Synthesis ya Hydroxypropyl Methyl Cellulose Acetate na Propionate

Ukoresheje hydroxypropyl methylcellulose (HPMC) nkibikoresho fatizo, anhydride ya acetike na anhydride ya protionic nka esterification agent, reaction ya esterification muri pyridine yateguye hydroxypropyl methylcellulose acetate na hydroxypropyl methylcellulose Cellulose propionate. Muguhindura ingano ya solvent yakoreshejwe muri sisitemu, ibicuruzwa bifite imitungo myiza nimpamyabumenyi yo gusimburwa byabonetse. Impamyabumenyi yo gusimburwa yagenwe nuburyo bwo gutanga titre, kandi ibicuruzwa byaranzwe kandi bipimwa kubikorwa. Ibisubizo byerekanaga ko sisitemu yo kwitwara yakiriwe kuri 110°C kuri 1-2.5 h, n'amazi ya deionisiyoneri yakoreshejwe nk'imvura igwa nyuma yo kubyitwaramo, kandi ibicuruzwa by'ifu bifite urwego rwo gusimbuza birenze 1 (urwego rwo hejuru rwo gusimbuza byari 2). Ifite ibisubizo byiza mumashanyarazi atandukanye nka Ethyl ester, acetone, acetone / amazi, nibindi.

Amagambo y'ingenzi: hydroxypropyl methylcellulose; hydroxypropyl methylcellulose acetate; hydroxypropyl methylcellulose propionate

Hydroxypropylmethylcellulose (HPMC) nikintu kitari ionic polymer hamwe na selulose ether hamwe nuburyo bwinshi bwo gukoresha. Nka chimique nziza cyane, HPMC ikoreshwa mubice bitandukanye kandi yitwa "inganda monosodium glutamate". Hydroxypropyl methylcellulose (HPMC) ntabwo ifite imikorere myiza ya emulisile, kubyimba, no guhuza, ariko kandi irashobora gukoreshwa mukubungabunga ubushuhe no kurinda colloide. Ikoreshwa cyane mubice byinshi nkibiryo, ubuvuzi, impuzu, imyenda, nubuhinzi. . Guhindura hydroxypropyl methylcellulose irashobora guhindura bimwe mubiranga, kugirango ikoreshwe neza mumurima runaka. Inzira ya molekuline ya monomer yayo ni C10H18O6.

Mu myaka yashize, ubushakashatsi kuri hydroxypropyl methylcellulose bukomoka buhoro buhoro bwabaye ahantu hashyushye. Muguhindura hydroxypropyl methylcellulose, ibice bitandukanye biva hamwe nibintu bitandukanye birashobora kuboneka. Kurugero, kumenyekanisha amatsinda ya acetyl birashobora guhindura imiterere ya firime yo kuvura.

Guhindura hydroxypropyl methylcellulose mubusanzwe bikorwa imbere ya catisale ya aside nka acide sulfurike yibanze. Ubushakashatsi busanzwe bukoresha aside ya asike nkumuti. Imiterere yimyitwarire iragoye kandi itwara igihe, kandi ibicuruzwa bivamo bifite urwego ruto rwo gusimburwa. (munsi ya 1).

Muri iyi nyandiko, anhydride ya acetike na anhydride ya protionic yakoreshejwe nkibikoresho bya esterification kugirango ihindure hydroxypropyl methylcellulose kugirango itegure hydroxypropyl methylcellulose acetate na hydroxypropyl methylcellulose propionate. Mugushakisha uko ibintu bimeze nko guhitamo ibishishwa (pyridine), ibipimo bya solvent, nibindi, twizeye ko ibicuruzwa bifite imitungo myiza nimpamyabumenyi yo gusimburwa bishobora kuboneka hakoreshejwe uburyo bworoshye. Muri iyi nyandiko, binyuze mubushakashatsi bwubushakashatsi, habonetse ibicuruzwa bigenewe imvura yifu n urugero rwo gusimbuza birenze 1 byabonetse, byatanze amabwiriza yubuyobozi bwo gukora hydroxypropyl methylcellulose acetate na hydroxypropyl methylcellulose propionate.

1. Igice cyubushakashatsi

1.1 Ibikoresho na reagent

Urwego rwa farumasi hydroxypropyl methylcellulose (KIMA CHEMICAL CO., LTD, 60HD100, agace ka metoxyl igice cya 28% -30%, agace ka hydroxypropoxyl 7% -12%); anhydride ya acetike, AR, Sinopharm Group Chemical Reagent Co., Ltd.; Anhydride ya Propionic, AR, Aziya y'Uburengerazuba Reagent; Pyridine, AR, Tianjin Kemiou Chemical Reagent Co, Ltd.; methanol, Ethanol, ether, Ethyl acetate, acetone, NaOH na HCl biraboneka mubucuruzi kubisesenguye neza.

KDM yubushyuhe bwo gushyushya amashanyarazi, JJ-1A umuvuduko wapima ibyuma byerekana amashanyarazi, NEXUS 670 Fourier ihindura infragre ya spekrometero.

1.2 Gutegura hydroxypropyl methylcellulose acetate

Umubare munini wa pyridine wongeyeho muri flask yamajosi atatu, hanyuma hongerwaho g 2,5 ya hydroxypropyl methylcellulose, reaction zabyutswe neza, ubushyuhe burazamuka bugera kuri 110°C. Ongeramo 4 mL ya anhydride ya acetike, reba kuri 110°C kuri 1 h, hagarika gushyushya, gukonjesha ubushyuhe bwicyumba, ongeramo amazi menshi ya deionion kugirango ugabanye ibicuruzwa, uyungurure hamwe na suction, woge hamwe namazi ya deionioni inshuro nyinshi kugeza igihe intore idafite aho ibogamiye, hanyuma wumishe ibicuruzwa bizigama.

1.3 Gutegura hydroxypropyl methylcellulose propionate

Umubare munini wa pyridine wongeyeho muri flask yamajosi atatu, hanyuma hongerwaho 0,5 g ya hydroxypropyl methylcellulose, reaction zabyutswe neza, ubushyuhe burazamuka bugera kuri 110°C. Ongeramo 1,1 mL ya anhydride ya propionic, reba kuri 110°C.

1.4 Kumenya infragre ya spekitroscopi

Hydroxypropyl methylcellulose, hydroxypropyl methylcellulose acetate, hydroxypropyl methylcellulose propionate na KBr byavanze nubutaka bikurikiranye, hanyuma bigakanda mubisate kugirango hamenyekane urwego rudasanzwe.

1.5 Kugena urwego rwo gusimburwa

Tegura ibisubizo bya NaOH na HCl hamwe na 0.5 mol / L, hanyuma ukore kalibrasi kugirango umenye neza neza; gupima 0,5 g ya hydroxypropylmethylcellulose acetate (hydroxypropylmethylcellulose propionic acide ester) muri flask ya 250 mL ya Erlenmeyer, ongeramo mL 25 ya acetone nigitonyanga 3 cyerekana ibimenyetso bya fenolphthalein, vanga neza, hanyuma ushyiremo mL 25 yumuti wa NaOH, ukangure na saponify kuri stirrer ya electronique. 2 h; titre hamwe na HCI kugeza ibara ritukura ryigisubizo kibuze, andika Ingano V1 (V2) ya aside hydrochloric yakoreshejwe; koresha uburyo bumwe bwo gupima ingano ya V0 ya acide hydrochloric ikoreshwa na hydroxypropyl methylcellulose, hanyuma ubare urwego rwo gusimburwa.

1.6 Ikigeragezo cyo gukemura

Fata urugero rukwiye rw'ibicuruzwa ngengabihe, ubyongereze ku musemburo wa organic, unyeganyeze gato, hanyuma urebe uko ibintu bigenda.

2. Ibisubizo n'ibiganiro

2.1 Ingaruka yubunini bwa pyridine (solvent)

Ingaruka zingana na pyridine kuri morphologie ya hydroxypropylmethylcellulose acetate na hydroxypropylmethylcellulose propionate. Iyo ingano ya solvent ari mike, bizagabanya kwaguka k'urunigi rwa macromolecular hamwe n'ubukonje bwa sisitemu, ku buryo urwego rwa esterifike ya sisitemu ya reaction ruzagabanuka, kandi ibicuruzwa bizagwa nk'imbaga nini. Kandi iyo ingano yumuti ari muke cyane, reaction iroroshye guhurira mukibumbano no kwizirika kurukuta rwa kontineri, ibyo ntibibangamire gusa ibyakozwe, ahubwo binatera ikibazo gikomeye kubuvuzi nyuma yo kubyitwaramo. . Muri synthesis ya hydroxypropyl methylcellulose acetate, ingano yumuti ukoreshwa irashobora gutoranywa nka 150 mL / 2 g; kuri synthesis ya hydroxypropyl methylcellulose propionate, irashobora gutoranywa nka 80 mL / 0.5 g.

2.2 Isesengura ridafite ishingiro

Imbonerahamwe yo kugereranya ya hydroxypropyl methylcellulose na hydroxypropyl methylcellulose acetate. Ugereranije nibikoresho fatizo, infragre ya spekrogramu yibicuruzwa hydroxypropyl methylcellulose acetate ifite impinduka zigaragara. Muri infrarafarike yibicuruzwa, impinga ikomeye yagaragaye kuri 1740cm-1, byerekana ko hakozwe itsinda rya karubone; hiyongereyeho, ubukana bwimisemburo irambuye ya OH kuri 3500cm-1 yari hasi cyane ugereranije n’ibikoresho fatizo, byanagaragaje ko -OH Hariho reaction.

Infragre ya spekrogramu yibicuruzwa hydroxypropyl methylcellulose propionate nayo yarahindutse cyane ugereranije nibikoresho fatizo. Muri infrarafarike yibicuruzwa, impinga ikomeye yagaragaye kuri cm 1740 cm-1, byerekana ko hakozwe itsinda rya karubone; hiyongereyeho, OH irambura ubukana bwa OH kuri cm 3500 cm-1 yari hasi cyane ugereranije n’ibikoresho fatizo, byanagaragaje ko OH yabyitwayemo.

2.3 Kugena urwego rwo gusimburwa

2.3.1 Kugena urwego rwo gusimbuza hydroxypropyl methylcellulose acetate

Kubera ko hydroxypropyl methylcellulose ifite OH ebyiri imwe muri buri gice, na acetate ya selile ni igicuruzwa cyabonetse mugusimbuza COCH3 imwe kuri H muri OH imwe, urwego ntarengwa rwo gusimbuza (Ds) ni 2.

2.3.2 Kugena urwego rwo gusimbuza hydroxypropyl methylcellulose propionate

2.4 Gukemura ibicuruzwa

Ibintu byombi byakoreshwaga byari bifite imiterere isa na solubilité, kandi hydroxypropyl methylcellulose acetate yashonga gato ugereranije na hydroxypropyl methylcellulose propionate. Igicuruzwa cyogukora gishobora gushonga muri acetone, Ethyl acetate, acetone / amazi avanze na solvent, kandi ikagira amahitamo menshi. Byongeye kandi, ubuhehere buri muri acetone / amazi avanze yumuti burashobora gutuma ibikomoka kuri selile birinda umutekano kandi bitangiza ibidukikije iyo bikoreshejwe nkibikoresho.

3. Umwanzuro

.° C, nigihe cyo kubyitwaramo 1 h.

.°C, nigihe cyo kwitwara cya 2 .5 h.

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