甘氨酸-Mg<sub>3</sub>Al水滑石的制备、剥离以及与蒙脱土的插层组装<sup>*</sup>

doi:10.11901/1005.3093.2013.372

材料研究学报

2014, Vol. 28

Issue (2): 100-106 DOI: 10.11901/1005.3093.2013.372

本期目录 | 过刊浏览

甘氨酸-Mg₃Al水滑石的制备、剥离以及与蒙脱土的插层组装^*

马小茜,周景龙,卢楠,吴旭,谢鲜梅

太原理工大学化学化工学院太原 030024

Preparation and Delaminating of Glycine-Mg₃Al LDHs and its Intercalation Compounding with Montmorillonite

Xiaoqian MA,Jinglong ZHOU,Nan LU,Xu WU,Xianmei XIE

College of Chemistry and Chemical Engineering, Taiyuan University of Technology, Taiyuan 030024

引用本文:

马小茜,周景龙,卢楠,吴旭,谢鲜梅. 甘氨酸-Mg₃Al水滑石的制备、剥离以及与蒙脱土的插层组装^*[J]. 材料研究学报, 2014, 28(2): 100-106.
Xiaoqian MA, Jinglong ZHOU, Nan LU, Xu WU, Xianmei XIE. Preparation and Delaminating of Glycine-Mg₃Al LDHs and its Intercalation Compounding with Montmorillonite[J]. Chinese Journal of Materials Research, 2014, 28(2): 100-106.

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摘要:

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Gly- Mg₃Al 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n_Gly∶n_NO3^-=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。

关键词 ：无机非金属材料, 甘氨酸, Mg₃Al水滑石, 剥离, 蒙脱土, 插层组装

Abstract：

Glycine(Gly)was intercalated into Mg₃Al layered double hydroxides(Gly-Mg₃Al LDHs)by coprecipitation method. The delaminating of Gly-Mg₃Al LDHs in aqueous solution of pH=3~4 was realized by making use of the isoelectric point of Gly. Then Mg₃Al LDHs/montmorillonite layered composite was gained through inserting LDHs sheets into montmorillonite. The composite was characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), electrophoresis apparatus and N₂-adsorption/desorption measurements. The results show that the formed Gly-Mg₃Al LDHs possesses well-defined crystallographic structure. When the raw material ratio is 0.5 (n_Gly:n_NO3^-=1:2), the obtained Gly-Mg₃Al LDHs exhibits the best performance of delaminating, while the zeta potential of the subsequence colloidal particles is between 35mV and 40mV. Additionally, the translucent colloidal solution may be kept stably for 72h.The interlayer space of the layered composite is 1.44 nm, which is the total thickness of LDHs sheet and montmorillonite sheet. The results prove that LDHs sheets and montmorillonite sheets are layer by layer staggered.

Key words： inorganic non-metallic materials glycine Mg₃Al LDHs delaminating montmorillonite intercalation compounding

收稿日期: 2013-05-31

基金资助:* 国家自然科学基金50872086, 山西省自然科学(青年科技研究)基金2012021006-3 资助项目。

作者简介: 本文联系人: 谢鲜梅, 教授

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https://www.cjmr.org/CN/10.11901/1005.3093.2013.372 或 https://www.cjmr.org/CN/Y2014/V28/I2/100

图1 不同nGly:nNO3-的Gly-Mg3Al LDHs的XRD谱图 (a 1∶4, b 1∶3, c 1∶2, d 1∶1, e 1∶0.5, f Mg3Al LDHs)

图2 不同合成pH下的Gly-Mg3Al LDHs的XRD谱图 (a 9, b 10, c 11, d 12, e Mg3Al LDHs)

图3 Gly-Mg3Al LDHs的超分子结构模型

图4 不同nGly∶nNO3-的Gly-Mg3Al LDHs的红外分析图 (a 1∶4, b 1∶3, c 1∶2, d 1∶1, e 1∶0.5, f Mg3Al LDHs)

图5 不同合成体系pH下的Gly-Mg3Al LDHs的红外分析图 (a 9, b 10, c 11, d 12, e Mg3Al LDHs)

表1 剥离体系的pH对剥离效果的影响

表2 nGly∶nNO3-对剥离效果的影响

表3 合成体系pH对剥离效果的影响

图6 (a) 剥离Gly-Mg3Al LDHs, (b) Gly-Mg3Al LDHs, (c) 蒙脱土, (d) Mg3Al水滑石/蒙脱土层状复合材料的XRD谱图

图7 Mg3Al水滑石/蒙脱土层状复合材料的制备过程

图8 (a) Gly-Mg3Al LDHs, (b) 蒙脱土, (c) Gly-Mg3Al LDHs与蒙脱土机械混合物, (d) Mg3Al水滑石/蒙脱土层状复合材料的红外分析图

表4 蒙脱土, Gly-Mg3Al LDHs, Mg3Al水滑石/蒙脱土层状复合材料的比表面积及孔结构性质

图9 Mg3Al水滑石/蒙脱土层状复合材料的N2吸附-脱附曲线

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