Ukuhlanganiswa kweHydroxypropyl Methyl Cellulose Acetate kunye nePropionate

Ukusebenzisa i-hydroxypropyl methylcellulose (HPMC) njengento eluhlaza, i-acetic anhydride kunye nepropionic anhydride njengee-esterification agents, i-esterification reaction kwi-pyridine ilungiselele i-hydroxypropyl methylcellulose acetate kunye ne-hydroxypropyl methylcellulose Cellulose propionate. Ngokutshintsha inani le-solvent esetyenziswayo kwinkqubo, imveliso eneempawu ezingcono kunye neqondo lokutshintsha lifunyenwe. Idigri yokutshintshwa inqunywe yindlela yokulinganisa, kwaye imveliso ibonakaliswe kwaye ivavanyelwe ukusebenza. Iziphumo zabonisa ukuba inkqubo yokusabela yasabela kwi-110°I-C ye-1-2.5 h, kunye namanzi adibeneyo asetyenziswe njenge-agent ye-precipitating emva kokusabela, kunye neemveliso ze-powdery kunye ne-degree of substitution enkulu kune-1 (i-degree degree of substitution was 2) inokufumaneka. Inokunyibilika okulungileyo kwiintlobo ezahlukeneyo ze-solvents eziphilayo ezifana ne-ethyl ester, i-acetone, i-acetone / amanzi, njl.

Amagama angundoqo: ihydroxypropyl i-methylcellulose; i-hydroxypropyl methylcellulose acetate; ihydroxypropyl methylcellulose propionate

I-Hydroxypropylmethylcellulose (i-HPMC) yi-polymer engabonakaliyo ye-ionic kunye ne-ether ye-cellulose eneendlela ezininzi zokusetyenziswa. Njengesihlomelo sekhemikhali esigqwesileyo, i-HPMC isoloko isetyenziswa kwiinkalo ezahlukeneyo kwaye ibizwa ngokuba yi “industrial monosodium glutamate”. I-Hydroxypropyl methylcellulose (HPMC) ayinayo kuphela i-emulsifying efanelekileyo, ukuqina, kunye nemisebenzi yokubopha, kodwa ingasetyenziselwa ukugcina umswakama kunye nokukhusela i-colloids. Isetyenziswa kakhulu kwiinkalo ezininzi ezifana nokutya, amayeza, iingubo, iingubo kunye nezolimo. . Ukuguqulwa kwe-hydroxypropyl methylcellulose kunokutshintsha ezinye iimpawu zayo, ukwenzela ukuba isetyenziswe ngcono kwintsimi ethile. I-molecular formula ye-monomer yayo yi-C10H18O6.

Kwiminyaka yakutshanje, uphando kwi-hydroxypropyl methylcellulose derivatives ngokuthe ngcembe ibe yindawo eshushu. Ngokuguqula i-hydroxypropyl methylcellulose, iikhompawundi ezahlukeneyo ze-derivative ezineempawu ezahlukeneyo zinokufumaneka. Ngokomzekelo, ukuqaliswa kwamaqela e-acetyl kunokutshintsha ukuguquguquka kweefilimu zokugubungela zonyango.

Ukuguqulwa kwe-hydroxypropyl methylcellulose ngokuqhelekileyo kuqhutyelwa kubukho be-acid catalyst efana ne-concentrated sulfuric acid. Uvavanyo ludla ngokusebenzisa iacetic acid njengesinyibilikisi. Iimeko zokusabela zinzima kwaye zidla ixesha, kwaye imveliso ebangelwayo inezinga eliphantsi lokutshintshwa. (ngaphantsi kwe-1).

Kweli phepha, i-acetic anhydride kunye nepropionic anhydride zisetyenziswe njenge-esterification agents ukuguqula i-hydroxypropyl methylcellulose ukulungiselela i-hydroxypropyl methylcellulose acetate kunye ne-hydroxypropyl methylcellulose propionate. Ngokuphonononga iimeko ezifana nokukhethwa kwe-solvent (pyridine), i-solvent dosage, njl., Kuthenjwa ukuba imveliso eneempawu ezingcono kunye ne-substitution degree inokufumaneka ngendlela elula. Kulo phepha, ngophando lovavanyo, imveliso ekujoliswe kuyo kunye ne-powdery precipitate kunye ne-degree of substitution enkulu kune-1 ifunyenwe, enika isikhokelo esithile sethiyori yokuvelisa i-hydroxypropyl methylcellulose acetate kunye ne-hydroxypropyl methylcellulose propionate.

1. Inxalenye yovavanyo

1.1 Iimathiriyeli kunye nee-reagents

Ibakala le-Pharmaceutical hydroxypropyl methylcellulose (KIMA CHEMICAL CO.,LTD, 60HD100, i-methoxyl mass fraction 28% -30%, i-hydroxypropoxyl mass fraction 7% -12%); acetic anhydride, AR, Sinopharm Group Chemical Reagent Co., Ltd.; I-Propionic Anhydride, i-AR, i-West Asia Reagent; I-Pyridine, i-AR, i-Tianjin Kemiou Chemical Reagent Co., Ltd.; I-methanol, i-ethanol, i-ether, i-ethyl acetate, i-acetone, i-NaOH kunye ne-HCl zifumaneka ngokurhweba ngokuhlalutya okucocekileyo.

I-KDM thermostat yombane yokufudumeza ingubo yombane, isantya se-JJ-1A sokulinganisa idijithi yesibonisi sombane, i-NEXUS 670 i-Fourier iguqula i-infrared spectrometer.

1.2 Ukulungiswa kwe-hydroxypropyl methylcellulose acetate

Umlinganiselo othile we-pyridine wongezwa kwi-flask yentamo emithathu, kwaye emva koko i-2.5 g ye-hydroxypropyl methylcellulose yongezwa apho, i-reactants yaxutywa ngokulinganayo, kwaye iqondo lokushisa liphakanyiswe kwi-110.°C. Yongeza i-4 mL ye-acetic anhydride, uphendule kwi-110°C ngeyure eyi-1, yeka ukufudumeza, uphole kwiqondo lobushushu begumbi, yongeza inani elikhulu lamanzi adityanisiweyo ukuthoba imveliso, ukucoca ngokufunxa, hlamba ngamanzi adiyiweyo kangangezihlandlo ezininzi de i-eluate ingathathi hlangothi, kwaye uyomise imveliso yonga.

1.3 Ukulungiswa kwe-hydroxypropyl methylcellulose propionate

Umlinganiselo othile we-pyridine wongezwa kwi-flask enentamo ezintathu, kwaye emva koko i-0.5 g ye-hydroxypropyl methylcellulose yongezwa apho, i-reactants yaxutywa ngokulinganayo, kwaye iqondo lokushisa liphakanyiswe kwi-110.°C. Yongeza i-1.1 mL yepropionic anhydride, uphendule kwi-110°C kwi-2.5 h, ukuyeka ukufudumeza, ukupholisa kwiqondo lokushisa, ukongeza amanzi amaninzi ahlanjululweyo ukukhupha imveliso, ukucoca ngokufunxa, uhlambe ngamanzi adibeneyo amaxesha amaninzi de i-eluate yipropati ephakathi, gcina imveliso yomile.

1.4 Ukumiselwa kwe-infrared spectroscopy

I-hydroxypropyl methylcellulose, i-hydroxypropyl methylcellulose acetate, i-hydroxypropyl methylcellulose propionate kunye ne-KBr zaxutywa kwaye zaphantsi ngokulandelelana, kwaye emva koko zicinezelwe kwiipilisi ukuze zibone i-spectrum ye-infrared.

1.5 Ukumiselwa kweqondo lokutshintshwa

Lungiselela izisombululo ze-NaOH kunye ne-HCl nge-concentration ye-0.5 mol / L, kwaye uqhube ukulinganisa ukumisela ukugxininiswa okuchanekileyo; linganisa i-0.5 g ye-hydroxypropylmethylcellulose acetate (i-hydroxypropylmethylcellulose propionic acid ester) kwi-flask ye-Erlenmeyer eyi-250 mL, yongeza i-25 mL ye-acetone kunye namaconsi ama-3 esalathisi se-phenolphthalein, xuba kakuhle, uze udibanise i-25 mL ye-NaOH yesisombululo se-saponicre kunye ne-saponicify ye-electromagnetic stivating 2 h; i-titrate nge-HCI de kube umbala obomvu wesisombululo unyamalale, bhala Umthamo we-V1 (V2) we-hydrochloric acid esetyenzisiweyo; sebenzisa indlela efanayo yokulinganisa umthamo we-V0 we-hydrochloric acid esetyenziswe yi-hydroxypropyl methylcellulose, kwaye ubale iqondo lokutshintshwa.

1.6 Uvavanyo lokunyibilika

Thatha inani elifanelekileyo leemveliso zokwenziwa, zongeze kwi-solvent ye-organic, qhaqhazela kancinci, kwaye uqaphele ukuchithwa kwento.

2. Iziphumo kunye neNgxoxo

2.1 Isiphumo sesixa sepyridine (solvent)

Iziphumo zezixa ezahlukeneyo zepyridine kwi-morphology ye-hydroxypropylmethylcellulose acetate kunye ne-hydroxypropylmethylcellulose propionate. Xa isixa se-solvent sincinci, siya kunciphisa ukwanda kwe-macromolecular chain kunye ne-viscosity yenkqubo, ukwenzela ukuba i-degree of esterification ye-reaction system iya kuncitshiswa, kwaye imveliso iya kuhlanjululwa njengobunzima obukhulu. Kwaye xa isixa se-solvent sisezantsi kakhulu, i-reactant kulula ukujiya ibe yintlama kwaye ibambelele eludongeni lwesikhongozeli, nto leyo engalunganga kuphela xa kusenziwa ukusabela, kodwa kwakhona kubangela ukuphazamiseka okukhulu kunyango emva kokusabela. . Kwi-synthesis ye-hydroxypropyl methylcellulose acetate, inani le-solvent esetyenzisiweyo lingakhethwa njenge-150 mL / 2 g; kwi-synthesis ye-hydroxypropyl methylcellulose propionate, inokukhethwa njenge-80 mL / 0.5 g.

2.2 Uhlalutyo lwe-infrared spectrum

Itshathi yokuthelekisa i-infrared ye-hydroxypropyl methylcellulose kunye ne-hydroxypropyl methylcellulose acetate. Xa kuthelekiswa nezinto eziluhlaza, i-spectrogram ye-infrared yemveliso ye-hydroxypropyl methylcellulose acetate inotshintsho olucacileyo ngakumbi. Kwi-spectrum ye-infrared yemveliso, i-peak eqinile yabonakala kwi-1740cm-1, ebonisa ukuba iqela le-carbonyl laveliswa; ukongeza, ubuninzi be-vibration yokwelula i-OH kwi-3500cm-1 yayiphantsi kakhulu kuneyona nto iluhlaza, ekwabonisa ukuba -OH Kwakukho ukusabela.

I-spectrogram ye-infrared yemveliso ye-hydroxypropyl methylcellulose propionate nayo itshintshile kakhulu xa ithelekiswa nezinto eziluhlaza. Kwi-spectrum ye-infrared yemveliso, i-peak eqinile ibonakala kwi-1740 cm-1, ebonisa ukuba iqela le-carbonyl laveliswa; ukongeza, i-OH yokwelula i-vibration i-peak intensity kwi-3500 cm-1 yayingaphantsi kakhulu kunento ekrwada, ekwabonisa ukuba i-OH iphendule.

2.3 Ukumiselwa kweqondo lokutshintshwa

2.3.1 Ukumiselwa kweqondo lokuthatha indawo ye-hydroxypropyl methylcellulose acetate

Ekubeni i-hydroxypropyl methylcellulose ine-OH ezimbini kwiyunithi nganye, kunye ne-cellulose acetate yimveliso efunyenwe ngokutshintsha i-COCH3 enye ye-H kwi-OH enye, i-degree degree of substitution (Ds) yi-2.

2.3.2 Ukumiselwa kweqondo lokutshintshwa kwe-hydroxypropyl methylcellulose propionate

2.4 Ukunyibilika kwemveliso

Ezi zinto zimbini zenziwe zaneempawu zokunyibilika ezifanayo, kwaye i-hydroxypropyl methylcellulose acetate yayinyibilika kancinci kune-hydroxypropyl methylcellulose propionate. Imveliso eyenziweyo inokunyibilika kwi-acetone, i-ethyl acetate, i-acetone / i-solvent exutywe ngamanzi, kwaye inokukhethwa ngakumbi. Ukongezelela, umswakama oqulethwe kwi-acetone / i-solvent edibeneyo yamanzi inokwenza i-cellulose derivatives ikhuseleke ngakumbi kwaye ikhuseleke ngokusingqongileyo xa isetyenziswe njengezinto zokugqoka.

3. Isiphelo

(1) Iimeko ze-synthesis ye-hydroxypropyl methylcellulose acetate zilandelayo: 2.5 g ye-hydroxypropyl methylcellulose, i-acetic anhydride njenge-esterification agent, i-150 mL ye-pyridine njenge-solvent, iqondo lokushisa kwi-110° C, kunye nexesha lokuphendula 1 h.

(2) Iimeko ze-synthesis ye-hydroxypropyl methylcellulose acetate zezi: 0.5 g ye-hydroxypropyl methylcellulose, i-propionic anhydride njenge-esterification agent, i-80 mL ye-pyridine njenge-solvent, ubushushu bokuphendula kwi-110°C, kunye nexesha lokusabela yi-2 .5 h.

(3) I-derivatives ye-cellulose eyenziwe phantsi kwesi simo ngokuthe ngqo kwindlela yomgubo ocolekileyo kunye neqondo elihle lokutshintshwa, kwaye ezi zimbini ze-cellulose derivatives zinokuchithwa kwiintlobo ezahlukeneyo ze-solvents eziphilayo ezifana ne-ethyl acetate, i-acetone, kunye ne-acetone / amanzi.