Mmeghachi omume etherification na cellulose ether

A na-enyocha ọrụ etherification nke cellulose site na igwe na-egweri na reactor na-akpali akpali n'otu n'otu, na chloroethanol na monochloroacetic acid kwadoro hydroxyethyl cellulose na carboxymethyl cellulose n'otu n'otu. Nsonaazụ gosiri na mmeghachi omume etherification nke cellulose mere site na mkpali reactor n'okpuru ọnọdụ nke oke mkpasu iwe. Cellulose nwere ezigbo etherification reactivity, nke dị mma karịa usoro kneader na-emeziwanye arụmọrụ etherification na ịkwalite nnyefe ọkụ nke ngwaahịa na ngwọta mmiri. ngwaahịa.

Isi okwu:mmeghachi omume etherification; Cellulose;Hydroxyethyl cellulose; Carboxymethyl cellulose

N'ime mmepe nke ngwaahịa ether cellulose owu a nụchara anụcha, a na-eji usoro ihe mgbaze eme ihe n'ọtụtụ ebe ma na-eji igwe kneading mee ihe dị ka ngwa mmeghachi omume. Agbanyeghị, cellulose owu bụ mpaghara kristal bụ ebe a na-ahazi ụmụ irighiri ihe nke ọma na nke ọma. Mgbe a na-eji igwe kneading mee ihe dị ka ngwa mmeghachi omume, ogwe aka nke na-eme ka ọkpụkpụ na-adị ngwa ngwa n'oge mmeghachi omume, na nguzogide nke etherifying na-abanye n'ụdị cellulose dị iche iche dị ukwuu ma na-agba ọsọ ngwa ngwa, na-akpata ogologo oge mmeghachi omume, akụkụ dị elu nke akụkụ. mmeghachi omume na nkesa na-ezighi ezi nke otu ndị nọchiri anya n'agbụ mkpụrụ ndụ cellulose.

Ọtụtụ mgbe mmeghachi omume etherification nke cellulose bụ mmeghachi omume dị iche iche n'èzí na n'ime. Ọ bụrụ na enweghị mpụta ike omume, etherifying gị n'ụlọnga siri ike ịbanye crystallization mpaghara nke cellulose. Na site na pretreatment nke a nụchara anụcha owu (dị ka iji anụ ahụ ụzọ dịkwuo elu nke nụchara anụcha owu), n'otu oge ahụ na-akpali akpali reactor maka mmeghachi omume akụrụngwa, na-eji ngwa ngwa akpali akpali etherification mmeghachi omume, dị ka echiche, cellulose ike ike ọzịza, ọzịza. nke mpaghara cellulose amorphous na mpaghara crystallization na-emekarị ka ọ bụrụ ihe na-agbanwe agbanwe, meziwanye ọrụ mmeghachi omume. Enwere ike nweta nkesa nkesa cellulose ether dị n'ụdị mmeghachi omume mmeghachi omume dị iche iche site n'ịbawanye ike mkpali mpụga. Ya mere, ọ ga-abụ ọdịnihu mmepe direction nke mba anyị ịzụlite elu àgwà cellulose etherification ngwaahịa na kpaliri ụdị mmeghachi omume kettle dị ka mmeghachi omume akụrụngwa.

1. Akụkụ nnwale

1.1 Ngwa igwe cellulose a nụchara anụcha maka nnwale

Dị ka ngwá ọrụ mmeghachi omume dị iche iche ejiri mee ihe na nnwale ahụ, ụzọ nhazi nke cellulose owu dị iche iche. Mgbe a na-eji kneader mee ihe dị ka ngwá ọrụ mmeghachi omume, ụzọ ndị a na-eme tupu ọgwụgwọ dị iche iche. Mgbe a na-eji kneader mee ihe dị ka ngwá ọrụ mmeghachi omume, crystallinity nke cellulose owu a nụchara anụcha eji bụ 43.9%, na nkezi ogologo nke cellulose owu a nụchara anụcha bụ 15 ~ 20mm. The crystallinity nke a nụchara anụcha cellulose owu bụ 32.3% na nkezi ogologo nke a nụchara anụcha cellulose owu bụ ihe na-erughị 1mm mgbe mkpali reactor na-eji dị ka mmeghachi omume akụrụngwa.

1.2 Mmepe nke carboxymethyl cellulose na hydroxyethyl cellulose

Enwere ike ime nkwadebe nke carboxymethyl cellulose na hydroxyethyl cellulose site na iji 2L kneader dị ka ngwa mmeghachi omume (nkezi ọsọ n'oge mmeghachi omume bụ 50r / min) na 2L na-akpali akpali dị ka ngwa mmeghachi omume (nkezi ọsọ n'oge mmeghachi omume bụ 500r / min).

N'oge mmeghachi omume ahụ, a na-enweta akụrụngwa niile sitere na mmeghachi omume ọnụọgụ. A na-asa ngwaahịa ahụ sitere na mmeghachi omume ahụ na w = 95% ethanol, wee kpoo ya site na agụụ maka 24h n'okpuru nrụgide na-adịghị mma nke 60 ℃ na 0.005mpa. Ọdịnaya mmiri nke ihe nlele enwetara bụ w = 2.7% ± 0.3%, a na-asachakwa ngwaahịa maka nyocha ruo mgbe ọdịnaya ash w <0.2%.

Usoro nkwadebe nke igwe igwakorita dị ka akụrụngwa mmeghachi omume bụ ndị a:

A na-eme mmeghachi omume etherification → ịsacha ngwaahịa → ihicha → grated grated → nkwakọ ngwaahịa na-eme na kneader.

The nkwadebe nzọụkwụ nke edemede reactor dị ka mmeghachi omume akụrụngwa bụ ndị a:

A na-eme mmeghachi omume etherification → ịsacha ngwaahịa → ihicha na granulation → nkwakọ ngwaahịa na-eme na reactor kpaliri.

Enwere ike ịhụ na a na-eji kneader mee ihe dị ka ngwá ọrụ mmeghachi omume maka nkwadebe nke njirimara nke obere mmeghachi omume mmeghachi omume, ihicha na ichikota granulation nzọụkwụ site na nzọụkwụ, na àgwà nke ngwaahịa ga-abụ nke ukwuu ibelata na-egweri usoro.

Njirimara nke usoro nkwadebe ya na reactor kpaliri dị ka akụrụngwa mmeghachi omume dị ka ndị a: arụmọrụ mmeghachi omume dị elu, granulation ngwaahịa anaghị anabata usoro usoro granulation omenala nke ihicha na ichikota, na ihicha na granulation usoro na-rụrụ n'otu oge. ngwaahịa ndị a na-amịghị amị mgbe ịsachara, na àgwà ngwaahịa na-anọgide na-agbanweghị na ihicha na granulation usoro.

1.3 X-ray diffraction analysis

A na-eme nyocha diffraction X-ray site na Rigaku D / max-3A X-ray diffractometer, graphite monochromator, Θ Angle bụ 8 ° ~ 30 °, CuKα ray, tube pressure na tube eruba bụ 30kV na 30mA.

1.4 Infrared spectrum analysis

Ejiri spectrum-2000PE FTIR infrared spectrometer mee ihe maka nyocha ụdịdị dị iche iche infrared. Nlereanya niile maka nyocha ụdịdị dị iche iche infrared nwere ibu nke 0.0020g. A na-ejikọta ihe atụ ndị a na 0.1600g KBr, n'otu n'otu, wee pịa (ya na ọkpụrụkpụ nke <0.8mm) ma nyochaa.

1.5 Nchọpụta nnyefe

Achọpụtara nnyefe ahụ site na 721 spectrophotometer. A na-etinye ngwọta CMC w=w1% n'ime efere 1cm colorimetric na 590nm wavelength.

1.6 ogo nchọpụta nnọchi

A tụrụ ogo nnọchi HEC nke hydroxyethyl cellulose site na usoro nyocha kemịkalụ ọkọlọtọ. Ụkpụrụ bụ na HEC nwere ike imebi ya site na HI hydroiodate na 123 ℃, na ogo nke nnọchi HEC nwere ike mara site n'ịtụ ihe ndị mebiri emebi ethylene na ethylene iodide emepụtara. Enwere ike ịnwale ogo nnọchi nke hydroxymethyl cellulose site na usoro nyocha kemịkalụ ọkọlọtọ.

2. Nsonaazụ na mkparịta ụka

A na-eji ụdị ọkụkọ abụọ dị iche iche eme ihe ebe a: otu bụ igwe na-egweri dị ka akụrụngwa mmeghachi omume, nke ọzọ na-akpali ụdị mmeghachi omume kettle dị ka akụrụngwa mmeghachi omume, na sistemu mmeghachi omume dị iche iche, ọnọdụ alkaline na sistemu ihe mgbaze mmiri, a na-amụ mmeghachi omume etherification nke cellulose a nụchara anụcha. N'ime ha, njirimara teknụzụ nke igwe kneading dị ka akụrụngwa mmeghachi omume bụ: N'ime mmeghachi omume, ngwa ngwa na-akụda ogwe aka na-adị ngwa ngwa, oge mmeghachi omume na-adị ogologo, akụkụ nke mmeghachi omume akụkụ dị elu, ọnụ ọgụgụ ojiji nke onye na-ahụ maka etherifying dị ala, na uniformity nke dochie otu nkesa na etherizing mmeghachi omume adịghị mma. Usoro nchọcha nwere ike ịbụ naanị na ọnọdụ mmeghachi omume dị warara dị warara. Na mgbakwunye, mgbanwe na njikwa nke ọnọdụ mmeghachi omume isi (dị ka bath ratio, alkali ịta, igwakota ngwa ngwa nke igwakorita igwe) dị nnọọ ogbenye. Ọ na-esiri ike iji nweta ihe dị ka otu mmeghachi omume etherification na iji mụọ oke nnyefe na ntinye nke usoro mmeghachi omume etherification na omimi. The usoro atụmatụ nke na-akpali akpali reactor dị ka mmeghachi omume akụrụngwa bụ: ngwa ngwa na-akpali ọsọ na mmeghachi omume, ngwa ngwa mmeghachi omume ọsọ, elu itinye n'ọrụ ọnụego nke etherizing gị n'ụlọnga, edo nkesa nke etherizing substituents, mgbanwe na controllable isi mmeghachi omume ọnọdụ.

A kwadebere Carboxymethyl cellulose CMC site na ngwa mmeghachi omume kneader na akụrụngwa mmeghachi omume na-akpali akpali n'otu n'otu. Mgbe a na-eji kneader mee ihe dị ka ngwa mmeghachi omume, ihe na-akpali akpali dị ala na nkezi ntụgharị ntụgharị bụ 50r / min. Mgbe eji reactor na-akpali akpali dị ka akụrụngwa mmeghachi omume, ike na-akpali akpali dị elu na nkezi ntụgharị ntụgharị bụ 500r / min. Mgbe oke molar nke monochloroacetic acid na cellulose monosaccharide bụ 1:5:1, oge mmeghachi omume bụ 1.5h na 68 ℃. Mbufe ọkụ nke CMC nwetara site na igwe igwakorita bụ 98.02% na arụmọrụ etherification bụ 72% n'ihi mma permeability nke CM na chloroacetic acid etherifying agent. Mgbe a na-eji reactor na-akpali akpali dị ka akụrụngwa mmeghachi omume, permeability nke onye na-ahụ maka etherifying dị mma, nnyefe nke CMC bụ 99.56%, na etherizing mmeghachi omume mmeghachi omume mụbara ruo 81%.

A kwadebere Hydroxyethyl cellulose HEC na kneader na reactor na-akpali akpali dị ka ngwa mmeghachi omume. Mgbe a na-eji kneader dị ka ngwa mmeghachi omume, mmeghachi omume mmeghachi omume nke onye na-ahụ maka etherizing bụ 47% na mmiri solubility adịghị mma mgbe permeability nke chloroethyl alcohol etherizing agent adịghị mma na molar ratio nke chloroethanol na cellulose monosaccharide bụ 3: 1 na 60 ℃ maka 4h. . Naanị mgbe oke nke chloroethanol na cellulose monosaccharides bụ 6: 1, enwere ike ịmepụta ngwaahịa ndị nwere ezigbo mmiri solubility. Mgbe a na-eji reactor na-akpali akpali dị ka ngwa mmeghachi omume, ikike nke chloroethyl mmanya etherification agent bịara ka mma na 68 ℃ maka 4h. Mgbe ọnụọgụ nke chloroethanol na cellulose monosaccharide bụ 3: 1, HEC na-esi na ya pụta nwere mmiri solubility ka mma, na mmeghachi omume etherification na-abawanye ruo 66%.

Nrụ ọrụ mmeghachi omume na ọsọ mmeghachi omume nke onye na-ahụ maka etherizing chloroacetic acid dị elu karịa nke chloroethanol, na ihe na-akpali akpali dị ka ngwa mmeghachi omume etherizing nwere uru doro anya karịa kneader, nke na-eme ka mmeghachi omume etherizing dịkwuo mma. The elu transmittivity nke CMC na-egosikwa na-apụtaghị ìhè na-akpali akpali reactor dị ka etherizing mmeghachi omume akụrụngwa nwere ike melite homogeneity nke etherizing mmeghachi omume. Nke a bụ n'ihi na agbụ cellulose nwere otu hydroxyl atọ na mgbanaka otu glucose ọ bụla, na naanị na ọnọdụ fụrụ akpụ ma ọ bụ gbazere ka a na-enweta ụzọ abụọ nke cellulose hydroxyl nke molecules etherifying. Mmeghachi omume etherification nke cellulose na-abụkarị mmeghachi omume dị iche iche site n'èzí gaa n'ime, karịsịa na mpaghara crystalline nke cellulose. Mgbe usoro kristal nke cellulose na-anọgide na-adịgide adịgide na-enweghị mmetụta nke ike mpụga, onye na-ahụ maka etherifying na-esiri ike ịbanye n'ụdị crystalline, na-emetụta ọdịdị nke mmeghachi omume dị iche iche. Ya mere, site n'ịkwado owu a nụchara anụcha (dịka ịbawanye elu nke owu a nụchara anụcha), enwere ike imeziwanye ọrụ nke owu a nụchara anụcha. Na nnukwu bath ratio (ethanol / cellulose ma ọ bụ isopropyl mmanya / cellulose na elu-ọsọ na-akpali akpali mmeghachi omume, dị ka echiche, usoro nke cellulose crystallization zone ga-ebelata, n'oge a cellulose nwere ike ịza, nke mere na ọzịza. nke mpaghara amorphous na crystalline cellulose na-emekarị ka ọ bụrụ ihe na-agbanwe agbanwe, Ya mere, mmeghachi omume nke mpaghara amorphous na mpaghara crystalline yiri ya.

Site na nyocha infrared spectrum analysis na X-ray diffraction analysis, usoro mmeghachi omume etherification nke cellulose nwere ike ịghọta nke ọma karịa mgbe a na-eji reactor na-akpali akpali dị ka ngwa mmeghachi omume etherification.

N'ebe a, a na-enyocha spectra infrared na X-ray diffraction spectra. Emere mmeghachi omume etherification nke CMC na HEC na reactor kpaliri n'okpuru ọnọdụ mmeghachi omume akọwara n'elu.

Nyocha nke infrared spectrum na-egosi na mmeghachi omume etheration nke CMC na HEC na-agbanwe mgbe nile na mgbatị nke oge mmeghachi omume, ogo nke nnọchi dị iche.

Site analysis nke X-ray diffraction ụkpụrụ, na crystallinity nke CMC na HEC nēche efu na ndọtị nke mmeghachi omume oge, na-egosi na decrystallisation usoro nwere ihu ọma e ghọtara na alkalization ogbo na kpo oku ogbo tupu etherification mmeghachi omume nke nụchara anụcha owu. . Ya mere, carboxymethyl na hydroxyethyl etherification reactivity nke owu a nụchara anụcha abụghịzi ihe mgbochi nke kristal nke owu a nụchara anụcha. Ọ na-metụtara permeability nke etherifying gị n'ụlọnga. Enwere ike igosi na a na-eme mmeghachi omume etherification nke CMC na HEC na reactor na-akpali akpali dị ka ngwá ọrụ mmeghachi omume. N'okpuru elu na-akpali akpali, ọ bara uru na decrystallization usoro nke nụchara anụcha owu na alkalization ogbo na kpo oku ogbo tupu etherification mmeghachi omume, na-enyere ndị etherification gị n'ụlọnga ka permeate n'ime cellulose, ka mma etherification mmeghachi omume arụmọrụ na nnọchi uniformity. .

N'ikpeazụ, ọmụmụ ihe a na-emesi mmetụta nke ike na-akpali akpali na ihe ndị ọzọ na mmeghachi omume mmeghachi omume n'oge usoro mmeghachi omume. Ya mere, amụma nke ọmụmụ a dabeere na ihe ndị na-esonụ: Na heterogeneous etheration mmeghachi omume usoro, ojiji nke nnukwu bath ruru na elu-akpali akpali ike, wdg, bụ isi ọnọdụ maka nkwadebe nke mkpokọta homogeneous cellulose ether na substituent otu. nkesa; Na a kpọmkwem heterogeneous etheration mmeghachi omume usoro, elu arụmọrụ cellulose ether na mkpokọta edo nkesa nke substituents nwere ike kwadebere site na iji akpali akpali reactor dị ka mmeghachi omume akụrụngwa, nke na-egosi na cellulose ether aqueous ngwọta nwere nnukwu transmittance, nke bụ nke dị oké mkpa iji gbasaa Njirimara. na ọrụ nke cellulose ether. A na-eji igwe igwakorita ihe dị ka akụrụngwa mmeghachi omume iji mụọ mmeghachi omume etherification nke owu a nụchara anụcha. N'ihi na obere akpali akpali ike, ọ dịghị mma maka penetration nke etherification gị n'ụlọnga, na nwere ụfọdụ ọghọm dị ka elu nkezi nke akụkụ Jeremaya mere na ogbenye nkesa uniformity nke etherification substituents.