SBS改性沥青的乳化对其应用性能影响的研究
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摘要
本文采用先SBS化学改性后乳化的方法制备SBS改性乳化沥青，通过针入度、软化点、5℃延度、针入度指数、弹性恢复、贮存稳定性等物理性能的测定，结合荧光显微镜、差示扫描量热、红外光谱等分析手段，以基质沥青、乳化剂结构类型以及改性剂类型等参数的变化为基础，研究乳化对SBS改性沥青的高温性能、低温性能、温度敏感性、弹性恢复能力、热贮存稳定性、微观形态以及微观结构的影响。
通过工艺条件的优化得到较好的SBS化学改性沥青制备工艺条件和配方为：剪切温度为175℃，剪切时间为1h，剪切速率为3000rpm，剪切后样品在163℃下发育1h，改性剂和稳定剂的加入量分别是3%和0.265%。在以上工艺条件下，SBS在中海油、辽河、加德士及齐鲁等沥青中的分散状态不同，在加德士沥青中分散的最为均匀，最适宜乳化。改性沥青适宜的乳化条件为：改性沥青加热到160～170℃，乳化剂水溶液加热至55℃。
乳化过程使改性沥青的物理性能减弱，但并未改变其微观结构。在较好的工艺条件和配方下，使用同种乳化剂乳化四种改性沥青（相同改性剂、不同基质沥青）得到相应的改性乳化沥青。与改性沥青相比，对应改性乳化沥青蒸发残留物的软化点、5℃延度、弹性恢复能力和贮存稳定性均有一定程度的下降，这主要未发生化学反应的SBS颗粒聚集的结果，因为荧光显微镜照片上可明显观测到黄绿色颗粒，部分粒径尺寸远大于改性沥青中SBS颗粒的粒径尺寸；DSC测试结果显示总吸热量均稍微上升（辽河改性沥青除外），说明热稳定性略有下降，这和常规性能减弱是相一致的；但FT-IR结果表明乳化过程中沥青和SBS分子之间的交联结构并没有发生化学变化，即改性沥青的微观结构未发生变化。
不同结构类型乳化剂对改性沥青性能的影响存在很大差异。在较好的工艺条件和配方下，使用三种结构类型乳化剂分别乳化同种改性沥青后得到相应的改性乳化沥青。分析结果表明，使用的酰胺型和咪唑啉型乳化剂（MA-1M和RAI-44）分子在沥青分子间起融合作用，不仅一定程度上提高了改性沥青的物理性能，而且乳化过程中没有改变改性沥青的微观结构；而使用的季铵盐型乳化剂（JFQ-2）在沥青分之间起阻碍作用，不仅使改性沥青的物理性能大幅度降低，甚至一定程度上破坏了SBS和沥青分子之间的交联状态，使改性沥青发生微观结构的改变。
乳化过程中，SBS改性剂的S/B嵌段比和分子构型对改性沥青的物理性能、热性能影响不同，但对微观结构无明显影响。在较好的工艺条件和配方下，使用同种乳化剂乳化四种改性沥青（相同基质沥青、不同改性剂）得到相应的改性乳化沥青。通过相关性能分析发现，对于不同S/B嵌段比的三种线型SBS改性剂，S/B嵌段比为30/70的SBS改性的沥青乳化前后均表现出较好的物理性能及热稳定性，主要是因为SBS在沥青中得到充分溶胀伸展，两相分散最均匀，形成三维网状结构最致密。对于S/B嵌段比均为30/70而分子构型不同的SBS改性剂，线性SBS改性的沥青乳化前后表现出较好的高温贮存稳定性和相容性，但是星型SBS改性的沥青表现出更好的高温性能、感温性能和弹性恢复能力，这主要是由于线型SBS在沥青中分散的更均匀，而星型SBS的立体结构复杂，分子结构支链较多，分散在沥青中后不易从三维网络中挣脱出来。不论哪种类型SBS改性的沥青，乳化过程中改性沥青的微观结构均没有发生变化，改性剂和沥青分子之间均不是完全交联，交联比率在12%～27%之间，部分交联不会对沥青的性能产生不利影响。
改性方式不同，改性沥青的性能差异很大。化学改性沥青可大大提高沥青的性能，而物理改性沥青仅能有限的提高沥青的各种指标性能。并且化学改性乳化沥青的颗粒较均匀，而物理改性乳化沥青的颗粒大小很不均匀，粒径范围较宽，颗粒之间相互聚集的趋势更明显。
In this work, the styrene-butadiene-styrene (SBS) modified asphalt emulsions wereprepared as SBS was pre-blended chemically with the asphalt prior to emulsification. On thebasis of base asphalt, emulsifier type and modifier type, the influences of emulsification onthe high-, low-temperature performance and temperature sensitivity, elastic recovery ability,thermal stability, micromorphology and microstructure of SBS modified asphalts were studied,by means of physical tests such as penetration, softening point, ductility at5℃, penetrationindex, elastic recovery, as well as fluorescence microscopy, differential scanning calorimetry(DSC) and fourier transform infrared (FT-IR) spectroscopy.
By optimization of the technological conditions, the preferable process conditions andformula of SBS chemically modified asphalts were found. The sample was sheared for60minat a shearing rate of3000rpm and then it was put into the oven for complete swelling whenthe modifier and stabilizer contents are3%and0.265%respectively. In that case, thedispersion of SBS particles in Zhonghaiyou, Liaohe, Caltex and Qilu asphalts is quitedifferent, and most uniform dispersion can be observed in Caltex asphalt, which is morepreferable for emulsification. Under the favorable emulsification conditions, the modifiedasphalts were heated to160～170℃and the emulsifier solutions were heated to55℃.
The physical properties of modified asphalts became inferior during emulsification, butthe microstructure is unchanged. The modified asphalt emulsions were prepared as fourmodified asphalts (prepared by the same modifier and different asphalts) emulsified by thesame emulsifier under the preferable process conditions. Compared to modified asphalt, itdisplays a decline in softening point, ductility at5℃, elastic recovery ability and storagestability for its corresponding emulsion residue. Changes for above mentioned properties arisefrom the aggregation of SBS particles that do not react with asphalt. Evidence about yellowgreen particles which mean size is far more than that of SBS particles in modified asphaltscan be verified on fluorescence microscope images. The DSC results indicate the totalabsorbed heat of modified asphalts increases slightly during emulsification, suggesting aslight decrease in thermal stability. However, FT-IR results suggest the cross-linking structurebetween asphalt and SBS molecules remains unchanged during emulsification, namely the microstructure of modified asphalt is invariable.
Different emulsifiers have distinct effect on the modified asphalt. The modified asphaltemulsions were prepared as the same modified asphalt emulsified by three emulsifiers underthe preferable process conditions. It is found that amide and imidazoline emulsifiers (MA-1Mand RAI-44) played an agglomerative roll between asphalt molecules, which makes themodified asphalt physical properties improved substantially and the microstructure ofmodified asphalt remains unchanged. On the other hand, the emulsifier that mainly containsquaternary ammonium salts (JFQ-2) exerts an inhibiting action between the asphalt molecules,which results in a great decline in the physical properties of modified asphalt and even causesthe cross-linking state between SBS and asphalt molecules broken so that the microstructureof modified asphalt changes.
The S/B block ratio and molecular structure of SBS have different effect on the physicalproperties and thermal behavior but no substantial influence on the microstructure of modifiedasphalts during emulsification. The modified asphalt emulsions were prepared as fourmodified asphalts (prepared by the same asphalt and different modifiers) emulsified by thesame emulsifier under the favorable process conditions. The conclusions can be drawnaccording to a series of relative tests. For three linear SBS modifiers with different S/B blockratio, the modified asphalt before and after emulsification displays the optimum physicalproperties and thermal stability when the S/B block ratio is30/70. It results from the SBS isfully swollen in asphalt so that the dispersion of SBS phase in asphalt phase is uniform andthe compact three-dimensional network is formed. On the other hand, for the SBS modifierswith the same S/B block ratio (30/70) and different molecular structure, the asphalt modifiedby the linear SBS before and after emulsification shows more preferable storage stability athigh temperature and compatibility than that modified by star SBS due to more uniformdispersion of linear SBS in asphalt. However, the latter represents better high temperatureproperty, temperature sensitivity and elastic recovery ability, which attribute to thecomplicated three-dimensional and branch structure in star SBS so that the SBS phase isdifficult to apart from asphalt phase after uniformly dispersed. Furthermore, themicrostructure of asphalt modified by the four various modifiers during emulsificationremains unchanged. And the cross-linking reaction is not complete between modifiers and asphalt molecules, revealing the cross-linking percentage between asphalt and modifiermolecules is from12%to27%, which have no harmful impact on the asphalt properties.
The modified asphalts properties are extremely different if the modification method isdistinct. The properties of modified asphalt can be improved greatly by chemical modificationand less by physical modification. What’s more, the emulsion particles for the former areuniform, whereas the emulsion particles for the latter are substantially nonuniform with abroad range of particles and the particles tend to aggregate.
通过工艺条件的优化得到较好的SBS化学改性沥青制备工艺条件和配方为：剪切温度为175℃，剪切时间为1h，剪切速率为3000rpm，剪切后样品在163℃下发育1h，改性剂和稳定剂的加入量分别是3%和0.265%。在以上工艺条件下，SBS在中海油、辽河、加德士及齐鲁等沥青中的分散状态不同，在加德士沥青中分散的最为均匀，最适宜乳化。改性沥青适宜的乳化条件为：改性沥青加热到160～170℃，乳化剂水溶液加热至55℃。
乳化过程使改性沥青的物理性能减弱，但并未改变其微观结构。在较好的工艺条件和配方下，使用同种乳化剂乳化四种改性沥青（相同改性剂、不同基质沥青）得到相应的改性乳化沥青。与改性沥青相比，对应改性乳化沥青蒸发残留物的软化点、5℃延度、弹性恢复能力和贮存稳定性均有一定程度的下降，这主要未发生化学反应的SBS颗粒聚集的结果，因为荧光显微镜照片上可明显观测到黄绿色颗粒，部分粒径尺寸远大于改性沥青中SBS颗粒的粒径尺寸；DSC测试结果显示总吸热量均稍微上升（辽河改性沥青除外），说明热稳定性略有下降，这和常规性能减弱是相一致的；但FT-IR结果表明乳化过程中沥青和SBS分子之间的交联结构并没有发生化学变化，即改性沥青的微观结构未发生变化。
不同结构类型乳化剂对改性沥青性能的影响存在很大差异。在较好的工艺条件和配方下，使用三种结构类型乳化剂分别乳化同种改性沥青后得到相应的改性乳化沥青。分析结果表明，使用的酰胺型和咪唑啉型乳化剂（MA-1M和RAI-44）分子在沥青分子间起融合作用，不仅一定程度上提高了改性沥青的物理性能，而且乳化过程中没有改变改性沥青的微观结构；而使用的季铵盐型乳化剂（JFQ-2）在沥青分之间起阻碍作用，不仅使改性沥青的物理性能大幅度降低，甚至一定程度上破坏了SBS和沥青分子之间的交联状态，使改性沥青发生微观结构的改变。
乳化过程中，SBS改性剂的S/B嵌段比和分子构型对改性沥青的物理性能、热性能影响不同，但对微观结构无明显影响。在较好的工艺条件和配方下，使用同种乳化剂乳化四种改性沥青（相同基质沥青、不同改性剂）得到相应的改性乳化沥青。通过相关性能分析发现，对于不同S/B嵌段比的三种线型SBS改性剂，S/B嵌段比为30/70的SBS改性的沥青乳化前后均表现出较好的物理性能及热稳定性，主要是因为SBS在沥青中得到充分溶胀伸展，两相分散最均匀，形成三维网状结构最致密。对于S/B嵌段比均为30/70而分子构型不同的SBS改性剂，线性SBS改性的沥青乳化前后表现出较好的高温贮存稳定性和相容性，但是星型SBS改性的沥青表现出更好的高温性能、感温性能和弹性恢复能力，这主要是由于线型SBS在沥青中分散的更均匀，而星型SBS的立体结构复杂，分子结构支链较多，分散在沥青中后不易从三维网络中挣脱出来。不论哪种类型SBS改性的沥青，乳化过程中改性沥青的微观结构均没有发生变化，改性剂和沥青分子之间均不是完全交联，交联比率在12%～27%之间，部分交联不会对沥青的性能产生不利影响。
改性方式不同，改性沥青的性能差异很大。化学改性沥青可大大提高沥青的性能，而物理改性沥青仅能有限的提高沥青的各种指标性能。并且化学改性乳化沥青的颗粒较均匀，而物理改性乳化沥青的颗粒大小很不均匀，粒径范围较宽，颗粒之间相互聚集的趋势更明显。
In this work, the styrene-butadiene-styrene (SBS) modified asphalt emulsions wereprepared as SBS was pre-blended chemically with the asphalt prior to emulsification. On thebasis of base asphalt, emulsifier type and modifier type, the influences of emulsification onthe high-, low-temperature performance and temperature sensitivity, elastic recovery ability,thermal stability, micromorphology and microstructure of SBS modified asphalts were studied,by means of physical tests such as penetration, softening point, ductility at5℃, penetrationindex, elastic recovery, as well as fluorescence microscopy, differential scanning calorimetry(DSC) and fourier transform infrared (FT-IR) spectroscopy.
By optimization of the technological conditions, the preferable process conditions andformula of SBS chemically modified asphalts were found. The sample was sheared for60minat a shearing rate of3000rpm and then it was put into the oven for complete swelling whenthe modifier and stabilizer contents are3%and0.265%respectively. In that case, thedispersion of SBS particles in Zhonghaiyou, Liaohe, Caltex and Qilu asphalts is quitedifferent, and most uniform dispersion can be observed in Caltex asphalt, which is morepreferable for emulsification. Under the favorable emulsification conditions, the modifiedasphalts were heated to160～170℃and the emulsifier solutions were heated to55℃.
The physical properties of modified asphalts became inferior during emulsification, butthe microstructure is unchanged. The modified asphalt emulsions were prepared as fourmodified asphalts (prepared by the same modifier and different asphalts) emulsified by thesame emulsifier under the preferable process conditions. Compared to modified asphalt, itdisplays a decline in softening point, ductility at5℃, elastic recovery ability and storagestability for its corresponding emulsion residue. Changes for above mentioned properties arisefrom the aggregation of SBS particles that do not react with asphalt. Evidence about yellowgreen particles which mean size is far more than that of SBS particles in modified asphaltscan be verified on fluorescence microscope images. The DSC results indicate the totalabsorbed heat of modified asphalts increases slightly during emulsification, suggesting aslight decrease in thermal stability. However, FT-IR results suggest the cross-linking structurebetween asphalt and SBS molecules remains unchanged during emulsification, namely the microstructure of modified asphalt is invariable.
Different emulsifiers have distinct effect on the modified asphalt. The modified asphaltemulsions were prepared as the same modified asphalt emulsified by three emulsifiers underthe preferable process conditions. It is found that amide and imidazoline emulsifiers (MA-1Mand RAI-44) played an agglomerative roll between asphalt molecules, which makes themodified asphalt physical properties improved substantially and the microstructure ofmodified asphalt remains unchanged. On the other hand, the emulsifier that mainly containsquaternary ammonium salts (JFQ-2) exerts an inhibiting action between the asphalt molecules,which results in a great decline in the physical properties of modified asphalt and even causesthe cross-linking state between SBS and asphalt molecules broken so that the microstructureof modified asphalt changes.
The S/B block ratio and molecular structure of SBS have different effect on the physicalproperties and thermal behavior but no substantial influence on the microstructure of modifiedasphalts during emulsification. The modified asphalt emulsions were prepared as fourmodified asphalts (prepared by the same asphalt and different modifiers) emulsified by thesame emulsifier under the favorable process conditions. The conclusions can be drawnaccording to a series of relative tests. For three linear SBS modifiers with different S/B blockratio, the modified asphalt before and after emulsification displays the optimum physicalproperties and thermal stability when the S/B block ratio is30/70. It results from the SBS isfully swollen in asphalt so that the dispersion of SBS phase in asphalt phase is uniform andthe compact three-dimensional network is formed. On the other hand, for the SBS modifierswith the same S/B block ratio (30/70) and different molecular structure, the asphalt modifiedby the linear SBS before and after emulsification shows more preferable storage stability athigh temperature and compatibility than that modified by star SBS due to more uniformdispersion of linear SBS in asphalt. However, the latter represents better high temperatureproperty, temperature sensitivity and elastic recovery ability, which attribute to thecomplicated three-dimensional and branch structure in star SBS so that the SBS phase isdifficult to apart from asphalt phase after uniformly dispersed. Furthermore, themicrostructure of asphalt modified by the four various modifiers during emulsificationremains unchanged. And the cross-linking reaction is not complete between modifiers and asphalt molecules, revealing the cross-linking percentage between asphalt and modifiermolecules is from12%to27%, which have no harmful impact on the asphalt properties.
The modified asphalts properties are extremely different if the modification method isdistinct. The properties of modified asphalt can be improved greatly by chemical modificationand less by physical modification. What’s more, the emulsion particles for the former areuniform, whereas the emulsion particles for the latter are substantially nonuniform with abroad range of particles and the particles tend to aggregate.
引文
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