Synthesis ea Hydroxypropyl Methyl Cellulose Acetate le Propionate

Ho sebelisa hydroxypropyl methylcellulose (HPMC) e le lisebelisoa tse tala, acetic anhydride le propionic anhydride e le li-esterification agents, karabelo ea esterification ho pyridine e lokiselitsoeng hydroxypropyl methylcellulose acetate le hydroxypropyl methylcellulose Cellulose propionate. Ka ho fetola palo ea solvent e sebelisitsoeng tsamaisong, sehlahisoa se nang le thepa e ntle le tekanyo ea ho fetola se ile sa fumanoa. Setifikeiti sa substitution se ne se khethoa ka mokhoa oa titration, mme sehlahisoa se ne se khetholloa le ho lekoa bakeng sa ts'ebetso. Liphetho li bonts'itse hore sistimi ea karabelo e arabiloe ho 110°C bakeng sa 1-2.5 h, 'me metsi a deionized a ne a sebelisoa e le moemeli oa precipitating ka mor'a karabelo,' me lihlahisoa tsa phofo tse nang le tekanyo ea phetoho e kholo ho feta 1 (tekanyo ea theory of substitution e ne e le 2) e ka fumanoa. E na le solubility e ntle ho lihlapolli tse fapaneng tsa manyolo joalo ka ethyl ester, acetone, acetone / metsi, jj.

Mantsoe a bohlokoa: hydroxypropyl methylcellulose; hydroxypropyl methylcellulose acetate; hydroxypropyl methylcellulose propionate

Hydroxypropylmethylcellulose (HPMC) ke motsoako oa polymer o seng oa ionic le cellulose ether e nang le mefuta e mengata ea tšebeliso. Joalo ka kenyelletso e ntle ea lik'hemik'hale, HPMC e sebelisoa hangata mafapheng a fapaneng mme e bitsoa "industrial monosodium glutamate". Hydroxypropyl methylcellulose (HPMC) ha e na feela mesebetsi e ntle ea emulsifying, thickening, le e tlamang, empa hape e ka sebelisoa ho boloka mongobo le ho sireletsa li-colloids. E sebelisoa haholo mafapheng a mangata a kang lijo, meriana, liaparo, masela le temo. . Phetoho ea hydroxypropyl methylcellulose e ka fetola tse ling tsa thepa ea eona, e le hore e ka sebelisoa hamolemo tšimong e itseng. Foromo ea molek'hule ea monoma ea eona ke C10H18O6.

Lilemong tsa morao tjena, lipatlisiso mabapi le lihlahisoa tsa hydroxypropyl methylcellulose butle-butle li fetohile sebaka se chesang. Ka ho fetola hydroxypropyl methylcellulose, metsoako e fapaneng e tsoang ho tse nang le thepa e fapaneng e ka fumanoa. Ka mohlala, ho kenyelletsoa ha lihlopha tsa acetyl ho ka fetola ho feto-fetoha ha lifilimi tsa ho roala meriana.

Phetoho ea hydroxypropyl methylcellulose hangata e etsoa ka boteng ba acid catalyst joalo ka concentrated sulfuric acid. Hangata teko e sebelisa acetic acid e le solvent. Maemo a karabelo a boima ebile a ja nako, 'me sehlahisoa se hlahisoang se na le boemo bo tlase ba ho nkela sebaka. (ka tlase ho 1).

Ka pampiri ena, acetic anhydride le propionic anhydride li sebelisitsoe e le li-esterification agents ho fetola hydroxypropyl methylcellulose ho lokisa hydroxypropyl methylcellulose acetate le hydroxypropyl methylcellulose propionate. Ka ho hlahloba maemo a kang khetho ea solvent (pyridine), tekanyo ea solvent, joalo-joalo, ho na le tšepo ea hore sehlahisoa se nang le thepa e ntle le tekanyo ea ho fetola se ka fumanoa ka mokhoa o batlang o le bonolo. Ka pampiri ena, ka lipatlisiso tsa liteko, sehlahisoa se lebisitsoeng se nang le phofshoana ea phofo le tekanyo ea phetoho e kholo ho feta 1 e ile ea fumanoa, e faneng ka tataiso e itseng ea theory bakeng sa tlhahiso ea hydroxypropyl methylcellulose acetate le hydroxypropyl methylcellulose propionate.

1. Karolo ea teko

1.1 Lisebelisoa le li-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, Moemeli oa Asia Bophirimela; Pyridine, AR, Tianjin Kemiou Chemical Reagent Co., Ltd.; methanol, ethanol, ether, ethyl acetate, acetone, NaOH le HCl li fumaneha khoebong ka mokhoa o hloekileng.

KDM thermostat electric mantle electric mantle, JJ-1A lebelo le methang dijithale display electric stirrer, NEXUS 670 Fourier transform infrared spectrometer.

1.2 Tokisetso ea hydroxypropyl methylcellulose acetate

Palo e itseng ea pyridine e ile ea kenngoa ka har'a botlolo ea melala e meraro, 'me joale 2.5 g ea hydroxypropyl methylcellulose e ile ea eketsoa moo, li-reactants li ile tsa tsosoa ka mokhoa o ts'oanang,' me mocheso o nyolohetse ho 110.°C. Kenya 4 mL ea acetic anhydride, etsa 110°C bakeng sa 1 h, emisa ho futhumatsa, e pholile ho mocheso oa kamore, eketsa metsi a mangata a deionized ho fokotsa sehlahisoa, sefa ka ho monya, hlatsoa ka metsi a deionized ka makhetlo a 'maloa ho fihlela eluate e sa nke lehlakore,' me u omise sehlahisoa se boloke.

1.3 Tokisetso ea hydroxypropyl methylcellulose propionate

Palo e itseng ea pyridine e ile ea kenngoa ka har'a botlolo e nang le melamo e meraro, 'me joale 0.5 g ea hydroxypropyl methylcellulose e ile ea kenngoa moo, li-reactants li ile tsa tsosoa ka mokhoa o ts'oanang,' me mocheso oa nyolohela ho 110.°C. Kenya 1.1 mL ea propionic anhydride, etsa 110°C bakeng sa 2.5 h, khaotsa ho futhumatsa, pholile ho mocheso kamoreng, eketsa palo e kholo ea metsi deionized precipitate sehlahiswa, filthara ka suction, hlatsoa ka metsi deionized ka makhetlo a 'maloa ho fihlela eluate ke seaplane thepa, boloka sehlahiswa omileng.

1.4 Boikemisetso ba spectroscopy ea infrared

Hydroxypropyl methylcellulose, hydroxypropyl methylcellulose acetate, hydroxypropyl methylcellulose propionate le KBr li ile tsa tsoakoa le fatše ka ho latellana, eaba li hatelloa ka har'a matlapa ho fumana hore na spectrum ea infrared ke efe.

1.5 Boikemisetso ba tekanyo ea ho fetola

Lokisetsa tharollo ea NaOH le HCl ka motsoako oa 0.5 mol / L, 'me u etse calibration ho fumana hore na mahloriso a nepahetseng ke afe; boima ba 0.5 g ea hydroxypropylmethylcellulose acetate (hydroxypropylmethylcellulose propionic acid ester) ka botlolong ea 250 ml Erlenmeyer, eketsa 25 ml ea acetone le marotholi a 3 a phenolphthalein indicator, kopanya hantle, ebe u eketsa 25 ml ea motsoako oa NaOH bakeng sa motsoako oa motsoako oa NaOH. 2 h; titrate le HCI ho fihlela 'mala o mofubelu oa tharollo o nyamela, rekota Molumo oa V1 (V2) oa hydrochloric acid o jeoang; sebelisa mokhoa o tšoanang ho lekanya molumo oa V0 oa hydrochloric acid e sebelisoang ke hydroxypropyl methylcellulose, le ho bala tekanyo ea ho fetola.

1.6 Teko ea ho qhibiliha

Nka palo e loketseng ea lihlahisoa tsa maiketsetso, u li kenye ka har'a motsoako oa manyolo, sisinya hanyenyane, 'me u shebe ho qhibiliha ha ntho.

2. Liphetho le Puisano

2.1 Phello ea palo ea pyridine (solvent)

Liphello tsa mefuta e fapaneng ea pyridine ho morphology ea hydroxypropylmethylcellulose acetate le hydroxypropylmethylcellulose propionate. Ha palo ea solvent e fokotsehile, e tla fokotsa ho atolosoa ha ketane ea macromolecular le viscosity ea tsamaiso, e le hore tekanyo ea esterification ea tsamaiso ea karabelo e fokotsehe, 'me sehlahisoa se tla fokotseha e le boima bo boholo. 'Me ha palo ea solvent e le tlase haholo, reactant e bonolo ho nyenyefatsa ho ba lesela le ho khomarela lebota la setshelo, e seng feela e sa rateheng bakeng sa ho etsa karabelo, empa hape e baka tšitiso e kholo ho phekolo ka mor'a karabelo. . Ha ho etsoa hydroxypropyl methylcellulose acetate, palo ea solvent e sebelisoang e ka khethoa e le 150 mL / 2 g; bakeng sa motsoako oa hydroxypropyl methylcellulose propionate, e ka khethoa e le 80 mL / 0.5 g.

2.2 Tlhahlobo ea mahlaseli a infrared

Chate ea papiso ea infrared ea hydroxypropyl methylcellulose le hydroxypropyl methylcellulose acetate. Ha ho bapisoa le thepa e tala, spectrogram ea infrared ea sehlahisoa sa hydroxypropyl methylcellulose acetate e na le phetoho e hlakileng haholoanyane. Ka sekhahla sa infrared sa sehlahisoa, tlhōrō e matla e ile ea hlaha ho 1740cm-1, e bontšang hore sehlopha sa carbonyl se hlahisoa; ho phaella moo, matla a tlhōrō e otlolohileng ea ho sisinyeha ha OH ho 3500cm-1 e ne e le tlase haholo ho feta ea lihlahisoa tse tala, tse ileng tsa boela tsa bontša hore -OH Ho ne ho e-na le karabelo.

The infrared spectrogram ea sehlahisoa sa hydroxypropyl methylcellulose propionate le eona e fetohile haholo ha e bapisoa le thepa e tala. Ka sekhahla sa infrared sa sehlahisoa, tlhōrō e matla e ile ea hlaha ho 1740 cm-1, e bontšang hore sehlopha sa carbonyl se hlahisoa; ho phaella moo, OH e otlollang ho sisinyeha tlhōrō e matla ho 3500 cm-1 e ne e le tlase haholo ho feta ea lihlahisoa tse tala, tse neng li boetse li bontša hore OH e ile ea itšoara.

2.3 Boikemisetso ba tekanyo ea ho fetola

2.3.1 Qeto ea tekanyo ea sebaka sa hydroxypropyl methylcellulose acetate

Kaha hydroxypropyl methylcellulose e na le OH tse peli tse le 'ngoe yuniti e' ngoe le e 'ngoe,' me cellulose acetate ke sehlahisoa se fumanoang ka ho kenya COCH3 e le 'ngoe bakeng sa H ho OH e le' ngoe, tekanyo e phahameng ea theory of substitution (Ds) ke 2.

2.3.2 Qeto ea tekanyo ea ho kenya sebaka sa hydroxypropyl methylcellulose propionate

2.4 Ho qhibiliha ha sehlahisoa

Lintho tse peli tse entsoeng li ne li e-na le litšobotsi tse tšoanang tsa ho qhibiliha, 'me hydroxypropyl methylcellulose acetate e ne e qhibiliha hanyane ho feta hydroxypropyl methylcellulose propionate. Sehlahisoa sa maiketsetso se ka qhibiliha ka acetone, ethyl acetate, acetone / metsi a motsoako oa solvent, 'me se na le khetho e eketsehileng. Ho phaella moo, mongobo o nang le motsoako oa motsoako oa acetone / metsi o ka etsa hore lihlahisoa tsa selulose li bolokehe le ho boloka tikoloho ha li sebelisoa e le lisebelisoa tsa ho roala.

3. Qetello

(1) Maemo a motsoako oa hydroxypropyl methylcellulose acetate ke a latelang: 2.5 g ea hydroxypropyl methylcellulose, acetic anhydride e le esterification agent, 150 mL ea pyridine e le solvent, mocheso o arabelang ho 110.° C, le nako ea karabelo 1 h.

(2) Maemo a motsoako oa hydroxypropyl methylcellulose acetate ke: 0.5 g ea hydroxypropyl methylcellulose, propionic anhydride e le esterification agent, 80 mL ea pyridine e le solvent, mocheso o arabelang ho 110.°C, le nako ea ho arabela ke 2 .5 h.

(3) Li-derivatives tsa cellulose tse entsoeng tlas'a boemo bona li ka tsela e tobileng ka sebōpeho sa phofo e ntle e nang le tekanyo e ntle ea ho fetola, 'me lihlahisoa tsena tse peli tsa cellulose li ka qhibiliha ka mefuta e sa tšoaneng ea metsoako e kang ethyl acetate, acetone le acetone / metsi.