Isku dhafka Hydroxypropyl Methyl Cellulose Acetate iyo Propionate

Isticmaalka hydroxypropyl methylcellulose (HPMC) sida alaabta ceeriin, acetic anhydride iyo propionic anhydride sida wakiilada esterification, falcelinta esterification ee pyridine diyaarisay hydroxypropyl methylcellulose acetate iyo hydroxypropyl methylcellulose Cellulose propionate. Beddelidda xaddiga dareeraha loo isticmaalo nidaamka, badeecad leh sifooyin wanaagsan iyo shahaado beddelaad ah ayaa la helay. Shahaadada beddelka waxaa lagu go'aamiyay habka titration, iyo badeecada waxaa lagu sifeeyay oo lagu tijaabiyay waxqabad. Natiijooyinka waxay muujiyeen in nidaamka falcelinta laga falceliyay 110°C ee 1-2.5 h, iyo biyaha deionized ayaa loo isticmaalay sidii wakiilka soo da'aya ka dib falcelinta, iyo alaabooyinka budada leh ee leh heerka beddelka ee ka weyn 1 (darajada aragtida beddelka waxay ahayd 2) ayaa la heli karaa. Waxay leedahay milmayn wanaagsan ee dareerayaasha organic kala duwan sida ethyl ester, acetone, acetone/biyo, iwm.

Erayada muhiimka ah: hydroxypropyl methylcellulose; hydroxypropyl methylcellulose acetate; hydroxypropyl methylcellulose propionate

Hydroxypropylmethylcellulose (HPMC) waa iskudhis polymer ah oo aan ahayn ionic iyo eter cellulose ah oo leh adeegsiyo kala duwan. Sida maaddo kiimiko ah oo aad u wanaagsan, HPMC waxaa badanaa loo isticmaalaa dhinacyo kala duwan waxaana loo yaqaan " monosodium glutamate warshadaha ". Hydroxypropyl methylcellulose (HPMC) kaliya ma leh emulsifying wanaagsan, dhumucdiisuna, iyo hawlaha xidhidhiyaha, laakiin sidoo kale waxaa loo isticmaali karaa si loo ilaaliyo qoyaan iyo ilaalinta kolloidyada. Waxaa si weyn looga isticmaalaa dhinacyo badan sida cuntada, daawada, dahaarka, dunta, iyo beeraha. . Wax ka beddelka hydroxypropyl methylcellulose waxay bedeli kartaa qaar ka mid ah hantideeda, si ay si fiican ugu isticmaali karto goob gaar ah. Qaabka molecular ee monomerkiisu waa C10H18O6.

Sanadihii la soo dhaafay, cilmi baarista hydroxypropyl methylcellulose derivatives ayaa si tartiib tartiib ah u noqday meel kulul. Iyadoo la bedelayo hydroxypropyl methylcellulose, xeryahooda kala duwan ee kala duwan oo leh sifooyin kala duwan ayaa la heli karaa. Tusaale ahaan, soo bandhigida kooxaha acetyl waxay bedeli kartaa dabacsanaanta filimada daahan caafimaadka.

Beddelka hydroxypropyl methylcellulose waxaa badanaa lagu fuliyaa joogitaanka kicinta aashitada sida sulfuric acid. Tijaabadu waxay caadi ahaan u isticmaashaa acetic acid sida dareere ahaan. Xaaladaha falcelintu waa kuwo adag oo waqti badan qaata, iyo badeecada ka soo baxday waxay leedahay heer hoose oo beddelaad ah. (in ka yar 1).

Warqadan, acetic anhydride iyo propionic anhydride ayaa loo isticmaalay sida wakiilada esterification si loo beddelo hydroxypropyl methylcellulose si loogu diyaariyo hydroxypropyl methylcellulose acetate iyo hydroxypropyl methylcellulose propionate. Marka la sahamiyo xaaladaha sida xulashada dareeraha (pyridine), qiyaasta dareeraha, iwm, waxaa la rajeynayaa in badeecad leh sifooyin wanaagsan iyo shahaadada beddelka lagu heli karo hab fudud. Warqadan, iyada oo loo marayo cilmi-baaris tijaabo ah, badeecada la beegsanayo oo leh qulqulo budada ah iyo heerka beddelka ee ka weyn 1 ayaa la helay, taas oo bixisay hagitaan aragti ah oo loogu talagalay soo saarista hydroxypropyl methylcellulose acetate iyo hydroxypropyl methylcellulose propionate.

1. Qaybta tijaabada ah

1.1 Qalabka iyo reagents

Heerka dawooyinka hydroxypropyl methylcellulose (KIMA CHEMICAL CO., LTD, 60HD100, jajab cufnaanta methoxyl 28%-30%, jajabka xajmiga hydroxypropoxyl 7%-12%); acetic anhydride, AR, Sinopharm Group Chemical Reagent Co., Ltd .; Propionic Anhydride, AR, Galbeedka Aasiya Reagent; Pyridine, AR, Tianjin Kemiou Chemical Reagent Co., Ltd.; methanol, ethanol, ether, ethyl acetate, acetone, NaOH iyo HCl ganacsi ahaan waa la heli karaa si lafo-gur ah.

KDM heerkulbeegga korantada korantada, JJ-1A xawaaraha cabbiraya soo bandhig koronto oo dhijitaal ah, NEXUS 670 Fourier wuxuu beddelaa spectrometer infrared.

1.2 Diyaarinta hydroxypropyl methylcellulose acetate

Qadar cayiman oo pyridine ah ayaa lagu daray weelka saddexda luqun, ka dibna 2.5 g oo ah hydroxypropyl methylcellulose ayaa lagu daray, falceliyeyaasha ayaa si siman loo walaaqay, heerkulku wuxuu kor u kacay 110.°C. Ku dar 4 mL oo ah anhydride acetic, ka fal celi 110°C ilaa 1 saac, jooji kuleyliyaha, qabooji heerkulka qolka, ku dar xaddi badan oo biyo ah oo dareere ah si ay u soo dedejiyaan alaabta, ku sifee nuugista, ku dhaq biyo fuuq-baxsan dhowr jeer ilaa eluate-ku dhexdhexaad yahay, oo qalaji kaydinta alaabta.

1.3 Diyaarinta hydroxypropyl methylcellulose propionate

Qadar cayiman oo pyridine ah ayaa lagu daray weelka saddexda luqun, ka dibna 0.5 g oo ah hydroxypropyl methylcellulose ayaa lagu daray, fal-celiyeyaasha ayaa si siman loo walaaqay, heerkulku wuxuu kor u kacay 110.°C. Ku dar 1.1 ml oo ah propionic anhydride, ka fal celi 110°C ilaa 2.5 saacadood, jooji kuleylka, qabooji heerkulka qolka, ku dar qadar badan oo biyo nadiif ah si ay u soo dedejiyaan alaabta, shaandheeya nuugista, ku maydh biyo deionized dhowr jeer ilaa eluate waa hanti dhexdhexaad ah, kaydi alaabta qalalan.

1.4 Go'aaminta infrared spectroscopy

Hydroxypropyl methylcellulose, hydroxypropyl methylcellulose acetate, hydroxypropyl methylcellulose propionate iyo KBr ayaa la isku daray oo la isku daray, ka dibna lagu riixay kiniinno si loo go'aamiyo spectrum infrared.

1.5 Go'aaminta heerka beddelka

U diyaari xalalka NaOH iyo HCl oo leh 0.5 mol/L, oo ​​samee qiyaasid si loo go'aamiyo diiradda saxda ah; Miisaanka 0.5 g oo ah hydroxypropylmethylcellulose acetate (hydroxypropylmethylcellulose propionic acid ester) ee 250 mL Erlenmeyer galaas, ku dar 25 mL oo acetone ah iyo 3 dhibcood oo phenolphthalein tusaha, si fiican u qas, ka dibna ku dar 25 mL of NaOH xal electromagnetic, walaaq iyo saponre. 2 saac; titrate leh HCI ilaa midabka cas ee xalku baaba'o, qor mugga V1 (V2) ee hydrochloric acid la isticmaalo; Isticmaal isla habkan si aad u cabbirto mugga V0 ee hydrochloric acid ee ay isticmaasho hydroxypropyl methylcellulose, oo aad xisaabiso heerka beddelka.

1.6 Tijaabada xalalka

Qaado qadar habboon oo ah alaabta synthetic, ku dar dareeraha organic, wax yar rux, oo u fiirso kala dirida walaxda.

2. Natiijooyinka iyo doodaha

2.1 Saamaynta qaddarka pyridine (millaha)

Saamaynta qiyaasaha kala duwan ee pyridine ee qaab-dhismeedka hydroxypropylmethylcellulose acetate iyo hydroxypropylmethylcellulose propionate. Marka qadarka dareeruhu uu yaraado, waxay hoos u dhigi doontaa xoojinta silsiladda macromolecular iyo viscosity ee nidaamka, si heerka esterification ee nidaamka falcelinta la dhimi doono, iyo badeecada waxaa lagu soo dajin doonaa sida tiro badan. Oo marka qadarka dareeruhu aad u yar yahay, fal-celinta way fududahay in lagu dhejiyo buro oo ku dhegto gidaarka weelka, taas oo aan u fiicnayn oo kaliya fulinta falcelinta, laakiin sidoo kale waxay keentaa dhib weyn daaweynta ka dib falcelinta. . Marka la isku daro hydroxypropyl methylcellulose acetate, qadarka dareeraha la isticmaalo waxaa loo dooran karaa 150 mL / 2 g; isku dhafka hydroxypropyl methylcellulose propionate, waxaa loo dooran karaa 80 mL/0.5 g.

2.2 Falanqaynta infrared spectrum

Shaxda isbarbardhigga infrared ee hydroxypropyl methylcellulose iyo hydroxypropyl methylcellulose acetate. Marka la barbardhigo alaabta ceeriin, spectrogram infrared ee alaabta hydroxypropyl methylcellulose acetate ayaa leh isbeddel muuqda. Infrared spectrum ee alaabta, ugu sarreeya ayaa ka soo muuqday 1740cm-1, taas oo muujinaysa in koox kaarboonyl ah la soo saaray; Intaa waxaa dheer, xoojinta gariirka fidinta ee OH ee 3500cm-1 ayaa aad uga hooseeya kan alaabta ceeriin, taas oo sidoo kale muujisay -OH Waxaa jiray falcelin.

spectrogram-ka infrared ee badeecada hydroxypropyl methylcellulose propionate ayaa sidoo kale si weyn isu bedelay marka la barbar dhigo alaabta ceeriin. Infrared spectrum ee alaabta, ugu sarreeya ayaa ka soo muuqday 1740 cm-1, taas oo muujinaysa in koox kaarboonyl ah la soo saaray; Intaa waxaa dheer, xoojinta gariirka fidinta OH ee 3500 cm-1 aad ayuu uga hooseeyaa kan alaabta ceyriinka ah, kaas oo sidoo kale tilmaamay in OH ay ka falcelisay.

2.3 Go'aaminta heerka beddelka

2.3.1 Go'aaminta heerka beddelka ee hydroxypropyl methylcellulose acetate

Maadaama hydroxypropyl methylcellulose uu leeyahay laba hal OH cutub kasta, iyo acetate cellulose waa badeecad la helay iyadoo lagu beddelayo hal COCH3 H hal OH, heerka ugu sarreeya ee beddelka (Ds) waa 2.

2.3.2 Go'aaminta heerka beddelka hydroxypropyl methylcellulose propionate

2.4 milanka alaabta

Labada walxood ee la sameeyay waxay lahaayeen astaamo isku mid ah oo milmayneed, iyo hydroxypropyl methylcellulose acetate ayaa waxoogaa ka milmay hydroxypropyl methylcellulose propionate. Alaabta synthetic waxaa lagu milmi karaa acetone, ethyl acetate, acetone/biyo dareere isku dhafan, oo leh xulasho badan. Intaa waxaa dheer, qoyaanka ku jira dareeraha isku-dhafka ah ee acetone/biyaha ayaa ka dhigi kara ka-faa'iideystayaasha cellulose mid ammaan ah oo deegaanka u wanaagsan marka loo isticmaalo sida alaabta dahaadhka ah.

3. Gabagabo

(1) Xaaladaha isku dhafan ee hydroxypropyl methylcellulose acetate waa sida soo socota: 2.5 g of hydroxypropyl methylcellulose, acetic anhydride sida wakiilka esterification, 150 mL of pyridine sida dareeraha, heerkulka falcelinta ee 110° C, iyo waqtiga falcelinta 1 saac.

(2) Xaaladaha isku dhafan ee hydroxypropyl methylcellulose acetate waa: 0.5 g of hydroxypropyl methylcellulose, propionic anhydride sida wakiilka esterification, 80 mL of pyridine sida dareeraha, heerkulka falcelinta at 110°C, iyo waqtiga falcelinta oo ah 2.5 saacadood.

(3) Qaybaha cellulose ee lagu sameeyay xaaladdan ayaa si toos ah u qaabaysan qaab budo ganaax ah oo leh heer wanaagsan oo beddelaad ah, labadan nooc ee cellulose-ka ayaa lagu milmi karaa dareerayaasha kala duwan ee organic sida ethyl acetate, acetone, iyo acetone / biyaha.