CN114870836A - 一种异黑素-纳米银复合催化剂及其制备方法 - Google Patents
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Abstract
本发明涉及一种异黑素‑纳米银复合催化剂及其制备方法,制备方法包括如下步骤:1)AMNPs制备:将1,8‑二羟基萘用乙腈和水溶解,然后添加NaIO4的水溶液,搅拌充分反应后,经多次离心水洗后,干燥,即得;2)AMNPs/Ag制备:将步骤1)中的AMNPs超声分散至去离子水中得分散液,然后取分散液并加入至银氨溶液中得混合液,冰水浴中搅拌充分反应后离心分离得固体,水洗后烘干,即得。优点为,以人工合成的异黑素纳米颗粒为载体,在其表面直接将银氨溶液中的银氨离子还原生成AgNPs并稳定分散和负载,工艺简单,可重复性好,原料来源广泛,成本低,利于推广;经证实得到的催化剂的催化性能较好且稳定,可以持久使用。
Description
技术领域
本发明涉及材料科学与催化领域,具体涉及一种异黑素-纳米银复合催化剂及其制备方法。
背景技术
银纳米颗粒(AgNPs)已经被证实是一种治疗感染、烧伤以及慢性伤处的抗菌剂,同时也是一种性能优异的催化材料,在污水处理方面有着非常重要的应用。但AgNPs未在载体上负载或负载效果不好时,易团聚和分散不均匀,导致抗菌活性能和催化性能不可避免地被削弱甚至丧失。为了更好的保证AgNPs抗菌、催化的效率,需要构建AgNPs的载体,载体通过空间限域作用、静电吸附作用或表面功能基团的螯合作用等在表面进行AgNPs负载,以提升AgNPs分散性,从而保证其较高且稳定的抗菌效率和催化效率。
申请人曾尝试以天然黑色素为载体进行AgNPs负载,获得的复合材料具备较好的效果,但天然黑色素存在提取麻烦、存量有限、生产成本高等缺陷。异黑素是黑色素的一种,它主要存在于植物中且易于进行人工合成。因此,探索以人工合成异黑素为载体复合AgNPs的研究具有重要意义。
发明内容
本发明所要解决的技术问题是提供一种异黑素-纳米银复合催化剂及其制备方法,旨在克服现有技术中以AgNPs为有效成分的复合催化剂因AgNPs易团聚而性能不稳定或者相应载体制备复杂、成本高等不足。
本发明解决上述技术问题的技术方案如下:一种异黑素-纳米银复合催化剂的制备方法,其包括如下步骤:
1)AMNPs制备:将1,8-二羟基萘用乙腈和水溶解,然后添加NaIO4的水溶液得反应液,搅拌充分反应后,经多次离心水洗后,干燥,即得异黑素纳米粒子AMNPs粉末,备用;
2)AMNPs/Ag制备:将步骤1)中的AMNPs粉末超声分散至去离子水中得AMNPs分散液,然后取AMNPs分散液并加入至银氨溶液中得混合液,混合液中AMNPs与银氨离子的质量比为0.1:0.15-1.5,冰水浴中搅拌充分反应后离心分离得固体,水洗后烘干,即得异黑素-纳米银复合催化剂AMNPs/Ag。
在上述技术方案的基础上,本发明还可以做如下进一步的具体选择或更优选择。
具体的,步骤1)中1,8-二羟基萘与乙腈和水的用量比为1.6g:80-100mL:1500-1600mL。
优选的,步骤1)中NaIO4的水溶液的浓度为0.5-0.8mol/L,反应液中1,8-二羟基萘与NaIO4的物质的量之比为2:1。
具体的,步骤2)中AMNPs粉末与去离子水的用量比为0.1g:4-6mL。
优选的,步骤2)中银氨溶液中银氨离子浓度为0.05-0.5wt%。
具体的,步骤2)冰水浴中搅拌的反应的时间为1h,搅拌转速为600-900rpm,离心分离时转速为12000rpm以上,单次离心处理时间20min。
具体的,步骤2)中离心得到的固体物水洗后的烘干处理是置于真空干燥箱内25-35℃下进行烘干。
本发明还提供一种异黑素-纳米银复合催化剂,其通过上述的方法制备得到。
与现有技术相比,本发明的有益效果是:
以人工合成的异黑素纳米颗粒为载体,在其表面直接将银氨溶液中的银氨离子还原生成AgNPs并稳定分散和负载,制备工艺简单,可重复性好,原料来源广泛,成本低,利于推广;得到的复合催化剂经实验证实催化性能较好,同时性能稳定,可以持久使用。
附图说明
图1为本发明实施例1制备的AMNPs和AMNPs/Ag不同标尺下的透射电镜图:a-c为不同标尺下AMNPs的透射电镜图;d-f为不同标尺下AMNPs/Ag复合催化剂的的透射电镜图;
图2为以各实施例制备的复合催化剂及实施例1制备的AMNPs为测试对象测得的红外光谱图;
图3为以实施例制备的复合催化剂催化还原4-硝基苯酚的紫外可见-吸收光谱图。
具体实施方式
以下结合附图及具体实施例对本发明作进一步的详细描述,所举实例只用于解释本发明,并非用于限定本发明的范围。
为免赘述,以下实施例中用到的方法若无特别说明则均为本领域的常规方法,用到的药品若无特别说明则均为市售产品。
实施例1
一种异黑素-纳米银复合催化剂,其通过如下方法制备得到,具体包括如下步骤:
1)AMNPs制备:首先准确称取1.6g的1,8-DHN溶于1520mL的蒸馏水和80mL的乙腈溶液中,再量取9.992mL的浓度为0.5mol/L的NaIO4并加入其中。充分反应搅拌12h后,用离心(9000rpm,15min)机提取异黑素纳米颗粒(AMNPs),将上层清液倒入废料桶,再使用蒸馏水洗涤5次。洗涤完毕后,将剩余液体倒入培养皿中,放入烘箱内烘干多余水分。烘干后,将粉末用研钵研磨成粉末状后就可以得到尺寸均一、形貌规整的AMNPs粉末,备用;
2)AMNPs/Ag制备:称取0.1g异黑素纳米颗粒粉末,将其研磨后与4mL去离子水混合,并放入超声设备中超声分散两次,每次10min。超声完毕后,然后将全部的AMNPs分散液加入至300g银氨溶液中得混合液,银氨溶液中银氨离子的质量浓度为0.05%,混合液中AMNPs与银氨离子的质量比为0.1:0.15,在冰水浴中搅拌反应一个小时后用离心(12000rpm,20min)机离心两次,将上层清液倒去后,再水洗三遍。放入真空干燥箱里用室温烘干,即得复合材料,并命名为AMNPs/Ag-0.05Ag。
实施例2
与实施例1相同,仅步骤2)中银氨溶液中银氨离子的质量浓度为0.1%,混合液中AMNPs与银氨离子的质量比为0.1:0.3,得到的复合材料命名为AMNPs/Ag-0.1Ag。
实施例3
与实施例1相同,仅步骤2)中银氨溶液中银氨离子的质量浓度为0.3%,混合液中AMNPs与银氨离子的质量比为0.1:0.9,得到的复合材料命名为AMNPs/Ag-0.3Ag。
实施例4
与实施例1相同,仅步骤2)中银氨溶液中银氨离子的质量浓度为0.5%,混合液中AMNPs与银氨离子的质量比为0.1:1.5,得到的复合材料命名为AMNPs/Ag-0.5Ag。
材料表征及性能测试
以实施例1制备的AMNPs和AMNPs/Ag-0.05Ag为样品,进行透射电镜表征,得到的不同标尺下对应样品的透射电镜图:图1(a-c)不同标尺下AMNPs的透射电镜图;图1(d-f)不同标尺下AMNPs/Ag-0.05Ag复合催化剂的的透射电镜图。从图1a-c可以发现本发明所制备的AMNPs有着粒径均一且规整的大小,随机100个样品的统计学平均尺寸为85.6±5.7nm。此外其表面相对粗糙(有着大量富氧官能团),可以为后续AgNPs的负载提供附着位点并与其紧密连接增强AMNPs/Ag催化剂的稳定性。本发明利用AMNPs表面的邻苯二羟基结构自发的向苯醌结构转变时所释放出的电子,在低温条件下调节反应速率,成功在制备出来AMNPs/Ag,图1d-f表明,有相对较均匀的AgNPs在AMNPs表面负载,随机100个样品中的AgNPs统计学平均尺寸为6.2±0.9nm。
以各实施例制备的复合催化剂及实施例1制备的AMNPs为测试对象,测得了相应的红外光谱,如图2所示。从图2可以分析得出,异黑素的波峰主要是在1600~1800cm-1、1100~1500cm-1以及700~1000cm-1这些区域。1710cm-1附近出现的特征峰出现的原因主要是由O-H伸缩振动产生的,1483cm-1的特征峰对应的官能团则是芳环上的C-H伸缩振动,1326cm-1的特征峰的出现代表着C-O的伸缩振动和OH弯曲振动的相互作用,而953cm-1和868cm-1这个特征峰则是表示芳香烃的C-H键面外弯曲振动而造成的。从AMNPs/Ag复合催化剂的红外光谱图则可以看出,对比纯异黑素的红外光谱图的特征峰的强度有着明显的减弱。出现这个数据的原因可能是银纳米粒子的存在对红外辐射光产生了一定的干扰,降低了官能团的吸收。异黑素纳米粒子含有大量的带负电的含氧官能团,所以对于带正电的银氨离子能进行一个有效地吸引,然后将其牢牢地结合住,图2红外光谱的变化情况,反映出银纳米粒子成功地负载在了异黑素的表面。
为了测试本发明制备的复合催化剂的催化性能,本发明设计了以各实施例制备的MNPs/Ag复合催化剂催化还原4-硝基苯酚的情况。在测试前,首先需要制备20mL的浓度为0.06mol/L的硼氢化钠溶液和0.2mol/L的4-硝基苯酚溶液30mL。将AMNPs/A复合催化剂粉末取2mg加入到4mL的去离子水中进行超声分散得到AMNPs/Ag复合催化剂溶液。在石英比色皿中加入2mL的4-硝基苯酚溶液和1mL硼氢化钠溶液以及200μLAMNPs/Ag复合催化剂溶液,然后后放入紫外分光光度计中进行检测,每分钟检测一次,由400纳米处吸光度的变化来表示反应的进行。结果如图3所示,在图3中a-d依次为实施例1至4制备得到的复合材料催化剂AMNPs/Ag-0.05Ag,AMNPs/Ag-0.1Ag,AMNPs/Ag-0.3Ag和AMNPs/Ag-0.5Ag催化还原4-硝基苯酚的紫外可见-吸收光谱,从紫外吸收波普图可看出,较短的时间内AMNPs/Ag可以有效的催化硼氢化钠还原4-硝基苯酚变为4-氨基苯酚。相同催化条件下使用AMNPs/Ag-0.5Ag催化剂的反应体系的完成用时最短,催化活性最高。
以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (8)
1.一种异黑素-纳米银复合催化剂的制备方法,其特征在于,包括如下步骤:
1)AMNPs制备:将1,8-二羟基萘用乙腈和水溶解,然后添加NaIO4的水溶液得反应液,搅拌充分反应后,经多次离心水洗后,干燥,即得异黑素纳米粒子AMNPs粉末,备用;
2)AMNPs/Ag制备:将步骤1)中的AMNPs粉末超声分散至去离子水中得AMNPs分散液,然后取AMNPs分散液并加入至银氨溶液中得混合液,混合液中AMNPs与银氨离子的质量比为0.1:0.15-1.5,冰水浴中搅拌充分反应后离心分离得固体,水洗后烘干,即得异黑素-纳米银复合催化剂AMNPs/Ag。
2.根据权利要求1所述的一种异黑素-纳米银复合催化剂的制备方法,其特征在于,步骤1)中1,8-二羟基萘与乙腈和水的用量比为1.6g:80-100mL:1500-1600mL。
3.根据权利要求1所述的一种异黑素-纳米银复合催化剂的制备方法,其特征在于,步骤1)中NaIO4的水溶液的浓度为0.5-0.8mol/L,反应液中1,8-二羟基萘与NaIO4的物质的量之比为2:1。
4.根据权利要求1所述的一种异黑素-纳米银复合催化剂的制备方法,其特征在于,步骤2)中AMNPs粉末与去离子水的用量比为0.1g:4-6mL。
5.根据权利要求1所述的一种异黑素-纳米银复合催化剂的制备方法,其特征在于,步骤2)中银氨溶液中银氨离子浓度为0.05-0.5wt%。
6.根据权利要求1所述的一种异黑素-纳米银复合催化剂的制备方法,其特征在于,步骤2)冰水浴中搅拌的反应的时间为1h,搅拌转速为600-900rpm,离心分离时转速为12000rpm以上,单次离心处理时间20min。
7.根据权利要求1至6任一项所述的一种异黑素-纳米银复合催化剂的制备方法,其特征在于,步骤2)中离心得到的固体物水洗后的烘干处理是置于真空干燥箱内25-35℃下进行烘干。
8.一种异黑素-纳米银复合催化剂,其特征在于,通过权利要求1至7任一项所述的方法制备得到。
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