CN108043399A - 一种纳米晶纤维素模板制备光催化剂的方法 - Google Patents
一种纳米晶纤维素模板制备光催化剂的方法 Download PDFInfo
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- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 32
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- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 14
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Abstract
本发明公开一种纳米晶纤维素模板制备光催化剂的方法,属于光催化剂制备领域。所述纳米晶纤维素模板制备光催化剂的方法,是在无水乙醇中加入纳米晶纤维素胶体、醋酸锌、硝酸银、硼氢化钠,得到NCC/ZnO/Ag复合物。该复合物经离心洗涤、真空冷冻干燥和高温煅烧,制成具有高催化能力的ZnO/Ag光催化剂。本发明制备的光催化剂借助纳米晶纤维素的高比表面积,赋予ZnO/Ag光催化剂高的比表面积和反应活性。性能测试表明:以纳米晶纤维素模板制备得到的ZnO/Ag光催化剂在可见光下光照2h内对20mg/L亚甲基蓝的光催化降解率达到85~95%。
Description
技术领域
本发明涉及光催化剂制备领域,具体涉及一种通过纳米晶纤维素模板制备可见光下具有高催化能力光催化剂的方法。
背景技术
纳米ZnO作为一种宽带隙(3.37eV)和高结合能(~60meV)光催化材料,具有无毒、高电子迁移率、理化性质稳定以及较高的光催化活性等特点。在紫外光或可见光下,纳米ZnO价带上的电子被激发到导带,形成电子-空穴对,与有机物反应生成自由基,将有机物氧化成水和二氧化碳。
采用纳米晶纤维素(nanocrystalline cellulose,NCC)为模板原位聚合制备NCC/ZnO复合胶体是近年来提高纳米ZnO催化活性的一个新方法。发明专利CN 106700784 A公开了一种通过NCC的吸附和ZnO光催化协同降解人造板甲醛的方法。但是由于纳米ZnO禁带宽度的限制,一般只在紫外光下具有很高的催化活性,可见光利用率低,而且光生电子-空穴对易于复合从而降低了NCC/ZnO复合胶体的光催化效率。贵金属Ag掺杂NCC/ZnO复合胶体,利用Ag表面等离子体共振效应,使得纳米ZnO中载流子重新分布形成肖特基势垒,其作为“电子陷阱”能够有效地俘获电子,降低光生电子和空穴的复合,增强其对可见光的吸收。发明专利CN 107189584 A公开了一种通过Ag掺杂NCC/ZnO的水性聚丙烯酸涂料及其制备方法,有效提高水性聚丙烯酸涂料在可见光下对室内有机挥发物(Volatile organiccompounds,VOC)的降解效率。
尽管上述公开的材料都提及以NCC为模板制备ZnO及Ag掺杂ZnO光催化剂的方法。然而,两个文件仍然存在不足:(1)限制了光催化剂的用途——分别使用在人造板和水性聚丙烯酸涂料的降醛方面;(2)光催化效率不高。发明专利CN 106700784 A提及紫外光下人造板甲醛浓度下降率达到65~88%;发明专利CN 107189584 A提及可见光下甲醛的光催化降解率达到30.3~45.2%。进一步提高光催化剂在可见光下的催化效率,扩大光催化剂的使用范围是追求的目标。
发明内容
本发明的目的:提供一种采用纳米晶纤维素为模板制备可见光下具有高催化能力光催化剂的方法。
本发明的技术解决方案:在无水乙醇中依次加入纳米晶纤维素胶体、醋酸锌、硝酸银、硼氢化钠,制得NCC/ZnO/Ag复合物,该复合物经离心洗涤、冷冻干燥和高温煅烧,制成具有高催化能力的ZnO/Ag光催化剂。具体方法如下:
(1)按质量比1.5~2.5∶100称取纳米晶纤维素、去离子水,充分混合,在冰水浴中进行超声分散,得到质量分数为1.5~2.5%的纳米晶纤维素胶体;
(2)按质量比100∶7.5~10∶0.2~0.4∶1000~1500称取步骤(1)的纳米晶纤维素胶体、醋酸锌、硝酸银、无水乙醇,并将纳米晶纤维素胶体、醋酸锌依次加入到无水乙醇中,超声分散均匀,然后加入硝酸银,超声分散均匀,用0.5mol/L的氢氧化钠调节体系pH值至7,升温至70~80℃,反应2~3h,然后向混合溶液中加入硼氢化钠(硼氢化钠的质量比为硝酸银的6%~8%),继续反应2~3h,制得复合物;将复合物置于110~130℃处理0.5~1h,制得白色NCC/ZnO/Ag复合物;
(3)将步骤(2)得到的NCC/ZnO/Ag复合物取出,加入去离子水,放置于离心机中,在10000~12000r/min离心处理2~3次,得到NCC/ZnO/Ag白色沉淀物;
(4)将步骤(3)得到的NCC/ZnO/Ag白色沉淀物放入真空冷冻干燥机中进行干燥,干燥时间48~56h,得到NCC/ZnO/Ag白色粉末物;
(5)将步骤(4)得到的NCC/ZnO/Ag白色粉末物放入管式炉中,在氮气保护下升温至550~600℃,处理2~3h,得到ZnO/Ag光催化剂。
本发明的优点:
本发明利用纳米晶纤维素的高比表面积、高分散性、高反应活性,作为反应模板,促进了ZnO、Ag在反应过程中的均匀分散;最后通过氮气保护进行煅烧,保留了纳米晶纤维素的高比表面积,赋予ZnO/Ag光催化剂高的比表面积和反应活性。性能测试表明:以纳米晶纤维素为模板制备得到的ZnO/Ag光催化剂在可见光下光照2h内对20mg/L亚甲基蓝的光催化降解率达到85~95%。
具体实施方式
实施例1,
(1)按质量比2∶100称取纳米晶纤维素、去离子水,充分混合,在冰水浴中进行超声分散,得到质量分数为2%的纳米晶纤维素胶体;
(2)按质量比100∶8∶0.25∶1200称取步骤(1)的纳米晶纤维素胶体、醋酸锌、硝酸银、无水乙醇,并将纳米晶纤维素胶体、醋酸锌依次加入到无水乙醇中,超声分散均匀,然后加入硝酸银,超声分散均匀,用0.5mol/L的氢氧化钠调节体系pH值至7,升温至70~80℃,反应2h,然后向混合溶液中加入硼氢化钠(硼氢化钠的质量比为硝酸银的6%),继续反应2~3h,制得复合物;将复合物置于110~130℃处理0.5~1h,制得白色NCC/ZnO/Ag复合物;
(3)将步骤(2)得到的NCC/ZnO/Ag复合物取出,加入去离子水,放置于离心机中,在10000r/min离心处理3次,得到NCC/ZnO/Ag白色沉淀物;
(4)将步骤(3)得到的NCC/ZnO/Ag白色沉淀物放入真空冷冻干燥机中进行干燥,干燥时间48h,得到NCC/ZnO/Ag白色粉末物;
(5)将步骤(4)得到的NCC/ZnO/Ag白色粉末物放入管式炉中,在氮气保护下升温至550℃,处理2~3h,得到ZnO/Ag光催化剂。
以上述制备得到的ZnO/Ag光催化剂对20mg/L亚甲基蓝进行光催化降解测试,在可见光下光照2h的光催化降解率达到95%。
实施例2,
(1)按质量比1.5∶100称取纳米晶纤维素、去离子水,充分混合,在冰水浴中进行超声分散,得到质量分数为1.5%的纳米晶纤维素胶体;
(2)按质量比100∶7.5∶0.2∶1000称取步骤(1)的纳米晶纤维素胶体、醋酸锌、硝酸银、无水乙醇,并将纳米晶纤维素胶体、醋酸锌依次加入到无水乙醇中,超声分散均匀,然后加入硝酸银,超声分散均匀,用0.5mol/L的氢氧化钠调节体系pH值至7,升温至70~80℃,反应2h,然后向混合溶液中加入硼氢化钠(硼氢化钠的质量比为硝酸银的6%),继续反应2~3h,制得复合物;将复合物置于110~130℃处理0.5~1h,制得白色NCC/ZnO/Ag复合物;
(3)将步骤(2)得到的NCC/ZnO/Ag复合物取出,加入去离子水,放置于离心机中,在12000r/min离心处理3次,得到NCC/ZnO/Ag白色沉淀物;
(4)将步骤(3)得到的NCC/ZnO/Ag白色沉淀物放入真空冷冻干燥机中进行干燥,干燥时间56h,得到NCC/ZnO/Ag白色粉末物;
(5)将步骤(4)得到的NCC/ZnO/Ag白色粉末物放入管式炉中,在氮气保护下升温至550℃,处理2~3h,得到ZnO/Ag光催化剂。
以上述制备得到的ZnO/Ag光催化剂对20mg/L亚甲基蓝进行光催化降解测试,在可见光下光照2h的光催化降解率达到85%。
实施例3,
(1)按质量比2.5∶100称取纳米晶纤维素、去离子水,充分混合,在冰水浴中进行超声分散,得到质量分数为2.5%的纳米晶纤维素胶体;
(2)按质量比100∶9∶0.3∶1500称取步骤(1)的纳米晶纤维素胶体、醋酸锌、硝酸银、无水乙醇,并将纳米晶纤维素胶体、醋酸锌依次加入到无水乙醇中,超声分散均匀,然后加入硝酸银,超声分散均匀,用0.5mol/L的氢氧化钠调节体系pH值至7,升温至70~80℃,反应3h,然后向混合溶液中加入硼氢化钠(硼氢化钠的质量比为硝酸银的8%),继续反应2~3h,制得复合物;将复合物置于110~130℃处理0.5~1h,制得白色NCC/ZnO/Ag复合物;
(3)将步骤(2)得到的NCC/ZnO/Ag复合物取出,加入去离子水,放置于离心机中,在12000r/min离心处理2次,得到NCC/ZnO/Ag白色沉淀物;
(4)将步骤(3)得到的NCC/ZnO/Ag白色沉淀物放入真空冷冻干燥机中进行干燥,干燥时间48h,得到NCC/ZnO/Ag白色粉末物;
(5)将步骤(4)得到的NCC/ZnO/Ag白色粉末物放入管式炉中,在氮气保护下升温至600℃,处理2~3h,得到ZnO/Ag光催化剂。
以上述制备得到的ZnO/Ag光催化剂对20mg/L亚甲基蓝进行光催化降解测试,在可见光下光照2h的光催化降解率达到88%。
实施例4,
(1)按质量比2.5∶100称取纳米晶纤维素、去离子水,充分混合,在冰水浴中进行超声分散,得到质量分数为2.5%的纳米晶纤维素胶体;
(2)按质量比100∶10∶0.4∶1500称取步骤(1)的纳米晶纤维素胶体、醋酸锌、硝酸银、无水乙醇,并将纳米晶纤维素胶体、醋酸锌依次加入到无水乙醇中,超声分散均匀,然后加入硝酸银,超声分散均匀,用0.5mol/L的氢氧化钠调节体系pH值至7,升温至70~80℃,反应2h,然后向混合溶液中加入硼氢化钠(硼氢化钠的质量比为硝酸银的8%),继续反应2~3h,制得复合物;将复合物置于110~130℃处理0.5~1h,制得白色NCC/ZnO/Ag复合物;
(3)将步骤(2)得到的NCC/ZnO/Ag复合物取出,加入去离子水,放置于离心机中,在12000r/min离心处理3次,得到NCC/ZnO/Ag白色沉淀物;
(4)将步骤(3)得到的NCC/ZnO/Ag白色沉淀物放入真空冷冻干燥机中进行干燥,干燥时间56h,得到NCC/ZnO/Ag白色粉末物;
(5)将步骤(4)得到的NCC/ZnO/Ag白色粉末物放入管式炉中,在氮气保护下升温至550℃,处理2~3h,得到ZnO/Ag光催化剂。
以上述制备得到的ZnO/Ag光催化剂对20mg/L亚甲基蓝进行光催化降解测试,在可见光下光照2h的光催化降解率达到92%。
Claims (2)
1.一种纳米晶纤维素模板制备光催化剂的方法,其特征在于按以下步骤进行:
(1)按质量比1.5~2.5∶100称取纳米晶纤维素、去离子水,充分混合,在冰水浴中进行超声分散,得到质量分数为1.5~2.5%的纳米晶纤维素胶体;
(2)按质量比100∶7.5~10∶0.2~0.4∶1000~1500称取步骤(1)的纳米晶纤维素胶体、醋酸锌、硝酸银、无水乙醇,并将纳米晶纤维素胶体、醋酸锌依次加入到无水乙醇中,超声分散均匀,然后加入硝酸银,超声分散均匀,用0.5mol/L的氢氧化钠调节体系pH值至7,升温至70~80℃,反应2~3h,然后向混合溶液中加入硼氢化钠,继续反应2~3h,制得复合物;将复合物置于110~130℃处理0.5~1h,制得NCC/ZnO/Ag复合物;
(3)将步骤(2)得到的NCC/ZnO/Ag复合物取出,加入去离子水,放置于离心机中,在10000~12000r/min离心处理2~3次,得到NCC/ZnO/Ag白色沉淀物;
(4)将步骤(3)得到的NCC/ZnO/Ag白色沉淀物放入真空冷冻干燥机中进行干燥,干燥时间48~56h,得到NCC/ZnO/Ag白色粉末物;
(5)将步骤(4)得到的NCC/ZnO/Ag白色粉末物放入管式炉中,在氮气保护下升温至550~600℃,处理2~3h,得到ZnO/Ag光催化剂;
所述步骤(2)的硼氢化钠,其质量比为硝酸银的6%~8%。
2.按照权利要求1任意方法制备得到的光催化剂。
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