PB-g-PS胶乳改性水泥砂浆的性能及微观结构
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摘要
本文合成了聚丁二烯接技聚苯乙烯(PB-g-PS)和聚丁二烯接技聚苯乙烯甲基丙烯酸环氧丙酯(PB-g-PSG)胶乳,并用于改性水泥砂浆,考察了改性砂浆的性能与微观结构,利用FTIR、DSC、TG以及XRD等分析手段研究了胶乳含量、硅灰和偶联剂单独和结合对水泥水化作用的影响,具体主要做了如下几项工作：
1、采用半连续种子乳液接技聚合技术,在聚丁二烯乳胶粒子上接技共聚苯乙烯,合成了PB-g-PS接技共聚物。研究了合成工艺条件对接技共聚反应的影响,结果发现,苯乙烯在聚丁二烯橡胶粒子上的接技效率和接技度随聚丁二烯对苯乙烯质量比的增加而降低,随反应温度的增加而增加,随引发剂浓度的增加呈先增加后降低的变化趋势,接技效率随单体滴加时间的增加而增加,接技度则呈先增加后降低的变化趋势。利用FTIR和1H NMR对PB-g-PS接技共聚物进行了表征,证明合成了目的产物。利用TEM对PB-g-PS乳胶粒子进行形态观察,接技物为球形粒子,且具有核壳结构。
2、将质量比为70/30、50/50和30/70的三种PB-g-PS胶乳用于改性水泥砂浆,在固定流动度为175±5mm和固定水灰比为0.5两种控制方式,以及在混合养护和水养护的两种养护条件下,考察了PB-g-PS胶乳改性水泥砂浆的物理、力学性能。在固定流动度和混合养护条件下并与SD623羧基丁苯胶乳改性水泥砂浆作性能对比。研究发现,三种胶乳能够改善砂浆的和易性,降低水灰比提高减水率,减水率超过56%。能有效地提高新拌砂浆的保水作用,保水率最高达99%。能够显著降低改性砂浆水吸收速率,P/C比为20%时,24h改性砂浆的水吸收速率仅为0.156Kg/m2。三种胶乳改性砂浆的体积密度随聚灰比的增加呈先降低后增加或先增加后降低的变化趋势。聚合物改性砂浆的抗压、抗折强度随聚灰比的增加呈波动的变化趋势。对比三种胶乳改性砂浆的性能发现,质量比为50/50的胶乳改性砂浆性能好于70/30和30/70两种胶乳改性砂浆的性能。三种胶乳改性砂浆性能与SD623羧基丁苯胶乳改性水泥砂浆作性能对比发现,质量比为50/50的胶乳改性砂浆性能与SD623羧基丁苯胶乳改性水泥砂浆性能相当。
3、利用SEM考察了PB-g-PS胶乳改性水泥砂浆的微观结构,研究发现,改性砂浆各组分紧密地结合在一起,砂浆结构更为致密。PB-g-PS胶乳在砂浆中可以形成膜结构。聚合物膜有时存在砂浆的孔洞中,有时存在于水化产物之间,有时也存在与水化产物与骨料之间。聚合物膜呈现为不同的形态,有时为树枝状结构、带状结构,有时形成了连续的互穿网络结构。改善了砂浆结构,有效的阻止了微裂纹的发展,填充和封闭了孔洞和缝隙,改善了砂浆的性能。
4、在固定水灰比为0.45以及水养护的情况下,将硅灰和偶联剂加入到质量比为50/50的PB-g-PS胶乳改性水泥砂浆中。研究发现,硅灰的加入对改性砂浆的性能产生重要影响,硅灰加入适量时能够改善砂浆的结构,有利于性能的提高,但硅灰的加入量达15%时,由于未加减水剂,导致砂浆的流动性不好,硅灰发生团聚作用,从而使性能降低,硅灰适宜的加入量为水泥质量的10%；偶联剂的加入对砂浆的性能也产生重要影响,偶联剂的加入量为1.0%时,导致新拌砂浆流动度过大,使砂浆产生了更多的孔洞和裂缝,从而使性能降低。偶联剂的适宜加入量为水泥质量的0.6%；将硅灰、偶联剂同时加入到PB-g-PS胶乳改性水泥砂浆中时,在固定硅灰的加入量时,发现随偶联剂含量的增加,性能逐渐改善；在固定偶联剂的加入量时,随硅灰含量的增加性能也逐渐得到改善。利用SEM考察了改性砂浆的微观结构,微观结构分析表明：改性砂浆结构更加致密,观察到了树枝状结构以及氢氧化钙的六角形片状晶体结构。同时利用FTIR、DSC、TG以及XRD等分析手段研究了PB-g-PS胶乳、硅灰及偶联剂等对水泥水化作用的影响。结果表明：随聚灰比的增加,水泥水化程度呈先增加后降低的变化趋势,聚灰比为10%时,水泥水化程度最高：在相同聚灰比时,随硅灰含量的增加,水泥水化程度呈降低的变化趋势,硅灰含量为5%时,水化程度最高；在相同聚灰比时,随偶联剂含量的增加,水泥水化程度呈先增加后降低的变化趋势,偶联剂含量为0.6%时,水泥水化程度最高；固定硅灰含量时,随偶联剂含量增加,水泥水化程度呈先降低后增加的变化趋势,偶联剂含量为0.2%时,水泥水化程度最高；固定偶联剂含量时,随硅灰含量增加,水泥水化程度呈先增加后降低的变化趋势,硅灰含量为10%时,水泥水化程度最高。
5、利用GMA对PB-g-PS胶乳进行改性,在PB-g-PS胶乳最佳制备工艺条件下,合成了质量比为50/50/0、50/49/1和50/46/4三种PB-g-PSG胶乳,并通过FTIR对合成的目的产物进行了表征。在固定水灰比为0.4以及混合养护条件下,考察了GMA含量对PB-g-PSG胶乳改性水泥砂浆的性能及微观结构的影响。研究发现,随GMA含量的增加,改性砂浆的性能也逐渐得到提高。同时利用FTIR和DSC考察了GMA对水泥水化作用的影响,发现Ca(OH)2含量随GMA含量的增加而减少,说明GMA与Ca(OH)2发生了螯合作用。利用SEM考察了改性砂浆的微观结构,在孔洞中观察到了Ca(OH)2的六角形的片状晶体结构,而且随GMA含量的增加孔洞中Ca(OH)2数量逐渐减少,进一步证明GMA与氢氧化钙发生了化学作用,与FTIR和DSC分析结果一致。
The paper synthesized polybutadiene-graft-polystyrene (PB-g-PS) latexes and polybutadiene-graft-polystyrene epoxypropyl methacrylate (PB-g-PSG), and be used to modify cement mortar. The properties and microstructure of modified mortar were investigated. The effect of PB-g-PS latex, silica fume and coupling agent on cement hydration were researched by FTIR、DSC、TG and XRD, the main works as follows:
Graft copolymers of styrene (St) onto polybutadiene (PB) were prepared via semiconscious seeded emulsion grafting copolymerization method using a redox initiator system. The effect of initiator, reaction temperature, qualitys ratio of PB/PS, and monomer dropping time on the graft copolymerization were investigated. The results show that the grafting efficiency (GE) and degree of grafting (DG) increase with increase reaction temperature and decrease quality ratio of PB/PS.The GE and DG is increased with increase initiator content for low content, and then begin to decrease of higher content of initiator. The GE is increased with increase monomer dropping time. The DG is increased first, and then decreased with increase monomer dropping time. The synthesized PB-g-PS was confirmed by FTIR and1H NMR. The morphology and diameter of PB-g-PS latex particle were studied by TEM and laser diameter analyzer. The study show that PB-g-PS latex particle is ball-like, and have a core-shell shaped structure.
The PB-g-PS latex with the mass ratios of70/30,50/50to30/70were used to modify cement mortar. In the fixed flow of175±5mm and a constant water-cement ratio(W/C) of0.5,and two curing methods(mixed curing methods:6d immersed in20℃water followed by21d at20℃,RH65%air; wet curing methods:27d immersed in20℃water).This study examines the effect of mass ratios of PB/PS on physical and mechanical properties of PB-g-PS latex-modified cement mortars, and compared with performance of the carboxyl SBR latex-modified cement mortar at fixed flow of175±5mm and mixed curing condition. The experimental results show that the three kinds of latex-modified mortars has a good workability, can decrease W/C, and improve water reduction rate, it exceeded56%. Its can improve the performance of mortar water retention during a certain range of P/C, and the maximum of water retention ratio are99%.The PB-g-PS latex can markedly reduce capillary water absorption rate, it reaches0.156Kg/m2at the P/C of20%and24h.The bulk density is decreased firstly, and increased with increase P/C,or is increased firstly, and then decreased.PB-g-PS latex can marked in influences much on the mechanical properties of modified mortars. The compressive and the flexural strength of the polymer modified mortar are fluctuated with increase P/C. By contrast, the properties of mass ratio of50/50latex modified mortar are best, and is almost with SD623carboxyl SBR latex-modified cement mortar.
The polymer modified mortar structure was studied by SEM. The microstructure analysis showed that mortar constituents in PMMs are compactly joined with each other, and the structure is close. Polymer film has already formed in the polymer-modified cement mortars, which exist in cave, hydrates, and between hydrates and aggregate.The polymer film may acquire different structures. They may appear as branch-like, band-like, and dense network structure. The structure was improved because of addition of polymer to cement mortars. The development of little crackle was effective prevented, and the holes and chink were packed and closed. Hence, the performance of the mortar has been improved.
In the constant water-cement ratio of0.45and using water curing methods. PB-g-PS latex with a mass ratio of50/50was used to modify cement mortar. This study examines the effects of silica fume and coupling agent content on properties and structure of latex modified cement mortar. The experimental results show that silica fume can marked in influences much on the properties of modified mortars. The suitable silica fume content can improve properties and structure of mortars. The flowability of mortar is bad at silica fume content of15%, and water-reducing agent not be added. Hence, the silica fume is aggregated, resulting in reducing performance. The suitable silica fume content is cement mass of10%; the coupling agent can also marked in influences much on the properties and structure of modified mortars. The flow of fresh mortar is bigger at coupling agent content of1.0%, which leaded in more caves and chink in PMMs. The suitable coupling agent content is cement mass of0.6%; the properties of modified mortar increase with increase silica fume and coupling agent content when its were added into PB-g-PS latex-modified mortars. The modified mortar structure was studied by SEM. The microstructure analysis showed that the structure is close.The tree structure and hexagonal sheet crystal structure of Ca(OH)2was seen.The effect of PB-g-PS latex, silica fume and coupling agent on cement hydration were researched by FTIR、DSC、TG and XRD. The experiments results show that the cement hydration increase with an increase of P/C for low P/C, and then begin to decrease of higher P/C, it reached a maximum at P/C of10%; with an increase silica fume content up to5%are accompanied by a significant increase in cement hydration, beyond this content, the cement hydration decrease markedly; it increase as the coupling agent content increase,the cement hydration increase and reaches a maximum at the content0.6%; at a constant silica fume content of15%, it can seen that as coupling agent content increase there is decrease in the cement hydration, at content of0.2%, it reaches a maximum value; at a fixed coupling agent content of0.6%,with an increase silica fume content, it causes an increase in the cement hydration, when the silica fume content was higher10%,the cement hydration decreased.
The PB-g-PSG were synthesized at the best process conditions of PB-g-PS, and the quality ratios of polybutadiene to styrene and epoxypropyl methacrylate ranged from50/50/0,50/49/1to50/46/4. The PB-g-PSG be confirmed by FTIR, and was used to modify cement mortar in the constant water-cement ratio of0.4and mixed curing.This study examines the effects of GMA content and the P/C ratios on properties of PB-g-PSG latex modified cement mortar, and compared with performance of the carboxyl SBR latex-modified cement mortar. The study show that the flow of modified mortar is increased with increasing polymer-cement ratios, and is almost change with increasing GMA content. The four kinds of latex can markedly reduce capillary water absorption rate, and can marked in influences much on the mechanical properties of modified mortars. The compressive strength of PB-g-PSG are decreased with increasing P/C, and are lower than control mortar, and flexural strength of polymer modified mortars are increased with increasing P/C at P/C lower than10%, and are higher than control mortar. The maximum of flexural strength of polymer-modified mortar are9.65MPa. The effect of polymer on cement hydration was explored by FTIR and DSC, the analysis results showed that the cement hydration was influenced by GMA content and P/C. Polymer modified mortar structure was studied by SEM. The microstructure analysis showed that the mortar constituents of polymer-modified cement mortars are compactly joined, have ultimate improved properties. The hexagonal sheet crystal structure of Ca(OH)2was seen.
1、采用半连续种子乳液接技聚合技术,在聚丁二烯乳胶粒子上接技共聚苯乙烯,合成了PB-g-PS接技共聚物。研究了合成工艺条件对接技共聚反应的影响,结果发现,苯乙烯在聚丁二烯橡胶粒子上的接技效率和接技度随聚丁二烯对苯乙烯质量比的增加而降低,随反应温度的增加而增加,随引发剂浓度的增加呈先增加后降低的变化趋势,接技效率随单体滴加时间的增加而增加,接技度则呈先增加后降低的变化趋势。利用FTIR和1H NMR对PB-g-PS接技共聚物进行了表征,证明合成了目的产物。利用TEM对PB-g-PS乳胶粒子进行形态观察,接技物为球形粒子,且具有核壳结构。
2、将质量比为70/30、50/50和30/70的三种PB-g-PS胶乳用于改性水泥砂浆,在固定流动度为175±5mm和固定水灰比为0.5两种控制方式,以及在混合养护和水养护的两种养护条件下,考察了PB-g-PS胶乳改性水泥砂浆的物理、力学性能。在固定流动度和混合养护条件下并与SD623羧基丁苯胶乳改性水泥砂浆作性能对比。研究发现,三种胶乳能够改善砂浆的和易性,降低水灰比提高减水率,减水率超过56%。能有效地提高新拌砂浆的保水作用,保水率最高达99%。能够显著降低改性砂浆水吸收速率,P/C比为20%时,24h改性砂浆的水吸收速率仅为0.156Kg/m2。三种胶乳改性砂浆的体积密度随聚灰比的增加呈先降低后增加或先增加后降低的变化趋势。聚合物改性砂浆的抗压、抗折强度随聚灰比的增加呈波动的变化趋势。对比三种胶乳改性砂浆的性能发现,质量比为50/50的胶乳改性砂浆性能好于70/30和30/70两种胶乳改性砂浆的性能。三种胶乳改性砂浆性能与SD623羧基丁苯胶乳改性水泥砂浆作性能对比发现,质量比为50/50的胶乳改性砂浆性能与SD623羧基丁苯胶乳改性水泥砂浆性能相当。
3、利用SEM考察了PB-g-PS胶乳改性水泥砂浆的微观结构,研究发现,改性砂浆各组分紧密地结合在一起,砂浆结构更为致密。PB-g-PS胶乳在砂浆中可以形成膜结构。聚合物膜有时存在砂浆的孔洞中,有时存在于水化产物之间,有时也存在与水化产物与骨料之间。聚合物膜呈现为不同的形态,有时为树枝状结构、带状结构,有时形成了连续的互穿网络结构。改善了砂浆结构,有效的阻止了微裂纹的发展,填充和封闭了孔洞和缝隙,改善了砂浆的性能。
4、在固定水灰比为0.45以及水养护的情况下,将硅灰和偶联剂加入到质量比为50/50的PB-g-PS胶乳改性水泥砂浆中。研究发现,硅灰的加入对改性砂浆的性能产生重要影响,硅灰加入适量时能够改善砂浆的结构,有利于性能的提高,但硅灰的加入量达15%时,由于未加减水剂,导致砂浆的流动性不好,硅灰发生团聚作用,从而使性能降低,硅灰适宜的加入量为水泥质量的10%；偶联剂的加入对砂浆的性能也产生重要影响,偶联剂的加入量为1.0%时,导致新拌砂浆流动度过大,使砂浆产生了更多的孔洞和裂缝,从而使性能降低。偶联剂的适宜加入量为水泥质量的0.6%；将硅灰、偶联剂同时加入到PB-g-PS胶乳改性水泥砂浆中时,在固定硅灰的加入量时,发现随偶联剂含量的增加,性能逐渐改善；在固定偶联剂的加入量时,随硅灰含量的增加性能也逐渐得到改善。利用SEM考察了改性砂浆的微观结构,微观结构分析表明：改性砂浆结构更加致密,观察到了树枝状结构以及氢氧化钙的六角形片状晶体结构。同时利用FTIR、DSC、TG以及XRD等分析手段研究了PB-g-PS胶乳、硅灰及偶联剂等对水泥水化作用的影响。结果表明：随聚灰比的增加,水泥水化程度呈先增加后降低的变化趋势,聚灰比为10%时,水泥水化程度最高：在相同聚灰比时,随硅灰含量的增加,水泥水化程度呈降低的变化趋势,硅灰含量为5%时,水化程度最高；在相同聚灰比时,随偶联剂含量的增加,水泥水化程度呈先增加后降低的变化趋势,偶联剂含量为0.6%时,水泥水化程度最高；固定硅灰含量时,随偶联剂含量增加,水泥水化程度呈先降低后增加的变化趋势,偶联剂含量为0.2%时,水泥水化程度最高；固定偶联剂含量时,随硅灰含量增加,水泥水化程度呈先增加后降低的变化趋势,硅灰含量为10%时,水泥水化程度最高。
5、利用GMA对PB-g-PS胶乳进行改性,在PB-g-PS胶乳最佳制备工艺条件下,合成了质量比为50/50/0、50/49/1和50/46/4三种PB-g-PSG胶乳,并通过FTIR对合成的目的产物进行了表征。在固定水灰比为0.4以及混合养护条件下,考察了GMA含量对PB-g-PSG胶乳改性水泥砂浆的性能及微观结构的影响。研究发现,随GMA含量的增加,改性砂浆的性能也逐渐得到提高。同时利用FTIR和DSC考察了GMA对水泥水化作用的影响,发现Ca(OH)2含量随GMA含量的增加而减少,说明GMA与Ca(OH)2发生了螯合作用。利用SEM考察了改性砂浆的微观结构,在孔洞中观察到了Ca(OH)2的六角形的片状晶体结构,而且随GMA含量的增加孔洞中Ca(OH)2数量逐渐减少,进一步证明GMA与氢氧化钙发生了化学作用,与FTIR和DSC分析结果一致。
The paper synthesized polybutadiene-graft-polystyrene (PB-g-PS) latexes and polybutadiene-graft-polystyrene epoxypropyl methacrylate (PB-g-PSG), and be used to modify cement mortar. The properties and microstructure of modified mortar were investigated. The effect of PB-g-PS latex, silica fume and coupling agent on cement hydration were researched by FTIR、DSC、TG and XRD, the main works as follows:
Graft copolymers of styrene (St) onto polybutadiene (PB) were prepared via semiconscious seeded emulsion grafting copolymerization method using a redox initiator system. The effect of initiator, reaction temperature, qualitys ratio of PB/PS, and monomer dropping time on the graft copolymerization were investigated. The results show that the grafting efficiency (GE) and degree of grafting (DG) increase with increase reaction temperature and decrease quality ratio of PB/PS.The GE and DG is increased with increase initiator content for low content, and then begin to decrease of higher content of initiator. The GE is increased with increase monomer dropping time. The DG is increased first, and then decreased with increase monomer dropping time. The synthesized PB-g-PS was confirmed by FTIR and1H NMR. The morphology and diameter of PB-g-PS latex particle were studied by TEM and laser diameter analyzer. The study show that PB-g-PS latex particle is ball-like, and have a core-shell shaped structure.
The PB-g-PS latex with the mass ratios of70/30,50/50to30/70were used to modify cement mortar. In the fixed flow of175±5mm and a constant water-cement ratio(W/C) of0.5,and two curing methods(mixed curing methods:6d immersed in20℃water followed by21d at20℃,RH65%air; wet curing methods:27d immersed in20℃water).This study examines the effect of mass ratios of PB/PS on physical and mechanical properties of PB-g-PS latex-modified cement mortars, and compared with performance of the carboxyl SBR latex-modified cement mortar at fixed flow of175±5mm and mixed curing condition. The experimental results show that the three kinds of latex-modified mortars has a good workability, can decrease W/C, and improve water reduction rate, it exceeded56%. Its can improve the performance of mortar water retention during a certain range of P/C, and the maximum of water retention ratio are99%.The PB-g-PS latex can markedly reduce capillary water absorption rate, it reaches0.156Kg/m2at the P/C of20%and24h.The bulk density is decreased firstly, and increased with increase P/C,or is increased firstly, and then decreased.PB-g-PS latex can marked in influences much on the mechanical properties of modified mortars. The compressive and the flexural strength of the polymer modified mortar are fluctuated with increase P/C. By contrast, the properties of mass ratio of50/50latex modified mortar are best, and is almost with SD623carboxyl SBR latex-modified cement mortar.
The polymer modified mortar structure was studied by SEM. The microstructure analysis showed that mortar constituents in PMMs are compactly joined with each other, and the structure is close. Polymer film has already formed in the polymer-modified cement mortars, which exist in cave, hydrates, and between hydrates and aggregate.The polymer film may acquire different structures. They may appear as branch-like, band-like, and dense network structure. The structure was improved because of addition of polymer to cement mortars. The development of little crackle was effective prevented, and the holes and chink were packed and closed. Hence, the performance of the mortar has been improved.
In the constant water-cement ratio of0.45and using water curing methods. PB-g-PS latex with a mass ratio of50/50was used to modify cement mortar. This study examines the effects of silica fume and coupling agent content on properties and structure of latex modified cement mortar. The experimental results show that silica fume can marked in influences much on the properties of modified mortars. The suitable silica fume content can improve properties and structure of mortars. The flowability of mortar is bad at silica fume content of15%, and water-reducing agent not be added. Hence, the silica fume is aggregated, resulting in reducing performance. The suitable silica fume content is cement mass of10%; the coupling agent can also marked in influences much on the properties and structure of modified mortars. The flow of fresh mortar is bigger at coupling agent content of1.0%, which leaded in more caves and chink in PMMs. The suitable coupling agent content is cement mass of0.6%; the properties of modified mortar increase with increase silica fume and coupling agent content when its were added into PB-g-PS latex-modified mortars. The modified mortar structure was studied by SEM. The microstructure analysis showed that the structure is close.The tree structure and hexagonal sheet crystal structure of Ca(OH)2was seen.The effect of PB-g-PS latex, silica fume and coupling agent on cement hydration were researched by FTIR、DSC、TG and XRD. The experiments results show that the cement hydration increase with an increase of P/C for low P/C, and then begin to decrease of higher P/C, it reached a maximum at P/C of10%; with an increase silica fume content up to5%are accompanied by a significant increase in cement hydration, beyond this content, the cement hydration decrease markedly; it increase as the coupling agent content increase,the cement hydration increase and reaches a maximum at the content0.6%; at a constant silica fume content of15%, it can seen that as coupling agent content increase there is decrease in the cement hydration, at content of0.2%, it reaches a maximum value; at a fixed coupling agent content of0.6%,with an increase silica fume content, it causes an increase in the cement hydration, when the silica fume content was higher10%,the cement hydration decreased.
The PB-g-PSG were synthesized at the best process conditions of PB-g-PS, and the quality ratios of polybutadiene to styrene and epoxypropyl methacrylate ranged from50/50/0,50/49/1to50/46/4. The PB-g-PSG be confirmed by FTIR, and was used to modify cement mortar in the constant water-cement ratio of0.4and mixed curing.This study examines the effects of GMA content and the P/C ratios on properties of PB-g-PSG latex modified cement mortar, and compared with performance of the carboxyl SBR latex-modified cement mortar. The study show that the flow of modified mortar is increased with increasing polymer-cement ratios, and is almost change with increasing GMA content. The four kinds of latex can markedly reduce capillary water absorption rate, and can marked in influences much on the mechanical properties of modified mortars. The compressive strength of PB-g-PSG are decreased with increasing P/C, and are lower than control mortar, and flexural strength of polymer modified mortars are increased with increasing P/C at P/C lower than10%, and are higher than control mortar. The maximum of flexural strength of polymer-modified mortar are9.65MPa. The effect of polymer on cement hydration was explored by FTIR and DSC, the analysis results showed that the cement hydration was influenced by GMA content and P/C. Polymer modified mortar structure was studied by SEM. The microstructure analysis showed that the mortar constituents of polymer-modified cement mortars are compactly joined, have ultimate improved properties. The hexagonal sheet crystal structure of Ca(OH)2was seen.
引文
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