CN115672356A - 一种CoP/MoS2复合光催化剂的制备方法及应用 - Google Patents
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Abstract
本发明属于复合纳米材料制备和环保技术领域,公开了一种复合光催化剂CoP/MoS2的制备方法及其应用。本发明技术主要由气‑固相低温磷化法合成催化剂。其制备过程如下:首先由Co(NO3)2·6H2O和NaH2PO2为原料制得CoP纳米颗粒,其次利用自组装方法成功制备出CoP/MoS2催化剂。这种制备方法操作简单、材料易得、廉价。所制备的催化剂在处理水体中污染物方面有很好的效果,因此,该催化剂在光催化剂领域具有良好的应用前景和价值。
Description
技术领域
本发明涉及半导体催化剂领域,涉及一种复合光催化剂CoP/MoS2的制备方法及光催化降解2-巯基苯并噻唑方面的应用,属于环境保护领域。
背景技术
近年来,随着经济的快速发展和工业化进程的加快,废水的排放量日益增加,对环境和人类健康构成了极大的威胁。2-巯基苯并噻唑(MBT)作为有机污染物的一种在水生生态系统中引起了严重的环境问题,已经对人类身体健康和生态系统造成了严重的影响,制约了人类自身和社会的可持续发展。因此,开发高效光催化剂治理水污染,降解水中有机污染,成为重要的研究方向之一。
MoS2作为一种典型的二维材料,具有稳定的物理化学性质且有较大的比表面积和活性位点,能够吸附更多的待降解物质,且其禁带宽度为1.8eV,可吸收可见光,使其在光催化降解、锂离子电池、场效应管、光电等领域得到了广泛的应用。但是纯MoS2本身作光催化剂时,由于其激子结合能高,光生电子和空穴容易复合,光生电子和空穴利用效率低,因而单独使用时光催化效率并不高。CoP作为一种过渡金属磷化物,由于其良好的稳定性、高导电性、电荷分离和电子传输能力,越来越受到人们的关注。因此,通过与CoP复合构建异质结制备CoP/MoS2复合光催化剂,从而提高其光催化活性。
发明内容
[技术问题]
针对目前存在的问题,提供一种复合半导体光催化剂CoP/MoS2的制备方案,所述制备方案实施成本较低,并且原材料简单易得。
[技术方案]
为了实现上述目的,更具本发明的一个实施方式提供了一种复合光催化剂CoP/MoS2的制备方法,所述制备方案包括以下步骤:
(1)制备CoP
将200mg Co(NO3)2·6H2O和50mg柠檬酸钠混合在100ml水溶液中,然后加入3ml0.5M氢氧化钠溶液,搅拌3.5小时,静置4小时后分离沉淀物。将沉淀物离心,并在60℃的真空烘箱中干燥8小时,得到Co(OH)2前驱体。然后,在玛瑙中均匀研磨50mg Co(OH)2和250mgNaH2PO2的混合物。随后,混合前体在氮气中以1℃/min的升温速率在300℃下煅烧2小时。
(2)制备MoS2
将6g NaNO3溶解在16ml浓盐酸中,置于烧杯中。随后,加入1.2g MoS2。30℃条件下超声处理制备的溶液10小时,然后离心、洗涤,干燥得到二硫化钼纳米片。
(3)制备CoP/MoS2
0.1g MoS2与0.02g CoP溶于30ml乙二醇溶液中,然后磁力搅拌5h,随后用水、乙醇洗涤、离心,并在60℃下干燥,得到最终产物。
在所述步骤(1)中,所述的钴盐可选自硝酸钴、氯化钴或者醋酸钴中的任意一种,优先选取硝酸钴;次磷酸钠和硝酸钴的摩尔比为5~5.5mol,加入柠檬酸钠的质量为50~55g,在300℃下煅烧2h;
通过步骤(2)中,NaNO3的质量为6.0~6.5g,浓盐酸的体积为16~20mL;MoS2的质量为1.2~1.5g;
在所述步骤(2)中,MoS2和CoP的摩尔比为5~5.5mol,乙二醇的体积30~35ml,磁力搅拌时间为5~6h;
根据本发明的一个实施方式提供了上述制备方法制得的复合光催化剂CoP/MoS2,应用于去除水中2-巯基苯并噻唑污染物。
物料来源
六水合硝酸钴、次磷酸钠、柠檬酸钠、无水乙醇、二硫化钼、硝酸钠、氢氧化钠(NaOH)、乙二醇,浓盐酸均为分析纯,购于国药化学试剂有限公司。
[有益效果]
综上所述,本发明具有以下有益效果:
本发明实现了制备CoP/MoS2复合光催化剂,使MoS2与CoP形成良好的异质结,有效地增强了催化剂对可见光的吸收,提高电子和空穴的分离效果。催化剂利用氙灯进行激发,与污染物分子接触,相互作用实现特殊的催化或转化效应,使周围的氧气及水分子激发成极具氧化力的自由负离子,从而达到降解环境废水2-巯基苯并噻唑的目的。同时,由这种方法制备的CoP/MoS2结构稳定,原材料容易获取,操作过程简单易行,是一种高效低废的绿色环保技术。
附图说明:
图1为不同催化剂的透射电镜图(a)CoP、(b)MoS2、(c)CoP/MoS2复合光催化剂。
图2为不同光照时间下CoP/MoS2复合光催化剂降解MBT的紫外-可见吸收图谱。
具体实施方式
本发明中所制备的光催化剂的光催化活性评价:取50mg催化剂加入到100mL 2-巯基苯并噻唑溶液中,用220W Xe灯进行照射30分钟,光照过程中每隔20分钟取一次样,取其上清液,在分光光度计λmax=316nm处测定吸光强度,并通过公式:Dr=(C0-C)×100/C0算出其降解率Dr,其中C0为初始浓度,C为t时刻测定的2-巯基苯并噻唑溶液的浓度,t为反应时间。
为了使本领域技术人员能够更清楚地理解本发明,以下结合实施例对本发明作进一步详细说明,但应当理解的是,以下实施例仅为本发明的优选实施方式,而本发明要求保护的范围并不仅局限于此。
实施例1:
采用以下方法来制备根据本发明的复合光催化剂CoP/MoS2:
(1)将200mg Co(NO3)2·6H2O和50mg柠檬酸钠混合在100ml水溶液中,然后加入3ml0.5M氢氧化钠溶液,搅拌3.5h,静置4h后分离沉淀物。将沉淀物离心,并在60℃的真空烘箱中干燥8h,得到Co(OH)2前驱体。然后,在玛瑙中均匀研磨50mg Co(OH)2和250mg NaH2PO2的混合物。随后,混合前体在氮气中以1℃/min的升温速率在300℃下煅烧2h。
(2)将6g NaNO3溶解在16ml浓盐酸中,置于烧杯中。随后,加入1.2g二硫化钼。30℃条件下超声处理制备的溶液10h,然后离心、洗涤,干燥得到MoS2纳米片;
(3)0.1g MoS2与0.02g CoP溶于30ml乙二醇溶液中,然后磁力搅拌5h,随后用水、乙醇洗涤、离心,并在60℃下干燥,得到复合光催化剂CoP/MoS2粉末;由此制得根据本发明的复合光催化剂CoP/MoS2。
实施例2:
按实施例1制备工艺同样步骤进行,不同的是(1)中称取50mg的CoP样品在光化学反应仪中进行光催化降解试验,测得该光催化剂对2-巯基苯并噻唑的降解率在120min内达到10.03%。
实施例3:
按实施例1制备工艺同样步骤进行,不同的是(2)中称取50mg的MoS2样品在光化学反应仪中进行光催化降解试验,测得该光催化剂对2-巯基苯并噻唑的降解率在120min内达到75.17%。
实施例4:
按实施例1制备工艺同样步骤进行,不同的是(3)中称取50mg的CoP/MoS2样品在光化学反应仪中进行光催化降解试验,测得该光催化剂对2-巯基苯并噻唑的降解率在120min内达到92.32%。
Claims (5)
1.一种复合光催化剂CoP/MoS2的制备方法,其特征在于,制备方法步骤如下:
(1)将钴盐、次磷酸钠以及柠檬酸钠制备CoP纳米颗粒;
(2)制备MoS2:将NaNO3溶解到浓盐酸中,将块状MoS2溶解到上述溶液中,然后在30℃条件下超声10h;
(3)将CoP和MoS2溶解到乙二醇溶液中,磁力搅拌,得到CoP/MoS2粉末。
2.根据权利要求1所述的制备方法,其特征在于,在所述步骤(1)中,
所述钴盐选自硝酸钴、氯化钴或者醋酸钴中的至少一种。
所述的P源选自次磷酸钠、三辛基膦或者白磷中的一种。
3.根据权利要求1所述的制备方法,其特征在于,所述步骤(1)为:硝酸钴的质量为200~250mg,加入柠檬酸钠的质量为50~55mg;次磷酸钠的质量250~300mg。
4.根据权利要求1所述的制备方法,其特征在于,所述步骤(2)为:NaNO3的质量为6.0~6.5g,浓盐酸的体积为16~20mL;MoS2的质量为1.2~1.5g。
5.根据权利要求1所述的制备方法,其特征在于,在所述步骤(3)中,MoS2和CoP的摩尔比为5~5.5mol,乙二醇的体积为30~35ml,磁力搅拌时间为5~6h。
权利要求1所述的合成方法制备的CoP/MoS2复合光催化剂,将其应用于环境中2-巯基苯并噻唑的降解。
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