CN113698681B - 纳米改性沥青改性剂及其制备方法 - Google Patents
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Abstract
本发明涉及沥青改性剂技术领域,具体涉及一种纳米改性沥青改性剂及其制备方法。所述纳米改性沥青改性剂,包含以下重量份数的原料:丁苯橡胶SBR100份,多壁碳纳米管0.5~3份,硬脂酸1~5份,碳酸钙20~40份,软化剂3~10份,聚乙烯蜡1~5份,塑解剂0.3~0.8份,偶联剂0.1~2份,分散助剂0.1~2份,隔离剂0.3~1份。本发明的自粘防水卷材沥青改性剂,只需要少量添加即可提高道路用沥青的相应性能,改性后的沥青低温性能好,软化点高,运动粘度小,耐磨性、抗撕裂性、导热性大幅提高,增加了道路寿命。
Description
技术领域
本发明涉及沥青改性剂技术领域,具体涉及一种纳米改性沥青改性剂及其制备方法。
背景技术
用于铺筑道路的沥青一般采用改性沥青,在沥青中掺加橡胶、树脂、高分子聚合物、磨细的橡胶粉或其他填料等外掺剂(改性剂),使沥青或沥青混合料的性能得以改善。
传统的道路沥青改性剂一般是指聚合物改性沥青,大体分为三类:
①热塑性橡胶类:即热塑性弹性体,主要是苯乙烯类嵌段共聚物,如苯乙烯-丁二烯-苯乙烯(SBS)、苯乙烯-异戊二烯苯乙烯(SIS)、苯乙烯~聚乙烯/丁基-聚乙烯(SB)等嵌段共聚物及聚烯烃等,由于它兼具橡胶和树脂两类改性沥青的性质,故也称橡胶树脂类。由于SBS的良好的弹性(变形的自恢复性及裂缝的自愈性),成为目前世界上最引人注目的道路沥青改性剂。
②橡胶类:如天然橡胶(NR)、丁苯橡胶(SBR)、氯丁橡胶(CR)、丁二烯橡胶(BR)、异戊二烯(IR)、乙丙橡胶(EPDM)、丙烯腈丁二烯共聚物(ABR)等。其中SBR胶乳是世界上应用最广泛的改性剂之一。氯丁橡胶(CR)具有极性,常作为煤沥青的改性剂使用。
③树脂类:热塑性树脂,如乙烯-乙酸乙烯酯共聚物(EVA)、聚乙烯(PE)、无规聚丙烯(APP)、聚氯乙烯(PVC)、聚苯乙烯(PS)、聚酰胺、乙烯丙烯类共聚物(APAO)等;热固性树脂也有作为改性剂使用的,如环氧树胎(EP)等。EVA由于其乙酸乙烯的含量及熔融指数MI的不同,不同牌号EVA的性能有较大差别。无规聚丙烯APP由于其价格低廉,用于改性沥青油毡较多,其缺点是与石料的粘结力较小。
但是传统改性剂只是提高沥青低温性能,耐磨、耐撕裂性能改善效果不明显,不能提高导热性能。例如专利CN201710593588.X中公开了一种改性高粘沥青,包括道路石油沥青、丁二烯-苯乙烯嵌段共聚物、低分子量高分子合成树脂、高分子量高分子合成树脂、稳定剂。具有储存稳定性好的优点,通过离析慢、不降解的高分子树脂进行复合改性,改性后的道路石油沥青其韧性、粘韧性良好,耐腐蚀性能良好。但是并未改善道路沥青的耐磨和耐撕裂性能。
发明内容
本发明要解决的技术问题是:提供一种纳米改性沥青改性剂,只需要少量添加即可提高道路用沥青的相应性能,改性后的沥青低温性能好,软化点高,运动粘度小,耐磨性、抗撕裂性、导热性大幅提高,增加了道路寿命;本发明同时提供了简单易行的制备方法。
本发明所述的纳米改性沥青改性剂,包含以下重量份数的原料:
所述多壁碳纳米管的管径为8~15nm,比表面积为230~280m2/g,微观结构为阵列式排列结构,俗称阵列管。
碳酸钙作为填料,除填充作用外,还可改善沥青的高温性能,提高软化点降低针入度,同时改善挤出造粒时的加工性能。
软化剂为多环芳香烃橡胶油、环烷基橡胶油、芳香基橡胶中的至少一种。软化剂的作用是软化橡胶,使各组分在制备过程中更易分散均匀,同时软化剂的加入,使橡胶大分子链断开,增加塑性,改善加工性能;大分子链的断开也使产品更加快速溶解于沥青。
聚乙烯蜡的平均分子量为2000-5000,熔点为60-70℃。
塑解剂为DBD(2,2'-二苯甲酰胺基二苯基二硫化物)、金属有机络合物及有机载体的混合物,优选为塑解剂A89。塑解剂在混炼阶段可以使橡胶的大分子链断链,降低橡胶分子量,增加塑性,使各组分分散均匀;同时降低分子量有助于改性剂在沥青中的溶解。
偶联剂为硅烷偶联剂KH580、硅烷偶联剂KH550、硅烷偶联剂KH792中的至少一种。偶联剂可以提高产品的表面活性,在其与沥青之间起到界面作用,加速在沥青中的溶解;同时其中的极性官能团起到“搭桥”作用,作为两者之间的弹性桥联剂,使改性剂在沥青中更加稳定。
分散助剂为不饱和脂肪酸锌盐,优选朗盛集团生产的橡胶加工助剂AktiplastPP。分散助剂改善组分的分散质量,使分散更加均匀,也是一种内润滑剂,可以改善挤出工艺,也有助于在沥青中的溶解。
隔离剂为硬脂酸钙。产品完成后表面附着的隔离剂,放置粘结成团。
本发明在改性剂中添加一定量的多壁碳纳米管,多壁碳纳米管具有管径分布窄、比表面积高、石墨化程度高、超高长径比的特点,少量添加即可改善材料的力学性能:在保持SBR对沥青低温性能的改善的同时,通过其纳米级材料的强界面效果,增加道路沥青的抗撕裂能力,并且由于其独特的管状六元环结构以及独特的阵列管式排列结构,可以大幅提高导热性能,使热量迅速扩散。另外,其他各助剂可以有效帮助高结构度的碳纳米管均匀分散,同时帮助改性剂在沥青中的溶解。软化剂、塑解剂与分散助剂的加入可以使碳纳米管等组分更加均匀的分散,不但提高加工性能,改善挤出造粒工艺;也使改性剂的性能更加稳定。同时,软化剂与塑解剂的加入,可以使橡胶分子链断链,降低其分子量;分散助剂作为一种内润滑剂不但可以改善加工过程,也有助于改性剂在沥青中的溶解;偶联剂可以作为表面活性剂起到界面作用,加速改性剂的溶解;同时其极性官能团也可起到搭桥作用,使改性剂更加稳定。改性剂由于自身有一定粘性,产品制备完成后表面添加隔离剂,可以有效防止黏连结块。
本发明所述的纳米改性沥青改性剂的制备方法,包括以下步骤:
(1)将丁苯橡胶SBR加入密炼机中,压栓,密炼15-30s,提栓,加入碳纳米管,密炼50-80s,提栓,排胶,得到碳纳米管的质量分数为10~20%碳纳米管母胶;
(2)将碳纳米管母胶加入密炼机中,密炼15-30s,提栓,加入硬脂酸、碳酸钙、软化剂、聚乙烯蜡、塑解剂、偶联剂和分散助剂,密炼70-100s,提栓,压栓,15-30s,排胶,将密炼好的胶料投入挤出机造粒,胶粒进入震动床冷却后,添加隔离剂混匀,得到纳米改性沥青改性剂。
步骤(1)和步骤(2)中,密炼机转速为40-60r/min,上顶栓压力为0.3-0.5Mpa,排胶温度不超过90℃。
与现有技术相比,本发明具有以下有益效果:
(1)本发明的纳米改性沥青改性剂,只需要少量添加即可提高道路用沥青的相应性能,改性后的沥青低温性能好,软化点高,运动粘度小,耐磨性、抗撕裂性、导热性大幅提高,增加了道路寿命;
(2)本发明的纳米改性沥青改性剂为颗粒状,方便运输、称量、使用,使用过程中几乎无粉尘,更加环保。
具体实施方式
实施例中用到的所有原料除特殊说明外,均为市购。
实施例和对比例
按表1的原料组成制备沥青改性剂,其中软化剂可以为多环芳香烃橡胶油、环烷基橡胶油、芳香基橡胶中的任意一种或多种,以上几种软化剂对产品的作用相同,相互替换对产品的性能影响不大;偶联剂可以为硅烷偶联剂KH580、硅烷偶联剂KH550、硅烷偶联剂KH792中的任意一种或多种,以上几种偶联剂对产品的作用相同,相互替换对产品的性能影响不大。为方便对比,实施例和对比例的软化剂采用多环芳香烃橡胶油,偶联剂采用KH550,其余助剂中,多壁碳纳米管采用管径8~15nm之间、比表面积230~280m2/g之间、微观结构为阵列式排列结构的多壁碳纳米管,塑解剂采用塑解剂A89,聚乙烯蜡采用平均分子量2000-5000之间、熔点60-70℃之间的聚乙烯蜡,分散助剂采用朗盛集团生产的AktiplastPP,隔离剂采用硬脂酸钙。
实施例和对比例的沥青改性剂原料组成如表1所示,以各原料的重量份数计。
表1实施例1-4的原料组成
按照表1的原料组成制备沥青改性剂,步骤如下:
将密炼机参数设定为:转速50r/min,上顶栓压力0.4Mpa,将丁苯橡胶SBR加入密炼机中,压栓,密炼20s,提栓,加入碳纳米管,密炼60s,提栓,降温至90℃以下排胶,得到碳纳米管母胶;将碳纳米管母胶再次加入密炼机中,密炼20s,提栓,加入除隔离剂之外的所有助剂,密炼80s,提栓,压栓,密炼20s,降温至90℃以下排胶;将密炼好的胶料投入挤出机造粒,胶粒进入震动床冷却后,添加隔离剂混匀,得到沥青改性剂。
将实施例1-4和对比例1-4制备的沥青改性剂用于道路沥青改性,方法如下:将3wt%的沥青改性剂、4wt%的SBS1301、93wt%的70#石油沥青混合,在剪切乳化机中于150℃下先以线速度为30m/s高速剪切30分钟,然后以线速度为1m/s继续搅拌1小时,得到改性道路沥青。
另外,设置对比例5,不添加沥青改性剂,将4wt%的SBS1301、96wt%的70#石油沥青混合,在剪切乳化机中于150℃下先以线速度为30m/s高速剪切30分钟,然后以线速度为1m/s继续搅拌1小时,得到改性道路沥青。
将上述改性道路沥青按照《公路沥青路面施工技术规范》(JTG F40-2004)的规定制备AC-13C沥青混合料。选用AC-13C级配,将上述改性道路沥青与矿料分别加热后,按照4.9∶95.1的重量比拌和均匀,得到沥青混合料;其中,矿料加热温度为180±5℃,沥青加热温度为165±5℃,沥青混合料击实温度为160±5℃。所用矿料的级配如表2所示,
表2矿料级配
筛孔,mm | 16 | 13.2 | 9.5 | 4.75 | 2.36 | 1.18 | 0.6 | 0.3 | 0.15 | 0.075 |
通过率,% | 100 | 94.5 | 72.7 | 35.8 | 27.6 | 21.5 | 17.1 | 12.4 | 10.9 | 7.7 |
对制备的道路改性沥青进行性能测试,测试结果如表3-4所示。对制备的沥青混合料进行性能测试,测试结果如表5-6所示。
表3道路改性沥青测试结果
测试项目 | 测试标准 | 实施例1 | 实施例2 | 实施例3 | 实施例4 |
5℃延度,cm | T0605-2011 | 35 | 37 | 42 | 42 |
运动粘度(135℃),mPa·s | T0625-2011 | 815 | 862 | 927 | 966 |
针入度,0.1mm | T0604-2011 | 50 | 47 | 42 | 41 |
软化点,℃ | T0606-2011 | 76 | 79 | 78 | 79 |
导热系数,W/(mK) | ISO 22007-2 | 0.711 | 0.768 | 0.827 | 0.912 |
表4道路改性沥青测试结果
表5沥青混合料测试结果
表6沥青混合料测试结果
从表3-6可以看出,碳纳米管的加入使沥青的性能提高,在与其他助剂相互作用下,所得沥青混合料具有更高的高温抗车辙性,能大幅提升道路的耐磨与撕裂破坏,提高寿命;同时,沥青的导热系数大幅提升,可以有效增加路面的导热效果,提高道路使用寿命。
Claims (8)
1.一种纳米改性沥青改性剂,其特征在于,包含以下重量份数的原料:
丁苯橡胶SBR 100 份,
多壁碳纳米管 0.5~3份,
硬脂酸 1~5份,
碳酸钙 20~40份,
软化剂 3~10份,
聚乙烯蜡 1~5份,
塑解剂 0.3~0.8份,
偶联剂 0.1~2份,
分散助剂 0.1~2份,
隔离剂 0.3~1份;
所述软化剂为多环芳香烃橡胶油、环烷基橡胶油中的至少一种;
所述塑解剂为A89;
所述分散助剂为AktiplastPP。
2.根据权利要求1所述的纳米改性沥青改性剂,其特征在于:多壁碳纳米管的管径为8~15nm,比表面积为230~280m2/g,微观结构为阵列式结构。
3.根据权利要求1所述的纳米改性沥青改性剂,其特征在于:聚乙烯蜡的平均分子量为2000-5000,熔点为60-70℃。
4.根据权利要求1所述的纳米改性沥青改性剂,其特征在于:偶联剂为硅烷偶联剂KH580、硅烷偶联剂KH550、硅烷偶联剂KH792中的至少一种。
5.根据权利要求1所述的纳米改性沥青改性剂,其特征在于:隔离剂为硬脂酸钙。
6.一种权利要求1-5任一项所述的纳米改性沥青改性剂的制备方法,其特征在于:包括以下步骤:
(1)将丁苯橡胶SBR加入密炼机中,压栓,密炼15-30s,提栓,加入碳纳米管,密炼50-80s,提栓,排胶,得到碳纳米管的质量分数为10-20%碳纳米管母胶;
(2)将碳纳米管母胶加入密炼机中,密炼15-30s,提栓,加入硬脂酸、碳酸钙、软化剂、聚乙烯蜡、塑解剂、偶联剂和分散助剂,密炼70-100s,提栓,压栓,15-30s,排胶,将密炼好的胶料投入挤出机造粒,胶粒进入震动床冷却后,添加隔离剂混匀,得到纳米改性沥青改性剂。
7.根据权利要求6所述的纳米改性沥青改性剂的制备方法,其特征在于:步骤(1)和步骤(2)中,密炼机转速为40-60r/min,上顶栓压力为0.3-0.5Mpa。
8.根据权利要求6所述的纳米改性沥青改性剂的制备方法,其特征在于:步骤(1)和步骤(2)中,排胶温度不超过90℃。
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