聚合物/二氧化硅纳米复合乳液及结构研究
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摘要
树脂水性化是人类可持续发展的必然需求。基于乳液聚合的聚合物胶乳和基于后乳化的水性化聚合物是常见的两种水性化树脂,但均存在使用性能不如溶剂型树脂的缺点。在聚合物胶乳方面,通过与纳米二氧化硅结合,可提高相应乳胶膜的性能。文献中对聚合物/二氧化硅纳米复合乳液的制备方法、乳胶粒子形态、纳米复合乳胶涂膜性能等方面进行了大量研究,但报道中涉及的成膜温度均以低温或室温为主,应用则偏重于力学性能增强型涂层、高耐候性涂层及有机无机复合微球等,而有关纳米复合乳液在高温下成膜的涂膜结构与性能的研究则未见报道。本文分别以原位聚合法、共混法聚(苯乙烯-丙烯酸丁酯-丙烯酸)/二氧化硅纳米复合乳液的制备为基础,通过乳液膜的直接高温干燥,分别制得了表面二维有序孔阵列结构薄膜和反蛋白石光子晶体薄膜,大大提升了传统纳米复合乳液涂膜的使用功能。在水性化聚合物方面,基于纳米二氧化硅粒子的聚合物后乳化工艺研究则未见报道,尽管其在聚合物粒子制备以及小分子油性液滴的稳定化方面的“pickering”稳定功能已得到很好证实。本文采用纳米二氧化硅粒子,成功实现了硅烷化聚合物的后乳化,大大减少了小分子乳化剂的应用,并以此为基础,成功制备了一种高性能的水性胶粘剂。另外,本文对聚有机硅倍半氧烷防腐涂层也进行了研究,通过特种酸催化剂植酸的原位接枝,大大改善了原有杂化涂层的防腐性能。
具体研究内容及结果如下:
(1)在酸性二氧化硅溶胶存在下,以烯丙氧基羟丙基磺酸钠(HAPS)为可聚合表面活性剂,采用原位乳液聚合方法合成了苯乙烯-丙烯酸丁酯-丙烯酸三元共聚物/二氧化硅纳米复合乳液(即原位聚合法)。当上述纳米复合乳液在大于100℃的温度下烘干成膜时,得到的涂膜表面具有二维有序的孔阵列结构。这种孔结构的形成是由于在高温下,水份快速挥发,聚合物乳胶粒子与纳米二氧化硅粒子共沉积时在涂膜中产生了较多的孔隙,同时,包覆在聚合物粒子周边的纳米二氧化硅粒子通过硅羟基缩合形成了固定的二氧化硅骨架,由于聚合物分子在高温下的流动及链段的扩散对空隙的填充导致表面聚合物粒子塌陷,从而产生表面孔结构。孔的直径、深度、孔间距可由纳米SiO_2粒子的用量、聚合物乳胶粒子尺寸、涂膜厚度、干燥温度调节。
(2)先用乳液聚合法合成了苯乙烯-丙烯酸丁酯-丙烯酸三元共聚物乳液,然后再与胶体纳米二氧化硅粒子混合制备了纳米复合乳液(即共混法)。通过高温下干燥,直接得到了具有较高力学强度的反蛋白石光子晶体。采用FTIR、ATR-FTIR、XPS、TEM、SEM、反射光谱仪等分析手段研究了聚合物乳液的粒径、纳米二氧化硅种类及粒径大小对多孔结构材料的结构及形貌、光子晶体的形成条件及禁带特征峰的影响。通过调节聚合物乳胶粒子的大小,可以得到不同颜色的光子晶体材料,实验结果与理论计算方法非常吻合。上述方法为光子晶体的制备提供了新的思路,有利于光子晶体的大规模制备及剪切加工。
(3)利用纳米二氧化硅粒子,在少量或不加乳化剂的条件下,以后乳化的方法实现了硅烷化聚合物的水性化,证实了纳米二氧化硅对低聚物液滴的“Pickering”乳化剂功能。采用FTIR、粒径分析仪、SEM、流变分析仪考察了纳米二氧化硅对水性硅烷化聚合物结构、稳定性和流变行为的影响。纳米二氧化硅粒径越小,含量越高,剪切变稀行为越明显,储存模量越高,损耗因子越低,粒子间的相互作用越强,有更高的弹性。上述流变行为是由于体系中形成了纳米二氧化硅与硅烷化聚合物粒子网络造成的。
(4)以基于胶体二氧化硅纳米粒子稳定功能的水性硅烷化聚合物为基础,再与纳米二氧化硅粉体、正硅酸乙酯、氨基硅烷相结合,制得了室温可固化、高粘结强度的水性胶粘剂。通过FTIR、TGA、SEM及电子拉力机考察了正硅酸乙酯用量、纳米二氧化硅溶胶用量、纳米二氧化硅粉体的种类及用量对胶粘剂性能的影响。研究发现,纳米二氧化硅溶胶粒子的增强作用不如纳米二氧化硅粉体,但溶胶的加入可以大大提高疏水性纳米二氧化硅粉体在胶粘剂中的分散,从而提高胶粘剂的强度。另外,纳米二氧化硅粉体表面适中的疏水特性有利于获得高剪切强度的胶粘剂。
(5)利用硅烷化植酸的反应活性和酸催化活性,与硅烷单体共水解缩聚,在聚有机硅倍半氧烷分子链上接枝植酸,合成了分子量大于50000的大分子植酸-聚有机硅倍半氧烷。采用GPC、~(13)C NMR、~(29)SiNMR核磁共振谱、XPS、Raman、SEM、电化学测试等分析手段,对比了不同酸催化聚有机硅倍半氧烷的结构和性能,发现植酸-聚有机硅倍半氧烷上的螯合基团与金属表面的活性基团反应而键合,在金属表面形成致密的保护膜,因而具有最优异的防腐性能。
The application of waterborne resins are the inevitable development in the coating industry and adhesive industry. There are many prepared technique such as emulsion polymerization method and post-emulsification technique used to obtain the waterborne resins, however, the properties of the waterborne resins are lower than that of the solvent-based resins.
Recently, a number of waterborne polymer/silica nanocomposite emulsions had been synthesized using various techniques such as in situ emulsion polymerization and blending method, since inorganic nanosilica particles could improve some performances and even endow polymers with novel properties. However, the previous studies mainly focused on the morphology and properties of the coating under ambient temperature, very few studies have been concerned the film formation of these nanocomposite emulsion under more than 100℃.
In ths dissertation, the polymer/silica nanocomposite emulsions were prepared by in situ surfactant-free emulsion polymerization, blending method and post-emulsification technique using nanosilica as a "Pickering" emulsifier. When the nanocomposite emulsions were dried to form a film at a certain temperature, the 2D surface porous structure, "inverse opal" structure and adhesives were fabricated by adjusting prepared technique, monomer composites, nanosilica content, temperature of forming film and etc.. A macromolecules Phytic acid-polysilsesquioxanes was prepared by silylated phytic acid reacting with MTES and TEOS, which had significantly excellent corrosion resistance.
All the research content and results are as follows:
(1) This paper presents a novel and facile method for the fabrication of nanocomposite films with ordered porous surface structures. In this approach, a water-borne poly(styrene-co-butyl acrylate-co-acrylic acid) /silica nanocomposite emulsion was synthesized in situ emulsion polymerization using 3-allyloxy-2-hydroxy-1-propanesulfonate as a polymerizable surfactant. When this emulsion was dried to form a film at a certain temperature, an ordered porous structure could be directly obtained on the surface of the nanocomposite film. This was probably duing at a fast evaporation rate of water, silica particles transform into hard silica framework via the condensation of silianol groups, meanwhile, soft polymer particles can easily collapseand immigrate into the voids existing in silica framework to form ordered porous structure on the surface of the nanocomposite film. SEM, TEM and AFM were employed to observe the morphology, XPS and particle analyzer were used to analyze the surface composition of the ordered porous nanocomposite film, and the particle size, respectively.
(2) An one-step strategy to fabricate large-scale inverse opal photonic crystals has been proposed, in which a nanocomposite emulsion composed of polymer latex and colloidal silica is blended first, and then forced-drying on a substrate under relatively high temperatures to directly obtain a film with three-dimensionally array of ordered pores. This strategy is really simple and inexpensive: Neither complex processes nor special equipments are needed, as large as several square meters inverse opal photonic crystal can be fabricated on any substrates without any templates. And the backbone of the inverse opal is composed of organic and inorganic phases, thus the optical, electric, magnetic and mechanical properties of the inverse opals can be modulated. This technique presents a new paradigm in the preparations of inverse opal photonic crystals.
The particle size of polymer particles, surface components, morphology and optical properties of photonic crystal films were investigated by FTIR, ATR-FTIR, XPS, TEM, SEM and Reflection spectra. The PCs films have very beautiful iridescence phenomena and regular periodicity. The reflectance spectra of PCs stimulated by layered-KKR method has a very good agreement with the experimental results.
(3)Stable waterborne silylated polymer latex was obtained via post-emulsification process by utilizing reaction between hydroxyl groups on the surface of nanosilica and alkoxysilyl groups on the molecular chain of the silylated polymer, only a small quantity of surfactant was needed. A large quantity of nanosilica was adsorbed on the surface of the silylated polymer latex particles. The nanosilica not only can serve as a Pickering emulsifying agent to stabilize the polymer latex particles, but also can inhibit the self-crosslinking of the silylated polymer in water and improve the mechnics properties, aging resistance properties.
The structure, stability and rheological behavior of the silylated latex was investigated by FTIR, particle size analysis, SEM, respectively. The smaller the colloidal silica size was or the more the silica content was, the greater the storage modulus was at low strain amplitude, indicating a stronger interparticle interaction and a solidlike viscoelastic behavior of the emulsion. This rheological behavior can be explained by the formation of the reversible particulate network in the emulsion.
(4) Waterborne nanocomposite adhesives were obtained via silylated polymer/silica nanocomposite emulsion cured with nanosilica stemming from tetraethyl orthosilicate (TEOS), silica sol and/or fumed silica powder. Effects of TEOS content, silica sol content and the type and content of fumed silica on the shear strength of the adhesive were investigated using a scanning electronic microscope and an electronic instron tester and the strengthening mechanisms of different silica source were discussed. Colloidal silica particles was less efficient than fumed silica particles for reinforcing the nanocomposite adhesive but can increase the shear strength of hydrophobic fumed silica embedded adhesive. Comparing the adhesives with the hydrophilic fumed silica (HS-5) or the extremely hydrophobic fumed silica (TS-720), the adhesive with moderate hydrophobic fumed silica (TS-610) had the highest shear strength. It seemed that TEOS, silica sol and fumed silica played crosslinking, dispersing (for fumed silica) and reinforcing roles on waterborne adhesive, respectively.
(5) The high-molecular-weight phytic acid-polysilsesquioxane was successfully synthesized via sol-gel process using silylated phytic acid reacting with MTES and TEOS without any low molecular acid, the molecular weight of phytic acid-polysilsesquioxanes was more than 50000. Phytic acid served as not only catalysts but also reactant and chelating agent, which was in-situ incorporated with polysilsesquioxane chain uniformly. GPC, ~(13)CNMR, ~(29)SiNMR, XPS, Raman, SEM, electro-chemical techniques were used to investigate the correlation between the microstructure and property of PAP, TAP and HCP. PAP could form a compacting protective film because of strong chemical interaction between metal substrate and phytic acid-polysilsesquioxane, which had significantly better corrosion resistance compared to tannin-catalyzed polysilsesquioxane and HCl-catalyzed polysilsesquioxane.
具体研究内容及结果如下:
(1)在酸性二氧化硅溶胶存在下,以烯丙氧基羟丙基磺酸钠(HAPS)为可聚合表面活性剂,采用原位乳液聚合方法合成了苯乙烯-丙烯酸丁酯-丙烯酸三元共聚物/二氧化硅纳米复合乳液(即原位聚合法)。当上述纳米复合乳液在大于100℃的温度下烘干成膜时,得到的涂膜表面具有二维有序的孔阵列结构。这种孔结构的形成是由于在高温下,水份快速挥发,聚合物乳胶粒子与纳米二氧化硅粒子共沉积时在涂膜中产生了较多的孔隙,同时,包覆在聚合物粒子周边的纳米二氧化硅粒子通过硅羟基缩合形成了固定的二氧化硅骨架,由于聚合物分子在高温下的流动及链段的扩散对空隙的填充导致表面聚合物粒子塌陷,从而产生表面孔结构。孔的直径、深度、孔间距可由纳米SiO_2粒子的用量、聚合物乳胶粒子尺寸、涂膜厚度、干燥温度调节。
(2)先用乳液聚合法合成了苯乙烯-丙烯酸丁酯-丙烯酸三元共聚物乳液,然后再与胶体纳米二氧化硅粒子混合制备了纳米复合乳液(即共混法)。通过高温下干燥,直接得到了具有较高力学强度的反蛋白石光子晶体。采用FTIR、ATR-FTIR、XPS、TEM、SEM、反射光谱仪等分析手段研究了聚合物乳液的粒径、纳米二氧化硅种类及粒径大小对多孔结构材料的结构及形貌、光子晶体的形成条件及禁带特征峰的影响。通过调节聚合物乳胶粒子的大小,可以得到不同颜色的光子晶体材料,实验结果与理论计算方法非常吻合。上述方法为光子晶体的制备提供了新的思路,有利于光子晶体的大规模制备及剪切加工。
(3)利用纳米二氧化硅粒子,在少量或不加乳化剂的条件下,以后乳化的方法实现了硅烷化聚合物的水性化,证实了纳米二氧化硅对低聚物液滴的“Pickering”乳化剂功能。采用FTIR、粒径分析仪、SEM、流变分析仪考察了纳米二氧化硅对水性硅烷化聚合物结构、稳定性和流变行为的影响。纳米二氧化硅粒径越小,含量越高,剪切变稀行为越明显,储存模量越高,损耗因子越低,粒子间的相互作用越强,有更高的弹性。上述流变行为是由于体系中形成了纳米二氧化硅与硅烷化聚合物粒子网络造成的。
(4)以基于胶体二氧化硅纳米粒子稳定功能的水性硅烷化聚合物为基础,再与纳米二氧化硅粉体、正硅酸乙酯、氨基硅烷相结合,制得了室温可固化、高粘结强度的水性胶粘剂。通过FTIR、TGA、SEM及电子拉力机考察了正硅酸乙酯用量、纳米二氧化硅溶胶用量、纳米二氧化硅粉体的种类及用量对胶粘剂性能的影响。研究发现,纳米二氧化硅溶胶粒子的增强作用不如纳米二氧化硅粉体,但溶胶的加入可以大大提高疏水性纳米二氧化硅粉体在胶粘剂中的分散,从而提高胶粘剂的强度。另外,纳米二氧化硅粉体表面适中的疏水特性有利于获得高剪切强度的胶粘剂。
(5)利用硅烷化植酸的反应活性和酸催化活性,与硅烷单体共水解缩聚,在聚有机硅倍半氧烷分子链上接枝植酸,合成了分子量大于50000的大分子植酸-聚有机硅倍半氧烷。采用GPC、~(13)C NMR、~(29)SiNMR核磁共振谱、XPS、Raman、SEM、电化学测试等分析手段,对比了不同酸催化聚有机硅倍半氧烷的结构和性能,发现植酸-聚有机硅倍半氧烷上的螯合基团与金属表面的活性基团反应而键合,在金属表面形成致密的保护膜,因而具有最优异的防腐性能。
The application of waterborne resins are the inevitable development in the coating industry and adhesive industry. There are many prepared technique such as emulsion polymerization method and post-emulsification technique used to obtain the waterborne resins, however, the properties of the waterborne resins are lower than that of the solvent-based resins.
Recently, a number of waterborne polymer/silica nanocomposite emulsions had been synthesized using various techniques such as in situ emulsion polymerization and blending method, since inorganic nanosilica particles could improve some performances and even endow polymers with novel properties. However, the previous studies mainly focused on the morphology and properties of the coating under ambient temperature, very few studies have been concerned the film formation of these nanocomposite emulsion under more than 100℃.
In ths dissertation, the polymer/silica nanocomposite emulsions were prepared by in situ surfactant-free emulsion polymerization, blending method and post-emulsification technique using nanosilica as a "Pickering" emulsifier. When the nanocomposite emulsions were dried to form a film at a certain temperature, the 2D surface porous structure, "inverse opal" structure and adhesives were fabricated by adjusting prepared technique, monomer composites, nanosilica content, temperature of forming film and etc.. A macromolecules Phytic acid-polysilsesquioxanes was prepared by silylated phytic acid reacting with MTES and TEOS, which had significantly excellent corrosion resistance.
All the research content and results are as follows:
(1) This paper presents a novel and facile method for the fabrication of nanocomposite films with ordered porous surface structures. In this approach, a water-borne poly(styrene-co-butyl acrylate-co-acrylic acid) /silica nanocomposite emulsion was synthesized in situ emulsion polymerization using 3-allyloxy-2-hydroxy-1-propanesulfonate as a polymerizable surfactant. When this emulsion was dried to form a film at a certain temperature, an ordered porous structure could be directly obtained on the surface of the nanocomposite film. This was probably duing at a fast evaporation rate of water, silica particles transform into hard silica framework via the condensation of silianol groups, meanwhile, soft polymer particles can easily collapseand immigrate into the voids existing in silica framework to form ordered porous structure on the surface of the nanocomposite film. SEM, TEM and AFM were employed to observe the morphology, XPS and particle analyzer were used to analyze the surface composition of the ordered porous nanocomposite film, and the particle size, respectively.
(2) An one-step strategy to fabricate large-scale inverse opal photonic crystals has been proposed, in which a nanocomposite emulsion composed of polymer latex and colloidal silica is blended first, and then forced-drying on a substrate under relatively high temperatures to directly obtain a film with three-dimensionally array of ordered pores. This strategy is really simple and inexpensive: Neither complex processes nor special equipments are needed, as large as several square meters inverse opal photonic crystal can be fabricated on any substrates without any templates. And the backbone of the inverse opal is composed of organic and inorganic phases, thus the optical, electric, magnetic and mechanical properties of the inverse opals can be modulated. This technique presents a new paradigm in the preparations of inverse opal photonic crystals.
The particle size of polymer particles, surface components, morphology and optical properties of photonic crystal films were investigated by FTIR, ATR-FTIR, XPS, TEM, SEM and Reflection spectra. The PCs films have very beautiful iridescence phenomena and regular periodicity. The reflectance spectra of PCs stimulated by layered-KKR method has a very good agreement with the experimental results.
(3)Stable waterborne silylated polymer latex was obtained via post-emulsification process by utilizing reaction between hydroxyl groups on the surface of nanosilica and alkoxysilyl groups on the molecular chain of the silylated polymer, only a small quantity of surfactant was needed. A large quantity of nanosilica was adsorbed on the surface of the silylated polymer latex particles. The nanosilica not only can serve as a Pickering emulsifying agent to stabilize the polymer latex particles, but also can inhibit the self-crosslinking of the silylated polymer in water and improve the mechnics properties, aging resistance properties.
The structure, stability and rheological behavior of the silylated latex was investigated by FTIR, particle size analysis, SEM, respectively. The smaller the colloidal silica size was or the more the silica content was, the greater the storage modulus was at low strain amplitude, indicating a stronger interparticle interaction and a solidlike viscoelastic behavior of the emulsion. This rheological behavior can be explained by the formation of the reversible particulate network in the emulsion.
(4) Waterborne nanocomposite adhesives were obtained via silylated polymer/silica nanocomposite emulsion cured with nanosilica stemming from tetraethyl orthosilicate (TEOS), silica sol and/or fumed silica powder. Effects of TEOS content, silica sol content and the type and content of fumed silica on the shear strength of the adhesive were investigated using a scanning electronic microscope and an electronic instron tester and the strengthening mechanisms of different silica source were discussed. Colloidal silica particles was less efficient than fumed silica particles for reinforcing the nanocomposite adhesive but can increase the shear strength of hydrophobic fumed silica embedded adhesive. Comparing the adhesives with the hydrophilic fumed silica (HS-5) or the extremely hydrophobic fumed silica (TS-720), the adhesive with moderate hydrophobic fumed silica (TS-610) had the highest shear strength. It seemed that TEOS, silica sol and fumed silica played crosslinking, dispersing (for fumed silica) and reinforcing roles on waterborne adhesive, respectively.
(5) The high-molecular-weight phytic acid-polysilsesquioxane was successfully synthesized via sol-gel process using silylated phytic acid reacting with MTES and TEOS without any low molecular acid, the molecular weight of phytic acid-polysilsesquioxanes was more than 50000. Phytic acid served as not only catalysts but also reactant and chelating agent, which was in-situ incorporated with polysilsesquioxane chain uniformly. GPC, ~(13)CNMR, ~(29)SiNMR, XPS, Raman, SEM, electro-chemical techniques were used to investigate the correlation between the microstructure and property of PAP, TAP and HCP. PAP could form a compacting protective film because of strong chemical interaction between metal substrate and phytic acid-polysilsesquioxane, which had significantly better corrosion resistance compared to tannin-catalyzed polysilsesquioxane and HCl-catalyzed polysilsesquioxane.
引文
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