ihe mejupụtara nke ngwakọta na-adị ezigbo mkpa ma gbalịa ịnọ na steeti nano-cell.

2.5 Mmekọrịta dị n'etiti Cel-Ngwakọta Ep/CAB na akụrụngwa anụ ahụ

N'iji Cel-Ep iji jikọta ya na CAB, ihe nyocha nke mkpuchi na-egosi na acetate cellulose nwere ike imeziwanye ihe mkpuchi nke ihe ahụ, karịsịa ngwa ngwa ihicha. Akụkụ dị ọcha nke Cel-Ep siri ike ịkpọ nkụ n'ime ụlọ okpomọkụ. Mgbe agbakwunyere CAB, ihe abụọ ahụ nwere mmekọ arụmọrụ doro anya.

2.6 nchọpụta ụdịdị dị iche iche FTIR

3. Nkwubi okwu

(1) Owu cellulose nwere ike ịza na 80°C na> 18% alkali na-etinye uche na usoro ihe mgbakwunye, na-amụba okpomọkụ mmeghachi omume, mee ka oge mmeghachi omume dịkwuo ogologo, na-abawanye ogo nke ọzịza na mmebi ruo mgbe ọ ga-ekpochapụ kpamkpam.

(2) Mmeghachi omume etherification, Cel-Ep molar feed ratio bụ 2, mmeghachi omume okpomọkụ bụ 100°C, oge bụ 5h, usoro onunu ogwu bụ 1%, na etherification grafting ọnụego nwere ike iru 32% ~ 42%.

(3) Blending mgbanwe, mgbe molar ratio nke Cel-Ep: CAB = 3: 2, arụmọrụ nke synthesized ngwaahịa dị mma, ma dị ọcha Cel-Ep enweghị ike iji dị ka mkpuchi, naanị dị ka nrapado.