活性炭负载硫化锡纳米颗粒作为高效可重复使用Lewis酸催化剂催化三组分一锅法合成4H-吡喃[2,3-c]吡唑衍生物(英文)

Tin sulfide nanoparticles(SnS -NPs) were prepared in aqueous solution at room temperature on the surface of activated carbon(AC) and were investigated using field-emission scanning electron mi-croscopy(FE-SEM), transmission electron microscopy(TEM), X-ray diffraction, reflective ultravio-let-visible spectrophotometry, and spectrofluorimetry. Calculations based on the SEM and TEM images showed that the sizes of the SnS -NPs immobilized on the AC were 30–70 nm. The prepared nanocomposite was used as a heterogeneous Lewis acid catalyst for the three-components one-pot synthesis of 4H-pyrano[2,3-c]pyrazole derivatives in ethanol at 80 ℃. The reactions were efficiently performed in the presence of the prepared catalyst in short reaction times, and gave the desired products in high yields. This catalyst can be easily recovered by simple filtration and recycled up to eight consecutive times without significant loss of its efficiency.     

镧-镍复合氧化物纳米微粒的固相合成及其催化性能

The La-Ni complex oxide catalyst was prepared by solid state reactions under microwave. The structure and reducibility of the catalyst were characterized by using TG-DTA, XRD, TEM and TPR methods. At the same time the catalytic activity of oxidative dehydrogenation of ethylbenzene to styrene with carbon dioxide over the complex oxide nanoparticle was investigated.The Results show that the product is K2NiF4 nanoparticles,and the size is 13nm.The complex oxide sample had high activity for the oxidative dehydrogenation of ethylbenzene to styrene.     

Impact and mechanism of TiO_2 nanoparticles on DNA synthesis in vitro

The impact of TiO2 nanoparticles on DNA synthesis in vitro in the dark and the molecular mechanism of such impact were studied. The impact of TiO2 nanoparticles on DNA synthesis was investigated by adding TiO2 nanoparticles in different sizes and at various concentrations into the polymerase chain reaction (PCR) system. TiO2 nanoparticles were premixed with the DNA polymerase, the primer or the template, respectively and then the supernatant and the precipitation of each mixture were added into the PCR system separately to observe the impact on DNA synthesis. Sequentially the interaction be- tween TiO2 nanoparticles and the DNA polymerase, the primer or the template was further analyzed by using UV-visible spectroscopy and polyacrylamide gel electrophoresis (PAGE). The results suggest that TiO2 nanoparticles inhibit DNA synthesis in the PCR system in the dark more severely than mi- croscale TiO2 particles at the equivalent concentration and the inhibition effect of TiO2 nanoparticles is concentration dependent. The molecular mechanism of such inhibition is that in the dark, TiO2 nanoparticles interact with the DNA polymerase through physical adsorption while TiO2 nanoparticles do with the primer or the template in a chemical adsorption manner. The disfunction levels of the bio-molecules under the impact of TiO2 nanoparticles are in the following order: the primer > the tem- plate > the DNA polymerase.     

磷掺杂TiO2薄膜的制备与表征及其可见光照射下光催化降解邻苯二甲酸丁苄酯性能（英文）

P‐doped TiO2 (PTIO) thin‐films with different P contents were prepared using a sol‐gel method. The thin‐film samples were characterized using various techniques. The photocatalytic activity was evaluated by decomposing butyl benzyl phthalate under visible‐light irradiation. The results showed that the transformation of anatase to the rutile phase was inhibited and grain growth of TiO2 was prevented by P doping. The results confirm that the doped P atoms existed in two chemical forms, and those incorporated in the TiO2 lattice may play a positive role in photocatalysis. The high photocatalytic activities of the PTIO thin‐films may be the result of extrinsic absorption through the creation of oxygen vacancies, rather than excitation of the intrinsic absorption band of bulk TiO2 . The PTIO can be recycled with little depression of the photocatalytic activity. After six cycles, the photocatalytic activity of the PTIO film was still higher than 98%.     

Mechanical and thermal properties of nanosized titanium dioxide filled rigid poly(vinyl chloride)

Nano-sized rod-like titanium dioxide (TiO2) filled rigid poly(vinyl chloride) (PVC) nanocomposites were prepared by using injection-molding method. Vicat, Charpy impact and tensile tests as well as thermogravimetric and dynamic mechanical analyses were used to characterize the structure and properties of the nanocomposites. The results showed that nano-TiO2 could improve Vicat softening temperature and also improve thermal stability of PVC during the stages of dehydrochlorination and formation of carbonaceous conjugated polyene sequences, which can be ascribed to restriction of the nanoparticles on the segmental relaxation as being evidenced by raises in glass transition and β-relaxation temperatures of PVC upon filling TiO2. Addition of TiO2 nanoparticles less than 40 phr (parts per hundreds of resin) could significantly improve impact strength of the composites while the TiO2 agglomeration at high contents leads to a reduction in impact toughness.     

A New Method for Preparing Ti-Si Mixed Oxides

Ti-Si mixed oxides with different TiO2 content were prepared by sol-gel one step hydrolysis, using TiCl4 as the precursor. The samples were characterized by BET, FT-IR and XRD. The results indicated that titanium is in fourfold coordination with oxygen in the SiO4^4- in mixed oxides, form the bond of Ti-O-Si, and the low titania materials are mixed on an atomic scale.The phase of anatase appeared when TiO2 content is up to 80%. The mixed oxides had high specific surface areas up to 681.5 m^2/g. 10TiSi is a better support than SiO2 in the reaction of CO oxidation.     

Partially crystallized Pd nanoparticles decorated TiO2 prepared by atmospheric-pressure cold plasma and its enhanced photocatalytic performance

TiO2 decorated with partially crystallized Pd nanoparticles （Pd/TiO2-P） was successfully prepared by atmospheric-pressure dielectric barrier discharge cold plasma. The XRD and XPS analyses proved that Pd ions were reduced to partially crystallized metallic Pd nanoparticles in Pd/TiO2-P. The XPS spectra also indicated that an enhanced metal-support interaction was formed due to the existence of partially crystallized Pd nanoparticles with lower coordination number in Pd/TiO2-P. Photocatalytic activity of Pd/TiO2-P was much higher than that of TiO2 samples decorated with well crystallized Pd nanoparticles.     

Structure and Property Characterization of Oyster Shell Cementing Material

Oyster shell powder was used as the admixture of ordinary portland cement.The effects of different addition amounts and grinding ways on the strength and stability of cement mortar were discussed and proper addition amount of oyster shell powder was determined.The structure and property changes of cementing samples with different oyster shell powder contents were tested by XRD and SEM means.The results revealed that compressive and rupture strengths of the sample with 10% oyster shell powder was close to those of the original one without addition.Stability experiment showed that the sample prepared by pat method had smooth surface without crack and significant expansion or shrinkage after pre-curing and boiling,which indicated that cementing material dosed with oyster shell powder had fine stability.XRD and SEM observation showed that oyster shell independently exists in the cementing material.     

Effect of Preparation Methods of Bi2O3 Nanoparticles on their Photocatalytic Activity

Bi2O3 nanoparticles were prepared by means of ammonia precipitation, polyol mediated methods and microemulsion chemical method. The structure and properties of the as-prepared nanoparticles, having been submitted to a heat-treatment test at 750℃, were characterized by means of XRD. BET, XPS and UV-Vis absorption techniques. The photocatalytic oxidation reactions of benzene, toluene and xylene were used as the model reaction to measure the photocatalytic activity of Bi2O3 nanoparticles, respectively. The results show that the crystallite size of Bi2O3 prepared with different methods and calcined at 750℃ were 50. 6, 38.5 and 31.5 nm, respectively. The photocatalytic activity of Bi2O3 nanoparticles prepared with the microemulsion chemical method was higher than that of the particles prepared with the polyol mediated method; and that of the particles prepared with the micromulsion chemical method was the highest among the three. The degradation rates of the three pollutants xylene, toluene and benzene decreased in sequence.     

可见光下具有高光子效应和光催化活性的CuS-石墨烯氧化物/TiO2复合材料的制备（英文）

CuS-graphene oxide/TiO2 composites were prepared using a sol-gel method to improve the photocatalytic performance of the photocatalyst. The composites were characterized by X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray analysis, and transmission electron microscopy. The photocatalytic activities were examined by the degradation of methylene blue (MB) under visible-light irradiation. The photodegradation of MB under visible-light irradiation reached 90.1% after 120 min. The kinetics of MB degradation was plotted alongside the values calculated from the Langmuir-Hinshelwood equation. The CuS-graphene oxide/TiO2 sample prepared using 0.2 mol of TiO2 showed the best photocatalytic activity. This was attributed to a cooperative reaction as a result of increased photoabsorption by graphene oxide and an increased photocatalytic effect by CuS.     

Enhanced photocatalytic degradation of C.I. Basic Violet 2 using TiO2-SiO2 composite nanoparticles

In this report, TiO(2) -SiO(2) composite nanoparticles were prepared by the thermal hydrolysis method using titanium tetrachloride and tetraethylorthosilicate as TiO(2) and SiO(2) precursors, respectively. The prepared nanoparticles were characterized by X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), nitrogen adsorption/desorption and UV-Vis diffuse reflectance spectroscopy (DRS). The results indicated that, in comparison with pure TiO(2), TiO(2)-SiO(2) composite nanoparticles had a higher thermal stability, which prevents phase transformation from anatase to rutile. In addition, the TiO(2)-SiO(2) nanoparticles had a higher specific surface area, larger pore volume, greater band gap energy and smaller crystallite size. Thus, the surface area of TiO(2)-40% SiO(2) composite nanoparticles was about 17 times higher than that of pure TiO(2) nanoparticles. The photocatalytic activity of TiO(2)-SiO(2) composite nanoparticles in the photodegradation of C.I. Basic Violet 2 was investigated. The photodegradation rate of Basic Violet 2 using TiO(2)-40% SiO(2) nanoparticles calcined at 600°C was much faster than that using pure TiO(2) and Degussa P25 TiO(2) by 10.9 and 4.3 times, respectively. The higher photoactivity of the TiO(2)-SiO(2) composite nanoparticles was attributed to their higher surface area, larger pore volume, greater band-gap energy and smaller crystallite size compared with pure TiO(2).     

TiO2/ACF的制备及光催化降解四氯乙烯性能

以钛酸四丁酯为前驱物,活性炭纤维(ACF)为载体,蔗糖为胶粘剂,采用真空吸附水解的方法制得了TiO₂/ACF催化剂.采用BET、XRD、SEM等手段对其物理化学特性进行表征,以四氯乙烯光降解反应为探针反应,考察了TiO₂/ACF催化剂的光催化降解性能.实验结果表明,采用真空吸附水解法可以将TiO₂很好地负载到活性炭纤维表面上.通过优化条件制备的TiO₂/ACF催化剂在光照2h条件下,可以将水中溶解量的四氯乙烯降解90%以上.催化剂可以多次循环使用,光催化反应活性不变.     

Gold-Titanium(IV) Oxide Plasmonic Photocatalysts Prepared by a Colloid-Photodeposition Method: Correlation Between Physical Properties and Photocatalytic Activities

Colloidal gold (Au) nanoparticles were prepared and successfully loaded on titanium(IV) oxide (TiO(2)) without change in the original particle size using a method of colloid photodeposition operated in the presence of a hole scavenger (CPH). The prepared Au nanoparticles supported on TiO(2) showed strong photoabsorption at around 550 nm due to surface plasmon resonance (SPR) of Au and exhibited a photocatalytic activity in mineralization of formic acid in aqueous suspensions under irradiation of visible light (>ca. 520 nm). A linear correlation between photocatalytic activity and the amount of Au loaded, that is, the number of Au nanoparticles, was observed, indicating that the activity of Au/TiO(2) plasmonic photocatalysts can be controlled simply by the amount of Au loading using the CPH method and that the external surface area of Au nanoparticles is a decisive factor in mineralization of formic acid under visible light irradiation. Very high reaction rates were obtained in samples with 5 wt % Au or more, although the rate tended to be saturated. The CPH method can be widely applied for loading of Au nanoparticles on various TiO(2) supports without change in the original size independent of the TiO(2) phase. The rate of CO(2) formation also increased linearly with increase in the external surface area of Au. Interestingly, the TiO(2) supports showed different slopes of the plots. The slope is important for selection of TiO(2) as a material supporting colloidal Au nanoparticles.     

TiO2-yNx纳米光催化剂的制备及其可见光响应机理

利用溶胶-凝胶技术,以尿素为氮源,采用原位掺杂方式制备了TiO2-yNx纳米粉体;以亚甲基蓝(MB)溶液在可见光下的光催化降解评价其可见光催化活性;考察了体系初始pH值、N的掺杂量和焙烧温度对样品可见光催化活性的影响。 结合XRD、XPS、ESR和DRS测试技术,研究了N掺杂纳米TiO2的可见光响应机理。 研究结果表明,TiO2-yNx纳米粉体的优化制备工艺条件为：体系初始pH=0.52,掺杂比n(N)∶n(Ti)=1∶6,焙烧温度为440 ℃。 此条件下制备的样品N含量为0.77%,为单一的锐钛矿相,平均粒径为19.0 nm,具有良好的可见光催化活性。 N掺杂导致TiO2纳米粉体的表面羟基含量增加,形成了大量束缚单电子的氧空位;N取代晶格O形成了N-Ti-O和O-N-Ti键合结构。 N掺杂导致TiO2纳米粒子的吸收带边红移,对可见光的吸收能力明显增强,这表明N掺杂改变TiO2电子结构,使带隙窄化,降低光响应阈值。 N掺杂TiO2纳米粒子的可见光响应归因于N取代掺杂形成的掺杂能级与氧空位形成的缺陷能级共同作用所致。     

TiO2与ZnO复合纳米结构电极的光电化学研究

利用尿素加压共沉淀法以Ti(SO4)2与Zn(NO3)2为原料制备了TiO2-ZnO复合纳米粒子, 其纳米结构电极的光电化学研究结果表明, 反应物摩尔比为3∶1, 于530 ℃煅烧制备的复合纳米结构电极的光电转换效率最高. 对吸附染料RuL2(SCN)2∶2TBA的纳米结构TiO2和各种复合纳米粒子的纳米结构电极进行光电研究的结果表明, 染料对各纳米结构电极都起到了敏化作用, 其中也是由反应物摩尔比为3∶1, 于530 ℃煅烧制备的纳米结构电极的光电转换效率最高. 对聚3-甲基噻吩修饰的纳米结构TiO2和摩尔比为3∶1, 于530 ℃煅烧的复合纳米粒子构成的纳米结构电极进行光电性能研究, 结果表明, 聚3-甲基噻吩与半导体纳米粒子之间存在p-n结, 在一定条件下p-n结的存在有利于光生电子/空穴的分离, 从而提高了光电转化效率.     

类蛋结构的可磁分离光催化剂纳米球的制备及催化性能

通过反胶束和静电自组装方法制备了一种类蛋结构的可磁分离光催化剂纳米材料SiO₂@NiFe₂O₄@TiO₂(TSN), 这种光催化剂对甲基橙废水有较好的降解效果, 并显示出了超顺磁性, 通过外加磁场方便地实现催化剂在水中的分离与回收. 该光催化剂纳米球的X射线衍射, TEM和FTIR结果表明, 铁酸镍纳米粒子被包裹在SiO₂内, 形成SiO₂@NiFe₂O₄(SN)纳米球载体, 纳米TiO₂颗粒组装在SN表面, 形成TiO₂光催化壳层. 利用甲基橙的降解考察了光催化剂纳米球的活性, 结果表明, 在NiFe₂O₄和TiO₂之间包覆一层无定形的SiO₂可以显著提高光催化剂纳米球TSN的催化活性.     

Hydrothermal synthesis, characterization, and photocatalytic performance of silica-modified titanium dioxide nanoparticles

Silica-modified titanium dioxides were prepared by a hydrothermal method and then characterized by XRD, FT-IR, XPS, TEM, and UV-visible spectroscopy. The silica-modified titanium dioxides were in anatase phase and had large surface areas. There was strong interaction between SiO2 and TiO2, and TiOSi bonds formed during the hydrothermal process. The addition of silica in TiO2 particles could effectively suppress the formation of the rutile phase and the growth of titanium dioxide crystals. DRS spectra proved an increase in the band-gap transition with the increase of silica. The silica-modified TiO2 nanoparticles exhibited better photocatalytic activity, which increased with the silica amount, in comparison with pure TiO2 nanoparticles. Due to better thermal stability, the photocatalytic activity of the silica-modified TiO2 sample held good photocatalytic activity even after calcined at 1273 K.     

TiO2纳米粒子包覆聚苯乙烯球的结晶性能与表面光电压特性

TiO2具有很高的光催化活性，同时TiO2纳米粒子具有耐酸碱和耐光化学腐蚀、低成本、无毒等性质，在许多领域引起广泛关注．据报道，TiO2的锐钛矿晶型比金红石晶型具有更好的光催化活性．由于金红石是TiO2的热力学稳定相，而锐钛矿是亚稳相，通常锐钛矿相在550-800℃温度范围内形成金红石相，从而降低其催化活性，限制了其应用．     

TiO2/活性炭负载型光催化剂的溶胶-凝胶法合成及表征

以钛酸四丁酯为钛源,采用溶胶-凝胶法在多孔活性炭(AC)表面合成TiO2前驱体,在氮气保护下程序升温处理制得TiO2/AC负载型光催化剂.采用X射线衍射、漫反射光谱、傅里叶变换红外光谱、扫描电镜、能量色散谱和低温液氮吸附等对光催化剂晶相结构、光谱特征及表面结构进行了表征.结果表明,AC可提高TiO2分散性能,降低TiO2团聚体的尺寸,并抑制其由锐钛矿相向金红石相的转变.TiO2与AC接触界面处有Ti-O-C键生成.另外,AC的含量对TiO2的能阈结构和晶粒大小影响不大.苯酚溶液的光催化降解测试结果表明,AC负载可为TiO2提供高浓度反应环境,适宜量的负载可显著提高TiO2对有机稀溶液的光催化降解活性.对于50mg/L苯酚的光催化降解,AC的质量分数分别为5%,9%和11%时催化剂协同系数分别为1.1,1.5和1.3.循环使用7次后,AC含量为9%的催化剂对苯酚的降解率仍达95.84%.     

高纯纳米氧化钛的制备及催化活性

以工业级硫酸钛为原料,在酸性环境下以EDTA作为络合剂,采用控制沉淀法制备高纯度纳米TiO2。考察了pH值、反应温度、煅烧温度等工艺条件对TiO2颗粒晶型、大小和分布影响。利用TEM、XRD、ICP等手段对产物进行表征,TiO2纯度超过99.9%,粒径为10-20nm,分布均匀。经过对其光催化降解苯酚反应活性实验,结果表明样品具有较好的光催化活性。