Studies on the Synthesis and Propeties of Polyimides; III. Effects of solvents on PMDA-Polyimides
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- Studies on the Synthesis and Propeties of Polyimides; III. Effects of solvents on PMDA-Polyimides
- Park, Lee Soon; Lee, Dong Ho; Son, In Hun; Koo, Seong Young
- Issue Date
- POLYMER SOC KOREA
- POLYMER-KOREA, v.13, no.6, pp.488 - 492
- Pyromellitic dianhydride (PMDA)와 4,4''-diaminodiphenylether (ODA) 혹은 benzidine (BZI)을 N-methyl-2-pyrrolidone (NMP) 또는 N,N-dimethylacetamide (DMAc)와 같은 극성용매에서 축합 중합시켜 얻은 polyamic acid (PAA)용액으로 필름을 제조하였으며 이를 전기로속에서 열이미드화시킬때 필름속에 남아있는 용매의 함량, 용매의 종류, 공용매의 종류 등에 따른 이미드화도의 변화를 조사하였다. 그 결과 DMAc용매를 사용하여 얻은 필름이 NMP용매를 사용한 경우보다 이미드화도가 크게 나타났으며 이런 현상은 공기존재나 질소기류하에서 같은 경향을 나타내었다. 또 diamine의 구조가 바뀌더라도 같은 경향을 보였다. 필름속에 남아있는 NMP의 잔류량이 변화되어도 진공하에서의 이미드화도는 비슷한 값을 나타내었으며 DMAc가 남아 있을 경우에도 유사한 결과를 볼 수 있었다. 공용매로 메탄올, 에탄올 및 톨루엔을 첨가하여 얻은 필름을 진공하에서 이미드화시킬 때에 공용매의 종류에 따라 이미드화도가 변화되었으며 적당한 공용매를 첨가하므로써 이미드화도를 증가시킬 수 있었다. 또 PAA 용액에 10%의 에탄올 또는 테트라히드로푸란을 첨가하여 시간에 따른 절도의 변화를 조사한 결과 이들 공용매가 PAA 용액의 안정세로 작용함을 알 수 있었다.
Polyamic acid(PAA) solution was prepared by the condensation polymerization of pyromellitic dianhydride (PMDA) and 4,4''-diaminodiphenylether (ODA) or benzidine (BZI) in a highly polar solvent such as N-methy1-2-pyrrolidone (NMP) or N,N-dimethyl acetamide (DMAc). The polyimide (PI) film was then obtained by the thermal imidization oa casted PAA film. For thermal imidization of PAA film obtained from PMDA and ODA, the effects of solvent i.e, the contents of solvent, the sorts of solvent and of cosolvents on the degree of imidization were investigated. It was found that the degree of imidization of which PAA film polymerized in DMAC was higher than that in NMP for the both conditions of under atmosphere and nitrogen flow. For the PAA film obtained from PMDA and BZI, the similar result was obtained. The degree of imidization was not much affected by the contents of NMP or DMAc in PAA film, however it was slightly changed by the addition of cosolvent such as methanol, ethanol or toluene. The addition of cosolvent such as ethanol or tetrahydrofuran was found to be used as a stabilizer of PAA solution from the observation of viscosity change with storage time.
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