Synthesis and Characterization of Magnesium-Aluminum-Indium Hydrotalcite-Like Compounds
-
摘要: 采用共沉淀法合成了含有金属铟离子的碳酸根型水滑石, 研究了沉淀方式、温度、pH值、老化时间和镁铝铟摩尔比这些对镁铝铟类水滑石(Mg-Al-InHTlc) 的纯度和结晶度有影响的合成条件.通过XRD及IR表征, 结果表明以恒定pH值的高过饱和沉淀法, 控制其沉淀和老化温度在65℃、洗涤温度为室温, pH值为10~11.5, 老化时间为8h, n (In3+)/n (M3+) 在0.1~0.8之间可以得到纯度高和结晶好的镁铝铟类水滑石.Abstract: Carbonate pillared Mg-Al-In hydrotalcites were synthesized by coprecipitation. Various preparative factors such as precipitation method, operation temperature, pH value, aging time and n (Mg): n (Al): n (In) molar ratio, which affect the purity and crystal form of Mg-Al-In hydrotalcite-like compound were studied. The results of product characterization by XRD and IR methods show that high supersaturation coprecipitation at constant pH, handing precepitation temperature and aging temperature at 65℃, washing temperature at room temperature, pH ranging from 10 to 11.5, aging for 8 h and n (In3+)/n (M3+) molar ratio ranging from 0.1 to 0.8, may give rise to high purity and better crystal form of Mg-Al-In hydrotalcite-like compounds.
-
Key words:
- indium /
- hydrotalcite-like compound /
- coprecipitation /
- preparation displine /
- characterization
-
图 1 样品的XRD谱
(1) MgAlInHT-3H-高过饱和沉淀法制备的Mg-Al-In HTlc; (2) MgAlInHT-3L-低过饱和沉淀法制备的Mg-Al-InHTlc
Fig. 1. XRD pattern of samples
图 2 不同pH值(a)、老化时间(b) 和n (Mg) ∶n (Al) ∶n (In) 比(c) 制备的MgAlInHT的XRD谱
Fig. 2. XRD patterns of MgAlInHT prepared at different pH values (a), aging time (b) and n (Mg) ∶n (Al) ∶n (In) molar ratios (c)
表 1 温度对水滑石晶形的影响
Table 1. Effect of temperature upon crystal form of hydrotalcite
表 2 老化时间对水滑石晶形的影响
Table 2. Effect of aging time upon crystal form of hydrotalcite
表 3 不同n (Mg) ∶n (Al) ∶n (In) 比的MgAlInHT的晶体结构参数
Table 3. Crystal structure parameters of MgAlInHT with different n (Mg) : n (Al) : n (In) ratios
表 4 不同n (Mg) ∶n (Al) ∶n (In) 比的MgAlInHT的红外光谱数据
Table 4. Data of IR spectra of MgAlInHT with different n (Mg) ∶n (Al) ∶n (In) ratios
-
[1] Cavani F, Trifiro F, Vaccari A. Hydrotalcite-type anionic clays: preparation, properties and application[J]. Catal Today, 1991, 11: 173-301. doi: 10.1016/0920-5861(91)80068-K [2] Kaneda K, Yamaguchi K, Mori K, et al. Catalyst design of hydrotalcite compounds for efficient oxidations[J]. Catal Surv Jpn, 2000, 4: 31-38. doi: 10.1023/A:1019048407764 [3] 张岩, 王梅祥, 黄志镗, 等. 水相中金属有机化学反应的研究进展[J]. 化学进展, 1999, 4: 394-402. doi: 10.3321/j.issn:1005-281X.1999.04.007ZHANG Y, WANG M X, HUANG Z T, et al. Advances in organometallic reactions in aqueous media[J]. Progress in Chemistry, 1999, 4: 394-402. doi: 10.3321/j.issn:1005-281X.1999.04.007 [4] 袁耀峰, 曹忠, 胡爱国, 等. 铟试剂在有机合成中的应用[J]. 有机化学, 2000, 3: 269-281. doi: 10.3321/j.issn:0253-2786.2000.03.001YUAN Y F, CAO Z, HUAG, et al. Application of indium reagents in organic synthesis[J]. Chinese Journal of Organic Chemistry, 2000, 3: 269-281. doi: 10.3321/j.issn:0253-2786.2000.03.001 [5] Aramendía M A, Borau V, Jiménez C, et al. Synthesis and characterization of a novel Mg/In hydrotalcite-like compound[J]. Mater Lett, 2000, 43: 118-121. doi: 10.1016/S0167-577X(99)00243-8 [6] 肖轶, 马骏, 杨锡尧, 等. 碳酸根离子柱撑钴铝水滑石的合成与表征[J]. 催化学报, 1999, 4: 459-462. doi: 10.3321/j.issn:0253-9837.1999.04.020XIAO Y, MA J, YANG X Y, et al. Synthesis and characterization of carbonate pillared Co-Al hydrotalcite-like compound[J]. Chinese Journal of Catalysis, 1999, 4: 459-462. doi: 10.3321/j.issn:0253-9837.1999.04.020 -
下载:
点击查看大图
计量
- 文章访问数: 3695
- HTML全文浏览量: 370
- PDF下载量: 5
- 被引次数: 0
