화학공학소재연구정보센터
Journal of the Korean Industrial and Engineering Chemistry, Vol.6, No.3, 492-500, June, 1995
수분산성 변성 알키드 수지의 합성과 특성 3.E-카프로락톤 변성 Oil Free 알키드의 합성과 물성
Synthesis and Characterization of Water-reducible Modified Alkyd Resin 3.Synthesis and Properties of ε-Caprolactone Modified Water-reducible Oil Free Alkyd Resin
초록
트리메틸올프로판(TMP), 1, 6-헥산디올(1, 6-HD) 및 이소프탈산(IPA)을 사용하여 기본적인 분지형 oil free 알키드를 합성하고, ε-카프로락톤을 개환 중합시켜 ε-카프로락톤 변성 알키드 수지를 합성하였다. 다시 트리멜리트산 무수물(TMA)을 반응시켜 음이온성기를 도입하고, N, N-디메틸에타놀아민(DMEA)으로 중화시켜 수분산화하여, ε-카프로락톤 변성 수분산성 oil free 알키드를 제조하였다. ε-카프로락톤 변성 알키드 수지의 상온(25℃)에서의 수용화 능력을 조사하기 위하여, TMP의 함량을 조절하여 알키드 수지를 합성하였으며, 상온(25℃)에서 투명한 수분산 용액이 되는 알키드 수지 영역에서 ε-카프로락톤을 첨가하여 개환 반응시켰다. ε-카프로락톤 모노머의 첨가량 변화에 의한 구조분석, 분자량, 유리전이온도, 반응율, 점성도 등의 물성 변화를 조사하였으며, 멜라민수지를 사용하여 가교 시킨 도막의 연필경도와 가공성 등의 변화를 조사하였다. TMP의 함량이 증가할수록 상전이 온도는 낮아졌으며, ε-카프로락톤의 첨가량이 증가할수록 분자량은 크게 변화하지 않았고, 점성도 변화는 고분형 55∼6owt%에서 감소하였다가 다시 증가하는 특성을 보였다. 반면에 유리전이온도는 낮아졌으며, 반응율은 촉매를 사용한 경우에 89.6∼92.7%었으며, 멜라민 경화막의 연필경도는 낮아지나 가공성은 증가하였다.
The basic ε-caprolactone modified oil free alkyd resin was synthesized from trimethylol propane(TMP), 1, 6-hexane diol(1, 6-HD), isophthalic acid(IPA) and trimellitic anhydride(TMA) by condensation polymerization at 220℃. ε-Caprolactone modified water-reducible oil free alkyd resins were synthesized with ε-caprolactone ring opening reaction onto the basic resin at 150℃. N, N'-Dimethylethanol amino(DMEA) was used as a neutralizing agent to prepare of the water-reducible oil free alkyd resin. The effect of TMP was studied by measuring clear point by using DSC. The effect of ε-caprolactone on the ring opening reaction of the resin was studied by measuring molecular weight, glass transition temperature(Tg), reaction efficiency, viscosity and flexibility, pencil hardness of melamine cured film. The clear pont was decreased according to the contents of TMA increased. The molecular weight was not much changed, and Tg was decreased according to the ε-caprolactone contents in the oil free alkyd resin increased. The viscosity was lower when the solid contents reached 55∼60wt% than that of 40∼45wt% content and the reaction efficiency was the range of 89.6∼92.7%. The pencil hardness of melamine cured film was decreased, but flexibility was increased according to the ε-caprolactone contents in the oil free alkyd resin increased.
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