Caged bicyclic phosphate (CBP) and its dimelamine salt (PDS) were synthesized and added to epoxy resins to obtain the flame retarded epoxy resin composites. The flammability of the composites was characterized by ...Caged bicyclic phosphate (CBP) and its dimelamine salt (PDS) were synthesized and added to epoxy resins to obtain the flame retarded epoxy resin composites. The flammability of the composites was characterized by the limiting oxygen index (LOI) and cone calorimeter tests. The LOI values of flame retarded composites increase consistently with the increase of flame retardant amounts, and they are almost the same when the loading of CBP is the same as that of PDS, although the phosphorus content of PDS is much lower than that of CBP. The total heat release increases in the order of CBP30/ER 〈 PDS30/ER 〈 PDS15/ER 〈 CBPI5/ER, whereas that of specific extinction area is CBP15/ER 〉 CBP30/ER 〉 PDS30/ER ≌ PDS15/ER. PDS exhibits more effective inhibition of oxidation of combustible gases. In the tests of thermogravimetric analyses (TG) and Fourier transform infrared spectroscopy (FT-IR), it is found that the degradation of the composites is influenced greatly by the addition of flame retardants. By scanning electron microscopy (SEM), a thick and tight char-layer is observed for PDS30/ER, resulting from the interaction of nitrogen species with phosphorus species. Therefore, the combination of CBP with melamine in the flame retarded system can improve the flame retardancy greatly.展开更多
Amphiphilic alkyl (dodecyl and hexadecyl)-2-hydroxy-3-chloropropyl phosphates (C 12 - and C 16 -AHCP) were synthesized, and then alkyl glycidyl phosphates (C 12 - and C 16 -AGP) were quantitatively obtained by the tre...Amphiphilic alkyl (dodecyl and hexadecyl)-2-hydroxy-3-chloropropyl phosphates (C 12 - and C 16 -AHCP) were synthesized, and then alkyl glycidyl phosphates (C 12 - and C 16 -AGP) were quantitatively obtained by the treatment of AHCP with NaOH in order to prepare a novel vesicle which has reactive and polymerizable epoxy group on its membrane surface. The bilayer vesicles were formed by ultrasonication of aqueous dispersion of C 16 -AHCP or C 16 -AGP, but the vesicles composed of C 12 -AHCP and C 12 -AGP were not obtained by the same treatment. Both of C 16 -AHCP and C 16 -AGP bilayer vesicles are only stable at pH 5—10 or the ionic strength below 0.15. The gel-filtration chromatography and the UV-Vis absorption spectroscopic studies on Co(Ⅱ) tetrakis(propyloxycarbonyl)phthalocyanine as a lipophilic probe indicated that the phthalocyanine was effectively incorporated into the C 16 -AHCP bilayer membranes and predominantly present in a monomeric state in the membranes, which is much different from its leading diameric state in SDS micelle and ethanol.展开更多
环氧树脂的磷酸化是制备水溶性环氧树酯的一种新的途径。研究了五氧化二磷磷酸化环氧树脂的工艺条件,讨论了温度、时间、投料比等因素对环氧树脂磷酸化过程的影响,利用红外光谱对合成的产物进行了结构表征,并对其水乳液的性能进行了测...环氧树脂的磷酸化是制备水溶性环氧树酯的一种新的途径。研究了五氧化二磷磷酸化环氧树脂的工艺条件,讨论了温度、时间、投料比等因素对环氧树脂磷酸化过程的影响,利用红外光谱对合成的产物进行了结构表征,并对其水乳液的性能进行了测试。实验结果表明,所制备的产物为环氧磷酸酯类化合物,且具有较好的表面活性,其临界胶束浓度(cmc)为0.3%(质量分数),当乳液质量分数增大到临界胶束浓度以上时,气-液表面张力缓慢增大到44.2 m N/m并保持稳定;乳液质量分数在30%以下时,具有良好的机械稳定性,属假塑性流体。展开更多
通过氧指数、垂直燃烧、热失重、锥形量热和电镜扫描等研究了由双酚 A 双(磷酸二苯酯)(BDP)与聚磷酸铵(APP)组成的膨胀型阻燃剂对环氧树脂的阻燃性能和阻燃机理。结果表明,BDP/APP 膨胀型阻燃剂对环氧树脂有较好的阻燃性能,使环氧树脂...通过氧指数、垂直燃烧、热失重、锥形量热和电镜扫描等研究了由双酚 A 双(磷酸二苯酯)(BDP)与聚磷酸铵(APP)组成的膨胀型阻燃剂对环氧树脂的阻燃性能和阻燃机理。结果表明,BDP/APP 膨胀型阻燃剂对环氧树脂有较好的阻燃性能,使环氧树脂氧指数达到29.9%,垂直燃烧通过 UL94 V-0级,500℃残炭量达到34 8%,平均热释放速率下降70.7%,热释放速率峰值下降67.3%,有效燃烧热平均值下降24.1%。扫描电镜分析表明,经膨胀阻燃剂阻燃的环氧树脂燃烧后能够形成连续、致密、封闭、坚硬的焦化炭层。展开更多
基金This work was supported by the financial support of the Commission of Science and Technology of Shanghai Municipality(No.05nm05039 and No.05QMX1413).
文摘Caged bicyclic phosphate (CBP) and its dimelamine salt (PDS) were synthesized and added to epoxy resins to obtain the flame retarded epoxy resin composites. The flammability of the composites was characterized by the limiting oxygen index (LOI) and cone calorimeter tests. The LOI values of flame retarded composites increase consistently with the increase of flame retardant amounts, and they are almost the same when the loading of CBP is the same as that of PDS, although the phosphorus content of PDS is much lower than that of CBP. The total heat release increases in the order of CBP30/ER 〈 PDS30/ER 〈 PDS15/ER 〈 CBPI5/ER, whereas that of specific extinction area is CBP15/ER 〉 CBP30/ER 〉 PDS30/ER ≌ PDS15/ER. PDS exhibits more effective inhibition of oxidation of combustible gases. In the tests of thermogravimetric analyses (TG) and Fourier transform infrared spectroscopy (FT-IR), it is found that the degradation of the composites is influenced greatly by the addition of flame retardants. By scanning electron microscopy (SEM), a thick and tight char-layer is observed for PDS30/ER, resulting from the interaction of nitrogen species with phosphorus species. Therefore, the combination of CBP with melamine in the flame retarded system can improve the flame retardancy greatly.
文摘Amphiphilic alkyl (dodecyl and hexadecyl)-2-hydroxy-3-chloropropyl phosphates (C 12 - and C 16 -AHCP) were synthesized, and then alkyl glycidyl phosphates (C 12 - and C 16 -AGP) were quantitatively obtained by the treatment of AHCP with NaOH in order to prepare a novel vesicle which has reactive and polymerizable epoxy group on its membrane surface. The bilayer vesicles were formed by ultrasonication of aqueous dispersion of C 16 -AHCP or C 16 -AGP, but the vesicles composed of C 12 -AHCP and C 12 -AGP were not obtained by the same treatment. Both of C 16 -AHCP and C 16 -AGP bilayer vesicles are only stable at pH 5—10 or the ionic strength below 0.15. The gel-filtration chromatography and the UV-Vis absorption spectroscopic studies on Co(Ⅱ) tetrakis(propyloxycarbonyl)phthalocyanine as a lipophilic probe indicated that the phthalocyanine was effectively incorporated into the C 16 -AHCP bilayer membranes and predominantly present in a monomeric state in the membranes, which is much different from its leading diameric state in SDS micelle and ethanol.
文摘环氧树脂的磷酸化是制备水溶性环氧树酯的一种新的途径。研究了五氧化二磷磷酸化环氧树脂的工艺条件,讨论了温度、时间、投料比等因素对环氧树脂磷酸化过程的影响,利用红外光谱对合成的产物进行了结构表征,并对其水乳液的性能进行了测试。实验结果表明,所制备的产物为环氧磷酸酯类化合物,且具有较好的表面活性,其临界胶束浓度(cmc)为0.3%(质量分数),当乳液质量分数增大到临界胶束浓度以上时,气-液表面张力缓慢增大到44.2 m N/m并保持稳定;乳液质量分数在30%以下时,具有良好的机械稳定性,属假塑性流体。