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1一种新星型大分子——六对甲酰胺乙酸甲酯苯氧基环三磷腈的合成及其热性能、水解性能的表征显示文摘本文以六氯环三磷腈(HCCP)为原料合成了一种以甘氨酸甲酯苯氧基为侧基的新星型环三磷腈化合物六对甲酰胺乙酸甲酯苯氧基环三磷腈(HGPCP)及其中间体,并采用1HNMR,13CNMR,31PNMR,FTIR和元素分析技术对其结构进行了确认.通过TGA、DSC、FTIR技术和测定水解液的紫外光谱,水解残余物剩余质量,残余物的磷含量方法分别对化合物的热性能和水解性能进行了表征.通过比较HGPCP在酸碱环境下的水解结果,发现水解504h,样品的水解过程尚处于化合物侧链断裂阶段,其37℃在酸性缓冲溶液(pH1.0)下较中性缓冲溶液(pH1.0)更易水解.由于其可能在高温下生成交联结构,六对醛基苯氧基环三磷腈(HCPCP),六对羧基苯氧基环三磷腈(HCPCP)和HGPCP在800℃时碳残余量分别为75%、47%和47%,都表现出良好的热稳定性.邴柏春 李斌 2009中国科学(B辑)2009,39,12:4
2Synthesis,thermal property and hydrolytic degradation of a novel star-shaped hexa[p-(carbonylglycinomethylester)phenoxy]cyclotriphosphazene显示文摘A novel star-shaped cyclotriphosphazene substituted by glycinomethylesterphenoxy and its intermediates are synthesized from hexachlorocyclotriphosphazene (HCCP). The structures are characterized by 1H NMR,13C NMR,31P NMR,FTIR and elemental analysis. Their thermal properties are clarified by thermogravimetric analysis (TGA),differential scanning calorimentry (DSC) and FTIR,while hydrolytic degradation behaviour is studied with UV-vis spectrophotometer and by measuring the weight loss,and the phosphorus content of residue. According to hydrolysis behaviour of hexa[p-(carbonylglycinomethylester)phenoxy]cyclotriphosphazene (HGPCP) under different conditions,it is easy to hydrolyze in hydrochloric acid (pH 1.0) than in phosphate buffer (pH 7.4) at 37℃. And the sample hydrolytic degradation still remains at the stage of side groups' break. The TGA data show that the thermal stability of the hexa[p-(aldehyde)phenoxy]cyclotriphosphazene (HAPCP),hexa[p-(carboxyl) phenoxy]cyclotriphosphazene (HCPCP) and HGPCP is so high that their char residues are 75%,47% and 47% at 800℃,respectively,probably due to cross-linking between molecules.BING BaiChun LI Bin 2009Science China Chemistry2009,52,12:3
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