Applied Chemistry for Engineering (공업화학)

The Korean Society of Industrial and Engineering Chemistry (한국공업화학회)
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Determination of Processing Parameters Affecting the Conversion and Thermal Stability of Photocurable Acrylate-based Binder

아크릴계 광바인더의 전환율과 열안정성 향상을 위한 공정변수 결정

  • 김병철 (한국생산기술연구원 청정공정소재연구그룹) ;
  • 서동학 (한양대학교 화학공학부) ;
  • 채헌승 (코오롱인더스트리) ;
  • 신승한 (한국생산기술연구원 청정공정소재연구그룹)
  • Published : 2012.02.10
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Abstract

Photocurable binder for a transparent glass fiber composite was prepared with alicyclic methacrylate and fluorene-based diacrylate. ANOVA (analysis of variance) analysis was used to know main factors affecting the conversion of photocurable binder. It showed radiation intensity and photoinitiator (PI) concentration were main factors. The conversion of photocurable binder was simply increased with radiation intensity. Its increment however was abated with increasing PI concentration. We found that average conversion of the binder measured by FTIR-ATR was 87% when it was exposed to $5J/cm^2$ of UV dose with 5 wt% of PI. Oxime ester type PI was very effective to get a high degree of conversion, but it caused a yellowing problem. Owing to post-baking process, UV cured film showed an improved thermal stability by increase of conversion and removal of volatile organic compounds. TG% at $260^{\circ}C$ of film cured with 5 wt% of PI (TPO+MBF) and $5J/cm^2$ of UV radiation increased from 95.4 to 99.0% by post-baking at $230^{\circ}C$ for 5 min.

투명 섬유복합체용 광경화성 바인더로 지환족 골격과 플루오렌계 골격을 갖는 아크릴계 수지 혼합물을 제조하여, 개시제의 종류 및 농도, 광량 등이 바인더의 전환율에 미치는 영향을 조사하였다. ANOVA 분석에 의하면, 바인더의 전환율 증가에는 광량, 개시제의 농도가 주요하였다. 광량에 대해 바인더의 전환율은 거의 선형적으로 증가하였고, 개시제 농도가 증가하게 되면 광량 증가에 따른 전환율 증가는 둔화되었다. FTIR-ATR을 이용하여 측정된 바인더의 평균 전환율은 개시제 농도 5 wt%, 광량 $5\;J/cm^2$의 조건에서는 87% 수준이었다. 옥심 에스테르계 개시제는 전환율 측면에서는 효과적이었으나, 황변현상을 초래하였다. 광경화 필름은 열처리에 의해 전환율이 증가하고, 휘발성 유기물이 제거되어 열안정성이 향상되었다. 한편, 트리메틸벤조일디페닐포스핀 옥시드와 메틸 벤조일포르메이트 혼합개시제 5 wt%, 광량 $5\;J/cm^2$ 조건에서 광경화된 필름은 $230^{\circ}C$, 5분 열처리로 TG% (@$260^{\circ}C$)가 95.4에서 99.0%로 증가하였다.

Keywords

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