Synthesis of texture-excellent mesoporous alumina using PEG1000 as structure-directing agent

By varying concentration of PEG1000 as a structure-directing agent,mesoporous alumina with excellent textural properties was synthesized.The prepared mesoporous alumina displays high thermal stability,as shown by its textural properties at different calcination temperatures of 600-850 °C.Characterization by SEM and TEM revealed that the added PEG surfactant induced the formation of petal-like alumina.XRD results clarified that all samples were amorphous and their peaks were around the peaks of γ-alumina.N_2 adsorption-desorption analysis showed that the prepared mesoporous alumina,if with PEG1000 in hydrolysis of aluminum isopropoxide,had excellent textural properties with large specific surface area,high pore volume and suitable pore size.The petal-like structure existing in the alumina samples improved their textural parameters,and the role and influential mechanism of PEG1000 were analyzed.     

Effect of Ferric Chloride on the Properties of Biological Sludge in Co-precipitation Phosphorus Removal Process

This paper studied the effect of ferric chloride on waste sludge digestion, dewatering and sedimentation under the optimized doses in co-precipitation phosphorus removal process. The experimental results showed that the concentration of mixed liquid suspended solid (MLSS) was 2436 mg稬^-1 and 2385 mg稬^-1 in co-precipitation phosphorus removal process (CPR) and biological phosphorous removal process (BPR), respectively. The sludge reduction ratio for each process was 22.6% and 24.6% in aerobic digestion, and 27.6% and 29.9% in anaerobic digestion, respectively. Due to the addition of chemical to the end of aeration tank, the sludge content of CPR was slightly higher than that of BPR, but the sludge reduction rate for both processes had no distinct difference. The sludge volume index (SVI) and sludge specific resistance of BPR were 126 ml穏^-1 and 11.7?10¹² m穔g^-1, respectively, while those of CPR were only 98 ml穏^-1 and 7.1?10¹² m穔g^-1, indicating that CPR chemical could improve sludge settling and dewatering.     

Application Performance of Microporous Sintered Alumina in Alumina Magnesia Castables for Ladles

In this study, a kind of microporous sintered alumina was analyzed and applied. The microporous sintered alumina has a lot of nano and sub-micron closed pores in the crystals, the average pore size of 140 nm, and the thermal conductivity of 4.864 at 800 ℃, 38% lower than that of common sintered alumina. The microporous sintered alumina was used as the aggregates in alumina magnesia castables for ladles to replace the common sintered alumina. The properties of the microporous alumina castable were measured, and the temperature field of the ladle outer wall was simulated and calculated. The results show that the refractoriness under load(T0.6) and the hot modulus of rupture(1 400 ℃, 0.5 h) of the microporous castable are the same as the common castable; the thermal conductivity at 800 ℃ decreases by 15%; the retention ratio of modulus of rupture increases by about 5% after five thermal shock cycles(1 100 ℃, water quenching); and the temperature of the ladle outer wall is reduced by 5-41 ℃.     

Modification and sequential treatment of EU-1 zeolite in mild alkali and alkaline-acid conditions

EU-1 zeolites were sequentially treated with low-concentration sodium carbonate(Na_2CO_3) and hydrochloric acid(HCl) solutions.The obtained samples were characterized by X-ray diffraction(XRD),scanning electron microscopy(SEM),N_2 adsorption/desorption,temperature programmed desorption of NH_3(NH_3-TPD),solid state~(27)A1 nuclear magnetic resonance(~(27)A1 NMR),and the catalytic performances of the treated samples were tested in the xylene isomerization reaction.The results showed that the external surface area and mesoporous volume of the sample sequentially treated with 0.05 mol·L~(-1) Na_2CO_3 and 0.1 mol·L~(-1) HCl solutions reached73.9 m~2·g~(-1) and 0.162 cm~3·g~(-1),respectively.The catalytic performances of EU-1 zeolites were significantly improved,that the activity of the probe reaction increased from 23.03%to 23.61%and the selectivity increased from85.09%to 87.14%compared with those of parent sample.Furthermore,it was found that only amorphous silica and alumina species was dissolved during the post-treatment process,but the framework structure and the acidic properties of EU-1 zeolite remained intact.     

介孔SBA-15的孔径尺寸对小牛血清蛋白和溶菌酶蛋白吸附的影响(英文)

In this paper,the effects of pore-size of SBA-15 on the adsorption kinetics and equilibrium of large protein molecules Bovine serum albumin(BSA)and lysozyme(LYS)have been investigated.The mesoporous molecular sieve SBA-15 with six different pore sizes were synthesized with P123 triblock copolymer as the template agent,and 1,3,5-trimethylbenzene(TMB)and isopropyl alcohol as the pore-expanding agent.The samples were characterized by N2 adsorption/desorption,Scanning Electron Microscopy(SEM),Transmission Electron Microscopy(TEM)and X-Ray Diffraction(XRD).It is found that BSA and LYS were adsorbed rapidly on SBA-15 materials with large pores.The BSA adsorption capacity of sieve with the pore diameter of 21.4 nm reached 500 mg·g-1 within 25 minutes.However,if the pore diameter was smaller than 14 nm,the BSA adsorption capacity of the sieve was only about 220 mg·g-1.The adsorption equilibrium data fits in the Langmuir model,where the coefficient of effective use of specific area of mesoporous molecular sieve was found to be 0.03,0.18,0.37 and 0.48,corresponding to the pore diameter of 10.1 nm,13.2 nm,15.4 nm and 21.4 nm,respectively.The equilibrium loading amount of LYS on SBA-15 materials with pore size of 15.4 nm could be up to 1000 mg·g-1.The coefficient of effective use of surface area of mesoporous molecular sieve with diameter of 3.9 nm,7.4 nm,10.1 nm,13.2 nm and 15.4 nm was 0.10,0.47,0.56,0.71 and 0.79,respectively.It is also noted that greater pore size of mesoporous molecular sieve would lead to a higher coefficient of effective use of surface area.     

Corrosion of Alumina and Mullite Based Refractories by an Ingot Casting Steel

The corrosion of refractory crucibles by a highly corrosive steel(18CrNiMo7-6) with a high aluminum content and casting temperature of 1580℃ was investigated. The tested refractories were alumina,mullite and alumina doped with zirconia and titania( AZT). The samples were decreasingly attacked in the sequence AZT,alumina and mullite with corrosion layers of about 14,6 and 1 mm,respectively. In the alumina and AZT,compositions corresponding to manganese aluminates and subsequently manganese aluminosilicates formed with manganese and silicon from the steel. In the mullite crucible,compositions corresponding to manganese aluminosilicates formed directly with manganese from the steel giving a highly viscous interfacial melt which retarded the further corrosion.     

蠕虫形管状镧铝复合介孔材料的合成及表征

The lanthanum aluminum mesoporous materials were synthesized using sodium dodecyl sulfate as a template agent by ultrasonic hydrothermal method.The resulting samples were characterized by low angle X-ray diffraction(XRD),N2 adsorption-desorption studies,transmission electron microscopy(TEM)and surface morphology analysis(SEM),surface acid(NH3-TPD),reducibility properties(TPR),X-ray energy dispersive spectrometer(EDS)and thermogravimetric analysis(TG/DTG).A l/La composite mesoporous material were synthesized with n(Al)︰n(La)=70︰1.0,80°C of reaction temperature,20 h of reaction time,12 h of crystallization time,650°C of calcination temperature.The specific surface area of the sample is 273.90 m 2 ·g ?1 ,with the average diameter 5.642 nm and pore volume 0.2354 cm 3 ·g ?1 .The samples have mesoporous structure and its particles are similar to a worm-shaped tubular structure.The influence of calcination temperature on the surface physical and chemical properties of Al/La composited mesoporous materials was examined,and the results showed that the acid strength was increased but the amount of acidic sites is decreased as the calcination temperature increased.It was found that the sample calcined at 650°C had appropriate acid content,acid strength and better reducibility.     

Aluminum impregnated silica catalyst for Friedel-Crafts reaction:Influence of ordering mesostructure

Friedel-Crafts alkylation of benzene with linear chain olefin (C10-C14),which is an important reaction of synthetic detergent,was studied via different catalysts of aluminum impregnated silica molecular sieves.AlCl3 was immobilized on silica molecular sieves with different channel structures,hexagonal packing channels network (SBA-15,MCM-41),and disordered channel network (SiO2,SiO2-Gel) by impregnation.XRD and N2 adsorption-desorption isotherms confirmed that the specific mesoporous structures were maintained for order channel network catalyst after impregnation.Catalytic activities were investigated under different conditions.The influences of channel structure were discussed.The results showed that catalyst based on mesoporous like SBA-15 had the highest catalytic activities and 2-LAB selectivity compared with other catalysts in this work.The highest 2-LAB selectivity was nearly 50％ when 1-dodecene conversion was nearly 100％.At low 1-dodecene conversion or higher benzene/1-dodecene molar ratio,2-LAB selectivity was nearly 60％.     

Porous TiO2-coated Magnetic Core-Shell Nanocomposites: Preparation and Enhanced Photocatalytic Activity

The core-shell structured TiO₂/SiO₂@Fe₃O₄ photocatalysts were prepared using Fe₃O₄ as magnetic core, tetraethoxysilane (TEOS) as silica source and tetrabutyl titanate (TBOT) as titanium sources. The as-obtained structure was composed of a SiO₂@Fe₃O₄ core and a porous TiO₂ shell. The diameter of SiO₂@Fe₃O₄ core was about 205 nm with thickness of porous TiO₂ of about 5-6 nm. The 9%TiO₂/6% SiO₂@Fe₃O₄ microspheres possess the highest BET surface area and the BJH pore volume, which are 373.5 m²穏^-1 and 0.28 cm³穏^-1, respectively. The 9%TiO₂/6%SiO₂@Fe₃O₄ photocatalyst exhibited an excellent performance for the degradation of methyl orange and methylene blue dyes. Two different dyes were completely decolorized in 60 min under UV irradiation. The photocatalytic activity and the amount of catalyst were almost not decrease after recycling for 6 times by using external magnetic field.     

使用加热空气的预混天然气催化燃烧的实验研究

In this paper the premixed catalytic combustion emissions such as CO, unburned hydrocarbon （UHC）, NOx and the temperature distribution in the catalytic monolith with ultra low concentration of Pd were studied. Three types of monoliths were used for experiments and the temperature of preheated air was respectively 50℃, 100℃ and 200℃. The results showed that preheated air made radial temperature in the catalytic monolith uniform which helped to avoid local hot spots so as to decrease NOx emission. The experiment also proved that the shorter monolith showed much better catalytic combustion performance than longer one and the temperature at the exit of the shorter monolith was relatively lower. On the contrary, the temperature was higher in the longer monolith and the lethal NOx emission was slightly increased.     

无机铝源合成有序介孔氧化铝的影响因素研究

有序介孔氧化铝具有较大的比表面积、均匀且窄的孔径分布、有序的孔结构等特点,在多相催化反应及吸附分离过程中具有十分重要的应用价值,研究其合成及应用具有重要意义。以廉价的无机铝盐为铝源,结合模板剂,利用溶胶-凝胶法,通过改变模板剂的种类、老化时间和温度等影响因素,制备有序介孔氧化铝。采用多种测试技术对其结构进行表征,探讨不同反应条件对合成有序介孔氧化铝结构的影响规律。结果表明,以二正丙胺为模板剂,在40℃条件下老化48 h,可合成比表面积为324.80 m~2·g~(-1),孔容为0.62 cm~3·g~(-1),平均孔径为6.07 nm的介孔氧化铝,且孔径分布较窄,孔道有序性良好。     

炭化工艺对酚醛树脂基碳分子筛性能的影响

以工业酚醛树脂为碳源,三嵌段聚合物F127为模板剂,制备碳分子筛。采用N_2吸附-脱附对制备的碳分子筛进行表征,研究炭化制备工艺对碳分子筛孔径分布的影响。结果表明,炭化温度、炭化时间和炭化升温速率对碳分子筛孔径分布影响较大。在炭化升温速率为1℃·min~(-1)、炭化温度800℃和炭化时间1 h条件下制备的碳分子筛孔径分布最为集中,BET比表面积716.59 m~2·g~(-1),单点总孔容0.557 75 cm~3·g~(-1),单点吸附微孔孔容0.301 81 cm~3·g~(-1)。     

工业氟硅酸合成钛硅介孔分子筛催化环己烯环氧化

利用磷肥工业副产的氟硅酸为原料,在十六烷基三甲基溴化铵（CTAB）溶液中与氨水和钛酸四丁酯（TBOT）反应,水热陈化制取钛硅介孔分子筛,通过改变水热时间、CTAB的加入量、硅钛比和模板剂的脱除方法研究实验条件对钛硅介孔分子筛的结构和性能的影响,采用氮气吸脱附、扫描电镜、透射电镜和固体紫外漫反射对样品进行表征。结果表明,SiO₂:CTAB:TBOT:NH₃:H₂O的摩尔比为1:1.50:0.03:10:150,水浴时间为5 h时,所得样品的比表面积可达1116 m²·g^-1,介孔体积为0.79 cm³·g^-1。合成的钛硅介孔分子筛作为催化剂应用于环己烯环氧化反应,环己烯的转化率可达68.10%,环氧环己烷产物选择性为96.60%,Ti活性位的转化频率达到99.5 h^-1。该方法可以提高磷肥副产低浓度氟硅酸的附加值,降低钛硅介孔分子筛催化剂的生产成本。     

Al2O3@TiO2复合生物载体的制备及其BSA吸附特性

通过钛酸盐和氧化钛溶胶两种制备途径在氧化铝（Al₂O₃）支撑体外包覆介孔氧化钛（TiO₂）层,分析了这两种途径制备的氧化钛表面结构与性质的差异及其对于BSA蛋白吸附性能的影响。以粒径分别为0.37、10.4和21.8 mm的三种氧化铝支撑体作为基材,用XRD、Raman分析了两种路径制备的氧化钛晶型均为锐钛矿相;N₂吸脱附分析其比表面积均在（100±10）m²·g^-1,两者具有相似的介孔结构。FESEM分析发现钛酸钾溶胶制备的氧化钛的形貌受到支撑体孔径的影响。对于在牛血清蛋白（BSA）吸附实验中,钛酸钾溶胶法包覆的20 mm粒径复合载体（SP20@K-TiO₂）吸附量为22.18 mg·g^-1,高于相同条件下氧化钛溶胶制备的Al₂O₃@TiO₂复合载体。SP20@K-TiO₂ 中TiO₂吸附量为150.88 mg·g^-1,相比于TiO₂粉体,复合载体中TiO₂对BSA蛋白吸附的性能得到提升。     

水分子对HKUST-1甲烷吸附性能的影响

以三水合硝酸铜和均苯三甲酸为反应物、N,N’-二甲基甲酰胺为溶剂,采用溶剂热法合成金属有机骨架材料HKUST-1。将HKUST-1浸渍于等体积去离子水中,考察浸渍时间对其理化性能的影响,并通过XRD、SEM、BET和高压气体吸附表征研究了水分子对HKUST-1吸附甲烷性能的影响。结果表明,水分子易于吸附在HKUST-1中不饱和金属活性位点且对其骨架结构产生影响,浸渍72 h后,HKUST-1的BET比表面积和孔容分别从1 478.8 m2·g~(-1)和0.700 cm3·g~(-1)降至53.6 m~2·g~(-1)和0.005 cm3·g~(-1),在298 K和3.5 MPa条件下,甲烷吸附量从203.91 cm3·g~(-1)降至13.74 cm3·g~(-1)。但24 h浸渍后的HKUST-1骨架中生成一定数量的介孔,有利于较大的气体或液体分子吸附存储,值得深入研究。     

制备工艺对淀粉基碳分子筛性能的影响

以淀粉为碳源,F127为结构导向剂,通过KOH活化一步合成法制备系列碳分子筛,采用SEM、TG、FT-IR和N_2吸附-脱附等技术对原料和碳分子筛样品的结构、表面官能团和性能进行表征。结果表明,温度、F127与淀粉添加质量比和KOH浓度对碳分子筛样品的孔隙结构性能影响显著。在KOH浓度为0.75 mol·L~(-1)、m(F127)∶m(淀粉)=4∶3、搅拌时间12 h和反应温度45℃时制备的碳分子筛孔径分布集中,BET比表面积达1 228.972 5 m~2·g~(-1),单点孔容0.807 113 cm~3·g~(-1),单点微孔体积0.636 869 cm~3·g~(-1)。     

Ti/Zr复合纳滤膜的制备及其性能

通过聚合溶胶路线制备出稳定的Ti/Zr(摩尔比=1:1)复合溶胶。采用浸浆法,在平均孔径为5～6 nm的片状a-Al₂O₃/g-Al₂O₃载体上制备出完整无缺陷的Ti/Zr复合纳滤膜。详细考察了焙烧温度对Ti/Zr粉体的影响,并考察了Ti/Zr复合纳滤膜的性能。结果表明:在较高烧成温度下(500℃),Ti/Zr粉体依然呈无定形态且保持微孔结构。在400℃烧成温度下制备出孔径为1.49 nm的Ti/Zr复合纳滤膜,该膜的截留分子量(MWCO)为880,纯水通量为4.3 L·m^-2·h^-1·MPa^-1。在pH=6,压力0.8 MPa的条件下,该膜对0.005 mol·L^-1的MgCl₂、CaCl₂的截留率分别为85%和78%。     

K_2CO_3活化制备淀粉基碳分子筛

以可溶性淀粉为碳源、三嵌段共聚物F127为模板剂和K_2CO_3为活化剂,采用一步合成法制备系列淀粉基碳分子筛。通过扫描电子显微镜和N_2吸附-脱附分析淀粉基碳分子筛孔隙形貌和孔结构,采用热重-TG和傅里叶红外光谱表征原料和样品的物质结构官能团。结果表明,K_2CO_3浓度、F127添加比例、反应时间和反应温度影响淀粉基碳分子筛的孔隙结构。在炭化温度800℃、K_2CO_3浓度为0.50 mol·L~(-1)、F127与淀粉质量比=1∶3、反应温度50℃和反应时间12 h条件下制备的淀粉基碳分子筛,孔径集中于0.63 nm,比表面积为1 069.290 4 m~2·g~(-1),单点孔容0.667 901 cm~3·g~(-1)。     

葡萄糖基多孔碳材料对CO2/CH4的分离性能

以淀粉糖（主要成分为葡萄糖）为碳前体,制备了一系列多孔碳材料（C-GLCs-800）,对其进行孔隙结构分析,并应用FT-IR、SEM、TGA对其进行了表征,测定了材料在288、298和308 K下的CO₂和CH₄吸附等温线,根据IAST理论预测了材料对CO₂/CH₄二元体系的吸附选择性。实验结果显示,活化条件对材料的孔隙结构有明显影响,随着KOH/C质量比的增加,所制备的C-GLCs-800比表面积和总孔容先增加后降低。其中C-GLC-800-4的BET比表面积高达3153 m²·g^-1,总孔容为2.056 cm³·g^-1。C-GLC-800-2的窄微孔（V_d<1 nm,孔容0.3538 cm³·g^-1）含量最高,为30.63%。C-GLC-800-2在298 K和10⁵ Pa下对CO₂吸附量高达3.96 mmol·g^-1,明显高于许多传统吸附材料和MOFs材料在相同条件下对CO₂的吸附容量。应用Clausiuse-Clapeyron方程计算了CO₂和CH₄在材料上的吸附热,应用IAST理论计算了CO₂/CH₄的吸附选择性,结果显示C-GLC-800-2对CO₂/CH₄的吸附选择性为8.35。     

Ni~(2+)-Fe~(3+)-C_7H_7SO_3~--LDHs催化剂的制备

以尿素为沉淀剂,柠檬酸钠为络合剂,采用均相沉淀法制备Ni~(2+)-Fe~(3+)-CO_3~(2-)-LDHs。以制备的Ni~(2+)-Fe~(3+)-CO_3~(2-)-LDHs为前驱体,分别与Na Cl和对甲苯磺酸钠进行离子交换反应得到Ni~(2+)-Fe~(3+)-C_7H_7SO_3~--LDHs新型催化剂,成功实现对甲苯磺酸根负载Ni~(2+)-Fe~(3+)-LDHs。研究表明,Ni~(2+)-Fe~(3+)-C_7H_7SO_3~--LDHs为介孔材料,比表面积为165.6 m~2·g~(-1),平均孔径为14.7 nm,较大比表面积和空隙结构增强了其吸附性能和催化活性。