CN116119725A - 一种还原型含铁水滑石材料的制备方法 - Google Patents
一种还原型含铁水滑石材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种制备还原型含铁水滑石材料的方法。该方法是在简单共沉淀法制备水滑石材料的基础上，通过向前驱体溶液中加入一定量的还原剂和表面活性剂，其中还原剂可以使水滑石材料中的少部分铁元素价态稳定在+2，表面活性剂可以稳定水滑石材料层板上的一些点缺陷和微小的结构畸变，进而调控水滑石材料的晶体结构，从而得到具有还原型且形貌可调控的还原型含铁水滑石材料。制备得到的产物在非均相Fenton降解和电催化分解水等领域表现出优异的性能。
Description
技术领域
本发明属于无机纳米材料合成领域，特别涉及一种通过添加还原剂和表面活性剂，合成含有部分低价态铁的还原型水滑石材料的制备方法。
背景技术
水滑石材料是层状双氢氧化物(Layered Double Hydroxides,LDHs)的俗称。LDHs是由带正电的类水镁石金属层板和带负电的层间阴离子交替组装形成的层状材料，其中层板上的金属阳离子通常由二价金属阳离子和高价金属阳离子组成。常见的二价金属阳离子有Mg2+、Zn2+、Co2+、Cu2+、Ni2+等，高价金属阳离子有Al3+、Cr3+、Fe3+、Ti4+等；层间的平衡电荷通常由CO3 2-、Cl-等阴离子和溶剂分子组成，层板和插层离子有序交替排列，通过静电作用等弱作用力形成三维稳定结构。在均相溶液中，通过调控溶液的pH值可以制备得到水滑石类材料，比如2008年权五玲等报道了通过沉淀结晶的方法制备镁铝水滑石材料(CN200880131817.5)，卫敏等报道了通过反相微乳液方法合成ZnTi和NiTi两种水滑石材料(CN201210434472.9和CN201210434511.5)。
含铁LDHs是水滑石材料中的重要成员，其中Fe元素经常作为反应活性中心或者辅助活性元素。例如李大鹏等报道了一种铁基水滑石的制备方法(CN201810443841.8)，其中NiFe-LDH在电催化析氧反应中表现出不错的性能；江鸿等报道了一种Co2FeAl-LDH的其制备方法，可以活化过一硫酸盐产生强氧化的硫酸根自由基快速催化降解污水中的污染物(CN201911148448.7)。最近研究表明含有+2价的还原型含铁LDHs因其表面电荷环境的改变，常常具有更为优异的特性。由于Fe2+具有较强的还原性，容易被空气中的氧气等各类氧化剂氧化失去一个电子转化为+3价，因此低价铁不能大量稳定存在于含铁LDHs材料中。例如光电子能谱显示，NiFe-LDH中的铁元素普遍以Fe3+的形式存在，几乎没有Fe2+。利用传统共沉淀法合成含铁LDHs的过程，往往需要在中温条件下成核生长从而形成LDHs，这样的环境进一步加速了Fe2+的氧化，从而制备得到的是具有+3价这种最稳定价态的含铁LDHs。最近孔祥贵等报道了一种通过引入聚乙烯亚胺保护，得到具有还原性水滑石的方法(CN202211152358.7)。我们考虑在低化学势的还原性溶剂条件下，通过加入表面活性剂，稳定LDHs层板结构的微小畸变，从而使LDHs中的部分铁离子处于较低化合价下。这些稳定的还原型含铁LDHs在电催化、非均相Fenton高级氧化技术等领域具有广阔的应用前景。
发明内容
本发明的目的是提供一种制备还原型含铁水滑石材料的方法。其原料廉价易得，合成步骤简单，易于规模化生产，所得到的还原型含铁水滑石材料结构稳定，可重复行好，在电催化和非均相Fenton高级氧化技术等方面具有优异的性能。
本发明的构思如下，在简单共沉淀法制备含铁水滑石材料合成方法的基础上，通过改变加料顺序，在混合溶液中添加还原剂和表面活性剂用以调节水滑石材料成核生长的环境，最终使得水滑石材料中的部分铁离子处于稳定的低价态，且通过调节溶液的反应温度、pH等参数实现对产品形貌一定程度的调控。
具体的，本发明给出的一种制备还原型水滑石材料的方法，包括以下步骤：
(1)配制含有铁盐和弱还原性的多糖混合溶液A：其中铁离子的浓度为5-100mmol；弱还原性的多糖物质总浓度为2-50mmol。
(2)配制含有其他金属盐和表面活性剂的混合溶液B：其中金属阳离子的总浓度为10-200mmol；表面活性剂的浓度为1-50mmol。
(3)将溶液A与溶液B快速混合后，用碱性试剂调节混合溶液的pH为7-11。进一步置于反应容器中，在中温条件下反应一段时间，得到还原型含铁水滑石材料。
本发明步骤(1)中所用的铁离子盐可以为含铁二价或者三价的硫酸盐，硝酸盐或者氯化盐中的一种或几种的任意混合；弱还原性的物质可以为葡萄糖或甘露糖等含醛基的多糖物质中的一种或几种的任意混合。
本发明步骤(2)中所用的金属盐中阳离子可以为Zn2+，Mg2+，Co2+，Ni2+等的一种或几种的任意组合，可以为硫酸盐、硝酸盐或氯化盐中的一种或几种的任意混合；表面活性剂可以为十二烷基硫酸钠、十二烷基苯磺酸钠和十六烷基三甲基溴化铵中的一种或几种的任意混合。
本发明步骤(3)中所用的碱性试剂可以为NaOH、KOH、Na2CO3和氨水中的一种或几种的任意混合；所用的反应容器包括但不限于烧瓶、反应釜等反应容器。
本发明取得的有益效果在于：通过添加适量的还原剂和表面活性剂，通过简单的共沉淀法，可以合成还原型水滑石材料。所用原料无毒、廉价，合成步骤简单，可用于大规模生产。所制得的还原型水滑石材料形貌均一、性能优异，可用于高效电解水、电催化有机小分子反应和非均相Fenton降解等领域。
附图说明
图1是实施例1中还原型ZnFe-LDH的扫描电镜图。
图2是实施例1中还原型ZnFe-LDH和正常ZnFe-LDH的XRD对比图。
图3是实施例1中还原型ZnFe-LDH的非均相Fenton降解亚甲基蓝效果图。
图4是实施例4中还原型NiFe-LDH的电催化分解水的线性扫描图。
由图1可知，还原型ZnFeLDH为卷边正六边形纳米片。
由图2可知，与正常ZnFeLDH相比，还原型ZnFeLDH的衍射峰强度减弱，但是仍能保持原来的晶体结构。
由图3可知，在10min内，还原型ZnFe-LDH对亚甲基蓝的降解效率几乎达到100％。
由图4可知，电流密度为100mA/cm2时，还原型NiFe-LDH的过电位只有323mV。
具体实施方式
以下实施例用于说明本发明。
实施例1合成还原型ZnFe-LDH
a：分别取12mmol FeSO4·7H2O与6mmol葡萄糖溶于16mL去离子水中，室温搅拌均匀，标记为溶液A；
b：分别取15mmol Zn(NO3)2·6H2O、5mmol ZnSO4·7H2O与20mmol十二烷基硫酸钠溶于54mL去离子水中，室温搅拌均匀，标记为溶液B；
c：将溶液A与溶液B快速混合后，用1M NaOH溶液调节混合溶液的pH至7，进一步置于100mL反应釜中，110℃加热10h。将得到的固体产物离心、洗涤，烘箱中干燥得到还原型ZnFe-LDH。
实施例2合成还原型MgFe-LDH
a：分别取5mmol FeSO4·7H2O、3mmol FeCl3·6H2O与3mmol葡萄糖溶于16mL去离子水中，室温搅拌均匀，标记为溶液A；
b：分别取24mmol Mg(NO3)2·6H2O与20mmol十六烷基三甲基溴化铵溶于84mL去离子水中，室温搅拌均匀，标记为溶液B；
c：将溶液A与溶液B于250mL圆底烧瓶中混合后，用1.5M NaOH和Na2CO3的混合溶液调节溶液的pH至8，80℃回流加热12h。将得到的固体产物离心、洗涤，烘箱中干燥得到还原型MgFe-LDH。
实施例3合成还原型CoFe-LDH
a：分别取50mmol Fe(NO3)3·9H2O与3mmol甘露糖溶于30mL去离子水中，室温搅拌均匀，标记为溶液A；
b：分别取40mmol Co(NO3)2·6H2O、40mmol CoCl2·6H2O与20mmol十二烷基苯磺酸钠溶于60mL去离子水中，室温搅拌均匀，标记为溶液B；
c：将溶液A与溶液B快速混合后，用1.5M KOH和Na2CO3的混合溶液调节溶液的pH至9，将悬浮液置于100mL反应釜中，75℃加热24h。将得到的固体产物离心、洗涤，烘箱中干燥得到还原型CoFe-LDH。
实施例4合成还原型NiFe-LDH
a：分别取15mmol Fe(NO3)3·9H2O、50mmol FeSO4·7H2O与6mmol甘露糖溶于50mL去离子水中，室温搅拌均匀，标记为溶液A；
b：分别取65mmol Ni(NO3)2·6H2O与15mmol十二烷基硫酸钠溶于200mL去离子水中，室温搅拌均匀，标记为溶液B；
c：将溶液A与溶液B于500mL圆底烧瓶中快速混合后，用1.5M NH3·H2O溶液调节混合溶液的pH至11，90℃回流加热12h。将得到的固体产物离心、洗涤，烘箱中干燥得到还原型NiFe-LDH。
Claims (8)
1.一种还原型层状双金属氢氧化物材料的制备方法，其特征在于包括以下步骤：
(1)配制含有铁盐和弱还原性多糖的混合溶液A：其中铁离子的浓度为5-100mmol；弱还原性的多糖物质总浓度为2-50mmol；
(2)配制含有其他金属盐和表面活性剂的混合溶液B：其中金属阳离子的总浓度为10-200mmol；表面活性剂的浓度为1-50mmol；
(3)将溶液A与溶液B快速混合后，用碱性试剂调节混合溶液的pH为7-11，进一步置于反应容器中，在中温条件下反应一段时间，得到还原型含铁水滑石材料。
2.根据权利要求1所述的制备方法，其特征在于步骤(1)中所用的铁离子盐是含铁二价或者铁三价的硫酸盐，硝酸盐或者氯化盐中的一种或几种的任意混合。
3.根据权利要求1所述的制备方法，其特征在于步骤(1)中所用的弱还原性的物质是葡萄糖或甘露糖含醛基的多糖物质中的一种或几种的任意混合。
4.根据权利要求1所述的制备方法，其特征在于步骤(2)中所用的金属盐中阳离子是Zn2 +，Mg2+，Co2+，Ni2+中的一种或几种的任意组合。
5.根据权利要求1所述的制备方法，其特征在于步骤(2)中所用的金属盐是硫酸盐、硝酸盐、氯化盐中的一种或几种的任意组合。
6.根据权利要求1所述的制备方法，其特征在于步骤(2)中所用的表面活性剂是十二烷基硫酸钠、十二烷基苯磺酸钠和十六烷基三甲基溴化铵中的一种或几种的任意混合。
7.根据权利要求1所述的制备方法，其特征在于步骤(3)中所用的碱性试剂为NaOH、KOH、Na2CO3和氨水中的一种或几种的任意混合。
8.根据权利要求1所述的制备方法，其特征在于步骤(3)中所用的反应容器是烧瓶或反应釜。
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