CN108452815A - 一种Ag/AgBr/BiOBr/Bi复合型光催化剂的制备 - Google Patents
一种Ag/AgBr/BiOBr/Bi复合型光催化剂的制备 Download PDFInfo
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- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 12
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 9
- 230000015556 catabolic process Effects 0.000 claims abstract description 8
- 238000006731 degradation reaction Methods 0.000 claims abstract description 8
- 238000006479 redox reaction Methods 0.000 claims abstract description 6
- 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 claims abstract description 6
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims abstract description 4
- 238000011065 in-situ storage Methods 0.000 claims abstract description 4
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 claims abstract description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 12
- 239000000975 dye Substances 0.000 claims description 10
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 241000692870 Inachis io Species 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 claims description 2
- 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 claims description 2
- 229940012189 methyl orange Drugs 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 7
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 238000007146 photocatalysis Methods 0.000 abstract description 6
- 238000005286 illumination Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000010748 Photoabsorption Effects 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000593 degrading effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000007540 photo-reduction reaction Methods 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- -1 bismuthino compounds Chemical class 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
本发明为一种Ag/AgBr/BiOBr/Bi复合型光催化剂的制备，提供了一种在可见光下具有光催化降解有机染料的复合型光催化剂的制备方法，其制备包括以下步骤：以单质铋为基质材料，采用一种原位氧化还原反应法，利用Bi与AgBr发生氧化还原反应，制备了具有异质结结构的Ag/AgBr/BiOBr/Bi复合型光催化剂。本发明制备的Ag/AgBr/BiOBr/Bi异质结复合型光催化剂具有良好的光催化性能，能够在可见光照射下，降解罗丹明B、结晶紫和金橙II在内的多种染料。本发明涉及的工艺简单，原料易得，光响应性能良好，可重复使用，适用于工业化生产，应用前景广泛。
Description
技术领域
本发明属于光催化技术领域，涉及一种在可见光下具有高降解多种染料活性的Ag/AgBr/BiOBr/Bi复合型光催化剂的制备。
背景技术
随着当今科技的迅速发展，人们生活水平提高的同时，环境污染及能源短缺问题成为人类可持续发展面临的严峻挑战。光催化技术通过利用太阳能来降解污染物，在其高效、节能和清洁的同时，又能降解并矿化许多结构稳定的污染物，无二次污染等优势成为当今最具发展前景的治理环境污染的技术之一。近些年，人们发现，铋在作为绿色元素且储量丰富的前提下，具有很高的研究价值。铋独特的6S2外层电子构型，使其具有窄的禁带宽度，容易被可见光激发。更引人注意的是，由铋扩展出的一系列铋基化合物，在对难降解有机物具有良好的催化作用，而且铋系化合物在反应过程中具有较高的稳定性。在现有的光催化材料中，复合型光催化材料因其通过组合不同电子结构的半导体材料并调整其光生载流子迁移。通过异质结的构建，有效提高光生电子空穴对分离效率，促进更多的电子空穴对参与光催化反应，提高其氧化还原能力。构建异质结的方法通常包括水热法、溶剂热法、沉积法和离子交换法等。如2011年Cheng等以BiOBr为基质材料和AgNO3进行离子交换，先得到AgBr，再将生成的AgBr部分光还原成Ag，制备了异质结结构的Ag/AgBr/BiOBr光催化剂，所得光催化剂具有优良的可见光降解有机染料和生物灭菌性能(Chem.Commun.，47(2011)7054-7056)。再如2017年Gupta等，同样以BiOBr为基质材料，通过与硝酸银作用，采用沉积法，再经高温煅烧，合成了可见光催化剂Ag/AgBr/BiOBr，其具有光催化降解制药废水的性能(Mater. Res.Bull，88(2017)148-155)。而本专利则是选用单质铋为基质材料，采用一种特殊的原位氧化还原方法，无需光还原或煅烧，即得到了一种具有高可见光活性的Ag/AgBr/BiOBr/Bi复合型光催化剂。
发明内容
与现有技术相比，本发明结合最新研究进展，提供了一种具有异质结结构复合型光催化剂的制备方法。
本发明的优点：本发明以单质铋为基质材料，不同于常见异质结复合型光催化剂的制备，采用一种原位氧化还原反应法，利用Bi与AgBr发生氧化还原反应，得到了 Ag/AgBr/BiOBr/Bi复合型光催化剂。单质铋不仅提供了反应基质，而且有利于生成的 Ag/AgBr/BiOBr分散，避免生成的异质结团聚，这有效的提高了所得光催化剂的光催化性能。光催化实验结果表明，此法制备的催化剂在模拟太阳光(300W氙灯)下对结晶紫、金橙II、甲基橙、孔雀绿和罗丹明B等在内的多种染料均具有很好的降解活性，且涉及工艺简单，设备要求低，原料价廉易得，适于工业化生产。
附图说明
图1为单质铋和Ag/AgBr/BiOBr/Bi复合型光催化剂的XRD图；
图2为可见光下Bi、P25和Ag/AgBr/BiOBr/Bi复合型光催化剂降解罗丹明B的降解效率图。
具体实施方式
(1)Ag/AgBr/BiOBr/Bi复合型光催化剂的制备
按照摩尔比Ag∶Br＝1∶1的比例，分别配制溴化钠溶液和硝酸银水溶液；称取0.3g的单质铋加入到溴化钠水溶液中，室温搅拌均匀分散后，缓慢滴加制备好的硝酸银水溶液，滴加完毕后，继续搅拌60～90min，控制Ag/Bi摩尔比为0.5～1；最后，产物用去离子水和乙醇洗涤，过滤，恒温干燥箱中60℃烘干，得到Ag/AgBr/BiOBr/Bi复合型光催化剂；所得催化剂的XRD见附图1。
(2)Ag/AgBr/BiOBr/Bi复合型光催化剂可见光催化降解有机染料实验
通过在可见光下，Ag/AgBr/BiOBr/Bi复合型光催化剂降解各种有机染料来评价其光催化性能。具体实施如下：
称取0.1g光催化剂，将其在搅拌条件下，分散于100ml所选染料溶液(10mg/L)中，随后置于暗室30min，使其达到吸附-脱附平衡。将达到吸附-脱附平衡后的溶液置于300W氙灯下(滤去紫外光)，每隔5min取一次反应液，反应液通过离心机分离后取上层清液。离心液经由紫外-可见分光光度计检测，并观测最大吸收峰值强度的变化来推测染料降解的浓度变化。结果表明，本发明所制备的光催化剂，对所选染料：罗丹明B、结晶紫、金橙II、甲基橙和孔雀绿均有很好的降解性能，均能在5～30min内降解率达98％以上，且较商用P25有了明显的提高(见附图2)。经离心分离，回收催化剂，再直接加入100mL浓度为10mg/L的罗丹明B水溶液，继续进行光照降解污染试验，催化剂可循环使用4次以上，表明 Ag/AgBr/BiOBr/Bi复合型光催化剂的稳定性良好。
Claims (3)
1.一种Ag/AgBr/BiOBr/Bi复合型光催化剂的制备方法，其特征在于，以单质铋为基质材料，采用一种原位氧化还原反应法，利用Bi与AgBr发生氧化还原反应，得到Ag/AgBr/BiOBr/Bi复合型光催化剂。
2.根据权利要求1所述的Ag/AgBr/BiOBr/Bi复合型光催化剂的制备方法，其制备特征包括以下步骤：
按照摩尔比Ag∶Br＝1∶1的比例，分别配制溴化钠溶液和硝酸银水溶液；将一定量的单质铋加入到溴化钠水溶液中，室温搅拌均匀分散后，缓慢滴加制备好的硝酸银水溶液，滴加完毕后，继续搅拌60～90min，其中Ag/Bi摩尔比为0.5～1；最后，产物用去离子水和乙醇洗涤，过滤，恒温干燥箱中60℃烘干，得到Ag/AgBr/BiOBr/Bi复合型光催化剂。
3.根据权利要求书所述的Ag/AgBr/BiOBr/Bi复合型光催化剂的制备方法，其特征在于，Ag/AgBr/BiOBr/Bi复合型光催化剂在可见光下，可催化降解的有机染料包括罗丹明B、结晶紫、金橙II、甲基橙和孔雀绿或者与前述染料分子具有相同生色团的有机染料。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115463674A (zh) * | 2022-09-14 | 2022-12-13 | 哈尔滨理工大学 | 一种部分出现氧空位的溴氧化铋的制备方法 |
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| US20150174567A1 (en) * | 2013-12-20 | 2015-06-25 | Massachusetts Institute Of Technology | Hybrid photocatalyst for wastewater remediation |
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| Title |
|---|
| LIQUN YE ET AL.: "Two Different Roles of Metallic Ag on Ag/AgX/BiOX (X = Cl, Br) Visible Light Photocatalysts: Surface Plasmon Resonance and Z-Scheme Bridge", 《ACS CATALYSIS》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115463674A (zh) * | 2022-09-14 | 2022-12-13 | 哈尔滨理工大学 | 一种部分出现氧空位的溴氧化铋的制备方法 |
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