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首页> 外文期刊>Polymer Degradation and Stability >Solid-state NMR on thermal and fire residues of bisphenol A polycarbonate/ silicone acrylate rubber/bisphenol A bis(diphenyl-phosphate)/(PC/SiR/BDP) and PC/SiR/BDP/zinc borate (PC/SiR/BDP/ZnB) - Part I: PC charring and the impact of BDP and ZnB
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Solid-state NMR on thermal and fire residues of bisphenol A polycarbonate/ silicone acrylate rubber/bisphenol A bis(diphenyl-phosphate)/(PC/SiR/BDP) and PC/SiR/BDP/zinc borate (PC/SiR/BDP/ZnB) - Part I: PC charring and the impact of BDP and ZnB

机译：对双酚A聚碳酸酯/硅丙烯酸酯橡胶/双酚A双（磷酸二苯酯）/（PC / SiR / BDP）和PC / SiR / BDP /硼酸锌（PC / SiR / BDP / ZnB）-第一部分：PC炭化以及BDP和ZnB的影响

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摘要

Structural changes in the condensed phase of bisphenol A polycarbonate (containing 0.45 wt% poly (tetrafluoroethylene))/silicone acrylate rubber/bisphenol A bis(diphenyl-phosphate) (PC/SiR/BDP) and PC/SiR/BDP/zinc borate (PC/SiR/BDP/ZnB) during thermal treatment in nitrogen atmosphere and in fire residues were investigated by solid-state NMR. ~1H, ~(11)B, ~(13)C and ~(31)P NMR experiments using direct excitation with a single pulse and ~1H-~(31)P cross-polarization (CP) were carried out including ~(31)P{~1H} and ~(13)C{~(31)P}double-resonance techniques (REDOR: Rotational Echo Double Resonance) on a series of heat-treated samples (580 K-850 K). Because many amorphous phases occur in the solid residues, and solid-state NMR spectroscopy addresses the most important sites carbon, phosphorus and boron, this paper is the key analytical approach for understanding the pyrolysis and flame retarding phenomenon in the condensed phase of PC/SiR/BDP and PC/SiR/BDP/ZnB. For the system PC/SiR/BDP it is shown that (i) at temperatures around 750-770 K (main decomposition step) carbonaceous charring of PC occurs and arylphosphate structures are still present, reacted in part with the decomposing PC; (ii) for higher temperatures from 770 K the phosphorus remaining in the solid phase increasingly converts to amorphous phosphonates and inorganic orthophosphates with a minor amount of crystalline orthophosphates; and (iii) ~1H-~(31)P{~1H} CP REDOR and ~H-~(31)C{~(31)P} CP REDOR NMR experiments suggest that the phosphates and phosphonates are bound via oxygen to aromatic carbons, indicating the interaction with the carbonaceous char. When ZnB is added to the system PC/SiR/BDP, (i) ZnB leads to a slightly enhanced PC decomposition for temperatures below 750 K; (ii) α-Zn_3(PO_4)_2 and borophosphate (BPO4) are formed in small amounts at high temperatures suggesting a reaction between BDP and ZnB during thermal decomposition; and (iii) most of the borate remains in the solid residues, forming an amorphous pure borate network, with the BO3/BO4 ratio increasing with higher temperatures. The NMR data of thermal and fire residues are highly correlated, underlining the importance of this work for understanding the pyrolysis and flame retardancy mechanisms in the condensed phase during the burning of the PC/SiR blends.
机译：双酚A聚碳酸酯（含0.45 wt％聚四氟乙烯）/丙烯酸硅橡胶/双酚A双（磷酸二苯酯）（PC / SiR / BDP）和PC / SiR / BDP /硼酸锌（通过固态NMR研究了在氮气氛和火残留物中进行热处理期间的PC / SiR / BDP / ZnB）。使用单脉冲直接激发和〜1H-〜（31）P交叉极化（CP）进行了〜1H，〜（11）B，〜（13）C和〜（31）P NMR实验，包括〜（ 31）P {〜1H}和〜（13）C {〜（31）P}双共振技术（REDOR：旋转回波双共振），用于一系列热处理的样品（580 K-850 K）。由于固体残留物中存在许多无定形相，并且固态NMR光谱法可分析碳，磷和硼的最重要位置，因此，本文是理解PC / SiR冷凝相中热解和阻燃现象的关键分析方法。 / BDP和PC / SiR / BDP / ZnB。对于PC / SiR / BDP系统，显示（i）在750-770 K（主要分解步骤）温度下发生PC的碳质炭化，并且芳基磷酸盐结构仍然存在，与分解的PC部分反应； （ii）对于从770 K开始的较高温度，固相中残留的磷逐渐转化为无定形的膦酸酯和无机正磷酸盐，并带有少量的结晶正磷酸盐； （iii）〜1H-〜（31）P {〜1H} CP REDOR和〜H-〜（31）C {〜（31）P} CP REDOR NMR实验表明，磷酸盐和膦酸酯通过氧与芳族化合物键合碳，表明与碳质炭的相互作用。当在系统PC / SiR / BDP中添加ZnB时，（i）ZnB导致温度低于750 K时PC分解略有增强； （ii）在高温下少量形成α-Zn_3（PO_4）_2和硼磷酸盐（BPO4），表明BDP和ZnB在热分解过程中发生反应； （iii）大多数硼酸盐保留在固体残渣中，形成无定形的纯硼酸盐网络，BO3 / BO4比随温度升高而增加。热残渣和火残渣的NMR数据高度相关，强调了这项工作对于理解PC / SiR共混物燃烧过程中冷凝相中的热解和阻燃机理的重要性。

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  • 来源
    《Polymer Degradation and Stability》 |2010年第12期|p.2525-2533|共9页
  • 作者

    A. Karrasch; E. Wawrzyn; B. Schartel; C. Jaeger;

  • 作者单位

    BAM Federal Institute for Materials Research and Testing, Division 1.3, Richard-Willstaetter Str. 11, D-12489 Berlin, Germany;

    BAM Federal Institute for Materials Research and Testing, Unter den Eichen 87, D-12205 Berlin, Germany;

    BAM Federal Institute for Materials Research and Testing, Unter den Eichen 87, D-12205 Berlin, Germany;

    BAM Federal Institute for Materials Research and Testing, Division 1.3, Richard-Willstaetter Str. 11, D-12489 Berlin, Germany;

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  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类
  • 关键词

    flame retardance; nmr; polycarbonate (PC) blends; bisphenol-a bis(diphenyl)phosPHAte (BDP); zinc borate;

    机译：阻燃性核磁共振聚碳酸酯（PC）混合物;双酚-a双（二苯基）膦（BDP）;硼酸锌;

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