紫外光固化型磷系阻燃劑之合成、動力學探討及熱性質分析

The Synthesis、Kinetics and Thermal Properties of UV curing Type Phosphorus Flame Retardant

丁逸恬(Yi-Tien Ting)

指導教授 ： 芮祥鵬

國立臺北科技大學/工程學院/有機高分子研究所/碩士(2013年)

摘要

本實驗之合成是將4-tert-butylphenyl dichlorophosphate （BPDCP）與2-Hydroxy Ethyl Acrylate(2-HEA)反應，形成末端帶有壓克力官能基之阻燃單體（BPDHA）。 使用FTIR、1HNMR及31PNMR鑑定其結構以確認反應完成。將BPDHA加入不同光起始劑濃度以及不同環境溫度下，利用DPA（Double Beam Photocalorimetric Accessory）測量其紫外光照射時光固化之放熱情形，經由放熱值計算其光固化轉化率（conversion）、反應速率（rate），探討光固化動力學反應參數之趨勢變化。將BPDHA與壓克力樹脂、稀釋單體依不同比例混合經由紫外光照光固化後，於熱重分析儀（TGA）測量在空氣及氮氣下之T5%及700℃之殘餘量來分析其熱穩定性；利用不同升溫速率測試，再經由Osawa’s method計算降解動力學，求得其降解活化能隨著BPDHA含量增加而降低，其升溫後所裂解之產物可藉由熱重-紅外線光譜儀（TG-IR）進行分析。燃燒性質可利用圓錐量熱儀及氧指數儀測得，依據CNS14705及ASTMD2863標準進行測試，當BPDHA含量達30%時限氧指數為26，已達到難燃材料之標準。使用鉛筆硬度計與百格刮刀在其物性方面作探討。

關鍵字

紫外光固化 ； 動力學 ； 阻燃劑 ； 熱性質

並列摘要

The acrylate of flame monomer (BPDHA) was been synthesised by allowing 4-tert-butylphenyl dichlorophosphate (BPDCP) to react with 2-HEA in this study. Its structure was characterized by FTIR, 1HNMR and 31PNMR. BPDHA was added into the solution with different concentration of photoinitiator and exposed to UV-light at different temperature, respectively in order to explore the effects of UV-curing kinetic, reaction order, rate and conversion. The major test equipment used in this experiment is DPA. BPDHA was blended with epoxy acrylate and diluent monomer at different ratios, and then cured with UV irradiation. It measurements T5% and residual at 700 ℃ by the thermal gravimetric analyzer (TGA) in nitrogen and air atmosphere to analyze its thermal stability. TGA tests in different heating rates is to calculate degradation kinetics by Osawa's method. The volatilized products during the thermal degradation of cured film were monitored by TG-IR respectively. The combustion properties was analyzed with cone calorimeter and oxygen index instrument, the tests was according to CNS14705 and ASTMD2863. Its physical properties was explored with pencil hardness test and cross-cut test.

並列關鍵字

UV curing ； Kinetic ； Flame Retardant ； Thermal Properties

參考文獻

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