脯氨酸、组氨酸、色氨酸水滑石蒙脱石复合插层材料的制备与表征

发布时间：2018-01-07 05:01

本文关键词：脯氨酸、组氨酸、色氨酸水滑石蒙脱石复合插层材料的制备与表征　出处：《北京化工大学》2015年硕士论文　论文类型：学位论文

【摘要】：层状材料是当今化学研究的热点之一,因其独特的结构使它在许多领域有着广泛的应用。水滑石、类水滑石化合物和蒙脱石都是典型的层状材料,水滑石及类水滑石化合物的层板主要由金属氢氧化物和层间阴离子组成,因层间阴离子的可交换性,在催化、离子载体等领域具有较大的潜力。蒙脱石是一种硅铝酸盐粘土矿物,层间阳离子也具有可交换性,在医药和化工领域有着广泛的应用。为了进一步研究层状材料的结构特性,发掘单一层状材料的应用潜力,本文以氨基酸为客体分子,制备了一种同时具有水滑石和蒙脱石特征层板的双极性层状化合物。首先采用共沉淀法制备镁铝水滑石(LDH)和脯氨酸插层镁铝水滑石(Pro-LDH),同时将脯氨酸引入蒙脱石层间制备脯氨酸插层蒙脱石(Pro-MMT)。通过XRD、FT-IR、TG-DTA和SEM等表征方法对产物进行表征。XRD谱图显示脯氨酸插层水滑石的003衍射面特征峰的位置与水滑石的003衍射面特征峰的位置有一定偏移,实验所得LDH的d003值为0.79nm, Pro-LDH的d003值为0.81nm,其中d003值为层板间距,这表明脯氨酸插入到水滑石层板之中。FT-IR和TG-DTA的图谱也从分子基团特征峰及热稳定性方面表征了脯氨酸插层水滑石的特性。通过对比XRD谱图,脯氨酸插层蒙脱石的层间距比单一蒙脱石有所增大,表明脯氨酸成功引入蒙脱石层板。用甲酰胺对Pro-LDH的层板进行剥离,用去离子水对Pro-MMT进行溶胀剥离。将二者剥离的溶液按照不同的质量比混合,分别通过XRD、FT-IR、 SEM、TG-DTA等测试方法对产物进行表征,SEM结果表明,在LDH:MMT=4:1以下时,产物的形貌与蒙脱石形貌基本相似,随着水滑石含量增加,卷曲形貌减少,总体形貌也接近于水滑石。水滑石的层板厚度为0.48nm,蒙脱石的层板厚度是0.91～0.95nm。通过平行实验,XRD结果表明在质量比为1：4和1：2时,复合物的层板间距为1.42nnm和1.43nm。两种复合产物层间距接近于水滑石与蒙脱石单一层板间距之和,表明产物可能形成由水滑石层板和蒙脱石层板构成的层层堆叠的结构,层板之间的连接是单片层连接。当质量比为1：1、2：1、4：1时,复合物的层板间距为1.63nm、1.64nm、1.76nm,层板间距较大,表明复合物的主体是蒙脱石,层间水滑石层板排列较为复杂。在质量比8：1时,复合物的层板间距为1.68nm,主体是水滑石,复合物的层板峰强度较弱。在质量比为10：1和15：1时,复合物中蒙脱石的001衍射面特征峰消失,说明产物中水滑石层板占主要部分,同时由于剥离影响层板长程无序排列。为了探索其他氨基酸对插层结构的影响,分别采用组氨酸和色氨酸作为层间离子进行了平行实验。通过XRD表征可以得知水滑石的d003值为0.79nm,Pro-LDH的d003值为0.81nm, His-LDH的d003值为0.88nm, Trp-LDH的d003值为0.92nm,蒙脱石的d00l值为1.28nm,Pro-MMT的d001值为1.36nm,His-MMT的d001值为1.35nm,Trp-MMT的d001值为1.49rm。从插层化合物的层间距可以看出相对于脯氨酸,组氨酸和色氨酸对层状材料结构的改变更明显。组氨酸和色氨酸剥离复合产物的dool值在1.46～1.54nm之间,符合形成双层板层状化合物的层间距条件,说明三种氨基酸均可以作为客体分子进入水滑石与蒙脱石的层板间形成双层板层状化合物。
[Abstract]:Layered materials is one of the hot research in chemistry, because of its unique structure. So it has been widely used in many fields. Hydrotalcite, hydrotalcite like compounds and montmorillonite are typical layered material, laminated hydrotalcite and hydrotalcite like compounds is mainly composed of metal hydroxide and interlayer anions, because exchangeable interlayer anions, has great potential in catalysis, ion carriers and other fields. Montmorillonite is an aluminosilicate clay mineral, interlayer cation has exchangeability, is widely used in the field of pharmaceutical and chemical engineering. In order to further study on structural characteristics of layered materials and application potential of single layered materials in this paper, using amino acids as guest molecules, a bipolar layered compound with hydrotalcite and montmorillonite were prepared. The characteristics of laminates prepared by coprecipitation using hydrotalcite (L first DH) and proline intercalation hydrotalcite (Pro-LDH), while the proline introduced montmorillonite prepared proline intercalated montmorillonite (Pro-MMT). Through XRD, FT-IR, TG-DTA and SEM characterization method has offset the structure of product was characterized by.XRD spectra showed that the diffraction peak position of 003 surface characteristics of proline intercalated hydrotalcite the 003 diffraction surface characteristic peaks and hydrotalcite on the position of the experimental LDH D003 value is 0.79nm, the Pro-LDH D003 value is 0.81nm, the D003 value of plate spacing, which indicates that the proline into hydrotalcite laminates.FT-IR and TG-DTA spectra from molecular group peaks and their thermal stability were characterized the characteristics of proline intercalation hydrotalcite. By comparing the XRD spectra of proline intercalated montmorillonite interlayer spacing is higher than single montmorillonite, montmorillonite layers showed that proline successfully. The Pro-LDH plate by formamide Peeling, swelling peeling of Pro-MMT with deionized water. The solution is two off according to different mass ratio, respectively by XRD, FT-IR, SEM, TG-DTA and other test methods were characterized. The SEM results showed that in the following LDH:MMT=4:1, the morphology and morphology of smectite are similar, with the increase of water the content of talc, crimp morphology decreased, overall morphology is also close to the hydrotalcite. The plate thickness of hydrotalcite was 0.48nm, 0.91 ~ 0.95nm. layer thickness of montmorillonite through parallel experiments, XRD results showed that the mass ratio of 1:4 and 1:2, composite plate spacing is 1.42nnm and 1.43nm. two composite product layer close to the distance hydrotalcite and montmorillonite single plate spacing and show that the structure of the product may be formed consisting of stacked layers of hydrotalcite laminates and montmorillonite plates, connecting plates between the single layer connection. When the matter Volume ratio is 1:1,2:1,4:1, composite plate spacing is 1.63nm, 1.64nm, 1.76nm, plate spacing is large, show that the main compound is montmorillonite interlayer hydrotalcite laminates arrangement is more complicated. When the mass ratio of 8:1, composite plate spacing is 1.68nm, is the main peak of hydrotalcite, weak strength composite laminates at the mass ratio of 10:1 and 15:1, the characteristics of 001 diffraction peaks of montmorillonite complexes disappeared, that products of water talc accounted for the main part of the plate, stripping effect laminates of long range disorder arrangement. In order to explore the effects of other amino acids on the intercalated structure, using histidine and tryptophan as interlayer ions the parallel experiment. The samples were characterized by XRD that the hydrotalcite D003 value is 0.79nm Pro-LDH, the D003 value is 0.81nm, the His-LDH D003 value is 0.88nm, Trp-LDH value of D003 is 0.92nm, d00l value of Montmorillonite 1.28nm Pro-MMT, the D001 value is 1.36nm, the His-MMT D001 value is 1.35nm, Trp-MMT value of D001 is 1.49rm. from the intercalation compound layer spacing can be seen with respect to the change of proline, histidine and tryptophan on the layered material structure is more obvious. The histidine and tryptophan composite product stripping at dool value of 1.46 ~ 1.54nm meet the conditions for the formation of interlayer spacing between double lamellar compounds, indicating that double lamellar compounds formed laminates of three kinds of amino acids can be used as guest molecules into hydrotalcite and montmorillonite.

【学位授予单位】：北京化工大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TB332

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