CN114392756B - 一种压电催化材料的制备方法、产品及其应用 - Google Patents
一种压电催化材料的制备方法、产品及其应用 Download PDFInfo
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- IAZSXUOKBPGUMV-UHFFFAOYSA-N 1-butyl-3-methyl-1,2-dihydroimidazol-1-ium;chloride Chemical compound [Cl-].CCCC[NH+]1CN(C)C=C1 IAZSXUOKBPGUMV-UHFFFAOYSA-N 0.000 claims abstract description 3
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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Abstract
本发明公开了一种压电催化材料的制备方法、产品及其应用,属于金属回收技术领域,所述方法包括以下步骤:将钼源和硫源溶于氯化(1‑丁基‑3‑甲基咪唑)中,加入盐酸,将所得混合溶液加热即得所述压电催化材料;本发明制备得到的压电催化材料MoS2,具有良好的吸附性和优异的压电催化效果,在超声作用下可将重金属单质转化成离子,之后加热蒸发得到单质,使溶出—吸附—脱附—回收这一复杂过程在同一催化材料中得以实现;本发明采用简单的水热合成法制备压电催化材料,且采用其回收重金属时不引入其它药物、强酸及有毒氟化物等,对环境友好无污染。
Description
技术领域
本发明属于金属回收技术领域,具体涉及一种压电催化材料的制备方法、产品及其应用。
背景技术
随着社会的逐步发展和人们生活水平的快速提高,大量的工业、农业和生活废弃物日益增多,电子废弃物的废弃现象亦日趋严重。电子废弃物不仅占据大量物理空间,而且在处理过程中产生的废烟、废气会严重影响人类身体健康。因此,电子废弃物的处理处置逐渐为人们所关注。目前,电子废弃物的处理方法一般有如下4种:化学处理、火法处理、机械处理和微生物处理。其中,化学处理的过程中要使用强酸和剧毒的氟化物等,易产生大量的废液并排放有毒气体,对环境产生的危害较大;火法处理由于使用了焚烧、熔炼、烧结和熔融等手段,也会造成环境污染并抑制可持续发展的过程;机械处理法中电子废弃物的拆卸通常是手工操作,以回收其中有用的电子元器件,但其中电子元器件数量多,而且结合方式复杂,使得手工处理效率非常低;微生物技术提取金、银等贵金属具有工艺简单、费用低、操作简单的优点,但提取时间较长。因此,发明一种提取周期短,成本低,便于实际应用的催化材料,对于回收有用金属具有重要的实用价值。
发明内容
为克服现有技术的上述问题,本发明提供了一种压电催化材料的制备方法、产品及其应用,以简单的水热法合成MoS2压电催化材料,采用其可方便地实现对废弃芯片中的重金属的回收,且脱附简单,对重金属的回收率高。
为实现上述目的,本发明提供了如下技术方案:
本发明提供了一种压电催化材料的制备方法,包括以下步骤:将钼源和硫源溶于氯化(1-丁基-3-甲基咪唑)中,加入盐酸,将所得混合溶液加热即得所述压电催化材料。
优选的,所述钼源为钼酸钠和/或钼酸铵,所述硫源为硫脲、硫代乙酰胺或L-半胱氨酸中的一种或多种。
优选的,所述盐酸的浓度为0.15~0.25mol/L;所述盐酸采用滴加的方式加入,加入后搅拌至溶液澄清透明。
优选的,所述加热温度为80~280℃,时间为0.5~24h。
优选的,所述加热后还包括对所得固体进行洗涤,并在25~100℃下干燥的操作。
本发明还提供了一种根据上述制备方法制备得到的压电催化材料。
本发明还提供了上述压电催化材料在重金属回收中的应用。
优选的,所述重金属为铜。
优选的,对重金属铜的回收包括以下步骤:将所述压电催化材料置于水中,之后加入含金属铜的芯片并超声,然后静置并过滤,对所得滤液进行加热干燥得到金属铜。
优选的,所述超声功率为0~500W,所述加热温度为70~90℃。
与现有技术相比,本发明具有以下有益效果:
本发明制备得到的压电催化材料MoS2,呈花瓣状,具有良好的吸附性和优异的压电催化效果,在超声作用下可将重金属单质转化成离子,之后加热蒸发形成单质,使溶出—吸附—脱附—回收这一复杂过程在同一催化材料中得以实现。
本发明采用简单的水热合成法制备压电催化材料,制备方法简单,成本低;且采用其回收重金属时不引入其它药物、强酸及有毒氟化物等,克服了传统金属回收过程中需投加药剂的问题,对环境友好无污染。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1为商品MoS2和实施例1制备的MoS2-1的X射线衍射图;
图2为商品MoS2和实施例1制备的MoS2-1的不同放大倍数下的场发射扫描电镜图,图2中(a)为商品MoS2的低倍场发射扫描电镜图,(b)为商品MoS2的高倍场发射扫描电镜图,(c)为实施例1制备的MoS2-1的低倍场发射扫描电镜图,(d)为实施例1制备的MoS2-1的高倍场发射扫描电镜图;
图3为商品MoS2和实施例1制备的MoS2-1的场发射透射电镜图,图3中(a)为商品MoS2的低倍场发射透射电镜图,(b)为商品MoS2的高倍场发射透射电镜图,(c)为实施例1制备的MoS2-1的低倍场发射透射电镜图,(d)为实施例1制备的MoS2-1的高倍场发射透射电镜图;
图4为商品MoS2及实施例1~7中制得的MoS2-1、MoS2-2、MoS2-3、MoS2-4、MoS2-5、MoS2-6及MoS2-7对铜单质的回收效果图。
具体实施方式
现详细说明本发明的多种示例性实施方式,该详细说明不应认为是对本发明的限制,而应理解为是对本发明的某些方面、特性和实施方案的更详细的描述。应理解本发明中所述的术语仅仅是为描述特别的实施方式,并非用于限制本发明。
另外,对于本发明中的数值范围,应理解为还具体公开了该范围的上限和下限之间的每个中间值。在任何陈述值或陈述范围内的中间值以及任何其他陈述值或在所述范围内的中间值之间的每个较小的范围也包括在本发明内。这些较小范围的上限和下限可独立地包括或排除在范围内。
除非另有说明,否则本文使用的所有技术和科学术语具有本发明所述领域的常规技术人员通常理解的相同含义。虽然本发明仅描述了优选的方法和材料,但是在本发明的实施或测试中也可以使用与本文所述相似或等同的任何方法和材料。本说明书中提到的所有文献通过引用并入,用以公开和描述与所述文献相关的方法和/或材料。在与任何并入的文献冲突时,以本说明书的内容为准。
在不背离本发明的范围或精神的情况下,可对本发明说明书的具体实施方式做多种改进和变化,这对本领域技术人员而言是显而易见的。由本发明的说明书得到的其他实施方式对技术人员而言是显而易见的。本发明说明书和实施例仅是示例性的。
关于本文中所使用的“包含”、“包括”、“具有”、“含有”等等,均为开放性的用语,即意指包含但不限于。
实施例1
将0.72g Na2MoO4·2H2O和0.69g CH4N2S粉末溶解于1mL 1M C8H15ClN2中,记为溶液A,取1mL浓度为12mol/L的盐酸于60mL去离子水中,稀释液缓慢滴入溶液A中,搅拌12h,溶液变成澄清透明状,将其转移至100mL聚四氟乙烯内衬的高压釜中,于220℃保持24h,待高压釜自然冷却至室温后,将合成的产物在蒸馏水中洗涤4次,得到黑色的MoS2纳米花,而后在60℃下烘干,即得MoS2压电催化材料,记为MoS2-1。
对本实施例制备得到的MoS2-1和购买的商品MoS2进行X射线衍射分析,得到的XRD图如图1所示,由图1可以看出,本发明所制备MoS2-1和商品MoS2的主要特征峰相同,说明本实施例合成了MoS2压电催化材料。
采用场发射扫描电子显微镜在不同放大倍数下对商品MoS2和本实施例制备得到的MoS2-1的形貌进行观察,结果如图2所示,其中,图2a和2b为商品MoS2的场发射扫描电镜照片,图2c和2d为本实施例制备得到的MoS2-1的场发射扫描电镜照片,由图可以看出,商品MoS2的形貌呈片状,有极少的暴露边缘;本实施例制备得到的MoS2-1呈花瓣状,结构相对紧密。
采用场发射透射电子显微镜在不同放大倍数下对商品MoS2和本实施例制备得到的MoS2-1进行观察,结果如图3所示,其中,图3a和3b为商品MoS2的场发射透射电子显微镜照片,图3c和3d为本实施例制备得到的MoS2-1的场发射透射电子显微镜照片。
实施例2
将0.72g Na2MoO4·2H2O和0.69g CH4N2S粉末溶解于1mL 1M C8H15ClN2中,记为溶液A,2mL HCl稀释于60mL去离子水中,稀释液缓慢滴入溶液A中,搅拌12h,溶液变成澄清透明状,将其转移至100mL聚四氟乙烯内衬的高压釜中,于220℃保持24h,待高压釜自然冷却至室温后,将合成的产物在蒸馏水中洗涤3次,得到黑色的MoS2纳米花,而后在60℃下烘干,即得MoS2压电催化材料,记为MoS2-2。
实施例3
将0.72g Na2MoO4·2H2O和0.69g CH4N2S粉末溶解于1mL 1M C8H15ClN2中,记为溶液A,1mL HCl稀释于80mL去离子水中,稀释液缓慢滴入溶液A中,搅拌12h,溶液变成澄清透明状,将其转移至100mL聚四氟乙烯内衬的高压釜中,于220℃保持24h,待高压釜自然冷却至室温后,将合成的产物在蒸馏水中洗涤5次,得到黑色的MoS2纳米花,而后在60℃下烘干,即得MoS2压电催化材料,记为MoS2-3。
实施例4
将0.72g Na2MoO4·2H2O和0.69g CH4N2S粉末溶解于1mL 1M C8H15ClN2中,记为溶液A,1mL HCl稀释于60mL去离子水中,稀释液缓慢滴入溶液A中,搅拌12h,溶液变成澄清透明状,将其转移至100mL聚四氟乙烯内衬的高压釜中,于220℃保持24h,待高压釜自然冷却至室温后,将合成的产物在蒸馏水中洗涤4次,得到黑色的MoS2纳米花,而后在80℃下烘干,即得MoS2压电催化材料,记为MoS2-4。
实施例5
将0.72g Na2MoO4·2H2O和0.69g CH4N2S粉末溶解于1mL 1M C8H15ClN2中,记为溶液A,1mL HCl稀释于60mL去离子水中,稀释液缓慢滴入溶液A中,搅拌12h,溶液变成澄清透明状,将其转移至100mL聚四氟乙烯内衬的高压釜中,于200℃保持24h,待高压釜自然冷却至室温后,将合成的产物在蒸馏水中洗涤4次,得到黑色的MoS2纳米花,而后在60℃下烘干,即得MoS2压电催化材料,记为MoS2-5。
实施例6
将0.72g钼酸铵和0.76g硫代乙酰胺溶解于1mL 1M C8H15ClN2中,记为溶液A,1mLHCl稀释于60mL去离子水中,稀释液缓慢滴入溶液A中,搅拌12h,溶液变成澄清透明状,将其转移至100mL聚四氟乙烯内衬的高压釜中,于80℃保持24h,待高压釜自然冷却至室温后,将合成的产物在蒸馏水中洗涤5次,得到黑色的MoS2纳米花,而后在40℃下烘干,即得MoS2压电催化材料,记为MoS2-6。
实施例7
将0.72g Na2MoO4·2H2O和0.97g L-半胱氨酸溶解于1mL 1M C8H15ClN2中,记为溶液A,1mL HCl稀释于60mL去离子水中,稀释液缓慢滴入溶液A中,搅拌12h,溶液变成澄清透明状,将其转移至100mL聚四氟乙烯内衬的高压釜中,于280℃保持0.5h,待高压釜自然冷却至室温后,将合成的产物在蒸馏水中洗涤3次,得到黑色的MoS2纳米花,而后在100℃下烘干,即得MoS2压电催化材料,记为MoS2-7。
效果验证
在室温下测定商品MoS2与实施例1~7所制备的样品对废旧芯片中金属铜的回收效果:对商品MoS2与实施例1~7所制备的样品各称取0.05g于250mL烧杯中,加入100mL去离子水,向每个烧杯中加入相同的质量为9.5g的芯片,使溶液没过芯片,以保证MoS2与芯片充分接触,将烧杯置于300W的超声清洗仪中,超声10h,将超声后的溶液静置约12h,使之彻底沉淀。然后取上层清液置于另一烧杯中,用0.22μm滤头过滤后于烘箱中80℃烘干即得金属铜。
各样品对金属铜的回收量如图4所示,由图4可知,MoS2-1显示出最好的压电催化性能,回收铜的量达53.33mg,表明本发明中制备的MoS2压电催化材料对于金属铜的回收具有明显的效果。
根据上述方法制备出的MoS2压电催化材料还可应用到铂、金或银的溶出—吸附—脱附—回收过程,其回收效果也较好。
以上所述,仅为本发明较佳的具体实施方式,本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明披露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围内。
Claims (5)
1.一种压电催化材料在重金属回收中的应用,其特征在于,所述重金属为铜;将所述压电催化材料置于水中,之后加入含金属铜的芯片并超声,然后静置并过滤,对所得滤液进行加热干燥得到金属铜;
所述压电催化材料的制备方法,包括以下步骤:将钼源和硫源溶于氯化(1-丁基-3-甲基咪唑)中,加入盐酸,将所得混合溶液加热即得所述压电催化材料。
2.根据权利要求1所述的应用,其特征在于,所述钼源为钼酸钠和/或钼酸铵,所述硫源为硫脲、硫代乙酰胺或L-半胱氨酸中的一种或多种。
3.根据权利要求1所述的应用,其特征在于,所述盐酸的浓度为0.15~0.25mol/L;所述盐酸采用滴加的方式加入,加入后搅拌至溶液澄清透明。
4.根据权利要求1所述的应用,其特征在于,所述加热温度为80~280℃,时间为0.5~24h。
5.根据权利要求1所述的应用,其特征在于,所述加热后还包括对所得固体进行洗涤、干燥的操作。
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