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Synthesis of New Layered Double Hydroxide Intercalates

新型层状双氢氧化物插层物的合成

基本信息

批准号：
04045054
负责人：
NARITA Eiichi
金额：
$ 0.64万
依托单位：
Hachinohe National College of Technology
依托单位国家：
日本
项目类别：
Grant-in-Aid for international Scientific Research
财政年份：
1992
资助国家：
日本
起止时间：
1992 至无数据
项目状态：
已结题

来源：
https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-04045054/
关键词：
Layerd Double Hydroxide Hydrotalcite Intercalation Coprecipitation Intercalate Layered Compound Heteropolyoxometallate Silicate

项目摘要

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

层状双氢氧化物（LDHs），[NM^<2+>_xM^<3+>_<1-x>(OH)_2][A^<n->_<x/n>·yH_2O]，由带正电的水镁石状层组成，由电荷平衡的水合通道阴离子A^<n->分隔。在本研究中，采用新技术制备了多金属氧酸盐（POM）为支柱的LDHs。采用离子交换法研究了不同层距的硅酸盐阴离子在羧酸柱状LDH的孔道空间中的烧结行为。通过在含有硅酸颗粒的NaOH溶液中加入起始母质LDH，在剧烈搅拌的条件下，将反应混合物回流至100‰/ h，发现硅酸阴离子可以从基底间距为11.4 ~ 12.1‰/ h的硅化LDH中插入。初始廊高对硅化LDH层间结构有一定的影响，基底间距稍大的亲本LDH和邻苯二甲酸柱状LDH （d_<003>=13.9A^^）得到了以二维硅酸盐阴离子为层间客体的有序LDH产物。硅化LDH产物的结晶度顺序为：己二酸酯柱状LDH [d_<003>=13.9A^^)>对苯二甲酸酯柱状LDH (14.5A^^)>癸二酸酯柱状LDH (16.8A^^)>氯化LDH (7.8A^^)> >月桂酸酯柱状LDH （31.5A^^）。并用XRD、IR、TG-DTA、MAS-NMR等方法对硅化LDHs进行了表征。用共沉淀法直接合成多金属氧柱层状双氢氧化物本文采用共沉淀法制备了聚金属氧柱LDH。首先，将α -[SiW_<11>O_<39>]^<8->溶于水中，并将POM溶液的pH调整为6.0。然后，将Zn^<2+>和Al^<3+>离子的混合溶液滴加到100‰的强力搅拌POM溶液中。在中酸性α -[SiW_<11>O_<39>]^<8->溶液中，Zn^<2+>和Al^<3+>离子直接共沉淀反应，得到了近似匹配组成为[Zn_<24>Al_8(OH)_<64>][α -SiW_<11>O_<39>]的LDH衍生物，其廊高异常有序，为9.8A^^ <s:1>。少