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空心碳材料的合成与气体吸附性能研究
论文作者:童鞋论文网  论文来源:www.txlunwenw.com  发布时间:2019/10/24 9:24:17  

摘要:本文以酚醛树脂为碳源,以正硅酸四乙/丙酯为硅源,通过共聚合反应将碳源涂覆二氧化硅。经过在惰性气体下高温碳化,酸刻蚀,活化等条件合成了具有可控空腔和长径比的空心碳材料。文中详细介绍了空心氮掺杂碳纳米管和空心碳纳米球的合成过程,使用透射电镜(TEM)、红外、热重(TGA)、氮气吸-脱附、X射线粉末衍射仪(XRD)、X射线光电子能谱分析(XPS)等表征手段对样品进行分析,利用BJH模型、DR方程和非定域密度函数理论(NLDFT)等计算分析所制备碳材料的孔结构,并通过二氧化碳等温吸附曲线和静/动态吸附实验考察不同样品的气体吸附应用性能。具体研究内容如下:

1. 首先在反胶束体系中生成镍肼@二氧化硅复合纳米棒,通过共缩合作用涂覆3-氨基酚甲醛树脂(APF)为碳源、氮源,经过氢氟酸刻蚀除去模板和杂质,合成出具有清晰管状结构和长径比的空心氮掺杂碳纳米管材料。通过调整浓度配比、碳化温度、碳/氮源的负载总量来改变模板的形状与结构。实验结果表明,加入1.9 mL氯化镍的条件下可以合成出具有最大长径比的管状结构,在负载适当质量的APF经700 °C碳化得到的空心氮掺杂碳纳米管样品拥有高比表面积和良好的吸附二氧化碳的能力,其吸附效果优于商业化的活性炭(AC)。

2. 以空心氮掺杂碳纳米管材料为原材料,使用NaOH、Na2CO3、KOH和K2CO3作为活化剂,经过再一次的高温煅烧后得到具有大比表面积、大孔体积和丰富微孔的改性空心氮掺杂碳纳米管材料。通过对样品的结构分析发现,对于同一空心氮掺杂碳纳米管材料,使用不同活化剂具有不同的活化效果。实验结果表明1:1的质量比例混合的K2CO3与空心氮掺杂碳纳米管为最佳活化条件,所制备的样品ANCT-1.0在1 bar压力与0°C和25 °C温度下,二氧化碳吸附量分别可达4.5 mmolg-1和3.17 mmol g-1。在6次的重复吸附-脱附实验后,仍可保持高达98%的吸附容量,具备良好的稳定性和吸附应用潜力。

3. 利用一步法、不使用表面活性剂,在氨水和乙醇体系中以两种硅源-正硅酸四乙酯(TEOS)和正硅酸四丙酯(TPOS)自缩合反应生成初级二氧化硅球形颗粒作为模板,以间苯二酚与甲醛缩合反应生成的酚醛树脂为碳源,利用酚醛树脂与二氧化硅表面羟基共缩合进行涂覆,经过高温碳化和酸刻蚀之后制备得到空心碳纳米球(HCNS)。通过调节TEOS/ TPOS摩尔比以调节原位产生的二氧化硅颗粒和聚合物低聚体之间的共缩合过程,合成具有粒径和壁厚可调、单分散性良好的空心碳纳米球,粒径280-420 nm,壁厚15-63 nm。以TEOS/ TPOS摩尔比为0/4合成的空心碳纳米球,具有大粒径(426 nm)、高比表面积(1216 m2 g-1)和高孔体积(0.51 cm3 g-1)。静/动态吸附实验结果表明,HCNS的VOC吸附能力远高于商业化AC。

In this paper, phenolic resin was used ascarbon source and tetraethyl orthosilicate / propyl orthosilicate as siliconsource. Hollow carbon materials with controllable cavity and aspect ratio weresynthesized by high temperature carbonation, acid etching and activation underthe condition of noble gas. In this paper, the synthesis process of hollownitrogen-doped carbon nanotubes and hollow carbon nanoparticles is introducedin detail. The samples were analyzed by Transmission electron microscope (TEM),infrared, thermogravimetric (TGA), nitrogen adsorption and desorption, X-raypowder diffractometer (XRD), X-ray photoelectron spectroscopy (XPS). The porestructures of the prepared carbon materials were calculated and analyzed by BJHmodel, DR equation and non-local density function theory (NLDFT). The gasadsorption properties of different samples were investigated by carbon dioxideisotherm adsorption curve and static / dynamic adsorption experiments. Thespecific contents of the study are as follows:

1. Firstly, a nickel-(NH2)2@SiO2 compositenanorod were formed in the reverse micelle system. 3-aminophenol formaldehyderesin (APF) is coated by co-condensation as carbon and nitrogen source, and thetemplate is removed by hydrofluoric acid etching. Hollow nitrogen-doped carbonnanotube materials with clear tubular structure and a long aspect ratio aresynthesized. The shape and structure of the hollow nitrogen-doped carbonnanotube materials is changed by adjusting the volume of NiCl2 solution (0.8mol L-1), carbonization temperature, and the total amount of carbon/nitrogensource loaded. The experimental results show that the hollow nitrogen-doped carbonnanotube with the largest aspect ratio can be synthesized by adding 1.9 mL ofnickel chloride. The hollow nitrogen-doped carbon nanotube samples obtained bycarbonization at 700 °C with the appropriate mass of APF has the largest aspectratio. The surface area and the best carbon dioxide adsorption effect aresuperior to commercial activated carbon (AC).

2. Using hollow nitrogen-doped carbonnanotube materials as raw materials, using NaOH, Na2CO3, KOH and K2CO3 asactivators, after further high-temperature calcination, modified hollownitrogen-doped carbon nanotube materials with larger specific surface area,larger pore volume and richer micropores are obtained. Through structuralanalysis of the sample, it can be found that different activators have differentactivation effects for the same hollow nitrogen-doped carbon nanotube. Theoptimal activation conditions were the mass ratio of K2CO3 and hollow nitrogendoped carbon nanotubes at 1:1 at 700 oC (ANCT-1.0). At 1 bar pressure and 0 °Cand 25 °C temperatures, the carbon dioxide adsorption capacity of ANCT-1.0 canreach 4.5 mmol g-1 and 3.17 mmol g-1, respectively. After 6 repeatedadsorption-desorption experiments, carbon dioxide adsorption capacity can stillmaintain up to 98%. The synthesized ANCTs have good stability and adsorptionapplication potential.

3. The composites of phenolic resin-silicawere obtained in one-step, without using surfactant, in which tetraethylorthosilicate (TEOS) and tetrapropyl orthosilicate (TPOS) were used to formprimary silica spherical particles as a template, and the phenolic resin(resorcinol and formaldehyde) was co-condensed with the hydroxyl groups ofsilica. Hollow carbon nanosphere (HCNS) were obtained after high temperaturecarbonization of phenolic resin-silica composites and acid etching. By varyingthe molar ratio TEOS/TPOS, hollow carbon nanospheres with good monodispersityand adjustable particle size and wall thickness were obtained. The particlesize and wall thickness are in the range of 280-420 nm and 15-63 nm,respectively. The hollow carbon nanospheres synthesized by only TPOS have largeparticle size(426 nm), surfacearea (1216 m2 g-1)and porevolume(0.51 cm3 g-1) with thelargest VOCs adsorption capacities.

关键词:空心碳材料;微孔;CO2吸附;VOCs吸附;稳定性

Hollow carbon material;Micropore; CO2 adsorption;VOCs adsorption ;Stability

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