氧化镧复合中孔氧化物的合成、表征及催化性能

以十二烷基硫酸钠（SDS）为模板剂,尿素和乙二胺为介质,当n（La）／n（SDS）／n（CO（NH2）2）／n（H2NCH2CH2NH2）／n（H2O）=1．0：1．0：0．6：1．0：200,反应温度为80℃、反应时间为4h时,用水热法合成了氧化镧／十二烷基硫酸钠复合中孔材料（LaOS）。通过XRD,IR,TG／DTA和N2吸附脱附等方法对样品的晶体结构和表面物性进行了研究。结果表明,合成的氧化镧／十二烷基硫酸钠复合物具有典型的六方中孔结构特征,比表面积为182m^2／g,平均孔径为2．6nm。将氧化镧／十二炕基硫酸钠复合物用于催化正辛醇乙氧基化反应,当LaOS的质量分数为10％,反应温度为120℃,初始反应压力0．5MPa时,环氧乙烷的平均反应速率为3．7mol／（mol·h）。产物正辛醇聚氧乙烯醚相对分子质量分布较窄。     

CuSO4／SiO2在合成苯甲醛甘油缩醛中的应用

通过溶胶-胶凝法和浸渍法制备了CuSO4／SiO2催化剂,用XRD、低温N2-吸附和NH3-TPD进行了表征,研究了CuSO4／SiO2在合成苯甲醛甘油缩醛上的催化性能,考察了催化剂的焙烧温度、CuSO4负载量、原料物质的量比、反应时间、环己烷体积等因素对产品收率的影响。结果表明：CuSO4高度分散在SiO2表面上形成中等酸强度、高表面积的中孔固体酸催化剂,并在苯甲醛和甘油的缩合反应中具有良好的催化活性和稳定性。催化剂制备的最佳条件为：焙烧温度550℃,CuSO4的负载量为15％,反应的最佳条件为：n（苯甲醛）：n（甘油）=1：1．1,催化剂质量为反应物总质量的1％,环己烷体积为10mL,反应时间2．0h。在最佳条件下,苯甲醛甘油缩醛的收率可达92．5％。     

微波散射MCM-41介孔分子筛担载醋酸镧的制备及表征

水热法合成了纯硅MCM-41介孔分子筛,通过微波散射制备了系列不同硅镧摩尔比的LaAc／MCM-41（LaAcM）介孔分子筛。通过XRD、IR、N2吸附脱附等方法对分子筛的晶体结构和表面物性进行了表征。结果表明,当担载量n（Si）：,2（La）=30：1．0时,LaAcM Hammett碱量最大,为0．20mmol／g,／40介于＋6．8与＋4．6之间,比表面积为1287m^2／g,孔容0．8273cm^3／g,孔径2．571nm。样品具有典型的六方介孔结构特征。     

焙烧温度对S2O8^2-／ZrO2介孔超强酸的结构与性能的影响

以硝酸锆为锆源,以阴离子表面活性剂十二烷基硫酸钠（SDS）为模板剂,S2O8^2-浸渍无定形Zr（OH）4,制得介孔S2O8^2-／ZrO2固体超强酸,通过N2吸附－脱附、XRD分析、Hammett非水滴定、TEM等方法,考察了不同焙烧温度对S2O8^2-／ZrO2介孔超强酸晶体结构、酸强度等性能的影响。结果表明,当焙烧温度600℃,S2O8^2-／ZrO2样品比表面积为140m2／g,平均孔径在3～4nm之间,酸强度H0≤-12．7,为介孔相固体超强酸。     

新型柴油十六烷值改进剂-草酸二丁酯的合成

以草酸和正丁醇为原料，在酸催化剂下进行醇化反应合成出一种新型柴油十六烷值改进剂——草酸二丁酯。考察了分别用浓硫酸，强酸性阳离子交换树脂和Fe2O3／SO4^2-固体超强酸3种不同的催化剂对该反应的催化性能;确定了各自的最佳合成工艺条件。以硫酸为催化剂，在n(酸)：n(醇)=1:3，ω(催化剂)=0．5％，带水剂10mL，反应时间5h条件下，草酸二丁酯的收率可达90．5％；以酸性阳离子交换树脂为催化剂，在n(酸)：n(醇)=1：2．5，ω(催化剂)=10％，带水剂30mL，反应时间4h条件下，草酸二丁酯的收率可达93．2％；以Fe2O3／SO4^2-固体超强酸为催化剂，在n(酸)：n(醇)=1：2．5，ω(催化剂)=1．5％，带水剂20mL，反应时间4h条件下，草酸二丁酯的收率可达96．0%。     

大孔径高比表面积介孔硅泡沫的制备和表征

以P123作为模板剂,正硅酸乙酯为硅源,苯为微乳剂,采用溶胶-凝胶水热合成法制备了大孔径高比表面积介孔硅泡沫材料,采用小角X-射线衍射、透射电镜、扫描电镜以及N2物理吸附等表征手段进行表征,考察了苯的加入量对介孔硅泡沫孔结构的影响。结果表明,苯的引入可以使有序介孔硅的孔结构从SBA-15的二维六方形向介孔硅泡沫的三维泡沫状结构转变,加大苯的含量可以增大介孔硅泡沫的孔径和孔容。当苯与P123的质量比为2.0时为最佳值,此时得到的介孔硅泡沫材料泡沫状结构最规整、比表面积高且孔径孔容较大,其中表面积可达641.3cm2/g,球形孔孔径可以达到43.8nm,孔容2.41cm3/g,过量苯会导致三维泡沫状结构的破坏。     

高比表面掺杂CeO2纳米粉体的TPR研究

利用BET法对掺杂CeO2纳米粉体的比表面积进行了测试．结果表明，该种粉体具有良好的高温稳定性和抗烧结性．利用程序升温还原法(TPR)测试了掺杂CeO2纳米粉体的催化特性．Ce0．8Sm0．2O1．9纳米粉体的催化转化温度与通常的铈锆体系相比降低了约l00℃．     

化学氧化及高级氧化工艺处理废碱液的研究

采用均相化学催化氧化及高级氧化两步工艺对石油化工乙烯裂解废碱液中的硫化物、有机物进行了处理研究,结果表明：在反应温度40℃、化学催化氧化反应时间90min、Mn^2 15mg／L、气水比(曝气量)75：1以及高级氧化反应时间120min、H2O2的加入量(H2O2／COD)为0．8等条件下,硫化物的转化率可达96％以上,COD去除率可达78％．BOD5／CODcr的比值可由处理前的0．21升至0．54．     

SO4^2-／ZrO2／Al2O3催化剂的制备及其催化性能

用微波、红外、烘箱3种干燥方法制备了负载型纳米ZrO2／Al2O3复合载体,同时在复合载体表面负载SO4^2-制成SO4^2-／ZrO2／Al2O3催化剂,将此催化剂用于α-蒎烯催化异构化反应中。用XRD、FT—IR、TPD等对催化剂的表面积、孔径、晶相结构、酸强度等进行了表征。结果表明,微波干燥法制备的复合载体催化剂（SO4^2-／ZA-W）中ZrO2的粒度较小（平均6nm）,比表面积为156．1m^2／g,平均孔径为4．95nm,其表面酸性中心数和酸强度均高于红外干燥法和烘箱干燥法制备的催化剂。SO4^2-／ZA-W催化剂在α-蒎烯催化异化反应中具有较高的活性,α-蒎烯转化率为95．6％,α-松油烯、柠檬烯等单环萜烯的含量达到56．5％。     

DSD酸的清洁生产工艺

以三氧化硫磺化对硝基甲苯(PNT)制取2-甲基-5-硝基苯磺酸(NTS)并副产98％硫酸，解决了老工艺的废酸污染问题；采用非水溶剂氧化法替代传统的氧化缩合工艺，使产品苄基物含量大幅度降低，无有害废水排放；以Pd／C为催化剂的催化加氢还原法生产4，4’-二氨基二苯乙烯-2，2’-二磺酸(DSD酸)，彻底革除了盐酸铁粉还原法的废渣废水，产品质量好，收率高。按照该工艺进行小试，产品总收率达到85．6％，实现了清洁生产。     

Preparation and characterization of carbon pillared clay material

Carbon pillared clay material was prepared from montmorillonite modified by C19H42BrN and C10H16ClN. SEM, FT-IR, XRD, N2 adsorption-desorption, thermal-gravimetric analysis and differential scanning calorimetry were employed to characterize the pore structure and test the effect of surfactant. The results show that organic modifier combines with montmorillonite particles by covalent bond and ion embedded. The microstructure of carbon pillared material looks like needle slice. The most probable pore size distribution is about 1.7 nm. The clay material slice mainly consists of two-dimensional aperture supported by a carbonization pillar. The high-temperature stability of carbon pillared clay is im- proved.     

Laminar mesoporous structure of modified montmorillonite clays and its formation mechanism

Zr-pillared clays were prepared by heating and ultrasonic methods in intercalation process.The resultants were characterized by XRD,N2 adsorption-desorption,SEM,and TG/DTA analysis.Ultrasonic technology accelerated the pillaring process effectively and obtained better ordered structure than by heating method.The specific surface area and pore volume of the Zr-pillared clays increased by about 13 and 3 times respectively.Rare earth metal(Ce)was introduced into Zr-pillared clays by co-intercalation and dipping method.The specific surface area was increased by co-intercalation approach,but it was decreased dramatically by dipping method.Thermal stability of Ce modified samples prepared by co-intercalation method was enhanced in comparison with Zr-pillared clays.Modification mechanism and "corrugation-like" structural mode of intercalation process was proposed basing on the double XRD peaks in small-angle range of pillared clays,which was related to the deformation of silicate layer.     

氧化铬负载氧化硅层柱磷酸锆的合成及催化性能

采用新途径制备了氧化铬负载氧化硅层柱磷酸锆催化剂 ,首先制备了 3 -胺丙基三乙氧基硅 (APS)层柱磷酸锆 ,浸渍Cr(NO3) 3·6H2 O溶液后在 5 5 0℃下焙烧 ,将其转化为氧化铬负载氧化硅层柱磷酸锆催化剂。与常规浸渍制备方法相比 ,所获得的催化剂样品中铬元素与载体间的相互作用强 ,促进了氧化铬在载体上的分散 ,在氧化铬负载量达到 5 0 %时无晶相氧化铬生成 ,催化剂的比表面积最高达到 2 30m2 /g。在苯羟基化反应中用新途径制备的催化剂苯的转化率可以达到 2 9.6 % ,高于常规方法制备的氧化铬负载氧化硅层柱磷酸锆催化剂。随铬负载量的提高 ,反应过程中活性组分的流失量降低 ,催化剂活性具有较强的抗流失性能     

PEG-300对SiO_2薄膜的修饰

应用溶胶凝胶法和浸渍提拉技术,以正硅酸乙酯为主要原料在玻璃载片上进行涂膜.在制备过程中引入聚乙二醇300（PEG-300）,研究对SiO2薄膜性能的影响.采用TG-DTG和FT-IR、BET等测试技术对膜性能、结构、孔径分布进行表征.结果表明,PEG-300对SiO2溶胶有降黏作用,其临界胶束（CMC）的体积分数约为6.16%;PEG-300对溶胶的稳定作用与其用量有关,最佳添加量为15%（质量分数）;PEG-300可以缩小薄膜的孔径和提高薄膜的比表面积与热稳定性.添加PEG-300后制备的二氧化硅薄膜的比表面积可达334.89m2/g,孔容为0.28cm3/g,平均孔半径为2.36nm,最可几孔半径为1.04nm.     

聚合物对发泡水泥制品孔结构和性能影响

以快硬硫铝酸盐水泥作为胶凝材料,干密度为200 kg/m3的发泡水泥为对象,研究乳液和胶粉对发泡水泥孔隙率、孔径分布、孔径大小和强度的影响.结果显示:随着聚合物掺量的增加,发泡水泥制品的孔隙率不随聚合物掺量的增加而发生变化,气孔的孔径逐渐变小,强度不断增大.当乳液和胶粉外掺量分别为2.5%时,发泡水泥28d的抗压强度、抗折强度和垂直表面拉伸强度分别增加8%、13%、28%和5%、10%、25%.     

Ce掺杂对Mn/ACN催化剂低温NH3-SCR脱硝活性的影响

采用浸渍法将活性组分Mn、Ce负载到酸处理后的椰壳活性炭(ACN)上,制备出采用浸渍法将活性组分Mn、Ce负载到酸处理后的椰壳活性炭(ACN)上,制备出Mn/CAN和Mn-Ce/ACN脱硝催化剂,在固定床上对所制备的催化剂进行了脱硝性能评价,着重探讨了两种活性组分的负载顺序、负载量对催化剂活性的影响,并对催化剂进行了BET、SEM、XRD、XPS表征。结果表明,通过比较Mn/CAN和Mn-Ce/ACN催化剂的脱硝活性,发现Ce的添加能明显提高催化剂的脱硝活性,在温度高于90oC时能达到90%以上的NO去除率,在120-250oC之间,NO转化率维持在100%。活性组分的负载顺序及负载量是影响催化剂活性的重要因素。同时负载活性组分,Ce、Mn负载量均为5%时,催化剂表现出最好的脱硝性能。Mn负载在活性炭上,降低了活性炭的比表面积和孔容,而Mn、Ce负载量均为5%的Mn-Ce/ACN的比表面积和微孔孔容降到695.0m2/g和0.130cm3/g,随着Mn、Ce负载量的增加,比表面积和孔容进一步降低;当Ce、Mn负载量均增加到10%时,其比表面积和微孔孔容只有539.8m2/g和0.106 cm3/g。Mn3+和Mn4+共存于两种催化剂上,而Ce4+ 和Ce3+共存并使Mn-Ce/CAN上Mn4+比例略微增加,导致催化剂表现出最好的脱硝性能.     

Low-cost preparation of mesoporous silica with high pore volume

Mesoporous silica materials with high pore volume were successfully prepared by the chemical precipitation method, with water glass and a biodegradable nonionic surfactant polyethylene glycol （PEG）. The obtained materials were characterized by transmission electron microscopy （TEM）, scanning electron microscopy （SEM）, thermo gravimetric analyzer and differential scanning calorimetry （TG-DSC）, nitrogen adsorption-desorption measurements, and X-ray diffraction （XRD）. The results showed that the changes of the pore parameters depended on both the surfactant content and heat treatment temperature. When the content of PEG was 10wt% and the obtained PEG/SiO2 composite was heated at 600℃, the mesoporous silica with a pore volume of 2.2 cma/g, a BET specific surface area of 361.55 m^2/g, and a diameter of 2-4 μm could be obtained. The obtained mesoporous silica materials have potential applications in the fields of paint and plastic, as thickening, reinforcing, and flatting agents.     

镧对WO3/ZrO2固体超强酸酸强度和结构的影响

通过共沉淀法制备了合适酸强度,比表面积为175.284 3 m2.g-1,最可几孔径在5.99 nm,负载镧的WO3/ZrO2固体超强酸催化剂。用Hammett指示剂法、XRD、N2等温吸附/脱附、DTA等方法考察了负载稀土镧后对催化剂的酸强度、比表面积、孔结构和热稳定性的影响。结果发现：La能均匀掺入WO3/ZrO2固体超强酸中,且适当加入稀土元素镧不但可以提高其酸强度,而且可以稳定结构、增加比表面积。     

Synthesis of carbon nanotubes with Ni/CNTs catalyst

Solid catalysts are widely used in industrial processes; their catalyses are closely related to not only the active elements but also support materials. The catalytic support plays the role of in-creasing surface area, dispersing active elements, improving heat resistance and mechanical strength. So it is requested that materials used as catalyst support should have excellent mechani-cal properties, enough thermal stability, proper pore structure and large surface area. The com-monly used supp…     

Effect of Adding Microwave Absorber on Structures and Properties of Hypercoal-Based Activated Carbons

Using lignite-based hypercoal as raw material,KOH as activator and CuO as microwave absorber,we prepared hypercoal-based activated carbons by microwave-assisted activation.The pore structure and the electrochemical performance of the activated carbons were tested,and the effects of adding CuO in the activation reaction process were also investigated.The activated carbons prepared were characterized by nitrogen adsorption-desorption,X-ray diffraction (XRD) and scanning electron microscopy (SEM).The specific surface area and mesoporous ratio of the hypercoal-based activated carbon are 1 257 m~2/g and 55.4%,respectively.When the activated carbons are used as the electrode materials,the specific capacitance reaches 309 F/g in 3 M KOH electrolyte.In comparison with those prepared without CuO absorber,the specific capacitance increases by 11.6%.It was proved that the addition of microwave absorber in microwave-assisted activation was a low-cost method for rapidly preparing activated carbon,and it could effectively promote the development of the pore structure and improve its electrochemical performance.