磷钨酸插层ZnAl层状双金属氢氧化物协同膨胀阻燃剂对环氧-聚酰胺树脂的阻燃作用

Flame retardant effect of phosphotungstic acid intercalated ZnAl layered double hydroxides and intumescent flame retardant on epoxy-polyamide resin

  • 摘要: 采用PW12O403−离子柱撑插层共沉淀法合成的ZnAl硝酸根(NO3-ZnAl)层状双金属氢氧化物(LDHs),制备了PW12O40-ZnAl LDHs,并利用XRD、FTIR、电感耦合等离子体(ICP)、SEM等进行组成和结构的表征。将NO3-ZnAl LDHs和PW12O40-ZnAl LDHs分别与含聚磷酸铵、三聚氰胺、季戊四醇的膨胀阻燃剂(IFRs)复合阻燃环氧-聚酰胺树脂(EP-PA),采用TGA、背温实验和锥形量热实验评价不同ZnAl LDHs与IFRs复合阻燃EP-PA的热及烟气的释放规律。TGA结果表明,PW12O40-ZnAl-IFRs/(EP-PA)复合材料的最大降解速率最小,残炭率最高,说明PW12O40-ZnAl LDHs提高了IFRs/(EP-PA)复合材料高温下的抗氧化能力。背温实验表明,相同热辐射强度下,PW12O40-ZnAl-IFRs/(EP-PA)复合材料的背温达到200℃和300℃用时最长,具有最低的背温升温速率,说明PW12O40-ZnAl LDHs使IFRs/(EP-PA)复合材料耐火能力明显增强。从锥形量热实验数据可知,PW12O40-ZnAl-IFRs使PW12O40-ZnAl-IFRs/(EP-PA)复合材料具有最低的热释放速率峰值(PHRR)、平均热释放速率(MHRR)、平均有效燃烧热(MEHC)和总热释放量(THR),其火势增长指数(FGI)仅为IFRs/(EP-PA)复合材料的14.5%,烟释放总量(TSP)比NO3-ZnAl-IFRs/(EP-PA)复合材料减少了27.6%,比IFRs/(EP-PA)复合材料减少了55.3%。说明PW12O40-ZnAl-IFRs比NO3-ZnAl-IFRs更能有效地减少EP-PA的热量释放,抑制烟气生成。

     

    Abstract: The PW12O40-ZnAl layered double hydroxides(LDHs) was prepared by using PW12O403− ion pillared intercalation NO3-ZnAl LDHs. The composition and structure were analyzed by XRD, FTIR, inductively coupled plasma(ICP) and SEM. The flame retardant epoxy-polyamide resin(EP-PA) were prepared by NO3-ZnAl LDHs or PW12O40-ZnAl LDHs compound with intumescent flame retardants(IFRs) containing ammonium polyphosphate, melamine, pentaerythritol. The heat and smoke release rules of different ZnAl LDHs-IFRs flame retardant EP-PA were evaluated by back temperature experiment and cone calorimetry experiment. TGA result shows that the maximum degradation rate of PW12O40-ZnAl-IFRs/(EP-PA) composite is the lowest, and the carbon residue rate is the highest, which indicate that PW12O40-ZnAl LDHs improve the oxidation resistance of PW12O40-ZnAl-IFRs/(EP-PA) composite at high temperature. The back temperature experiment results show that under the same heat radiation intensity, the back temperature of PW12O40-ZnAl-IFRs/(EP-PA) composite reaches to 200℃ and 300℃ with the longest time and the lowest rate of back temperature rise. The results show that PW12O40-ZnAl LDHs can obviously enhance the fire resistance of EP-PA. From cone calorimetry experimental data, it can be seen that PW12O40-ZnAl-IFRs makes PW12O40-ZnAl-IFRs/(EP-PA) composite have the lowest peak of heat release rate(PHRR), mean heat release rate(MHRR), mean effective heat of combustion(MEHC) and total heat release(THR). Its fire growth index (FGI) is only 14.5% of IFRs/(EP-PA) composite, and the total smoke production (TSP) is 27.6% lower than NO3-ZnAl-IFRs/(EP-PA) composite and 55.3% lower than IFRs/(EP-PA) composite. The results suggest that PW12O40-ZnAl-IFRs is more effective than NO3-ZnAl-IFRs in reducing the heat release and inhibiting the generation of flue gas.

     

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