CN110961119B - 一种氧化银和氧化锌复合磁性可分离光催化剂的制备方法 - Google Patents
一种氧化银和氧化锌复合磁性可分离光催化剂的制备方法 Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 41
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 30
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 15
- 239000002131 composite material Substances 0.000 title claims abstract description 14
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- 229910001923 silver oxide Inorganic materials 0.000 title claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 47
- 101710134784 Agnoprotein Proteins 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000011259 mixed solution Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 13
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 10
- -1 iron ions Chemical class 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
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- 238000003760 magnetic stirring Methods 0.000 claims description 7
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- 159000000014 iron salts Chemical class 0.000 claims description 3
- 239000010865 sewage Substances 0.000 abstract description 7
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- 239000002245 particle Substances 0.000 abstract description 4
- 230000005389 magnetism Effects 0.000 abstract description 3
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 239000011592 zinc chloride Substances 0.000 description 2
- 235000005074 zinc chloride Nutrition 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
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- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
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- 238000005215 recombination Methods 0.000 description 1
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- 239000004065 semiconductor Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
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Abstract
本发明公开了一种氧化银和氧化锌复合磁性可分离光催化剂的制备方法，具体包括如下步骤：步骤1，制备ZnO‑ZnFe2O4粉体；步骤2，配置AgNO3溶液，根据AgNO3溶液与步骤1制备的ZnO‑ZnFe2O4粉体制备Ag2O‑ZnO‑ZnFe2O4粉体光催化剂。本发明通过将Ag2O，ZnO和ZnFe2O4三种物质进行有效复合，光催化剂粉体粒径大小为0.5μm‑1000μm，且具有磁性，易于与污水进行有效分离回收，使该催化剂在治理污水处理方面具有实际应用价值。
Description
技术领域
本发明属于环境保护技术领域，涉及一种氧化银和氧化锌复合磁性可分离光催化剂的制备方法。
背景技术
光催化剂被称为绿色催化剂，对污水中的污染物的处理具有能耗低、无二次污染、深度氧化等优点而备受重视。其中光催化剂的成分决定光催化效率和多次可循环使用的实用性的关键。传统光催化剂的粒径小，在水流的冲击作用下，不利于其与降解液得到有效的分离，容易造成二次污染，限制了其广泛的应用。ZnFe2O4禁带宽度为1.9eV，在可见光照射下便可使光生电子-空穴对进行有效的分离，而且具有别的光催化材料所不具有的性能—磁性能，在外加电场存在的情况下，使其和污水可以进行有效的分离。然而纯相的ZnFe2O4光生电子-空穴对的复合效率很高，严重的限制了在光催化领域的应用。研究表明，采用别的半导体光催化剂与ZnFe2O4进行复合得到的复合光催化剂较ZnFe2O4的催化性能有显著提高。
发明内容
本发明的目的是提供一种氧化银和氧化锌复合磁性可分离光催化剂的制备方法，通过该方法制得的催化剂粉体粒径大小为0.5μm-1000μm，该催化剂具有磁性，易于与污水进行有效分离。
本发明所采用的技术方案是，一种氧化银和氧化锌复合磁性可分离光催化剂的制备方法，具体包括如下步骤：
步骤1，制备ZnO-ZnFe2O4粉体；
步骤2，配置AgNO3溶液，根据AgNO3溶液与步骤1制备的ZnO-ZnFe2O4粉体制备Ag2O-ZnO-ZnFe2O4粉体光催化剂。
本发明的特点还在于，
步骤1的具体过程为：配制包含有锌离子和铁离子的混合溶液A，在50～100℃下，对混合溶液A进行搅拌干燥，随后在马弗炉里进行煅烧，以0.5-3℃/min升温速率升至300-1100℃，保温1-5h，随后自然冷却，得到ZnO-ZnFe2O4的块状物质，研磨后，得ZnO-ZnFe2O4粉体。
步骤1中，混合溶液A中锌离子和铁离子的摩尔比为1:0.1-1。
步骤1中，混合溶液A中的锌离子和铁离子从锌盐和铁盐中获得。
铁盐和锌盐为氯化盐、硝酸盐、有机盐中的至少一种。
步骤2的具体过程为：
在黑暗条件下配置100mL浓度为0.1-1g/L的AgNO3溶液，将步骤1得到的ZnO-ZnFe2O4粉体加入到AgNO3溶液中，在磁力搅拌的条件下加入浓度为0.01-1mol/L的NaOH溶液1-10mL，随后洗涤，真空干燥，得到Ag2O-ZnO-ZnFe2O4粉体光催化剂。
步骤2中，ZnO-ZnFe2O4粉体的质量和AgNO3溶液的体积比为100:1g/L。
本发明的有益效果是，本发明提供的一种Ag和ZnO复合磁性可分离光催化剂，通过将Ag2O，ZnO和ZnFe2O4三种物质进行有效复合，光催化剂粉体粒径大小为0.5μm-1000μm，且具有磁性，易于与污水进行有效分离回收，使该催化剂在治理污水处理方面具有实际应用价值。
附图说明
图1是本发明一种氧化银和氧化锌复合磁性可分离光催化剂的制备方法实施例1中制得的Ag2O-ZnO-ZnFe2O4粉体的X射线衍射图谱；
图2是本发明一种氧化银和氧化锌复合磁性可分离光催化剂的制备方法实施例1中制得的Ag2O-ZnO-ZnFe2O4粉体光催化剂在可见光照射下降解罗丹明B的曲线。
具体实施方式
下面结合附图和具体实施方式对本发明进行详细说明。
本发明一种氧化银和氧化锌复合磁性可分离光催化剂的制备方法，具体包括如下步骤：
步骤1，制备ZnO-ZnFe2O4粉体；
步骤1的具体过程为：配制包含有锌离子和铁离子的混合溶液A，在50～100℃下，对混合溶液A进行搅拌干燥，随后在马弗炉里进行煅烧，以0.5-3℃/min升温速率升至300-1100℃，保温1-5h，随后自然冷却，得到ZnO-ZnFe2O4的块状物质，研磨后，得ZnO-ZnFe2O4粉体。
步骤1中，混合溶液A中锌离子和铁离子的摩尔比为1:0.1-1。
混合溶液A中锌离子和铁离子浓度分别为1-2mol/L和0.1-2mol/L
步骤1中，混合溶液A中的锌离子和铁离子从锌盐和铁盐中获得。
铁盐和锌盐为氯化盐、硝酸盐、有机盐中的至少一种。
步骤2，配置AgNO3溶液，根据AgNO3溶液与步骤1制备的ZnO-ZnFe2O4粉体制备Ag2O-ZnO-ZnFe2O4粉体光催化剂。
步骤2的具体过程为：
在黑暗条件下配置100mL浓度为0.1-1g/L的AgNO3溶液，将步骤1得到的ZnO-ZnFe2O4粉体加入到AgNO3溶液中，在磁力搅拌的条件下加入浓度为0.01-1mol/L的NaOH溶液1-10mL，随后洗涤，真空干燥，得到Ag2O-ZnO-ZnFe2O4粉体光催化剂。
步骤2中，ZnO-ZnFe2O4粉体的质量和AgNO3溶液的体积比为100:1g/L。
实施例1
步骤1，配置浓度为1.5mol/L氯化锌和1mol/L氯化铁的混合溶液，然后在100℃条件下，搅拌12h进行干燥，随后在马弗炉里进行煅烧，以1℃/min升温速率至700℃，保温3h，随后自然冷却，再将块状物质研磨，得到ZnO-ZnFe2O4粉体；
步骤2，在黑暗条件下配置100mL浓度为0.1g/L的AgNO3溶液，将步骤2得到的10gZnO-ZnFe2O4粉体加入到AgNO3溶液中，在磁力搅拌的条件下加入浓度为0.01mol/L的NaOH溶液1mL，随后洗涤，真空干燥，得到Ag2O-ZnO-ZnFe2O4粉体光催化剂。
图1是实施例1中制得的Ag2O-ZnO-ZnFe2O4粉体的X射线衍射图谱；
图2是实施例1中制得的Ag2O-ZnO-ZnFe2O4粉体光催化剂在可见光照射下降解罗丹明B的曲线。
实施例2
步骤1，配置浓度为1mol/L硝酸锌和0.1mol/L硝酸铁的混合溶液，然后在50℃条件下，搅拌12h进行干燥，随后在马弗炉里进行煅烧，以0.5℃/min升温速率至300℃，保温1h，随后自然冷却，再将块状物质研磨，得到ZnO-ZnFe2O4粉体；
步骤2，在黑暗条件下配置100mL浓度为1g/L的AgNO3溶液，将步骤2得到的10gZnO-ZnFe2O4粉体加入到上述溶液中，在磁力搅拌的条件下加入浓度为0.05mol/L的NaOH溶液5mL，随后洗涤，真空干燥，得到Ag2O-ZnO-ZnFe2O4粉体光催化剂。
实施例3
步骤1，配置浓度为2mol/L醋酸锌和2mol/L醋酸铁的混合溶液，然后在80℃条件下，搅拌12h进行干燥，随后在马弗炉里进行煅烧，以3℃/min升温速率至1100℃，保温5h，随后自然冷却，再将块状物质研磨，得到ZnO-ZnFe2O4粉体；
步骤2，在黑暗条件下配置100mL浓度为0.5g/L的AgNO3溶液，将步骤2得到的10gZnO-ZnFe2O4粉体加入到AgNO3溶液中，在磁力搅拌的条件下加入浓度为1mol/L的NaOH溶液10mL，随后洗涤，真空干燥，得到Ag2O-ZnO-ZnFe2O4粉体光催化剂。
实施例4
步骤1，配置浓度为2mol/L氯化锌和1mol/L硝酸铁的混合溶液，然后在100℃条件下，搅拌12h进行干燥，随后在马弗炉里进行煅烧，以0.5℃/min升温速率至1100℃，保温1h，随后自然冷却，再将块状物质研磨，得到ZnO-ZnFe2O4粉体；
步骤2，在黑暗条件下配置100mL浓度为0.1g/L的AgNO3溶液，将步骤2得到的10gZnO-ZnFe2O4粉体加入到AgNO3溶液中，在磁力搅拌的条件下加入浓度为1mol/L的NaOH溶液1mL，随后洗涤，真空干燥，得到Ag2O-ZnO-ZnFe2O4粉体光催化剂。
Claims (3)
1.一种氧化银和氧化锌复合磁性可分离光催化剂的制备方法，其特征在于：具体包括如下步骤：
步骤1，制备ZnO-ZnFe2O4粉体；
所述步骤1的具体过程为：配制包含有锌离子和铁离子的混合溶液A，在50～100℃下，对混合溶液A进行搅拌干燥，随后在马弗炉里进行煅烧，以0.5-3℃/min升温速率升至300-1100℃，保温1-5h，随后自然冷却，得到ZnO-ZnFe2O4的块状物质，研磨后，得ZnO-ZnFe2O4粉体；
所述步骤1中，混合溶液A中锌离子和铁离子的摩尔比为1:0.1-1；
步骤2，配置AgNO3溶液，根据AgNO3溶液与步骤1制备的ZnO-ZnFe2O4粉体制备Ag2O-ZnO-ZnFe2O4粉体光催化剂；
所述步骤2的具体过程为：
在黑暗条件下配置100mL浓度为0.1-1g/L的AgNO3溶液，将步骤1得到的ZnO-ZnFe2O4粉体加入到AgNO3溶液中，在磁力搅拌的条件下加入浓度为0.01-1mol/L的NaOH溶液1-10mL，随后洗涤，真空干燥，得到Ag2O-ZnO-ZnFe2O4粉体光催化剂；
所述步骤2中，ZnO-ZnFe2O4粉体的质量和AgNO3溶液的体积比为100:1g/L。
2.根据权利要求1所述的一种氧化银和氧化锌复合磁性可分离光催化剂的制备方法，其特征在于：所述步骤1中，混合溶液A中的锌离子和铁离子从锌盐和铁盐中获得。
3.根据权利要求2所述的一种氧化银和氧化锌复合磁性可分离光催化剂的制备方法，其特征在于：所述铁盐和锌盐为氯化盐、硝酸盐、有机盐中的至少一种。
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