침전법에 의한 폴리비닐부티랄의 제조 및 특성분석

서광원; 김덕준; Kwang Won Seo; Dukjoon Kim

Polymer(Korea), Vol.26, No.2, 168-173, March, 2002

Export Citation

침전법에 의한 폴리비닐부티랄의 제조 및 특성분석

Preparation of Poly(vinyl butyral) by Precipitation Method and Its Characterization

서광원, 김덕준 ^†

성균관대학교 화학공학과

Kwang Won Seo, and Dukjoon Kim^†

Department of Chemical Engineering, Sungkyunkwan University, Suwon, Kyungki 440-746, Korea

E-mail:

초록

폴리비닐알코올(PVA)을 부틸알데히드로 아세탈화하여 폴리비닐부티랄(PVB)을 합성하였다. PVB는 물을 용매로 침전법에 의하여 입자형태로 제조되었으며 생성된 PVB의 화학적 물리적 특성을 여러 방법을 이용하여 분석, 측정하였다. 제조된 PVB입자는 100∼700 μm의 입도분포내에서 약 380 μm의 평균입자크기를 나타내었다. PVB의 화학구조는 FT/IR과 NMR을 이용하여 확인할 수 있었으며 적정분석 결과 아세탈화정도는 약 77%로 나타났다. DSC 분석결과 PVA가 PVB로 아세탈화됨에 따라 PVA의 결정성이 사라졌으며, 유리전이온도가 70 ℃근처에서 나타났다. TGA 분석결과 제조된 PVB는 반응물인 PVA에 비해 열적으로 매우 안정하여 300 ℃까지 열분해를 보이지 않았다. 용해도 분석결과 PVB는 PVA와는 달리 알콜류에는 용해되었으나 물에는 용해되지 않았다.

Poly(vinyl butyral) (PVB) was synthesized by acetalization of poly(vinyl alcohol) (PVA). PVB was prepared in particulate forms in water, and chemical and physical properties of the products were characterized using various techniques. The prepared PVB had size distribution from 100 to 700 μm with mean diameter of about 380 μm. The chemical structure of PVB was characterized using FT/IR and NMR, and the average degree of acetalization was determined to be 77% from the titration measurement. DSC data showed that the crystalline structure of PVA vanished as acetalization reaction proceeded to produce PVB, and the glass transition temperature emerged at about 70 ℃. TGA data showed that PVB was much more thermally stable than PVA, and showed no degradation up to 300 ℃. Solubility test showed that PVB was soluble in alcohols but insoluble in water, being totally different from PVA.

Keywords:poly(vinyl butyral);precipitation;acetalization

[References]

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[Related Articles]

[1] Odian G, "Principle of Polymerization", 3rd ed., John Wiley & Sons, Canada, 711 (1991)

[2] Stevens MP, "Polymer Chemistry", Oxford Universtiy Press, 264 (1999)

[3] Mark HF, "Encyclopedia of Polymer Science and Engineering", 2nd ed., Wiley-Interscience, 17, 137 (1989)

[4] Leach LL, U. S. Patent 2,430,065 (1947)

[5] Bisch J, U.S. Patent 2,561,458 (1951)

[6] Gruber W, Heckmaier J, Zoebelein H, U.S. Patent 2,652,387 (1953)

[7] Shibata Y, Kodera Y, Tanaka M, Ohyamazaki FK, Ohtsu N, U.S. Patent 3,926,918 (1975)

[8] Kricheldorf HR, "Handbook of Polymer Synthesis", part B, Marcel Dekker Inc., New York, 1506 (1992)

[9] McMurry J, "Organic Chemistry", 4rh ed., ch19, Brooks/Cole Publishing Co., California (1995)

[10] Nicho ME, Hu H, Solar Energy Mater. Solar Cells., 63, 423 (2000)

[11] Salam LA, Matthews RD, Robertson H, J. Eu. Ceramic Soc., 20, 1375 (2000)

[12] El-Din NMS, Sabaa MW, Polym. Degrad. Stabil., 47, 283 (1995)

[13] Mark JE, "Polymer Data Handbook", Oxford University Press, New York, 915 (1999)