低温等离子体改性碳材料吸附性能的研究
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摘要
材料作为现代社会经济发展的物质基础和先导，对人类文明的发展起着极其重要的作用，同时也是造成目前环境问题的主要原因之一。开发环境友好型材料，减少环境的污染，恢复被破坏的生态环境，用材料科学与技术来改善生态环境，是历史发展的必然。碳材料化学性能稳定，方便易得，价格低廉，在环境中被广泛用于吸附处理、有机物回收、电化学反应电极材料等。本文从材料的表面改性入手，利用低温等离子体对碳材料的蚀刻与官能团加载，建立利用固相微萃取技术对材料的吸附性能进行快速考察的方法，探索了在水中与电化学结合对水中有机污染物的增强吸附性能。以分布最广的大气和水等典型的环境进行吸附研究，为碳材料改性提供基础数据和理论依据。
在15.7 kV电压下，以空气作为反应气体，采用直流电源电晕放电对石墨材料进行辐照改性。借助扫描电镜、傅里叶红外光谱、元素分析、失重率测定仪等现代分析技术，考察了等离子体对碳材料表面的改性效果，在等离子体改性过程中氧化和蚀刻反应共同进行，相互影响。改性后材料比表面积和孔容积增加，表面出现C=O，OH等新的官能团，失重率有所下降，材料的稳定性提高。证实了电晕放电低温等离子体辐照会改变碳材料表面的物理以及化学性状。
将不同改性碳材料制成固相微萃取的萃取纤维，装备在固相微萃取器上，通过对比不同处理时间的萃取纤维对同种气体样品的吸附评价其吸附性能，建立固相微萃取技术可作为评价材料吸附性能的方法。空气低温等离子体改性3-8 min的碳材料对有机污染物的吸附容量最大；改性后的碳材料对弱极性、中等分子量的有机物(正丁醇，苯)吸附性能提高。在前5 min内对苯系物的吸附大于对醇类的吸附，随着吸附时间的延长，不同物质之间存在竞争吸附。
通过对苯、甲苯、乙苯、二甲苯，以及甲醇、乙醇、异丙醇、正丁醇八种有机物的吸附和脱附实验发现，改性石墨的吸附在前5 min内较快，35 min后吸附达到平衡，脱附在200℃、3 min内可完成，再生方便。改性石墨对极性和非极性物质都有良好的吸附效果；改性石墨纤维使用寿命达400多次，并且可以保持良好的吸附性能。
将改性石墨浸入水中，考察其对水中的极性有机污染物如甲醇、乙醇、异丙醇、正丁醇的吸附性能。水样中的盐含量、温度、pH等对改性材料吸附水中的极性污染物都有一定的影响。改性石墨对水中醇类的吸附在10 min左右达到吸附平衡，比吸附气体中的同样物质更容易达到饱和吸附容量。脱附温度220℃就足够使吸附在纤维表面的醇脱附下来，在240℃下脱附1 min，石墨纤维表面的醇可以完全脱附。
将改性碳材料用于电助吸附水中异丙醇以及2，4-二氯苯酚。物质结构、极化电压对材料的电吸附有不同的影响。对于异丙醇正极化可以促进碳材料对其的吸附，而负电压的加载对吸附有阻碍作用，而电化学对2，4-二氯苯酚的影响则相反。电解质浓度的增加对电吸附有机物有促进作用，但是浓度的继续升高材料对无机离子的吸附也增加，占据部分活性吸附位，阻碍了对有机物的吸附。弱酸性环境下碳材料对对异丙醇和2，4-二氯苯酚的电吸附最显著。
将改性石墨纤维作为固相微萃取的萃取纤维对水中的硝基苯含量进行了分析，探讨了无机盐浓度、pH、水温、吸附时间、脱附温度和脱附时间等参数对样品前处理的影响。吸附的硝基苯利用气相色谱-氢火焰离子检测器进行分析，方法的线性范围在10-1000μg L~(-1)之间，检测限为5μg L~(-1)，是良好的样品前处理技术。
Material as a basis and pilot of the modern socio-economic progress, plays anextremely important role for the development of human civilization. Developingenvironment-friendly materials, reducing environmental pollution, restoring thedamaged ecological environment, and improving the surrounding of people by makinguse of materials science and technology are an inevitable historical advance. Carbonmaterials have the advantages of stable to chemical, easy to gain, low cost, so they arewidely used in environmental fields, such as adsorption process, organic substancesrecycle and electrochemical reactions. This paper started with surface modification ofmaterial, creatively adopted nonthermal plasma to etch and load functional groups,established the methodology of rapid evaluation of carbon materials properties usingsolid-phase microextraction(SPME) method, and explored the combination ofelectrochemistry with adsorption to enhance the adsorption properties of organicpollutants in the water. The adsorption studies were conducted for the most widelydistributed typical pollutants at atmosphere and in water environment, and providedbasic data and theoretical evidence for modification of carbon materials.
The nonthermal plasma was produced by air, under 15.7 kV potential. Thechanges of the materials surface which were treated by the plasma were surveyed usingscanning electron microscopy, Fourier transform infrared spectroscopy, elementalanalysis, thermogravimetric analysis and other modern techniques. The resultsindicated the etching process and oxidation reaction were happened simultaneouslyduring the modifying process. After modification, the surface area and pore volume ofthe carbon material increased, and new functional groups such as C=O, OH wereenriched. Also, the weight loss decreased and stability improved were observed on themodified materials. The fact that the nonthermal plasma was efficient for changing thephysical and chemical characteristics of the material was proved.
The adsorption performance and the selectivity of the material were evaluated by adsorption on same gas with same conditions by different modified carbon materialsand different gases by the same modified carbon material, respectively. It was foundthat the material with treatment of 3 to 8 min by nonthermal plasma has bestadsorption performance to organic pollutants; and the adsorption performance of thecarbon materials for weak polar, middle-molecular weight organic compounds(n-butylalcohol, benzene) is improved after modification. The results also showed that theadsorption speed of benzene is greater than that of alcohols in the first 5 min, and withthe extension of the adsorption time, competition adsorption will happen amongdifferent compounds.
The adsorption of gaseous organic pollutants by modified carbon material wasdeveloped in the research. Through adsorption experiments by adsorption anddesorption of eight organic pollutants, including benzene, toluene, ethylbenzene andxylene, as well as methanol, ethanol, isopropanol and n-butanol on modified carbongraphite, it was found that the modified fiber has rapid adsorption in the first 5 min,and the balance of adsorption is achieved after 35 min; desorption can be finished in 3min at 200℃. Modified graphite has good adsorption performance on both polar andnon-polar substances, and it has good adsorption performance even after 400 timesusage. The modified graphite fiber is suitable for industrial applications.
The adsorption performance of polarity organic pollutants in water wasinvestigated for the modified graphite fiber. It was found that the modified fiber hasvery high adsorption efficiency for methanol, ethanol, isopropanol and n-butanoldissolved in water. The salt content, temperature and the pH values of the watersamples were all have certain impacts on the adsorption of polarity organic pollutantsby modified graphite fiber. It cost 10 min to reach adsorption equilibrium for alcoholsusing modified graphite, and it was easier to reach saturation adsorption capacitycompared with the same conditions in gas sample. The temperature 220℃is enoughto desorb the alcohols absorbed on graphite fiber and 1 min is enough to completedesorption of the alcohols with 240℃.
The methods of electro-assisted adsorption of organic pollutants in water by modified carbon materials were probed. It was found that the different substancestructure and polarization voltage both have different effects on electro-adsorption. Asfor isopropanol, the polarization improved its adsorption, and the negative voltageblocked its adsorption; whereas the electrochemical effects is reversed to theadsorption of 2, 4-dichlorophenol. The inproveing of the of the electrolyte was goodfor the eledtro-adsorption, while high concentration will intrduce more ions adsorbedon the material which was for organic compounds before. The electro-adsorption of thecarbon materil was significantly improved in acid solution for isoproanol and 2, 4-DCP.
The nitrobenzene in the water was sampled by the modified graphite fiber as asolid-phase microextraction fiber. Concentration of inorganic salts, pH, temperature,adsorption time, desorption temperature and desorption time parameters on the impactof pre-treatment samples were discussed. The adsorbed nitrobenzene was analyzed bygas chromatography-flame ionization detector. The linear range of the method wasbetween 10 and 1000μg L~(-1), and the detection limit was 5μg L~(-1), and the approach isshowna good sample preparation method.
在15.7 kV电压下，以空气作为反应气体，采用直流电源电晕放电对石墨材料进行辐照改性。借助扫描电镜、傅里叶红外光谱、元素分析、失重率测定仪等现代分析技术，考察了等离子体对碳材料表面的改性效果，在等离子体改性过程中氧化和蚀刻反应共同进行，相互影响。改性后材料比表面积和孔容积增加，表面出现C=O，OH等新的官能团，失重率有所下降，材料的稳定性提高。证实了电晕放电低温等离子体辐照会改变碳材料表面的物理以及化学性状。
将不同改性碳材料制成固相微萃取的萃取纤维，装备在固相微萃取器上，通过对比不同处理时间的萃取纤维对同种气体样品的吸附评价其吸附性能，建立固相微萃取技术可作为评价材料吸附性能的方法。空气低温等离子体改性3-8 min的碳材料对有机污染物的吸附容量最大；改性后的碳材料对弱极性、中等分子量的有机物(正丁醇，苯)吸附性能提高。在前5 min内对苯系物的吸附大于对醇类的吸附，随着吸附时间的延长，不同物质之间存在竞争吸附。
通过对苯、甲苯、乙苯、二甲苯，以及甲醇、乙醇、异丙醇、正丁醇八种有机物的吸附和脱附实验发现，改性石墨的吸附在前5 min内较快，35 min后吸附达到平衡，脱附在200℃、3 min内可完成，再生方便。改性石墨对极性和非极性物质都有良好的吸附效果；改性石墨纤维使用寿命达400多次，并且可以保持良好的吸附性能。
将改性石墨浸入水中，考察其对水中的极性有机污染物如甲醇、乙醇、异丙醇、正丁醇的吸附性能。水样中的盐含量、温度、pH等对改性材料吸附水中的极性污染物都有一定的影响。改性石墨对水中醇类的吸附在10 min左右达到吸附平衡，比吸附气体中的同样物质更容易达到饱和吸附容量。脱附温度220℃就足够使吸附在纤维表面的醇脱附下来，在240℃下脱附1 min，石墨纤维表面的醇可以完全脱附。
将改性碳材料用于电助吸附水中异丙醇以及2，4-二氯苯酚。物质结构、极化电压对材料的电吸附有不同的影响。对于异丙醇正极化可以促进碳材料对其的吸附，而负电压的加载对吸附有阻碍作用，而电化学对2，4-二氯苯酚的影响则相反。电解质浓度的增加对电吸附有机物有促进作用，但是浓度的继续升高材料对无机离子的吸附也增加，占据部分活性吸附位，阻碍了对有机物的吸附。弱酸性环境下碳材料对对异丙醇和2，4-二氯苯酚的电吸附最显著。
将改性石墨纤维作为固相微萃取的萃取纤维对水中的硝基苯含量进行了分析，探讨了无机盐浓度、pH、水温、吸附时间、脱附温度和脱附时间等参数对样品前处理的影响。吸附的硝基苯利用气相色谱-氢火焰离子检测器进行分析，方法的线性范围在10-1000μg L~(-1)之间，检测限为5μg L~(-1)，是良好的样品前处理技术。
Material as a basis and pilot of the modern socio-economic progress, plays anextremely important role for the development of human civilization. Developingenvironment-friendly materials, reducing environmental pollution, restoring thedamaged ecological environment, and improving the surrounding of people by makinguse of materials science and technology are an inevitable historical advance. Carbonmaterials have the advantages of stable to chemical, easy to gain, low cost, so they arewidely used in environmental fields, such as adsorption process, organic substancesrecycle and electrochemical reactions. This paper started with surface modification ofmaterial, creatively adopted nonthermal plasma to etch and load functional groups,established the methodology of rapid evaluation of carbon materials properties usingsolid-phase microextraction(SPME) method, and explored the combination ofelectrochemistry with adsorption to enhance the adsorption properties of organicpollutants in the water. The adsorption studies were conducted for the most widelydistributed typical pollutants at atmosphere and in water environment, and providedbasic data and theoretical evidence for modification of carbon materials.
The nonthermal plasma was produced by air, under 15.7 kV potential. Thechanges of the materials surface which were treated by the plasma were surveyed usingscanning electron microscopy, Fourier transform infrared spectroscopy, elementalanalysis, thermogravimetric analysis and other modern techniques. The resultsindicated the etching process and oxidation reaction were happened simultaneouslyduring the modifying process. After modification, the surface area and pore volume ofthe carbon material increased, and new functional groups such as C=O, OH wereenriched. Also, the weight loss decreased and stability improved were observed on themodified materials. The fact that the nonthermal plasma was efficient for changing thephysical and chemical characteristics of the material was proved.
The adsorption performance and the selectivity of the material were evaluated by adsorption on same gas with same conditions by different modified carbon materialsand different gases by the same modified carbon material, respectively. It was foundthat the material with treatment of 3 to 8 min by nonthermal plasma has bestadsorption performance to organic pollutants; and the adsorption performance of thecarbon materials for weak polar, middle-molecular weight organic compounds(n-butylalcohol, benzene) is improved after modification. The results also showed that theadsorption speed of benzene is greater than that of alcohols in the first 5 min, and withthe extension of the adsorption time, competition adsorption will happen amongdifferent compounds.
The adsorption of gaseous organic pollutants by modified carbon material wasdeveloped in the research. Through adsorption experiments by adsorption anddesorption of eight organic pollutants, including benzene, toluene, ethylbenzene andxylene, as well as methanol, ethanol, isopropanol and n-butanol on modified carbongraphite, it was found that the modified fiber has rapid adsorption in the first 5 min,and the balance of adsorption is achieved after 35 min; desorption can be finished in 3min at 200℃. Modified graphite has good adsorption performance on both polar andnon-polar substances, and it has good adsorption performance even after 400 timesusage. The modified graphite fiber is suitable for industrial applications.
The adsorption performance of polarity organic pollutants in water wasinvestigated for the modified graphite fiber. It was found that the modified fiber hasvery high adsorption efficiency for methanol, ethanol, isopropanol and n-butanoldissolved in water. The salt content, temperature and the pH values of the watersamples were all have certain impacts on the adsorption of polarity organic pollutantsby modified graphite fiber. It cost 10 min to reach adsorption equilibrium for alcoholsusing modified graphite, and it was easier to reach saturation adsorption capacitycompared with the same conditions in gas sample. The temperature 220℃is enoughto desorb the alcohols absorbed on graphite fiber and 1 min is enough to completedesorption of the alcohols with 240℃.
The methods of electro-assisted adsorption of organic pollutants in water by modified carbon materials were probed. It was found that the different substancestructure and polarization voltage both have different effects on electro-adsorption. Asfor isopropanol, the polarization improved its adsorption, and the negative voltageblocked its adsorption; whereas the electrochemical effects is reversed to theadsorption of 2, 4-dichlorophenol. The inproveing of the of the electrolyte was goodfor the eledtro-adsorption, while high concentration will intrduce more ions adsorbedon the material which was for organic compounds before. The electro-adsorption of thecarbon materil was significantly improved in acid solution for isoproanol and 2, 4-DCP.
The nitrobenzene in the water was sampled by the modified graphite fiber as asolid-phase microextraction fiber. Concentration of inorganic salts, pH, temperature,adsorption time, desorption temperature and desorption time parameters on the impactof pre-treatment samples were discussed. The adsorbed nitrobenzene was analyzed bygas chromatography-flame ionization detector. The linear range of the method wasbetween 10 and 1000μg L~(-1), and the detection limit was 5μg L~(-1), and the approach isshowna good sample preparation method.
引文
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