Haɗin gwiwar Hydroxypropyl Methyl Cellulose Acetate da Propionate

Yin amfani da hydroxypropyl methylcellulose (HPMC) a matsayin albarkatun kasa, acetic anhydride da propionic anhydride a matsayin esterification jamiái, da esterification dauki a pyridine shirya hydroxypropyl methylcellulose acetate da hydroxypropyl methylcellulose Cellulose propionate. Ta hanyar canza adadin sauran ƙarfi da aka yi amfani da su a cikin tsarin, an sami samfur tare da mafi kyawun kaddarorin da digiri na maye gurbin. An ƙaddara matakin maye gurbin ta hanyar titration, kuma samfurin an siffata kuma an gwada shi don aiki. Sakamakon ya nuna cewa an mayar da martani ga tsarin amsawa a 110°C don 1-2.5 h, kuma an yi amfani da ruwan da aka lalata a matsayin wakili mai tasowa bayan amsawa, kuma ana iya samun samfurori na foda tare da digiri na maye gurbin fiye da 1 (digiri na ka'idar maye gurbin shine 2). Yana da kyau solubility a daban-daban Organic kaushi kamar ethyl ester, acetone, acetone / ruwa, da dai sauransu.

Mabuɗin kalmomi: hydroxypropyl methylcellulose; hydroxypropyl methylcellulose acetate; hydroxypropyl methylcellulose propionate

Hydroxypropylmethylcellulose (HPMC) wani fili ne na polymer wanda ba na ionic ba da ether cellulose tare da fa'idar amfani. A matsayin ingantaccen ƙari na sinadarai, ana amfani da HPMC sau da yawa a fannoni daban-daban kuma ana kiransa "monosodium glutamate masana'antu". Hydroxypropyl methylcellulose (HPMC) ba wai kawai yana da kyawawan emulsifying, thickening, da kuma ɗaure ayyuka ba, amma kuma ana iya amfani dashi don kula da danshi da kare colloid. Ana amfani da shi sosai a fannoni da yawa kamar abinci, magani, sutura, masaku, da noma. . Gyaran hydroxypropyl methylcellulose na iya canza wasu kaddarorinsa, ta yadda za a iya amfani da shi mafi kyau a wani fanni. Tsarin kwayoyin halittar monomer ɗin sa shine C10H18O6.

A cikin 'yan shekarun nan, bincike kan abubuwan da suka samo asali na hydroxypropyl methylcellulose ya zama wuri mai zafi a hankali. Ta hanyar gyaggyarawa hydroxypropyl methylcellulose, ana iya samun nau'o'in mahadi daban-daban tare da kaddarorin daban-daban. Alal misali, gabatarwar ƙungiyoyin acetyl na iya canza sassaucin fina-finai na likitanci.

Ana yin gyare-gyaren hydroxypropyl methylcellulose yawanci a gaban mai kara kuzari na acid kamar sulfuric acid. Gwajin yawanci yana amfani da acetic acid azaman sauran ƙarfi. Yanayin amsawa yana da wahala kuma yana ɗaukar lokaci, kuma samfurin da ya haifar yana da ƙaramin matsayi na maye gurbin. (kasa da 1).

A cikin wannan takarda, an yi amfani da acetic anhydride da propionic anhydride a matsayin wakilai na esterification don gyara hydroxypropyl methylcellulose don shirya hydroxypropyl methylcellulose acetate da hydroxypropyl methylcellulose propionate. Ta hanyar binciko yanayi kamar zaɓin ƙarfi (pyridine), adadin ƙarfi, da sauransu, ana fatan za a iya samun samfur tare da mafi kyawun kaddarorin da digiri na maye gurbin ta hanya mai sauƙi. A cikin wannan takarda, ta hanyar bincike na gwaji, samfurin da aka yi niyya tare da ƙwayar foda da kuma digiri na maye gurbin fiye da 1 an samu, wanda ya ba da wasu jagorar ka'idar don samar da hydroxypropyl methylcellulose acetate da hydroxypropyl methylcellulose propionate.

1. Bangaren gwaji

1.1 Materials da reagents

Pharmaceutical sa hydroxypropyl methylcellulose (KIMA CHEMICAL CO., LTD, 60HD100, methoxyl taro juzu'i 28%-30%, hydroxypropoxyl taro juzu'i 7%-12%); acetic anhydride, AR, Sinopharm Group Chemical Reagent Co., Ltd .; Propionic Anhydride, AR, Yammacin Asiya Reagent; Pyridine, AR, Tianjin Kemiou Chemical Reagent Co., Ltd.; methanol, ethanol, ether, ethyl acetate, acetone, NaOH da HCl ana samunsu ta kasuwanci mai tsafta.

KDM thermostat lantarki dumama mantle, JJ-1A gudun auna dijital nuni lantarki stirrer, NEXUS 670 Fourier canza infrared spectrometer.

1.2 Shiri na hydroxypropyl methylcellulose acetate

An saka wani adadin pyridine a cikin kwandon wuyansa uku, sa'an nan kuma an ƙara 2.5 g na hydroxypropyl methylcellulose a ciki, masu amsawa suna motsawa daidai, kuma zafin jiki ya tashi zuwa 110.°C. Ƙara 4 ml na acetic anhydride, amsa a 110°C don 1 h, dakatar da dumama, sanyi zuwa zafin jiki, ƙara ruwa mai yawa don haɓaka samfurin, tace tare da tsotsa, wanke tare da ruwan da aka lalata sau da yawa har sai eluate ya kasance tsaka tsaki, kuma bushe samfurin ya ajiye.

1.3 Shiri na hydroxypropyl methylcellulose propionate

An saka wani adadin pyridine a cikin kwalba mai wuya uku, sa'an nan kuma an ƙara 0.5 g na hydroxypropyl methylcellulose a ciki, masu amsawa suna motsawa daidai, kuma zafin jiki ya tashi zuwa 110.°C. Ƙara 1.1 ml na propionic anhydride, amsa a 110°C don 2.5 h, dakatar da dumama, sanyi zuwa dakin da zafin jiki, ƙara yawan adadin ruwan da aka lalata don haɓaka samfurin, tacewa tare da tsotsa, wanke tare da ruwa mai laushi na sau da yawa har sai eluate ya zama matsakaiciyar dukiya, adana samfurin bushe.

1.4 Ƙaddamar da infrared spectroscopy

Hydroxypropyl methylcellulose, hydroxypropyl methylcellulose acetate, hydroxypropyl methylcellulose propionate da KBr an gauraye da ƙasa bi da bi, sa'an nan kuma danna cikin allunan don ƙayyade infrared bakan.

1.5 Tabbatar da matakin maye gurbin

Shirya mafita na NaOH da HCl tare da ƙaddamarwa na 0.5 mol / L, da aiwatar da daidaitawa don ƙayyade ainihin ƙaddamarwa; auna 0.5 g na hydroxypropylmethylcellulose acetate (hydroxypropylmethylcellulose propionic acid ester) a cikin 250 ml Erlenmeyer flask, ƙara 25 ml na acetone da 3 saukad da na phenolphthalein nuna alama, Mix da kyau, sa'an nan kuma ƙara 25 ml na NaOH bayani don motsawa da saponre. 2 h ; titrate tare da HCI har sai launin ja na maganin ya ɓace, rikodin ƙarar V1 (V2) na hydrochloric acid cinye; yi amfani da wannan hanyar don auna ƙarar V0 na hydrochloric acid da hydroxypropyl methylcellulose ke cinyewa, da ƙididdige matakin maye gurbin.

1.6 Gwajin narkewa

Ɗauki adadin da ya dace na samfuran roba, ƙara su zuwa ga kaushi na halitta, girgiza dan kadan, kuma lura da rushewar abu.

2. Sakamako da Tattaunawa

2.1 Sakamakon adadin pyridine (mai narkewa)

Tasirin adadi daban-daban na pyridine akan ilimin halittar jiki na hydroxypropylmethylcellulose acetate da hydroxypropylmethylcellulose propionate. Lokacin da adadin sauran ƙarfi ya ragu, zai rage girman sarkar macromolecular da danko na tsarin, don haka za a rage matakin esterification na tsarin amsawa, kuma samfurin zai haɓaka azaman babban taro. Kuma a lokacin da adadin sauran ƙarfi ya yi ƙasa da ƙasa, mai amsawa yana da sauƙi don tattarawa a cikin dunƙule kuma manne da bangon ganga, wanda ba kawai rashin jin daɗi ba ne don aiwatar da amsawa, amma kuma yana haifar da rashin jin daɗi ga jiyya bayan amsawa. . A cikin kira na hydroxypropyl methylcellulose acetate, adadin sauran ƙarfi da aka yi amfani da shi za a iya zaba a matsayin 150 ml / 2 g; don haɗin hydroxypropyl methylcellulose propionate, ana iya zaɓar shi azaman 80 ml / 0.5 g.

2.2 Binciken bakan infrared

Taswirar kwatanta Infrared na hydroxypropyl methylcellulose da hydroxypropyl methylcellulose acetate. Idan aka kwatanta da albarkatun ƙasa, infrared spectrogram na samfurin hydroxypropyl methylcellulose acetate yana da ƙarin canji a bayyane. A cikin bakan infrared na samfurin, ƙaƙƙarfan tsayi ya bayyana a 1740cm-1, yana nuna cewa an samar da ƙungiyar carbonyl; Bugu da kari, tsananin mikewa kololuwa na OH a 3500cm-1 ya kasance da yawa ƙasa da na albarkatun kasa, wanda kuma ya nuna cewa -OH Akwai wani dauki.

Siffar infrared na samfurin hydroxypropyl methylcellulose propionate shima ya canza sosai idan aka kwatanta da albarkatun ƙasa. A cikin nau'in infrared na samfurin, tsayi mai ƙarfi ya bayyana a 1740 cm-1, yana nuna cewa an samar da ƙungiyar carbonyl; Bugu da kari, OH mikewa kololuwar rawar jiki a 3500 cm-1 ya yi ƙasa da na albarkatun kasa, wanda kuma ya nuna cewa OH ya amsa.

2.3 Ƙaddamar da matakin maye gurbin

2.3.1 Ƙaddamar da matakin maye gurbin hydroxypropyl methylcellulose acetate

Tunda hydroxypropyl methylcellulose yana da OH guda biyu a kowace raka'a, kuma acetate cellulose samfuri ne da aka samu ta hanyar maye gurbin COCH3 ɗaya don H a cikin OH ɗaya, matsakaicin matsakaicin matakin maye gurbin (Ds) shine 2.

2.3.2 Tabbatar da matakin maye gurbin hydroxypropyl methylcellulose propionate

2.4 Solubility na samfurin

Abubuwan biyu da aka haɗa suna da halaye iri ɗaya na solubility, kuma hydroxypropyl methylcellulose acetate ya ɗan fi narkewa fiye da hydroxypropyl methylcellulose propionate. Za a iya narkar da samfurin roba a cikin acetone, ethyl acetate, acetone/ruwa gauraye sauran ƙarfi, kuma yana da ƙarin zaɓi. Bugu da kari, damshin da ke ƙunshe a cikin gaurayewar acetone/ruwa na iya sa abubuwan da suka samo asali na cellulose su zama mafi aminci da aminci ga muhalli idan aka yi amfani da su azaman kayan shafa.

3. Kammalawa

(1) Halin da ake kira hydroxypropyl methylcellulose acetate kamar haka: 2.5 g na hydroxypropyl methylcellulose, acetic anhydride a matsayin esterification wakili, 150 ml na pyridine a matsayin sauran ƙarfi, da dauki zazzabi a 110.° C, da lokacin amsawa 1 h.

(2) Halin da ake kira hydroxypropyl methylcellulose acetate shine: 0.5 g na hydroxypropyl methylcellulose, propionic anhydride a matsayin wakili na esterification, 80 ml na pyridine a matsayin mai narkewa, zazzabi mai zafi a 110.°C, da lokacin amsawa na 2.5h.

(3) Abubuwan da aka samo asali na cellulose da aka haɗa a ƙarƙashin wannan yanayin suna kai tsaye a cikin nau'i mai kyau tare da kyakkyawan matsayi na maye gurbin, kuma waɗannan nau'o'in cellulose guda biyu za a iya narkar da su a cikin nau'o'in kwayoyin halitta kamar ethyl acetate, acetone, da acetone / ruwa.