CN110479243A - 一种花状Zn3(OH)2V2O7·2H2O光催化剂及其制备方法 - Google Patents
一种花状Zn3(OH)2V2O7·2H2O光催化剂及其制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 28
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 239000011701 zinc Substances 0.000 claims description 60
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 27
- 229910052725 zinc Inorganic materials 0.000 claims description 26
- 229910052720 vanadium Inorganic materials 0.000 claims description 15
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 11
- 229910021550 Vanadium Chloride Inorganic materials 0.000 claims description 10
- RPESBQCJGHJMTK-UHFFFAOYSA-I pentachlorovanadium Chemical group [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[V+5] RPESBQCJGHJMTK-UHFFFAOYSA-I 0.000 claims description 10
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 7
- 239000004202 carbamide Substances 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000011592 zinc chloride Substances 0.000 claims description 5
- 235000005074 zinc chloride Nutrition 0.000 claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- 229960002050 hydrofluoric acid Drugs 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000006276 transfer reaction Methods 0.000 claims description 2
- 238000004062 sedimentation Methods 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 19
- 230000015556 catabolic process Effects 0.000 abstract description 4
- 238000006731 degradation reaction Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000013508 migration Methods 0.000 abstract description 3
- 230000005012 migration Effects 0.000 abstract description 3
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- 239000012467 final product Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000012805 post-processing Methods 0.000 abstract description 2
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000002253 acid Substances 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 3
- 229940012189 methyl orange Drugs 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000013078 crystal Chemical group 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 2
- 229960004011 methenamine Drugs 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 description 2
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- 229910007541 Zn O Inorganic materials 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 239000004312 hexamethylene tetramine Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal vanadate Chemical group 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
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Abstract
本发明公开一种花状Zn3(OH)2V2O7·2H2O光催化剂及其制备方法，采用一步溶剂热反应直接合成最终产物，具有温和的合成温度，易于操作，产物后处理简单，对环境友好，适合大规模工业生产，有望推广到实际生产中；制备的花状Zn3(OH)2V2O7·2H2O，形成了纳米片组装的花状结构，产品形貌完整，其V‑O中层间存在层状通道，有利于光生电子和空穴的迁移，使得光生载流子更易进行氧化还原反应，对于实现较高光催化降解效应有非常重要的意义。
Description
技术领域
本发明属纳米无机材料制备领域，涉及一种花状Zn3(OH)2V2O7·2H2O光催化剂及其制备方法。
背景技术
随着各类工业的高速发展，全球环境污染问题更加引人注目。近年来，在治理污染方面纳米半导体光催化剂有巨大的应用潜力，光催化剂是绿色技术在污染物降解治理污水等方面是有潜力的候选方法。
焦钒酸锌是一种重要的过渡金属钒酸盐，其晶体结构属六方晶系，由Zn-O四面体层和V-O八面体层交替连接形成，其V-O中层间存在层状通道，这样的结构有利于光生电子和空穴的迁移，使得光生载流子更易进行氧化还原反应，具有较高光催化效应。
在焦钒酸锌合成方面，应用较多的方法主要包括：化学沉淀法、超声波法、水热法、电化学法等，现有焦钒酸锌的制备中钒源大多都是，氧化钒、偏钒酸铵、偏钒酸钠、钒酸钠；锌源大多都是，氧化锌、氯化锌、醋酸锌、硝酸锌、硫酸锌、碳酸锌；且一般需要加入其它有机的复杂的物质，合成时间较长工艺复杂，不利于工业大规模生产。
发明内容
针对上述现有技术的不足，本发明目的在于提出一种的花状Zn3(OH)2V2O7·2H2O光催化剂及其制备方法，操作简单，制备过程条件温和，制备的产品形貌完整，具有较高光催化降解效应。
为了实现上述目的，本发明采用以下技术方案。
一种花状Zn3(OH)2V2O7·2H2O光催化剂的制备方法，包括如下步骤：
(1)按锌和钒摩尔比为(0.6～1):(1.8～3)称取锌源和钒源，将锌源、钒源和碱性沉淀剂依次溶解到乙醇溶剂中，搅拌均匀后得到深紫色溶液，深紫色溶液中沉淀剂质量浓度为2～2.8g/L；
(2)将所得深紫色溶液转移反应釜中，在140～155℃恒温反应20～26h，水热反应结束后冷却至室温；
(3)将步骤(2)所得产物进行洗涤、抽滤后收集产物，收集的产物进行干燥即得花状Zn3(OH)2V2O7·2H2O光催化剂。
进一步，所述步骤(2)中将锌源、钒源和碱性沉淀剂依次溶解到乙醇溶剂中超声分散10～15min得到深紫色溶液。
进一步，所述步骤(3)中将步骤(2)所得产物分别用蒸馏水和无水乙醇洗涤、抽滤后收集产物，收集的产物60℃下干燥12h，即得花状Zn3(OH)2V2O7·2H2O光催化剂。
进一步，所述锌源是七水合硫酸锌、氯化锌、硝酸锌、乙酸锌或氟酸锌。
进一步，所述钒源是氯化钒。
进一步，所述碱性沉淀剂是尿素、六亚甲基四胺。
一种花状Zn3(OH)2V2O7·2H2O光催化剂，其为纳米片组装的花状结构。
本发明具有以下有益效果：
(1)本发明采用一步溶剂热反应直接合成最终产物，具有温和的合成温度，易于操作，产物后处理简单，对环境友好，适合大规模工业生产，有望推广到实际生产中。
(2)该方法制备的花状Zn3(OH)2V2O7·2H2O，形成了纳米片组装的花状结构，产品形貌完整，其V-O中层间存在层状通道，这样的结构有利于光生电子和空穴的迁移，使得光生载流子更易进行氧化还原反应，对于实现较高光催化降解效应有非常重要的意义。
附图说明
图1为本发明实施例2制备的花状Zn3(OH)2V2O7·2H2O光催化剂的X-射线衍射(XRD)图谱
图2为本发明实施例3制备的花状Zn3(OH)2V2O7·2H2O光催化剂的X-射线衍射(XRD)图谱
图3本发明实施例2制备的花状Zn3(OH)2V2O7·2H2O光催化剂的扫描电镜(SEM)照片
图4为本发明实施例3制备的花状Zn3(OH)2V2O7·2H2O光催化剂的扫描电镜(SEM)照片
图5为本发明实施例2制备的花状Zn3(OH)2V2O7·2H2O光催化剂降解甲基橙的性能测试图
具体实施方式
下面结合具体实施例对本发明作进一步详细描述，但不作为对本发明的限定。
实施例1：
(1)按锌和钒摩尔比0.6:3称取七水合硫酸锌和氯化钒，将七水合硫酸锌、氯化钒和尿素依次溶解到50mL乙醇溶剂中超声分散10min得到澄清的深紫色溶液，深紫色溶液中尿素质量浓度为2g/L；
(2)将所得深紫色溶液转移到100mL不锈钢反应釜中填充比为50％，将反应釜放入烘箱加热至140℃后恒温反应26h，最后冷却至室温；
(3)所得产物分别用蒸馏水和无水乙醇洗涤，抽滤，收集的产物60℃下干燥12h，即得到花状Zn3(OH)2V2O7·2H2O。
实施例2：
(1)按锌和钒摩尔比0.8:2.4称取氯化锌和氯化钒，将氯化锌、氯化钒和六亚甲基四胺依次溶解到50mL乙醇溶剂中超声分散15min得到澄清的深紫色溶液，深紫色溶液中六亚甲基四胺质量浓度为2.4g/L；
(2)将所得深紫色溶液转移到100mL不锈钢反应釜中填充比为50％，将反应釜放入烘箱加热至150℃后恒温反应24h，最后冷却至室温；
(3)所得产物分别用蒸馏水和无水乙醇洗涤，抽滤，收集的产物60℃下干燥12h，即得到花状Zn3(OH)2V2O7·2H2O。
图1是实施例2制备的花状Zn3(OH)2V2O7·2H2O光催化剂的X-射线衍射(XRD)图谱，从图中可以看到XRD响应峰显示实例2制备的样品结晶度不高，但能与Zn3(OH)2V2O7·2H2O的标准卡片完全对应，说明成功合成了焦钒酸锌这种物质。
图3是实施例2制备的花状Zn3(OH)2V2O7·2H2O光催化剂的扫描电镜(SEM)照片，从图中明显观察到较小且密集的花片状结构。
实施例3：
(1)按锌和钒摩尔比1:1.8称取硝酸锌和氯化钒，将硝酸锌、氯化钒和尿素依次溶解到50mL乙醇溶剂中超声分散15min得到澄清的深紫色溶液，深紫色溶液中六亚甲基四胺质量浓度为2.8g/L；
(2)将所得深紫色溶液转移到100mL不锈钢反应釜中填充比为50％，将反应釜放入烘箱加热至155℃后恒温反应20h，最后冷却至室温；
(3)所得产物分别用蒸馏水和无水乙醇洗涤，抽滤，收集的产物60℃下干燥12h，即得到花状Zn3(OH)2V2O7·2H2O。
图2是实施例3制备的花状Zn3(OH)2V2O7·2H2O光催化剂的X-射线衍射(XRD)图谱，从图中可以看到XRD响应峰显示实例3制备的样品结晶度很高且能与Zn3(OH)2V2O7·2H2O的标准卡片完全对应，说明成功合成了Zn3(OH)2V2O7·2H2O这种物质。
图4是实施例3制备的花状Zn3(OH)2V2O7·2H2O光催化剂的扫描电镜(SEM)照片，图中制备面积较大的片状组装的花状结构。
图5为实施例3制备的花状Zn3(OH)2V2O7·2H2O光催化剂降解甲基橙的性能测试图，能够较好的光催化降解甲基橙。
实施例4：
(1)按锌和钒摩尔比0.7:2.5称取氟酸锌和氯化钒，将氟酸锌、氯化钒和尿素依次溶解到50mL乙醇溶剂中超声分散12min得到澄清的深紫色溶液，深紫色溶液中六亚甲基四胺质量浓度为2.8g/L；
(2)将所得深紫色溶液转移到100mL不锈钢反应釜中填充比为50％，将反应釜放入烘箱加热至145℃后恒温反应23h，最后冷却至室温；
(3)所得产物分别用蒸馏水和无水乙醇洗涤，抽滤，收集的产物60℃下干燥12h，即得到花状Zn3(OH)2V2O7·2H2O。
最后应该说明的是：以上实施例仅用于说明本发明的技术方案而非对其限制，尽管参照上述实施例对本发明进行了详细说明，所属领域的普通技术人员应当理解：依然可以对本发明的具体实施方式进行修改或者等同替换，而未脱离本发明精神和范围的任何修改或者等同替换，其均应涵盖在本权利要求范围当中。
Claims (7)
1.一种花状Zn3(OH)2V2O7·2H2O光催化剂的制备方法，其特征在于包括如下步骤：
(1)按锌和钒摩尔比为(0.6～1):(1.8～3)称取锌源和钒源，将锌源、钒源和碱性沉淀剂依次溶解到乙醇溶剂中，搅拌均匀后得到深紫色溶液，深紫色溶液中沉淀剂质量浓度为2～2.8g/L；
(2)将所得深紫色溶液转移反应釜中，在140～155℃恒温反应20～26h，水热反应结束后冷却至室温；
(3)将步骤(2)所得产物进行洗涤、抽滤后收集产物，收集的产物进行干燥即得花状Zn3(OH)2V2O7·2H2O光催化剂。
2.如权利要求1所述的花状Zn3(OH)2V2O7·2H2O光催化剂的制备方法，其特征在于：所述步骤(2)中将锌源、钒源和碱性沉淀剂依次溶解到乙醇溶剂中超声分散10～15min得到深紫色溶液。
3.如权利要求1所述的花状Zn3(OH)2V2O7·2H2O光催化剂的制备方法，其特征在于：所述步骤(3)中将步骤(2)所得产物分别用蒸馏水和无水乙醇洗涤、抽滤后收集产物，收集的产物60℃下干燥12h，即得花状Zn3(OH)2V2O7·2H2O光催化剂。
4.如权利要求1所述的花状Zn3(OH)2V2O7·2H2O光催化剂的制备方法，其特征在于：所述锌源是七水合硫酸锌、氯化锌、硝酸锌、乙酸锌或氟酸锌。
5.如权利要求1所述的花状Zn3(OH)2V2O7·2H2O光催化剂的制备方法，其特征在于：所述钒源是氯化钒。
6.如权利要求1所述的花状Zn3(OH)2V2O7·2H2O光催化剂的制备方法，其特征在于：所述碱性沉淀剂是尿素、六亚甲基四胺。
7.一种采用如权利要求1-6任一项所述方法制备的花状Zn3(OH)2V2O7·2H2O光催化剂，其特征在于：其为纳米片组装的花状结构。
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