修饰纳米SiO_2的表面功能团测定及在尼龙6中的应用
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摘要
γ-氨丙基三乙氧基硅烷(APS)表面修饰的纳米二氧化硅(AMNS)和γ-(2,3-环氧丙氧基)丙基三甲氧基硅烷(GPS)表面修饰的纳米二氧化硅(GMNS)作为催化剂和新材料在生命科学、分析化学、光学等领域具有广阔的应用前景。目前其相关的制备技术研究正步入全面的工艺完善阶段,应用研究也已经开始受到关注。然而,目前针对AMNS和GMNS的应用研究大多还处于经验探索阶段,其主要原因是对AMNS和GMNS表面的功能团(即氨基和环氧基)的存在浓度及形态缺乏了解,其中功能团的浓度影响是最主要的因素。另外,针对AMNS的应用开发研究亟需进行。据此,本论文主要从三个方面开展相关研究:
一、AMNS表面氨基浓度的测定
分别建立了盐酸-乙醇非水滴定法、高氯酸-冰乙酸非水滴定法、分光光度法、循环伏安法(对氨基苯甲酸化学修饰电极法)和凯氏定氮法等测定AMNS表面氨基浓度的方法;系统地研究了各种实验条件对测定结果的影响,探讨了影响测定结果准确度的主要因素;讨论了不同分析方法的优缺点以及导致其测量结果出现差异的主要原因;为该类纳米材料的合成和应用研究建立了分析测试平台。结果表明:所建立的各种分析方法均能用于对AMNS表面氨基进行比较准确的测定。在两种滴定分析法中,在滴定终点附近对样品进行超声振荡处理,有利于缩短滴定过程;在高氯酸-冰乙酸非水滴定法中加入异辛醇作为分散剂,可以改善体系的互溶性,降低体系的冰点,拓宽体系的应用范围;分光光度法灵敏度高,pH值是影响其测定结果的重要因素;化学修饰电极法较好地避免了纳米颗粒的吸附和光反射等对测定结果的影响,使测定结果更加准确;凯氏定氮法相应的测量结果较高,其原因在于采用凯氏定氮法测定的是AMNS中的总氮,而采用其他分析方法测定的是AMNS中氨基氮。
二、GMNS表面环氧基浓度的测定
分别建立了盐酸-丁酮滴定法、高氯酸-冰乙酸非水滴定法、紫外分光光度法、荧光分光光度法、示波极谱法和电位滴定分析法(聚对硝基苯胺化学修饰电极法)等测定GPS的浓度及GMNS表面环氧基浓度的方法。详细研究了各种实验条件对测定结果的影响及影响测定结果准确度的主要因素,分析了不同分析方法的特点和使用范围,为该类纳米材料的合成和应用研究建立了分析测试平台。研究结果表明:利用所建立的各种分析方法均能实现对GMNS表面环氧基官能团浓度的准确分析,且不同分析方法所得到的测定结果无明显差异。盐酸-丁酮滴定法、高氯酸-冰乙酸非水滴定法中准确确定终点指示剂颜色的变化是保证分析准确性的最主要因素;紫外分光光度法、荧光分光光度法灵敏度较高;示波极谱法避开了纳米粒子的干扰,测定结果的准确性和重现性较高;电位滴定法在盐酸-丁酮法的基础上,以聚对硝基苯胺修饰电极指示终点,可有效地提高测定结果的准确性。
三、AMNS/尼龙6复合材料的结构和性能研究
在准确测定AMNS表面氨基的基础上,分析了熔融共混法制备的AMNS/尼龙6纳米复合材料的结构;建立了不同氨基浓度的AMNS与尼龙6基体界面相互作用的模型;提出了临界氨基浓度概念,确定了在尼龙6中添加AMNS的最佳浓度;探讨了AMNS表面氨基浓度对AMNS/尼龙6纳米复合材料机械性能的影响。探索出了从纳米填充材料表面功能团的浓度去研究其对纳米复合材料性能影响的新途径。
结果表明:①AMNS表面的有机官能团能够与尼龙6基体发生反应,形成一种基于共价键和氢键连接的界面层结构;当AMNS表面氨基浓度达到某一临界值时,AMNS颗粒与尼龙6基体之间的相互作用最强,有利于实现复合材料的性能优化。②引入表面含不同浓度氨基的AMNS纳米颗粒都可以提高尼龙6的力学性能;当AMNS颗粒表面氨基浓度为2.86mmol·g-1时,复合材料的综合力学性能最佳,其拉伸强度、拉伸模量、弯曲强度、弯曲模量和缺口冲击强度分别提高了19.02%、47.16%、27.11%、38.69%、17.11%。③引入不同氨基浓度的AMNS均使得尼龙6的热稳定性能得到提高,并且复合材料的热稳定性能随着AMNS中氨基浓度的增加而提高;与尼龙6相比,在热重分析中复合材料发生10%失重时的温度随AMNS中氨基浓度的增加而提高6～10℃。④引入表面氨基浓度较高的AMNS作为添加剂有利于促进复合材料中尼龙6基体沿(002)/(202)面的生长;复合材料的结晶温度随着AMNS表面氨基浓度的增加而降低,但尼龙6基体的晶体结构基本保持不变。
As a kind of catalyst and novel functional materials, surface-modified nanosilica withγ-aminopropyltriethoxysilane (APS) andγ-glycidoxypropyltrimethoxysilane (GPS), coded as AMNS and GMNS, have been widely applied in the fields of life science, analytical chemistry and optics etc. At present, focus is being placed on modifying and integrating processes in terms of the preparation technology for AMNS and GMNS. And researches on the application of AMNS and GMNS are also begining to attract attention. However, current studies in relation to the applications of AMNS and GMNS are largely limited to exploration of experiences in labs, mainly due to insufficient understanding of the states and concentrations of the functional groups (i.e., amino and epoxy groups) on the surface of AMNS and GMNS, where the concentrations of the functional groups play a more critical role on the application. Besides, efforts are urgently needed to promote the application and development of AMNS in engineering. Therefore, the following three parts of research are to be highlighted in this dissertation:
Part I: Determination of Amino Concentration on AMNS
Methods such as hydrochloric acid-ethanol non-aqueous titration, perchloric acid-acetic acid non-aqueous titration, spectrophotometry and cyclic voltammetry (using glassy carbon electrode modified with p-aminobenzoic acid) were established for determining amino group on AMNS. The effects of various experimental conditions on the results of measurement were studied in detail. The main factors that affect the accuracy of measurement were investigated. The advantages and disadvantages of each method are discussed, and the main causes leading to differences from the measurement results by various methods are explored. Based on the above-mentioned studies, the analysis and test platforms have been established in relation to the synthesis and application of this type of nanomaterials. Results indicate that all the proposed methods could be well used to determine the amino concentration on AMNS with a good accuracy. For the both titration methods, treating the samples with ultrasonic vibration near the end point is favorable to shortening the titration process. For the perchloric acid-acetic acid method, the addition of 2-ethylhexanol as a dispersant could improve the inter-solubility of the titration system and decrease the system’s freezing point, leading to broadening the application scope of the method. For spectrophotometry method, it was of great sensitivity, and pH value had the most important role in affecting the results of measurement. In terms of the cyclic voltammetry, the effects of the adsorption of indicator by nanoparticles and the light reflectance by the nanoparticles were eliminated, helping to reaching good accuracy. Besides, higher the results of measurement was obtained along with Kjeldahl Method, mainly because Kjeldahl Method was used to determine the total nitrogen in AMNS while the other methods were applied to determine only amino nitrogen in AMNS.
Part II: Determination of Epoxy Concentration on GMNS
Various methods including non-aqueous titration with hydrochloric acid-butanone and perchloric acid-acetic acid, ultraviolet (UV) and fluorescence spectrophotometry, osciliopolarography and potential titration (using an electrode chemically modified with poly(p-nitro aniline)) were established to determine the content of GPS and the concentration of epoxy group on GMNS. The influences of various experimental conditions on the measurement results and the major factors significantly affecting the accuracy of measurement were investigated in detail. The characteristics of each method and its applicable scopes were discussed. And the analysis and test platforms in relation to the synthesis and application on this kind of nanomaterials were established. Results indicate that every established method could be well used to determine epoxy on GMNS accurately, showing insignificant difference in terms of the measurement results. For non-aqueous titration with hydrochloric acid-butanone and perchloric acid-acetic acid, the confirmation of the end point was the key factor to guarantee the accuracy of measurement. UV and fluorescence spectrophotometry methods had good sensitivity. Osciliopolarography method, without the interference by nanoparticles, had better accuracy and reproducibility than the other methods. Besides, potential titration, based on hydrochloric acid-butanone method and using an electrode modified with poly(p-nitro aniline) as the indicator electrode, had effectively increased accuracy.
Part III: Structure and Properties of AMNS/Nylon 6 Composites
Based on the accurate determination of amino group on AMNS, the structures of AMNS/nylon 6 nanocomposites prepared by melt blending were analyzed. A model was established to illustrate the interfacial interactions between AMNS with different concentrations of amino group and nylon 6 matrixes. A concept of critical concentration of amino group was put forward. The optimized concentration of AMNS added in nylon 6 matrixes was determined. And the effect of amino group concentration of AMNS on the mechanical properties of AMNS/nylon 6 nanocomposites was explored. Results are obtained as follows:
①The amino groups on AMNS surface reacted with the end carboxyl groups and acylamino groups of nylon 6, forming interfacial structures based on hydrogen bonding and covalent bonding. There might exist an optimum concentration of the functional groups in AMNS, at which maximum interfacial interactions between nanosilica as the filler and nylon 6 matrix would be realized, hence acquiring effectively improved mechanical properties of the filled nylon 6 composites.
②The introduction of AMNS resulted in improvement of the mechanical properties of nylon 6. When the amino concentration was 2.86 mmol·g-1, the tensile strength, tensile modulous, flexural strength, flexural modulus, and notched impact strength of the nanocomposite were increased by 19.02%, 47.16%, 27.11%, 38.69%, and 17.11%, respectively, as compared with that of nylon 6 matrix.
③The thermal stability of nylon 6 increased with the increase of amino concentration of AMNS. Compared with nylon 6, the temperature at which AMNS/nylon 6 composites showed weight loss of 10% was increased by 6~10 oC as compared with the nylon 6 matrix.
④Increasing the amino concentration on AMNS favored the growth of nylon 6 along the (002)/(202) planes. The crystallization temperature of the nanocomposites decreased with the increase of amino concentration on AMNS, while the crystallinity of nylon 6 matrix kept also unchanged.
一、AMNS表面氨基浓度的测定
分别建立了盐酸-乙醇非水滴定法、高氯酸-冰乙酸非水滴定法、分光光度法、循环伏安法(对氨基苯甲酸化学修饰电极法)和凯氏定氮法等测定AMNS表面氨基浓度的方法;系统地研究了各种实验条件对测定结果的影响,探讨了影响测定结果准确度的主要因素;讨论了不同分析方法的优缺点以及导致其测量结果出现差异的主要原因;为该类纳米材料的合成和应用研究建立了分析测试平台。结果表明:所建立的各种分析方法均能用于对AMNS表面氨基进行比较准确的测定。在两种滴定分析法中,在滴定终点附近对样品进行超声振荡处理,有利于缩短滴定过程;在高氯酸-冰乙酸非水滴定法中加入异辛醇作为分散剂,可以改善体系的互溶性,降低体系的冰点,拓宽体系的应用范围;分光光度法灵敏度高,pH值是影响其测定结果的重要因素;化学修饰电极法较好地避免了纳米颗粒的吸附和光反射等对测定结果的影响,使测定结果更加准确;凯氏定氮法相应的测量结果较高,其原因在于采用凯氏定氮法测定的是AMNS中的总氮,而采用其他分析方法测定的是AMNS中氨基氮。
二、GMNS表面环氧基浓度的测定
分别建立了盐酸-丁酮滴定法、高氯酸-冰乙酸非水滴定法、紫外分光光度法、荧光分光光度法、示波极谱法和电位滴定分析法(聚对硝基苯胺化学修饰电极法)等测定GPS的浓度及GMNS表面环氧基浓度的方法。详细研究了各种实验条件对测定结果的影响及影响测定结果准确度的主要因素,分析了不同分析方法的特点和使用范围,为该类纳米材料的合成和应用研究建立了分析测试平台。研究结果表明:利用所建立的各种分析方法均能实现对GMNS表面环氧基官能团浓度的准确分析,且不同分析方法所得到的测定结果无明显差异。盐酸-丁酮滴定法、高氯酸-冰乙酸非水滴定法中准确确定终点指示剂颜色的变化是保证分析准确性的最主要因素;紫外分光光度法、荧光分光光度法灵敏度较高;示波极谱法避开了纳米粒子的干扰,测定结果的准确性和重现性较高;电位滴定法在盐酸-丁酮法的基础上,以聚对硝基苯胺修饰电极指示终点,可有效地提高测定结果的准确性。
三、AMNS/尼龙6复合材料的结构和性能研究
在准确测定AMNS表面氨基的基础上,分析了熔融共混法制备的AMNS/尼龙6纳米复合材料的结构;建立了不同氨基浓度的AMNS与尼龙6基体界面相互作用的模型;提出了临界氨基浓度概念,确定了在尼龙6中添加AMNS的最佳浓度;探讨了AMNS表面氨基浓度对AMNS/尼龙6纳米复合材料机械性能的影响。探索出了从纳米填充材料表面功能团的浓度去研究其对纳米复合材料性能影响的新途径。
结果表明:①AMNS表面的有机官能团能够与尼龙6基体发生反应,形成一种基于共价键和氢键连接的界面层结构;当AMNS表面氨基浓度达到某一临界值时,AMNS颗粒与尼龙6基体之间的相互作用最强,有利于实现复合材料的性能优化。②引入表面含不同浓度氨基的AMNS纳米颗粒都可以提高尼龙6的力学性能;当AMNS颗粒表面氨基浓度为2.86mmol·g-1时,复合材料的综合力学性能最佳,其拉伸强度、拉伸模量、弯曲强度、弯曲模量和缺口冲击强度分别提高了19.02%、47.16%、27.11%、38.69%、17.11%。③引入不同氨基浓度的AMNS均使得尼龙6的热稳定性能得到提高,并且复合材料的热稳定性能随着AMNS中氨基浓度的增加而提高;与尼龙6相比,在热重分析中复合材料发生10%失重时的温度随AMNS中氨基浓度的增加而提高6～10℃。④引入表面氨基浓度较高的AMNS作为添加剂有利于促进复合材料中尼龙6基体沿(002)/(202)面的生长;复合材料的结晶温度随着AMNS表面氨基浓度的增加而降低,但尼龙6基体的晶体结构基本保持不变。
As a kind of catalyst and novel functional materials, surface-modified nanosilica withγ-aminopropyltriethoxysilane (APS) andγ-glycidoxypropyltrimethoxysilane (GPS), coded as AMNS and GMNS, have been widely applied in the fields of life science, analytical chemistry and optics etc. At present, focus is being placed on modifying and integrating processes in terms of the preparation technology for AMNS and GMNS. And researches on the application of AMNS and GMNS are also begining to attract attention. However, current studies in relation to the applications of AMNS and GMNS are largely limited to exploration of experiences in labs, mainly due to insufficient understanding of the states and concentrations of the functional groups (i.e., amino and epoxy groups) on the surface of AMNS and GMNS, where the concentrations of the functional groups play a more critical role on the application. Besides, efforts are urgently needed to promote the application and development of AMNS in engineering. Therefore, the following three parts of research are to be highlighted in this dissertation:
Part I: Determination of Amino Concentration on AMNS
Methods such as hydrochloric acid-ethanol non-aqueous titration, perchloric acid-acetic acid non-aqueous titration, spectrophotometry and cyclic voltammetry (using glassy carbon electrode modified with p-aminobenzoic acid) were established for determining amino group on AMNS. The effects of various experimental conditions on the results of measurement were studied in detail. The main factors that affect the accuracy of measurement were investigated. The advantages and disadvantages of each method are discussed, and the main causes leading to differences from the measurement results by various methods are explored. Based on the above-mentioned studies, the analysis and test platforms have been established in relation to the synthesis and application of this type of nanomaterials. Results indicate that all the proposed methods could be well used to determine the amino concentration on AMNS with a good accuracy. For the both titration methods, treating the samples with ultrasonic vibration near the end point is favorable to shortening the titration process. For the perchloric acid-acetic acid method, the addition of 2-ethylhexanol as a dispersant could improve the inter-solubility of the titration system and decrease the system’s freezing point, leading to broadening the application scope of the method. For spectrophotometry method, it was of great sensitivity, and pH value had the most important role in affecting the results of measurement. In terms of the cyclic voltammetry, the effects of the adsorption of indicator by nanoparticles and the light reflectance by the nanoparticles were eliminated, helping to reaching good accuracy. Besides, higher the results of measurement was obtained along with Kjeldahl Method, mainly because Kjeldahl Method was used to determine the total nitrogen in AMNS while the other methods were applied to determine only amino nitrogen in AMNS.
Part II: Determination of Epoxy Concentration on GMNS
Various methods including non-aqueous titration with hydrochloric acid-butanone and perchloric acid-acetic acid, ultraviolet (UV) and fluorescence spectrophotometry, osciliopolarography and potential titration (using an electrode chemically modified with poly(p-nitro aniline)) were established to determine the content of GPS and the concentration of epoxy group on GMNS. The influences of various experimental conditions on the measurement results and the major factors significantly affecting the accuracy of measurement were investigated in detail. The characteristics of each method and its applicable scopes were discussed. And the analysis and test platforms in relation to the synthesis and application on this kind of nanomaterials were established. Results indicate that every established method could be well used to determine epoxy on GMNS accurately, showing insignificant difference in terms of the measurement results. For non-aqueous titration with hydrochloric acid-butanone and perchloric acid-acetic acid, the confirmation of the end point was the key factor to guarantee the accuracy of measurement. UV and fluorescence spectrophotometry methods had good sensitivity. Osciliopolarography method, without the interference by nanoparticles, had better accuracy and reproducibility than the other methods. Besides, potential titration, based on hydrochloric acid-butanone method and using an electrode modified with poly(p-nitro aniline) as the indicator electrode, had effectively increased accuracy.
Part III: Structure and Properties of AMNS/Nylon 6 Composites
Based on the accurate determination of amino group on AMNS, the structures of AMNS/nylon 6 nanocomposites prepared by melt blending were analyzed. A model was established to illustrate the interfacial interactions between AMNS with different concentrations of amino group and nylon 6 matrixes. A concept of critical concentration of amino group was put forward. The optimized concentration of AMNS added in nylon 6 matrixes was determined. And the effect of amino group concentration of AMNS on the mechanical properties of AMNS/nylon 6 nanocomposites was explored. Results are obtained as follows:
①The amino groups on AMNS surface reacted with the end carboxyl groups and acylamino groups of nylon 6, forming interfacial structures based on hydrogen bonding and covalent bonding. There might exist an optimum concentration of the functional groups in AMNS, at which maximum interfacial interactions between nanosilica as the filler and nylon 6 matrix would be realized, hence acquiring effectively improved mechanical properties of the filled nylon 6 composites.
②The introduction of AMNS resulted in improvement of the mechanical properties of nylon 6. When the amino concentration was 2.86 mmol·g-1, the tensile strength, tensile modulous, flexural strength, flexural modulus, and notched impact strength of the nanocomposite were increased by 19.02%, 47.16%, 27.11%, 38.69%, and 17.11%, respectively, as compared with that of nylon 6 matrix.
③The thermal stability of nylon 6 increased with the increase of amino concentration of AMNS. Compared with nylon 6, the temperature at which AMNS/nylon 6 composites showed weight loss of 10% was increased by 6~10 oC as compared with the nylon 6 matrix.
④Increasing the amino concentration on AMNS favored the growth of nylon 6 along the (002)/(202) planes. The crystallization temperature of the nanocomposites decreased with the increase of amino concentration on AMNS, while the crystallinity of nylon 6 matrix kept also unchanged.
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