Mechanisms and performance of rejuvenated asphalt modified with wastt ire pyrolysis-derived carbon black clusters for airport pavement
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摘要: 针对机场道面在高温重载环境下的抗变形需求，以及轮胎裂解固相副产物的高值化利用问题，本文以轮胎胶粉热解残余物为原料制备再生炭黑胶团，并将其用于再生沥青的二次改性；设置基质沥青、短期老化沥青及炭黑改性再生沥青等试验组，采用热重-微分热重分析获取挥发分、碳质残留与灰分信息，并结合红外光谱与透射电镜分别分析再生炭黑胶团的表面官能团组成、颗粒形貌及聚集结构特征；通过动态剪切流变试验与多应力蠕变恢复试验评价改性再生沥青的高温承载稳定性与抗车辙能力。研究结果表明：再生炭黑胶团由碳质骨架、残余有机相与无机灰分构成，可通过界面相互作用与颗粒搭接在沥青基体中构建骨架网络；随再生处理强度提高，胶团结构趋于均质致密，无机残留呈现类填料增强效应；流变测试显示在45 ℃~64 ℃范围内，220炭胶沥青相较于多数对比组表现出较高模量和较低相位角，说明其弹性响应与抗变形能力同步提升；在0.1、3.2 kPa应力水平下，该沥青不可恢复蠕变柔量分别为3.04、3.28 kPa-1，恢复率分别为22.67%、13.60%，显示出较低的应力敏感性，表明其高温性能改善主要与结构网络的约束作用有关，并能够在重载循环条件下保持稳定。本文提出的基于热解副产固相的结构型改性策略，可为提升重载道面高温稳定性提供理论支撑与应用依据。Abstract: To meet the deformation resistance requirements of airport pavement under high-temperature and heavy-load conditions and to promote the value-added use of solid by-products from waste tire pyrolysis, recycled carbon black clusters were prepared from waste tire rubber pyrolysis residues and used for secondary modification of rejuvenated asphalt. Base asphalt, short-term aged asphalt, and carbon-black-modified rejuvenated asphalt were set as test groups. Thermogravimetry and derivative thermogravimetry were used to obtain information on volatile matter, carbonaceous residue, and ash. Fourier transform infrared spectroscopy and transmission electron microscopy were used to analyze the surface functional groups, particle morphology, and aggregation structure of the recycled carbon black clusters. Dynamic shear rheometry and multiple stress creep recovery tests were used to evaluate the high-temperature load-bearing stability and rutting resistance of the modified rejuvenated asphalt. Research results indicate that the recycled carbon black clusters consist of a carbonaceous skeleton, a residual organic phase, and inorganic components and can form a skeletal network in the asphalt matrix through interfacial interactions and particle bridging. With increasing treatment intensity, the cluster structure becomes more homogeneous and compact, and the inorganic residue shows a filler-like reinforcing effect. Rheological tests show that at 45 ℃-64 ℃, the rejuvenated asphalt modified with clusters treated at 220 ℃ exhibits a higher modulus and a lower phase angle than most comparison groups, indicating simultaneous improvements in elastic response and deformation resistance. At stress levels of 0.1 and 3.2 kPa, its non-recoverable creep compliances are 3.04 and 3.28 kPa-1, respectively, this asphalt recovery rates are 22.67% and 13.60%, respectively, indicating low stress sensitivity. These results suggest that the improved high-temperature performance is mainly associated with the constraint imposed by the structural network, which enables the material to remain stable under cyclic heavy-load conditions. The proposed structural modification strategy based on pyrolysis-derived solid residues can provide theoretical support and an application basis for improving the high-temperature stability of heavy-duty pavement.
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图 3 200再生炭黑胶团、220再生炭黑胶团、商用炭黑N330及废橡胶粉在回温程序下的TG-DTG曲线
Figure 3. TG-DTG curves of 200 ℃- and 220 ℃-treated recycled carbon black clusters, commercial carbon black N330, and waste tire rubber powder under programmed heating conditions
图 5 220再生炭黑胶团与商用炭黑N330在不同尺度下的透射电镜图像
Figure 5. Transmission electron microscope images of 220 ℃-treated recycled carbon black clusters and commercial carbon black N330 at different scales
图 6 不同沥青样品|G*|与δ随温度的变化曲线
Figure 6. Temperature variation curves of |G*| and δ for different asphalt samples
图 7 不同沥青样品在0.1、3.2 kPa应力水平下的累积应变响应及MSCR指标
Figure 7. Accumulated strain responses and MSCR indices of different asphalt samples at stress levels of 0.1 and 3.2 kPa
表 1 沥青常规技术指标
Table 1. Conventional technical properties of asphalt
沥青 25 ℃针入度/0.1 mm 软化点/℃ 10 ℃延度/cm 135 ℃黏度/(Pa·s) 基质沥青 67.9 48.8 19.2 0.520 短期老化沥青 50.2 53.8 14.2 0.878 
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表 2 废橡胶粉主要技术指标
Table 2. Main technical properties of waste tire rubber powder
% 组分 操作油 橡胶烃 炭黑 无机填料 C H N O S 质量分数 4.53 56.21 30.48 8.78 67.34 14.76 0.65 12.57 1.03
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表 3 废机油主要理化性质及元素组成
Table 3. Main physicochemical properties and elemental composition of waste engine oil
参数 酸值/(mg·g-1) 运动黏度/(mm2·s-1) 密度/(g·cm-3) 质量分数/% Zn P Al Pb Mo Cu 实测值 3.92 146.60 0.90 32.01 30.09 11.37 7.87 1.87 1.81
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表 4 固废轻质油制备参数
Table 4. Preparation parameters of solid waste light oil
条件 总质量/g 温度/℃ 时间/h 1 200 180 0.5 2 200 180 1.0 3 200 180 2.0 4 200 200 0.5 5 200 200 1.0 6 200 200 2.0 7 200 220 0.5 8 200 220 1.0 9 200 220 2.0 10 200 240 0.5 11 200 240 1.0 12 200 240 2.0
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表 5 不同制备条件下固废轻质油的浓缩产物质量与溶胶含量
Table 5. Concentrated product mass and sol content of soliw aste light oil under different preparation conditions
条件 样品质量/g 浓缩质量/g 溶胶含量/% 溶胶含量标准差/% 1 2.38 1.07 71.59 3.72 2 2.74 2.05 75.78 1.67 3 2.11 1.17 75.45 1.81 4 2.89 2.07 73.28 2.93 5 2.57 1.92 76.68 1.93 6 2.23 1.58 73.66 2.58 7 2.96 1.64 74.98 3.41 8 2.45 1.83 77.58 1.46 9 2.68 1.85 71.88 2.23 10 2.32 1.62 73.49 1.72 11 2.81 2.01 71.54 1.24 12 2.52 1.49 70.65 2.08 注：各序号对应的数据为5个平行样本的加权平均值。需注意，萃取液的浓缩质量并不等同于索氏提取前后样品质量差m1－m2。
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表 6 磁力搅拌机制备参数
Table 6. Preparation parameters of magnetic stirrer
参数 搅拌速度/(r·min-1) 搅拌时间/h 搅拌温度/℃ 固液比 数值 400 1.0 55±2 1∶10
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表 7 不同固废轻质油与再生炭黑胶团掺量组合下复合改性再生沥青的基本性能指标
Table 7. Basic performance indicators of composite-modified rejuvenated asphalt with different solid waste light oil anr ecycled carbon black clusters dosage combinations
条件 固废轻质油掺量/% 再生炭黑胶团掺量/% 25 ℃针入度/0.1 mm 软化点/℃ 10 ℃延度/cm 135 ℃旋转黏度/(Pa·s) 1 4 4 46.2 55.3 13.2 0.864 2 6 4 51.3 53.1 14.4 0.751 3 8 4 58.7 50.5 16.8 0.692 4 10 4 74.1 48.9 20.7 0.528 5 4 5 47.5 56.2 13.9 0.934 6 6 5 49.8 54.0 15.1 0.812 7 8 5 63.8 50.7 17.6 0.639 8 10 5 71.6 49.8 19.8 0.589 9 4 6 45.9 55.7 13.5 0.947 10 6 6 48.3 54.9 14.7 0.843 11 8 6 55.6 52.4 15.9 0.726 12 10 6 69.7 51.6 18.9 0.603
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表 8 TG-DTG温度程序与气氛条件
Table 8. Temperature program and atmosphere conditionf or TG-DTG
阶段 温度条件/℃ 升/降温速率/(℃·min-1) 保温时间/min 气氛 气体流速/(mL·min-1) 初始平衡 50 2 氮气 50 惰性热解 50~560 10 氮气 50 降温 560~300 -10 氮气 50 气氛切换
前平衡300 2 氮气 50 氧化燃烧 300~800 10 空气 50
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表 9 不同沥青样品的羰基、亚砜官能团指数
Table 9. Carbonyl and sulfoxide functional group indices of different asphalt samples
沥青 IC=O IS=O 基质沥青 0.034 5 0.032 6 老化沥青 0.038 5 0.045 8 220炭胶沥青 0.034 0 0.034 4 N330改性沥青 0.025 6 0.026 9
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表 10 不同沥青样品|G*|与δ的重复性误差
Table 10. Repeatability errors of |G*|and δ for different asphalt samples
温度/℃ 基质沥青 220炭胶沥青 N330沥青 短期老化沥青 |G*|变异系数/% δ标准差/(°) |G*|变异系数/% δ标准差/(°) |G*|变异系数/% δ标准差/(°) |G*|变异系数/% δ标准差/(°) 46 4.79 1.19 5.65 1.30 6.69 1.93 3.07 0.99 52 3.92 0.67 5.36 0.78 7.41 1.49 5.19 1.60 58 3.76 1.33 5.97 1.34 4.37 1.21 4.35 0.56 64 3.29 1.09 5.95 0.79 4.38 1.10 5.36 1.52 70 3.97 1.44 6.24 1.72 4.53 1.33 3.15 1.66 76 3.27 0.95 4.45 1.35 7.20 1.45 6.80 1.86 82 3.92 0.41 5.65 1.31 4.81 1.41 3.14 1.28 注：|G*|的变异系数按标准差与平均值之比计算，用于表征相对离散性；δ的重复性误差以标准差表示。
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表 11 不同沥青样品在64 ℃下的储能模量与损耗因子
Table 11. Storage modulus and loss tangents of differena sphalt samples at 64 ℃
样品名称 G′/Pa tan(δ) 基质沥青 72.60 19.74 短期老化沥青 296.82 11.32 220炭胶沥青 119.11 14.23 N330沥青 97.17 14.63 注：储能模量与损耗因子均基于3组平行试验的|G* |与δ均值进行计算。
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