Fa'asologa o le Hydroxypropyl Methyl Cellulose Acetate ma le Propionate

Faʻaaogaina o le hydroxypropyl methylcellulose (HPMC) e pei o mea mata, acetic anhydride ma propionic anhydride e pei o le esterification agents, o le esterification reaction i pyridine saunia hydroxypropyl methylcellulose acetate ma hydroxypropyl methylcellulose Cellulose propionate. E ala i le suia o le aofaʻi o le solvent na faʻaaogaina i totonu o le faiga, na maua ai se oloa e sili atu mea totino ma sui tulaga. O le tikeri sui na fuafuaina i le titration method, ma o le oloa na faʻaalia ma faʻataʻitaʻiina mo le faʻatinoga. O faʻaiʻuga na faʻaalia ai na tali atu le faiga faʻaalia i le 110°C mo le 1-2.5 h, ma le vai deionized na faʻaaogaina e fai ma sui faʻafefe pe a maeʻa le tali, ma oloa paʻu ma se tikeri o le suitulaga sili atu nai lo le 1 (tulaga faʻavae o le suitulaga o le 2) e mafai ona maua. E iai le solubility lelei i solu faʻalaʻau eseese e pei ole ethyl ester, acetone, acetone / vai, ma isi.

upu autu: hydroxypropyl methylcellulose; hydroxypropyl methylcellulose acetate; hydroxypropyl methylcellulose propionate

O le Hydroxypropylmethylcellulose (HPMC) o se polymer non-ionic compound ma se cellulose ether ma le tele o faʻaoga. I le avea ai o se vailaʻau sili ona lelei, e masani ona faʻaaogaina le HPMC i vaega eseese ma e taʻua o le "industrial monosodium glutamate". Hydroxypropyl methylcellulose (HPMC) e le gata e lelei emulsifying, mafiafia, ma fusifusia galuega, ae mafai foi ona faaaoga e faatumauina le susu ma puipuia colloids. E masani ona faʻaaogaina i le tele o matata e pei o meaʻai, vailaʻau, paʻu, ie, ma faʻatoʻaga. . Suiga o le hydroxypropyl methylcellulose e mafai ona suia nisi o ona meatotino, ina ia mafai ona sili atu ona faʻaaogaina i se fanua faapitoa. O le fua mole mole o lona monomer o le C10H18O6.

I tausaga talu ai nei, o suʻesuʻega ile hydroxypropyl methylcellulose derivatives ua faasolosolo malie lava ona avea ma nofoaga vevela. E ala i le suia o le hydroxypropyl methylcellulose, e mafai ona maua ni mea faʻapipiʻi eseese ma meatotino eseese. Mo se faʻataʻitaʻiga, o le faʻaofiina o vaega acetyl e mafai ona suia le fetuutuunaʻi o ata tifaga faʻamaʻi.

O le suiga ole hydroxypropyl methylcellulose e masani lava ona faia i le i ai o se faʻamaʻi gaʻo e pei ole sulfuric acid concentrated. Ole fa'ata'ita'iga e masani ona fa'aogaina le acetic acid e fai ma so'o. O tulaga faʻaalia e faigata ma faʻaalu taimi, ma o le mea e maua mai ai e maualalo le tikeri o le sui. (itiiti ifo i le 1).

I totonu o lenei pepa, o le acetic anhydride ma le propionic anhydride na faʻaaogaina e fai ma sui esterification e sui ai le hydroxypropyl methylcellulose e saunia ai le hydroxypropyl methylcellulose acetate ma le hydroxypropyl methylcellulose propionate. E ala i le suʻesuʻeina o tulaga e pei o le solvent selection (pyridine), solvent dose, ma isi, e faʻamoemoe e mafai ona maua se oloa e sili atu mea totino ma sui tulaga e ala i se auala faigofie. I totonu o lenei pepa, e ala i suʻesuʻega faʻataʻitaʻiga, na maua ai le oloa faʻatatau ma se paʻu paʻu ma se tikeri o le suitulaga sili atu nai lo le 1 na maua, lea na maua ai ni taʻiala faʻapitoa mo le gaosiga o le hydroxypropyl methylcellulose acetate ma le hydroxypropyl methylcellulose propionate.

1. Vaega faataitai

1.1 Meafaitino ma reagents

vaila'au vaila'au hydroxypropyl methylcellulose (KIMA CHEMICAL CO., LTD, 60HD100, methoxyl vaega vaega 28% -30%, hydroxypropoxyl vaega vaega 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, eter, ethyl acetate, acetone, NaOH ma le HCl o lo'o maua fa'apisinisi fa'atauva'a mama.

KDM thermostat eletise faʻavevela ofu talaloa, JJ-1A saoasaoa fuaina numera faʻaalia faʻamalosi eletise, NEXUS 670 Fourier liliu infrared spectrometer.

1.2 Sauniuniga ole hydroxypropyl methylcellulose acetate

O se aofaiga patino o le pyridine na faʻaopoopoina i totonu o le fagu tolu-ua, ona faʻaopoopoina lea o le 2.5 g o le hydroxypropyl methylcellulose i ai, o mea faʻafefe na faʻafefeteina tutusa, ma siitia le vevela i le 110.°C. Fa'aopoopo le 4 mL o le acetic anhydride, fa'agaoi i le 110°C mo le 1 itula, taofi le faʻamafanafanaina, faʻamalie i le vevela o le potu, faʻaopopo le tele o vai faʻafefeteina e faʻafefe ai le oloa, faʻamama i le suction, fufulu ile vai faʻafefe mo le tele o taimi seia oʻo ina le tutusa le luate, ma faʻagogo le oloa sefe.

1.3 Sauniuniga ole hydroxypropyl methylcellulose propionate

O se aofaiga patino o le pyridine na faʻaopopo i totonu o le fagu tolu-ua, ona faʻaopoopoina lea o le 0.5 g o le hydroxypropyl methylcellulose i ai, o mea faʻafefe na faʻafefeteina tutusa, ma siitia le vevela i le 110.°C. Fa'aopoopo le 1.1 mL o le propionic anhydride, fa'agaioi ile 110°C mo le 2.5 h, taofi le vevela, malulu i le vevela o le potu, faʻaopopo se aofaiga tele o vai deionized e faʻafefe ai le oloa, faʻamama i le suction, fufulu i le vai deionized mo le tele o taimi seia oʻo ina avea le eluate ma meatotino feololo, teu le oloa mago.

1.4 Fuafuaga ole spectroscopy infrared

O le hydroxypropyl methylcellulose, hydroxypropyl methylcellulose acetate, hydroxypropyl methylcellulose propionate ma KBr na faʻafefiloi ma eleele taʻitasi, ona oomiina lea i totonu o laupepa e fuafua ai le fusi o le infrared.

1.5 Fuafuaga o le tikeri o le suitulaga

Saunia vaifofo NaOH ma HCl faʻatasi ma le faʻaogaina o le 0.5 mol / L, ma faʻatino le faʻavasegaina e fuafua ai le faʻatonuga tonu; fuaina le 0.5 g o le hydroxypropylmethylcellulose acetate (hydroxypropylmethylcellulose propionic acid ester) i totonu o se fagu Erlenmeyer 250 mL, faaopoopo le 25 mL o le acetone ma le 3 mataua o le phenolphthalein indicator, faʻafefiloi lelei, ona faʻaopopo lea o le 25 mL o le NaOH magnetic solution, faʻafefeteina ma faʻafefeteina. 2 h; titrate i le HCI seia mou atu le lanu mumu o le vaifofo, faamaumau Le voluma V1 (V2) o le suka o le hydrochloric na fa'aaogaina; fa'aoga le auala lava e tasi e fua ai le voluma V0 ole vaila'au oona o lo'o fa'aaogaina e le hydroxypropyl methylcellulose, ma fuafua le tikeri o le sui.

1.6 Su'ega solubility

Ave se aofaiga talafeagai o oloa gaosi, faaopoopo i latou i le solu oona, lulu teisi, ma matau le faʻamavaeina o le vailaʻau.

2. I'uga ma Talanoaga

2.1 Le aʻafiaga o le aofaʻi o le pyridine (solvent)

Aafiaga o aofaiga eseese o pyridine i luga o le morphology o le hydroxypropylmethylcellulose acetate ma le hydroxypropylmethylcellulose propionate. A itiiti ifo le aofaʻi o le solvent, o le a faʻaitiitia ai le faʻalauteleina o le filifili macromolecular ma le viscosity o le faiga, ina ia faʻaitiitia le tikeri o le esterification o le faiga tali, ma o le a faʻafefeteina le oloa e pei o se tele tele. Ma afai o le aofaiga o le solvent e maualalo tele, o le reactant e faigofie ona faʻafefe i totonu o se paluga ma pipii i le puipui puipui, lea e le gata ina le lelei mo le faʻatinoina o le tali, ae e mafua ai foi le faʻalavelave tele i le togafitiga pe a uma le tali. . I le faʻapipiʻiina o le hydroxypropyl methylcellulose acetate, o le aofaʻi o le solvent faʻaaogaina e mafai ona filifilia e pei o le 150 mL / 2 g; mo le faʻapipiʻiina o le hydroxypropyl methylcellulose propionate, e mafai ona filifilia e pei o le 80 mL / 0.5 g.

2.2 Iloiloga o alaleo infrared

Siata faʻatusatusaga infrared o le hydroxypropyl methylcellulose ma le hydroxypropyl methylcellulose acetate. Pe a faatusatusa i mea mata, o le spectrogram infrared o le oloa hydroxypropyl methylcellulose acetate e sili atu ona manino suiga. I le alaleo infrared o le oloa, o se tumutumu malosi na aliali mai i le 1740cm-1, e faʻaalia ai na gaosia se vaega carbonyl; e le gata i lea, o le malosi o le faʻalauteleina o le vibration peak o le OH i le 3500cm-1 na sili atu le maualalo nai lo le mea mataʻutia, lea na faʻaalia ai foi -OH Sa i ai se tali.

O le spectrogram infrared o le oloa hydroxypropyl methylcellulose propionate ua matua suia foi pe a faatusatusa i mea mata. I le fusi infrared o le oloa, o se tumutumu malosi na faʻaalia i le 1740 cm-1, e faʻaalia ai na gaosia se vaega carbonyl; e le gata i lea, o le maualuga o le vibration o le OH i le 3500 cm-1 na sili atu le maualalo nai lo le mea mata, lea na faʻaalia ai foi na tali atu se OH.

2.3 Fuafuaga o le tikeri o le suitulaga

2.3.1 Fuafuaga o le tikeri sui o le hydroxypropyl methylcellulose acetate

Talu ai ona o le hydroxypropyl methylcellulose e lua tasi le OH i iunite taʻitasi, ma le cellulose acetate o se oloa e maua e ala i le suia o le tasi COCH3 mo H i le tasi OH, o le maualuga maualuga o le suʻega (Ds) e 2.

2.3.2 Fuafuaina o le tikeri o le suia o le hydroxypropyl methylcellulose propionate

2.4 Solubility o le oloa

O mea e lua na fa'apipi'iina e tutusa lelei le solubility, ma o le hydroxypropyl methylcellulose acetate sa sili atu ona soluble nai lo le hydroxypropyl methylcellulose propionate. O le oloa gaosia e mafai ona faʻamavaeina i le acetone, ethyl acetate, acetone / vai faʻafefiloi solvent, ma e sili atu le filifilia. E le gata i lea, o le susu o loʻo i totonu o le acetone / vai faʻafefiloi faʻafefiloi e mafai ona sili atu le saogalemu o mea e maua mai i le cellulose ma faʻafeiloaʻi le siosiomaga pe a faʻaaogaina e fai ma mea faʻapipiʻi.

3. Faaiuga

(1) O tulaga faʻapipiʻi o le hydroxypropyl methylcellulose acetate e faʻapea: 2.5 g o le hydroxypropyl methylcellulose, acetic anhydride e pei o le esterification agent, 150 mL o le pyridine o le solvent, le vevela o le tali ile 110° C, ma le taimi tali 1 h.

(2) O tulaga faʻapipiʻi o le hydroxypropyl methylcellulose acetate o: 0.5 g o le hydroxypropyl methylcellulose, propionic anhydride e pei o le esterification agent, 80 mL o le pyridine e pei o le solvent, le vevela o le tali ile 110°C, ma le taimi e tali atu ai i le 2.5 itula.

(3) O mea e maua mai i le cellulose o loʻo faʻapipiʻiina i lalo o lenei tulaga o loʻo tuʻu saʻo i foliga o paʻu lelei ma se tikeri lelei o le suia, ma o nei mea e lua o le cellulose e mafai ona faʻamavaeina i soʻo faʻalagona eseese e pei o le ethyl acetate, acetone, ma le acetone / vai.