丙烯酸酯可再分散乳胶粉的制备及再分散稳定机理与应用研究
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摘要
现有的建筑乳胶涂料含有消泡剂、流平剂、防腐剂、增稠剂等十多种助剂,是建筑涂料带来环境污染物VOC(有机挥发性化合物)的主要来源。随着环保要求的日趋严苛,涂料正向水性化、高固体份和粉末涂料方向发展。可再分散乳胶粉是一种可以在水中重新分散成稳定的分散液,并保持原聚合物乳液性能的聚合物粉末,它的出现为建筑涂料的干粉化提供了物质基础。开展可再分散乳胶粉的制备与性能研究,并与其他粉体材料结合使用开发干粉涂料,在理论和应用上都具有重要的意义。
本研究根据喷雾干燥制备乳胶粉及乳胶粉应用要求,首先设计并制备具有“软核硬壳”粒子结构的丙烯酸酯乳液,再采用喷雾干燥法制得丙烯酸酯可再分散乳胶粉,建立喷雾干燥模型,探讨乳胶粉的再分散性影响因素及乳胶粉再分散液稳定机理。以此乳胶粉为主要成膜物质,开发干粉建筑涂料。应用核壳乳液聚合技术制备了具有核壳结构的磁性Fe_3O_4/PMAA(聚甲基丙烯酸)聚合物复合微球。具体研究工作如下:
为制备可再分散乳胶粉,合成具有“软核硬壳”粒子结构的丙烯酸酯乳液。通过探讨乳胶粒子核壳层聚合物玻璃化温度(T_g)和核壳层单体质量比对乳胶粉外观和分散性的影响,确定了乳胶粒子的核壳结构参数。通过考察乳液聚合过程中聚合工艺、乳化剂、引发剂、种子单体、功能单体等用量对乳液凝胶率、固含量、粘度、粒径及其分布的影响,确定了最优合成工艺及配方。采用傅立叶红外光谱(FTIR)、透射电镜(TEM)、差示扫描量热仪(DSC)和扫描电镜(SEM)等分析表明,制备的丙烯酸酯乳液,乳胶粒具有清晰的核壳结构,核壳层聚合物T_g分别为-25℃和45℃,乳液具有良好的成膜性能。
采用喷雾干燥法制备可再分散乳胶粉。通过探讨乳液粘度、固含量、干燥助剂硅溶胶及保护胶体聚乙烯醇(PVA)用量对乳胶粉再分散性、含水率、滤渣率等因素的影响,确定了干燥预处理工艺参数。考察喷雾干燥温度、雾化盘转速对乳胶粉含水率、滤渣率、再分散性及再分散液成膜性的影响,得到最优喷雾干燥工艺参数。通过FTIR、SEM、TEM、DSC、UVSP(紫外分光光度计)等分析显示,与原乳液相比,乳胶粉主要分子结构未发生明显改变,再分散液粒子呈球形且大小分布均匀,粒径略有增加。再分散液胶膜有两个T_g(?25℃和50℃),再分散液稳定性好。所有分析表明,制得的乳胶粉再分散后能较好的回复原乳液形态。通过引入动态质量控制方程和动态能量控制方程,建立乳胶粉喷雾干燥动态模型。将两方程关联起来,通过计算机Matlab程序计算,可模拟干燥过程中雾化液滴温度和水分随时间的动态变化过程。
探讨了乳胶粉再分散液的稳定机理。为使乳胶粉及再分散液获得好的再分散性和稳定性,功能单体甲基丙烯酸(MAA)添加量占合成单体总质量的4%~5%,调节乳液pH至9.0以上,乳胶粒表面羧基转化为羧酸离子,亲水性基团在喷雾干燥时得到保护,避免乳胶粒子表面羧基之间发生缩聚反应,再分散液粒子表面具有多的羧基离子和高的Zeta电位,粒子间有强的静电斥力。同时粒子之间存在由静电作用产生的水合作用力。PVA用作保护胶体,乳胶粉再分散后,PVA包覆在乳胶粒子表面。其羟基伸向水中,庞大的聚乙烯长链基团则呈卷曲态吸附在乳胶粒子表面,为乳胶粒子提供了大的空间位阻,避免乳胶粒子之间发生碰撞,提高了再分散液的稳定性。这种空间位阻与粒子间的静电斥力、水合作用力一起,维持着再分散液乳胶粒子的稳定。
以乳胶粉为主要成膜物质,重质碳酸钙、高岭土、滑石粉、纤维素醚等原料开发干粉涂料。乳胶粉用量对干粉涂料成膜性、耐水性和耐洗刷性有重要影响。纤维素醚可改善涂料施工性并调整干燥时间。较好的配方是:乳胶粉用量为30%,纤维素醚用量为0.6%,干粉涂料具有较好的施工性、耐水性和耐洗刷性能。
应用制备具有核壳粒子结构聚合物技术,以油酸修饰的Fe_3O_4为核,采用细乳液聚合法,在超声作用下,制备Fe_3O_4/PMAA复合微球。通过考察超声功率对细乳液液滴粒径及其分散粒度的影响,确定了反应超声功率,同时考察乳化剂量对复合微球粒径的影响。乳化剂浓度低于或接近临界胶束浓度(CMC)时,单体液滴易发生团聚,磁性复合微球粒径分布变宽;乳化剂浓度远大于CMC浓度时,乳化剂会形成大量胶束,MAA会在乳化剂形成的胶束内成核,导致Fe_3O_4裸露形成空白粒子。合适的乳化剂浓度是大于CMC,聚合后复合物微球分散性好,粒径在100 nm左右。
Modern architectural coatings consist of many additives, including the defoaming agent, viscosity-increasing agent, etc. These additives are the source of volatile organic compounds (VOCs) produced from coatings. As environmental policy becomes stricter, these coatings are developing toward waterborne, high solid content and powder based coatings. Redispersible latex powder, a type of polymer powder, provides large improvements in the prepation of dry powdered coatings. When redispersible latex powder is dispersed in water, it is stable and has the same properties as the original latex. Research on preparing redispersible latex powder and developing dry powdered coatings combined with other powder materials shows great significance both in theory and practice.
Based on the requirements of redispersible latex powder on spray drying and coating on application, firstly acrylate latex was synthesized with the configuration of a―soft core and hard shell‖, nextly the redispersible latex powder was prepared using the spray drying method. A spray drying model was established, and influencing factors on the powder’s redispersibility and stabilization mechanism of reconstituted latex were investigated. Dry powdered coating was developed in which the latex powder serves as the major constituent of the film forming material. Using emulsion polymerization technology on the core shell configuration, the magnetic composite microsphere (Fe3O4/PMAA) was prepared. The following describes the main focus of this work.
Acrylate latex with the“soft core and hard shell”configuration was synthesized to prepare redispersible latex powder. Through investigation of the effect of the glass transition temperature (T_g) of the core and shell layer on the appearance and redispersibility of powder, the configuration parameters of the latex particles were determined. Furthermore, by investigation on the effect of the polymerization process, emulsifier, initiator, seed monomer and functional monomer on coagulation rate, solid content, viscosity, particle size and distribution, the optimized polymerization process was established. By Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM), it was determined that the latex particles have a clear core-shell configuration and two T_g s (-25℃and 45℃). In addition, the acrylate has good film forming properties.
The redispersible latex powder was prepared by spray drying. Through investigation on the effects of latex viscosity, solid content, silicon sol and protective colloid (PVA) amount on redispersibility, water content, and residual content of the powder, the pretreatment parameters were determined. Moreover, by investigating the effect of drying temperature and atomizer speed on water content, residual content, redispersibility and film forming ability, the optimized spray drying parameters were established. By FTIR, SEM, TEM, DSC and UV-visible spectrometer, and comparison with the original latex, it was determined that the molecular configuration of redispersible powders does not change, while the particles have a spherical shape of uniform size slightly larger than original particle. The reconstituted latex is stable and the film has T_gs (-25℃and 50℃). All of the analyses show that after the powder is dispersed in water, it can return to its orginal conditions. The dynamic governing equations of mass and energy were utilized to establish a spray drying model for redispersible latex powder. By coupling the two equations and running a code developed in Matlab, the dynamic change of temperature and water content in the water droplet can be obtained.
The stabilization mechanism of the reconstituted latex was also investigated. 4%~5% (of total monomers) MAA was added during polymerization, and the acrylate latex was neutralized to a pH above 9.0. The carboxyl group distributed on the surface of the particles was transformed into carboxylic ions in order to protect these groups during spray drying. In this way, the powder has good redispersiblity and the reconstituted latex has good stability. The particle also has a high zeta potential as much of the carboxylic ions were distributed on the particle surface. The particles also demonstrated a strong electrostatic repulsion force as well as hydration force caused by the interparticle electrostatic effect. PVA served as a protective colloid for the particles. After the powder was dispersed in the water, the particles were surrounded by PVA whose hydroxyl group bonded with the water and long chain poly-ethylene groups were absorbed on the surface of particles. These poly-ethylene groups provide enormous steric force and help to prevent particles aggregation. The electrostatic force, hydration force and steric force together stabilized the particles in the reconstituted latex.
Based on redispersible latex powder, a dry powdered coating was developed using other inorganic materials and cellulose ether. The redispersible powder has a large influence on film forming ability, water resistance and abrasive resistance of the coating. Cellulose improves the working ability of the coating. Taking the formula amount of dry-powdered coating as follows, redispersible latex powder is 30% (mass percentage of total powder), cellulose ether is 0.6% (mass percentage of total powder), the dry-powdered coating possesses good film forming ability, good water and abrasive resistance, and good workability.
Considering polymer technology with core shell configuration, based on Fe_3O_4 modified by oleic acid, the Fe_3O_4/PMAA composite microsphere was prepared by miniemulsion under sonication. The sonication power was determined by investigations on the effect of sonication power on droplet size and poly dispersing index (PDI). The effect of emulsifier amount on microsphere size was also investigated. When the emulsifier concentration was below or close to its critical micelle concentration (CMC), the monomer droplets easily aggregate with each other and the composite microsphere has a wide size distribution. When the emulsifier concentration was much higher than CMC, a large amount of micelle was formed. MAA will form cores inside the micelle and cause the magnetite particles to be exposed. The suitable emulsifier concentration is slightly higher than its CMC resulting in a composite microsphere with good dispersibiliy and a size of about 100 nm.
本研究根据喷雾干燥制备乳胶粉及乳胶粉应用要求,首先设计并制备具有“软核硬壳”粒子结构的丙烯酸酯乳液,再采用喷雾干燥法制得丙烯酸酯可再分散乳胶粉,建立喷雾干燥模型,探讨乳胶粉的再分散性影响因素及乳胶粉再分散液稳定机理。以此乳胶粉为主要成膜物质,开发干粉建筑涂料。应用核壳乳液聚合技术制备了具有核壳结构的磁性Fe_3O_4/PMAA(聚甲基丙烯酸)聚合物复合微球。具体研究工作如下:
为制备可再分散乳胶粉,合成具有“软核硬壳”粒子结构的丙烯酸酯乳液。通过探讨乳胶粒子核壳层聚合物玻璃化温度(T_g)和核壳层单体质量比对乳胶粉外观和分散性的影响,确定了乳胶粒子的核壳结构参数。通过考察乳液聚合过程中聚合工艺、乳化剂、引发剂、种子单体、功能单体等用量对乳液凝胶率、固含量、粘度、粒径及其分布的影响,确定了最优合成工艺及配方。采用傅立叶红外光谱(FTIR)、透射电镜(TEM)、差示扫描量热仪(DSC)和扫描电镜(SEM)等分析表明,制备的丙烯酸酯乳液,乳胶粒具有清晰的核壳结构,核壳层聚合物T_g分别为-25℃和45℃,乳液具有良好的成膜性能。
采用喷雾干燥法制备可再分散乳胶粉。通过探讨乳液粘度、固含量、干燥助剂硅溶胶及保护胶体聚乙烯醇(PVA)用量对乳胶粉再分散性、含水率、滤渣率等因素的影响,确定了干燥预处理工艺参数。考察喷雾干燥温度、雾化盘转速对乳胶粉含水率、滤渣率、再分散性及再分散液成膜性的影响,得到最优喷雾干燥工艺参数。通过FTIR、SEM、TEM、DSC、UVSP(紫外分光光度计)等分析显示,与原乳液相比,乳胶粉主要分子结构未发生明显改变,再分散液粒子呈球形且大小分布均匀,粒径略有增加。再分散液胶膜有两个T_g(?25℃和50℃),再分散液稳定性好。所有分析表明,制得的乳胶粉再分散后能较好的回复原乳液形态。通过引入动态质量控制方程和动态能量控制方程,建立乳胶粉喷雾干燥动态模型。将两方程关联起来,通过计算机Matlab程序计算,可模拟干燥过程中雾化液滴温度和水分随时间的动态变化过程。
探讨了乳胶粉再分散液的稳定机理。为使乳胶粉及再分散液获得好的再分散性和稳定性,功能单体甲基丙烯酸(MAA)添加量占合成单体总质量的4%~5%,调节乳液pH至9.0以上,乳胶粒表面羧基转化为羧酸离子,亲水性基团在喷雾干燥时得到保护,避免乳胶粒子表面羧基之间发生缩聚反应,再分散液粒子表面具有多的羧基离子和高的Zeta电位,粒子间有强的静电斥力。同时粒子之间存在由静电作用产生的水合作用力。PVA用作保护胶体,乳胶粉再分散后,PVA包覆在乳胶粒子表面。其羟基伸向水中,庞大的聚乙烯长链基团则呈卷曲态吸附在乳胶粒子表面,为乳胶粒子提供了大的空间位阻,避免乳胶粒子之间发生碰撞,提高了再分散液的稳定性。这种空间位阻与粒子间的静电斥力、水合作用力一起,维持着再分散液乳胶粒子的稳定。
以乳胶粉为主要成膜物质,重质碳酸钙、高岭土、滑石粉、纤维素醚等原料开发干粉涂料。乳胶粉用量对干粉涂料成膜性、耐水性和耐洗刷性有重要影响。纤维素醚可改善涂料施工性并调整干燥时间。较好的配方是:乳胶粉用量为30%,纤维素醚用量为0.6%,干粉涂料具有较好的施工性、耐水性和耐洗刷性能。
应用制备具有核壳粒子结构聚合物技术,以油酸修饰的Fe_3O_4为核,采用细乳液聚合法,在超声作用下,制备Fe_3O_4/PMAA复合微球。通过考察超声功率对细乳液液滴粒径及其分散粒度的影响,确定了反应超声功率,同时考察乳化剂量对复合微球粒径的影响。乳化剂浓度低于或接近临界胶束浓度(CMC)时,单体液滴易发生团聚,磁性复合微球粒径分布变宽;乳化剂浓度远大于CMC浓度时,乳化剂会形成大量胶束,MAA会在乳化剂形成的胶束内成核,导致Fe_3O_4裸露形成空白粒子。合适的乳化剂浓度是大于CMC,聚合后复合物微球分散性好,粒径在100 nm左右。
Modern architectural coatings consist of many additives, including the defoaming agent, viscosity-increasing agent, etc. These additives are the source of volatile organic compounds (VOCs) produced from coatings. As environmental policy becomes stricter, these coatings are developing toward waterborne, high solid content and powder based coatings. Redispersible latex powder, a type of polymer powder, provides large improvements in the prepation of dry powdered coatings. When redispersible latex powder is dispersed in water, it is stable and has the same properties as the original latex. Research on preparing redispersible latex powder and developing dry powdered coatings combined with other powder materials shows great significance both in theory and practice.
Based on the requirements of redispersible latex powder on spray drying and coating on application, firstly acrylate latex was synthesized with the configuration of a―soft core and hard shell‖, nextly the redispersible latex powder was prepared using the spray drying method. A spray drying model was established, and influencing factors on the powder’s redispersibility and stabilization mechanism of reconstituted latex were investigated. Dry powdered coating was developed in which the latex powder serves as the major constituent of the film forming material. Using emulsion polymerization technology on the core shell configuration, the magnetic composite microsphere (Fe3O4/PMAA) was prepared. The following describes the main focus of this work.
Acrylate latex with the“soft core and hard shell”configuration was synthesized to prepare redispersible latex powder. Through investigation of the effect of the glass transition temperature (T_g) of the core and shell layer on the appearance and redispersibility of powder, the configuration parameters of the latex particles were determined. Furthermore, by investigation on the effect of the polymerization process, emulsifier, initiator, seed monomer and functional monomer on coagulation rate, solid content, viscosity, particle size and distribution, the optimized polymerization process was established. By Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM), it was determined that the latex particles have a clear core-shell configuration and two T_g s (-25℃and 45℃). In addition, the acrylate has good film forming properties.
The redispersible latex powder was prepared by spray drying. Through investigation on the effects of latex viscosity, solid content, silicon sol and protective colloid (PVA) amount on redispersibility, water content, and residual content of the powder, the pretreatment parameters were determined. Moreover, by investigating the effect of drying temperature and atomizer speed on water content, residual content, redispersibility and film forming ability, the optimized spray drying parameters were established. By FTIR, SEM, TEM, DSC and UV-visible spectrometer, and comparison with the original latex, it was determined that the molecular configuration of redispersible powders does not change, while the particles have a spherical shape of uniform size slightly larger than original particle. The reconstituted latex is stable and the film has T_gs (-25℃and 50℃). All of the analyses show that after the powder is dispersed in water, it can return to its orginal conditions. The dynamic governing equations of mass and energy were utilized to establish a spray drying model for redispersible latex powder. By coupling the two equations and running a code developed in Matlab, the dynamic change of temperature and water content in the water droplet can be obtained.
The stabilization mechanism of the reconstituted latex was also investigated. 4%~5% (of total monomers) MAA was added during polymerization, and the acrylate latex was neutralized to a pH above 9.0. The carboxyl group distributed on the surface of the particles was transformed into carboxylic ions in order to protect these groups during spray drying. In this way, the powder has good redispersiblity and the reconstituted latex has good stability. The particle also has a high zeta potential as much of the carboxylic ions were distributed on the particle surface. The particles also demonstrated a strong electrostatic repulsion force as well as hydration force caused by the interparticle electrostatic effect. PVA served as a protective colloid for the particles. After the powder was dispersed in the water, the particles were surrounded by PVA whose hydroxyl group bonded with the water and long chain poly-ethylene groups were absorbed on the surface of particles. These poly-ethylene groups provide enormous steric force and help to prevent particles aggregation. The electrostatic force, hydration force and steric force together stabilized the particles in the reconstituted latex.
Based on redispersible latex powder, a dry powdered coating was developed using other inorganic materials and cellulose ether. The redispersible powder has a large influence on film forming ability, water resistance and abrasive resistance of the coating. Cellulose improves the working ability of the coating. Taking the formula amount of dry-powdered coating as follows, redispersible latex powder is 30% (mass percentage of total powder), cellulose ether is 0.6% (mass percentage of total powder), the dry-powdered coating possesses good film forming ability, good water and abrasive resistance, and good workability.
Considering polymer technology with core shell configuration, based on Fe_3O_4 modified by oleic acid, the Fe_3O_4/PMAA composite microsphere was prepared by miniemulsion under sonication. The sonication power was determined by investigations on the effect of sonication power on droplet size and poly dispersing index (PDI). The effect of emulsifier amount on microsphere size was also investigated. When the emulsifier concentration was below or close to its critical micelle concentration (CMC), the monomer droplets easily aggregate with each other and the composite microsphere has a wide size distribution. When the emulsifier concentration was much higher than CMC, a large amount of micelle was formed. MAA will form cores inside the micelle and cause the magnetite particles to be exposed. The suitable emulsifier concentration is slightly higher than its CMC resulting in a composite microsphere with good dispersibiliy and a size of about 100 nm.
引文
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