梳状有机硅改性丙烯酸树脂的研究
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摘要
聚硅氧烷具有耐低温、低表面能、良好的耐水性、耐老化、和耐候性等一系列优异独特的性能,将聚硅氧烷进入到其它聚合物中,可以得到性能优异的材料。本文合成了两种不同类型的聚硅氧烷,并将其接枝到聚丙烯酸树脂分子中,并对有机硅改性的丙烯酸树脂做了初步的研究。
以八甲基环四硅氧烷(D4)、γ-甲基丙烯酰氧基丙基三甲氧基硅烷(KH-570)和三甲基氯硅烷为原料合成含有三个硅氧烷链段且含有碳碳不饱和双键的有机硅低聚物(MAPT-PDMS)。此低聚物在乳液中与丙烯酸酯单体共聚,可形成具有梳状结构的聚合物。聚合物的膜表面性能由红外光谱(FT-TR),X射线光电子能谱分析(XPS),原子力显微镜(AFM)进行表征。X射线光电子能谱分析结果证实膜的表面C/Si原子比为2.24,接近于有机硅低聚物(MAPT-PDMS)的C/Si原子比,此外,接触角及膜的吸水率的测定结果表明有机硅有效增强共聚物膜的疏水性(接触角可达105°)。
以有机硅低聚物(MAPT-PDMS)和甲基丙烯酸三氟乙酯为改性单体,以乳液聚合方法合成了氟硅改性的梳状丙烯酸树脂乳液。在乳液成膜过程中,MAPT-PDMS在膜表面形成了疏水层,进而能有效地抵抗水和有机溶剂对其的溶胀作用。甲基丙烯酸三氟乙酯在膜表面形成的氟碳链有序排列则显著降低了膜的表面能,从而显著提高了膜的防水、防油性能。接触角实验测试表明,所合成的氟硅改性丙烯酸树脂具有较好的防水性能。
以六甲基环三硅氧烷(D3)、二甲基氯硅烷(TMCS)、芘、6-溴己酰氯、甲基丙烯酸烯丙酯为原料制备新型含有荧光团且含有碳碳不饱和双键的含芘基团有机硅低聚物(PY-PDMS),此低聚物在乳液中与丙烯酸酯单体共聚,可形成具有梳状结构的聚合物。聚合物的膜表面性能由红外光谱(FT-TR)进行表征。着重研究含芘基团有机硅低聚物(PY-PDMS)的引入对聚合物膜的荧光性能,以及硝基芳烃对聚合物膜荧光猝灭的影响。
Polysiloanes posses a variety of unique and superior properties such as low temperature resistance ,low surface energy, good water resistance, aging resistance, climate resistance and so on. Polysiloanes can endow other polymers with the excellent properties so that new polymer materials can be obtained. In this theis two different types of polysiloanes were synthesized to conpolymerize with other acrylate monomers in emulsion and the properties of modified polyacrylates with polysiloanes were simply studied.
An organosilicone oligomer, which has three siloxane chains and a double bond at one of its ends, was synthesized from trimethy chlorosilane,γ-methylacryloylorg- anosiloxane (KH-570) and octamethyl cyclotetrasiloxane (D4). The terminal double bond enables it to conpolymerize with other acrylate monomers in emulsion, therefore gives out a comb-like structured polymer. This polymer are characterized by 1H NMR, FT-IR, XPS, and AFM. The result of XPS shows that the ratio of C to Si in the surface of the polymer film is 2.24:1, almost the same as that in the organosilicone oligomer. The contact angle could reach 105°. All these dates indicates an increase of surface water resistance.
The fluoro-siloxane polyacrylate latex, which was obtained by seed emulsion polymerization of acrylate with organosilicone oligomer (MAPT-PDMS) and 2,2,2-Trifluoroethyl methacrylate as modifiers. The efficient crosslinking structure was formed due to the MAPT-PDMS in formation process of the film. Consequently, the water and solvent.Resistance properites of flim were dramatically improved.The surface energy of films was reduced due to the order arrangement of fluorocarbon chain of 2,2,2-Trifluoroethyl methacrylate on the flim surface, and therefore, the water and oil repellency properties of film was significantly increased. In addition, The contact angle finished by this emulsion exhibited good water repellency property.
An organosilicone oligomer with Pyrene (MAPT-PDMS), which has fluorescence and a double bond at one of its ends, was synthesized from Pyrene, 6-bromohexanoyl chloride, allyl methacrylate, dimethylchlorosilane, hexamethylcyclotrisiloxane (D3). The terminal double bond enables it to conpolymerize with other acrylate monomers in emulsion, therefore gives out a comb-like structured polymer. This polymer are characterized by FT-IR. the fluorescence properties of modified polyacrylates with PY-PDMS and the fluorescence quenching of the films upon exposure to nitro compounds were studied.
以八甲基环四硅氧烷(D4)、γ-甲基丙烯酰氧基丙基三甲氧基硅烷(KH-570)和三甲基氯硅烷为原料合成含有三个硅氧烷链段且含有碳碳不饱和双键的有机硅低聚物(MAPT-PDMS)。此低聚物在乳液中与丙烯酸酯单体共聚,可形成具有梳状结构的聚合物。聚合物的膜表面性能由红外光谱(FT-TR),X射线光电子能谱分析(XPS),原子力显微镜(AFM)进行表征。X射线光电子能谱分析结果证实膜的表面C/Si原子比为2.24,接近于有机硅低聚物(MAPT-PDMS)的C/Si原子比,此外,接触角及膜的吸水率的测定结果表明有机硅有效增强共聚物膜的疏水性(接触角可达105°)。
以有机硅低聚物(MAPT-PDMS)和甲基丙烯酸三氟乙酯为改性单体,以乳液聚合方法合成了氟硅改性的梳状丙烯酸树脂乳液。在乳液成膜过程中,MAPT-PDMS在膜表面形成了疏水层,进而能有效地抵抗水和有机溶剂对其的溶胀作用。甲基丙烯酸三氟乙酯在膜表面形成的氟碳链有序排列则显著降低了膜的表面能,从而显著提高了膜的防水、防油性能。接触角实验测试表明,所合成的氟硅改性丙烯酸树脂具有较好的防水性能。
以六甲基环三硅氧烷(D3)、二甲基氯硅烷(TMCS)、芘、6-溴己酰氯、甲基丙烯酸烯丙酯为原料制备新型含有荧光团且含有碳碳不饱和双键的含芘基团有机硅低聚物(PY-PDMS),此低聚物在乳液中与丙烯酸酯单体共聚,可形成具有梳状结构的聚合物。聚合物的膜表面性能由红外光谱(FT-TR)进行表征。着重研究含芘基团有机硅低聚物(PY-PDMS)的引入对聚合物膜的荧光性能,以及硝基芳烃对聚合物膜荧光猝灭的影响。
Polysiloanes posses a variety of unique and superior properties such as low temperature resistance ,low surface energy, good water resistance, aging resistance, climate resistance and so on. Polysiloanes can endow other polymers with the excellent properties so that new polymer materials can be obtained. In this theis two different types of polysiloanes were synthesized to conpolymerize with other acrylate monomers in emulsion and the properties of modified polyacrylates with polysiloanes were simply studied.
An organosilicone oligomer, which has three siloxane chains and a double bond at one of its ends, was synthesized from trimethy chlorosilane,γ-methylacryloylorg- anosiloxane (KH-570) and octamethyl cyclotetrasiloxane (D4). The terminal double bond enables it to conpolymerize with other acrylate monomers in emulsion, therefore gives out a comb-like structured polymer. This polymer are characterized by 1H NMR, FT-IR, XPS, and AFM. The result of XPS shows that the ratio of C to Si in the surface of the polymer film is 2.24:1, almost the same as that in the organosilicone oligomer. The contact angle could reach 105°. All these dates indicates an increase of surface water resistance.
The fluoro-siloxane polyacrylate latex, which was obtained by seed emulsion polymerization of acrylate with organosilicone oligomer (MAPT-PDMS) and 2,2,2-Trifluoroethyl methacrylate as modifiers. The efficient crosslinking structure was formed due to the MAPT-PDMS in formation process of the film. Consequently, the water and solvent.Resistance properites of flim were dramatically improved.The surface energy of films was reduced due to the order arrangement of fluorocarbon chain of 2,2,2-Trifluoroethyl methacrylate on the flim surface, and therefore, the water and oil repellency properties of film was significantly increased. In addition, The contact angle finished by this emulsion exhibited good water repellency property.
An organosilicone oligomer with Pyrene (MAPT-PDMS), which has fluorescence and a double bond at one of its ends, was synthesized from Pyrene, 6-bromohexanoyl chloride, allyl methacrylate, dimethylchlorosilane, hexamethylcyclotrisiloxane (D3). The terminal double bond enables it to conpolymerize with other acrylate monomers in emulsion, therefore gives out a comb-like structured polymer. This polymer are characterized by FT-IR. the fluorescence properties of modified polyacrylates with PY-PDMS and the fluorescence quenching of the films upon exposure to nitro compounds were studied.
引文
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[2]王剑,储富祥.机硅氧烷改性丙烯酸酯乳液的制备及结构与性能研究[J].高分子材料科学与工程,2005,21(5):110-113
[3]王月菊,刘杰,杨建军等.有机硅改性丙烯酸酯最新乳液聚合方法研究进展[J].涂料技术与文摘,2009,30(2):7-10
[4] Liu B. L., Deng X. B., Cao S. S., et al. Preparation and characterization of core/shell particles with siloxane in the shell[J]. Applied Surface Science, 2006, 252 (6): 2235-2241
[5] Zou M. X., Wang S. J., Zhang Z. C., et al. Preparation and characterization of polysiloxane-poly(butylacrylate–styrene) composite latices and their film properties[J]. European Polymer Journal, 2005, 41(11): 2602-2613
[6] Bats F. S., Ferdickson G. H. Block coplymer thermodynamics: Theory and experiment[J]. Annu Rev Phys Chem, 1990, 41: 525-557
[7] Noshya A., MeGrhat J. E. Block Coplymers: Overview and Critical Survey[M]. NewYork: Academic press, 1977: 13-14
[8] Saam J. C., Godron D. J. Block coplymers of polydimethylsiloxane and polystyrene[J]. Maocrmolecuels, 1970, 3(1): l-4
[9] Saam J. C.,Ward A. H., Fearon F. W. G. Polystyrene-polydimehtylsiloxane multi-block copolmyers[J]. Poylm PrPer, 1972, 13(l): 524-528
[10] Zilliox J. G., Roovers J. E. L., Bywater S. Preparation and properties of polydimethylsiloxane and its block copolymers with styrene[J]. Maocrmolecuels, 1975, 8(5): 573-578
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