高比表面积三维有序大孔炭材料的合成与表征

将粒径为540nm的SiO2胶体微球通过自然沉积组装为胶体晶体模板,以葡萄糖的水溶液为前体填充模板间隙,高温炭化后,以HF溶液溶去模板,得到三维有序大孔炭材料。根据SEM检测,大孔以六方有序的方式排列,其孔径及孔径收缩率分别为510nm和5.6%。大孔之间由小窗口连通,构成内部三维交联的大孔网络。低温N2吸附测试表明,大孔孔壁上存在2～10nm为主的中孔孔隙,同时由于前体的表面复制作用,使样品BET比表面积达到948m2/g。XRD表征显示,所制备的3DOM材料由无序石墨结构的炭质组成。     

Preparation and characterization of nitrogen-doped mesoporous titania with high specific surface area

Nitrogen-doped mesoporous titania aerogel photocatalysts were prepared by supercritical drying technique with carbon dioxide (SCCO₂) and calcination the urea impregnated TiO₂ aerogel at 773 K under NH₃ or N₂ + NH₃aq gaseous atmosphere. The pore properties were investigated from nitrogen adsorption measurement at 77 K. The prepared N-doped TiO₂ aerogel had a high specific surface area (116 m²/g), a total pore volume (0.33 cm³/g) and a sharp pore radius distribution (r_peak = 4.2 nm). The doping of the nitrogen atom into the TiO₂ lattice is expected from X-ray photoelectron spectroscopy (XPS), X-ray powder diffraction (XRD), and UV–Vis spectroscopy. Nitrogen states in the lattice and crystalline structure were measured using X-ray photoelectron spectroscopy and X-ray diffractometry. The N-doped TiO₂ aerogel absorbed well into the visible region up to 600 nm.     

Soft-template synthesis of ordered mesoporous carbon/nanoparticle nickel composites with a high surface area

Ordered mesoporous carbon/nanoparticle nickel composites have been synthesized via multi-component co-assembly strategy associated with a direct carbonization process from resol, tetraethyl orthosilicate, Ni(NO₃)₂·6H₂O and triblock copolymer F127 and subsequent silicates removal with NaOH solution. The incorporation of rigid silicates in the pore walls can reduce framework shrinkage significantly during the pyrolysis process, creating large mesopores. Moreover, plenty of complementary small pores caused by silica removal are observed in the carbon pore walls, which contribute to the large surface area. The mesoporous carbon/nanoparticle nickel composites with a low Ni content (1.7 wt%) possess ordered two-dimensional hexagonal structure, large mesopores (6.8 nm), high surface area (1580 m² g⁻¹) and large pore volume (1.42 cm³ g⁻¹). Magnetic Ni nanocrystals with particle size of ∼16.0 nm are confined in the matrix of carbon frameworks. With increase of Ni content, the surface area and pore volume of the composites decrease. The particle size of metallic Ni nanocrystals increases up to 20.3 nm, when its content increases to 10 wt%. These carbon/nanoparticle nickel composites with high surface area, large pore size and superparamagnetic property show excellent adsorption properties for bulky dye fuchsin base and an easy separation procedure.     

高比表面积介孔碳材料的混合模板法制备

以纳米氧化锌和氧化镁为混合模板剂,以氢氧化钾为活化剂,中温煤沥青为碳源,经热处理、酸洗、干燥制备出介孔碳材料。通过X射线衍射分析介孔碳材料制备过程中组分的变化情况,通过扫描电子显微镜观察介孔碳材料的表面形貌,通过氮气吸脱附等温线对所得的介孔碳材料进行表征。结果表明,随着温度的升高,由于体系内反应越来越剧烈,体系内呈现碎片状,因而所得的介孔碳材料比表面积逐渐增大;随着模板剂含量的增加,酸洗后的介孔碳材料由于孔的联结而使所得介孔碳材料的比表面积逐渐减小,平均孔径逐渐增大。所得介孔碳材料比表面积最大为2 509.76 m²/g。     

高比表面磁性有序介孔炭的合成及对亚甲基蓝的吸附性能

具有高比表面积、大孔容的铁磁性有序介孔炭(Fe/OMCs)对含染料废水的处理提供了一种简单有效的方法。采用苯酚树脂作炭源,三嵌段共聚物F127为模板剂,正硅酸乙酯为硅前驱体,硝酸铁为磁源,通过软模路线合成了Fe/OMCs。利用X射线衍射仪(XRD),氮气吸附仪,透射电镜(TEM)和综合物性测试仪研究了硝酸铁加入量对Fe/OMCs的相态、孔结构参数和磁性的影响;并以亚甲基蓝(MB)为染料探针分子,研究了Fe/OMCs对MB的吸附行为。结果表明材料有序性、比表面和孔容随着硝酸铁加入量的增加而降低,而饱和磁化强度明显增强。Fe/OMCs对MB有快速吸附能力,其行为符合Sips吸附方程。     

Preparation of ordered mesoporous SiCN ceramics with large surface area and high thermal stability

For the first time, highly ordered two-dimensional (2-D) and three-dimensional (3-D) mesoporous SiCN ceramics with high surface area and high thermal stability were prepared by nanocasting a preceramic polymer solution into mesoporous carbon templates, CMK-3 and CMK-8, respectively. As a negative replica of CMK-3 carbon, the obtained mesoporous SiCN ceramic possessed an ordered 2-D hexagonal mesostructure, which is similar to the structure of SBA-15 silica except for the reduced dimensions. An ordered 3-D cubic mesoporous SiCN ceramic was also fabricated using CMK-8 as a template. The wall of the mesoporous SiCN replicas consisted of an amorphous SiCN ceramic phase, which possessed high thermal stability at high temperature up to 1000 °C. N₂-sorption isotherms revealed that these ordered mesoporous SiCN ceramics have high BET surface areas (up to 472 m² g⁻¹) and narrow pore-size distributions, which was preserved even after a re-treatment at 1000 °C in air. The use of carbon template played an important role in the preparation of mesoporous SiCN replicas and enhanced the thermal stability of the SiCN products. It is expected that many other types of ordered mesoporous ceramics can be prepared from nanoporous carbon by nanocasting method.     

高比表面均苯型聚酰亚胺的合成与研究

本实验采用正向加料工艺,将二酸酐加入已溶解的二胺中,通过两步法控制反应温度、反应物以及脱水剂用量等条件,以此来控制聚合物的分子量。发现控制反应的温度,其中包括水浴反应与加热反应两个阶段,以及控制脱水剂用量这两种方式是提升均苯型聚酰亚胺性能的有效方式。     

Synthesis of nanostructured magnesium silicate with high surface area and mesoporous structure

Nanostructured magnesium silicate with high BET surface area and mesoporous structure was prepared by a hydrothermal method using polyethylene glycol (PEG) as surfactant and magnesium nitrate and sodium silicate aqueous solution as magnesium and silicate sources, respectively. The effects of different parameters such as hydrothermal treatment, reaction temperature, pH, ethanol/PEG ratio and etc. on the structural properties of the synthesized sample were examined. The prepared samples were characterized by X-ray diffraction (XRD), N₂ adsorption (BET) and scanning electron microscopy (SEM) techniques. The results indicated that hydrothermal treatment increased BET surface area from 290 to 394.2 m²/g and transfer amorphous phase to crystalline. Also, increasing in aging temperature, aging time, pH value and ethanol/PEG ratio did not change surface area by specific procedure, whereas increasing calcination temperature decreased surface area. Furthermore, hydrothermal treatment and increasing in pH value will change hysteresis loop. The highest BET surface area obtained in this paper is 619.8 m²/g.     

软模法磁性有序介孔炭的合成与表征

以三嵌段共聚物为软模,间苯二酚-甲醛为炭前躯体,硝酸铁为铁源合成了磁性有序介孔炭,用XRD、氮气吸附、磁性测试等方法对样品进行表征.结果表明,当硝酸铁与间苯二酚摩尔比为0.025、0.05及0.10时得到的介孔炭具有有序性,随着铁质量分数的增加,有序性降低,比表面积、孔容都相应减小.基本磁化曲线结果表明,随着铁质量分数的增加,饱和磁化强度随之增加(0.01～0.10 emu/g),材料具有较好的磁性,容易从溶液中分离,表现出良好的分离性能.为磁性有序介孔炭的优化合成及磁性分离应用提供科学依据.     

Synthesis and characterization of high surface area molybdenum phosphide

A high surface area molybdenum phosphide (MoP) was successfully synthesized by combining citric acid (CA) and temperature-programmed reduction (TPR) (CA-TPR) method. Reduction of the precursor which was modified by citric acid produced MoP with a high surface area of 122.0 m² g⁻¹ under optimum conditions. Fourier transform infrared (FTIR) results showed that the chelating interaction between the moderate amount of citric acid and the molybdenum ion was effective in suppressing the aggregation of Mo during drying through the formation of a molybdenum citrate, which was decomposed in calcination. Reduction of the precursor from the CA-TPR method showed an obvious decrease in degree of the aggregation of the MoP particles when compared to that from the conventional TPR method. The MoP prepared by the CA-TPR method was characterized by X-ray diffraction (XRD), N₂ adsorption–desorption, TPR, transmission electron microscopy (TEM), scanning electron microscopy (SEM), and CO adsorption microcalorimetry. An increase in reduction temperature led to the formation of MoP crystalline and a change of morphology. The increase of surface area in the reduction process was a result of the formation of pores. The porous MoP from the CA-TPR method had a higher CO chemisorption uptake than from the conventional TPR method, indicating that the high surface area MoP possessed more active sites. The preliminary testing showed that the high surface area MoP exhibited a superior activity for hydrazine decomposition with a conversion of 85%, which was much higher than the conventional MoP of 55%.     

Synthesis and optimization of high surface area mesoporous date palm fiber-based nanostructured powder activated carbon for aluminum removal

Date palm fiber (DPF) derived from agrowaste was utilized as a new precursor for the optimized synthesis of a cost-effective, nanostructured, powder-activated carbon (nPAC) for aluminum (Al3+) removal from aqueous solutions using carbonization, KOH activation, response surface methodology (RSM) and central composite design (CCD). The optimum synthesis condition, activation temperature, time and impregna-tion ratio were found to be 650 ℃, 1.09 hour and 1:1, respectively. Furthermore, the optimum conditions for removal were 99.5％and 9.958 mg·g-1 in regard to uptake capacity. The optimum conditions of nPAC was analyzed and characterized using XRD, FTIR, FESEM, BET, TGA and Zeta potential. Moreover, the adsorption of the Al3+ conditions was optimized with an integrated RSM-CCD experimental design. Regression results revealed that the adsorption kinetics data was well fitted by the pseudo-second order model, whereas the adsorption isotherm data was best represented by the Freundlich isotherm model. Optimum activated carbon indicated that DPF can serve as a cost-effective precursor adsorbent for Al3+removal.     

简易模板法制备有序介孔碳及其表征

目前制备有序介孔碳的方法工艺复杂、繁琐耗时,为了简化其制备工艺,缩短实验流程,本文提出一种不需要添加额外溶剂直接制备有序介孔碳的方法。以三嵌段共聚物F127为模板剂,自制低分子量酚醛树脂为碳前体,制备了具有二维六方结构的介孔碳。采用红外光谱对酚醛树脂和F127进行表征,研究了两者之间的作用力;采用X射线衍射、透射电镜和N2吸附/脱附等手段对介孔碳结构进行表征,研究了酚醛树脂的合成温度和模板剂用量对介孔碳结构的影响。结果表明酚醛树脂合成温度为70℃,F127：PF=1时,得到的介孔碳比表面积、孔容和孔径分别为490m2/g、0.41cm3/g和4.15nm。     

高比表面积活性炭吸附存储天然气性能研究

天然气中少量乙烷和丙烷的存在会直接影响活性炭对天然气的吸附存储容量。为此,体积法测定了高比表面积活性炭对甲烷、乙烷和丙烷的吸附等温线,吸附温度分别为283,293,303和313K;采用Langmuir-Freundlich(LF)方程拟合吸附等温线,得到各气体的方程参数,进而采用LRC关联式预测多组分吸附平衡数据,并计算活性炭对模拟天然气的存储能力。结果表明:活性炭对3种气体的吸附等温线都属于I型等温线,采用L-F方程可以很好地描述各气体的吸附等温线;高比表面积活性炭对模拟天然气的存储量随吸附温度的升高而显著降低,在吸附存储压力为3.5 MPa,吸附温度从283 K上升到313 K,相应的存储量(体积比)由139降低为103;与纯甲烷的吸附存储相比,模拟天然气的吸附储量(体积比)提高约20。     

具有介孔孔壁的三维有序大孔氧化铝的制备与表征

以260 nm的聚苯乙烯胶体微球组装的胶体晶体作为模板,采用硝酸铝为原料制备了γ晶相的三维有序大孔(3DOM)Al2O3。首先将Al(NO3)3.9H2O溶解在体积分数70%的甲醇溶液中并填充到胶体晶体模板中,然后取出模板室温干燥,再用质量分数10%的稀氨水浸泡并干燥,最后经550℃焙烧3 h得到3DOMAl2O3。所得材料具有三维有序的大孔孔道,大孔之间由小窗口连通,构成内部交联的大孔网络。3DOMAl2O3孔壁由10 nm左右的Al2O3纳米粒子组成,形成丰富的介孔孔隙,并使材料构成大孔/介孔多级孔道体系,材料的BET比表面积达到315 m2/g。     

高比表面积煤质活性炭的制备与活化机理

以煤为原料,采用KOH活化法制备了高比表面积活性炭,分别考察了活化温度、浸渍比和活化时间等工艺参数对活性炭吸附性能的影响;测试了高比表面积活性炭在-196℃对N₂的吸附等温线、比表面积和孔径分布。结果表明,当活化工艺参数为活化温度900℃,浸渍比4,活化时间1.5 h的条件下可以制得较好的高比表面积活性炭产品,其比表面积为3135 m²·g^-1,孔容为1.72 cm³·g^-1,碘吸附值为2657 mg·g^-1;采用扫描电子显微镜观察了高比表面积活性炭的微观结构,采用气体分析仪检测了活化过程中的尾气成分,提出了高比表面积活性炭的活化机理。     

Aqueous-based,high-density nanoporous carbon xerogels with high specific surface area for supercapacitors

Journal of Porous Materials - Electrode materials with high density for assembling supercapacitors with high volumetric capacitance are urgently needed. Herein, nanoporous carbon xerogels (NPCXs)...     

Synthesis and characterization of highly ordered mesoporous YSZ by tri-block copolymer

A highly ordered mesoporous yttria-stabilized zirconia (YSZ) has been successfully prepared by evaporation-induced self-assembly method (EISA) using tri-block copolymer Pluronic F127 as a structure-directing agent and inorganic chlorides as precursors in a non-aqueous medium. The characterization of the mesoporous YSZ materials was carried out by using small angle X-ray diffraction (SAXRD), transmission electron microscopy (TEM) and N₂ adsorption/desorption. The well ordered mesoporous YSZ is thermally stable up to 600^∘C with an average pore size of 5.4 nm and specific surface area of 90 m²/g. The walls of mesoporous YSZ are composed of ∼6.5 nm nano-crystalline domains.     

Synthesis and characterization of highly ordered mesoporous YSZ by tri-block copolymer

A highly ordered mesoporous yttria-stabilized zirconia (YSZ) has been successfully prepared by evaporation-induced self-assembly method (EISA) using tri-block copolymer Pluronic F127 as a structure-directing agent and inorganic chlorides as precursors in a non-aqueous medium. The characterization of the mesoporous YSZ materials was carried out by using small angle X-ray diffraction (SAXRD), transmission electron microscopy (TEM) and N₂ adsorption/desorption. The well ordered mesoporous YSZ is thermally stable up to 600^°C with an average pore size of 5.4 nm and specific surface area of 90 m²/g. The walls of mesoporous YSZ are composed of ～6.5 nm nano-crystalline domains.