脯氨酸、組氨酸、色氨酸水滑石蒙脫石復(fù)合插層材料的制備與表征
發(fā)布時間:2018-01-07 05:01
本文關(guān)鍵詞:脯氨酸、組氨酸、色氨酸水滑石蒙脫石復(fù)合插層材料的制備與表征 出處:《北京化工大學(xué)》2015年碩士論文 論文類型:學(xué)位論文
更多相關(guān)文章: 水滑石 蒙脫石 脯氨酸 色氨酸 組氨酸 復(fù)合物
【摘要】:層狀材料是當(dāng)今化學(xué)研究的熱點之一,因其獨特的結(jié)構(gòu)使它在許多領(lǐng)域有著廣泛的應(yīng)用。水滑石、類水滑石化合物和蒙脫石都是典型的層狀材料,水滑石及類水滑石化合物的層板主要由金屬氫氧化物和層間陰離子組成,因?qū)娱g陰離子的可交換性,在催化、離子載體等領(lǐng)域具有較大的潛力。蒙脫石是一種硅鋁酸鹽粘土礦物,層間陽離子也具有可交換性,在醫(yī)藥和化工領(lǐng)域有著廣泛的應(yīng)用。為了進一步研究層狀材料的結(jié)構(gòu)特性,發(fā)掘單一層狀材料的應(yīng)用潛力,本文以氨基酸為客體分子,制備了一種同時具有水滑石和蒙脫石特征層板的雙極性層狀化合物。首先采用共沉淀法制備鎂鋁水滑石(LDH)和脯氨酸插層鎂鋁水滑石(Pro-LDH),同時將脯氨酸引入蒙脫石層間制備脯氨酸插層蒙脫石(Pro-MMT)。通過XRD、FT-IR、TG-DTA和SEM等表征方法對產(chǎn)物進行表征。XRD譜圖顯示脯氨酸插層水滑石的003衍射面特征峰的位置與水滑石的003衍射面特征峰的位置有一定偏移,實驗所得LDH的d003值為0.79nm, Pro-LDH的d003值為0.81nm,其中d003值為層板間距,這表明脯氨酸插入到水滑石層板之中。FT-IR和TG-DTA的圖譜也從分子基團特征峰及熱穩(wěn)定性方面表征了脯氨酸插層水滑石的特性。通過對比XRD譜圖,脯氨酸插層蒙脫石的層間距比單一蒙脫石有所增大,表明脯氨酸成功引入蒙脫石層板。用甲酰胺對Pro-LDH的層板進行剝離,用去離子水對Pro-MMT進行溶脹剝離。將二者剝離的溶液按照不同的質(zhì)量比混合,分別通過XRD、FT-IR、 SEM、TG-DTA等測試方法對產(chǎn)物進行表征,SEM結(jié)果表明,在LDH:MMT=4:1以下時,產(chǎn)物的形貌與蒙脫石形貌基本相似,隨著水滑石含量增加,卷曲形貌減少,總體形貌也接近于水滑石。水滑石的層板厚度為0.48nm,蒙脫石的層板厚度是0.91~0.95nm。通過平行實驗,XRD結(jié)果表明在質(zhì)量比為1:4和1:2時,復(fù)合物的層板間距為1.42nnm和1.43nm。兩種復(fù)合產(chǎn)物層間距接近于水滑石與蒙脫石單一層板間距之和,表明產(chǎn)物可能形成由水滑石層板和蒙脫石層板構(gòu)成的層層堆疊的結(jié)構(gòu),層板之間的連接是單片層連接。當(dāng)質(zhì)量比為1:1、2:1、4:1時,復(fù)合物的層板間距為1.63nm、1.64nm、1.76nm,層板間距較大,表明復(fù)合物的主體是蒙脫石,層間水滑石層板排列較為復(fù)雜。在質(zhì)量比8:1時,復(fù)合物的層板間距為1.68nm,主體是水滑石,復(fù)合物的層板峰強度較弱。在質(zhì)量比為10:1和15:1時,復(fù)合物中蒙脫石的001衍射面特征峰消失,說明產(chǎn)物中水滑石層板占主要部分,同時由于剝離影響層板長程無序排列。為了探索其他氨基酸對插層結(jié)構(gòu)的影響,分別采用組氨酸和色氨酸作為層間離子進行了平行實驗。通過XRD表征可以得知水滑石的d003值為0.79nm,Pro-LDH的d003值為0.81nm, His-LDH的d003值為0.88nm, Trp-LDH的d003值為0.92nm,蒙脫石的d00l值為1.28nm,Pro-MMT的d001值為1.36nm,His-MMT的d001值為1.35nm,Trp-MMT的d001值為1.49rm。從插層化合物的層間距可以看出相對于脯氨酸,組氨酸和色氨酸對層狀材料結(jié)構(gòu)的改變更明顯。組氨酸和色氨酸剝離復(fù)合產(chǎn)物的dool值在1.46~1.54nm之間,符合形成雙層板層狀化合物的層間距條件,說明三種氨基酸均可以作為客體分子進入水滑石與蒙脫石的層板間形成雙層板層狀化合物。
[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.
【學(xué)位授予單位】:北京化工大學(xué)
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2015
【分類號】:TB332
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