CN110075874B - 二硒化钼改性二氧化钛纳米光催化剂及其制备方法和应用 - Google Patents
二硒化钼改性二氧化钛纳米光催化剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及二硒化钼改性二氧化钛纳米光催化剂及其制备方法和应用。该纳米光催化剂粒径是100～200nm，主要成份为MoSe2与TiO2，其中MoSe2的含量为5‑20wt％。该催化剂的制备方法是：将可溶性钼盐、硒粉、还原剂溶于乙醇水溶液中，恒温水热反应并过滤、洗涤和干燥，得到MoSe2粉末；将该粉末分散到可溶性钛盐的乙醇或水溶液中，恒温水热反应后洗涤和干燥，得到所述纳米光催化剂，将其加入到成膜剂、分散剂、消泡剂、增白剂的水溶液中，搅拌，加入稳定剂、流平剂和防霉剂，调节pH值到7.0‑8.0，陈化，即可制得具有甲醛降解能力的环保涂料。本发明的方法成本价廉，生产工艺简单易控，适合大规模工业生产。
Description
技术领域
本发明涉及纳米材料及环保材料领域，具体涉及一种二硒化钼改性二氧化钛纳米光催化剂及其制备方法和应用。
背景技术
以二氧化钛为代表的传统光催化材料因其优异的物理化学性能而被广泛应用于光催化净化环境，是解决当前日趋严重的环境污染问题的重要途径之一。然而二氧化钛仅能吸收太阳光谱中4％～5％的紫外光,因此拓展二氧化钛的吸收光谱，提高其光催化效率是当前光催化领域研究的重要方向。此外，传统的光催化材料也是当前环保涂料的重要的添加剂或助剂，国家发明专利201410104099.X、201110196966.3、201410781164.2公布了光催化材料在涂料领域的应用，因此发展高性能的二氧化钛光催化剂具有广阔的应用前景。
近来，研究人员将各种各样的半导体纳米材料应用于二氧化钛的改性，并取得了较好的成果。特别是近期热点的二维层状材料如石墨烯、g-C3N4及过度金属硫族化合物等，因其在光催化领域优异的性能，而被广泛用于光催化剂材料的复合，其中石墨烯与g-C3N4在光催化领域已得到了广泛的应用。而层状结构的MoSe2纳米材料成为当前纳米材料领域的热点，中国发明专利201510907556.3，201810457292X，201810241753X等报道了其应用于润滑摩擦、锂电及光催化领域的应用，然而有关其应用于环保涂料的报道较少。
发明内容
针对现有技术的不足，本发明的目的之一在于提供一种二硒化钼改性二氧化钛纳米光催化剂。
上述目的是通过如下技术方案实现的：
一种二硒化钼改性二氧化钛纳米光催化剂，所述催化剂是100～200nm粒径的粉末，其主要成份为MoSe2与TiO2，其中MoSe2的质量百分含量为5-20％，余量为TiO2。
本发明的目的之二在于提供一种所述二硒化钼改性二氧化钛纳米光催化剂的制备方法，具体技术方案如下：
一种二硒化钼改性二氧化钛纳米光催化剂的制备方法，包括如下步骤：
(1)MoSe2的水热合成：将可溶性钼盐、硒粉、还原剂溶于40-60wt％的乙醇水溶液中，磁力搅拌20-40分钟，然后在150-250℃恒温水热反应5-7h后，冷却至室温，得到反应产物；将上述反应产物加入热碱液中，磁力搅拌10-20分钟后置于70-90℃的烘箱中1-3h以去除多余的硒，自然冷却至室温，过滤、洗涤和干燥后，得到MoSe2粉末；
(2)MoSe2/TiO2的合成：将步骤(1)中制备的MoSe2粉末分散到浓度为8-12g/L的可溶性钛盐的乙醇或水溶液中，超声分散20-40min后在160-220℃恒温水热反应10-14h；自然冷却至室温后，经过洗涤和干燥，得到所述MoSe2/TiO2纳米光催化剂。
优选地，所述可溶性钼盐为钼酸铵、钼酸钠或五氯化钼；还原剂为盐酸羟胺或硼氢化钠；可溶性钛盐为钛酸四丁酯或氟钛酸铵；热碱液为60-80℃的氢氧化钠(NaOH)或氢氧化钾(KOH)溶液，浓度为1～3mol/L。
优选地，步骤(1)所述可溶性钼盐、硒粉、还原剂在所述乙醇水溶液中的浓度分别为30～35g/L、30～35g/L、5～6g/L，所述热碱液与乙醇水溶液的体积比为1:1～2；步骤(2)所述MoSe2粉末和可溶性钛盐的质量比为0.04～0.16:1。
本发明的目的之三是提供一种二硒化钼改性二氧化钛纳米光催化剂的应用，具体技术方案如下：
所述二硒化钼改性二氧化钛纳米光催化剂应用于一种光催化环保涂料，按照质量百分比，其组成如下：成膜物质26％-60％，分散剂2-5％，消泡剂0.1-0.5％，防霉剂0.5-1.5％，稳定剂2-5％，流平剂0.3-0.6％，增白剂10-15％，纳米光催化助剂MoSe2/TiO22-8％,去离子水或蒸馏水15-40％。
优选地，所述成膜物质为水溶性丙烯酸乳液与聚氨酯乳液的混合物，其中水溶性丙烯酸乳液占所述环保涂料的21-45wt％，聚氨酯乳液占所述环保涂料的5％-20wt％；所述分散剂为十二烷基苯磺酸钠；所述防霉剂为氯酚钠涂料专用防腐防霉剂；所述消泡剂为聚硅氧烷类消泡剂；所述稳定剂为受阻胺类光稳定剂，所述流平剂为聚醚改性聚硅氧烷；所述增白剂为钛白粉。
所述光催化环保涂料的制备方法如下：以所述光催化涂料的质量百分比计，将21-45％的水溶性丙烯酸乳液、5-20％的聚氨酯乳液、2-5％的分散剂、0.1-0.5％的消泡剂、10-15％的增白剂分散到20-45％的去离子水或蒸馏水中，以800～1000r/min的转速均匀搅拌10-20min后缓缓加入2-8％的MoSe2/TiO2光催化剂粉末，在1500～2500r/min的转速下搅拌分散30-60min，然后以2500～3000r/min的转速搅拌20-40min，再在800～1500r/min的转速搅拌下加入2-5％的稳定剂、0.3-0.6％的流平剂、4.0-6.0％的防霉剂，同时用NaOH或KOH调节pH值到7.0-8.0，以800～1000r/min的转速搅拌均匀后陈化2-5h，制得所述MoSe2/TiO2光催化涂料。
本发明的有益效果
本发明提供了一种二硒化钼改性二氧化钛纳米光催化剂，其制备方法成本价廉，生产工艺简单易控，产物差率高，适合大规模的工业生产。该催化剂可应用于自清洁环保光催化涂料，有效清除甲醛等有毒有害气体，方便有效地净化空气。
附图说明
图1为本发明制得的MoSe2/TiO2复合纳米材料的EDS谱图。
图2为本发明制得的MoSe2/TiO2复合纳米材料的微观形貌扫描电镜(SEM)图。
图3为本发明制得的MoSe2/TiO2复合纳米材料的微观形貌透射电镜图(TEM)。
具体实施方式
以下通过具体实施方式进一步描述本发明，由技术常识可知，本发明也可通过其它的不脱离本发明技术特征的方案来描述，因此所有在本发明范围内或等同本发明范围内的改变均被本发明包含。
实施例1
MoSe2/TiO2纳米光催化剂的合成(MoSe2含量为5wt％)
(1)将1.6452g钼酸钠(Na2MoO4·2H2O)、1.5492g硒(Se)粉、0.2595g硼氢化钠(NaBH4)溶于50mL的乙醇水溶液(50wt％)中，磁力搅拌30min后转移至100mL不锈钢反应釜中，置于真空干燥箱，200℃下保温6h后，冷却至室温；将制备的黑色产物转入60℃的NaOH溶液(50mL，2mol/L)，磁力搅拌10min后转移至烘箱中80℃保温2h以除去多余的Se，再自然冷却至室温后，用去离子水、乙醇分别洗涤2-3次，离心分离(1600rpm/min)，真空干燥箱80℃条件干燥24h，得到MoSe2粉末。
(2)根据MoSe2在MoSe2/TiO2中5wt％的理论值，将步骤(1)中制备的MoSe2粉末0.02g分散到50mL的氟钛酸铵[(NH4)2TiF6]的乙醇溶液(10g/L)中,超声分散30min后将该混合液移至100mL内衬聚四氟乙烯的高温水热反应釜中密封，将反应釜放入真空干燥箱，180℃下保温12h。自然冷却至室温后，用去离子水、乙醇分别洗涤2-3次，离心分离(1600rpm/min)，真空干燥箱80℃条件干燥24h，得到MoSe2/TiO2纳米光催化剂。
MoSe2/TiO2光催化涂料的制备
以所述光催化涂料的质量百分比计，将成膜物质(25％的水溶性丙烯酸乳液、20％的聚氨酯乳液)、2％的分散剂(十二烷基苯磺酸钠)，0.1％的消泡剂(聚硅氧烷类消泡剂)，10％的增白剂(钛白粉)分散到34.6％的蒸馏水中，以800r/min的转速均匀搅拌10min后缓缓加入2％的MoSe2/TiO2光催化剂粉末作为纳米光催化助剂，在2000r/min的转速下搅拌分散45min左右，得到水性胶体。然后以2500r/min的转速搅拌30min使之充分分散，再800r/min的转速搅拌下加入2％的稳定剂(受阻胺类光稳定剂)、0.3％的流平剂(聚醚改性聚硅氧烷)、4.0％的防霉剂(氯酚钠涂料专用防腐防霉剂)，同时用2M的NaOH调节pH值到8.0，最后以800r/min的转速搅拌均匀后陈化2h，制得MoSe2/TiO2光催化涂料。
实施例2
MoSe2/TiO2纳米光催化剂的合成(MoSe2含量为10wt％)
(1)将1.6452g钼酸钠(Na2MoO4·2H2O)、1.5492g硒(Se)粉、0.2595g硼氢化钠(NaBH4)溶于50mL的乙醇水溶液(50wt％)中，磁力搅拌30min后转移至100mL不锈钢反应釜中，置于真空干燥箱，200℃下保温6h后，冷却至室温；将制备的黑色产物转入80℃的NaOH溶液(50mL，3mol/)，磁力搅拌10min后转移至烘箱中80℃保温2h以除去多余的Se，再自然冷却至室温后，用去离子水、乙醇分别洗涤2-3次，离心分离(1600rpm/min)，真空干燥箱80℃条件干燥24h，得到MoSe2粉末。
(2)根据MoSe2在MoSe2/TiO2中10wt％的理论值，将步骤(1)中制备的MoSe2粉末0.04g分散到50mL的氟钛酸铵[(NH4)2TiF6]的乙醇溶液(10g/L)中,超声分散30min后将该混合液移至100mL内衬聚四氟乙烯的高温水热反应釜中密封，将反应釜放入真空干燥箱，180℃下保温12h。自然冷却至室温后，用去离子水、乙醇分别洗涤2-3次，离心分离(1600rpm/min)，真空干燥箱80℃条件干燥24h，得到MoSe2/TiO2纳米光催化剂。
MoSe2/TiO2光催化涂料的制备:
以所述光催化涂料的质量百分比计，将成膜物质(21％的水溶性丙烯酸乳液、5％的聚氨酯乳液)、4％的分散剂(十二烷基苯磺酸钠)，0.3％的消泡剂(聚硅氧烷类消泡剂)，15％的增白剂(钛白粉)分散到41.3％的蒸馏水中，以1000r/min的转速均匀搅拌10min后缓缓加入4％的MoSe2/TiO2光催化剂粉末作为纳米光催化助剂，在2000r/min的转速下搅拌分散45min左右，得到水性胶体。然后以3000r/min的转速搅拌30min使之充分分散，再以1000r/min的转速搅拌下加入3％的稳定剂(受阻胺类光稳定剂)、0.4％的流平剂(聚醚改性聚硅氧烷)、6.0％的防霉剂(氯酚钠涂料专用防腐防霉剂)，同时用2M的NaOH调节pH值到8.0，最后以1000r/min的转速搅拌均匀后陈化2h，制得MoSe2/TiO2光催化涂料。
实施例3
MoSe2/TiO2纳米光催化剂的合成(MoSe2含量为20wt％)
(1)将1.6452g钼酸钠(Na2MoO4·2H2O)、1.5492g硒(Se)粉、0.2595g硼氢化钠(NaBH4)溶于50mL的乙醇水溶液(50wt％)中，磁力搅拌30min后转移至100mL不锈钢反应釜中，置于真空干燥箱，200℃下保温6h后，冷却至室温；将制备的黑色产物转入的70℃的NaOH溶液(50mL，2mol/L)，磁力搅拌10min后转移至烘箱中80℃保温2h以除去多余的Se，再自然冷却至室温后，用去离子水、乙醇分别洗涤2-3次，离心分离(1600rpm/min)，真空干燥箱80℃条件干燥24h，得到MoSe2粉末。
(2)根据MoSe2在MoSe2/TiO2中20wt％的理论值，将步骤(1)中制备的MoSe2粉末0.08g分散到50mL的氟钛酸铵[(NH4)2TiF6]的水溶液(10g/L)中,超声分散30min后将该混合液移至100mL内衬聚四氟乙烯的高温水热反应釜中密封，将反应釜放入真空干燥箱，180℃下保温12h。自然冷却至室温后，用去离子水、乙醇分别洗涤2-3次，离心分离(1600rpm/min)，真空干燥箱80℃条件干燥24h，得到MoSe2/TiO2纳米光催化剂。
MoSe2/TiO2光催化涂料的制备:
以所述光催化涂料的质量百分比计，将成膜物质(25％的水溶性丙烯酸乳液、20％的聚氨酯乳液)、5％的分散剂(十二烷基苯磺酸钠)，0.5％的消泡剂(聚硅氧烷类消泡剂)，10％的增白剂(钛白粉)分散到21.9％的蒸馏水中，以900r/min的转速均匀搅拌10min后缓缓加入8％的MoSe2/TiO2光催化剂粉末作为纳米光催化助剂，在2000r/min的转速下搅拌分散45min左右，得到水性胶体。然后以2800r/min的转速搅拌30min使之充分分散，再以900r/min的转速搅拌下加入5％的稳定剂(受阻胺类光稳定剂)、0.6％的流平剂(聚醚改性聚硅氧烷)、4.0％的防霉剂(氯酚钠涂料专用防腐防霉剂)，同时用2M的KOH调节pH值到8.0，最后以900r/min的转速搅拌均匀后陈化2h，制得MoSe2/TiO2光催化涂料。
图1为EDS图谱，表明产物由Mo、Se、Ti、O元合成产物MoSe2/TiO2的素组成，无其它杂质，其Mo：Se为1:1.98，Ti：O为1：2.05，与化学式相一致，证明了MoSe2/TiO2的成功制备。图2和图3分别为合成产物MoSe2/TiO2的SEM和TEM图，由图可知四方结构TiO2纳米颗粒生长在花状MoSe2之上，其平均颗粒尺度约为200nm。
为了考察光催化涂料降解甲醛的实际效果，本发明利用欧盟普遍采用的HJC-1型环境测试舱模拟可见光源下室内环境。采用乙酰丙酮分光光度法(GB/T 15516-1995)，选择每隔2h采样5L舱内的气体，检测环境测试舱中甲醛气体的浓度变化,从而可以计算出MoSe2/TiO2光催化涂料光催化降解甲醛气体的效率，具体见表1。从表1中可以看出本发明的光催化剂8小时的甲醛降解率最高可达34.5％。
表1.对比实施例光催化涂料光催化降解甲醛气体的效率(％)
Claims (3)
1.一种二硒化钼改性二氧化钛纳米光催化剂作为光催化环保涂料在光催化除甲醛中的应用，其特征在于，所述催化剂是100～200nm粒径的粉末，其成分为MoSe2与TiO2，其中MoSe2的质量百分含量为5-20％，余量为TiO2；且通过如下步骤制得：
(1)MoSe2的水热合成：将可溶性钼盐、硒粉、还原剂溶于40-60wt％的乙醇水溶液中，磁力搅拌20-40分钟，然后在150-250℃恒温水热反应5-7h后，冷却至室温，得到反应产物；将上述反应产物加入热碱液中，磁力搅拌10-20分钟后置于70-90℃的烘箱中1-3h以去除多余的硒，自然冷却至室温，过滤、洗涤和干燥后，得到MoSe2粉末；其中所述可溶性钼盐、硒粉、还原剂在所述乙醇水溶液中的浓度分别为30～35g/L、30～35g/L、5～6g/L，所述热碱液与乙醇水溶液的体积比为1:1～2；
(2)MoSe2/TiO2的合成：将步骤(1)中制备的MoSe2粉末分散到浓度为8-12g/L的可溶性钛盐的乙醇或水溶液中，超声分散20-40min后在160-220℃恒温水热反应10-14h；自然冷却至室温后，经过洗涤和干燥，得到所述MoSe2/TiO2纳米光催化剂；其中所述MoSe2粉末和可溶性钛盐的质量比为0.04～0.16:1。
2.根据权利要求1所述的二硒化钼改性二氧化钛纳米光催化剂作为光催化环保涂料在光催化除甲醛中的应用，其特征在于，所述可溶性钼盐为钼酸铵、钼酸钠或五氯化钼；所述还原剂为盐酸羟胺或硼氢化钠；所述可溶性钛盐为钛酸四丁酯或氟钛酸铵；所述热碱液为60-80℃的氢氧化钠或氢氧化钾溶液，浓度为1-3mol/L。
3.根据权利要求1所述的二硒化钼改性二氧化钛纳米光催化剂作为光催化环保涂料在光催化除甲醛中的应用，其特征在于，所述光催化环保涂料的制备方法如下：
以所述光催化环保涂料的质量百分比计，将21-45％的水溶性丙烯酸乳液、5-20％的聚氨酯乳液、2-5％的分散剂、0.1-0.5％的消泡剂、10-15％的增白剂分散到20-45％的去离子水或蒸馏水中，以800～1000r/min的转速均匀搅拌10-20min后缓缓加入2-8％的MoSe2/TiO2光催化剂粉末，在1500～2500r/min的转速下搅拌分散30-60min，然后以2500～3000r/min的转速搅拌20-40min，再在800～1500r/min的转速搅拌下加入2-5％的稳定剂、0.3-0.6％的流平剂、4.0-6.0％的防霉剂，同时用NaOH或KOH调节pH值到7.0-8.0，以800～1000r/min的转速搅拌均匀后陈化2-5h，制得所述光催化环保涂料；所述分散剂为十二烷基苯磺酸钠；所述防霉剂为氯酚钠涂料专用防腐防霉剂；所述消泡剂为聚硅氧烷类消泡剂；所述稳定剂为受阻胺类光稳定剂，所述流平剂为聚醚改性聚硅氧烷；所述增白剂为钛白粉。
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