碳纳米管聚氨酯纳米复合涂料合成及性能研究
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摘要
本文研究了碳纳米管聚氨酯纳米复合涂料的合成以及碳纳米管的加入对聚氨酯涂料性能的影响,主要做了关于碳纳米管聚氨酯纳米复合涂料的合成工艺过程以及碳纳米管独特的性能对聚氨酯涂料弹性模量、拉伸强度、动态力学性能、硬度、耐冲击性、柔韧性、导电性和漆膜颜色等方面影响的基础性探索研究。
首先利用浓硫酸和浓硝酸组合的混酸对碳纳米管进行酸化处理,并结合傅立叶红外光谱、X射线光电子能谱、拉曼光谱、电子显微镜和分散稳定性观察来分析酸化处理对碳纳米管物理性质和化学性质的影响。结果表明：碳纳米管经过浓硫酸和浓硝酸组合的混酸处理后,羧基被成功地接枝到碳纳米管上,并且随着酸化处理时间的延长在碳纳米管上产生的羧基越来越多,同时随着酸化处理时间的延长其管长逐渐变短,物理结构也逐渐地被一定程度的破坏。碳纳米管经过酸化处理后羧基的产生使其极性增加,使其在极性溶剂中的分散性明显提高。
本文研究的聚氨酯涂料是溶剂型双组分聚氨酯涂料,多异氰酸酯组分采用甲苯-2,4-二异氰酸酯(TDI)和三羟甲基丙烷(TMP)所合成的加成物,多羟基组分采用蓖麻油。在确定此种聚氨酯涂料合成和固化工艺过程的基础上,重点研究和优化了碳纳米管聚氨酯纳米复合涂料的合成和固化工艺过程,并分别采用原位聚合法和共混聚合法制备了纳米复合涂料。
漆膜力学性能方面的研究利用微机控制电子万能试验机、动态力学分析仪和漆膜性能测试方法测试分析了碳纳米管的加入对聚氨酯漆膜力学性能的影响。结果表明：碳纳米管可以有效地提高聚氨酯漆膜的弹性模量、拉伸强度、储能模量、玻璃化转变温度和硬度。但当碳纳米管含量过大时,反而会降低漆膜的弹性模量、拉伸强度、储能模量、玻璃化转变温度和硬度,并且漆膜的弹性模量、拉伸强度、储能模量、玻璃化转变温度和硬度随着碳纳米管酸化处理程度的提高而提高。在其他条件相同情况下,利用原位聚合法制备的漆膜的弹性模量、拉伸强度、储能模量、玻璃化转变温度和硬度要高于利用共混法制备的漆膜的弹性模量、拉伸强度、储能模量、玻璃化转变温度和硬度。同时碳纳米管的加入不会降低聚氨酯漆膜的耐冲击性和柔韧性。
漆膜导电性方面的研究利用数字超高电阻、微电流测量仪测试分析了碳纳米管的加入对聚氨酯漆膜导电性的影响。结果表明：碳纳米管的加入使聚氨酯漆膜的导电性得到了一定程度的提高。随着碳纳米管含量的增加漆膜的体积电阻率降低,当碳纳米管含量为1%时,其体积电阻率降低了2个数量级。并且漆膜的导电性随着碳纳米管酸化处理程度的提高而增强。在其他条件相同情况下,利用原位聚合法制备的漆膜的体积电阻率都低于利用共混法制备的漆膜的体积电阻率
利用全自动色差计测量分析了碳纳米管的加入对聚氨酯漆膜颜色的影响。结果表明：碳纳米管的加入使聚氨酯漆膜的颜色有所加深,随着碳纳米管含量的增加,颜色不断加深,当碳纳米管的含量低于0.1%时,对聚氨酯漆膜颜色的影响不大,含量超过0.1%时,漆膜的颜色变化很大,明显变黑。并且在其他条件相同情况下,漆膜的颜色随碳纳米管酸化处理程度的提高而加深,利用原位聚合法制备的漆膜的颜色比利用共混聚合法制备的漆膜的颜色更深。同时还研究了碳纳米管在聚氨酯漆膜中的分散情况。结果表明：碳纳米管在聚氨酯漆膜中的分散随着碳纳米管酸化处理程度的提高而更加均匀,并且利用原位聚合法制备的漆膜中碳纳米管的分散情况要比利用共混聚合法更理想。
The paper studied the synthesis of carbon nanotubes polyurethane composite coatings and the influence of carbon nanotubes on the properties of polyurethane coatings, the basic groping investigation of carbon nanotubes polyurethane composite coating synthesis procedure and the influence of carbon nanotubes special properties on the elastic modulus, tensile strength, dynamic mechanical properties, harhness, impact resistance, flexibility, electrical conductivity and colour appearance of polyurethane coating were done.
First carbon nanotubes were treated by the mixture of sulphuric acid and nitric acid, the influence of acid treatment on the physical properties and chemical properties of carbon nanotubes were characterised by Fourier tansform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy (Raman), Scanning electron microscopy (SEM) and dispersion stability evaluation. It resulted that, through acid treatment of the mixture of sulphuric acid and nitric acid, carboxylic goups (-COOH) could be successfully introduced onto the surface of carbon nanotubes, and longer acid treatment time afforded a larger number of the carboxylic groups (-COOH) to be attached onto the carbon nanotubes, also after acid treatment the carbon nanotubes became shorter and less well defined in terms of morphology. The polarity of carbon nanotubes was increased by acid treatment due to carboxylic groups (-COOH), and the dispersion stability of carbon nanotubes in polar solvent became better.
The polyurethane coating in the paper was a kind of solvent-thinned two-component polyurethane coating, the iscoyanates component was synthesized by toluene-2,4-diisocyanate (TDI) and trimethylol propane (TMP), and castor oil was used as the hydroxyls component. On the base of synthesis and polymerization procedure of this kind of polyurethane coating, the investigation and optimum of carbon nanotubes polyurethane composite coatings synthesis and polymerization were done mainly, and the nano-composite coatings were synthesized and polymerization via in situ polymerization and blending polyurethane.
About mechanical properties of coatings, tensile tester machine, dynamic mechanical analysis and coating properties evaluation were employed to assess the effects of carbon nanotubes on mechanical properties of polyurethane coatings. It resulted that, the elastic modulus, tensile strength, storage modulus, glass transition temperature and harhness of polyurethane coating could be improved by carbon nanotubes significantly. But if the concentration of carbon nanotubes was too high, the elastic modulus, tensile strength, storage modulus, glass transition temperature and harhness of polyurethane coating would decrease, and the elastic modulus, tensile strength, storage modulus, glass transition temperature and harhness of polyurethane coating increased with the increase of the length time of acid treatment to carbon nanotubes. Under the same other conditions, the elastic modulus, tensile strength, storage modulus, glass transition temperature and harhness of composite coating synthesized via in situ polymerization were better than that synthesized via blending polymerization. Carbon nanotubes would not decrease the impact resistance and flexibility of polyurethane coating.
About electrical conductivity properties of coatings, ohmmeter was employed to assess the effects of carbon nanotubes on electrical conductivity of polyurethane coatings. It resulted that, the electrical conductivity of polyurethane coatings could be improved by carbon nanotubes. The volume resistivity of composite coating decreased with the increasing of carbon nanotubes concentration, and when the concentration of cabon nanotubes was1%, the value of volume resistivity was102order of magnitude lower. The electrical conductivity of composite coatings increased with the increase of the length of time of acid treatment to carbon nanotubes. Under the same other conditions, the volume resistivity of composite coating synthesized via in situ polymerization was lower than that synthesized via blending polymerization.
Spectrophotometer was employed to assess the effects of carbon nanotubes on the colour appearance of polyurethane coatings. It resulted that, the colour depth of polyurethane coatings became deeper by carbon nanotubes, and the colour depth of composite coatings became deeper with the concentration of carbon nanotubes increasing, but when the concentration of carbon nanotubes was lower than0.1%, the carbon nanotubes would not influence the colour appearance significantly, but as the concentration was higher than0.1%, the colour change of composite coating was significantly and tured to black. Under the same other conditions, the colour depth of composite coating became deeper with the increase of the length of time of acid treatment to carbon nanotubes, the colour depth of composite coating synthesized via in situ polymerization was deeper than that synthesized via blending polymerization. Also the dispersion of carbon nanotubes in polyurethane coatings was studied. It result that, the dispersion of carbon nanotubes in polyurethane coatings became better with the increase of the length of time of acid treatment to carbon nanotubes, and the dispersion of carbon nanotubes in composite coating synthesized via in situ polymerization was better than that synthesized via blending polymerization.
首先利用浓硫酸和浓硝酸组合的混酸对碳纳米管进行酸化处理,并结合傅立叶红外光谱、X射线光电子能谱、拉曼光谱、电子显微镜和分散稳定性观察来分析酸化处理对碳纳米管物理性质和化学性质的影响。结果表明：碳纳米管经过浓硫酸和浓硝酸组合的混酸处理后,羧基被成功地接枝到碳纳米管上,并且随着酸化处理时间的延长在碳纳米管上产生的羧基越来越多,同时随着酸化处理时间的延长其管长逐渐变短,物理结构也逐渐地被一定程度的破坏。碳纳米管经过酸化处理后羧基的产生使其极性增加,使其在极性溶剂中的分散性明显提高。
本文研究的聚氨酯涂料是溶剂型双组分聚氨酯涂料,多异氰酸酯组分采用甲苯-2,4-二异氰酸酯(TDI)和三羟甲基丙烷(TMP)所合成的加成物,多羟基组分采用蓖麻油。在确定此种聚氨酯涂料合成和固化工艺过程的基础上,重点研究和优化了碳纳米管聚氨酯纳米复合涂料的合成和固化工艺过程,并分别采用原位聚合法和共混聚合法制备了纳米复合涂料。
漆膜力学性能方面的研究利用微机控制电子万能试验机、动态力学分析仪和漆膜性能测试方法测试分析了碳纳米管的加入对聚氨酯漆膜力学性能的影响。结果表明：碳纳米管可以有效地提高聚氨酯漆膜的弹性模量、拉伸强度、储能模量、玻璃化转变温度和硬度。但当碳纳米管含量过大时,反而会降低漆膜的弹性模量、拉伸强度、储能模量、玻璃化转变温度和硬度,并且漆膜的弹性模量、拉伸强度、储能模量、玻璃化转变温度和硬度随着碳纳米管酸化处理程度的提高而提高。在其他条件相同情况下,利用原位聚合法制备的漆膜的弹性模量、拉伸强度、储能模量、玻璃化转变温度和硬度要高于利用共混法制备的漆膜的弹性模量、拉伸强度、储能模量、玻璃化转变温度和硬度。同时碳纳米管的加入不会降低聚氨酯漆膜的耐冲击性和柔韧性。
漆膜导电性方面的研究利用数字超高电阻、微电流测量仪测试分析了碳纳米管的加入对聚氨酯漆膜导电性的影响。结果表明：碳纳米管的加入使聚氨酯漆膜的导电性得到了一定程度的提高。随着碳纳米管含量的增加漆膜的体积电阻率降低,当碳纳米管含量为1%时,其体积电阻率降低了2个数量级。并且漆膜的导电性随着碳纳米管酸化处理程度的提高而增强。在其他条件相同情况下,利用原位聚合法制备的漆膜的体积电阻率都低于利用共混法制备的漆膜的体积电阻率
利用全自动色差计测量分析了碳纳米管的加入对聚氨酯漆膜颜色的影响。结果表明：碳纳米管的加入使聚氨酯漆膜的颜色有所加深,随着碳纳米管含量的增加,颜色不断加深,当碳纳米管的含量低于0.1%时,对聚氨酯漆膜颜色的影响不大,含量超过0.1%时,漆膜的颜色变化很大,明显变黑。并且在其他条件相同情况下,漆膜的颜色随碳纳米管酸化处理程度的提高而加深,利用原位聚合法制备的漆膜的颜色比利用共混聚合法制备的漆膜的颜色更深。同时还研究了碳纳米管在聚氨酯漆膜中的分散情况。结果表明：碳纳米管在聚氨酯漆膜中的分散随着碳纳米管酸化处理程度的提高而更加均匀,并且利用原位聚合法制备的漆膜中碳纳米管的分散情况要比利用共混聚合法更理想。
The paper studied the synthesis of carbon nanotubes polyurethane composite coatings and the influence of carbon nanotubes on the properties of polyurethane coatings, the basic groping investigation of carbon nanotubes polyurethane composite coating synthesis procedure and the influence of carbon nanotubes special properties on the elastic modulus, tensile strength, dynamic mechanical properties, harhness, impact resistance, flexibility, electrical conductivity and colour appearance of polyurethane coating were done.
First carbon nanotubes were treated by the mixture of sulphuric acid and nitric acid, the influence of acid treatment on the physical properties and chemical properties of carbon nanotubes were characterised by Fourier tansform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy (Raman), Scanning electron microscopy (SEM) and dispersion stability evaluation. It resulted that, through acid treatment of the mixture of sulphuric acid and nitric acid, carboxylic goups (-COOH) could be successfully introduced onto the surface of carbon nanotubes, and longer acid treatment time afforded a larger number of the carboxylic groups (-COOH) to be attached onto the carbon nanotubes, also after acid treatment the carbon nanotubes became shorter and less well defined in terms of morphology. The polarity of carbon nanotubes was increased by acid treatment due to carboxylic groups (-COOH), and the dispersion stability of carbon nanotubes in polar solvent became better.
The polyurethane coating in the paper was a kind of solvent-thinned two-component polyurethane coating, the iscoyanates component was synthesized by toluene-2,4-diisocyanate (TDI) and trimethylol propane (TMP), and castor oil was used as the hydroxyls component. On the base of synthesis and polymerization procedure of this kind of polyurethane coating, the investigation and optimum of carbon nanotubes polyurethane composite coatings synthesis and polymerization were done mainly, and the nano-composite coatings were synthesized and polymerization via in situ polymerization and blending polyurethane.
About mechanical properties of coatings, tensile tester machine, dynamic mechanical analysis and coating properties evaluation were employed to assess the effects of carbon nanotubes on mechanical properties of polyurethane coatings. It resulted that, the elastic modulus, tensile strength, storage modulus, glass transition temperature and harhness of polyurethane coating could be improved by carbon nanotubes significantly. But if the concentration of carbon nanotubes was too high, the elastic modulus, tensile strength, storage modulus, glass transition temperature and harhness of polyurethane coating would decrease, and the elastic modulus, tensile strength, storage modulus, glass transition temperature and harhness of polyurethane coating increased with the increase of the length time of acid treatment to carbon nanotubes. Under the same other conditions, the elastic modulus, tensile strength, storage modulus, glass transition temperature and harhness of composite coating synthesized via in situ polymerization were better than that synthesized via blending polymerization. Carbon nanotubes would not decrease the impact resistance and flexibility of polyurethane coating.
About electrical conductivity properties of coatings, ohmmeter was employed to assess the effects of carbon nanotubes on electrical conductivity of polyurethane coatings. It resulted that, the electrical conductivity of polyurethane coatings could be improved by carbon nanotubes. The volume resistivity of composite coating decreased with the increasing of carbon nanotubes concentration, and when the concentration of cabon nanotubes was1%, the value of volume resistivity was102order of magnitude lower. The electrical conductivity of composite coatings increased with the increase of the length of time of acid treatment to carbon nanotubes. Under the same other conditions, the volume resistivity of composite coating synthesized via in situ polymerization was lower than that synthesized via blending polymerization.
Spectrophotometer was employed to assess the effects of carbon nanotubes on the colour appearance of polyurethane coatings. It resulted that, the colour depth of polyurethane coatings became deeper by carbon nanotubes, and the colour depth of composite coatings became deeper with the concentration of carbon nanotubes increasing, but when the concentration of carbon nanotubes was lower than0.1%, the carbon nanotubes would not influence the colour appearance significantly, but as the concentration was higher than0.1%, the colour change of composite coating was significantly and tured to black. Under the same other conditions, the colour depth of composite coating became deeper with the increase of the length of time of acid treatment to carbon nanotubes, the colour depth of composite coating synthesized via in situ polymerization was deeper than that synthesized via blending polymerization. Also the dispersion of carbon nanotubes in polyurethane coatings was studied. It result that, the dispersion of carbon nanotubes in polyurethane coatings became better with the increase of the length of time of acid treatment to carbon nanotubes, and the dispersion of carbon nanotubes in composite coating synthesized via in situ polymerization was better than that synthesized via blending polymerization.
引文
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