CN106336675B - 一种抑制沥青燃烧过程的复合阻燃剂配方及其制备方法 - Google Patents

一种抑制沥青燃烧过程的复合阻燃剂配方及其制备方法 Download PDF

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CN106336675B
CN106336675B CN201610838408.5A CN201610838408A CN106336675B CN 106336675 B CN106336675 B CN 106336675B CN 201610838408 A CN201610838408 A CN 201610838408A CN 106336675 B CN106336675 B CN 106336675B
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许涛
周培
石华泉
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Abstract

本发明目的是提供一种抑制道路沥青材料燃烧的复合阻燃剂配方及其制备方法，从而解决目前沥青阻燃剂阻燃效果差，不能对沥青燃烧全过程进行高效阻燃的问题。首先对沥青进行四组分试验，得到各组分含量；然后针对沥青各组分燃烧分解温度区间呈梯度分布特性，优选与各组分相匹配的环保型无机阻燃剂；再对已选的阻燃剂进行表面改性，并且确定每种阻燃剂的添加量及添加方法；最后根据热重试验结果，优化阻燃剂或复配阻燃剂掺加量，并按照沥青各组分含量对各阻燃剂进行复配，提出一种适应沥青多阶段燃烧行为的复合阻燃剂配方及其制备方法。本发明提供的方法能实现对沥青燃烧全过程进行高效阻燃，提高沥青路面火灾安全。

Description

一种抑制沥青燃烧过程的复合阻燃剂配方及其制备方法
技术领域
本发明是一种抑制道路沥青燃烧的复合阻燃剂配方及其制备方法，属于沥青路面火灾安全技术领域。
背景技术
随着我国高速公路的发展以及城镇化建设步伐的加快，隧道数量越来越多。与此同时隧道火灾事故也频频发生，有国外统计数据显示隧道火灾的发生频率为10～17次/亿车公里。究其原因，一方面是由于隧道处于半封闭状态，洞内外能见度差别较大且交通量和行车荷载日益增加；另一方面隧道多以沥青混合料为路面材料，而沥青是由碳、氢等元素组成的复杂高分子材料，本身易燃且会加剧隧道火灾的蔓延，还容易在燃烧过程中产生大量有毒烟气。已有研究表明，火灾中85％的人员死亡是由于吸入了有毒烟气。因此，了解沥青路面在隧道火灾过程中的危害，研究沥青的燃烧性能及其抑制方法具有重要的现实意义。
目前，国内外大量研究人员对沥青材料热解燃烧的详细过程和特性进行探索。但是，已有的研究均将沥青看做一个整体，而实际上沥青是一种多组分聚合物材料，按照现行有关规范四组分划分方法，沥青包括饱和分、芳香分、胶质和沥青质四种组分，各组分之间在化学成分、燃烧温度区间、燃烧性能、挥发物种类等方面存在明显的差异，不了解沥青各组分的燃烧性能，难以进一步揭示沥青燃烧的本质。
此外，国内外研究者们已逐步重视对抑烟、无毒、环保型无机阻燃剂进行研究。一方面以无机阻燃剂作为基本阻燃剂，另选择合适的无机材料制备成复合阻燃剂，并研究各阻燃剂之间的协同效应，来提高无机阻燃剂的阻燃效率；另一方面采用宏观试验方法来评价阻燃剂对沥青路用性能的影响以及与沥青相容性的问题。但是，目前的研究很少涉及各种环保型阻燃剂对沥青各组分燃烧动力学特性的影响，更没有深入研究沥青各组分燃烧特性的梯度分布特征和逸出气体挥发物的释放规律，揭示沥青各组分的燃烧特性对沥青燃烧性能的影响，并基于沥青组分的层面确定与各组分相匹配的环保型无机阻燃剂及其添加量，对所选取的无机阻燃剂进行复配，也鲜有研究复配阻燃剂在沥青及其混合料中微观分散机制，分析复配阻燃剂对沥青微观结构组成影响及配伍性。
因此，针对沥青各组分燃烧分解温度区间呈梯度分布特性，分别优选与其燃烧温度区间相匹配的环保型无机阻燃剂，对沥青各组分进行阻燃，再通过分析环保型阻燃剂对沥青各组分燃烧行为的影响，调整阻燃剂种类和配方，最终依据沥青各组分含量对所选阻燃剂进行复配，制备一种既能满足沥青阻燃要求，又能保证沥青以及沥青混合料路用性能的复合阻燃剂显得十分迫切。
发明内容
(1)技术问题
本发明目的是提供一种抑制道路沥青材料燃烧的复合阻燃剂配方及其制备方法，该方法针对沥青各组分燃烧分解温度区间呈梯度分布特性来选择与各组分燃烧特性相匹配的环保型无机阻燃剂，并确定其复配比例和制备方法，从而解决目前沥青阻燃剂成分单一、阻燃效果差、只能针对沥青某个燃烧阶段起到阻燃作用，不能对沥青燃烧全过程进行高效阻燃的问题。
(2)技术方案
首先对沥青进行四组分试验，制得沥青四组分，并测得各组分含量，如表1；然后根据沥青各组分的燃烧性能之间的差异，针对沥青各组分燃烧分解温度区间呈梯度分布特性，如表2，优选与沥青各组分燃烧温度相匹配的环保型无机阻燃剂，如表3；再对已选的阻燃剂进行表面改性，使其更好地与沥青各组分相容，并且确定每种阻燃剂的添加量及添加方法；再分析阻燃剂对沥青各组分燃烧性能的影响，对所选阻燃剂以及添加量进行调整；最后根据沥青各组分含量对各种阻燃剂进行复配，提出一种适应沥青多阶段燃烧行为的复合阻燃剂配方及其制备方法。
(3)有益效果
采用本发明提供的抑制道路沥青材料燃烧的复合阻燃剂配方及其制备方法，根据沥青各组分燃烧性能的差异性来选择与各组分燃烧特性相匹配的阻燃剂，再根据沥青各组分的含量制备高效复合阻燃剂。通过对复合阻燃改性沥青进行TG-DSC-FTIR联测后发现，添加复合阻燃剂后，沥青燃烧失重阶段从四个变为三个，复合阻燃改沥青的起始分解温度提高了25℃，各燃烧阶段的最大热失重分解温度均有不同程度的提高，复合材料在720℃的炭渣残留量为15.2wt％，这表明复合阻燃改性沥青具有较好的热稳定性；沥青的各燃烧阶段的吸放热量均有不同程度的减小，并且峰值温度也与TG曲线的最大燃烧温度相近；与高粘沥青相比，复合阻燃改性沥青燃烧第一阶段和第三阶段生成气体的释放量明显减少，说明阻燃剂的添加有效抑制了这两个阶段沥青燃烧气体的释放，复合阻燃剂具有较好的抑烟性能。最后，通过对复合阻燃改性沥青进行FESEM和EDS分析，发现添加复合阻燃剂后，沥青燃烧后形成了高质量的致密炭层，这种高质量的炭层极大的提高了沥青的热稳定性，并且可以承受住高温的破坏，有效地阻碍热量和氧气的进入以及可燃性气体的析出，从而起到较好的阻燃抑烟作用。
附表说明
表1沥青四组分含量
表2沥青四组分在空气气氛下燃烧的TG分析结果
表3阻燃剂在空气气氛下燃烧的TG分析结果
具体实施方式
本发明提供一种抑制沥青燃烧过程的复合阻燃剂制备方法，具体实施步如下：
(1)按照《公路工程沥青与沥青混合料试验规程》(JTG E20-2011)对所取沥青进行四组分试验，制备沥青四组分，测得各组分含量，对沥青各组分进行热重分析，明确沥青各组分燃烧温度区间及其梯度分布特征；
(2)针对沥青各组分燃烧温度区间呈梯度分布特性，选择与沥青各组分燃烧温度区间相匹配的环保型无机阻燃剂，初步确定饱和分的复配阻燃剂为膨胀型石墨/氢氧化铝＝1/2，芳香分的阻燃剂为膨胀型石墨/氢氧化镁＝1/4，胶质的阻燃剂为氢氧化钙，沥青质的复配阻燃剂为微胶囊红磷/氢氧化镁＝1/4；
(3)将选取的阻燃剂或复配阻燃剂放置于真空干燥箱中，温度为105℃±5℃，真空度93kPa±1kPa条件下干燥2h，取出后在干燥器中冷却至室温，用乙醇作为溶剂与钛酸酯偶联剂配成10％的溶液，将冷却的阻燃剂或复配阻燃剂放入配置的溶液中在常温下浸泡3h，取出阻燃剂或复配阻燃剂并放入真空干燥箱中干燥2h，取出后在干燥器中冷却至室温，从而对所选阻燃剂或复配阻燃剂进行表面偶联剂改性；
(4)先将一定量的沥青各组分和掺加量为10％的阻燃剂或复配阻燃剂置于真空干燥箱内，在温度为105℃±5℃，真空度93kPa±1kPa条件下干燥1h，将干燥的沥青各组分分别升温到160℃，缓慢加入掺加量为10％相应的阻燃剂或复配阻燃剂，手动搅拌5min，再采用高剪切分散机在165±5℃条件下先以1000rpm转速搅拌5min，然后用4000rpm转速搅拌20min，继续使用搅拌棒搅拌除去试样中的气泡，制取试验所需样品；
(5)根据热重试验结果，优化阻燃剂或复配阻燃剂掺加量，确定复合阻燃剂复配方案为膨胀型石墨/氢氧化铝/氢氧化镁/氢氧化钙/微胶囊红磷＝13∶8∶48∶9∶3，并将所需一定量的阻燃剂或复配阻燃剂置于封闭中的高速搅拌5分钟使各种阻燃剂或复配阻燃剂混合均匀，制备复合阻燃剂，用于对沥青进行阻燃改性，多阶段抑制沥青燃烧过程。

Claims (1)

1.一种抑制沥青燃烧过程的复合阻燃剂制备方法，其特征在于该方法的具体步骤如下：
(1)按照《公路工程沥青与沥青混合料试验规程》(JTG E20-2011)对所取沥青进行四组分试验，制备沥青四组分，测得各组分含量，对沥青各组分进行热重分析，明确沥青各组分燃烧温度区间及其梯度分布特征；
(2)针对沥青各组分燃烧温度区间呈梯度分布特性，选择与沥青各组分燃烧温度区间相匹配的环保型无机阻燃剂，初步确定饱和分的复配阻燃剂为膨胀型石墨/氢氧化铝＝1/2，芳香分的阻燃剂为膨胀型石墨/氢氧化镁＝1/4，胶质的阻燃剂为氢氧化钙，沥青质的复配阻燃剂为微胶囊红磷/氢氧化镁＝1/4；
(3)将选取的阻燃剂或复配阻燃剂放置于真空干燥箱中，温度为105℃±5℃，真空度93kPa±1kPa条件下干燥2h，取出后在干燥器中冷却至室温，用乙醇作为溶剂与钛酸酯偶联剂配成10％的溶液，将冷却的阻燃剂或复配阻燃剂放入配置的溶液中在常温下浸泡3h，取出阻燃剂或复配阻燃剂并放入真空干燥箱中干燥2h，取出后在干燥器中冷却至室温，从而对所选阻燃剂或复配阻燃剂进行表面偶联剂改性；
(4)先将一定量的沥青各组分和掺加量为10％的阻燃剂或复配阻燃剂置于真空干燥箱内，在温度为105℃±5℃，真空度93kPa±1kPa条件下干燥1h，将干燥的沥青各组分分别升温到160℃，缓慢加入掺加量为10％相应的阻燃剂或复配阻燃剂，手动搅拌5min，再采用高剪切分散机在165±5℃条件下先以1000rpm转速搅拌5min，然后用4000rpm转速搅拌20min，继续使用搅拌棒搅拌除去试样中的气泡，制取试验所需样品；
(5)根据热重试验结果，优化阻燃剂或复配阻燃剂掺加量，确定复合阻燃剂复配方案为膨胀型石墨/氢氧化铝/氢氧化镁/氢氧化钙/微胶囊红磷＝13∶8∶48∶9∶3，并将所需一定量的阻燃剂或复配阻燃剂置于封闭中的高速搅拌5分钟使各种阻燃剂或复配阻燃剂混合均匀，制备复合阻燃剂，用于对沥青进行阻燃改性，多阶段抑制沥青燃烧过程。
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