朱晓斌1,2,洪锦祥1,2,李炜2,3
(1.江苏苏博特新材料股份有限公司,南京 211103;2.高性能土木工程材料国家重点实验室,南京 210008; 3.东南大学 材料科学与工程学院,南京 211189)
摘要:
为揭示水泥沥青砂浆(CA砂浆)中水泥对乳化沥青和减水剂的吸附规律，采用微量热仪分析了减水剂、乳化沥青(单掺及同掺)对水泥水化诱导期的延迟作用.采用“固含法”研究了减水剂种类对水泥-乳化沥青经时吸附规律的影响，以及减水剂在不同添加顺序时对水泥-乳化沥青经时吸附规律的影响.采用偏光显微镜对减水剂作用下水泥-乳化沥青的吸附行为进行了原位观测.结果表明：CA砂浆中的乳化沥青和减水剂均能显著延迟水泥的水化诱导期，两者同掺使延迟作用产生了明显的协同效应；聚羧酸减水剂与乳化沥青对水泥的吸附作用存在明显的竞争关系，两者同掺时水泥优先吸附减水剂分子，减水剂耗尽后，水泥再吸附乳化沥青.减水剂后掺时可使部分吸附的乳化沥青发生解吸附.
关键词: CA砂浆 吸附行为 竞争吸附 减水剂 机理
DOI：10.11918/j.issn.0367-6234.201706184
分类号:TU535
文献标识码:A
基金项目:国家自然科学基金(1,3)
Adsorption behaviors of superplasticizer and emulsified asphalt in cement-asphalt mortar
ZHU Xiaobin1,2,HONG Jinxiang 1,2,LI Wei2,3
(1. Jiangsu Sobute New Materials Co., Ltd., Nanjing 211103, China; 2. State Key Laboratory of High Performance Civil Engineering Materials, Nanjing 210008, China; 3.School of Materials Science and Engineering,Southeast University,Nanjing 211189,China)
Abstract:
To investigate the adsorption mechanism of cement on emulsified asphalt and superplasticizer in cement-asphalt mortar (CA mortar), the retardation effects of superplasticizer and emulsified asphalt on cement hydration were analyzed by the result of hydration heat measured by microcalorimetry. The effects of the type and adding sequence of superplasticizer on the adsorption of cement-emulsified asphalt were studied. In addition, the in-situ observation of the adsorption between cement and emulsified asphalt under the function of superplasticizer was conducted by using the polarizing microscope. Results showed that both emulsified asphalt and superplasticizer could retard the cement hydration and evidently extend the induction, while the co-adding of superplasticizer and emulsified asphalt resulted in evident synergistic effect in respect of the induction's extension. Competitive relationship obviously existed between the adsorption of polycarboxylate superplasticizer and emulsified asphalt on cement. In the case of coexistence of superplasticizer and emulsified asphalt, the cement was adsorbed by the former in priority. When the superplasticizer was added after emulsified asphalt, the adsorbed emulsified asphalt particles could be substituted by superplasticizer.
Key words: CA mortar adsorption behavior competitive adsorption superplasticizer mechanism
朱晓斌, 洪锦祥, 李炜. 水泥沥青浆体中减水剂与乳化沥青的竞争吸附行为[J]. 哈尔滨工业大学学报, 2018, 50(9): 55-60. DOI: 10.11918/j.issn.0367-6234.201706184.
ZHU Xiaobin, HONG Jinxiang, LI Wei. Adsorption behaviors of superplasticizer and emulsified asphalt in cement-asphalt mortar[J]. Journal of Harbin Institute of Technology, 2018, 50(9): 55-60. DOI: 10.11918/j.issn.0367-6234.201706184.
基金项目 国家自然科学基金(51278231，51708483) 作者简介 朱晓斌(1982—)，男，硕士，高级工程师 通信作者 朱晓斌，xbzhu@163.com 文章历史 收稿日期: 2017-06-29
Contents -->Abstract Full text Figures/Tables PDF
水泥沥青浆体中减水剂与乳化沥青的竞争吸附行为
朱晓斌1,2
, 洪锦祥1,2, 李炜2,3 1. 江苏苏博特新材料股份有限公司，南京 211103;
2. 高性能土木工程材料国家重点实验室，南京 210008;
3. 东南大学 材料科学与工程学院，南京 211189
收稿日期: 2017-06-29
基金项目: 国家自然科学基金(51278231，51708483)
作者简介: 朱晓斌(1982—)，男，硕士，高级工程师
通信作者: 朱晓斌，xbzhu@163.com
摘要: 为揭示水泥沥青砂浆(CA砂浆)中水泥对乳化沥青和减水剂的吸附规律，采用微量热仪分析了减水剂、乳化沥青(单掺及同掺)对水泥水化诱导期的延迟作用.采用“固含法”研究了减水剂种类对水泥-乳化沥青经时吸附规律的影响，以及减水剂在不同添加顺序时对水泥-乳化沥青经时吸附规律的影响.采用偏光显微镜对减水剂作用下水泥-乳化沥青的吸附行为进行了原位观测.结果表明：CA砂浆中的乳化沥青和减水剂均能显著延迟水泥的水化诱导期，两者同掺使延迟作用产生了明显的协同效应；聚羧酸减水剂与乳化沥青对水泥的吸附作用存在明显的竞争关系，两者同掺时水泥优先吸附减水剂分子，减水剂耗尽后，水泥再吸附乳化沥青.减水剂后掺时可使部分吸附的乳化沥青发生解吸附.
关键词: CA砂浆 吸附行为 竞争吸附 减水剂 机理
Adsorption behaviors of superplasticizer and emulsified asphalt in cement-asphalt mortar
ZHU Xiaobin1,2
, HONG Jinxiang1,2, LI Wei2,3 1. Jiangsu Sobute New Materials Co., Ltd., Nanjing 211103, China;
2. State Key Laboratory of High Performance Civil Engineering Materials, Nanjing 210008, China;
3. School of Materials Science and Engineering, Southeast University, Nanjing 211189, China
Abstract: To investigate the adsorption mechanism of cement on emulsified asphalt and superplasticizer in cement-asphalt mortar (CA mortar), the retardation effects of superplasticizer and emulsified asphalt on cement hydration were analyzed by the result of hydration heat measured by microcalorimetry. The effects of the type and adding sequence of superplasticizer on the adsorption of cement-emulsified asphalt were studied. In addition, the in-situ observation of the adsorption between cement and emulsified asphalt under the function of superplasticizer was conducted by using the polarizing microscope. Results showed that both emulsified asphalt and superplasticizer could retard the cement hydration and evidently extend the induction, while the co-adding of superplasticizer and emulsified asphalt resulted in evident synergistic effect in respect of the induction's extension. Competitive relationship obviously existed between the adsorption of polycarboxylate superplasticizer and emulsified asphalt on cement. In the case of coexistence of superplasticizer and emulsified asphalt, the cement was adsorbed by the former in priority. When the superplasticizer was added after emulsified asphalt, the adsorbed emulsified asphalt particles could be substituted by superplasticizer.
Keywords: CA mortar adsorption behavior competitive adsorption superplasticizer mechanism
CA砂浆是一种由水泥，乳化沥青，水，细砂及多种化学添加剂经水化、破乳作用形成的新型建筑材料[1-4]，它保留了水泥基材料力学性能高和沥青材料柔性好的特点，因此具有广泛的应用空间，已经应用于高速铁路，城市抗车辙路面工程中. CA砂浆已经在德国、日本、西班牙和中国的高速铁路工程中广泛使用[5-8]，用于填充板式无砟轨道系统的轨道板与混凝土底座之间的充填层，主要起到减震消能及调整施工误差的作用；在市政道路工程中[9]，CA砂浆用于填充大孔隙沥青混凝土路面的空隙，形成柔性-刚性互穿的半柔性路面结构可用于减少交通道口和重交通区域的车辙现象；在油田固井工程领域，CA砂浆有望作为一类新型的固井材料，其良好的韧性可减少水泥环因套管内压力反复变化带来的疲劳损伤以及消除后期射孔作业引起的龟裂纹.
新拌CA砂浆存在多种带电粒子，如水泥颗粒，乳化沥青颗粒，游离乳化剂分子，减水剂分子等.带电粒子之间的相互作用与浆体宏观流变性能和工作性密不可分[9-13].减水剂是调节CA砂浆工作性能的重要外加剂[14]，减水剂分子通过吸附作用延迟水泥水化并使水泥颗粒分散，其机理已为人们所熟知[15-16]，水泥吸附乳化沥青颗粒，引起水泥水化进程及浆体工作性能变化的研究也有所报道[13-16]，但乳化沥青与减水剂同掺时水泥与其的吸附行为及机理却鲜有报道.减水剂和乳化沥青均与水泥有吸附关系，吸附关系是影响CA砂浆流变性能的重要因素，探明三者间的复杂吸附关系是揭示CA砂浆流变性时温效应作用机制的关键环节.文献[17-20]研究发现聚合物水泥砂浆中掺加减水剂后抑制了水泥对聚合物颗粒的吸附，在含有萘系减水剂的聚合物水泥砂浆中，减水剂分子优先于聚合物颗粒被水泥颗粒吸附，聚合物水泥砂浆中制备时掺入聚羧酸减水剂，水泥优先吸附聚羧酸减水剂，且吸附不是无限量的，饱和后就不再吸附聚合物颗粒.聚合物乳液与乳化沥青乳液具有一定的相似性，因此减水剂在聚合物水泥砂浆中的吸附规律可以为乳化沥青水泥砂浆的研究提供参考.此外，文献[21-22]研究减水剂对CA砂浆流变参数的影响后提出了减水剂与乳化沥青对水泥的吸附存在竞争性的猜想，但是缺乏直接的证据来加以证明.为此，本文研究了聚羧酸减水剂在CA砂浆中的吸附行为，以期揭示减水剂与乳化沥青对水泥粒子的吸附规律.
1 试验 1.1 原材料采用中联水泥有限公司生产的P·I 42.5水泥，其化学组分见表 1.分别采用了江苏苏博特新材料股份有限公司和美德维实伟克公司生产的EA-601和LA型乳化沥青，两者的沥青蒸发残留物含量均为60%，乳化沥青粒径分布如图 1所示，两者的峰值粒径分别为1.64、2.84 μm，X90分别为3.97、17.49 μm.相应的乳化剂均为慢裂型阴离子乳化剂.
表 1
表 1 水泥的化学组成 Table 1 Compositions of Portland cement 氧化物 Al2O3 CaO Fe2O3 K2O MgO Na2O SO3 SiO2 TiO2 w/% 4.600 61.083 3.186 0.682 2.093 0.154 4.434 20.300 0.282
表 1 水泥的化学组成 Table 1 Compositions of Portland cement
Figure 1
图 1 乳化沥青的粒径分布曲线 Figure 1 Particle size distribution of emulsified asphalt 采用PCA-Ⅰ、PCA-Ⅲ型聚羧酸减水剂和JM-A萘系减水剂，皆由江苏苏博特新材料股份有限公司生产，前两者皆为浅褐色液体，固含量分别为21.7%、30.0%，最后者为深褐色固态粉体.聚羧酸减水剂的重均相对分子质量、相对分子质量分布、酸醚比(物质的量之比)和电荷密度(质量)见表 2.
表 2
表 2 聚羧酸减水剂的性能 Table 2 Performance parameters of polycarboxylate superplasticizer 减水剂 重均相对分子质量/(g·mol-1) 相对分子质量分布 酸醚比 电荷密度/
(mmol·g-1)
PCA-Ⅰ 23 550 1.93 3:1 1.78
PCA-Ⅲ 38 640 1.85 2:1 1.22
表 2 聚羧酸减水剂的性能 Table 2 Performance parameters of polycarboxylate superplasticizer
1.2 测试方法水化热采用美国TA公司生产的TAM Air型等温量热仪进行测定，其操作方法参考文献[23]，测试时间持续72 h.水泥-乳化沥青吸附实验方法参考文献[23]，其原理为水泥吸附沥青颗粒后乳液的沥青固含量发生改变，通过精确测量吸附作用前后乳液固含量之差计算得到水泥对乳化沥青的吸附量.水泥与乳化沥青的显微吸附实验采用尼康公司生产的Eclipse E400型显微镜进行观测，采用文献[24]所述的特制样品托盛放样品.
2 结果与讨论本文首先总结了减水剂、乳化沥青同掺时水泥水化诱导期延迟的叠加效应规律，从宏观层面提出了减水剂和乳化沥青与水泥的吸附行为可能存在先后的猜想；其次，从微观层面上考查了减水剂对水泥乳化沥青吸附经时规律的影响，并结合显微观测对CA砂浆中减水剂、乳化沥青对水泥的吸附存在竞争性的规律进行了佐证；基于宏观及微观方面的研究结论提出了含减水剂的水泥乳化沥青经时的吸附模型.
2.1 水化诱导期的延长W/C为0.41的水泥净浆中分别掺加0.7%(以水泥质量计)的PCA-Ⅰ和PCA-Ⅲ减水剂，掺加聚羧酸减水剂后水泥水化诱导期明显延长，如图 2所示，水化诱导期分别延长了3.87、3.09 h.
Figure 2
图 2 减水剂对水泥水化的影响 Figure 2 Influence of superplasticizer on cement hydration 以EA-601和LA两种乳化沥青为原料按照W/C为0.41，A/C(沥青水泥质量比)为0.24的配合比制备水泥沥青砂浆，两者的水泥水化诱导期较水泥净浆明显延长，如图 3所示，水化诱导期分别延长了2.11、1.51 h.
Figure 3
图 3 乳化沥青水泥水化的影响 Figure 3 Influence of emulsified asphalt on cement hydration 上述两种CA砂浆中分别掺入PCA-Ⅰ和PCA-Ⅲ聚羧酸减水剂，CA砂浆中水泥的水化诱导期进一步得到延长，如图 4所示. PCA-Ⅰ和PCA-Ⅲ分别使EA-601水泥沥青砂浆的水泥水化诱导期延长了5.24、4.06 h，如图 4(a)所示，分别使LA水泥沥青砂浆的水泥水化诱导期分别延长了4.39、3.43 h，如图 4(b)所示.
Figure 4
图 4 减水剂与乳化沥青复掺对水泥水化的影响 Figure 4 Influence of co-adding of superplasticizer and emulsified asphalt on cement hydration 由上可知，聚羧酸减水剂和乳化沥青都能延长水泥水化历程的诱导期长度，且两者单独掺加时的延长效果小于两者同掺时的效果，即两者的共存对水泥水化诱导期的延迟产生了明显的协同效应，如图 5所示.
Figure 5
图 5 水化诱导期延长的协同效应 Figure 5 Synergistic effect of hydration induction period 乳化沥青延迟水泥水化诱导期是由于水泥吸附了乳化沥青中的未参与乳化的乳化剂分子和乳化沥青颗粒[16]，减水剂延迟水泥水化诱导期是由于水泥吸附了减水剂分子[15-16]，乳化剂或减水剂分子通过吸附、络合、静电斥力及空间位阻的作用，有效抑制初期C3A和C3S水化，导致水化速率放缓[25].乳化沥青和减水剂同掺对水泥水化延迟的协同效应在一定程度上反应了水泥对此二者的吸附存在先后顺序，由此在宏观上表现出了延迟作用的“接力”效果.
2.2 减水剂对吸附的影响前期研究发现无减水剂时水泥-乳化沥青经时吸附曲线的形状呈“双峰形”，并按照阶段性吸附特征将吸附曲线分为了4个阶段：曲线第一个的峰的上升段和下降段分别对应了“溶解吸附阶段”和“竞争吸附阶段”，第二个峰的上升段和下降段分别对应了“加速吸附阶段”和“饱和吸附阶段”[24].
减水剂(有效物质与水泥质量比相同)对水泥吸附乳化沥青的影响见图 6所示.掺加减水剂后水泥乳化沥青吸附曲线的形状仍呈“双峰形”，不同之处在于吸附曲线的各吸附阶段的起止时间，历程长度以及饱和吸附率均发生了明显变化.主要体现在以下几个方面：1)对溶解吸附阶段影响不明显；2)延长了竞争吸附阶段，两种聚羧酸减水剂都显著延长了竞争吸附阶段，而萘系减水剂的延迟效果不明显(可能与质量浓度低有关及吸附快有关)；3)提高了加速吸附阶段的吸附速率；4)增大了饱和吸附率，使饱和吸附阶段发生了明显的解吸附(掺PCA-Ⅰ后的解吸附现象可能在观测期后延期间发生).
Figure 6
图 6 减水剂种类对吸附的影响 Figure 6 Influence of superplasticizer type on adsorption 聚羧酸减水剂分子优先于乳化沥青颗粒被水泥所吸附使竞争吸附阶段历程得以延长，水泥吸附聚羧酸减水剂分子的过程不吸附乳化沥青颗粒.
将不同剂量的PCA-Ⅰ减水剂按“先加”和“后加”两种顺序添加，前者减水剂先掺加到乳化沥青中再和水泥混合，后者乳化沥青先与水泥混合，2 h后再往混合液中添加减水剂.改变减水剂添加顺序后的吸附规律如图 7所示.添加方式Ⅰ：吸附曲线的竞争吸附阶段历程显著延长，加速吸附阶段平均吸附速率明显提高，且预掺减水剂的量越大，竞争吸附阶段历程延长效果越显著，加速吸附阶段平均吸附速率越快.竞争吸附阶段水泥优先吸附减水剂分子，浆体中游离减水剂分子耗尽后水泥才再次吸附乳化沥青颗粒.因此，减水剂初始质量浓度越高，则吸附过程所用的时间越长.添加方式Ⅱ：掺加后部分已吸附的乳化沥青逐渐解吸附，0.5 h内使吸附率降至竞争吸附阶段末期的吸附率水平，并使随后一段时间内水泥对乳化沥青吸附基本停滞.减水剂掺量为1.0%时，添加8 h后水泥对乳化沥青的吸附速率再次上升，而掺量为1.5%时在添加后10 h内水泥对乳化沥青的吸附依旧处于基本停止状态，即掺量越高，延迟效果越明显.该现象也反映了减水剂与乳化沥青竞争吸附关系：减水剂吸附的优先性使得部分吸附不牢固的乳化沥青颗粒与水泥的吸附作用减弱而解吸附，吸附使浆体中减水剂质量浓度逐渐下降，减水剂耗尽后水泥颗粒才再次吸附乳化沥青颗粒，所以后掺减水剂质量浓度越高延迟效果约明显.
Figure 7
图 7 减水剂掺加顺序对吸附的影响 Figure 7 Influence of adding order of superplasticizer on adsorption 上述CA砂浆中水泥优先吸附减水剂分子的规律可总结如下：溶解吸附阶段与水泥颗粒表层高水化活性矿物相的溶解以及润湿作用有关，持续时间短，水泥对乳化沥青和减水剂的吸附没有明显的选择性；水泥在竞争吸附阶段有明显的拣选性，减水剂分子先于乳化沥青被吸附，吸附意味着水泥水化活性位点被占据.水化反应和水化产物的溶解生成了新的界面和新的活性位点，被吸附的减水剂分子逐渐被水化产物“掩埋”而减少.当浆体中减水剂分子不足以维持水化产物新界面和水泥颗粒新活性位点的吸附需要时，水泥颗粒再次吸附乳化沥青，即竞争吸附阶段结束，吸附进入加速吸附阶段.减水剂分子远小于乳化沥青颗粒，电荷密度集中，故而其扩散能力强于乳化沥青，因此能够进入水泥颗粒与乳化沥青颗粒间的空间，削弱水泥与乳化沥青间的吸附力，最终使吸附的乳化沥青解吸附.
2.3 显微吸附乳化沥青稀释200倍后与水泥按照质量比30:1混合，然后吸取少许样品置于样品托的微腔内，加盖盖玻片使微腔体边缘一侧留出一狭小加料口.混合3 min时吸取少许稀释的PCA-Ⅰ减水剂滴在加料口处，使减水剂溶液缓慢渗入样品托的微腔体内，试验过程中用相机记录水泥乳化沥青的吸附行为.
图 8为水泥乳化沥青吸附行为的显微观测结果.水泥吸附乳化沥青的过程分为4个阶段：1)溶解吸附，3 min以前水泥对乳化沥青的吸附量逐渐增大；2)解吸附阶段，3 min以后部分吸附的乳化沥青颗粒逐渐发生解吸附，解吸附作用在15 min时减弱；3)快速吸附阶段，15 min以后水泥再度开始吸附乳化沥青，并且速率明显加快；4)饱和吸附阶段，30 min时水泥吸附乳化沥青量逐渐趋于饱和.
Figure 8
图 8 减水剂优先吸附 Figure 8 Preferential adsorption of superplasticizer 溶解吸附是由于水泥颗粒表面水化活性高的矿物相溶解以及润湿作用引起的；随着减水剂分子进入混合物溶液，减水剂分子与吸附的乳化沥青发生了置换，部分乳化沥青颗粒发生解吸附；混合物溶液中减水剂质量浓度逐渐下降，当其质量浓度低于一定值后水泥颗粒再度开始吸附乳化沥青；水泥对乳化沥青的吸附量增加，然后逐渐趋于饱和.聚羧酸减水剂与吸附乳化沥青发生置换的事实说明了在CA砂浆体系中水泥优先吸附减水剂.吸附行为的显微观测结果与吸附率试验结果完全吻合.
2.4 竞争吸附模型基于上述宏观及微观方面的研究结论，CA砂浆中减水剂的吸附规律可用如下模型(图 9)进行描述：1)溶解吸附阶段，水泥乳化沥青砂浆自拌和起即进入溶解吸附阶段，期间水泥颗粒对其周围的乳化沥青颗粒和减水剂分子进行无选择性的吸附，该阶段的吸附作用持续时间短，峰值吸附率总体较低；2)竞争吸附阶段，水泥颗粒吸附其附近的减水剂，使部分吸附的乳化沥青颗粒解吸附，该阶段内水泥对乳化沥青的吸附基本停滞；3)加速吸附阶段，吸附的减水剂分子被水化产物掩埋而逐渐耗尽，当减水剂不足以维持水泥水化的吸附需要时，水泥颗粒再次吸附乳化沥青颗粒.
Figure 9
图 9 减水剂乳化沥青竞争吸附模型 Figure 9 Competitive adsorption model of superplasticizer and emulsified asphalt 3 结论1) CA砂浆中的乳化沥青和减水剂均能显著延迟水泥的水化诱导期，两者共掺时的延迟作用产生了叠加效应.
2) 聚羧酸减水剂能显著延长水泥乳化沥青的竞争吸附阶段，提高加速吸附阶段的吸附速率，增大饱和吸附率.减水剂掺量越高，竞争吸附延长效应越明显，加速吸附阶段平均吸附速率越高，饱和吸附率也越高.
3) 含减水剂的CA砂浆中，水泥对减水剂与乳化沥青的吸附表现出明显的选择性.在竞争吸附阶段水泥吸附减水剂的优先度高于乳化沥青，减水剂可使部分已吸附的乳化沥青解吸附.浆体溶液中减水剂耗尽后水泥颗粒再次吸附乳化沥青，吸附进入加速吸附阶段.
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