高分子复合材料的界面研究
摘要
界面在高分子复合材料中占有很大比例,界面相互作用力的强弱决定着高分子复合材料的性能和应用,因此高分子复合材料的界面改性研究有着十分重要的意义。
本论文首先开展了对有机填料型高分子复合材料-木质素/酚醛树脂的界面改性研究。第一种方法,通过两步磺化法提高了木质素中磺酸根的含量,增强了填料的极性,进而增强了界面粘结力。第二种方法通过酚化法增加了木质素中酚羟基的数量,改性后的木质素可与基底形成更多的共价键。两种方法都提高了产品的产率、耐热、耐光等性质。针对无机填料型高分子复合材料-碳酸钙/聚酯原位制备困难,碳酸钙分散差,界面作用力弱等问题,我们采用了聚乙二醇磷酸酯进行界面改性。由于这一高分子表面活性剂在无机粒子和基底之间形成了共价键桥,界面化学键的增加有助于产品性能的改善。实验表明产品的分散性、粘度、耐热等性质都得到改善。除此之外,我们还研究了高分子表面活性剂聚乙二醇磷酸酯对碳酸钙的界面诱导生长作用。结果表明在粒子生长过程中,高分子表面活性剂与无机粉体在界面的相互作用以及表面活性剂之间的相互作用,都对碳酸钙的结构和性质有影响。
Interface research has an important effect on the properties and application of the polymer composites. More and more people pay their attention to this area.
This paper studies the interface of lignin/phenol formaldehyde(PF), CaCO3/poly (ethylene terephthalate) (PET), and CaCO3/polyethylene glycol phosphate (PGP).
The first chapter describes two routes for improving the potential for partially replacing phenol with lignin in PF resin. The first method is the refinement of ligninsulphonate. The product prepared by the two-step sulfonation has a higher sulfonation degree, purity, and lower sugar content. The number of the polar function groups of lignin is increased, so it has the stronger interaction with PF. In the second method, phenolation and three-step polymerization were combined to increase the reactivity of black liquor lignin. The number of covalent bonds is increased between PF resin and lignin. Temperature stability, infrared and ultraviolet radiation resistances of the resins prepared by the two methods are both improved.
Due to the reaction of CaCO3 with terephthalic acid (TPA), the interaction of CaCO3 and PET in the compound prepared by the in-situ polymerization is weak. PGP solves the main problems: the reaction of CaCO3 with TPA, the agglomeration of CaCO3 nanoparticles, and the morphology control of CaCO3 nanoparticles. PGP provides a large of hydroxy groups which can form covalent bonds with carboxyl groups of PET during the polymerization, enabling CaCO3 nanoparticles to attach to PET matrix via the covalent bond. Based on these researches, stearic acid (SA) was modified on the surface of PGP-CaCO3 nanoparticles by the post-treatment, and the hydrophobic CaCO3 is obtained. This kind of the hydrophobic CaCO3 has the better compatibility with the polymer, which can be filled in PET at the process of polycondensation. The two kinds of nanocomposite exhibite a better dispersion of small primary nanoparticles, a higher polymerization degree, a better thermal stability and lower carboxyl end group content.
In the third chapter, the interface of PGP and CaCO3 is studied. PGP is modified on calcite surface via chemical bond,which controls and tunes the growth of CaCO3. The nanoparticles have a better dispersion in ethylene glycol. We discuss the influence of the experimental conditions on the dispersion. Based on this, hydrophobic CaCO3 was prepared at room temperature via a carbonization route in the presence of SA and PGP. FTIR demonstrates that SA and PGP are modified on CaCO3 surface via chemical bonds. The effects of the additives on the surface hydrophobicity of CaCO3 are examined. The cooperative interaction of SA and PGP at the interface plays a key role in the formation of the hydrophobic CaCO3. The modified CaCO3 with the contact angle of 106°is used to steady the emulsion of water and n-hexanol. We discuss the influence of the surfactant, time and the electrolyte on the stability of the Pickering emulsion.
本论文首先开展了对有机填料型高分子复合材料-木质素/酚醛树脂的界面改性研究。第一种方法,通过两步磺化法提高了木质素中磺酸根的含量,增强了填料的极性,进而增强了界面粘结力。第二种方法通过酚化法增加了木质素中酚羟基的数量,改性后的木质素可与基底形成更多的共价键。两种方法都提高了产品的产率、耐热、耐光等性质。针对无机填料型高分子复合材料-碳酸钙/聚酯原位制备困难,碳酸钙分散差,界面作用力弱等问题,我们采用了聚乙二醇磷酸酯进行界面改性。由于这一高分子表面活性剂在无机粒子和基底之间形成了共价键桥,界面化学键的增加有助于产品性能的改善。实验表明产品的分散性、粘度、耐热等性质都得到改善。除此之外,我们还研究了高分子表面活性剂聚乙二醇磷酸酯对碳酸钙的界面诱导生长作用。结果表明在粒子生长过程中,高分子表面活性剂与无机粉体在界面的相互作用以及表面活性剂之间的相互作用,都对碳酸钙的结构和性质有影响。
Interface research has an important effect on the properties and application of the polymer composites. More and more people pay their attention to this area.
This paper studies the interface of lignin/phenol formaldehyde(PF), CaCO3/poly (ethylene terephthalate) (PET), and CaCO3/polyethylene glycol phosphate (PGP).
The first chapter describes two routes for improving the potential for partially replacing phenol with lignin in PF resin. The first method is the refinement of ligninsulphonate. The product prepared by the two-step sulfonation has a higher sulfonation degree, purity, and lower sugar content. The number of the polar function groups of lignin is increased, so it has the stronger interaction with PF. In the second method, phenolation and three-step polymerization were combined to increase the reactivity of black liquor lignin. The number of covalent bonds is increased between PF resin and lignin. Temperature stability, infrared and ultraviolet radiation resistances of the resins prepared by the two methods are both improved.
Due to the reaction of CaCO3 with terephthalic acid (TPA), the interaction of CaCO3 and PET in the compound prepared by the in-situ polymerization is weak. PGP solves the main problems: the reaction of CaCO3 with TPA, the agglomeration of CaCO3 nanoparticles, and the morphology control of CaCO3 nanoparticles. PGP provides a large of hydroxy groups which can form covalent bonds with carboxyl groups of PET during the polymerization, enabling CaCO3 nanoparticles to attach to PET matrix via the covalent bond. Based on these researches, stearic acid (SA) was modified on the surface of PGP-CaCO3 nanoparticles by the post-treatment, and the hydrophobic CaCO3 is obtained. This kind of the hydrophobic CaCO3 has the better compatibility with the polymer, which can be filled in PET at the process of polycondensation. The two kinds of nanocomposite exhibite a better dispersion of small primary nanoparticles, a higher polymerization degree, a better thermal stability and lower carboxyl end group content.
In the third chapter, the interface of PGP and CaCO3 is studied. PGP is modified on calcite surface via chemical bond,which controls and tunes the growth of CaCO3. The nanoparticles have a better dispersion in ethylene glycol. We discuss the influence of the experimental conditions on the dispersion. Based on this, hydrophobic CaCO3 was prepared at room temperature via a carbonization route in the presence of SA and PGP. FTIR demonstrates that SA and PGP are modified on CaCO3 surface via chemical bonds. The effects of the additives on the surface hydrophobicity of CaCO3 are examined. The cooperative interaction of SA and PGP at the interface plays a key role in the formation of the hydrophobic CaCO3. The modified CaCO3 with the contact angle of 106°is used to steady the emulsion of water and n-hexanol. We discuss the influence of the surfactant, time and the electrolyte on the stability of the Pickering emulsion.
引文
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