L-天冬酸插层水滑石的组装及其结构表征

以镁铝水滑石(Mg-AlLDHs)为插层主体、L-天冬酸离子为插层客体,分别用返混沉淀法和共沉淀法制备了L-天冬酸根插层镁铝水滑石手性层柱材料,并用FT-IR、XRD和DTA对其结构进行了表征.实验结果表明,用这两种方法制备的L-天冬酸插层镁铝水滑石都具有良好的结晶度和规整的层状结构,L-天冬酸根垂直插层后的特征衍射峰(003)的层间距在1.22～1.27 nm之间,并得出了超分子结构模型.     

丙烯酸根离子柱撑Mg-Al-LDHs水滑石的合成及紫外屏蔽性能研究

以Mg-Al水滑石为前体,采用返混沉淀法进行插层组装合成丙烯酸根离子柱撑水滑石.利用红外光谱、X射线衍射、紫外分光光度法对其结构和性能进行了表征.结果表明,丙烯酸根阴离子可以插入纳米Mg-Al水滑石层间,其层间距由0.76nm增大到1.17nm,形成具有超分子结构的丙烯酸根离子柱撑水滑石,并模拟出其分子结构模型.这种新的插层结构材料可以增强其紫外吸收性能,进而使得其紫外屏蔽作用增强,从而成为一种集屏蔽和吸收双重功能的新型无机-有机复合紫外阻隔材料.     

MgCuAl类水滑石的制备及插层聚合与结构表征

以共沉淀法制备了间氨基苯甲酸插层水滑石(LDHs)复合材料,借助X射线衍射、红外光谱、热失重分析等手段对样品进行表征。结果表明,客体成功进入层间,层间距由0.79 nm扩至1.54 nm,并给出了层间排列模型,组装后依然保持良好的层状结构,且客体进入层间提高了自身的热稳定性。采用热聚合和引发剂引发聚合层间间氨基苯甲酸,引发剂质量大于0.05 g时,LDHs层间距由1.54 nm减小到1.43 nm和1.42 nm,间氨基苯甲酸单体在层间发生了聚合,推测了聚合机理。LDHs可以作为制备聚合物粒子的"微反应器"。     

乙二胺四乙酸根插层镁-铝水滑石的制备与性能

通过共沉淀法合成乙二胺四乙酸根(EDTA~(4-))插层的镁-铝水滑石(MgAl-EDTA-LDH),并采用X射线衍射和红外光谱对其结构和化学组成进行表征,研究MgAl-EDTA-LDH对水溶液中铜离子的去除能力。结果表明,乙二胺四乙酸根已插入镁-铝水滑石的层间,且插层水滑石能有效吸附水溶液中的铜离子,在2 h时吸附效率可达93.05%。     

管状纳米氧化物的制备与表征

利用共沉淀法合成苯甲酸根插层镁铝水滑石,并在温度为800℃时对插层水滑石进行焙烧;采用X射线衍射、红外光谱、透射电子显微镜、扫描电子显微镜、X射线能量色散谱等分析手段对制得的样品进行表征。结果表明,800℃焙烧后的样品出现卷曲得较完整的纳米管状结构,平均管长约为10μm,管径约为1μm。     

L-(-)-苹果酸柱撑水滑石的合成及结构表征

用返混沉淀方法和共沉淀法实现了L-(-)-苹果酸柱撑水滑石(LDHs)超分子结构手性层柱材料的插层组装, 得到结晶度高、晶相单一,且L-(-)-苹果酸在层间垂直插层有序排列的超分子结构手性层柱材料.用X射线衍射、红外光谱及差热分析表征了超分子结构手性层柱材料的结构,并给出了L-(-)-苹果酸柱撑水滑石超分子结构模型.     

D-(+)-对甲基二苯甲酰酒石酸插层锌铝水滑石的制备及表征

以Zn0.676Al0.328(OH)2(NO3)0.377·0.682H2O为前体,无水乙醇作分散剂,在pH值为5～6、温度80℃条件下采用离子交换法组装了手性拆分剂D-(+)-对甲基二苯甲酰酒石酸(DTTA)插层锌铝水滑石,并采用XRD、FT-IR、DSC-TG、ICP和EA等现代物理化学分析技术对样品进行表征.结果表明,通过控制离子交换条件,可成功将DTTA插入到锌铝水滑石层间,得到的有机-无机复合材料结构完整,晶相单一,具有良好的层状结构,其层间距从0.90nm扩大为2.07nm.DTTA插入水滑石后,完全燃烧分解温度从346℃升高到470℃.     

荧光发色团插层镁铝水滑石的制备和光物理性质

以层状镁铝水滑石[Mg 0.66 Al 0.34(OH)2](CO3)0.17.0.67H2O为主体,通过离子交换法,分别将乙基橙(EO-)和4-氨基偶氮苯基-4-磺酸阴离子(4A-)插入到层状镁铝水滑石层间和吸附在镁铝水滑石表面.插层产物及表面吸附产物分别采用XRD、IR、TG-DTA等测试技术进行结构表征,采用UV-Vis吸收光谱和荧光光谱研究其光谱特征.并用G03w软件包中ab initio分子轨道法(HF/6-31G)计算了客体分子结构和电荷分布,认为客体阴离子以单层形式垂直排布于层板之间.结果表明,客体进入层间后,由于客体与主体的相互作用,在限域空间内客体微环境的改变造成荧光发射强度发生改变,与纯客体相比EO插层产物的荧光强度提高,而4A插层产物的荧光发射强度却大大减弱,EO与4A的吸附产物荧光发射强度均降低,说明通过主体与客体或客体与客体的相互作用可以改变客体的光物理性质.     

Zn-Al—[V10O28]^6-水滑石在镁合金防腐中的机理研究

采用化学共沉淀法制备一种环境友好、可以吸附腐蚀性阴离子、释放缓蚀剂的钒酸盐插层锌铝水滑石新型颜料用于镁合金的抗腐蚀保护。采用N2吸附-脱附等温线,ICP分析以及极化曲线的方法研究此水滑石的吸附和抗腐蚀机理;通过盐雾试验检验钒酸盐插层锌铝水滑石/环氧涂层对镁合金的抗腐蚀保护性能。结果表明:该材料防腐蚀性能优良,可以为镁合金基体提供阳极钝化和屏障式双重保护功能。     

二维层状磁性镁铝水滑石的制备与表征

采用共沉淀法将磁性基质与镁铝水滑石组装制备二维层状磁性镁铝水滑石,考察了在一定的pH值、沉淀生成温度及陈化时间下,不同n(Mg2 )/n(Al3 ),n(Fe2 )/n(Mg2 )比值及焙烧温度对合成磁性镁铝水滑石结构的影响,并借助HRTEM、XRD、VSM、TG-DSC、FT-IR等手段对其晶型结构、磁学性能及结晶度等进行表征,结果表明镁铝水滑石在赋予磁性后,并没有改变其典型的层状结构,证实了将磁性基质与层状材料组装合成的可行性.     

铁铝柱撑二硫化钼的合成与表征

采用取代反应获得了具有Keggin结构的聚合羟基铁铝离子,并通过单分子层技术将聚合羟基离子嵌入到二硫化钼的层间,制得了层间距1.394至1.513nm的柱撑二硫化钼复合材料.研究表明,随着Fe/Al比的增加,层间距逐渐下降,颗粒度逐渐增大,比表面积逐渐降低.催化实验表明,柱撑材料将S2-催化氧化为S2O3^2-,其催化活性是2H-MoS2的4～5倍,且光催化活性大于催化活性.这与材料比表面积增加所导致催化活性部位的增多,以及光致电子-空穴对的产生有关.     

水滑石作为药物载体--萘普生的插层和缓释

水滑石(LDHs)是由带正电荷类水镁石层和层间的可交换阴离子组成的阴离子型粘土化合物,由于它的生物适应性,能够以它为主体,以药物为客体,插层组装成超分子结构复合物.抗炎药萘普生采用共沉淀法一步插层进入LDHs,用X射线衍射、红外光谱及热分析方法表征了超分子结构,表明层间距离扩大了,即萘普生已经插层组装成功,并且以单层、垂直作用在层间.萘普生柱撑水滑石的药物释放度在模拟肠液(pH7.4的缓冲液)条件下测定,结果表明萘普生柱撑水滑石释放速度降低,具有缓释作用,说明药物--无机混合物材料能够用作有效的药物传输系统.     

Reduction of residual stress in montmorillonite/epoxy compounds

An epoxy resin was cured while in intimate contact with small amounts of epoxyphilic montmorillonites. It was determined that cured epoxy exists within the montmorillonite interlayer by the observation of very high interlayer spacings, even greater than 8 nm, Generally, epoxy compounds containing montmorillonites that had been swollen in the curing agent prior to curing exhibited larger interlayer spacings, especially among the non-dispersed montmorillonite layers. The maximum observed residual stress was reduced by greater than 50% in the epoxyphilic montmorillonite/epoxy compounds over that of the pure epoxy. The epoxyphilic montmorillonite/epoxy compounds generally exhibited higher values of glass transition temperature, flexural modulus, and ultimate flexural strength than the pure epoxy. The tyramine-montmorillonite compounds typically had the highest values overall.     

Synthesis of Ga2O3-pillared fluorine micas

Synthesis of gallium oxide pillared fluorine micas has been undertaken by using hydroxogallium solutions having different OH/Ga ratios and aging conditions as pillaring agents. The gallium oxide pillared fluorine micas obtained from aged hydroxogallium solutions have larger basal spacings and higher specific surface areas than those obtained from freshly prepared hydroxogallium solutions. Thermal durability of the pillared structure depends on the aging conditions of the hydroxogallium solutions; thermal durability of the pillared micas was enhanced by using the solutions aged under the optimized conditions. The pillared micas obtained from the hydroxogallium solution (OH/Ga = 2.0) aged at room temperature for 24 hours retained larger basal spacings and specific surface areas even after heated up to 750 °C.     

微波场下纳米Mg-Al-LDHs及PO_4~(3-),P_2O_7~(4-)柱撑Mg-Al层状双氢氧化物的合成

用微波加热反应-变速滴加共沉淀法合成了[Mg-Al-CO3]纳米层状双氢氧化物,并以[Mg-Al-CO3]纳米层状双氢氧化物为前体,用微波加热反应-离子交换法制备了PO43-,P2O74-柱撑Mg-Al层状双氢氧化物。该法合成的[Mg-Al-CO3]纳米层状双氢氧化物的粒径约为10-40nm。讨论了微波和变速滴加碱液的速度对纳米层状双氢氧化物的合成的影响。用FT-IR、TEM与XRD对产物进行了表征,结果表明在微波加热反应的条件下可在短时间内用PO43-,P2O74-彻底交换CO32-。     

Preparation of inorganic–organic pillared montmorillonite using ultrasonic treatment

Montmorillonite (Mt) is a clay mineral with expandable layer structure. Mesoporous pillared montmorillonite can be prepared by introducing gallery templates, such as simple metal cations, quaternary ammonium cations, long chain amines, and hydroxyed inorganic metal ions. In this paper, inorganic–organic pillared montmorillonite intercalated by aluminium and alkyl ammonium chloridize (HDTMA–Cl) was successfully prepared by ultrasonic treatment, and the physicochemical properties of the materials were systematically characterized by XRD, FT-IR, SEM and TEM techniques. The d₀₀₁ basal spacings and microstructures of Mt–Al–HDTMA were characterized by XRD. The function group, crystal surface morphology, structural and chemical analysis of Mt–Al–HDTMA were measured by FT-IR, SEM, TEM and EDX. The results indicated that ultrasonic method might accelerate the diffusion of the intercalating species, which enhanced the textural properties and the morphologies. The results also suggested that aluminium and HDTMA–Cl reagent entered the interlayer of Mt, and that the crystal structure of the final Mt was preserved.     

SiO2/TiO2柱撑层状钛酸的制备及表征

采用预膨润技术成功制备了SiO2/TiO2柱撑层状钛酸。将氢型钛酸TiO2(H)于正丙胺溶液中利用离子交换方法得到正丙胺插层的钛酸C-3TiO,C-3TiO在正硅酸乙酯和异丙醇钛的混合溶剂中160℃溶剂热处理2天,得到SiO2/TiO2柱撑层状钛酸。利用X-射线衍射,红外光谱,透射电子显微镜,热重-差热分析等手段对材料进行表征,结果表明制备材料具有层状结构,层间距为1.1nm。     

聚马来酸/LDH插层型纳米复合材料的制备与表征

采用离子交换法将马来酸单体插入Mg/Al-Cl-LDH层间,然后通过热或氧化还原引发层间单体链式原位缩聚制备聚马来酸/水滑石(LDH)插层型纳米复合材料。研究了插层组装的条件和引发聚合的方法。采用X射线衍射(XRD)、红外光谱(FT-IR)、热重及差热分析(TG-DTA)和扫描电子显微镜(SEM)等手段对样品进行了表征与测试。结果表明,马来酸插层LDH使层间距由0.767 nm增大至1.19 nm,H2O2引发剂或热引发聚合使层间距由1.19 nm分别减小至1.114 nm和1.085 nm,产物粒径为50 nm~100 nm。聚马来酸分子进入LDH层间形成超分子结构,使其热稳定性提高100℃以上。     

The Inhibitive Effect of para-Amino Benzoic Acid and Its Polymer on Corrosion of Iron in 1 mol/L HC1 Solution

Poly p-aminobenzoic acid has been synthesized by chemical oxidation method. The inhibitive effect of poly p-aminobenzoic acid on iron in 1 mol/L HCl solution was investigated by polarization and electrochemical impedance spectroscopy and compared with that of monomer p-aminobenzoic acid. The effectiveness of poly p-aminobenzoic acid is very high in comparison with that of monomer. The results show that both cathodic and anodic processes were suppressed by p-aminobenzoic acid and poly p-aminobenzoic acid of iron dissolution in 1 mol/L HCI by their adsorption on the iron surface. The inhibition efficiency of both p-aminobenzoic acid and poly p-aminobenzoic acid were found to increase with the inhibitor concentrations. Ultraviolet (UV) reflectance studies of the iron surface after exposure to inhibitor acid show that poly p-aminobenzoic acid is strongly adsorbed on iron surface.