Kaphatikizidwe ka Hydroxypropyl Methyl Cellulose Acetate ndi Propionate

Pogwiritsa ntchito hydroxypropyl methylcellulose (HPMC) ngati zopangira, acetic anhydride ndi propionic anhydride monga esterification agents, esterification reaction mu pyridine inakonza hydroxypropyl methylcellulose acetate ndi hydroxypropyl methylcellulose Cellulose propionate. Posintha kuchuluka kwa zosungunulira zomwe zimagwiritsidwa ntchito m'dongosolo, chinthu chokhala ndi katundu wabwino komanso digirii yolowa m'malo chinapezedwa. Digiri yolowa m'malo idatsimikiziridwa ndi njira ya titration, ndipo mankhwalawo adadziwika ndikuyesedwa kuti agwire ntchito. Zotsatira zake zidawonetsa kuti ma reaction system adachita pa 110°C kwa 1-2.5 h, ndi madzi deionized ankagwiritsidwa ntchito precipitating wothandizira pambuyo anachita, ndi powdery mankhwala ndi digiri ya m'malo wamkulu kuposa 1 (ongoyerekeza digiri ya m'malo anali 2) akanatha anapezedwa. Ili ndi kusungunuka kwabwino mu zosungunulira zosiyanasiyana organic monga ethyl ester, acetone, acetone/madzi, etc.

Mawu ofunikira: hydroxypropyl methylcellulose; hydroxypropyl methylcellulose acetate; hydroxypropyl methylcellulose propionate

Hydroxypropylmethylcellulose (HPMC) ndi gulu lopanda ionic polima komanso cellulose ether yokhala ndi ntchito zambiri. Monga chowonjezera chamankhwala, HPMC imagwiritsidwa ntchito nthawi zambiri m'magawo osiyanasiyana ndipo imatchedwa "industrial monosodium glutamate". Hydroxypropyl methylcellulose (HPMC) sikuti imangokhala ndi emulsifying, thickening, ndi kumanga ntchito zabwino, komanso ingagwiritsidwe ntchito kusunga chinyezi ndi kuteteza colloids. Amagwiritsidwa ntchito kwambiri m'magawo ambiri monga chakudya, mankhwala, zokutira, nsalu, ndi ulimi. . Kusintha kwa hydroxypropyl methylcellulose kumatha kusintha zina mwazinthu zake, kuti zitha kugwiritsidwa ntchito bwino m'munda wina. Mapangidwe a maselo a monoma yake ndi C10H18O6.

M'zaka zaposachedwa, kafukufuku wokhudzana ndi zotumphukira za hydroxypropyl methylcellulose pang'onopang'ono wakhala malo otentha. Posintha hydroxypropyl methylcellulose, mitundu yosiyanasiyana yochokera kuzinthu zosiyanasiyana imatha kupezeka. Mwachitsanzo, kuyambitsidwa kwa magulu a acetyl kungasinthe kusinthasintha kwa mafilimu opaka mankhwala.

Kusintha kwa hydroxypropyl methylcellulose nthawi zambiri kumachitika pamaso pa chothandizira cha asidi monga sulfuric acid. Kuyeserako nthawi zambiri kumagwiritsa ntchito acetic acid ngati zosungunulira. Zomwe zimachitika zimakhala zovuta komanso zimawononga nthawi, ndipo zotsatira zake zimakhala zochepa kwambiri m'malo. (osakwana 1).

Mu pepalali, acetic anhydride ndi propionic anhydride anagwiritsidwa ntchito ngati esterification agents kuti asinthe hydroxypropyl methylcellulose kukonzekera hydroxypropyl methylcellulose acetate ndi hydroxypropyl methylcellulose propionate. Pofufuza zinthu monga kusankha zosungunulira (pyridine), zosungunulira mlingo, etc., tikuyembekeza kuti mankhwala ndi katundu wabwinoko ndi digiri m'malo angapezeke mwa njira yosavuta. Mu pepalali, kupyolera mu kafukufuku woyesera, chinthu chomwe chapangidwira chokhala ndi powdery precipitate ndi digiri ya kusintha kwakukulu kuposa 1 inapezedwa, yomwe inapereka malangizo ena okhudza kupanga hydroxypropyl methylcellulose acetate ndi hydroxypropyl methylcellulose propionate.

1. Gawo loyesera

1.1 Zipangizo ndi ma reagents

Pharmaceutical grade hydroxypropyl methylcellulose (KIMA CHEMICAL CO.,LTD, 60HD100, methoxyl mass fraction 28% -30%, hydroxypropoxyl mass fraction 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 ndi HCl ndizomwe zimapezeka pamalonda poyera.

KDM thermostat choyatsira magetsi chotenthetsera, JJ-1A liwiro la kuyeza chiwonetsero chamagetsi chowonetsa magetsi, NEXUS 670 Fourier amasintha ma infrared spectrometer.

1.2 Kukonzekera kwa hydroxypropyl methylcellulose acetate

Kuchuluka kwa pyridine kunawonjezeredwa mu botolo la khosi lachitatu, ndiyeno 2.5 g ya hydroxypropyl methylcellulose inawonjezeredwa pamenepo, zowonongeka zinagwedezeka mofanana, ndipo kutentha kunakwezedwa ku 110.°C. Onjezani 4 mL ya acetic anhydride, ikani pa 110°C kwa 1 h, siyani kutenthetsa, kuzizira mpaka kutentha, onjezerani madzi ochulukirapo kuti muchepetse mankhwalawo, fyuluta ndi kuyamwa, sambani ndi madzi osakanizidwa kangapo mpaka madziwo salowerera ndale, ndikuumitsa mankhwalawo.

1.3 Kukonzekera kwa hydroxypropyl methylcellulose propionate

Kuchuluka kwa pyridine kunawonjezeredwa mu botolo la makosi atatu, ndiyeno 0,5 g ya hydroxypropyl methylcellulose inawonjezeredwa pamenepo, zosakanizazo zinagwedezeka mofanana, ndipo kutentha kunakwezedwa mpaka 110.°C. Onjezani 1.1 mL ya propionic anhydride, itani pa 110°C kwa 2.5 h, siyani Kutentha, kuzizira mpaka kutentha, onjezerani madzi ochulukirapo kuti muchepetse mankhwalawo, fyuluta ndi kuyamwa, kusamba ndi madzi opangidwa ndi deionized kangapo mpaka loate ndi katundu wapakati, sungani mankhwalawo mouma.

1.4 Kutsimikiza kwa infrared spectroscopy

Ma hydroxypropyl methylcellulose, hydroxypropyl methylcellulose acetate, hydroxypropyl methylcellulose propionate ndi KBr adasakanizidwa ndikugwa motsatana, kenako adakanikizidwa m'mapiritsi kuti adziwe mawonekedwe a infrared.

1.5 Kutsimikiza kwa digiri yolowa m'malo

Konzani mayankho a NaOH ndi HCl okhala ndi 0.5 mol / L, ndikuyesa kuyesa kuti mudziwe kuchuluka kwake; kulemera 0.5 g wa hydroxypropylmethylcellulose acetate (hydroxypropylmethylcellulose propionic acid ester) mu 250 mL Erlenmeyer botolo, kuwonjezera 25 mL acetone ndi 3 madontho phenolphthalein chizindikiro, sakanizani bwino, kenaka onjezerani 25 mL wa NaOH maginito chipwirikiti chipwirikiti ndi electromagnetic kusonkhezera. 2 h; titrate ndi HCI mpaka mtundu wofiira wa yankho utatha, lembani Voliyumu V1 (V2) ya hydrochloric acid yomwe yadyedwa; gwiritsani ntchito njira yomweyo kuyeza voliyumu V0 ya hydrochloric acid yomwe imadyedwa ndi hydroxypropyl methylcellulose, ndikuwerengera kuchuluka kwa m'malo.

1.6 Kuyesa kwa Solubility

Tengani kuchuluka koyenera kwa zinthu zopangidwa, onjezerani ku zosungunulira za organic, gwedezani pang'ono, ndikuwona kusungunuka kwa chinthucho.

2. Zotsatira ndi Zokambirana

2.1 Zotsatira za kuchuluka kwa pyridine (zosungunulira)

Zotsatira zamitundu yosiyanasiyana ya pyridine pa morphology ya hydroxypropylmethylcellulose acetate ndi hydroxypropylmethylcellulose propionate. Pamene kuchuluka kwa zosungunulira ndi zochepa, izo kuchepetsa extensibility unyolo macromolecular ndi mamasukidwe akayendedwe a dongosolo, kotero kuti mlingo wa esterification dongosolo anachita kuchepetsedwa, ndipo mankhwala adzakhala mpweya ngati misa lalikulu. Ndipo pamene kuchuluka kwa zosungunulira ndi otsika kwambiri, reactant n'zosavuta condense mu mtanda ndi kumamatira ku khoma chidebe, amene osati zoipa kuchita zimene anachita, komanso kumayambitsa vuto lalikulu kwa mankhwala pambuyo anachita. . Mu kaphatikizidwe ka hydroxypropyl methylcellulose acetate, kuchuluka kwa zosungunulira zomwe zimagwiritsidwa ntchito zimatha kusankhidwa ngati 150 mL / 2 g; popanga hydroxypropyl methylcellulose propionate, imatha kusankhidwa ngati 80 mL/0.5 g.

2.2 Kusanthula kwa ma infrared spectrum

Tchati chofananitsa cha infrared cha hydroxypropyl methylcellulose ndi hydroxypropyl methylcellulose acetate. Poyerekeza ndi zopangira, infrared spectrogram ya mankhwala hydroxypropyl methylcellulose acetate ali ndi kusintha koonekeratu. Mu mawonekedwe a infrared a mankhwala, nsonga yamphamvu inawonekera pa 1740cm-1, kusonyeza kuti gulu la carbonyl linapangidwa; kuonjezera apo, mphamvu ya kutambasula kugwedezeka kwapamwamba kwa OH pa 3500cm-1 kunali kochepa kwambiri kusiyana ndi zopangira, zomwe zimasonyezanso kuti -OH Panalipo kanthu.

Infrared spectrogram ya mankhwala hydroxypropyl methylcellulose propionate yasinthanso kwambiri poyerekeza ndi zopangira. Mu mawonekedwe a infrared a mankhwala, nsonga yamphamvu inawonekera pa 1740 cm-1, kusonyeza kuti gulu la carbonyl linapangidwa; kuonjezera apo, OH yotambasula kugwedezeka kwapamwamba pa 3500 cm-1 inali yotsika kwambiri kuposa yazinthu zopangira, zomwe zimasonyezanso kuti OH inachitapo kanthu.

2.3 Kutsimikiza kwa digiri yolowa m'malo

2.3.1 Kutsimikiza kwa digiri ya m'malo mwa hydroxypropyl methylcellulose acetate

Popeza hydroxypropyl methylcellulose ili ndi OH iwiri pagawo lililonse, ndipo cellulose acetate ndi chinthu chomwe chimapezedwa polowetsa COCH3 imodzi ya H mu OH imodzi, theoretical maximum degree of substitution (Ds) ndi 2.

2.3.2 Kutsimikiza kwa digiri ya kusintha kwa hydroxypropyl methylcellulose propionate

2.4 Kusungunuka kwa zinthu

Zinthu ziwiri zomwe zidapangidwazo zinali ndi mawonekedwe ofanana, ndipo hydroxypropyl methylcellulose acetate inali yosungunuka pang'ono kuposa hydroxypropyl methylcellulose propionate. Chopangacho chimatha kusungunuka mu acetone, ethyl acetate, acetone / madzi osungunulira osakanikirana, ndipo amakhala ndi zosankha zambiri. Kuonjezera apo, chinyezi chomwe chili mu acetone / madzi osakaniza osungunulira amatha kupanga zotengera za cellulose kukhala zotetezeka komanso zachilengedwe zikagwiritsidwa ntchito ngati zida zokutira.

3. Mapeto

(1) The kaphatikizidwe zinthu za hydroxypropyl methylcellulose acetate ndi motere: 2.5 g wa hydroxypropyl methylcellulose, acetic anhydride monga esterification wothandizira, 150 mL wa pyridine monga zosungunulira, kutentha anachita pa 110° C, ndi nthawi yochitira 1 h.

(2) The synthesis mikhalidwe ya hydroxypropyl methylcellulose acetate ndi: 0.5 g wa hydroxypropyl methylcellulose, propionic anhydride monga esterification agent, 80 mL wa pyridine monga zosungunulira, kutentha anachita pa 110°C, ndi nthawi yochitira 2 .5 h.

(3) Ma cellulose omwe amapangidwa pansi pa chikhalidwe ichi ali mwachindunji mu mawonekedwe a ufa wabwino wokhala ndi digiri yabwino yolowa m'malo, ndipo zotumphukira ziwiri za cellulose zimatha kusungunuka muzosungunulira zosiyanasiyana za organic monga ethyl acetate, acetone, ndi acetone / madzi.