含磺酸基介孔分子筛SBA-15-SO3H催化合成油酸乙酯

采用水热法直接合成含磺酸基的介孔分子筛SBA-15-SO₃H。以油酸和乙醇为原料催化合成油酸乙酯，进行了不同催化剂的对比实验以及催化剂组成、反应温度、酸醇物质的量比和催化剂用量等反应条件的考察。得到最佳反应条件：温度130 ℃，n(酸)∶n(醇)=1∶2.5，反应时间4 h，催化剂质量分数为10%。     

对甲苯磺酸改性SBA-15的合成及催化合成乙酸正丁酯

采用浸渍法将含有磺酸基的对甲苯磺酸负载在SBA-15表面上,合成含有一定酸性的固体酸催化剂TsOH-SBA-15。催化剂的制备条件为:对甲苯磺酸的浸渍浓度为0.5 mol/L,焙烧温度为300℃,焙烧时间为4 h。用XRD,IR,DTA/TGA,氮吸附-脱附等方法对改性后的样品进行表征。结果表明,改性后的SBA-15分子筛的结构未发生变化,仍具有有序孔道结构。TsOH-SBA-15催化剂对冰乙酸和正丁醇的酯化反应具有较高的活性,正交实验结果为:反应时间80 m in,n(冰乙酸)∶n(正丁醇)=1∶1.2,催化剂用量为冰乙酸质量的5%,此时酯化率可达到95%。     

有序介孔分子筛SBA-15的改性研究进展

综述了有序介孔分子筛SBA-15材料由于其骨架缺陷少,导致催化活性较低,为了扩展其在催化、大分子吸附领域的应用,需要在SBA-15表面引入活性组分的现状。从改性机理和方法出发,并结合了近年来国内外研究现状,SBA-15在金属改性和酸改性领域的应用,对今后的研究方向做出了展望。     

有序介孔分子筛SBA-15的改性研究进展

综述了有序介孔分子筛SBA-15材料由于其骨架缺陷少,导致催化活性较低,为了扩展其在催化、大分子吸附领域的应用,需要在SBA-15表面引入活性组分的现状。从改性机理和方法出发,并结合了近年来国内外研究现状,SBA-15在金属改性和酸改性领域的应用,对今后的研究方向做出了展望。     

硅酸钠为硅源的介孔分子筛SBA-15-SO3H的研究

在强酸性和水热条件下以硅酸钠（Na₂SiO₃·9H₂O）为硅源合成表面含磺酸基的介孔分子筛催化剂SBA-15-SO₃H。XRD结果表明，该分子筛具有规则的六方立柱形介孔结构。SBA-15-SO3H用于叔丁醇和乙醇合成乙基叔丁基醚（ETBE）的醚化反应研究，分别考察了反应温度、原料配比和反应时间等因素对醚化反应的影响。最佳操作条件为：温度120 ℃，n(乙醇)∶n(叔丁醇)=2∶1，反应时间5 h，m(催化剂) ∶m(原料)=1∶10。在此条件下，叔丁醇的转化率为62.83%。     

改性SBA-15介孔分子筛的催化研究进展

SBA-15介孔分子筛,以其独特的结构、所能提供的特殊微环境以及广阔的应用前景,成为催化与纳米材料领域长久以来研究和开发的热点之一。综述了近年来SBA-15介孔分子筛的研究进展情况,侧重于改性原理、改性方法以及金属改性、酸改性和有机物改性3个具体的改性方向,并对其今后的研究方向进行了展望。     

磺酸基官能化介孔材料的表征及其催化性能

由高水热稳定的巯基官能化介孔硅基材料经氧化得到磺酸基官能化介孔固体酸催化剂。经过一系列的表征测试,所得固体酸具有发达的孔道结构和大量Br尴nsted酸性位。将其应用于苯甲醛与醇类缩合反应中,与传统沸石固体酸催化剂HY相比,显示了更好的催化性能,缩醛收率在90%左右。所合成的磺酸基官能化介孔固体酸催化剂的催化性能基本不受醇类分子体积影响,具有很好的重复使用性能。     

介孔分子筛SBA-15的研究进展

自从介孔分子筛SBA - 15首次合成出来 ,成为众多研究领域的一个研究热点。文章综述了介孔分子筛SBA -15的合成及机理 ,影响孔径尺寸的因素及研究应用进展 ,介孔分子筛SBA - 15在催化、吸附和分离及纳米材料等领域具有广泛的应用前景。     

油酸丁酯的合成研究

以油酸和正丁醇为原料,采用对甲苯磺酸作催化剂合成油酸丁酯,考察了影响反应的因素。实验结果表明,酯化反应的优化条件为油酸、正丁醇、对甲苯磺酸摩尔比为1:2:0.15,反应时间70min,产率可达93.92%。     

粒径对磺酸官能化介孔材料性能的影响

以聚乙氧基-聚丙氧基-聚乙氧基三嵌段共聚物(P123)为模板剂、正硅酸乙酯(TEOS)为硅源,保持P123和TEOS的浓度比,改变P123和TEOS在合成体系中的浓度,水热法合成了系列具有不同粒径的介孔分子筛SBA-15.采用后合成法,将3-巯基丙摹三甲氧基硅烷(MPTMS)嫁接到具有不同粒径的介孔分子筛SBA-15表面上,经氧化后得到含有强酸性的磺酸基因的固体酸样品SBA-15-SO_3H.采用SEM、XRD、FT-IR、TG-DTA、N_2吸附以及酯化反应考察了粒径对所制备的SBA-15-SO_3H的物化性能和催化性能的影响.结果表明,SBA-15的粒径大小对MPTMS在其上的嫁接量没有很人影响,但对后续氧化过程有较大的影响,SBA-15粒径的减小有利于巯基被氧化为磺酸基,导致磺酸的负载量随着粒径的减少而增大.SBA-15-SO_3H在乙酸和乙醇的酯化反应中表现出不同的催化性能,催化性能的差异是粒径大小、酸量及磺酸基和巯基相互作用的综合结果.     

介孔分子筛SBA-15的改性研究进展

从金属改性、酸改性和氧化物改性三方面综述了介孔分子筛SBA-15的改性研究进展,重点介绍了SBA-15表面功能化后引入金属改性的方法。评述了金属纳米粒子的制备对改性的SBA-15催化剂催化性能的影响。     

Tuning of nanostructured SBA-15 silica using phosphoric acid

A simple method is described to synthesize mesoporous SBA-15 with controlled distinct morphologies. Using the same initial synthesis mixture composition consisting of non-ionic P123 block co-polymer, tetra-ethyl orthosilicate as silica source and phosphoric acid, well-ordered mesoporous films, cakes, fibers and bundle-like structures were produced simply by changing the stirring rate. Free-standing films at the air–water interface and cake-like structures were obtained simultaneously under static conditions. On the other hand, fibers and bundles of threads resulted under vigorous and slow stirring conditions, respectively. Transmission electron microscopy (TEM) images of these bundles revealed straight parallel nanochannels oriented along the long axis of the bundles. X-ray fluorescence (XRF) measurements of the calcined samples indicated the presence of phosphorus, which might provide additional Brønsted acid sites for potential applications in catalysis.     

介孔分子筛SBA-15表面改性对脂肪酶固定化的强化作用

引言 脂肪酶可以催化酯水解或醇解、酯合成、酯交换、多肽合成及高聚物合成等多种有机反应,已被广泛应用于食品、精细化工及制药工业中[1].作为重要的生物催化剂,脂肪酶应用的有效性和经济性很大程度上取决于酶的固定化.     

P/SBA-15催化合成十六烷基苯

采用负载磷酸的SBA-15分子筛作为催化剂,以苯和十六碳烯为原料,经烷基化反应合成十六烷基苯。在微型液相固定床反应器上考察了反应温度、空速、体系压力、磷酸负载量以及苯烯摩尔比等反应条件对催化剂性能的影响。研究结果表明,磷酸的适宜负载量约为7%(质量分数),适宜反应条件为反应温度180℃、空速为2.0 h-1、体系压力为2.0 MPa和苯、烯摩尔比为10。在此条件下,十六碳烯的转化率可达到94.5%,十六烷基苯选择性可达93%。催化剂单程寿命达到120 h以上。负载磷酸的SBA-15催化剂呈现较好的催化活性和稳定性。     

On the mechanical stability of mesoporous silica SBA-15

Mesoporous silica SBA-15 was synthesised at 80 °C. The calcined solids were exposed to a unilateral external pressure in the range 16–191 MPa in order to monitor the impact of the mechanical pressure on the properties of SBA-15. N₂ adsorption–desorption measurements, XRD and UV-Raman spectroscopy was used in order to evaluate the changes occurring in the SBA-15. For the XRD measurement, an internal Si standard was used to correct the position of the SBA-15 patterns. It appeared that the elevated pressure has no influence on the hexagonal cell parameter a. Through the N₂ sorption measurements the fraction of the preserved mesoporous structure was estimated to be 60% when the highest pressure has been used. As the remaining part of the material is irreversibly disintegrated into small particles, the pressed sample is considered to be heterogeneous. However, the preserved fraction is slightly modified, showing a smaller pore width and plugs located within the mesopores. The plugs most likely originate from a disintegrated fraction of the SBA-15. UV-Raman spectroscopy shows that the relative intensity of the band associated with the siliceous network (ω₁) has decreased on the pressed samples resulting in a less ordered material possessing an enhanced population of silanols as compared to parent SBA-15. We propose that the disorder introduced by pressing is responsible for the observed expansion of the SBA-15 walls, which is detected for the samples treated at higher pressures (112, 191 MPa).     

不同硅源合成介孔分子筛SBA-15的研究

采用两种不同硅源——硅酸钠（Na2SiO3·9H2O）和正硅酸四乙酯（TEOS）合成介孔分子筛SBA-15。通过X射线粉末衍射（XRD）对样品进行表征，发现两种硅源合成的SBA-15都具有高度有序的二维六方立柱形结构。它们的比表面积相近，用TEOS作为硅源的SBA-15的孔容比用硅酸钠作为硅源的SBA-15的略大；用硅酸钠作为硅源的SBA-15有更高的微孔率和更厚的孔壁。以硅酸钠为硅源的SBA-15显示出分子自组装过程时间从24 h减少到3 h，并且对SBA-15模板性质没有有害影响。     

Synthesis of high surface area mesoporous silica SBA-15 for hydrogen storage application

In the present report, mesoporous silica SBA-15 was synthesized by different methods such as room temperature aging, hydrothermal, and sonication-mediated hydrothermal methods. The effect of different time and temperature on the synthesis method was investigated by conventional characterization techniques. The powders synthesized by different methods showed different properties, mainly in morphology and pore volume. In comparison to others, the powder synthesized by the hydrothermal method at 100°C for 48 hours showed exceptionally high surface area of 3274 m²/g. To date, as per our knowledge, no such value was reported in literature. Finally, the powders were characterized by H₂ storage capacity by the adsorption-desorption method using 99.999% H₂. The hydrogen adsorption capacity of the same powder was observed at 6.02 wt%. Also, this value seems to be the highest H₂ adsorption capacity in comparison to other powders described in literature.