利用双头季铵盐合成特殊形貌的EU-1分子筛及其催化性能

以双头季铵盐C_(18-6-6)Br_2为辅助模板剂,分别通过水热法和蒸汽相法合成了具有特殊形貌的EU-1分子筛。利用XRD、SEM、NH_3-TPD和N_2吸附-脱附等手段对样品进行表征,使用二甲苯异构化作为探针反应进行催化性能评价。结果表明:双头季铵盐C_(18-6-6)Br_2的加入可明显改变EU-1分子筛的形貌,尤其在蒸汽相条件下作用效果更为显著,合成的EU-1分子筛形貌呈蜂巢形,同时其强酸量和弱酸量下降,总比表面积和总孔体积分别增加了83.65%和126.72%,二甲苯异构化反应中对二甲苯(PX)收率、选择性(Y(C_8))和催化活性([PX]/ΣX)均显著提高,分别增加了8.94%,6.44%和6.01%。     

新型NU-85分子筛的物性表征与合成时间优化

首次采用预置晶种法,以溴化六甲双铵(HMBr_2)为模板剂,(160～180)℃合成分子筛NU-85。采用XRD、SEM及FT-IR等表征手段对样品物性进行表征。结果表明,该合成样品NU-85分子筛为EU-1和NU-87共晶生长,具有典型的EU-1分子筛和NU-87分子筛的特征衍射峰,结晶度较高。SEM照片显示,合成NU-85分子筛形貌为较规整长方体的堆积层叠物,聚集现象较常见。实验考察NU-85分子筛的二甲苯异构化催化性能,发现产物具有较高的二甲苯异构化反应活性和选择性。     

HMS介孔分子筛合成及其在丙烷脱氢制丙烯反应中的应用

分别以正硅酸乙酯和伯胺表面活性剂为原料和模板剂成功制备HMS介孔分子筛，经负载活性组分后得到Pt-Sn/HMS催化剂并将其应用于丙烷脱氢制丙烯反应。探究合成过程中伯胺表面活性剂碳链长度及水和乙醇的比例对HMS介孔分子筛孔结构的影响。XRD和N₂吸附-脱附等分析结果表明，模板剂链长增长时，介孔分子筛孔径、孔壁厚、比表面积及孔容均增大。适当的水/乙醇比例有利于获得更大比表面积和孔体积的介孔分子筛，并表现出更有序的介孔结构。丙烷脱氢制丙烯反应评价和热分析等表征结果表明，HMS介孔分子筛孔道特征直接影响Pt-Sn/HMS催化剂的催化性能。使用孔体积且比表面积较大的HMS样品作为载体制备的脱氢催化剂在丙烷脱氢反应中表现出优异的催化活性。性能最优的Pt-Sn/HMS-0.60-16催化剂上，平均丙烷转化率达到46.5%,平均丙烯选择性为94.1%,反应24 h后积炭量仅为质量分数3.4%。     

无钠法合成EU-1分子筛及其催化性能

分别以四甲基氢氧化铵(TMAOH)、四乙基氢氧化铵(TEAOH)和氢氧化钠(NaOH)为碱源合成了EU-1分子筛,采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、氨气程序升温脱附(NH3-TPD)和低温N2吸附等对合成样品进行了表征,并以二甲苯异构化反应表征其催化性能。结果表明:与以NaOH为碱源相比,采用TMAOH和TEAOH可一步合成铵型EU-1分子筛,以TEAOH为碱源合成样品的粒径在200~500 nm之间,比表面积高达390.2 m2·g-1。     

ZSM-5/EU-1共生分子筛的可控合成及催化裂解性能

采用双模板剂两步晶化法设计合成了ZSM-5/EU-1共生分子筛,通过调整预晶化过程,实现了两种分子筛的共生和晶相比例的可控调变。研究两段凝胶组成的影响发现,第一段凝胶组成,尤其是模板剂浓度对所得共生样品晶相比例具有较大影响。与机械混合和纯相样品相比,ZSM-5/EU-1共生分子筛表现出最大的BET表面积和孔体积尤其是外表面积和介孔体积。而且EU-1相含量为39%的ZSM-5/EU-1共生分子筛在正己烷催化裂解制低碳烯烃反应中表现出比机械混合样品和ZSM-5分子筛更高的反应活性稳定性和低碳烯烃选择性,尤其是丙烯选择性。在反应120 min时,该共生分子筛上低碳烯烃选择性比相同EU-1相含量机械混合样品和ZSM-5分子筛均高出约10.7个百分点,丙烯选择性分别高出8.5和9.1个百分点,P/E比分别高出0.42和0.46。     

ZSM-5/EU-1共生分子筛的可控合成及催化裂解性能

采用双模板剂两步晶化法设计合成了ZSM-5/EU-1共生分子筛,通过调整预晶化过程,实现了两种分子筛的共生和晶相比例的可控调变。研究两段凝胶组成的影响发现,第一段凝胶组成,尤其是模板剂浓度对所得共生样品晶相比例具有较大影响。与机械混合和纯相样品相比,ZSM-5/EU-1共生分子筛表现出最大的BET表面积和孔体积尤其是外表面积和介孔体积。而且EU-1相含量为39%的ZSM-5/EU-1共生分子筛在正己烷催化裂解制低碳烯烃反应中表现出比机械混合样品和ZSM-5分子筛更高的反应活性稳定性和低碳烯烃选择性,尤其是丙烯选择性。在反应120 min时,该共生分子筛上低碳烯烃选择性比相同EU-1相含量机械混合样品和ZSM-5分子筛均高出约10.7个百分点,丙烯选择性分别高出8.5和9.1个百分点,P/E比分别高出0.42和0.46。     

含锆介孔分子筛的微波合成与表征(英文)

在微波辐射条件下,以硅酸钠和硫酸锆为原料、十六烷基三甲基溴化铵为模板剂合成含锆介孔分子筛(zirconium-containing mesoporous molecular sieves,Zr-MCM-41).用X射线粉末衍射、红外光谱,透射电子显微镜、等离子发射光谱和比表面积孔径测定等测试手段表征经550℃焙烧后样品,同时研究锆添加量与分子筛比表面积及孔体积之间的关系.结果表明:利用微波技术合成Zr-MCM-41介孔分子筛,操作便利,节能省时,所得产物具有典型的MCM-41介孔分子筛结构,其比表面积为598.1～971.4m2/g,平均孔径大约为2.46～3A3nm.随着介孔分子筛中锆含量的增加,介孔分子筛的比表面积、孔体积变小,介孔有序性变差.     

磷酸铝介孔分子筛的合成

选用了不同类型的表面活性剂作为模板剂合成磷酸铝介孔分子筛,实验结果表明,脂肪胺模板剂的浓度不会影响分子筛介孔相构型,介孔分子筛的孔径随烷基胺的链长增加而增大,其比表面积均达到了200 m2/g以上.类型相同的表面活性剂作模板剂时,分子筛的孔径和比表面积并不随其浓度增加而增加.所合成的磷酸铝分子筛TG和DTA曲线表明,磷酸铝分子筛在850 ℃以前具有一定的热稳定性.     

剑麻纤维素合成多级孔SAPO-11分子筛及其临氢异构化性能EI北大核心CSCD

用酸碱处理的剑麻纤维素作为模板剂,采用一步水热法合成多级孔SAPO-11分子筛。对合成分子筛的形貌、孔结构和酸类型进行表征;以正十二烷作为原料,考察Pt负载量为0.5%（质量分数）的SAPO-11分子筛的异构化反应性能。结果表明：利用酸碱处理后的剑麻纤维素合成的多级孔SAPO-11分子筛具有较大的BET比表面积,分子筛中有明显的介孔产生,分子筛孔道内B酸和L酸的比值增加,在正十二烷的临氢异构化反应中表现出更为优异的催化性能。在反应温度为320℃,反应空速为2.0 h^-1,反应压力为2 MPa,氢与油体积比为200：1条件下正十二烷转化率为95.36%时,异构烃收率为69.36%。     

剑麻纤维素合成多级孔SAPO-11分子筛及其临氢异构化性能

用酸碱处理的剑麻纤维素作为模板剂,采用一步水热法合成多级孔SAPO-11分子筛。对合成分子筛的形貌、孔结构和酸类型进行表征;以正十二烷作为原料,考察Pt负载量为0.5%(质量分数)的SAPO-11分子筛的异构化反应性能。结果表明:利用酸碱处理后的剑麻纤维素合成的多级孔SAPO-11分子筛具有较大的BET比表面积,分子筛中有明显的介孔产生,分子筛孔道内B酸和L酸的比值增加,在正十二烷的临氢异构化反应中表现出更为优异的催化性能。在反应温度为320℃,反应空速为2.0 h-1,反应压力为2 MPa,氢与油体积比为200:1条件下正十二烷转化率为95.36%时,异构烃收率为69.36%。     

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.     

季铵盐型改性淀粉辅助蒸汽相法合成多级孔EU-1沸石及其催化性能

以季铵盐型改性淀粉为介孔模板,采用蒸汽相法成功合成多级孔EU-1沸石。通过XRD,FT-IR,SEM,N_2吸附-脱附和NH_3-TPD等手段对合成样品的物化性质进行表征。研究表明:通过调节季铵盐型改性淀粉的量,样品的介孔孔容增加了0.081 cm~3/g,外表面积增加了23.35 cm~2/g。通过二甲苯异构化测试来考察样品的催化性能,发现:对二甲苯(PX)平衡浓度提高了0.88个百分点,乙苯的转化率提高了8.47个百分点,C_8烃收率提高了1.66个百分点。     

MOR/EU-1复合分子筛合成及其二甲苯异构催化性能

丝光沸石(MOR)为复合分子筛骨架载体,利用碱溶抽提活化有效硅铝,并保留MOR沸石骨架,以复配廉价模板剂代替溴化六甲双铵,水热晶化合成高纯度和高结晶度MOR/EU-1复合分子筛。以复合分子筛为酸性组元制备C8双功能异构化催化剂,在反应压力0.8MPa、反应温度653K、液体重时空速4.5h^-1和氢烃物质的量比4.0条件下,新型复合催化剂表现出优异的异构化催化性能,对二甲苯(PX)浓度([PX]/∑X)为23.58%,乙苯转化率为42.86%,C8烃收率为95.38%。     

Synthesis,characteristics of hierarchical EU-1 zeolite for xylene isomerization probe reaction

Introduced a method of synthesizing hierarchical EU-1 zeolite with organosilanes as additive, and studied the influences of following different kinds of organosilanes on the synthesis of hierarchical EU-1 zeolite: γ-glycidoxy propyl trimethoxy silane(GPTMS), N-β-(aminoethyl)-γ-aminopropyl methyl dimethoxyl silane(APAEDMS),and N-(β-aminoethyl)-γ-aminopropyl dimethoxyl(ethyoxyl) silane(TMPED). The hierarchical EU-1 samples were characterized by XRD, SEM, N_2 adsorption, FT-IR and NH_3-TPD to analyze the crystallinity, morphology, surface area, pore size distribution and acidity. The results showed that hierarchical EU-1 zeolites were successfully synthesized; organosilanes have great influence on crystal morphology of EU-1 zeolites; the exterior surface area of hierarchical EU-1 zeolite, which synthesized with organosilanes(APAEDMS) adding into synthesis system, increased by 62.1% and mesopore volume increased by 129.1% compared with conventional EU-1 zeolites, thus can reduce the diffusional restriction markedly in catalytic reaction. The catalytic performance of hierarchical EU-1zeolites were evaluated in m-xylene isomerization on fixed bed reactor. The catalytic data showed that the isomerization activity PX/X of the hierarchical EU-1 zeolites reached around 24.09% in theoretical thermodynamic equilibrium from 23.83%, and the selectivity of C_8 aromatic hydrocarbon increased from 75.16% to 84.87%. The conversion of p-xylene increased from 16.30% to 18.41%.     

Characterization of polystyrene latexes

Polystyrene latexes were prepared by emulsion polymerization. Styrene was used as monomer, potassium persulfate was the reaction initiator and sodium hydrogen carbonate was used as buffer. Surfactant may or may not be used. Three types of surfactant, ie sodium dodecylbenzene sulfonate (anionic), Triton X‐100 and Vulcastab LW (nonionic), and hexadecyltrimethyl ammonium bromide (cationic), were used. The prepared latexes were characterized according to concentration, density, pH, ionic strength, particle size, particle size distribution and surface charge. For prepared latexes with anionic surfactant, the effects of temperature, initiator concentration, surfactant concentration and amount of monomer on the latex size were investigated. Scanning electron microscopy was used as a tool for latex characterization. The results show that by increasing temperature, initiator and emulsifier concentration, the latex diameter decreases. However, size increases by increasing the amount of monomer. A potentiometric titration technique was employed for determination of surface charge. It was found that for all latexes, surface charge densities are in the same range. © 2000 Society of Chemical Industry     

Synthesis of layered MCM-22(P) in the presence of hexamethonium cations and its transformation into EUO- and MWW-type zeolites

Layered MCM-22(P) was synthesized in the presence of hexamethonium (HM) cations. Compared to zeolite EU-1 (EUO-type structure), which crystallizes in similar conditions, its formation is favored at high HM concentrations (HM/SiO₂ ≥ 0.3) and in the absence of Na₂O. HM-containing MCM-22(P) was used as starting material for zeolite formation. Upon hydrothermal treatment, HM-MCM-22(P) transforms into zeolite EU-1 and upon calcination into a MWW-type zeolite. Transformation mechanisms were studied by standard characterization techniques such as XRD, SEM and TEM. Catalytic properties of the MWW-type zeolite obtained from this precursor were evaluated in a m-xylene isomerization reaction. Compared to zeolite MCM-22 prepared with hexamethyleneimine, a higher catalytic activity and an increased isomerization selectivity were observed and discussed.     

Optimisation of Detergent Ingredients for Stain Removal Using Statistical Modelling

Artificially soiled test fabrics are widely used to study the cleaning performance of detergents formulations. In this study, artificial soiled cotton test fabrics were prepared in the laboratory using carbon black as a model soil. Design of experiments was used to optimise the concentration of detergent ingredients for stain removal. A multi‐factorial analysis of variance was used to model the effect of sodium dodecylbenzene sulfonate, nonylphenol ethoxylate, sodium silicate, sodium citrate and sodium carbonate as builders on soil removal. A colourimetric evaluation using the CIELAB system was used to measure soil removal. In general, performance increases with increasing concentration of surfactant, silicate and soda ash.     

硝酸溶液中十二烷基苯磺酸钠对锌的缓蚀作用及吸附热力学研究

采用失重法研究了硝酸介质中烷基磺酸盐类阴离子表面活性剂对锌的缓蚀及吸附作用,考察了在不同温度的3%硝酸中,不同浓度的十二烷基苯磺酸钠对锌的缓蚀作用。实验结果表明,十二烷基苯磺酸钠能很好的抑制锌的腐蚀,当其含量达到一定浓度后,缓蚀作用基本保持不变,而其在锌表面上的吸附是产生缓蚀作用的重要原因。在浓度为0~300 mg/L时,十二烷基苯磺酸钠在锌表面的吸附规律服从Langmuir吸附等温式。用Sekine方法处理实验数据,从而获得了ΔH0、ΔS0和ΔG0等一系列相关的热力学参数。     

系列磺酸钠型Gemini表面活性剂的合成及表征

通过两步反应,合成了三种磺酸钠型Gemini表面活性剂6, 6’-（丙基-1, 3-二基双氧）双（3-壬基苯磺酸钠）（9B-3-9B）、6, 6’-（正丁基-1, 4-二基双氧）双（3-壬基苯磺酸钠）（9B-4-9B）和6, 6’-（正戊基-1, 5-二基双氧）双（3-壬基苯磺酸钠）（9B-5-9B）,并讨论了反应温度和反应时间对产物产率的影响,优化了反应条件。利用傅里叶变换红外光谱仪（FTIR）、核磁共振仪（¹H NMR）和元素分析仪表征产物结构,并通过DCTA21表面界面张力仪测定其在水溶液中的表面张力。结果表明：与传统表面活性剂十二烷基苯磺酸钠（SDBS）相比,Gemini表面活性剂9B-m-9B（m=3, 4, 5）具有更高的表面活性,其临界胶束浓度（CMC）分别为0.14、0.11、0.12 mmol·L^-1,对应的表面张力g_CMC分别为29.43、29.26、28.22 mN·m^-1。