阻燃剂对杨木抑烟效果的研究和机理探索
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摘要
为了探索阻燃工艺,获得良好的阻燃效果尤其是抑烟效果,同时改进无机阻燃剂吸湿性高和抗流失性能差的缺点,该研究使用氮磷系阻燃剂,选用不同的浸渍方法处理杨木,通过多种评价方法研究处理方式对杨木阻燃效果的影响。将不同浓度的氮磷系阻燃剂,添加不同比例的MH/ATH(Mg(OH)2/Al(OH)3)进行复配,采用微波加热后超声波浸渍的方法处理杨木,分析阻燃性能。采用纳米Si02溶胶对阻燃木材进行二次超声波浸渍,探究硅溶胶对杨木性能的改进效果。研究结果表明：
(1)应用微波加热处理1.5min,微波功率850W,超声波浸渍30min,处理温度40℃,超声功率500W,液料比10：1,15%氮磷阻燃液的工艺对杨木进行阻燃处理,边材和心材载药量达到94kg／m3和76kg／m3,浸渍深度分别为10.0mm和9.7mm,氧指数达68.4%和66.8%,阻燃性能良好。
(2)将氮磷阻燃剂与MH/ATH复配后,杨木的烟密度等级SDR均远小于75。20%和25%氮磷阻燃液添加10%的MH/ATH,有较好的抑烟效果。锥形量热仪测试表明,50kW／m2的辐射强度下,20%和25%氮磷阻燃液添加比例10%的MH／ATH能够明显降低阻燃木材的释热速率、释热总量、平均有效燃烧热和平均质量损失速率,质量损失速率最大降低60%,增加残炭量。环境扫描电镜分析,复配阻燃杨木燃烧后的炭层更加密实,残炭表面有熔融物覆盖,ATH与MH与氮磷阻燃剂的催化成炭作用相互辅助,有较好的阻燃协同作用。
(3)为了改善氮磷系阻燃剂及复配阻燃剂吸湿性较高的缺点,提高抗流失性能,采用纳米SiO2溶胶进行二次超声波浸渍,结果表明SiO2溶胶使阻燃杨木吸湿率降至1.15%,抗浸提值LRV提高至98%。
(4) TG-DTG热分析可得复配阻燃剂处理试件剩炭率可明显提高至35.5%。氮磷阻燃剂的催化脱水和催化成炭作用与MH/ATH分解氧化物膨胀隔氧和消烟作用具有良好的协同效果。ATH与SiO2结合后,在催化成炭方面优于MH。
(5) FTIR分析可得,硅溶胶浸渍试样在800cm-1处出现CH2-Si-CH2-申缩振动吸收峰；在1050-1060cm-1处出现Si-O-C伸缩振动吸收峰；在1100cm-1处出现Si-O-Si特征吸收峰,表明纳米二氧化硅粒子和复合木材发生了有效的化学结合。
In order to explore the flame retardant technology, obtain good flame retardant effect especially smoke suppression effect and improve disadvantages such as high hygroscopicity and poor anti erosion performance of inorganic flame retardant, nitrogen-phosphorus flame retardant was used to impregnate Poplar with different treatment method. Fire retardant effect was evaluated through a variety of measurements. Different concentrations of nitrogen-phosphorus-boron flame retardant agent were added with different proportion of MH/ATH(Mg(OH)2/A1(OH)3) by ultrasonic impregnation treatment after microwave heating. Flame retardant properties were analyzed. Nano SiO2sol was impregnated on the crude material and fire retardant wood with the same ultrasonic method and the improved effect of silica sol on Poplar was studied. The results were showed as follows:
There were significant differences between different treatment methods. The application of microwave heating time of1.5min at microwave power of850W and ultrasonic immersion30min at40℃with an ultrasonic power of500W was better for impreganation of poplar at the ratio of liquid to solid was10:1. Drug loading of sapwood and heartwood was up to94kg/m3and76kg/m3, while impregnation depth was respectively10.0mm and9.7mm when treated with15%nitrogen-phosphorus flame retardant liquid. Good flame retardant property was observed with oxygen index of treated Poplar up to68.4%and66.8%.
When nitrogen-phosphorus-boron flame retardant was blended with MH/ATH, SDR of all samples was far less than75.20%NP+10%MH/ATH and25%NP+10%MH/ATH treated Poplar had good effect of smoke suppression. The cone calorimeter test showed that, with the radiation intensity of50kW/m, heat release rate, total heat release, average effective heat of combustion and average mass loss rate of20%NP+10%MH/ATH and25%NP+10%MH/ATH could be significantly reduced and the mass loss rate was decreased by60%as well as charcoal yield increased. Analysis of environmental scanning electron microscope indicated that structure of char after burning was denser after blended flame retardant treatment and surface of char was covered by molten layer, which showed that ATH and MH decomposed and formed expansion layer in combustion. Catalytic char forming effect of nitrogen-phosphorus-boron flame retardant had synergistic flame retardant effect with MH/ATH.
In order to improve higher moisture absorption and worse anti-loss performance of nitrogen-phosphorus flame retardant agent and compound flame retardant, nano silica sol was used in this study with method of ultrasonic impregnation. It was found the SiO2sol could significantly improve the properties of flame retardant Poplar. Moisture absorption rate was decreased to1.15%and LRV reached as high as98%
TG-DTG thermal analysis indicated char yield of blended flame retardant treatment samples significantly increased to35.5%. Fire retardance of Poplar was significantly improved by the blended flame retardant. Catalytic dehydration and catalytic carbon effect of nitrogen-phosphorus-boron flame retardant had good cooperative effect with the oxygen barrier and smoke suppression effect of the expansion oxide decomposition of MH/ATH. Catalytic charring effect of ATH combined with SiO? was better than that of MH.
FTIR showed that small absorption in800cm-1wave number was CH2-Si-CH2stretching vibration in silica sol specimens, the1050-1060cm-1absorption peak was Si-O-C bond, the1100cm-1absorption peak was Si-O-Si bond. These confirmed nano silica particles and composite wood had effective chemical combination.
(1)应用微波加热处理1.5min,微波功率850W,超声波浸渍30min,处理温度40℃,超声功率500W,液料比10：1,15%氮磷阻燃液的工艺对杨木进行阻燃处理,边材和心材载药量达到94kg／m3和76kg／m3,浸渍深度分别为10.0mm和9.7mm,氧指数达68.4%和66.8%,阻燃性能良好。
(2)将氮磷阻燃剂与MH/ATH复配后,杨木的烟密度等级SDR均远小于75。20%和25%氮磷阻燃液添加10%的MH/ATH,有较好的抑烟效果。锥形量热仪测试表明,50kW／m2的辐射强度下,20%和25%氮磷阻燃液添加比例10%的MH／ATH能够明显降低阻燃木材的释热速率、释热总量、平均有效燃烧热和平均质量损失速率,质量损失速率最大降低60%,增加残炭量。环境扫描电镜分析,复配阻燃杨木燃烧后的炭层更加密实,残炭表面有熔融物覆盖,ATH与MH与氮磷阻燃剂的催化成炭作用相互辅助,有较好的阻燃协同作用。
(3)为了改善氮磷系阻燃剂及复配阻燃剂吸湿性较高的缺点,提高抗流失性能,采用纳米SiO2溶胶进行二次超声波浸渍,结果表明SiO2溶胶使阻燃杨木吸湿率降至1.15%,抗浸提值LRV提高至98%。
(4) TG-DTG热分析可得复配阻燃剂处理试件剩炭率可明显提高至35.5%。氮磷阻燃剂的催化脱水和催化成炭作用与MH/ATH分解氧化物膨胀隔氧和消烟作用具有良好的协同效果。ATH与SiO2结合后,在催化成炭方面优于MH。
(5) FTIR分析可得,硅溶胶浸渍试样在800cm-1处出现CH2-Si-CH2-申缩振动吸收峰；在1050-1060cm-1处出现Si-O-C伸缩振动吸收峰；在1100cm-1处出现Si-O-Si特征吸收峰,表明纳米二氧化硅粒子和复合木材发生了有效的化学结合。
In order to explore the flame retardant technology, obtain good flame retardant effect especially smoke suppression effect and improve disadvantages such as high hygroscopicity and poor anti erosion performance of inorganic flame retardant, nitrogen-phosphorus flame retardant was used to impregnate Poplar with different treatment method. Fire retardant effect was evaluated through a variety of measurements. Different concentrations of nitrogen-phosphorus-boron flame retardant agent were added with different proportion of MH/ATH(Mg(OH)2/A1(OH)3) by ultrasonic impregnation treatment after microwave heating. Flame retardant properties were analyzed. Nano SiO2sol was impregnated on the crude material and fire retardant wood with the same ultrasonic method and the improved effect of silica sol on Poplar was studied. The results were showed as follows:
There were significant differences between different treatment methods. The application of microwave heating time of1.5min at microwave power of850W and ultrasonic immersion30min at40℃with an ultrasonic power of500W was better for impreganation of poplar at the ratio of liquid to solid was10:1. Drug loading of sapwood and heartwood was up to94kg/m3and76kg/m3, while impregnation depth was respectively10.0mm and9.7mm when treated with15%nitrogen-phosphorus flame retardant liquid. Good flame retardant property was observed with oxygen index of treated Poplar up to68.4%and66.8%.
When nitrogen-phosphorus-boron flame retardant was blended with MH/ATH, SDR of all samples was far less than75.20%NP+10%MH/ATH and25%NP+10%MH/ATH treated Poplar had good effect of smoke suppression. The cone calorimeter test showed that, with the radiation intensity of50kW/m, heat release rate, total heat release, average effective heat of combustion and average mass loss rate of20%NP+10%MH/ATH and25%NP+10%MH/ATH could be significantly reduced and the mass loss rate was decreased by60%as well as charcoal yield increased. Analysis of environmental scanning electron microscope indicated that structure of char after burning was denser after blended flame retardant treatment and surface of char was covered by molten layer, which showed that ATH and MH decomposed and formed expansion layer in combustion. Catalytic char forming effect of nitrogen-phosphorus-boron flame retardant had synergistic flame retardant effect with MH/ATH.
In order to improve higher moisture absorption and worse anti-loss performance of nitrogen-phosphorus flame retardant agent and compound flame retardant, nano silica sol was used in this study with method of ultrasonic impregnation. It was found the SiO2sol could significantly improve the properties of flame retardant Poplar. Moisture absorption rate was decreased to1.15%and LRV reached as high as98%
TG-DTG thermal analysis indicated char yield of blended flame retardant treatment samples significantly increased to35.5%. Fire retardance of Poplar was significantly improved by the blended flame retardant. Catalytic dehydration and catalytic carbon effect of nitrogen-phosphorus-boron flame retardant had good cooperative effect with the oxygen barrier and smoke suppression effect of the expansion oxide decomposition of MH/ATH. Catalytic charring effect of ATH combined with SiO? was better than that of MH.
FTIR showed that small absorption in800cm-1wave number was CH2-Si-CH2stretching vibration in silica sol specimens, the1050-1060cm-1absorption peak was Si-O-C bond, the1100cm-1absorption peak was Si-O-Si bond. These confirmed nano silica particles and composite wood had effective chemical combination.
引文
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