CN114887591A - 一种MXene/GO/NbFeB水凝胶一步法简单回收黄金的方法和应用 - Google Patents
一种MXene/GO/NbFeB水凝胶一步法简单回收黄金的方法和应用 Download PDFInfo
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Abstract
本发明提供了一种MXene/GO/NbFeB水凝胶一步法简单回收黄金的方法和应用，该制备方法包括：MXene在水溶液中形成MXene水溶液；在MXene水溶液内加入氧化石墨烯GO得到第一混合溶液；在第一混合溶液内加入NbFeB得到第二混合溶液；在第二混合溶液内加入乙二胺四乙酸EDTA，得到第三混合溶液；制备的混合物于超声混合6小时；将制备的混合物置于95℃水浴中8小时。本发明的MXene/GO/NbFeB水凝胶具有强酸性条件(pH＝2)具有超强的吸附还原性能。在凝胶表面快速形成疏松金壳，可轻松剥离；本方法利用二维材料MXene的不稳定性被用于选择性地还原金。GO辅助富集Au。
Description
技术领域
本发明属于环境材料合成技术领域，具体涉及一种MXene/GO/NbFeB水凝胶及其制备方法和一步法简单回收黄金的应用。
背景技术
以往研究的问题是还原金分布在复合材料内外。不能直接回收，需要额外的浸出步骤，浸出效率低。该行业最常见的回收方法涉及高腐蚀性和有毒的王水和氰化物，它们会危害环境。鉴于王水和氰化物的毒性，已开发出替代的无毒浸出剂，如硫脲、硫代硫酸盐和碘来溶解黄金，但它们的浸出性仍然很差，反应过程通常非常复杂。MXene是一类新兴的二维材料，其独特的结构和表面化学性质赋予了MXene许多关键特性，如金属导电性、亲水性表面、丰富的官能团、这与其他二维材料不同.Ti(III)和Ti(IV)在MXene中的转化导致MXene独特的氧化还原特性。
发明内容
针对现有技术中的不足，本发明的首要目的是提供一种MXene/GO/NbFeB 水凝胶，达到一步法黄金。
本发明的第二个目的是提供上述MXene/GO/NbFeB水凝胶的制备方法。
本发明的第三个目的是提供上述MXene/GO/NbFeB水凝胶的用途。
为达到上述目的，本发明的解决方案是：
一种MXene/GO/NbFeB水凝胶的制备方法，其包括如下步骤：
(1)MXene在水溶液中形成MXene水溶液；
(2)在MXene水溶液内加入氧化石墨烯GO得到第一混合溶液；
(3)在第一混合溶液内加入NbFeB得到第二混合溶液；
(4)在第二混合溶液内加入乙二胺四乙酸EDTA，得到第三混合溶液；
(5)将制备的混合物于超声混合6小时；
(6)将制备的混合物置于95℃水浴中8小时；；
优选地，在步骤(1)中，MXene水溶液中，MXene的浓度为10mg/mL。
优选地，在步骤(2)中，氧化石墨烯GO的浓度为20mg/mL。
优选地，在步骤(3)中，所述的NbFeB浓度为15mg/mL。
优选地，在步骤(4)中，所添加的乙二胺四乙酸EDTA的浓度为1mL。
优选地，在步骤(5)中，超声时间为6h。
优选地，在步骤(6)中，水浴的温度为95℃，所述加热的时间为8h。。
一种MXene/GO/NbFeB水凝胶由上述制备方法得到。
一种上述的MXene/GO/NbFeB水凝胶作为吸附剂的使用。
由于采用上述方案，本发明的有益效果是：
第一、本发明采用氧化石墨烯GO形成凝胶，不仅具有较好的生物相容性，而且还具有优良的成胶性能，凝胶机械性能良好；GO对Au(III)具有强烈的吸附亲和性，能帮助MXene富集Au离子。
第二、本发明的Mxene具有优异的电化学性能，表面具有大量官能团，活性位点。通过使Mxene与氧化石墨烯GO结合提升了氧化石墨烯GO的吸附性能，还提升了有机凝胶的机械强度。Ti(III)和Ti(IV)在MXene中的转化导致MXene 独特的氧化还原特性，能帮助选择性的还原回收黄金。
第三、形成的MXene/GO/NbFeB水凝胶在回收黄金时，凝胶表面快速形成疏松金壳，可轻松剥离金壳。
第四、本发明的制备方法中设备简单，工艺简单易行，可以连续化操作，从而适于大规模生产。
总之，本发明的MXene/GO/NbFeB水凝胶，氧化石墨烯GO结合MXene形成的有机凝胶，材料具有大量官能团，在吸附过程中可以提供丰富的吸附位点。通过MXene的还原特性对金离子进行简单高效的选择性吸附和还原；通过GO 增强材料电子传输；乙醇浸泡后松散金层的应力降低。外层金纳米层可以很容易地用刷子分离，并保留完整的凝胶结构。
附图说明
图1为本发明的MXene/GO/NbFeB水凝胶在加磁和不加磁条件下，对环保沙星吸附动力学效果示意图。
图2为本发明的MXene/GO/NbFeB水凝胶在加磁和不加磁条件下，对铜离子吸附动力学效果示意图。
图3为本发明的MXene/GO/NbFeB水凝胶与氧化石墨烯GO/CoFeO凝胶球的压缩应力-应变曲线对比示意图。(横坐标Strain表示应变，纵坐标 CompressionStress表示压缩应力)
图4为本发明的MXene/GO/NbFeB水凝胶的透射电子显微镜表征结果示意图。
图5为本发明的MXene/GO/NbFeB水凝胶扫描电子显微镜表征结果示意图。
具体实施方式
以下结合实施例对本发明作进一步的说明。
实施例1：
本实施例的MXene/GO/NbFeB水凝胶的制备方法包括如下步骤：
(1)称量100mgMXene在10ml中性水溶液内溶解，并移入50ml的容量瓶内，其中，MXene的浓度为10mg/mL；
(2)在MXene水溶液内加入200mg氧化石墨烯GO，得到第一混合溶液其中，GO的浓度为20mg/mL；
(3)在第一混合溶液内加入150mg NbFeB，得到第二混合溶液；其中，NbFeB 的浓度为15mg/mL；
(4)量取1ml乙二胺四乙酸加入到第二混合溶液其中，得到第三混合溶液；
(5)将第三混合溶液超声6小时，得到MXene/GO/NbFeB分散液；
(6)将得到MXene/GO/NbFeB分散液在水浴锅内加热(温度为95℃，时间为8h)，得到MXene/GO/NbFeB水凝胶。
<实验>
以上述实施例的产品分别进行如下实验。
<实验1>
本实验的目的是为了探究MXene/GO/NbFeB水凝胶在加磁和不加磁条件下对不同污染物吸附性能的影响。
如图1，图2所示，准一级(PF)和准二级(PS)动力学模型吸附动力学模型用于拟合金离子提取的实验数据。拟合数据(图1)表明PS的拟合效果很好，Au(III)的理论饱和吸收量为1809.068mg/g，几乎是MXene膜(理论容量153.53 mg/g)的13倍。)如图S2所示。吸附模型的参数在表S3中给出。分析表明化学吸附是萃取过程的速率控制步骤。通过图4b可以发现，随着磁场的加入，萃取前半段的回收率大大提高。通过增强物质的传输，磁场促进了AuCl4-在材料表面更快更均匀的吸附，Au(III)被还原为金元素[21]。在磁场的作用下，MXH表面快速形成金层，会阻断水凝胶由外到内的通道，从而进一步保证只有金在外部被还原，为剥金的简单步骤。结合表征分析，说明MXene对Au(III)的相互作用有决定性的影响。MXene和Au直接交换电子，发生的氧化还原反应促进了 Au元素的还原。通过数据处理可知，MXene对Au的还原反应符合所提出的二次反应动力学模型(图1)，且起始反应浓度越大，浓度减半所需的时间越短。
为了进一步研究MXene水凝胶的吸附能力，在25-250mg/L的初始Au (III)浓度下应用吸附等温线。发现图2所示的吸附等温线数据与Freundlich模型而不是Langmuir模型相匹配，这证明化学吸附发生在材料表面。等温线模型拟合给出的饱和吸附容量为2821.8mg/g。上述等温线模型的拟合结果也证明水凝胶与金离子在表面交换电子，发生氧化还原反应。表征分析和实验数据拟合结果表明，金离子的还原发生在MXene凝胶表面，因此金离子浓度对还原反应速率的影响应遵循Langmuir-Hinshelwood动力学模型。从图2的右下角可以看到1/r 和1/c之间的良好线性关系(R2＝0.991)，其中k(朗缪尔速率常数)为2.51， Kr(表观速率常数)为0.047。
<实验2>
本实验的目的是为了探究MXene/GO/NbFeB水凝胶的机械性能的影响。
图3为MXene/GO/NbFeB水凝胶压缩应力-应变曲线。为了测试凝胶的机械性能，将材料制成一个半径为50毫米(±0.1毫米)，高度为100毫米的小圆柱体。根据压缩应力-应变曲线图S4c，GO/MXene/NbFeB在24.89％应变下的断裂应力为0.81MPa，相应的弹性模量为3.25MPa，表现非常好。
<实验3>
本实验的目的是为了研究MXene/GO/NbFeB水凝胶在不同分辨率下的SEM 形貌图。
由图4可知，SEM图像显示功能性复合材料的表面表现出相分离和不均匀性，并且该表面具有无孔结构。由图可以清楚地区分MXene的层状结构和CoFeO 的块状晶体。图3显示了薄片的典型MXene结构，这证明MXene和CoFeO已经很好地混入了材料中。
上述对实施例的描述是为了便于该技术领域的普通技术人员能理解和使用本发明。熟悉本领域技术人员显然可以容易的对这些实施例做出各种修改，并把在此说明的一般原理应用到其他实施例中，而不必经过创造性的劳动。因此，本发明不限于上述实施例。本领域技术人员根据本发明的原理，不脱离本发明的范畴所做出的改进和修改都应该在本发明的保护范围之内。
Claims (9)
1.一种MXene/GO/NbFeB水凝胶的制备方法，其特征在于：其包括如下步骤：
(1)MXene在水溶液中形成MXene水溶液；
(2)在MXene水溶液内加入氧化石墨烯GO得到第一混合溶液；
(3)在第一混合溶液内加入NbFeB得到第二混合溶液；
(4)在第二混合溶液内加入乙二胺四乙酸EDTA，得到第三混合溶液；
(5)将制备的混合物于超声混合多个小时；
(6)将制备的混合物置于水浴中多个小时。
2.根据权利要求1所述的MXene/GO/NbFeB水凝胶的制备方法，其特征在于：步骤(1)中，所述MXene水溶液中，MXene的浓度为10mg/mL。
3.根据权利要求1所述的MXene/GO/NbFeB水凝胶的制备方法，其特征在于：步骤(2)中，所述氧化石墨烯GO的浓度为20mg/mL。
4.根据权利要求1所述的MXene/GO/NbFeB水凝胶的制备方法，其特征在于：步骤(3)中，所述的NbFeB浓度为15mg/mL。
5.根据权利要求1所述的MXene/GO/NbFeB水凝胶的制备方法，其特征在于：步骤(4)中，所添加的乙二胺四乙酸EDTA体积是1ml。
6.根据权利要求1所述的MXene/GO/NbFeB水凝胶的制备方法，其特征在于：步骤(5)中，制备的混合物于超声混合6小时。
7.根据权利要求1所述的MXene/GO/NbFeB水凝胶的制备方法，其特征在于：步骤(6)中，所述水浴的温度为95℃，所述加热的时间为8h。
8.一种MXene/GO/NbFeB水凝胶，其特征在于：其由如权利要求1-7任一项所述的制备方法得到。
9.一种如权利要求9所述的MXene/GO/NbFeB水凝胶作为吸附-还原剂的使用。
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| CN112876712A (zh) * | 2021-01-21 | 2021-06-01 | 北京理工大学 | 一种MXene基柔性聚乙烯醇电磁屏蔽复合薄膜及制备方法 |
| CN112973645A (zh) * | 2021-03-26 | 2021-06-18 | 同济大学 | 旋转磁场增强海藻酸钠/MXene/CoFeO凝胶及制备方法和高效富集污染物应用 |
| CN113877614A (zh) * | 2021-10-27 | 2022-01-04 | 北京石墨烯技术研究院有限公司 | 改性石墨烯卷及其制备方法与应用 |
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| CN112876712A (zh) * | 2021-01-21 | 2021-06-01 | 北京理工大学 | 一种MXene基柔性聚乙烯醇电磁屏蔽复合薄膜及制备方法 |
| CN112973645A (zh) * | 2021-03-26 | 2021-06-18 | 同济大学 | 旋转磁场增强海藻酸钠/MXene/CoFeO凝胶及制备方法和高效富集污染物应用 |
| CN113877614A (zh) * | 2021-10-27 | 2022-01-04 | 北京石墨烯技术研究院有限公司 | 改性石墨烯卷及其制备方法与应用 |
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