CN106076336A - 一种磁性氧化铁纳米片的制备方法 - Google Patents
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- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title claims abstract description 15
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Abstract
本发明公开一种磁性氧化铁纳米片的制备方法。依次包括如下步骤：取500mL FeCl2溶液，置于恒温70～80℃水浴中，向溶液中同时滴加30％(质量分数)双氧水2～4mL和一定量的NaOH稀溶液，保持pH值为12～13，反应2～3h，转入高压釜中，在1h内升温到150～180℃，继续反应4～8h，自然冷却到室温，在该过程中形成具有层状结构的沉淀，沉淀分离，去离子水洗2～3遍；将沉淀得到的固体加入到浓度为2～4mol/L的乳酸钠溶液中，固液比为1：10～1：50，搅拌4～5h，沉淀分离，获得的固体在用去离子水洗涤2～3遍之后，在400～450℃的温度下煅烧，去除其中的乳酸根，即可得到一种氧化铁纳米片。该结构有利于吸附和催化污染物，同时有利于分离。
Description
技术领域
本发明涉及环境污染控制新材料的开发，尤其涉及一种氧化铁纳米片的制备方法。
背景技术
有机废气处理是指在工业生产过程中产生的有机废气进行吸附、过滤、净化的处理工作。通常有机废气处理有甲醛有机废气处理、苯甲苯二甲苯等苯系物有机废气处理等等。有机废气一般都存在易燃易爆、有毒有害、不溶于水、溶于有机溶剂、处理难度大的特点。在有机废气处理时普遍采用的是有机废气活性炭吸附处理法、催化燃烧法、催化氧化法、酸碱中和法、等离子法等多种原理。催化氧化是一种比较经济有效的方法。但需要有经济适合普遍适用的催化剂。
纳米氧化铁具有良好的耐候性、耐光性、磁性和对紫外线具有良好的吸收和屏蔽效应，是一种重要的无机材料。在催化、功能陶瓷、磁性材料和透明颜料等领域具有重要的应用。纳米氧化铁具有巨大的比表面积，表面效应显著，也是一种很好的催化剂。用纳米粒子制成的催化剂的活性、选择性都高于普通催化剂，并且寿命长易操作。将用纳米氧化铁做成的空心小球，浮在含有机物的废水表面上。利用太阳光进行有机物的降解可加速废水处理过程。纳米氧化铁已直接用作高分子聚合物氧化、还原及合成的催化剂，纳米氧化铁催化剂可使石油的裂解速度提高1～5倍，以其作为燃烧催化剂制成的固体推进剂的燃烧速度较普通推进剂可提高1～10倍，这对制造高性能火箭及导弹十分有利。纳米氧化铁还可以催化分解水，制成清洁能源。
通过将磁性纳米颗粒分散在某种基体中制成磁性纳米复合材料可有效防止纳米颗粒间的相互团聚，有效地控制其颗粒尺寸。此外，磁性颗粒镶嵌在不能混合的介质中将导致一些奇异的物理和化学特征。
水滑石类化合物(LDHs)是由层间阴离子及带正电荷层板堆积而成的化合物。水滑石化学结构通式为：[M2+ 1-xM3+x(OH)2]x+[(An-)x/n·mH2O]，其中M2+和M3+分别为位于主体层板上的二价和三价金属阳离子，如Mg2+、Ni2+、Zn2+、Mn2+、Cu2+、Co2+、Pd2+、Fe2+等二价阳离子和Al3 +、Cr3+、Co3+、Fe3+等三价阳离子均可以形成水滑石；An–为层间阴离子，可以包括无机阴离子，有机阴离子，配合物阴离子、同多和杂多阴离子；x为M3+/(M2++M3+)的摩尔比值，大约是4:1到2:1；m为层间水分子的个数。其结构类似于水镁石Mg(OH)2，由八面体共用棱边而形成主体层板。位于层板上的二价金属阳离子M2+可以在一定的比例范围内被离子半价相近的三价金属阳离子M3+同晶取代，使得层板带正电荷，层间存在可以交换的的阴离子与层板上的正电荷平衡，使得LDHs的整体结构呈电中性。层间的阴离子可被交换，经过一系列改性，水滑石材料可以得到许多种性能各异的物质。
发明内容
本发明的目的是为克服现有技术中氧化铁结构单一的不足，提供一种氧化铁纳米片的制备方法。
本发明采用的技术方案是依次包括如下步骤：
1)将FeCl2溶解到水中，配置为浓度为2～3mol/L的溶液，取将500mL该溶液，向其中置于恒温70～80℃水浴中，同时滴加30％(质量分数)双氧水2～4mL和一定量的NaOH稀溶液，保持pH值为12～13，反应2～3h，转入高压釜中，在1h内升温到150～180℃，继续反应4～8h，自然冷却到室温，在该过程中形成具有层状结构的沉淀，沉淀分离，去离子水洗2～3遍；
2)将沉淀得到的固体加入到浓度为2～4mol/L的乳酸钠溶液中，固液比为1：10～1：50，搅拌4～5h，沉淀分离，获得的固体在用去离子水洗涤2～3遍之后，在400～450℃的温度下煅烧，去除其中的乳酸根，即可得到一种磁性氧化铁纳米片。
本发明的优点是：部分二价铁离子被双氧水氧化生成的三价铁，二价离子和生成的三价离子在70～80℃水浴中碱的作用下，产生磁性共沉淀，形成片层水滑石结构，再在片层间交换入乳酸根，最后通过高温煅烧将乳酸根去除，形成相对散开的片层结构。该结构有利于吸附和催化污染物。
具体实施方式
以下进一步提供本发明的3个实施例：
实施例1
将FeCl2溶解到水中，配置为浓度为3mol/L的溶液，取将500mL该溶液，向其中置于恒温80℃水浴中，同时滴加30％(质量分数)双氧水4mL和一定量的NaOH稀溶液，保持pH值为13，反应3h，转入高压釜中，在1h内升温到180℃，继续反应8h，自然冷却到室温，在该过程中形成具有层状结构的沉淀，沉淀分离，去离子水洗3遍；将沉淀得到的固体加入到浓度为4mol/L的乳酸钠溶液中，固液比为1：50，搅拌5h，沉淀分离，获得的固体在用去离子水洗涤3遍之后，在450℃的温度下煅烧，去除其中的乳酸根，即可得到一种磁性氧化铁纳米片。
取1g氧化铁纳米片，加入到1.0L待处理的亚甲基蓝废水中，再加入0.01毫升质量分数为30％的双氧水，搅拌20min，有机物被分解，磁场分离，去除率97.2％，上清液可以排放。
实施例2
将FeCl2溶解到水中，配置为浓度为2mol/L的溶液，取将500mL该溶液，向其中置于恒温70℃水浴中，同时滴加30％(质量分数)双氧水2mL和一定量的NaOH稀溶液，保持pH值为12，反应2h，转入高压釜中，在1h内升温到150℃，继续反应4h，自然冷却到室温，在该过程中形成具有层状结构的沉淀，沉淀分离，去离子水洗2遍；将沉淀得到的固体加入到浓度为2mol/L的乳酸钠溶液中，固液比为1：10，搅拌4h，沉淀分离，获得的固体在用去离子水洗涤2遍之后，在400℃的温度下煅烧，去除其中的乳酸根，即可得到一种磁性氧化铁纳米片。
取1g氧化铁纳米片，加入到1.0L待处理的亚甲基蓝废水中，再加入0.01毫升质量分数为30％的双氧水，搅拌20min，有机物被分解，磁场分离，去除率97.5％，上清液可以排放。
实施例3
将FeCl2溶解到水中，配置为浓度为3mol/L的溶液，取将500mL该溶液，向其中置于恒温80℃水浴中，同时滴加30％(质量分数)双氧水3mL和一定量的NaOH稀溶液，保持pH值为13，反应3h，转入高压釜中，在1h内升温到180℃，继续反应6h，自然冷却到室温，在该过程中形成具有层状结构的沉淀，沉淀分离，去离子水洗3遍；将沉淀得到的固体加入到浓度为4mol/L的乳酸钠溶液中，固液比为1：50，搅拌5h，沉淀分离，获得的固体在用去离子水洗涤3遍之后，在450℃的温度下煅烧，去除其中的乳酸根，即可得到一种磁性氧化铁纳米片。
取1g氧化铁纳米片，加入到1.0L待处理的亚甲基蓝废水中，再加入0.01毫升质量分数为30％的双氧水，搅拌20min，有机物被分解，磁场分离，去除率94.3％，上清液可以排放。
Claims (1)
1.一种磁性氧化铁纳米片的制备方法，其特征是依次包括如下步骤：
1)将FeCl2溶解到水中，配置为浓度为2～3mol/L的溶液，取将500mL该溶液，向其中置于恒温70～80℃水浴中，同时滴加30％(质量分数)双氧水2～4mL和一定量的NaOH稀溶液，保持pH值为12～13，反应2～3h，转入高压釜中，在1h内升温到150～180℃，继续反应4～8h，自然冷却到室温，在该过程中形成具有层状结构的沉淀，沉淀分离，去离子水洗2～3遍；
2)将沉淀得到的固体加入到浓度为2～4mol/L的乳酸钠溶液中，固液比为1：10～1：50，搅拌4～5h，沉淀分离，获得的固体在用去离子水洗涤2～3遍之后，在400～450℃的温度下煅烧，去除其中的乳酸根，即可得到一种磁性氧化铁纳米片。
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107899578A (zh) * | 2017-10-25 | 2018-04-13 | 浙江科技学院 | 一种粽状微米级氧化铁非均相类光芬顿催化剂及其制备方法 |
| CN108186677A (zh) * | 2018-01-05 | 2018-06-22 | 中国科学院上海硅酸盐研究所 | 新型自由基高效产生的可降解纳米材料及其制备方法和应用 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107899578A (zh) * | 2017-10-25 | 2018-04-13 | 浙江科技学院 | 一种粽状微米级氧化铁非均相类光芬顿催化剂及其制备方法 |
| CN107899578B (zh) * | 2017-10-25 | 2020-05-26 | 浙江科技学院 | 一种粽状微米级氧化铁非均相类光芬顿催化剂及其制备方法 |
| CN108186677A (zh) * | 2018-01-05 | 2018-06-22 | 中国科学院上海硅酸盐研究所 | 新型自由基高效产生的可降解纳米材料及其制备方法和应用 |
| CN108186677B (zh) * | 2018-01-05 | 2020-05-19 | 中国科学院上海硅酸盐研究所 | 自由基高效产生的可降解纳米材料及其制备方法和应用 |
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