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Thermal,spectral and morphological studies on cellulose diisoamylaminophosphate in air

机译:空气中纤维素二异戊基氨基磷酸的热,光谱和形态研究

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The thermal behaviour of cellulose and cellulose diisoamylaminophosphate (CDAP) samples having different degrees of substitution have been studied using DTA and TG techniques from ambient temperature to 700 deg C in static air.The various reactions involved,namely,dehydration,dephosphorylation,dehydrohalogenation,oxidative decomposition and oxidation of charred residue,have been discussed.Brodio method is used to obtain various kinetic and thermodynamic parameters from TG curves for different stages of thermal degradation.The values of activation energies for the oxidative decomposition of CDAP samples are found to be in the range of 49.02-64.19 kJ mol~(-1) and are lower than that of cellulose (160.74 kJmol~(-1)).The IR spectra of the pyrolysis residues of CDAP indicate formation of compounds containing C=O,C=C and P=O groups.The EPR signals indicate that the free radical mechanism is not dominant in the degradation of CDAP.Higher char yields of CDAP samples as compared to cellulose along with related observations suggest that CDAP is an effective flame retardant.Scanning electron micrographs of CDAP show that the fibrillar reaction sites of cellulose have mostly reacted,although the general morphology of the original fibre remains intact.Internal axial cracking and the increased surface area in the chars of treated samples show the intumescent nature of CDAP.The mechanism of thermal degradation of CDAP has been proposed.
机译:使用DTA和TG技术在室温至700摄氏度的静态空气中研究了具有不同取代度的纤维素和纤维素二异戊基氨基磷酸(CDAP)样品的热行为。涉及的各种反应包括脱水,脱磷酸化,脱卤化氢,氧化讨论了焦化残渣的分解和氧化过程。溴化方法用于从TG曲线获得不同热降解阶段的各种动力学和热力学参数。发现CDAP样品氧化分解的活化能值在CDAP的热解残基的红外光谱表明形成了含C = O,C = C的化合物,其范围为49.02-64.19 kJ mol〜(-1),低于纤维素的160.74 kJmol〜(-1)。 EPR信号表明自由基机制在CDAP的降解中并不占主导地位。与纤维素酶相比,CDAP样品的焦炭产率更高以及相关的观察结果表明,CDAP是一种有效的阻燃剂。CDAP的扫描电子显微镜照片显示,尽管原纤维的一般形态保持完好,但纤维素的纤维状反应部位已发生了大部分反应。内部轴向开裂和表面积的增加经处理的样品的焦炭表现出CDAP的膨胀特性。提出了CDAP的热降解机理。

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