纳米SiO_2/含氟丙烯酸酯复合乳液及高硬度透明疏水涂层的制备与表征
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摘要
近年来，透明疏水材料在建筑、汽车玻璃、文物保护、望远镜、太阳能电池板等领域中表现出极大的潜在应用价值。含氟聚合物由于其独特的疏油疏水性，耐热性，化学品惰性，低介电常数和生物相容性，已被广泛用来制备疏水材料。随着人们环境保护和能源意识的增强以及特殊应用场合对疏水材料透明性的要求，水性含氟丙烯酸酯乳液及其透明疏水涂层开始受到广泛关注。然而，由于含氟单体价格贵，含氟丙烯酸酯乳液涂层力学性能差等问题，含氟丙烯酸酯乳液及其透明、疏水涂层的大规模实际应用仍然受到限制。纳米SiO_2是一种性能优异、来源广泛的无机纳米粒子，能够增强有机聚合物的硬度、改善其耐磨性、抗刮伤性、紫外光屏蔽性能等。如何将纳米SiO_2通过简单、有效的工艺引入含氟丙烯酸酯乳液制备兼顾有机和无机特性的纳米复合乳液，实现纳米SiO_2在含氟丙烯酸酯聚合物中的良好分散，得到高硬度，高透明，强疏水，高耐热等综合性能优异的涂层材料一直是材料工作者努力追求的目标和方向。
本论文以纳米SiO_2/丙烯酸酯单体分散液或氮硅烷改性的气相法纳米SiO_2，通过原位聚合、种子乳液聚合、细乳液聚合等技术，制备了纳米SiO_2/（含氟）丙烯酸酯乳液及高硬度透明疏水的复合乳胶涂层，并对复合乳液及其涂层进行了研究。论文的研究内容和成果主要包括以下几个方面：
(1)以甲基丙烯酸甲酯(MMA)和丙烯酸丁酯(BA)混合单体作为油相介质，以正硅酸乙酯(TEOS)为前驱体，γ-甲基丙烯酰氧基丙基三甲氧基硅烷(MPS)为改性剂，通过乳液法制备出稳定的纳米SiO_2/丙烯酸酯单体分散液(DSAM)，考察了乳化剂用量、油水比、SiO_2用量对DSAM稳定性的影响和pH值、乳化剂用量对SiO_2生成率的影响。DSAM的最佳制备条件为：pH值为2，DNS-86用量为6wt%，油水比为1:1，SiO_2用量为5.5wt%。傅里叶变换红外光谱(FTIR)验证了TEOS在乳液体系中水解生成SiO_2，MPS以共价键形式实现其对SiO_2表面的亲油改性，在SiO_2表面接枝上了甲基丙烯酰氧基团，这有利于纳米SiO_2粒子在单体液滴中的稳定存在和后续的聚合反应。
(2)基于稳定的DSAM，以原位乳液聚合技术和半连续种子乳液聚合技术，采用反应性乳化剂DNS-86，水溶性引发剂KPS，主单体MMA和BA，成功制备了纳米SiO_2/丙烯酸酯复合乳液，乳胶粒子具有窄的粒径分布。发现MMA/BA的质量比减小，膜的硬度减小，附着力增加；纳米SiO_2粒子能提高复合乳胶膜的硬度，纳米SiO_2用量为5.5wt%时，复合乳胶膜的硬度高达3H。纳米SiO_2引入丙烯酸酯乳胶粒子后，还能提高复合乳胶膜耐水性、耐热性能和紫外光屏蔽性能。
(3)采用原位聚合与半连续-种子乳液聚合相结合的技术，在壳层聚合阶段引入含氟丙烯酸酯单体，成功制备了稳定、单分散的核壳型纳米SiO_2/含氟丙烯酸酯复合乳液及高硬度，强疏水，透明，耐热的复合乳胶涂层。结果表明，含氟丙烯酸酯单体用量的增加有利于水接触角的提高，MMA/BA质量比对复合乳胶膜的水接触角也有重要的影响，当DFHMA用量为6wt%，MMA/BA质量比为1/3时,水接触角可以达到121.0°。侧链长、含氟率高的含氟丙烯酸酯单体有利于提高复合乳胶膜的透光率和降低雾度。纳米SiO_2的引入对纳米SiO_2/含氟丙烯酸酯乳胶膜硬度的改善作用较大，纳米SiO_2还能明显提高复合乳胶膜的热稳定性和紫外光屏蔽性能。TEM、FTIR和XPS等测试表明纳米SiO_2和含氟丙烯酸酯具有良好的结合，复合乳胶膜是含氟基团呈梯度分布的涂层材料，并建构了在不同MMA/BA条件下，纳米SiO_2/含氟丙烯酸酯复合乳胶膜中含氟基团向表面迁移和富集过程的理论模型。
(4)在亲油性纳米SiO_2粒子存在的条件下，进行MMA、BA、甲基丙烯酸十三氟辛酯(PFOMA)的原位细乳液聚合成功制备了具有良好稳定性的纳米SiO_2/含氟丙烯酸酯复合细乳液。结果表明，反应温度、乳化剂浓度、引发剂浓度对单体转化率以及聚合速率影响明显，细乳液聚合反应的表观活化能(Ea)为171.9kJ/mol，聚合反应是以细乳液单体液滴成核机理控制的反应过程。增加含氟单体的用量可以提高复合乳胶膜的疏水性。在浸水、浸酸碱处理后，复合乳胶膜还具有自增强、自修复能力。复合乳胶膜具有良好透明性，乳化剂SDS用量和纳米SiO_2用量增加，复合乳胶膜透光率降低。纳米SiO_2用量增加，复合乳胶膜雾度升高。浸水处理后，复合乳胶膜的透光率降低、雾度升高。纳米SiO_2的引入能明显改善乳胶膜的热稳定性，当纳米SiO_2用量为6.0wt%，复合乳胶膜的T10%比未引入纳米SiO_2时提高67.0oC。复合乳液应用于纸纤维改性，可在纸纤维表面构建“纳微”双粗糙度结构，将完全亲水性的纸纤维转变为高度疏水的纸纤维，使水接触角由0o提升至128.5o。
Recently, transparent and hydrophobic materials have exhibited huge potential in thefields of building materials, automobile glass, historic monuments protection, telescope lenses,and solar panels and so on. Due to its unique properties of amphiphobicity, thermal stabilityand chemical inertness, low dielectric constant and good biocompatibility, fluorinatedpolymers are mostly used to prepare hydrophobic materials. Accompanying withstrengthening of consciousness of environment protection and energy, and demands ontransparency of hydrophobic materials on some special cases, people pay more and moreattentions to prepare aqueous fluorinated polyacrylate composite latex and transparent andhydrophobic coatings. However, the large-scale applications of fluorinated polyacrylate latexand its transparent and hydrophobic coatings are still limited by the high price of fluorinatedacrylate monomers and weak mechanical property of fluorinated polyacrylate latex film.Nano-silica is a kind of inorganic nanoparticles with excellent properties and wide rawmaterial source，which can improve organic polymers in their hardness，scratch-resistance，UV-resistance and so on. Thus, how to incorporate nano-silca into fluorinated polyacrylatelatex simply and effectively and make nano-silica well dispersed in fluorinated polymers toprepare eventually the high hardness, transparent, hydrophobic and thermal stable coatings isalways the goal of material researcher.
In this work，nano-silica/(fluorinated) polyacrylate composite latex were prepared by thecombined techniques of in stiu polymerization, seeded emulsion polymerization andminiemulsion polymerization. The high hardness, transparent and hydrophobic compositelatex coatings were prepared and the properties and structures of composite latex and resultantfilms were investigated in detail. The main research contents and achievements are listed asfollowing:
First，the stable dispersion of nano-silica/acrylate monomers (DSAM) was prepared byemulsion method with methylmethacrylate (MMA) and butyl acrylate (BA) in the micelles asdispersing media, tetrethoxysilicate (TEOS) as prescuror and γ-methacryloylpropyltrimethoxysilane (MPS) as modifier. The effects of emulsifier content, mass ratio of oil towater (Ro/w), and silica content on stability of DSAM and the effects of pH value andemulsifier content on yields of silica were studied. The optimal conditions for DSAM arefollows: pH value is2, DNS-86content is6wt%, Ro/wis1:1, silica content is5.5wt%.Fourier transform infrared spectroscopy (FTIR) confirmed that silica formed from TEOS inemulsion system and oleophilic surface of silica were achieved by condensation of hydroxyl groups between silica and hydrolysis from MPS. The methacryloyl groups grafted on thesurface of silica improved the stability of silica dispersed in acrylate monomer droplets andprovided double bond for the subsequent polymerization with acrylate monomer.
Second, the monodisperse nano-silica/polyacrylate composite latex was successfullyprepared by the combination of in situ polymerization and semi-continuous seeded emulsionpolymerization based on the stable DSAM. In the above polymerization, the reactiveemulsifier DSN-86, MMA, BA and initiantor KPS were used. The results show that the pencilhardness decreases while adhesion increases with the increase of MMA/BA mass ratio. Thenano-silica can improve the pencil hardness. When the nano-silica content is5.5wt%, thecomposite latex film has the high pencil hardness of3H. The incorporation of nano-silica intocomposite film can also improve thermal stability and performance of shielding fromultraviolet.
Third，the stable and monodisperse nano-silica/fluorinated polyacrylate latex and theresultant transparent and hydrophobic composite films with high hardness and thermalstability were prepared by in situ polymerization and semi-continuous emulsionpolymerization. The fluorinated acrylate monomers were introduced into the second stage. Itis found that more fluorinated content, higher water contact angle and MMA/BA mass ratiohas important an influence on water contact angles. When DFHMA content was6wt%andMMA/BA mass ratio was1/3, water contact angle of the compostite film could reach121.0o.In addition, the longer fluorinated side chain will resulted in higher transmittance and lowerhaze. The incorporation of nano-silica can obviously improve the hardness of the compositefilm. Nano-silica can also improve the thermal stability and ultraviolet shielding performanceof the composite film. TEM, FTIR and XPS confirm that there are good combined forcebetween nano-silica and fluorinated polyacrylate at nano-scale and fluorinated groups has agradient distribution along the depth of film. The possible mechanism of migration andenrichment of fluorinated groups to the film surface under different MMA/BA mass ratio wasproposed.
Fourth，the stable nano-silica/fluorinated polyacrylate composite latex was prepared byin situ miniemulsion polymerization with MMA, BA and PFOMA as monomers in thepresence of oleophilic nano-silica. Kinetics of miniemulsion polymerization was studied. Themonomer conversion and rate of polymerization was influenced by reaction temperature, thecontent of emulsifier and initiator. The apparent activation energy of reaction of miniemulsionpolymerization was171.9kJ/mol. DLS analysis shows that main nucleation mechanism is monomer droplet nucleation. The measurement of water contact angle shows that theincreasing fluorinated monomer content will improve the hydrophobicity of the compositefilm. Compared with non-fluorinated latex film, the composite film not only has betterhydrophobicity but also has a certain self-healing ability after immersion in water or acid orbase. Moreover，the composite film has good transparency. The increase in SDS content andnano-silica content will decreases the transmittance while the increase in nano-silica willincrease the haze. The transmittance reduces and haze rises after water immersion treatment.The incorporation of nano-silica into composite film also improves the thermal stabilitydramatically. Compared with that of film without nano-silica, T10%of composite film with6.0wt%silica content improved by67.0oC. The construction of nano-micro double roughness onthe surface of paper fibers was achieved when paper fibers was treated by the composite latexand the water contact angle of the paper fibers improved from0oto128.5o, which illustratesthat paper fibers has transformed from total hydrophily to strong hydrophobicity.
本论文以纳米SiO_2/丙烯酸酯单体分散液或氮硅烷改性的气相法纳米SiO_2，通过原位聚合、种子乳液聚合、细乳液聚合等技术，制备了纳米SiO_2/（含氟）丙烯酸酯乳液及高硬度透明疏水的复合乳胶涂层，并对复合乳液及其涂层进行了研究。论文的研究内容和成果主要包括以下几个方面：
(1)以甲基丙烯酸甲酯(MMA)和丙烯酸丁酯(BA)混合单体作为油相介质，以正硅酸乙酯(TEOS)为前驱体，γ-甲基丙烯酰氧基丙基三甲氧基硅烷(MPS)为改性剂，通过乳液法制备出稳定的纳米SiO_2/丙烯酸酯单体分散液(DSAM)，考察了乳化剂用量、油水比、SiO_2用量对DSAM稳定性的影响和pH值、乳化剂用量对SiO_2生成率的影响。DSAM的最佳制备条件为：pH值为2，DNS-86用量为6wt%，油水比为1:1，SiO_2用量为5.5wt%。傅里叶变换红外光谱(FTIR)验证了TEOS在乳液体系中水解生成SiO_2，MPS以共价键形式实现其对SiO_2表面的亲油改性，在SiO_2表面接枝上了甲基丙烯酰氧基团，这有利于纳米SiO_2粒子在单体液滴中的稳定存在和后续的聚合反应。
(2)基于稳定的DSAM，以原位乳液聚合技术和半连续种子乳液聚合技术，采用反应性乳化剂DNS-86，水溶性引发剂KPS，主单体MMA和BA，成功制备了纳米SiO_2/丙烯酸酯复合乳液，乳胶粒子具有窄的粒径分布。发现MMA/BA的质量比减小，膜的硬度减小，附着力增加；纳米SiO_2粒子能提高复合乳胶膜的硬度，纳米SiO_2用量为5.5wt%时，复合乳胶膜的硬度高达3H。纳米SiO_2引入丙烯酸酯乳胶粒子后，还能提高复合乳胶膜耐水性、耐热性能和紫外光屏蔽性能。
(3)采用原位聚合与半连续-种子乳液聚合相结合的技术，在壳层聚合阶段引入含氟丙烯酸酯单体，成功制备了稳定、单分散的核壳型纳米SiO_2/含氟丙烯酸酯复合乳液及高硬度，强疏水，透明，耐热的复合乳胶涂层。结果表明，含氟丙烯酸酯单体用量的增加有利于水接触角的提高，MMA/BA质量比对复合乳胶膜的水接触角也有重要的影响，当DFHMA用量为6wt%，MMA/BA质量比为1/3时,水接触角可以达到121.0°。侧链长、含氟率高的含氟丙烯酸酯单体有利于提高复合乳胶膜的透光率和降低雾度。纳米SiO_2的引入对纳米SiO_2/含氟丙烯酸酯乳胶膜硬度的改善作用较大，纳米SiO_2还能明显提高复合乳胶膜的热稳定性和紫外光屏蔽性能。TEM、FTIR和XPS等测试表明纳米SiO_2和含氟丙烯酸酯具有良好的结合，复合乳胶膜是含氟基团呈梯度分布的涂层材料，并建构了在不同MMA/BA条件下，纳米SiO_2/含氟丙烯酸酯复合乳胶膜中含氟基团向表面迁移和富集过程的理论模型。
(4)在亲油性纳米SiO_2粒子存在的条件下，进行MMA、BA、甲基丙烯酸十三氟辛酯(PFOMA)的原位细乳液聚合成功制备了具有良好稳定性的纳米SiO_2/含氟丙烯酸酯复合细乳液。结果表明，反应温度、乳化剂浓度、引发剂浓度对单体转化率以及聚合速率影响明显，细乳液聚合反应的表观活化能(Ea)为171.9kJ/mol，聚合反应是以细乳液单体液滴成核机理控制的反应过程。增加含氟单体的用量可以提高复合乳胶膜的疏水性。在浸水、浸酸碱处理后，复合乳胶膜还具有自增强、自修复能力。复合乳胶膜具有良好透明性，乳化剂SDS用量和纳米SiO_2用量增加，复合乳胶膜透光率降低。纳米SiO_2用量增加，复合乳胶膜雾度升高。浸水处理后，复合乳胶膜的透光率降低、雾度升高。纳米SiO_2的引入能明显改善乳胶膜的热稳定性，当纳米SiO_2用量为6.0wt%，复合乳胶膜的T10%比未引入纳米SiO_2时提高67.0oC。复合乳液应用于纸纤维改性，可在纸纤维表面构建“纳微”双粗糙度结构，将完全亲水性的纸纤维转变为高度疏水的纸纤维，使水接触角由0o提升至128.5o。
Recently, transparent and hydrophobic materials have exhibited huge potential in thefields of building materials, automobile glass, historic monuments protection, telescope lenses,and solar panels and so on. Due to its unique properties of amphiphobicity, thermal stabilityand chemical inertness, low dielectric constant and good biocompatibility, fluorinatedpolymers are mostly used to prepare hydrophobic materials. Accompanying withstrengthening of consciousness of environment protection and energy, and demands ontransparency of hydrophobic materials on some special cases, people pay more and moreattentions to prepare aqueous fluorinated polyacrylate composite latex and transparent andhydrophobic coatings. However, the large-scale applications of fluorinated polyacrylate latexand its transparent and hydrophobic coatings are still limited by the high price of fluorinatedacrylate monomers and weak mechanical property of fluorinated polyacrylate latex film.Nano-silica is a kind of inorganic nanoparticles with excellent properties and wide rawmaterial source，which can improve organic polymers in their hardness，scratch-resistance，UV-resistance and so on. Thus, how to incorporate nano-silca into fluorinated polyacrylatelatex simply and effectively and make nano-silica well dispersed in fluorinated polymers toprepare eventually the high hardness, transparent, hydrophobic and thermal stable coatings isalways the goal of material researcher.
In this work，nano-silica/(fluorinated) polyacrylate composite latex were prepared by thecombined techniques of in stiu polymerization, seeded emulsion polymerization andminiemulsion polymerization. The high hardness, transparent and hydrophobic compositelatex coatings were prepared and the properties and structures of composite latex and resultantfilms were investigated in detail. The main research contents and achievements are listed asfollowing:
First，the stable dispersion of nano-silica/acrylate monomers (DSAM) was prepared byemulsion method with methylmethacrylate (MMA) and butyl acrylate (BA) in the micelles asdispersing media, tetrethoxysilicate (TEOS) as prescuror and γ-methacryloylpropyltrimethoxysilane (MPS) as modifier. The effects of emulsifier content, mass ratio of oil towater (Ro/w), and silica content on stability of DSAM and the effects of pH value andemulsifier content on yields of silica were studied. The optimal conditions for DSAM arefollows: pH value is2, DNS-86content is6wt%, Ro/wis1:1, silica content is5.5wt%.Fourier transform infrared spectroscopy (FTIR) confirmed that silica formed from TEOS inemulsion system and oleophilic surface of silica were achieved by condensation of hydroxyl groups between silica and hydrolysis from MPS. The methacryloyl groups grafted on thesurface of silica improved the stability of silica dispersed in acrylate monomer droplets andprovided double bond for the subsequent polymerization with acrylate monomer.
Second, the monodisperse nano-silica/polyacrylate composite latex was successfullyprepared by the combination of in situ polymerization and semi-continuous seeded emulsionpolymerization based on the stable DSAM. In the above polymerization, the reactiveemulsifier DSN-86, MMA, BA and initiantor KPS were used. The results show that the pencilhardness decreases while adhesion increases with the increase of MMA/BA mass ratio. Thenano-silica can improve the pencil hardness. When the nano-silica content is5.5wt%, thecomposite latex film has the high pencil hardness of3H. The incorporation of nano-silica intocomposite film can also improve thermal stability and performance of shielding fromultraviolet.
Third，the stable and monodisperse nano-silica/fluorinated polyacrylate latex and theresultant transparent and hydrophobic composite films with high hardness and thermalstability were prepared by in situ polymerization and semi-continuous emulsionpolymerization. The fluorinated acrylate monomers were introduced into the second stage. Itis found that more fluorinated content, higher water contact angle and MMA/BA mass ratiohas important an influence on water contact angles. When DFHMA content was6wt%andMMA/BA mass ratio was1/3, water contact angle of the compostite film could reach121.0o.In addition, the longer fluorinated side chain will resulted in higher transmittance and lowerhaze. The incorporation of nano-silica can obviously improve the hardness of the compositefilm. Nano-silica can also improve the thermal stability and ultraviolet shielding performanceof the composite film. TEM, FTIR and XPS confirm that there are good combined forcebetween nano-silica and fluorinated polyacrylate at nano-scale and fluorinated groups has agradient distribution along the depth of film. The possible mechanism of migration andenrichment of fluorinated groups to the film surface under different MMA/BA mass ratio wasproposed.
Fourth，the stable nano-silica/fluorinated polyacrylate composite latex was prepared byin situ miniemulsion polymerization with MMA, BA and PFOMA as monomers in thepresence of oleophilic nano-silica. Kinetics of miniemulsion polymerization was studied. Themonomer conversion and rate of polymerization was influenced by reaction temperature, thecontent of emulsifier and initiator. The apparent activation energy of reaction of miniemulsionpolymerization was171.9kJ/mol. DLS analysis shows that main nucleation mechanism is monomer droplet nucleation. The measurement of water contact angle shows that theincreasing fluorinated monomer content will improve the hydrophobicity of the compositefilm. Compared with non-fluorinated latex film, the composite film not only has betterhydrophobicity but also has a certain self-healing ability after immersion in water or acid orbase. Moreover，the composite film has good transparency. The increase in SDS content andnano-silica content will decreases the transmittance while the increase in nano-silica willincrease the haze. The transmittance reduces and haze rises after water immersion treatment.The incorporation of nano-silica into composite film also improves the thermal stabilitydramatically. Compared with that of film without nano-silica, T10%of composite film with6.0wt%silica content improved by67.0oC. The construction of nano-micro double roughness onthe surface of paper fibers was achieved when paper fibers was treated by the composite latexand the water contact angle of the paper fibers improved from0oto128.5o, which illustratesthat paper fibers has transformed from total hydrophily to strong hydrophobicity.
引文
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