Njikọ nke Hydroxypropyl Methyl Cellulose Acetate na Propionate

Iji hydroxypropyl methylcellulose (HPMC) dị ka akụrụngwa, acetic anhydride na propionic anhydride dị ka esterification ihe, mmeghachi omume esterification na pyridine kwadebere hydroxypropyl methylcellulose acetate na hydroxypropyl methylcellulose Cellulose propionate. Site n'ịgbanwe ọnụọgụ ihe mgbaze ejiri na sistemụ ahụ, a nwetara ngwaahịa nwere njirimara ka mma na ogo nnọchi. Ekpebiri ogo nnọchi anya site na usoro titration, yana ngwaahịa a mara ma nwalee maka ịrụ ọrụ. Nsonaazụ gosiri na mmeghachi omume mmeghachi omume na 110°C maka 1-2.5 h, na mmiri deionized na-eji dị ka onye na-emepụta ihe na-emepụta ihe mgbe mmeghachi omume ahụ gasịrị, na ngwaahịa powdery nwere ogo nke nnọchi karịa 1 (nhazi usoro mgbanwe bụ 2). Ọ nwere ezigbo solubility dị iche iche organic mgbaze dị ka ethyl ester, acetone, acetone / mmiri, wdg.

Isi okwu: hydroxypropyl methylcellulose; hydroxypropyl methylcellulose acetate; hydroxypropyl methylcellulose propionate

Hydroxypropylmethylcellulose (HPMC) bụ ngwakọta polymer na-abụghị ionic yana ether cellulose nwere ọtụtụ ojiji. Dị ka ihe mgbakwunye kemịkalụ magburu onwe ya, a na-ejikarị HPMC eme ihe n'ọhịa dị iche iche, a na-akpọkwa ya "monosodium glutamate ụlọ ọrụ". Hydroxypropyl methylcellulose (HPMC) ọ bụghị naanị na ọ nwere ezigbo emulsifying, thickening, and bonding function, kamakwa enwere ike iji ya mee ka mmiri dịgide ma chebe colloid. A na-eji ya n'ọtụtụ ebe dị ka nri, ọgwụ, mkpuchi, textiles na ọrụ ugbo. . Mgbanwe nke hydroxypropyl methylcellulose nwere ike ịgbanwe ụfọdụ n'ime ihe onwunwe ya, ka e wee nwee ike iji ya mee ihe nke ọma na mpaghara ụfọdụ. Usoro ihe omimi nke monomer ya bụ C10H18O6.

N'ime afọ ndị na-adịbeghị anya, nchọpụta banyere ihe mmepụta hydroxypropyl methylcellulose ejirila nwayọọ nwayọọ ghọọ ebe na-ekpo ọkụ. Site n'ịgbanwe hydroxypropyl methylcellulose, enwere ike nweta ogige dị iche iche nwere ihe dị iche iche. Dịka ọmụmaatụ, iwebata otu acetyl nwere ike gbanwee mgbanwe nke ihe nkiri mkpuchi ahụike.

A na-eme mgbanwe nke hydroxypropyl methylcellulose na ọnụnọ nke ihe na-eme ka acid dị ka sulfuric acid gbanyere mkpọrọgwụ. Nnwale ahụ na-ejikarị acetic acid dị ka ihe mgbaze. Ọnọdụ mmeghachi omume dị njọ ma na-ewe oge, na ngwaahịa na-esi na ya nwere obere ngbanwe nke mgbanwe. (ihe na-erughị 1).

N'ime akwụkwọ a, a na-eji acetic anhydride na propionic anhydride mee ihe dị ka ihe esterification iji gbanwee hydroxypropyl methylcellulose iji kwadebe hydroxypropyl methylcellulose acetate na hydroxypropyl methylcellulose propionate. Site n'inyocha ọnọdụ dị ka mgbaze nhọrọ (pyridine), ihe mgbaze usoro, wdg, a na-atụ anya na ngwaahịa nwere mma Njirimara na nnọchi n'ókè nwere ike nweta site a dịtụ mfe usoro. N'ime akwụkwọ a, site na nyocha nyocha, a na-enweta ngwaahịa a na-atụ anya ya na ntụ ntụ ntụ na ogo nke nnọchi karịa 1, nke nyere ụfọdụ ntuziaka usoro maka mmepụta nke hydroxypropyl methylcellulose acetate na hydroxypropyl methylcellulose propionate.

1. Akụkụ nnwale

1.1 Akụrụngwa na reagents

Pharmaceutical ọkwa hydroxypropyl methylcellulose (KIMA CHEMICAL CO., LTD, 60HD100, methoxyl uka ntakiri 28%-30%, hydroxypropoxyl uka akụkụ 7%-12%); acetic anhydride, AR, Sinopharm Group Chemical Reagent Co., Ltd .; Propionic Anhydride, AR, West Asia Reagent; Pyridine, AR, Tianjin Kemiou Chemical Reagent Co., Ltd.; methanol, ethanol, ether, ethyl acetate, acetone, NaOH na HCl dị na azụmaahịa dị ọcha.

Igwe ọkụ ọkụ ọkụ KDM KDM, JJ-1A na-atụ ọsọ ọsọ dijitalụ ihe ngosi ọkụ eletrik, NEXUS 670 Fourier na-agbanwe spectrometer infrared.

1.2 Nkwadebe nke hydroxypropyl methylcellulose acetate

A na-etinye pyridine ụfọdụ n'ime ite olu atọ ahụ, wee tinye 2.5 g nke hydroxypropyl methylcellulose na ya, a na-emegharị ndị na-emegharị ahụ nke ọma, ma mee ka okpomọkụ dị elu ruo 110.°C. Tinye 4 ml nke acetic anhydride, meghachi omume na 110°C maka 1 h, kwụsị ikpo ọkụ, dị jụụ n'ime ụlọ, gbakwunye nnukwu mmiri deionized iji mee ka ngwaahịa ahụ dị elu, nyochaa ya na mmiri ara ehi, na-asa ya na mmiri deionized ruo ọtụtụ oge ruo mgbe eluate na-anọpụ iche, ma kpoo ngwaahịa ahụ.

1.3 Nkwadebe nke hydroxypropyl methylcellulose propionate

A na-etinye pyridine ụfọdụ n'ime flask olu atọ ahụ, wee tinye 0,5 g hydroxypropyl methylcellulose na ya, a na-emegharị ihe ndị na-emegharị ahụ nke ọma, na okpomọkụ dị elu ruo 110.°C. Tinye 1.1 ml nke propionic anhydride, meghachi omume na 110°C maka awa 2.5, kwụsị ikpo ọkụ, dị jụụ na ụlọ okpomọkụ, gbakwunye nnukwu mmiri mmiri na-ekpo ọkụ iji mee ka ngwaahịa ahụ dị elu, nyochaa ya na mmiri ara ehi, na-asa ya na mmiri na-ekpo ọkụ ruo ọtụtụ oge ruo mgbe eluate bụ ihe onwunwe nke ọkara, chekwaa ngwaahịa ahụ.

1.4 Mkpebi nke infrared spectroscopy

A gwakọtara hydroxypropyl methylcellulose, hydroxypropyl methylcellulose acetate, hydroxypropyl methylcellulose propionate na KBr na ala n'otu n'otu, wee pịa ya na mbadamba nkume iji chọpụta ụdịdị infrared.

1.5 Mkpebi nke ogo nnọchi anya

Kwadebe ngwọta NaOH na HCl na ntinye nke 0.5 mol / L, ma mee nhazi nhazi iji chọpụta kpọmkwem ntinye uche; tụọ 0.5 g nke hydroxypropylmethylcellulose acetate (hydroxypropylmethylcellulose propionic acid ester) na 250 ml Erlenmeyer flask, tinye 25 ml nke acetone na 3 tụlee nke phenolphthalein egosi, mix ọma, wee tinye 25 mL nke NaOH ngwọta na electromagnetic. 2 h; titrate na HCI ruo mgbe agba uhie nke ngwọta na-apụ n'anya, dekọọ olu V1 (V2) nke hydrochloric acid riri; jiri otu usoro tụọ olu V0 nke hydrochloric acid nke hydroxypropyl methylcellulose na-eri, wee gbakọọ ogo nnọchi.

1.6 Nnwale solubility

Were ngwaahịa sịntetịt kwesịrị ekwesị, tinye ya na ihe mgbaze organic, maa jijiji ntakịrị, wee hụ nhụsianya nke ihe ahụ.

2. Nsonaazụ na mkparịta ụka

2.1 Mmetụta nke ọnụọgụ pyridine (ihe mgbaze)

Mmetụta dị iche iche nke pyridine na morphology nke hydroxypropylmethylcellulose acetate na hydroxypropylmethylcellulose propionate. Mgbe ọnụ ọgụgụ nke ihe mgbaze na-adị ntakịrị, ọ ga-ebelata mmepụta nke agbụ macromolecular na viscosity nke usoro ahụ, nke mere na a ga-ebelata ogo nke esterification nke usoro mmeghachi omume, na ngwaahịa ahụ ga-ebuli dị ka nnukwu uka. Na mgbe ọnụ ọgụgụ nke ihe mgbaze dị oke ala, onye na-emeghachi omume na-adị mfe ịbanye n'ime akpụ ma na-arapara n'ahụ mgbidi nke akpa ahụ, nke na-abụghị nanị na-adịghị mma maka ịmepụta mmeghachi omume ahụ, kamakwa na-akpata nnukwu nsogbu na ọgwụgwọ mgbe mmeghachi omume ahụ gasịrị. . Na njikọ nke hydroxypropyl methylcellulose acetate, ọnụ ọgụgụ nke ihe mgbaze e ji mee ihe nwere ike ịhọrọ dị ka 150 mL / 2 g; maka njikọ nke hydroxypropyl methylcellulose propionate, enwere ike ịhọrọ ya dị ka 80 ml / 0.5 g.

2.2 Infrared spectrum analysis

Chaatị ntụnyere infrared nke hydroxypropyl methylcellulose na hydroxypropyl methylcellulose acetate. E jiri ya tụnyere akụrụngwa, infrared spectrogram nke ngwaahịa hydroxypropyl methylcellulose acetate nwere mgbanwe doro anya karị. Na ụdị infrared nke ngwaahịa ahụ, ọnụ ọgụgụ siri ike pụtara na 1740cm-1, na-egosi na e mepụtara otu carbonyl; Tụkwasị na nke ahụ, ike nke na-agbatị elu vibration nke OH na 3500cm-1 dị nnọọ ala karịa nke akụrụngwa, nke gosikwara na -OH Enwere mmeghachi omume.

spectrogram infrared nke ngwaahịa hydroxypropyl methylcellulose propionate agbanweela nke ukwuu ma e jiri ya tụnyere akụrụngwa. Na ụdị infrared nke ngwaahịa ahụ, ọnụ ọgụgụ siri ike pụtara na 1740 cm-1, na-egosi na e mepụtara otu carbonyl; na mgbakwunye, OH na-agbatị oke ịma jijiji na 3500 cm-1 dị obere karịa nke akụrụngwa, nke gosikwara na OH meghachiri omume.

2.3 Mkpebi nke ogo nnọchi anya

2.3.1 Mkpebi nke nnọchi nnọchi nke hydroxypropyl methylcellulose acetate

Ebe hydroxypropyl methylcellulose nwere OH abụọ na nkeji nke ọ bụla, na cellulose acetate bụ ngwaahịa enwetara site n'ịgbanwe otu COCH3 maka H n'otu OH, usoro nhazi kachasị nke nnọchi (Ds) bụ 2.

2.3.2 Mkpebi nke ngbanwe nke hydroxypropyl methylcellulose propionate.

2.4 Solubility nke ngwaahịa

Ihe abụọ ahụ ejikọtara nwere ụdị solubility yiri nke ahụ, na hydroxypropyl methylcellulose acetate dị ntakịrị soluble karịa hydroxypropyl methylcellulose propionate. Enwere ike ịgbaze ngwaahịa sịntetik na acetone, ethyl acetate, acetone/mmiri agwakọta ihe mgbaze, ma nwee nhọrọ karịa. Na mgbakwunye, mmiri dị n'ime acetone / mmiri agwakọta ihe mgbaze nwere ike ime ka mkpụrụ ndụ cellulose dịkwuo mma na gburugburu ebe obibi mgbe ejiri ya dị ka ihe mkpuchi.

3. Nkwubi okwu

(1) Ọnọdụ njikọ nke hydroxypropyl methylcellulose acetate bụ ndị a: 2.5 g nke hydroxypropyl methylcellulose, acetic anhydride dị ka esterification, 150 ml nke pyridine dị ka ihe mgbaze, mmeghachi omume okpomọkụ na 110.° C, na oge mmeghachi omume 1 h.

(2) Ọnọdụ njikọ nke hydroxypropyl methylcellulose acetate bụ: 0.5 g nke hydroxypropyl methylcellulose, propionic anhydride dị ka esterification ihe, 80 ml nke pyridine dị ka ihe mgbaze, mmeghachi omume okpomọkụ na 110.°C, na oge mmeghachi omume nke 2.5 h.

(3) Ihe ndị na-emepụta cellulose nke a na-emepụta n'okpuru ọnọdụ a bụ kpọmkwem n'ụdị ntụ ntụ dị mma nke nwere ezigbo ngbanwe, na ihe abụọ a na-emepụta cellulose nwere ike ịgbaze n'ụdị ihe mgbaze dị iche iche dị ka ethyl acetate, acetone, na acetone / mmiri.