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.     

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.     

镁铝水滑石的制备与应用研究

镁铝水滑石因其阴离子的特殊性,具有诸多优点且应用广泛,引起了国内外诸多研究人员的关注。天然水滑石数量很少,而且大部分以尖晶石的形式出现,纯度极低,通过除去杂质得到纯度更高的天然水滑石成本非常高,因此通过人工合成获得高纯度的水滑石成为首选方法。目前我国合成水滑石(LDHs)的产量以15%左右的年增长率稳定增长,市场规模也维持15%以上高速增长。本文总结了近年来国内外镁铝水滑石的典型制备方法和应用,对比分析了各方法的优缺点以及最近几年镁铝水滑石在各领域的研究结果,最后对镁铝水滑石制备方法后续的研究与优化进行了展望。     

插层改性水滑石的制备及结构研究

采用还原法制备十二烷基硫酸钠插层改性水滑石,采用XRD、FTIR、SEM和TG表征水滑石的结构和热性能,结果表明:十二烷基硫酸钠能够有效改性水滑石,提高水滑石的热稳定性。     

生色基团插层锌铝水滑石的制备和性质

以层状锌铝水滑石为主体, 在乙二醇介质中, 通过离子交换法, 将一对具有给体－受体性质的生色团香豆素-3-甲酸(3-CCA)与9-蒽甲酸(9-ACA)共插入到层状锌铝水滑石层间, 组装得到晶体结构良好的共插层类水滑石, 且通过控制离子交换的时间、温度、客体投料比, 可制得一系列具有不同摩尔比客体的共插层产物. 产物采用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性. 结果表明, 给体受体进入层间后, 不仅客体与主体层板存在静电力和氢键相互作用, 而且在限域空间内有利于客体之间的相互作用, 从而产生了给体受体间的能量转移过程.     

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.     

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%。     

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.     

甘氨酸-Mg_3Al水滑石的制备、剥离以及与蒙脱土的插层组装

用共沉淀法制备甘氨酸(简称Gly)插层Mg3Al水滑石(简称Gly-Mg3Al LDHs),利用甘氨酸等电点的性质实现了Mg3Al水滑石在pH=3~4水溶液中的剥离,并将剥离出的LDHs纳米片层与蒙脱土进行插层组装,制备出Mg3Al水滑石/蒙脱土层状复合材料。用X射线粉末衍射、红外光谱、N2吸附-脱附以及电泳仪等手段对样品进行了表征。结果表明,制备出的GlyMg3Al LDHs结构规整,晶相单一,甘氨酸以42°的倾角排列于水滑石层间。在nGly∶nNO3-=1∶2的条件下制备的Gly-Mg3Al LDHs剥离效果最好,剥离后形成的无机聚合粒子的zeta电位介于35 mV~40 mV之间,剥离液可以稳定存在72 h。所得层状复合材料的层间距为1.44nm,此值为单元LDHs片层与单元蒙脱土片层的厚度之和,证明LDHs纳米片层与蒙脱土进行了有序交叉叠层。     

对氨基苯甲酸插层镁铝水滑石的合成、表征及紫外吸收性能

以微波结晶法制备的碳酸根型镁铝水滑石(LDHs)为前体, 对氨基苯甲酸为客体, 由水热法、离子交换法、焙烧复原法三种方法组装合成了对氨基苯甲酸插层镁铝水滑石复合材料。并用XRD、FTIR、TG-DSC、SEM等对其结构进行表征。结果表明: 各种方法均能合成相应的插层水滑石层柱材料, 层间距分别扩大为0.81 nm、0.79 nm、1.45 nm。三种合成材料的紫外吸收强弱与对氨基苯甲酸插层水滑石分子后的层间距大小有关。该研究指出对氨基苯甲酸插层水滑石作为一种紫外吸收层柱材料在化妆品领域具有应用潜力。      

Ageing behaviour of unary hydroxides in trivalent metal salt solutions: Formation of layered double hydroxide (LDH)-like phases

The hydroxides of Mg, Ni, Cu and Zn transform into layered double hydroxide (LDH)-like phases on ageing in solutions of Al or Cr salts. This reaction is similar to acid leaching and proceeds by a dissolution-reprecipitation mechanism offering a simple method of LDH synthesis, with implications for the accepted theories of formation of LDH minerals in the earth’s crust.     

类水滑石的制备与改性及其在聚丙烯阻燃中的应用

采用共沉淀法制备了镁铝类水滑石（LDHs）前驱体,加入少量聚磷酸铵（APP）制得APP-LDHs,探讨了不同质量分数APP对LDHs晶体生长的影响;当APP在LDHs前驱浆液中添加量为0.8wt%时,将APP-LDHs与季戊四醇（PER）、硅烷偶联剂KH-550进行球磨混合,制备插层包覆改性的LDHs;通过XRD、FTIR、SEM和TG等对改性前后的LDHs进行了表征;采用极限氧指数（LOI）、垂直燃烧测试（UL-94）、缺口冲击和弯曲实验等方法研究了LDHs改性前后LDHs/聚丙烯（PP）复合材料的阻燃性能及力学性能的差异。研究结果表明：APP的加入,未显著影响LDHs的层板生长,但其层板堆叠受到抑制;SEM观察表明,所制备的LDHs为片状,且经插层包覆改性后的LDHs粉体形貌较为规整,颗粒粒径为100~250 nm;改性LDHs在较高温度下的热稳定性显著优于未改性的LDHs;当PP中加入质量分数为20%的LDHs及改性LDHs时,可抑制PP燃烧时产生的熔滴,并促使LDHs/PP复合材料表面形成炭层;改性LDHs/PP复合材料具有更好的阻燃性能,且其冲击强度、弯曲强度等力学性能下降不明显。     

Sorption of an anionic dye by uncalcined and calcined layered double hydroxides: a case study

Layered double hydroxides (LDHs) with a Mg/Al molar ratio of 2:1 were synthesized by using a co-precipitation method and their calcined products (CLDHs) were obtained by heating Mg/Al-LDHs at 500 °C. Sorption of a weak acid dye, Brilliant Blue R (BBR), by LDHs and CLDHs indicated equilibrium time required for BBR sorption by CLDHs was less than 12 h, regardless of initial concentration of BBR, whereas BBR sorption by LDHs was longer than 20 h. Sorption capacity of CLDHs was much larger than that of LDHs. Therefore, CLDHs could be used to remove anionic dyes of relatively high concentrations while LDHs may only be used to remove anionic dyes of low concentrations. Isotherms for BBR sorption by CLDHs and LDHs were well described using the Freundlich and Langmuir equations, respectively. When the initial pH of BBR solutions was lower than 8.0, the final pH of the solution after sorption was enhanced and stabilized at 10.6–10.8. The effect of initial pH (<8.0) on BBR removal was negligible, which would be environmentally important for precipitation/co-precipitation of co-existing metal cations. The effects of both Cl⁻ and SO₄²⁻ on BBR sorption by CLDHs were minimal; but the presence of CO₃²⁻ markedly reduced BBR removal. Thermal regeneration for re-use of LDHs and CLDHs after BBR sorption was feasible only within the first two cycles, after which the regenerated materials suffered from a large loss in their sorption capacities.     

ZnAlTi型层状双氢氧化物光催化降解亚甲基蓝的性能研究

利用动态尿素水解法制备了3种不同比例的ZnAlTi型层状双氢氧化物,取部分样品分别在温度为500、600、700和900℃条件下煅烧4h,制得具有光催化性能的材料。研究催化剂不同摩尔比、催化剂用量、煅烧温度等不同因素对光催化降解亚甲基蓝过程的影响。结果表明,紫外光照射下,在反应温度为30℃、催化剂中Ti和Al的摩尔比为2、催化剂投加浓度为1.0g/L、亚甲基蓝初始浓度为10mg/L、煅烧温度为600℃的反应条件下,催化剂对亚甲基蓝的降解效果最好,光照反应12h后亚甲基蓝的降解率为94.4%。     

Sorption study of an acid dye from an aqueous solution on modified Mg-Al layered double hydroxides

In this paper, experimental methods and results are reported on the removal of the dye Green Bezanyl-F2B (an acid dye) from MgAlCO(3) (HT) and from intercalated anionic surfactant, "sodium dodecylsulfate (SDS)", into the Mg-Al layered double hydroxides by the calcination-rehydration reaction using Mg-Al oxide precursors calcined at 773 K. Dodecylsulfate hydrotalcite was prepared by the calcination-rehydration method. The surfactant intercalation in the interlayer space of hydrotalcite was investigated by XRD and FT-IR spectroscopy where the resulting materials were found to be similar to those reported in the literature and were used to remove an acid dye from an aqueous solution. Equilibrium time and rate-determining step of the dye Green Bezanyl-F2B sorption were determined. Two simplified kinetic models were tested to investigate the sorption. The adsorption capacity data were also fitted to Langmuir and Freundlich equation as well. The sorption data fitted to the Langmuir model gave good values of the determination coefficient.     

酒石酸柱撑水滑石吸附水中的Ni~(2+)的特性研究

采用离子交换法制得酒石酸插层MgAl水滑石(MgAl-TA LDHs),并进行了XRD、IR、SEM、比表面积及孔径分析表征。考察了MgAl-TA LDHs吸附剂对溶液中Ni 2+的吸附能力,探讨了水滑石吸附剂投加量、Ni 2+溶液浓度、pH值以及吸附温度对Ni 2+吸附率的影响,并进行了动力学和热力学特征的研究。结果表明,适宜的水滑石投加量为2g/L,pH值以中性为宜,对于Ni 2+浓度不超过100 mg/L的溶液室温下Ni 2+吸附率在60%以上,而高温有利于提高Ni 2+吸附率。吸附过程符合二级动力学模型,吸附等温曲线可用R-P模型来描述。吸附过程能够自发进行,为吸热过程,属于化学吸附。