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插层高岭石层间醋酸钾的作用和取向 总被引:9,自引:1,他引:9
利用X粉晶衍射和激光拉曼光谱实验分析高岭石及其醋酸钾插层物的结构。通过实验表明醋酸钾对结晶指数(HI)为0.9的高岭石进行插层.插层率为73%,使高岭石的d(001)由0.72075nm增加到1.42093nm。进入高岭石层间的醋酸根利用其羧基上的两个氧同时和高岭石的面内羟基形成氢键,在高岭石层间直立取向,而对其内羟基基本无影响。当温度升高时,与面内羟基伸缩振动有关的峰(3698cm^-1,3684cm^-1,3672cm^-1等)发生红移,且强度增加;而与内羟基伸缩振动有关的峰(3621cm^-1)则发生蓝移。温度升高到100C以上,开始发生去插层过程;直到250C,插层分子还不能完全从高岭石层间脱去。 相似文献
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甲酰胺在高岭石层间的定向研究 总被引:6,自引:1,他引:6
甲酰胺插层作用使高岭石层间距从0.717nm膨胀为1.020nm。其增加值(0.303nm)小于甲酰胺的范得瓦尔分子直径(0.47nm)。DRIFT光谱研究表明插层作用破坏了原高岭石层间氢键,并分别在高岭石Si—O基与甲酰胺NH基和高岭石OH基与甲酰胺C=O基之间形成氢键,甲酰胺HN基还部分嵌入高岭石复三方孔洞。 相似文献
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首先研究了大同高岭石的矿物学特征,结果表明大同高岭石晶粒粗大,主要由高岭石组成,样品的有序度高,Hinckley指数为1.12。在此基础上,用二甲基亚砜对大同高岭石进行插层,采用XRD、IR和TG-DSC研究插层复合物的结构。XRD结果表明DMSO已插入高岭石层间,d001由原来的0.717nm增至1.13nm,插层率达96.01%;红外光谱证明DMSO中的S=O基团与高岭石的外羟基发生了化学键合作用;热分析结果显示插层复合物于120℃~240℃发生DMSO的脱嵌作用,高岭石的脱羟基温度在400℃~750℃。 相似文献
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采用共沉淀法和离子交换法实现了谷氨酸与Zn/Al水滑石的插层组装,并采用X射线粉末衍射、差热分析、红外光谱表征了谷氨酸插层水滑石的结构,并在模拟胃液和肠液中测试了复合材料中谷氨酸的缓释性能。结果表明,合成的水滑石前躯体(LDHs-NO3)结构规整、晶相单一,层间距为0.879 nm;2种方法合成的谷氨酸插层水滑石,其层间距分别增加到1.251 nm和1.334 nm,可以推测谷氨酸以垂直方式分布于水滑石层间。插层后水滑石样品在1588 cm-1和1346 cm-1处出现了谷氨酸中羧酸根的不对称伸缩振动和对称伸缩振动峰,也佐证了氨基酸插层成功。谷氨酸插层水滑石后,其热稳定性大大提高,热分解温度由230℃升高至397~434℃。与物理混合法相比,谷氨酸与水滑石复合后增加了谷氨酸的耐酸性,使其具有较好的缓释性能。谷氨酸释放曲线符合Bhaskar方程,表明微粒间的扩散作用是谷氨酸分子释放的限速步骤。LDHs-Glu经海藻酸钠包裹后,在模拟肠液中缓慢释放而在模拟胃液中不释放,起到了肠液定向释放的效果。 相似文献
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1,4-丁二醇插层高岭石的实验研究 总被引:3,自引:0,他引:3
以二甲亚砜为前驱物,1,4-丁二醇为插层剂,采用二步插层法制备1,4-丁二醇与高岭石的复合材料。实验研究了温度、时问对插层效果的影响及该复合物在水中的稳定性。采用XRD和IR法对试样进行分析表征。结果表明,在140℃,180℃条件下插层一定时间,均可获得1,4-丁二醇插层高岭石,在180(、条件下反应16h以上,同时高岭石的层间距增大到1.157nm,制备的1,4-丁二醇插层高岭石结构稳定,180℃反应32h可导致高岭石层间1,4-丁二醇转变为其他物质,形成稳定的有机插层高岭石。 相似文献
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高岭土/肼插层材料的制备与表征 总被引:4,自引:0,他引:4
以高岭土为原料,选取50%水合肼作为插层剂,采用直接液相插层法,并辅以磁力搅拌,成功地将肼分子插入到高岭石结构层间,制得肼插层高岭土材料。利用红外光谱和粒度分析仪对产品进行了表征。IR谱表明, 插层中肼分子中的NH基与高岭石内表面羟基之间产生了N-H-OH作用,形成了新的氢键;插层反应后的样品,其粒径小于5 μm的颗粒占总颗粒数的比例降低了10.55%,平均粒径增大了46.84%。 相似文献
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高岭石插层复合物作为新型矿物材料现已被广泛应用。然而,插层复合物热稳定性较难控制使其在聚合物中的应用一直受到限制。本文应用热分析、X射线衍射、质谱及发射红外光谱等表征技术对煤系高岭石/醋酸钾插层复合物受热分解产物及微结构变化进行了研究。结果表明,煤系高岭石/醋酸钾插层复合物热相变主要经历以下几个阶段:插层水脱嵌(约350℃),插层剂醋酸钾脱嵌(约400℃),脱羟基(约450℃),偏高岭石形成(450~550℃),KHCO3出现(约600℃),KHCO3热分解形成K2CO3和KAl Si O4出现(约700℃),热解产品K2Al2Si O4出现(约800℃),K4Al2Si2O3出现(900~1000℃),大量K3Al O3形成阶段(1100℃及以上)。此外,还发现通过控制插层率和加热温度,可实现高岭石插层复合物的可控分解、新物相合成与转变,从而有利于新材料的合成。 相似文献
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R. L. Frost J. Kristof G. N. Paroz J. T. Kloprogge 《Physics and Chemistry of Minerals》1999,26(3):257-263
Upon intercalation of both ordered (low defect) and disordered (high defect) kaolinites with acetamide, two types of interaction
are observed. Firstly, hydrogen bonding between the NH2 groups of the acetamide with the siloxane oxygens is formed, as evidenced by the formation of two new bands at 3400 and 3509
cm–1. Secondly, the appearance of additional bands at ∼3600 cm–1 in both the infrared and Raman spectra of the acetamide intercalates is attributed to a second type of hydrogen bonding by
the interaction of the C=O group and the inner surface hydroxyls. Changes in the intensity of the hydroxyl deformation modes
in the 895 to 940 cm–1 region are attributed to the changes in the hydrogen bonding of the kaolinite surfaces. It is proposed that the hydrogen
bonding between the adjacent kaolinite layers is replaced with hydrogen bonding between both kaolinite surfaces and the acetamide
molecule. Changes in the molecular structure of acetamide are observed upon intercalation. The amide 1 band is lost and replaced
with a well-defined NH2 deformation vibration. The loss of the amide 1 band is attributed the hydrogen bond formation between the amide hydrogens
and the siloxane surface. The bands of the C=O group at 1680 and 1740 cm–1 become a single band at 1680 cm–1. The amide 2 band remains unchanged. The lack of intensity of the 1740 cm–1 band is attributed to the formation of hydrogen bonding between the inner surface hydroxyl groups and the carbonyl group.
Received: 4 February 1998/ Revised, accepted: 30 June 1998 相似文献
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珍珠陶石的夹层化合物法鉴定 总被引:1,自引:0,他引:1
应用联氨、使珍珠陶石形成其夹层物,然后再用水洗获是水合珍珠陶石,这种水合珍珠陶石具有十分特征的0.835nmX射线衍射峰,而高岭石族的其它矿物却保持不变,利用这一明显的特征,可以容易地区分出混合在高岭石中的少量珍珠陶石。 相似文献
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The hydroxyl stretching frequencies of four phyllosilicates have been measured at high pressures and temperatures using an externally heated diamond-anvil cell and synchrotron infrared spectroscopy. Spectra were measured up to 26, 31, 21 and 8 GPa at room temperature for samples of talc, pyrophyllite, muscovite and 10-Å phase, respectively. Spectra were also measured in the range 273–500 K at ambient pressure for all samples and at 8–9 GPa for talc and pyrophyllite. The frequency of the Mg3OH band in talc increases with pressure due to the absence of hydrogen bonding. The different orientation of the hydroxyl group in pyrophyllite and muscovite leads to hydrogen bonding and a decrease in the frequency of the Al2OH band with pressure. 10-Å phase is approximately equivalent to talc with the addition of interlayer H2O. In a spectrum of a sample synthesised for 143 h, two hydroxyl stretching bands are clearly resolved on compression. One is the same as the Mg3OH band in talc, indicating the presence of intra-layer hydroxyl in a talc-like environment with no hydrogen bonding. The other, which separates from the talc-like band at 1 GPa, is associated with intra-layer hydroxyl that is hydrogen bonded to interlayer H2O. There are equivalent bands in high-pressure spectra of a sample of deuterated 10-Å phase, synthesised for 400 h. This sample shows a greater extent of hydrogen bonding at ambient pressure than the 143 h sample. For all of the phases studied, increasing temperature leads to a decrease in frequency for every hydroxyl stretching vibration, both at low and high pressures. The shifts in frequency with temperature are an order of magnitude greater than the shifts with pressure when normalised to previously measured structural parameters. 相似文献
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综述了近几十年来国内外高岭石有机插层纳米复合材料领域中有机插层理论的研究进展,主要对插层剂在纳米层问的形态及结构、插层过程中水的作用、吸附与插层、脱嵌过程等方面以及纳米复合材料的应用进行了详细的阐述,并在此基础上提出了该领域研究的重点及热点。 相似文献