Synthesis o Hydroxypropyl Methyl Cellulose Acetate a me Propionate

Ke hoʻohana nei i ka hydroxypropyl methylcellulose (HPMC) i mea maka, acetic anhydride a me propionic anhydride e like me nā mea esterification, ka hopena esterification i ka pyridine i hoʻomākaukau ʻia hydroxypropyl methylcellulose acetate a me hydroxypropyl methylcellulose Cellulose propionate. Ma ka hoʻololi ʻana i ka nui o ka solvent i hoʻohana ʻia i ka ʻōnaehana, ua loaʻa kahi huahana me nā waiwai maikaʻi aʻe a me ke degere pani. Ua hoʻoholo ʻia ka degere pani ma ke ʻano titration, a ua hōʻike ʻia ka huahana a hoʻāʻo ʻia no ka hana. Ua hōʻike ʻia nā hopena ua hoʻokō ʻia ka ʻōnaehana pane ma 110°C no ka 1-2.5 h, a me ka wai deionized ua hoʻohana 'ia e like me ka precipitating luna ma hope o ka hopena, a me ka pauda huahana me ka degere o ka hoʻololi 'oi aʻe ma mua o 1 (theoretical degere o ka hoʻololi 'ia he 2) hiki ke loaʻa. Loaʻa iā ia ka solubility maikaʻi i nā mea hoʻoheheʻe organik e like me ka ethyl ester, acetone, acetone / wai, etc.

Hua'ōlelo nui: hydroxypropyl methylcellulose; hydroxypropyl methylcellulose acetate; hydroxypropyl methylcellulose propionate

ʻO ka Hydroxypropylmethylcellulose (HPMC) kahi hui polymer non-ionic a me kahi cellulose ether me kahi ākea o ka hoʻohana. Ma ke ʻano he mea hoʻohui kemika maikaʻi loa, hoʻohana pinepine ʻia ka HPMC ma nā ʻano āpau a ua kapa ʻia ʻo "industrial monosodium glutamate". ʻO ka Hydroxypropyl methylcellulose (HPMC) ʻaʻole wale ka emulsifying maikaʻi, mānoanoa, a me nā hana paʻa, akā hiki ke hoʻohana ʻia no ka mālama ʻana i ka makū a pale i nā colloids. Hoʻohana nui ʻia ia ma nā ʻano he nui e like me ka meaʻai, ka lāʻau lapaʻau, ka uhi, textiles, a me ka mahiʻai. . Hiki i ka hoʻololi ʻana o ka hydroxypropyl methylcellulose ke hoʻololi i kekahi o kāna mau waiwai, i hiki ke hoʻohana maikaʻi ʻia i kekahi kahua. ʻO ke kumu molekala o kāna monomer C10H18O6.

I nā makahiki i hala iho nei, ua lilo ka noiʻi ʻana i nā derivatives hydroxypropyl methylcellulose i wahi wela. Ma ka hoʻololi ʻana i ka hydroxypropyl methylcellulose, hiki ke loaʻa i nā pūhui derivative like ʻole me nā waiwai like ʻole. No ka laʻana, hiki i ka hoʻokomo ʻana i nā hui acetyl ke hoʻololi i ka maʻalahi o nā kiʻi ʻoniʻoni lāʻau.

Hana ʻia ka hoʻololi ʻana o ka hydroxypropyl methylcellulose i mua o kahi catalyst acid e like me ka sulfuric acid concentrated. Hoʻohana maʻamau ka hoʻokolohua acetic acid ma ke ʻano he solvent. He paʻakikī a hoʻopau manawa ka hopena o ka hopena, a he haʻahaʻa haʻahaʻa ka hopena o ka huahana. (emi iho i ka 1).

Ma kēia pepa, ua hoʻohana ʻia ka anhydride acetic a me ka propionic anhydride ma ke ʻano he esterification agents e hoʻololi i ka hydroxypropyl methylcellulose e hoʻomākaukau ai i ka hydroxypropyl methylcellulose acetate a me ka hydroxypropyl methylcellulose propionate. Ma ka ʻimi ʻana i nā kūlana e like me ke koho solvent (pyridine), solvent dosage, a me nā mea ʻē aʻe, ua manaʻo ʻia e hiki ke loaʻa kahi huahana me nā waiwai maikaʻi aʻe a me ke kēkelē hoʻololi ma o ke ʻano maʻalahi. I loko o kēia pepa, ma o ka noiʻi hoʻokolohua, ua loaʻa ka huahana i hoʻopaʻa ʻia me ka pauka pauka a me kahi degere o ka hoʻololi ʻana i ʻoi aku ma mua o 1, i hāʻawi i kekahi alakaʻi kumu no ka hana ʻana o ka hydroxypropyl methylcellulose acetate a me ka hydroxypropyl methylcellulose propionate.

1. Māhele hoʻokolohua

1.1 Nā mea a me nā reagents

ʻO ka lāʻau lapaʻau 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.; ʻO ka methanol, ethanol, etera, ethyl acetate, acetone, NaOH a me HCl ke kūʻai aku ma ke ʻano maʻemaʻe.

KDM thermostat uila hoʻomehana ʻaʻahu, JJ-1A ana wikiwiki i ka hōʻike kikohoʻe uila stirrer, NEXUS 670 Fourier transform infrared spectrometer.

1.2 Hoʻomākaukau i ka hydroxypropyl methylcellulose acetate

Ua hoʻokomo ʻia kekahi nui o ka pyridine i loko o ka ipu ʻāʻī ʻekolu, a laila ua hoʻohui ʻia he 2.5 g o ka hydroxypropyl methylcellulose i laila, ua hoʻoulu like ʻia nā mea hana, a ua hoʻonui ʻia ka mahana i 110.°C. E hoʻonui i 4 mL o ka anhydride acetic, e hoʻololi i ka 110°C no 1 h, hooki i ka wela, hooluolu i ka lumi wela, hoonui i ka nui o ka wai deionized e precipitate ka huahana, kānana me ka momi, holoi me ka wai deionized no kekahi mau manawa a hiki i ka eluate ku ole, a maloo i ka huahana hoola.

1.3 Hoʻomākaukau i ka hydroxypropyl methylcellulose propionate

Ua hoʻohui ʻia kekahi nui o ka pyridine i loko o ka ipu ʻāʻī ʻekolu, a laila ua hoʻohui ʻia he 0.5 g o ka hydroxypropyl methylcellulose i laila, ua hoʻoulu like ʻia nā mea hana, a ua hoʻonui ʻia ka mahana i 110°C. E hoʻohui i 1.1 mL o ka propionic anhydride, e hoʻololi i ka 110°C no 2.5 h, hooki i ka wela, hooluolu i ka lumi wela, e hoonui i ka nui o ka wai deionized e precipitate ka huahana, kānana me ka suction, holoi me ka wai deionized no kekahi mau manawa a hiki i ka eluate waiwai waena, e mālama i ka huahana maloʻo.

1.4 Ka hoʻoholo ʻana o ka spectroscopy infrared

ʻO ka hydroxypropyl methylcellulose, hydroxypropyl methylcellulose acetate, hydroxypropyl methylcellulose propionate a me KBr i hui pū ʻia me ka lepo, a laila kaomi ʻia i loko o nā papa e hoʻoholo ai i ka spectrum infrared.

1.5 Ka hoʻoholo ʻana o ke degere o ka hoʻololi ʻana

E hoʻomākaukau i nā hāʻina NaOH a me HCl me ka hoʻopaʻa ʻana o 0.5 mol/L, a hoʻokō i ka calibration e hoʻoholo i ka ʻike pololei; kaupaona 0.5 g o ka hydroxypropylmethylcellulose acetate (hydroxypropylmethylcellulose propionic acid ester) i loko o ka pahu Erlenmeyer 250 mL, e hoʻohui i 25 mL o ka acetone a me 3 kulu o ka phenolphthalein indicator, e hui maikaʻi, a laila e hoʻohui i 25 mL o ka solution NaOHmagnetic, hoʻoulu a me ka hoʻoulu ʻana i ka electrorr 2 h; titrate me ka HCI a hiki i ka nalo ana o ke kala ulaula o ka solution, e kakau i ka Volume V1 (V2) o ka waika hydrochloric i pau; e hoʻohana i ke ʻano like e ana i ka nui V0 o ka waika hydrochloric i hoʻopau ʻia e ka hydroxypropyl methylcellulose, a e helu i ke degere o ka hoʻololi ʻana.

1.6 Hoʻokolohua solubility

E lawe i ka nui kūpono o nā huahana synthetic, hoʻohui iā lākou i ka mea hoʻoheheʻe organik, lulu liʻiliʻi, a nānā i ka hemo ʻana o ka mea.

2. Nā hopena a me ke kūkākūkā

2.1 Ka hopena o ka nui o ka pyridine (solvent)

Nā hopena o nā nui like ʻole o ka pyridine i ka morphology o hydroxypropylmethylcellulose acetate a me hydroxypropylmethylcellulose propionate. Ke emi ka nui o ka solvent, e hōʻemi ia i ka extensibility o ke kaulahao macromolecular a me ka viscosity o ka ʻōnaehana, no laila e hoʻemi ʻia ka degere o ka esterification o ka ʻōnaehana hopena, a e hoʻomāliʻi ʻia ka huahana e like me ka nui nui. A i ka haʻahaʻa loa o ka solvent, ua maʻalahi ka reactant e hoʻopili i loko o kahi puʻupuʻu a pili i ka paia o ka ipu, ʻaʻole maikaʻi wale no ka hoʻokō ʻana i ka hopena, akā ke kumu nui ʻole i ka mālama ʻana ma hope o ka hopena. . I ka synthesis o ka hydroxypropyl methylcellulose acetate, hiki ke koho ʻia ka nui o ka solvent e like me 150 mL / 2 g; no ka synthesis o hydroxypropyl methylcellulose propionate, hiki ke koho ʻia e like me 80 mL / 0.5 g.

2.2 Ka nānā 'ana i ka spectrum infrared

Ka palapala hoʻohālikelike infrared o ka hydroxypropyl methylcellulose a me ka hydroxypropyl methylcellulose acetate. Ke hoʻohālikelike ʻia me ka mea maka, ʻo ka spectrogram infrared o ka huahana hydroxypropyl methylcellulose acetate he loli ʻoi aku ka ʻike. I loko o ka infrared spectrum o ka huahana, ua ʻike ʻia kahi piko ikaika ma 1740cm-1, e hōʻike ana ua hana ʻia kahi hui carbonyl; Eia kekahi, ʻoi aku ka haʻahaʻa o ka haʻahaʻa haʻahaʻa haʻahaʻa o OH ma 3500cm-1 ma mua o ka mea maka, i hōʻike pū ʻia -OH Aia kahi pane.

Ua loli nui ka spectrogram infrared o ka huahana hydroxypropyl methylcellulose propionate i ka hoʻohālikelike ʻia me ka mea maka. I loko o ka infrared spectrum o ka huahana, ua ʻike ʻia kahi piko ikaika ma 1740 cm-1, e hōʻike ana ua hana ʻia kahi hui carbonyl; Eia kekahi, ʻoi aku ka haʻahaʻa o ka OH stretching vibration peak intensity ma 3500 cm-1 ma mua o ko ka mea maka, kahi i hōʻike ʻia he OH reacted.

2.3 Ka hoʻoholo ʻana o ke degere o ka hoʻololi ʻana

2.3.1 Ka hoʻoholo ʻana o ka degere pani o ka hydroxypropyl methylcellulose acetate

No ka mea he ʻelua ʻelua OH ka hydroxypropyl methylcellulose i loko o kēlā me kēia ʻāpana, a ʻo ka cellulose acetate kahi huahana i loaʻa ma ka hoʻololi ʻana i hoʻokahi COCH3 no H i hoʻokahi OH, ʻo ka degere kiʻekiʻe o ka hoʻololi ʻana (Ds) he 2.

2.3.2 Ka hoʻoholo ʻana o ke degere o ka hoʻololi ʻana o ka hydroxypropyl methylcellulose propionate.

2.4 Solubility o ka huahana

He ʻano hoʻoheheʻe like ko nā mea ʻelua i hoʻohui ʻia, a ʻoi aku ka maʻalahi o ka hydroxypropyl methylcellulose acetate ma mua o ka hydroxypropyl methylcellulose propionate. Hiki ke hoʻoheheʻe ʻia ka huahana synthetic i ka acetone, ethyl acetate, acetone / wai i hui ʻia i ka solvent, a ʻoi aku ka nui o ke koho. Eia kekahi, hiki i ka makū i loko o ka acetone / wai i hui pū ʻia ka mea hiki ke hoʻolilo i nā derivatives cellulose i ʻoi aku ka palekana a me ke aloha o ke kaiapuni ke hoʻohana ʻia e like me nā mea uhi.

3. Ka hopena

(1) ʻO nā kūlana synthesis o ka hydroxypropyl methylcellulose acetate penei: 2.5 g o ka hydroxypropyl methylcellulose, acetic anhydride ma ke ʻano he esterification agent, 150 mL o ka pyridine e like me ka solvent, ka mahana hopena ma 110° C, a me ka manawa pane 1 h.

(2) ʻO nā kūlana synthesis o ka hydroxypropyl methylcellulose acetate he: 0.5 g o ka hydroxypropyl methylcellulose, propionic anhydride ma ke ʻano he esterification agent, 80 mL o ka pyridine e like me ka solvent, ka wela o ka hopena ma 110°C, a me ka manawa pane o 2 .5 h.

(3) ʻO ka cellulose derivatives i hoʻohui ʻia ma lalo o kēia ʻano he pololei ia i ke ʻano o nā pauka maikaʻi me kahi kūlana maikaʻi o ka hoʻololi ʻana, a hiki ke hoʻoheheʻe ʻia kēia mau ʻāpana cellulose ʻelua i nā mea hoʻoheheʻe organik like ʻole e like me ka ethyl acetate, acetone, a me ka acetone / wai.