Synthesis of New Layered Double Hydroxide Intercalates

分层双氢氧化物（LDhs），[NM^<2+>_xM ^<3+>_<1-x>（OH）_2][A^<n->_<x/n>·yH_2O]，一个正电荷电荷平衡的氢化画廊动画A^<n->。在本研究中，聚氧酸盐（POM）-柱LDH已由新技术准备好。通过羧基-柱预cursorsIntercalation of silicate-intercalated LDH的制备和表征，Intercalation of silicate anions in gallery space of carboxylate-pillared LDH with different layer distance has been investigated by ion exchange method。通过在NaOH溶液中添加一个起始父LDH的NaOH溶液中加入硅酸颗粒，并通过在100个反应混合物中重新冲洗发现了硅酸洋葱，可以从硅LDH的基础间隔中插入11.4-12.1A^在> O.5M NaOH的条件和反应时间为2.5小时。However，硅化LDH的中间层结构受到初始画廊高度O的影响 ... More f父母LDH和双柱LDH有一个小的大基础空间[d_<003>=13.9A^^]）提供了最好的LDH产品，其中两个尺寸硅离子作为中间客人。硅化LDH产品按顺序排列：双柱LDH [d_<003>=13.9A^^]） &gt;三柱LDH （14.5A^^]） &gt;六柱LDH（16.8A^^]）&gt;氯化LDH （7.8A^^]）&gt;低柱LDH （31.5A^^]）。还对XRD、IR、TG-DTA、MAS-NMR等进行了调查。Direct synthesis of a polyoxometallate-pillared layered double hydrooxide by copreciptationA new method for the preparation of POM-pillared LDH has been accomplished by using the corecipitation reaction as follows。第一，alpha-[SiW_<11>O_<39>]^&lt;8-&gt;在水中被分解，pH值被调整到6.0以下。然后，锌&lt;2+&gt;和Al &lt;3+&gt;的混合解决方案被添加到100 ℃的明显僵硬POM解决方案中。锌^&lt;2+&gt;和Al^&lt;3+&gt;离子在中等酸性Alpha-[SiW_<11>O_<39>]^&lt;8-&gt;直接找到了一个含有[Zn_<24>Al_8（OH）_<64>][α-SiW_<11>O_<39>]的近似伴侣组合物的LDH衍生物的解决方案，以及一个非常好的9.8A^。Less（低）

Layered Double Hydroxides (LDHs),[NM^<2+>_xM^<3+>_<1-x>(OH)_2][A^<n->_<x/n>・yH_2O], consist of positively charged brucite-like layers separated by charge-balancing hydrated gallery anions A^<n->. In this study, polyoxometallate (POM)-pillared LDHs have been prepared by the new techniques.1. Preparation and characterization of silicate-intercalated LDHs via carboxylate-pillared precursorsIntercalation of silicate anions in gallery space of carboxylate-pillared LDH with different layer distance has been investigated by ion exchange method. The intercalation was carried out by adding a starting parent LDH in NaOH solution containing silicic acid granulas with vigorous stirring and by refluxing the reaction mixture at 100 ﾟCSilicate anions were found to be intercalated to from the silicated LDH with basal spacing of 11.4-12.1A^^ﾟ at the conditions of > O.O5 M NaOH and reaction time of 2.5 h. However, the interlayer structure of the silicated LDH was influenced with initial gallery height o … More f the parent LDH and the adipate-pillared LDH having a little bigger basal spacing [d_<003>=13.9A^^ﾟ) has givern the most well-ordered LDH product with two-dimensional silicate anions as the interlayer guest. The crystallinity of the sillicated LDH products was in order: adipate-pillared LDH [d_<003>=13.9A^^ﾟ) > terephthalate-pillared LDH (14.5A^^ﾟ) > sebacate-pillared LDH (16.8A^^ﾟ)> chlorinated LDH (7.8A^^ﾟ) > > laurate-pillared LDH (31.5A^^ﾟ). The silicated LDHs were also investigated by XRD, IR, TG-DTA, MAS-NMR etc.2. Direct synthesis of a polyoxometallate-pillared layered double hydroxide by copreciptationA new method for the preparation of POM-pillared LDH has been accomplished by using the corecipitation reaction as follows. First, alpha-[SiW_<11>O_<39>]^<8-> was dissolved in water and pH the POM solution was adjusted to6.0. Then, the mixed solution of Zn^<2+> and Al^<3+> ions was added drop-wise to the vigorously stirred POM solution at 100 ﾟC. The coprecipita-tion reaction of Zn^<2+> and Al^<3+> ions in moderately acidic alpha-[SiW_<11>O_<39>]^<8-> solution directly was found to afford a LDH derivative with an approxi-mate composition of [Zn_<24>Al_8(OH)_<64>][alpha-SiW_<11>O_<39>] and an exceptionally well-ordered gallery height of 9.8A^^ﾟ. Less