炭气凝胶的制备

通过对ＲＦ有机气凝胶进行炭化,成功地制备了具有纳米网络结构的炭气凝胶。系统考察了炭化条件及溶胶－凝胶过程条件对炭气凝胶性质的影响,并对所得的炭气凝胶进行了ＴＥＭ表征。     

炭气凝胶的常压干燥制备研究

实验以间苯二酚(Resorcinol,简称R)与甲醛(Formaldehyde,简称F)以一定的摩尔比混合,加入二次去离子水作为溶剂并用碱性试剂作为催化剂,在恒温水浴中生成RF湿凝胶。在常温下用丙酮浸泡湿凝胶以置换水,制备出RF凝胶。最后将RF气凝胶置于管式炉中,在氮气保护气氛下,高温炭化得到炭气凝胶,并用TG-DTA,XRD、高倍显微镜等方法对其表面形貌及结构进行分析。     

酚醛基炭气凝胶的研究进展

炭气凝胶是一种多孔纳米炭材料,具有低密度、高孔隙率、高比表面积、优异的导电性和良好的成型性能等优点,是炭材料研究的热点和重要方向。本文旨在通过阐明酚醛基炭气凝胶的制备原料和制备工艺的发展过程,从而突出未来酚醛基炭气凝胶的发展方向。基于此,本文首先重点介绍了酚醛基炭气凝胶的制备方法,主要包括溶胶-凝胶化、干燥以及炭化过程三个最主要的步骤;进而详述了以三种不同的前体,即间苯二酚、苯酚、生物质单宁/木质素分别制备酚醛基炭气凝胶的方法及其优缺点;接下来对酚醛基炭气凝胶作为吸附材料（气体吸附/液体吸附）的吸附量以及在电化学储能以及其他领域的应用进行了综述;最后对酚醛基炭气凝胶未来的研究方向和发展前景进行了总结和展望。文章指出,传统的以间苯二酚为原料辅以超临界干燥的方法制备的酚醛基炭气凝胶,原料成本较高,反应条件苛刻,实际生产应用受限;以苯酚取代间苯二酚,亦或是采用冷冻干燥等方法改进其制备工艺,可以大幅度降低原料和生产成本;但未来的发展方向和重点将是绿色、可再生的生物质原料（单宁、木质素、腰果酚等）及复合气凝胶材料的研发。因此,酚醛基炭气凝胶在未来的发展还需要进一步改进其制备工艺和方法,拓宽其原料来源,从而提高性能,扩大应用领域。     

炭气凝胶研究进展

介绍了一种新型轻质纳米级多孔性非晶炭素材料－－炭气凝胶的制备方法、性能以用途，提出了存在的问题和发展的前景。     

炭气凝胶的制备、性能及应用

炭气凝胶是一种新型、轻质、纳米、多孔、非晶态炭材料,具有可在纳米尺度控制和剪裁的连续的三维网络结构,具有许多优异的性能和广阔的应用前景。通过结合所从事研究工作,综述了气凝胶的制备、性能及应用,分析了目前存在的问题和发展前景。     

新型RF炭气凝胶微球的制备及结构表征

以间苯二酚和甲醛为原料，在催化剂和表面活性剂的作用下经溶胶-凝胶、超临界干燥、炭化等过程合成一种新型的炭气凝胶微球。采用扫描电镜（SEM）、X射线衍射（XRD）、低温氮吸附（BET）等表征了炭气凝胶微球的微观形貌、结构。研究结果表明：炭气凝胶微球具有规整的球形度，骨架结构为纳米网络结构，孔径集中分布在3．5nm左右，微球直径≤40μm，比表面积为555m^2／g。     

多元酸催化炭气凝胶的常压制备及表征

在多元有机酸催化和表面活性剂的作用下,间苯二酚和甲醛反应生成有机凝胶,经过常压干燥、高温炭化得到炭气凝胶。用扫描电镜(SEM)、X射线衍射(XRD)和亚甲基蓝吸附测试表征所制备的样品。结果表明,所制备的炭气凝胶属于非晶态物质,呈现均匀的球状结构,且微球内富含连通的电荷转移的孔道,其比表面积达到740m2/g。循环伏安扫描测试表明,所制备的炭气凝胶具有良好的电化学性能,有望成为超级电容器的电极材料。     

超电容器用炭气凝胶预凝动态过程的电导法研究

以间苯二酚和甲醛为反应物，氢氧化钙和碳酸钠为催化剂，通过溶胶一凝胶法制备出有机凝胶。研究了不同催化剂及其含量下凝胶化过程中电导率的变化。结果表明，电导法是一种有效的监测凝胶化动态过程的方法，具有方便、实时、精确、快捷的优点，对深入认识和研究反应体系有重要意义。     

炭气凝胶的制备及应用进展

炭气凝胶是一种结构新颖的中孔材料,具有很多特殊的性质。本文在简要介绍炭气凝胶制备过程的基础上,综述了近年来炭气凝胶结构改性和应用方面的最新研究进展,主要包括球形和杂化炭气凝胶的研究现状,最后指出未来的发展方向。     

超临界流体干燥法制备炭气凝胶

以间苯二酚和甲醛为原料, Ca(OH)2为催化剂,经溶胶—凝胶过程得水凝胶 ;以超临界 CO2干燥水凝胶,得到网络间充满气体的固态材料气凝胶,再经高温热解得炭气凝胶。 TEM表征结果显示：气凝胶和炭气凝胶均具有规则的纳米网络结构,网络节点粒径约 10 nm,典型网络孔径小于 50 nm。     

采用钠硼解石生产硼酸的工艺研究

由青海大柴旦钠硼解石矿中提取硼酸，找出了最佳工艺条件，即：矿粒细度〈1．7mm，反应温度80～90℃，反应液酸度（pH）2～3，结晶温度20～25℃，反应液中硼酸质量分数15％～16％，蒸发过程镁离子质量分数〈4％，渣带失（以三氧化二硼计）质量分数〈2％。在此条件下对其工艺技术的稳定性、可靠性及适应性进行了研究。结果表明，硼的总收率达85％以上，利用本地资源生产硼酸，投资少，见效快。     

络合结晶法制备高纯硼酸的研究

以工业硼酸为原料,利用络合结晶分离技术对硼酸中杂质进行选择性分离提取,制备高纯硼酸产品,通过化学滴定分析、电感耦合等离子体原子发射光谱（ICP-AES）、紫外分光光度法、热重分析（TGA）等对产物的纯度和性能进行表征。考察了氧化剂与络合剂的种类和用量、结晶的级数等因素对硼酸产品纯度的影响,确定的最佳工艺条件为：硼酸饱和溶液中加入2%（体积分数）的H₂O₂,搅拌反应后热过滤,滤液中加入质量分数为0.2%的氨羧络合剂,80 ℃下反应,热过滤后缓慢降温结晶,经重结晶分离获得的硼酸产品的纯度达99.99%。     

Zirconia aerogels: Effect of acid used in the sol-gel process on morphological properties

Zirconia aerogels have been prepared from butanolic zirconium(IV) tetra-n-butoxide diluted in ethanol via stoichiometric hydrolysis with water in ethanol. Nitric acid or acetic acid were used to modify the sol-gel process. After calcination in air at 573 K, the aerogel prepared with nitric acid possesses a specific surface area of 240 m² · g^–1 and a unimodal pore size distribution with a maximum at ca. 24 nm, whereas the use of acetic acid results in an aerogel with specific surface area of 228 m² · g^–1 and bimodal pore size distribution with maxima at 3 and 65 nm. The crystalline fractions of both aerogels are predominantly tetragonal with a small contribution of monoclinic ZrO₂.     

Porosity and surface area of monolithic carbon aerogels prepared using alkaline carbonates and organic acids as polymerization catalysts

Carbon aerogels were prepared by polymerization of a resorcinol-formaldehyde mixture using different polymerization catalysts such as: sodium or potassium carbonates, oxalic acid or para-toluenesulfonic acid. The carbon aerogel obtained with this last acid was further CO₂-activated to 8.5% and 22% burn-off. All samples were characterized by N₂ and CO₂ adsorption at −196 and 0 °C, respectively, and by mercury porosimetry, scanning electron microscopy, and thermogravimetric analysis. Samples prepared using Na₂CO₃ were denser than those prepared using K₂CO₃. In addition, the density of samples prepared under acidic conditions was greater than that of samples prepared using alkaline carbonates as catalysts. Most of the carbon aerogels prepared were mesoporous with narrow pore size distributions. Results obtained showed that the nature of the acid used in the preparation of these aerogels only affected the gelation process. Finally, it is noteworthy that CO₂ activation of the carbon aerogel prepared with para-toluenesulfonic acid as catalyst only increased and widened the microporosity and had virtually no effect on the mesoporosity.     

月桂酸咪唑啉硼酸酯的合成

采用两步法合成月桂酸味唑啉硼酸酯.首先研究了月桂酸味唑噼中间体的合成.通过检测反应生成的水的量和对产物进行IR表征,确定了合成中间体的最佳工艺;然后利用这一中间体与硼酸反应,合成咪唑啉硼酸酯,用同样的研究方法考察了各因素对硼酸酯合成的影响,进而得出了硼酸酯合成的最佳工艺为:以甲苯为反应溶剂,采用分批加料的方式.咪唑啉中间体与硼酸的摩尔比大于1,反应滠度160℃,反应时间4h,反应在此条件下进行时,目标产物收率高,反应时间短.     

Preparation and characterization of antibacterial silver-dispersed activated carbon aerogels

Silver-dispersed carbon aerogels (CAs) were obtained by direct immersion of organic aerogels prepared by ambient pressure drying technique in AgNO₃ aqueous solution and then carbonization. The effect of preparation conditions such as the resorcinol/catalyst ratio, the feed AgNO₃ concentration, the ratio of aerogel mass/solution volume, immersion time and carbonization temperature on the bulk density and silver content as well as the BET surface area of the dispersed CAs was studied. The dispersion and structure of silver nanoparticles in obtained materials were investigated by means of scanning electron microscopy, transmission electron microscopy and X-ray diffraction. The Ag-dispersed CAs prepared exhibit strong and long-term antibacterial activity.     

Preparation of low-density carbon aerogels by ambient pressure drying

With the addition of hexamethylenetetramine (HMTA) and alcohol as solvent, an ambient pressure drying technique was developed for the fabrication of low-density organic aerogels and related carbon aerogels. When a suitable ratio of resorcinol to HMTA (R/H ratio) and ratio of resorcinol to solvents (R/S ratio) are selected, the low-density alco-gels obtained can be dried under ambient pressure conditions without observable shrinkage. The addition of HMTA increases the size of carbon nano-particles and the pore size of the aerogels that are produced. The carbon aerogels prepared in this work have similar nano-particle structures typical of the aerogels prepared with CO₂ or by the isopropanol supercritical drying technique.     

Zirconia aerogels and xerogels: Influence of solvent and acid on structural properties

High-surface-area zirconia aerogels with meso- to macroporosity have been prepared by an acid-catalyzed alkoxide-sol-gel route with tetrabutoxyzirconium(IV) and subsequent high-temperature supercritical drying at 578 K. The effect of solvent (ethanol, propanol, butanol, t-amylalcohol), amount of nitric acid, calcination temperature, and drying method was studied by nitrogen physisorption, X-ray diffraction, Fourier transform Raman and diffuse reflectance infrared Fourier transform spectrosopy, scanning electron microscopy, thermal analysis, and temperature-programmed desorption of NH₃. After calcination in air at 573 or 773 K, the aerogels possess specific surface areas of up to 270 or 180 m² · g^–1, respectively. The use of ethanol as solvent resulted in the highest specific surface areas and pore volumes (up to 1.5 cm³ · g^–1) among all samples studied, whereas bulky t-amylalcohol caused a shift of the maxima of the broad pore size distributions from 30 to 70 nm. With the corresponding xerogels, prepared via the same wet-chemical procedure but evaporatively dried at ambient temperature, butanol resulted in a maximum at 3 nm and t-amylalcohol in a bimodal pore size distribution with maxima at 3 and 15 nm. The variation of the acid-to-alkoxide ratio in the range 0.08–0.12 at a hydrolysis level of 4 did not significantly influence the structural properties of aerogels and related xerogels. In contrast to the aerogels, the xerogels had significantly lower specific surface areas and prominent microporosity. All uncalcined aerogels contained crystalline ZrO₂, whereas the corresponding uncalcined xerogels were X-ray amorphous and crystallized only during calcination at 573 K. Both aerogels and xerogels possessed Brønsted-type and Lewis-type acid sites. With the xerogels, the density of acid sites on the surface was significantly lower. This behaviour is attributed to the higher amounts of organic residues which persisted in and on the xerogels up to 773 K and thus blocked the acid sites partially.     

Catalytic combustion of toluene on platinum-containing monolithic carbon aerogels

Monolithic organic aerogels were prepared by the sol–gel procedure from the polymerisation reaction of resorcinol and formaldehyde in water. The organic aerogels were heat treated in inert atmosphere at either 500 or 1000 °C to obtain the carbon aerogels. The catalysts were prepared by impregnation with an aqueous solution of [Pt(NH₃)₄]Cl₂ or by dissolving this salt in the initial aerogel mixture. Supported catalysts were pretreated in He at 400 °C or H₂ at 300 °C before their characterization by H₂ chemisorption, high-resolution transmission electron microscopy and X-ray photoelectron spectroscopy or before testing their catalytic activity. Catalyst activities in toluene combustion were evaluated by conversion versus temperature (light-off curves) and conversion versus time catalytic tests. In the case of catalysts prepared by impregnation, the light-off curves for the total combustion of toluene were shifted to lower temperatures with increasing Pt particle size. This suggests that the reaction was sensitive to the Pt structure within the dispersion range of these catalysts. However, the reverse occurred with catalysts prepared by mixing the precursor in the initial aerogel mixture. Results found could be due to the different surface Pt content of these catalysts as revealed by X-ray photoelectron spectroscopy. This difference was related to the growth of large three-dimensional Pt particles on the surface of the less dispersed catalyst. This means that there is a critical Pt particle size above which the toluene combustion activity decreases with increasing Pt particle size, due to the reduction in active surface sites available for the combustion reaction. Other effect that might influence the activity of these last catalysts is the encapsulation of some Pt particles by the carbon matrix.