超增溶自组装原位合成ZSM-5纳米分子筛

采用超增溶胶团法制备纳米ZSM-5分子筛。考察体系水含量、乳化剂用量、晶化温度和焙烧温度等因素对合成分子筛产品的粒径、晶体形貌、孔径、孔容和比表面积等的影响,并采用BET、XRD和TEM等手段对其进行表征。结果表明,制备纳米ZSM-5分子筛的最佳条件：n（H₂O）∶n（SiO₂）=90,乳化剂（RHP）质量分数为10%,晶化温度180 ℃,焙烧温度500 ℃。制得的粒子平均粒径（50～70） nm,大多数粒子为球形,粒径分布较窄,呈单分散且微粒不易团聚。     

超增溶胶团自组装原位制备单分散纳米TiO2

以四氯化钛为原料，应用自制模板剂，采用超增溶胶团自组装原理制备TiO₂纳米微粒,利用XRD、TEM和BET吸附等分析测试手段对所得TiO₂微粒的晶相组成、粒径大小和形貌进行表征，表明制备的锐钛矿型TiO2纳米微粒具有较好的分散性，一次粒径大小为8～16 nm，二次粒径80～120 nm。     

溶胶-水热合成法制备纳米4A分子筛

以磷肥行业副产的含氟硅胶为原料,采用溶胶-水热合成法成功制备纳米4A分子筛,并采用XRD、SEM、激光粒度分析等手段与常规水热合成的4A分子筛进行了对比。结果表明,纳米4A分子筛钙交换容量为325mg/g,白度为95%,可满足洗涤助剂的要求。     

超增溶自组装制备纳米氧化镍

采用超增溶自组装合成了纳米氧化镍,并通过透射电镜（TEM）、X射线衍射（XRD）、N2吸附脱附BET法和热重分析（TG）表征了其结构。结果表明,形成的纳米粒子分散性良好,粒径分布较窄(10～20 nm),晶粒度良好,微晶晶化比较完全,氧化镍纳米粒子具有较大的孔径,比表面积和孔容符合纳米粒子特性。确定了超增溶自组装制备纳米氧化镍的最佳工艺条件。     

溶胶-凝胶法制备纳米TiO2及其分散性研究

本文研究了以钛酸丁酯为起始原料通过溶胶—凝胶法制备纳米TiO2粒子,分别从醇钛比、水钛比、pH值等可控条件设计正交实验,优化制备纳米TiO2的工艺条件。并在此基础上,选择不同的表面活性剂以及不同的加入方式对纳米TiO2粒子进行表面改性,利用粒度分析仪分析了表面活性剂对TiO2颗粒团聚行为以及稳定性的影响。并利用稳定机理对水溶液中TiO2分散稳定性作了解释。     

表面活性剂辅助溶胶-凝胶法制备掺Ba纳米MgO及其负载钌基氨合成催化剂

在表面活性剂聚乙二醇（PEG）、聚丙烯酸钠（PAAS）、聚乙烯醇（PVA）的辅助下,采用溶胶-凝胶法制备了一系列掺Ba纳米MgO及其负载的氨合成Ru催化剂。并采用场发射扫描电镜、X射线粉末衍射、N2物理吸附-脱附、X射线能谱仪对样品进行表征。结果表明：表面活性剂的添加可改善掺Ba纳米MgO的织构性质和表面性质,并增强钡、镁之间的相互作用,促使了钡在载体中的分散。其中,在10 MPa、425 ℃、10000 h－1的测试条件下,添加5%的PAAS时制得的2%Ru/Ba-MgO催化剂出口氨生成速率达65.9 mmol/(g?h)。     

纳米ZSM-5分子筛的合成研究

相比于微米ZSM-5分子筛,纳米ZSM-5分子筛具有孔道短,酸量多,外表面积大,抗积炭失活等优势。通过添加分散介质、分散剂、矿化剂及晶种导向剂等手段抑或通过不同的合成方法,可以得到纳米ZSM-5分子筛。文章综述了纳米ZSM-5分子筛的合成影响因素及合成方法。     

介-微孔ZSM-5分子筛的原位合成

在ZSM-5合成过程中引入高分子量三嵌段共聚物P123,原位合成介-微孔ZSM-5分子筛,采用XRD、IR、BET和TEM对材料进行表征。结果表明,合成材料的主体结构为ZSM-5分子筛,比表面积为372 m²·g^-1,孔体积为0.226 mL·g^-1,其中,介孔比表面积为44 m²·g^-1,介孔孔体积为0.068 mL·g^-1,为介-微孔分子筛的合成开发了一条全新的技术路线。     

纳米晶SnO2合成的溶胶-凝胶制备方法

采用一种新的溶胶-凝胶法制备了氧化锡纳米晶.通过向硝酸锡溶液中加入酒石酸形成稳定的酒石酸锡的配合物,再向上述稳定的配合物溶液中滴加乙腈溶剂,配合物溶液出现了溶胶,再形成凝胶.对凝胶进行洗涤烘干后直接得到晶粒大小为4.5 nm的氧化锡纳米晶.200 ℃和400 ℃热处理得到的氧化锡纳米晶的晶粒大小分别为8.4 nm和13.7 nm.透射电子显微镜显示获得的纳米晶的分散性能很好.本方法对于无氯离子方法制备高纯度氧化物纳米晶具有推广意义.     

超增溶自组装法合成纳米AlPO_4-5分子筛

采用超增溶自组装法合成纳米级AlPO4-5分子筛,考察了焙烧温度、乳化剂质量分数对分子筛粒径及其分布的影响,结果表明在超增溶纳米自组装的条件下能够合成出类球形的纳米磷铝分子筛,并且通过调节乳化剂的质量分数可以控制纳米分子筛的粒径大小,纳米磷铝分子筛直径为10~80 nm,长度为0.1~0.2μm。     

Rod-like micelle templated synthesis of porous hydroxyapatite

Use of macromolecular templates for controlling nanostructures of inorganic materials is an active area of research. In particular, oriented growth of hydroxyapatite in organic matrix is of great relevance to understand biomineralisation of bone and its potential biomedical applications. Natural bone being a composite of hydroxyapatite and collagen fibers, crystallization of hydroxyapatite in fibrous assemblies could mimic such biomineralisation. This motivated us to investigate the role of long rod-like micelles in modulating the structure of hydroxyapatite particles. In this article, we report the preparation of porous hydroxyapatite nanorods using rod-like micelles made up of a cationic surfactant cetyltrimethylammonium bromide (CTAB) and anionic hydrotrope sodium salicylate (SS) as a templating agent. The successful formation of hydroxyapatite crystals is evident from XRD, FTIR, TGA, SEM and TEM analyses. It has been observed that large hydroxyapatite nanorods of diameter ～50 nm are formed in surfactant mediated synthesis, whereas irregular shaped nanoaggregates of hydroxyapatite are obtained in the absence of surfactant. A comparative study on the porosity of hydroxyapatite clearly shows that monomodal distribution of mesopores with a peak at ～30 nm in the absence of surfactant while bimodal distribution of mesopores having maxima at ～4 nm and ～45 nm appear in hydroxyapatite prepared in the presence of surfactant template.     

Synthesis of macroporous poly(styrene-divinyl benzene) microspheres by surfactant reverse micelles swelling method

Macroporous poly(styrene-divinyl benzene) microspheres with pore size of about 500 nm were prepared by a new method, surfactant reverse micelles swelling method. The macroporous microspheres were prepared by convenient suspension polymerization. The difference from conventional suspension polymerization was that a higher concentration of surfactant was added in the oil phase. The effects of the amount and type of surfactants on the morphology of microspheres were investigated, and the formation mechanism was also discussed. Macropores were formed when the concentration of surfactant was much higher than critical micelle concentration (cmc). It was proposed that a large amount of reverse micelles formed by adding a large amount of surfactant in the oil droplet phase, and the reverse micelles could absorb water from the external aqueous phase. The water in the oil phase formed macropores after polymerization. The method developed in this study was convenient to prepare microspheres with larger pore size than the conventional method such as agglomeration method of nanoparticles.     

In situ synthesis of Si2N2O/Si3N4 composite ceramics using polysilyloxycarbodiimide precursors

In situ synthesis of Si₂N₂O/Si₃N₄ composite ceramics was conducted via thermolysis of novel polysilyloxycarbodiimide ([SiOSi(NCN)₃]_n) precursors between 1000 and 1500 °C in nitrogen atmosphere. The relative structures of Si₂N₂O/Si₃N₄ composite ceramics were explained by the structural evolution observed by electron energy-loss spectroscopy but also by Fourier transform infrared and ²⁹Si-NMR spectrometry. An amorphous single-phase Si₂N₂O ceramic with porous structure with pore size of 10–20 μm in diameter was obtained via a pyrolyzed process at 1000 °C. After heat-treatment at 1400 °C, a composite ceramic was obtained composed of 53.2 wt.% Si₂N₂O and 46.8 wt.% Si₃N₄ phases. The amount of Si₂N₂O phase in the composite ceramic decreased further after heat-treatment at 1500 °C and a crystalline product containing 12.8 wt.% Si₂N₂O and 87.2 wt.% Si₃N₄ phases was obtained. In addition, it is interesting that residual carbon in the ceramic composite nearly disappeared and no SiC phase was observed in the final Si₂N₂O/Si₃N₄ composite.     

焙烧法水热合成5A沸石分子筛

焙烧活化化工原料氢氧化钙、氢氧化钠、硅酸钠和二氧化硅，探索焙烧法水热合成5A沸石分子筛的条件。并通过X射线粉末衍射(XPS)和扫描电镜(SEM)对产品进行表征。焙烧原料合成5A沸石分子筛的优化条件为焙烧温度550 ℃, 焙烧时间4 h, 晶化时间4 h。     

ZSM-5分子筛的合成与改性研究进展

ZSM-5分子筛是一种在石油催化裂化过程中常用的择型分子筛,具有良好的热稳定性、耐酸性和择型选择性。催化剂中ZSM-5分子筛的添加可以提高汽油辛烷值和烯烃产率。目前,中国已经形成了以催化裂化为主的重质油加工工艺,2013年原油加工量超过4亿t/a。在未来相当长一段时间,催化裂化加工重质劣质原料油仍是炼油厂的工作重点。综述了近年来国内外ZSM-5分子筛的合成与改性研究进展,为今后ZSM-5分子筛合成与改性方面的研究提供了一定的借鉴和参考。     

ZSM-5沸石合成与改性技术进展

ZSM-5沸石在石油化工过程中得到广泛应用。阐述了ZSM-5沸石的合成、改性技术现状及其应用以及近年来的研究和开发应用最新进展，为ZSM-5沸石的开发利用提供新的思路。     

In-situ synthesis and catalytic activity of ZSM-5 zeolite

ZSM-5 zeolite has been hydrothermally synthesized in-situ on the external surface of calcined kaolinite in the presence of n-butylamine. This supported zeolite was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy and N₂ adsorption. Several synthesis variables were systematically investigated, including SiO₂ to Al₂O₃ ratio, pH, crystallization time, and crystallization temperature. After mixing the ZSM-5 with a Fluid Catalytic Cracking (FCC) catalyst, catalytic performance was evaluated by cracking vacuum gas oil (VGO) in a micro-fixed bed reactor. ZSM-5 addition was favorable for the production of light olefins by catalytic cracking of VGO.     

微波辅助合成5-[4-(4-溴代丁氧基)苯基]-10,15,20-三对甲氧基苯基卟啉

探讨采用微波辅助合成尾式卟啉（p-BrTMOPP）的制备工艺及其影响因素。以吡咯、对羟基苯甲醛和对甲氧基苯甲醛为原料,以丙酸为溶剂,制备得到p-HTMOPP;以1,4-二溴丁烷为原料,微波辅助加热条件下制备得到目标化合物尾式卟啉p-BrTMOPP;目标产物经过UV-vis、IR、ESI-MS等方法表征。在90℃、DMF溶剂条件下微波辐射加热30min,快速高效得到目标化合物,反应产率89.2%。和传统加热方法相比较,微波辅助合成尾式卟啉化合物明显缩短了反应时间,提高了反应效率。     

4A沸石合成工艺研究与产物表征

利用正交优选实验研究了硅铝比、钠硅比、水钠比、反应温度和反应时间等5个因素对水热合成4A沸石的影响,在此基础上还研究了超声波辅助水热合成4A沸石,利用XRD、场发射扫描电子显微镜(FESEM)和钙离子交换能力对4A沸石进行了表征。正交优选实验结果表明:硅铝比是影响4A沸石钙离子交换能力的主要因素,其次是钠硅比和反应时间,水钠比和反应温度的影响最小;水热合成4A沸石的最佳工艺为以硅铝物质的量比为1.5、钠硅物质的量比为2.05、水钠物质的量比为150配制硅铝酸钠凝胶,于130℃下晶化5 h。通过水热合成及超声波辅助水热合成的4A沸石的对比表明:一定时间的超声波辅助水热合成更容易得到较高性能的4A沸石。