CN112588301B - 一种复合金属纳米材料及其制备和应用 - Google Patents
一种复合金属纳米材料及其制备和应用 Download PDFInfo
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Abstract
本发明涉及吸附技术,具体说是一种复合金属的材料及其制备和应用。通过两步合成光催化性能、酶催化性能和杀菌性能优异的复合金属纳米材料。制备方法简单,所发明制备的材料成本低、性能显著,在纳米材料催化氧化领域中具有广阔的应用前景。
Description
技术领域
本发明涉及吸附技术,具体说是一种复合金属的材料及其制备和应用。
背景技术
由细菌引起的疾病被认为是全世界致命的疾病之一,目前已影响了数以百万计的人的生命健康。为了应对细菌感染的威胁,全世界开发了各种抗菌材料,包括抗生素、金属离子和季铵盐化合物。然而,这些物质会造成细菌耐药性、环境污染、花费增多等问题。
高浓度的活性氧(·O2 -、·OH、H2O2)会导致细胞膜破裂、细胞质外流,进而引起细胞的死亡。因此,开发可以有效得到产生高浓度活性氧的纳米材料具有重要意义。近年来,光催化剂和酶催化剂被证实具有制备简单、稳定性高、可以产生活性氧等优点。因此制备多远、催化活性高、性能稳定的光、酶催化剂是解决细菌疾病的重要途径之一。
发明内容
本发明的目的在于提供一种具有光催化和酶催化活性的复合金属纳米材料及其制备和应用。
为实现上述目的,本发明采用的技术方案为:
一种复合金属纳米材料的制备方法,以钴盐、钼盐作为原料首先通过水热法、再引入硫源通过管式炉焙烧,合成具有光催化性能、酶催化性能和杀菌性能的CoS2/MoS2复合金属纳米材料。
具体为:
1)将钴盐、钼盐、4,4-联吡啶混合而后分散至水中,于100-140℃下反应4-8h,反应后洗涤,待用;
2)将步骤1)所得产物与硫粉在管式炉中,以400-600℃下焙烧反应1-3h,即得CoS2/MoS2复合金属纳米材料。
其中,步骤1)所得粉末置于管式炉下游,S粉置于管式炉上游。
所述钴盐为六水合氯化钴或六水合硝酸钴;所述钼盐为钼酸钠;
所述钴盐中Co、钼盐中的钼盐和4,4-联吡啶摩尔比为3:1:1-1:3:1;4,4-联吡啶与硫粉中的S摩尔比为1:10。
所述钴盐、钼盐、4,4-联吡啶混合分散至水中,磁力搅拌20-40min得到分散均匀的混合物,而后进行水热反应,反应结束后自然冷却至室温,依次用超纯水离心反复清洗,60-80℃干燥得到MOF前体材料。
一种所述制备的复合金属纳米材料,按所述方法制备获得CoS2/MoS2复合金属纳米材料。
一种复合金属纳米材料的应用,所述CoS2/MoS2复合金属纳米材料在作为光催化剂中的应用。
所述光催化剂的底物是亚甲基蓝、甲基橙或罗丹明B。
一种复合金属纳米材料的应用,所述CoS2/MoS2复合金属纳米材料在作为酶催化剂中的应用。
所述酶催化的底物是O2、H2O2或TMB。
一种复合金属纳米材料的应用,所述CoS2/MoS2复合金属纳米材料在作为杀菌剂的应用。
本发明与现有技术相比,具有以下优点及突出性效果:
本发明通过对MOF前体进行S化,制备复合金属纳米材料,得到具有强光催化性能、酶催化性能和杀菌性能的CoS2/MoS2材料。通过XRD分析,该材料具有纯净的物相组成。
本发明制备方法成本低、方法简单、重复性好;所得复合材料具有良好的针对亚甲基蓝、甲基橙和罗丹明B的光降解作用,同时复合材料具有针对H2O2和TMB的酶催化作用,与此同时复合材料对大肠杆菌具有明显的杀灭作用。进而本发明材料可作为一种新颖模拟酶在免疫分析、生物检测和临床诊断等领域具有潜在的应用价值,在新型催化氧化分析中具有广阔的应用前景。
附图说明:
图1为本发明实施例提供的定性分析为CoS2/MoS2的X射线衍射图;
图2为本发明实施例提供的CoS2/MoS2材料的TEM图;
图3为本发明实施例提供的CoS2/MoS2材料光催化性能图,其中,A为暗处理30min、B光处理30min、C为光处理90min、D为光处理120min;
图4为本发明实施例提供的CoS2/MoS2材料酶催化性能图;
图5为本发明实施例提供的CoS2/MoS2材料的杀菌性能图。
具体实施方式
以下通过具体的实施例对本发明作进一步说明,有助于本领域的普通技术人员更全面的理解本发明,但不以任何方式限制本发明。
实施例1:
向烧杯中分别加入10mmol硝酸钴,5mmol 4,4-联吡啶和10mmol钼酸钠,加入70mL去离子水,搅拌均匀,磁力搅拌20min得到分散均匀的混合物,转移至于100mL水热反应釜120℃下结晶4h。晶化结束后自然冷却至室温,取出产物,首先经去离子水离心洗涤3次,离心条件为4000r/min,离心10min,洗涤后60℃干燥,得到MOF前体材料待用。
取0.4g上述产物放置于管式炉下游,4g硫粉放置于管式炉上游,于500℃反应1h,得CoS2/MoS2复合金属纳米材料(参见图1和图2)。
XRD测试结果如图1所示,从中可看出合成的材料和成分与CoS2、MoS2的标准卡片(JCPDS No.37-1492,JCPDS No.41-1471)相吻合;并且由图2中可见,CoS2/MoS2产物为片径约为100-150nm的片状结构。
当按照实施例1中的元素比例进行反应时,才可以得到片径约为100-150nm的CoS2/MoS2复合产物。
实施例2-6:
CoS2/MoS2复合材料制备过程:
向5个烧杯中按表1的不同比例进行六水合硝酸钴和钼酸钠的添加,再加入4,4-联吡啶,加入30-70mL去离子水,搅拌均匀,磁力搅拌30min得到分散均匀的混合物,转移至于100mL水热反应釜于100-120℃下结晶6-12h。晶化结束后自然冷却至室温,取出产物,首先经去离子水离心洗涤3次,离心条件为4000r/min,离心10min,洗涤后60℃干燥,得到MOF前体材料待用(参见表1);
取0.4g上述产物放置于管式炉下游,4g硫粉放置于管式炉上游,于500℃反应1h,得CoS2/MoS2复合金属纳米材料。
表1
按照表1中记载,实施例2-6所得的不同比例制备所得复合物具有与实例1相同的物相组成和结构形貌。
应用例1
分别在20mg/L的亚甲基蓝、甲基橙或罗丹明B溶液中,加入1mg/mL CoS2/MoS2纳米片作为实验组,同时以不加纳米片作为对照,观察实验组和对照组在光照和黑暗情况处理条件下,不同染料的褪色情况(参见图3)。
由上述各体系可见,对照组中在光处理和暗处理的120min内,亚甲基蓝、甲基橙和罗丹明B的空白组的颜色基本没变。黑暗状态下的实验组颜色变色可忽略不计,光照状态下的实验组,随着光照时间的增长,颜色逐渐变浅。因此,该材料具有优异的光催化降解染料的活性。
应用例2
过氧化物酶性能的检测:
按照体系1-4的不同配比,进行过模拟酶性能的检测,(参见图4)。
体系1:10mM H2O2+0.4mg/mL CoS2/MoS2纳米材料
体系2:10mM H2O2+0.05mg/mL CoS2/MoS2纳米材料
体系3:0.4mM TMB+0.05mg/mL CoS2/MoS2纳米材料
体系4:10mM H2O2+0.4mM TMB+0.05mg/mL CoS2/MoS2纳米材料
由图4可以看出,管1、2无色透明,管3呈浅蓝色,管4呈较深的蓝色,因此材料不仅具有氧化物酶活性,还具有优异的过氧化物酶性能。
应用例3
杀菌检测:
取4个离心管,分别标记为1,2,3,4。1号为空白组,加入100μL菌液和40mL超纯水;2号为实验组,加入100μL菌液,0.1μg/mL CoS2/MoS2纳米材料和40mL超纯水;3号为实验组,加入100μL菌液,1μg/mL CoS2/MoS2纳米材料和40mL超纯水;4号为实验组,加入100μL菌液,10μg/mL CoS2/MoS2纳米材料和40mL超纯水。在0、30、60min时,分别取1mL菌液进行逐级稀释,稀释后涂板,实验结果参见图5。
从图5可以看出,在黑暗条件下,当加入10μg/mL CoS2/MoS2纳米材料,孵育60min时,可以实现针对大肠杆菌的100%杀灭。由此采用本发明材在一定条件下具有突出的杀菌活性,并且极大地减少了材料用量,而且减少了反应时间。
综上所示,本文制备的CoS2/MoS2纳米片不仅具有优异的光催化活性、酶催化活性还具有优异的杀菌活性。
Claims (3)
1.一种复合金属纳米材料的应用,其特征在于:CoS2/MoS2复合金属纳米材料在作为光催化剂中的应用;
所述光催化剂的底物是亚甲基蓝、甲基橙或罗丹明B;
所述CoS2/MoS2复合金属纳米材料的制备方法,以钴盐、钼盐作为原料首先通过水热法、再引入硫源通过管式炉焙烧,合成具有光催化性能、酶催化性能和杀菌性能的CoS2/MoS2复合金属纳米材料;
具体为:
1)将钴盐、钼盐、4,4-联吡啶混合而后分散至水中,于100-140 oC下反应4-8 h,反应后洗涤,待用;
2)将步骤1)所得产物与硫粉在管式炉中,以400-600 oC下焙烧反应1-3 h,即得CoS2/MoS2复合金属纳米材料;
所述钴盐中Co、钼盐中的钼盐和4,4-联吡啶摩尔比为3:1:1-1:3:1; 4,4-联吡啶与硫粉中的S摩尔比为1:10;
所述钴盐、钼盐、4,4-联吡啶混合分散至水中,磁力搅拌20-40min得到分散均匀的混合物,而后进行水热反应,反应结束后自然冷却至室温,依次用超纯水离心反复清洗,60-80℃干燥得到MOF前体材料。
2.一种复合金属纳米材料的应用,其特征在于:CoS2/MoS2复合金属纳米材料在作为酶催化剂中的应用;
所述酶催化的底物是O2、H2O2或TMB;所述CoS2/MoS2复合金属纳米材料的制备方法,以钴盐、钼盐作为原料首先通过水热法、再引入硫源通过管式炉焙烧,合成具有光催化性能、酶催化性能和杀菌性能的CoS2/MoS2复合金属纳米材料;
具体为:
1)将钴盐、钼盐、4,4-联吡啶混合而后分散至水中,于100-140 oC下反应4-8 h,反应后洗涤,待用;
2)将步骤1)所得产物与硫粉在管式炉中,以400-600 oC下焙烧反应1-3 h,即得CoS2/MoS2复合金属纳米材料;
所述钴盐中Co、钼盐中的钼盐和4,4-联吡啶摩尔比为3:1:1-1:3:1; 4,4-联吡啶与硫粉中的S摩尔比为1:10;
所述钴盐、钼盐、4,4-联吡啶混合分散至水中,磁力搅拌20-40min得到分散均匀的混合物,而后进行水热反应,反应结束后自然冷却至室温,依次用超纯水离心反复清洗,60-80℃干燥得到MOF前体材料。
3.一种复合金属纳米材料的应用,其特征在于:CoS2/MoS2复合金属纳米材料在作为杀菌剂的应用;所述CoS2/MoS2复合金属纳米材料的制备方法,以钴盐、钼盐作为原料首先通过水热法、再引入硫源通过管式炉焙烧,合成具有光催化性能、酶催化性能和杀菌性能的CoS2/MoS2复合金属纳米材料;
具体为:
1)将钴盐、钼盐、4,4-联吡啶混合而后分散至水中,于100-140 oC下反应4-8 h,反应后洗涤,待用;
2)将步骤1)所得产物与硫粉在管式炉中,以400-600 oC下焙烧反应1-3 h,即得CoS2/MoS2复合金属纳米材料;
所述钴盐中Co、钼盐中的钼盐和4,4-联吡啶摩尔比为3:1:1-1:3:1; 4,4-联吡啶与硫粉中的S摩尔比为1:10;
所述钴盐、钼盐、4,4-联吡啶混合分散至水中,磁力搅拌20-40min得到分散均匀的混合物,而后进行水热反应,反应结束后自然冷却至室温,依次用超纯水离心反复清洗,60-80℃干燥得到MOF前体材料。
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