Njikọ na njirimara nke Butane Sulfonate Cellulose Ether Water Reducer

A na-eji microcrystalline cellulose (MCC) nwere ogo polymerization nke enwetara site na acid hydrolysis nke cellulose owu pulp dị ka akụrụngwa. N'okpuru mmalite nke sodium hydroxide, a na-emeghachi ya na 1,4-butane sultone (BS) iji nweta A cellulose butyl sulfonate (SBC) mmiri na-ebelata mmiri nke nwere ezigbo mmiri solubility. E ji ihe owuwu ngwaahịa a mara site na infrared spectroscopy (FT-IR), nuklia magnetik resonance spectroscopy (NMR), nyocha microscopy eletrọnịkị (SEM), diffraction X-ray (XRD) na ụzọ nyocha ndị ọzọ, yana ogo polymerization, oke akụrụngwa, a nyochara mmeghachi omume nke MCC. Mmetụta nke ọnọdụ usoro sịntetik dị ka okpomọkụ, oge mmeghachi omume, na ụdị onye na-akwụsịtụ ọrụ na-ebelata mmiri nke ngwaahịa. Nsonaazụ na-egosi na: mgbe ogo nke polymerization nke akụrụngwa MCC bụ 45, oke nha nke ndị na-eme ihe bụ: AGU (cellulose glucoside unit): n (NaOH): n (BS) = 1.0: 2.1: 2.2, The Onye nkwusioru bụ isopropanol, oge ịgbalite ngwa ngwa na ụlọ okpomọkụ bụ 2 h, na oge njikọ ngwaahịa bụ 5 h. Mgbe okpomọkụ dị 80 Celsius C, ngwaahịa enwetara nwere ogo kachasị elu nke nnọchi nke otu butanesulfonic acid, na ngwaahịa ahụ nwere arụmọrụ na-ebelata mmiri kacha mma.

Isi okwu:cellulose; butylsulfonate cellulose; onye na-ebelata mmiri; mmiri na-ebelata arụmọrụ

1,Okwu mmalite

Concrete superplasticizer bụ otu n'ime ihe ndị dị mkpa nke sink ọgbara ọhụrụ. Ọ bụ kpọmkwem n'ihi ọdịdị nke onye na-ebelata mmiri na-arụ ọrụ dị elu, ịdịte aka dị mma na ọbụna ike dị elu nke ihe nwere ike ijide n'aka. Ndị na-ebelata mmiri dị elu nke a na-ejikarị eme ihe ugbu a gụnyere ụdị ndị a: naphthalene-based water reducer (SNF), sulfonated melamine resin based water-reducer (SMF), sulfmate-based water-reducer (ASP), modified Lignosulfonate superplasticizer ML), na polycarboxylate superplasticizer (PC), nke a na-eme nyocha nke ọma ugbu a. N'ịtụle usoro njikọ nke ndị na-ebelata mmiri, ọtụtụ n'ime ndị na-ebelata mmiri condensate gara aga na-eji formaldehyde nwere isi ísì siri ike dị ka akụrụngwa maka mmeghachi omume polycondensation, a na-ejikarị sulfuric acid fuming na-emebi emebi ma ọ bụ sulfuric acid gbanyere mkpọrọgwụ. Nke a ga - abụrịrị na ọ ga - ebute mmetụta ọjọọ na ndị ọrụ na gburugburu ebe obibi, ma na - emepụtakwa nnukwu ihe mkpofu na mmiri mmiri na - ekpofusị ihe, nke na-adịghị akwado mmepe mmepe; Otú ọ dị, ọ bụ ezie na ndị na-ebelata mmiri nke polycarboxylate nwere uru nke obere nkwụsị nke ihe na-eme ka oge na-aga, obere usoro onunu ogwu, nke ọma na-asọba Ọ nwere uru nke njupụta dị elu na ọ dịghị ihe ndị na-egbu egbu dị ka formaldehyde, ma ọ na-esiri ike ịkwalite ya na China n'ihi oke dị elu. ọnụ ahịa. Site na nyocha nke isi iyi nke akụrụngwa, ọ naghị esiri ike ịchọta na ọtụtụ n'ime ndị na-ebelata mmiri a kpọtụrụ aha n'elu na-ejikọta ya na-adabere na ngwaahịa / ngwaahịa petrochemical, ebe mmanụ ala, dị ka ihe na-enweghị ike imeghari, na-esiwanye ike na ọnụ ahịa ya na-arị elu mgbe niile. Ya mere, otu esi eji ọnụ ala na ụbara akụ na-emegharịghachi nke sitere n'okike dị ka akụrụngwa iji mepụta ihe ọhụrụ dị elu nke na-arụ ọrụ nke ọma bụ ihe ntụzi nyocha dị mkpa maka ihe superplasticizers.

Cellulose bụ macromolecule linear guzobere site na ijikọ ọtụtụ D-glucopyranose na β- (1-4) glycosidic bonds. Enwere otu hydroxyl atọ na mgbanaka glucopyranosyl ọ bụla. Ọgwụgwọ kwesịrị ekwesị nwere ike nweta mmeghachi omume ụfọdụ. N'akwụkwọ a, a na-eji cellulose owu pulp mee ihe dị ka ihe mbụ, na mgbe acid hydrolysis nweta microcrystalline cellulose na ogo polymerization kwesịrị ekwesị, sodium hydroxide na-arụ ọrụ ya ma meghachi omume na 1,4-butane sultone iji kwadebe butyl sulfonate Acid. cellulose ether superplasticizer, na ihe ndị na-emetụta mmeghachi omume nke ọ bụla a tụlere.

2. Nnwale

2.1 Akụrụngwa

Cellulose owu pulp, polymerization ogo 576, Xinjiang Aoyang Technology Co., Ltd .; 1,4-butane sultone (BS), ụlọ ọrụ mmepụta ihe, nke Shanghai Jiachen Chemical Co., Ltd mepụtara .; 52.5R nkịtị Portland ciment, Urumqi nyere site ciment factory; China ISO ọkọlọtọ ájá, nke Xiamen Ace Ou Standard Sand Co., Ltd mepụtara; sodium hydroxide, hydrochloric acid, isopropanol, methanol anhydrous, ethyl acetate, n-butanol, petroleum ether, wdg, niile dị ọcha na nyocha, dị na azụmaahịa.

2.2 Usoro nnwale

Tụnye obere mkpụrụ osisi owu wee gwerie ya nke ọma, tinye ya na karama olu atọ, gbakwunye ntakịrị ihe nke dilute hydrochloric acid, kpalite ikpo ọkụ na hydrolyze ruo oge ụfọdụ, dị jụụ n'ime ụlọ, iyo, na-asa mmiri ruo na-anọpụ iche, na agụụ akọrọ na 50 ° C iji nweta Mgbe ọ nwetasịrị microcrystalline cellulose raw material na dị iche iche degrees nke polymerization, tụọ ogo ha polymerization dị ka akwụkwọ, tinye ya na a atọ olu mmeghachi omume karama, kwụsịtụ ya na. onye na-akwụsị akwụsị 10 ugboro ya uka, tinye ụfọdụ ego nke sodium hydroxide aqueous ngwọta n'okpuru edemede, kpalie ma rụọ ọrụ na ụlọ okpomọkụ ruo oge ụfọdụ, tinye gbakọọ ego nke 1,4-butane sultone (BS), kpo oku elu. na okpomọkụ mmeghachi omume, meghachi omume na okpomọkụ na-adịgide adịgide ruo oge ụfọdụ, mee ka ngwaahịa ahụ dị jụụ n'ime ụlọ, ma nweta ngwaahịa crude site na nzacha mmiri. Jiri mmiri na methanol sachaa ugboro 3, wee jiri mmiri na-ekpocha mmiri iji nweta ngwaahịa ikpeazụ, ya bụ cellulose butylsulfonate water reducer (SBC).

2.3 Nyocha ngwaahịa na njirimara

2.3.1 Mkpebi nke ọdịnaya sọlfọ ngwaahịa na ngụkọta nke ogo nnọchi

Eji FLASHEA-PE2400 elemental analyzer mee nyocha elemental na ngwaahịa mbelata mmiri cellulose butyl sulfonate akpọnwụwo iji chọpụta ọdịnaya sọlfọ.

2.3.2 Mkpebi nke fluidity nke ngwa agha

A tụrụ dịka 6.5 na GB8076-2008 si dị. Ya bụ, buru ụzọ tụọ ngwakọta mmiri / ciment / ájá ọkọlọtọ na NLD-3 cement mortar fluidity tester mgbe dayameta mgbasawanye bụ (180± 2) mm. ciment, ihe a tụrụ atụ nke mmiri oriri bụ 230g), wee gbakwunye onye na-ebelata mmiri nke oke ya bụ 1% nke ciment uka na mmiri, dị ka ciment/mmiri na-ebelata ihe / mmiri ọkọlọtọ / ájá ọkọlọtọ = 450g/4.5g/ 230 g/ A na-etinye nha nke 1350 g n'ime igwe na-agwakọta ụrọ simenti JJ-5 ma kpalie ya nke ọma, a na-atụkwa dayameta nke ngwa agha ahụ na igwe mmiri mmiri nke ngwa agha, nke bụ mmiri mmiri a tụrụ atụ.

2.3.3 Njirimara ngwaahịa

Ihe nlele ahụ bụ FT-IR na-eji ụdị EQUINOX 55 nke Fourier transform infrared spectrometer nke ụlọ ọrụ Bruker; H NMR ụdịdị dị iche iche nke sample e ji INOVA ZAB-HS plow superconducting nuclear magnetik resonance ngwá nke Varian Company; Ahụrụ ọdịdị nke ngwaahịa ahụ n'okpuru microscope; A na-eme nyocha XRD na nlele ahụ site na iji X-ray diffractometer nke MAC Company M18XHF22-SRA.

3. Nsonaazụ na mkparịta ụka

3.1 Nsonaazụ njirimara

3.1.1 FT-IR nsonaazụ njirimara

A na-eme nyocha infrared na akụrụngwa microcrystalline cellulose nwere ogo polymerization Dp=45 na ngwaahịa SBC mebere site na akụrụngwa a. Ebe ọ bụ na ọnụ ọgụgụ kachasị elu nke SC na SH adịghị ike, ha adịghị mma maka njirimara, ebe S = O nwere oke mmịpụta siri ike. Ya mere, ma enwere otu sulfonic acid n'ime usoro ihe omimi nwere ike ikpebi site n'ịkwado ịdị adị nke S=O elu. N'ụzọ doro anya, na cellulose spectrum, e nwere ike absorption ọnụ ọgụgụ kasị elu nke 3344 cm-1, nke a na-ekwu na hydroxyl na-agbatị vibration elu na cellulose; ọnụ ọgụgụ kachasị elu nke mmịpụta siri ike na ọnụ ọgụgụ ebili mmiri nke 2923 cm-1 bụ oke ịma jijiji na-agbatị nke methylene (-CH2). ọnụ ọgụgụ kasị elu nke ịma jijiji; usoro nke band nke mejupụtara 1031, 1051, 1114, na 1165cm-1 na-egosipụta ọnụ ọgụgụ kasị elu nke hydroxyl na-agbatị vibration na absorption elu nke ether bond (COC) na-ehulata vibration; nọmba ebili mmiri 1646cm-1 na-egosipụta hydrogen nke hydroxyl na mmiri efu kpụrụ ọnụ ọgụgụ kasị elu nke absorption nke njikọ; band nke 1432 ~ 1318cm-1 na-egosipụta ịdị adị nke cellulose crystal Ọdịdị. Na ụdịdị IR nke SBC, ike nke band 1432 ~ 1318cm-1 na-ebelata; ebe ịdị elu nke absorption kacha elu na 1653 cm-1 na-abawanye, na-egosi na ike ịmepụta njikọ hydrogen na-ewusi ike; 1040, 605cm-1 na-egosi ọnụ ọgụgụ kasị elu nke Absorption siri ike, na abụọ ndị a adịghị egosipụta na infrared spectrum nke cellulose, nke mbụ bụ njirimara absorption elu nke S = O bond, na nke ikpeazụ bụ njirimara absorption elu nke njikọ SO. Dabere na nyocha nke dị n'elu, enwere ike ịhụ na mgbe mmeghachi omume etherification nke cellulose gasịrị, e nwere otu sulfonic acid dị na agbụ molekụla ya.

3.1.2 H NMR nsonaazụ njirimara

H NMR ụdịdị dị iche iche nke cellulose butyl sulfonate nwere ike ịhụ: n'ime γ=1.74~2.92 bụ hydrogen proton chemical mgbanwe nke cyclobutyl, na n'ime γ=3.33~4.52 bụ cellulose anhydroglucose unit The chemical mgbanwe nke oxygen proton na γ=4.52 ~ 6 bụ mgbanwe kemịkalụ nke methylene proton na otu butylsulfonic acid jikọtara na oxygen, ọ nweghịkwa ọnụ ọgụgụ kasị elu na γ=6 ~ 7, na-egosi na ngwaahịa ahụ abụghị protons ndị ọzọ dị.

3.1.3 nsonaazụ njirimara SEM

Nyocha SEM nke cellulose owu pulp, microcrystalline cellulose na ngwaahịa cellulose butylsulfonate. Site n'ịtụle nsonaazụ nyocha SEM nke mkpụrụ osisi cellulose owu, microcrystalline cellulose na ngwaahịa cellulose butanesulfonate (SBC), achọpụtara na microcrystalline cellulose enwetara mgbe hydrolysis na HCL nwere ike gbanwee nhazi nke eriri cellulose. Ebibiri ihe owuwu fibrous, a na-enwetakwa ihe ndị dị mma agglomerated cellulose. SBC nwetara site n'ịmeghachi omume na BS enweghị ihe owuwu fibrous ma gbanwee n'ụzọ bụ isi ghọọ ihe amorphous, nke bara uru na mgbasa ya na mmiri.

3.1.4 XRD njiri mara

Kristalinity nke cellulose na ihe ndị sitere na ya na-ezo aka na pasentị nke mpaghara kristal nke usoro cellulose unit guzobere n'ozuzu ya. Mgbe cellulose na ihe ndị na-emepụta ya na-enweta mmeghachi omume kemịkalụ, a na-ebibi njikọ hydrogen dị na molecule na n'etiti ụmụ irighiri ihe, na mpaghara crystalline ga-aghọ mpaghara amorphous, si otú ahụ na-ebelata crystallinity. Ya mere, mgbanwe nke crystallinity tupu na mgbe mmeghachi omume bụ ihe atụ nke cellulose Otu n'ime njirisi isonye na nzaghachi ma ọ bụ na ọ bụghị. Emere nyocha XRD na microcrystalline cellulose na cellulose butanesulfonate ngwaahịa. Enwere ike ịhụ ya site n'iji ya tụnyere na mgbe etherification gasịrị, kristal na-agbanwe agbanwe, na ngwaahịa ahụ agbanweela kpamkpam n'ime usoro amorphous, nke mere na ọ ga-agbaze na mmiri.

3.2 Mmetụta nke ogo polymerization nke akụrụngwa na-ebelata mmiri nke ngwaahịa ahụ

Mmiri mmiri nke ngwa agha na-egosipụta kpọmkwem na-ebelata mmiri nke ngwaahịa ahụ, na ọdịnaya sọlfọ nke ngwaahịa ahụ bụ otu n'ime ihe ndị kachasị mkpa na-emetụta mmiri nke ngwa ngwa. Mmiri mmiri nke ngwa agha na-atụle ọrụ na-ebelata mmiri nke ngwaahịa ahụ.

Mgbe ịgbanwere ọnọdụ mmeghachi omume hydrolysis iji kwadebe MCC nwere ogo dị iche iche nke polymerization, dị ka usoro a dị n'elu, họrọ otu usoro njikọ iji kwadebe ngwaahịa SBC, tụọ ọdịnaya sọlfọ iji gbakọọ ogo nnọchi ngwaahịa, wee tinye ngwaahịa SBC na mmiri. /cement/usoro ngwakọta ájá ọkọlọtọ Tulee mmiri nke ngwa agha ahụ.

Enwere ike ịhụ ya site na nsonaazụ nnwale na n'ime nyocha nyocha, mgbe ogo polymerization nke microcrystalline cellulose raw material dị elu, ọdịnaya sọlfọ (nchịkọta nnọchi) nke ngwaahịa na mmiri mmiri nke ngwa agha dị ala. Nke a bụ n'ihi na: ịdị arọ molekụla nke ihe eji eme ihe dị ntakịrị, nke na-eme ka ngwakọta ahụ dị n'otu nke ihe eji eme ihe na ntinye nke onye na-ahụ maka etherification, si otú ahụ na-emeziwanye ogo nke etherification nke ngwaahịa ahụ. Agbanyeghị, ọnụego mbelata mmiri ngwaahịa anaghị ebili n'ahịrị kwụ ọtọ na mbelata ogo polymerization nke akụrụngwa. Nsonaazụ nnwale na-egosi na mmiri mmiri mmiri nke ciment ụrọ ngwakọta agwakọta na SBC kwadebere site na iji microcrystalline cellulose na ogo nke polymerization Dp<96 (molecular arọ <15552) karịrị 180 mm (nke dị ukwuu karịa nke na-enweghị mmiri reducer) . mmiri mmiri benchmark), na-egosi na enwere ike ịkwadebe SBC site na iji cellulose nwere ịdị arọ molekụla nke na-erughị 15552, na enwere ike nweta ụfọdụ mbelata mmiri; A na-akwado SBC site na iji microcrystalline cellulose na ogo nke polymerization nke 45 (molecular arọ: 7290), ma gbakwunye ya na ngwakọta ihe , mmiri a tụrụ atụ nke ngwa agha bụ nke kasị ukwuu, n'ihi ya, a na-ewere ya na cellulose nwere ogo polymerization. nke ihe dị ka 45 kachasị mma maka nkwadebe nke SBC; mgbe ogo nke polymerization nke akụrụngwa dị elu karịa 45, mmiri mmiri nke ngwa agha ji nwayọọ nwayọọ na-ebelata, nke pụtara na mmiri na-ebelata ọnụego. Nke a bụ n'ihi na mgbe molekụla arọ dị ukwuu, n'otu aka ahụ, viscosity nke usoro ngwakọta ga-abawanye, na dispersion uniformity nke ciment ga-akawanye njọ, na mgbasa na ihe ga-adị ngwa ngwa, nke ga-emetụta mgbasa mmetụta; n'aka nke ọzọ, mgbe molekụla arọ bụ nnukwu, The macromolecules nke superplasticizer na-na random eriri igwe conformation, nke dịtụ ike adsorb n'elu nke simenti irighiri. Ma mgbe ogo polymerization nke akụrụngwa dị ihe na-erughị 45, ọ bụ ezie na ọdịnaya sọlfọ (nchịkọta nnọchi) nke ngwaahịa ahụ dị ntakịrị, mmiri nke ngwakọta ngwa agha na-amalitekwa ibelata, ma mbelata dị ntakịrị. Ihe kpatara ya bụ na mgbe ịdị arọ nke molekụla nke mmiri na-ebelata mmiri dị ntakịrị, ọ bụ ezie na mgbasa ozi molekụla dị mfe ma nwee ezigbo wettability, ngwa ngwa adsorption nke molecule ahụ dị ukwuu karịa nke molecule, na mmiri na-ebugharị mmiri dị mkpụmkpụ. na esemokwu n'etiti ahụ bụ nnukwu, nke na-emerụ ihe. Mmetụta mgbasa ozi adịghị mma dị ka nke onye na-ebelata mmiri nke nwere ibu arọ molekụla buru ibu. Ya mere, ọ dị ezigbo mkpa ijikwa ịdị arọ molekụla nke ihu ezi (akụkụ cellulose) iji meziwanye arụmọrụ nke onye na-ebelata mmiri.

3.3 Mmetụta nke ọnọdụ mmeghachi omume na-ebelata mmiri nke ngwaahịa

A na-achọta ya site na nnwale na na mgbakwunye na ogo polymerization nke MCC, oke nke reactants, mmeghachi omume okpomọkụ, ịgbalite ngwa ngwa, oge njikọ ngwaahịa, na ụdị onye na-akwụsịtụ ihe niile na-emetụta ọrụ na-ebelata mmiri nke ngwaahịa ahụ.

3.3.1 Mmeghachi omume

(1) Usoro onunu ogwu nke BS

N'okpuru ọnọdụ nke usoro ndị ọzọ kpebisiri ike (ogo nke polymerization nke MCC bụ 45, n (MCC): n (NaOH) = 1: 2.1, onye na-emechi anya bụ isopropanol, oge ọrụ cellulose na ụlọ okpomọkụ bụ 2h, na Okpomọkụ njikọ bụ 80 Celsius C, yana njikọ oge 5h), iji nyochaa mmetụta nke ọnụọgụ etherification 1,4-butane sultone (BS) na ogo nnọchi nke otu butanesulfonic acid nke ngwaahịa na ịdị omimi nke ngwa agha.

Enwere ike ịhụ na ka ọnụọgụ BS na-abawanye, ogo ngbanwe nke otu butanesulfonic acid na mmiri nke ngwa agha na-abawanye nke ukwuu. Mgbe oke nke BS na MCC ruru 2.2: 1, mmiri mmiri nke DS na ngwa agha ruru oke. uru, a na-ewere na arụmọrụ na-ebelata mmiri bụ ihe kacha mma n'oge a. Uru BS gara n'ihu na-abawanye, ma ogo nke nnọchi na mmiri mmiri nke ngwa agha malitere ibelata. Nke a bụ n'ihi na mgbe BS karịrị oke, BS ga-emeghachi omume na NaOH iji mepụta HO- (CH2) 4SO3Na. Ya mere, akwụkwọ a na-ahọrọ ihe kachasị mma nke BS na MCC dịka 2.2: 1.

(2) Usoro onunu ogwu nke NaOH

N'okpuru ọnọdụ ndị ọzọ na-ekpebi usoro (n'ókè nke polymerization nke MCC bụ 45, n (BS): n (MCC) = 2.2: 1. Onye na-emechi anya bụ isopropanol, oge ọrụ cellulose na ụlọ okpomọkụ bụ 2h, na Okpomọkụ njikọ bụ 80 Celsius C, yana oge njikọ 5h), iji nyochaa mmetụta nke ọnụọgụ sodium hydroxide na ogo nnọchi nke otu butanesulfonic acid na ngwaahịa na mmiri mmiri nke ngwa agha.

Enwere ike ịhụ na, na mmụba nke ọnụ ọgụgụ mbelata, ogo nke nnọchi nke SBC na-abawanye ngwa ngwa, ma malite ibelata mgbe ọ nwetasịrị uru kachasị elu. Nke a bụ n'ihi na, mgbe ọdịnaya NaOH dị elu, enwere ọtụtụ ntọala n'efu na sistemụ ahụ, yana ohere nke mmeghachi omume n'akụkụ na-abawanye, na-eme ka ndị ọrụ etherification karịa (BS) na-ekere òkè na mmeghachi omume akụkụ, si otú ahụ belata ogo nke nnọchi nke sulfonic. otu acid dị na ngwaahịa. N'ebe okpomọkụ dị elu, ọnụnọ nke oke NaOH ga-emebikwa cellulose, na ọrụ na-ebelata mmiri nke ngwaahịa ahụ ga-emetụta na ọkwa dị ala nke polymerization. Dịka nsonaazụ nnwale ahụ si kwuo, mgbe ọnụọgụ nke NaOH na MCC dị ihe dịka 2.1, ogo ngbanwe bụ nke kachasị ukwuu, yabụ akwụkwọ a na-ekpebi na oke molar nke NaOH na MCC bụ 2.1: 1.0.

3.3.2 Mmetụta nke mmeghachi omume okpomọkụ na ngwaahịa na-ebelata arụmọrụ

N'okpuru ọnọdụ nke ndị ọzọ usoro parameters (n'ókè nke polymerization nke MCC bụ 45, n (MCC): n (NaOH): n (BS) = 1: 2.1: 2.2, onye nkwusioru gị n'ụlọnga bụ isopropanol, na ebighị oge. cellulose na ụlọ okpomọkụ bụ 2h. Oge 5), a na-enyocha mmetụta nke mmeghachi omume mmeghachi omume na ogo nke nnọchi nke otu butanesulfonic acid na ngwaahịa ahụ.

Enwere ike ịhụ na ka mmeghachi omume okpomọkụ na-abawanye, ogo sulfonic acid dochie anya DS nke SBC ji nwayọọ nwayọọ na-abawanye, ma mgbe mmeghachi omume okpomọkụ karịrị 80 Celsius C, DS na-egosi ọnọdụ ala. Mmeghachi omume etherification n'etiti 1,4-butane sultone na cellulose bụ mmeghachi omume endothermic, na ịba ụba nke mmeghachi omume okpomọkụ na-aba uru na mmeghachi omume n'etiti etherifying agent na cellulose hydroxyl otu, ma na mmụba nke okpomọkụ, mmetụta nke NaOH na cellulose ji nwayọọ nwayọọ na-abawanye. . Ọ na-esiwanye ike, na-eme ka cellulose daa ma daa, na-ebute mbelata nke ịdị arọ nke cellulose na ọgbọ nke obere sugar molecular. Mmeghachi omume nke obere ụmụ irighiri ihe dị otú ahụ na ndị na-eme ka etherifying dị mfe, a ga-erikwa ihe ndị ọzọ na-eme ka etherifying, na-emetụta ogo ngbanwe nke ngwaahịa ahụ. Ya mere, nke a tesis na-ewere na kasị adabara mmeghachi omume okpomọkụ maka etherification mmeghachi omume nke BS na cellulose bụ 80 ℃.

3.3.3 Mmetụta nke oge mmeghachi omume na ngwaahịa na-ebelata mmiri

A na-ekewa oge mmeghachi omume n'ime ime ụlọ okpomọkụ na-arụ ọrụ nke akụrụngwa na mgbe niile okpomọkụ njikọ oge ngwaahịa.

(1) Oge ntinye okpomọkụ nke ụlọ nke akụrụngwa

N'okpuru usoro kachasị mma n'elu (MCC ogo nke polymerization bụ 45, n (MCC): n (NaOH): n (BS) = 1: 2.1: 2.2, onye nkwusioru bụ isopropanol, mmeghachi omume mmeghachi omume okpomọkụ bụ 80 ° C, ngwaahịa ahụ. Ngwakọta okpomọkụ na-adịgide adịgide oge 5h), nyochaa mmetụta nke oge ịgbalite okpomọkụ ụlọ na ogo nke nnọchi nke butanesulfonic acid otu ngwaahịa.

Enwere ike ịhụ na ogo nnọchi nke otu butanesulfonic acid nke ngwaahịa SBC na-abawanye na mbụ wee belata site na ịgbatị oge ịgbalite. Ihe kpatara nyocha nwere ike ịbụ na mmụba nke oge ọrụ NaOH, mmebi nke cellulose dị njọ. Belata ịdị arọ nke cellulose ka ọ na-emepụta obere shuga molekụla. Mmeghachi omume nke obere ụmụ irighiri ihe dị otú ahụ na ndị na-eme ka etherifying dị mfe, a ga-erikwa ihe ndị ọzọ na-eme ka etherifying, na-emetụta ogo ngbanwe nke ngwaahịa ahụ. Ya mere, akwụkwọ a na-atụle na oge ịgbalite ụlọ okpomọkụ nke akụrụngwa bụ 2h.

(2) Oge nchịkọta ngwaahịa

N'okpuru usoro kachasị mma nke dị n'elu, a na-enyocha mmetụta nke oge ịgbalite n'ime ụlọ okpomọkụ na ogo nke nnọchi nke butanesulfonic acid otu ngwaahịa. Enwere ike ịhụ na site na ịgbatị oge mmeghachi omume ahụ, ogo nke nnọchi na-ebu ụzọ na-abawanye, ma mgbe oge mmeghachi omume ruru 5h, DS na-egosi ọnọdụ ala. Nke a metụtara ntọala efu dị na mmeghachi omume etherification nke cellulose. Na okpomọkụ dị elu, ịgbatị oge mmeghachi omume na-eduga n'ịbawanye ogo nke alkali hydrolysis nke cellulose, mbelata nke cellulose molecular chain, mbelata ịdị arọ nke ngwaahịa ahụ, na mmụba nke mmeghachi omume n'akụkụ, na-akpata ya. nnọchi. ogo na-ebelata. N'ime nnwale a, oge njikọ kacha mma bụ 5h.

3.3.4 Mmetụta nke ụdị onye na-egbochi ihe na-ebelata mmiri nke ngwaahịa ahụ

N'okpuru ezigbo usoro ọnọdụ (MCC polymerization ogo bụ 45, n (MCC): n (NaOH): n (BS) = 1: 2.1: 2.2, ebighị oge nke akụrụngwa na ụlọ okpomọkụ bụ 2h, mgbe niile okpomọkụ njikọ oge. nke ngwaahịa bụ 5h, na mmeghachi omume mmeghachi omume okpomọkụ 80 ℃), n'otu n'otu họrọ isopropanol, ethanol, n-butanol, ethyl acetate na mmanụ ala ether dị ka ndị na-akwụsịtụ, na-atụle mmetụta ha na mmiri na-ebelata arụmọrụ nke ngwaahịa.

N'ụzọ doro anya, a pụrụ iji isopropanol, n-butanol na ethyl acetate mee ihe dị ka onye na-akwụsịtụ na mmeghachi omume etherification a. Ọrụ nke onye na-akwụsịtụ, na mgbakwunye na ịgbasa ndị na-emegharị ihe, nwere ike ịchịkwa okpomọkụ mmeghachi omume. Isi ihe na-esi ísì ụtọ nke isopropanol bụ 82.3 Celsius C, yabụ a na-eji isopropanol dị ka onye na-akwụsịlata, enwere ike ịchịkwa ọnọdụ okpomọkụ nke usoro ahụ n'akụkụ ezigbo mmeghachi omume mmeghachi omume, yana ogo nke nnọchi nke otu butanesulfonic acid na ngwaahịa na mmiri mmiri. ngwa agha dị oke elu; ebe isi ihe na-esi ísì ụtọ nke ethanol dị oke ala, mmeghachi omume okpomọkụ adịghị emezu ihe ndị a chọrọ, ogo nke nnọchi nke otu butanesulfonic acid na ngwaahịa na mmiri mmiri nke ngwa agha dị ala; petroleum ether nwere ike isonye na mmeghachi omume ahụ, yabụ enweghị ike ịnweta ngwaahịa achụsasịrị.

4 Nkwubi okwu

(1) Iji pulp owu mee ihe dị ka akụrụngwa mbụ.microcrystalline cellulose (MCC)A kwadebere ogo dị mma nke polymerization, nke NaOH na-arụ ọrụ, ma meghachi omume na 1,4-butane sultone iji dozie mmiri-soluble butylsulfonic acid Cellulose ether, ya bụ, mmiri na-eme ka mmiri dị na cellulose. A na-akọwa usoro nke ngwaahịa ahụ, a chọpụtakwara na mgbe mmeghachi omume etherification nke cellulose gasịrị, e nwere otu sulfonic acid dị na ụdọ molekụla ya, nke gbanwere ghọọ usoro amorphous, na ngwaahịa mmiri na-ebelata mmiri nwere ezigbo mmiri solubility;

(2) Site na nyocha, a na-achọpụta na mgbe ogo polymerization nke microcrystalline cellulose bụ 45, ọrụ na-ebelata mmiri nke ngwaahịa enwetara bụ ihe kacha mma; n'okpuru ọnọdụ na ogo nke polymerization nke akụrụngwa kpebisiri ike, ruru nke reactants bụ n (MCC): n (NaOH): n ( BS) = 1: 2.1: 2.2, ebighị oge nke akụrụngwa na ụlọ okpomọkụ bụ. 2h, okpomọkụ njikọ ngwaahịa bụ 80 ° C, na oge njikọ bụ 5h. Ịrụ ọrụ mmiri kacha mma.