Journal of the Korean Industrial and Engineering Chemistry, Vol.15, No.1, 41-47, February, 2004
저독성 난연제를 첨가한 에폭시 수지의 경화 동력학 및 유변학적 특성
Cure Kinetics and Rheological Properties of Epoxy Resins Containing Low Toxicity Flame Retardant
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초록
본 실험에서는 2관능성 에폭시 수지(EP)에 저독성 난연제인 tris (chloroisopropyl) phosphate (TCPP)를 100:0 ~ 100:40 phr의 비율로 첨가한 후 이에 따른 경화 동력학과 유변학적 특성을 고찰하였다. 2EP/TCPP 시스템의 경화 활성화 에너지(Ea)와 전화량 (α)은 동적 DSC와 등온 DSC를 통하여 알아 보았으며, 유변학적 특성은 레오미터를 이용하여 등온 조건하에서 고찰하였다. 또한, 난연성 test인 UL94를 통하여 TCPP 함량에 따른 난연성의 변화를 살펴보았다. 실험 결과, Ea는 에폭시 수지 내에 TCPP의 함량이 증가할수록 증가하는 반면, 전화량(α)의 전환속도(d/dt)는 감소하는 경향을 나타내었다. 가교 활성화 에너지(Ec) 값은 구한 Ea값과 유사한 경향을 나타내었으며, 이러한 결과는 TCPP의 증가로 인해 2EP 고유의 interpenetrating polymer network (IPN) 구조형성이 방해받기 때문이라 판단된다. 또한, TCPP의 함량이 30 phr 이상인 경우 난연성이 향상되었는데, 이는 TCPP 내의 난연성을 갖는 인과 염소의 영향으로 판단된다.
In this work, the cure kinetics and rheological properties of difunctional epoxy (2EP) resins containing a low toxicity flame-retardant based on tris (chloroisopropyl) phosphate (TCPP) are investigated. The 2EP/TCPP content was varied within 100:0 ~ 100:40 phr. The cure activation energy (Ea) and conversion (α) of 2EP/TCPP system are examined using isothermal and dynamic DSC. The rheological properties of the system are studied under the isothermal condition using a rheometer. Also, the flame resistance is determined by UL94 vertical test. From experimental results, the Ea of 2EP/TCPP system is higher than that of pure 2EP. While, the conversion (α) and conversion rate (d/dt) are decreased with increasing of the TCPP content. The cross-linking activation energy (Ec) of the system is similar to Ea. This is probably due to the increase of TCPP content, which obstructs the formation of interpenetrating polymer network (IPN) structure of the 2EP. Also, the improvement of flame resistance is achieved by addition of 30 phr TCPP in the 2EP/TCPP system, which can be attributed to the existence of incombustible phosphorous and chlorines in the TCPP.
Keywords:difunctional epoxy resin (2EP);tris (chloroisopropyl) phosphate (TCPP);cure kinetics;rheological properties;flame resistance
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