CN109331846A - 纳米溴化银复合钨酸铋的制备方法及其产品和应用 - Google Patents
纳米溴化银复合钨酸铋的制备方法及其产品和应用 Download PDFInfo
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- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 title claims abstract description 49
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 24
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 24
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 24
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 150000001875 compounds Chemical class 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000011065 in-situ storage Methods 0.000 claims abstract description 11
- 238000005286 illumination Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 230000015556 catabolic process Effects 0.000 claims abstract description 8
- 238000006731 degradation reaction Methods 0.000 claims abstract description 8
- 238000005342 ion exchange Methods 0.000 claims abstract description 6
- 239000002114 nanocomposite Substances 0.000 claims abstract description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- 239000011941 photocatalyst Substances 0.000 claims abstract description 4
- 239000002131 composite material Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- -1 tungstate dihydrate Chemical class 0.000 claims description 7
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 5
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 5
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 5
- 229910052753 mercury Inorganic materials 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 239000004098 Tetracycline Substances 0.000 claims description 3
- 239000000693 micelle Substances 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 229960002180 tetracycline Drugs 0.000 claims description 3
- 229930101283 tetracycline Natural products 0.000 claims description 3
- 235000019364 tetracycline Nutrition 0.000 claims description 3
- 150000003522 tetracyclines Chemical class 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 230000031709 bromination Effects 0.000 abstract description 3
- 238000005893 bromination reaction Methods 0.000 abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000356 contaminant Substances 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229910052709 silver Inorganic materials 0.000 abstract description 2
- 239000004332 silver Substances 0.000 abstract description 2
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 10
- 239000007787 solid Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Natural products CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 239000005447 environmental material Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 229940072172 tetracycline antibiotic Drugs 0.000 description 1
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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
- 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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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/30—Ion-exchange
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
本发明公开了一种纳米溴化银复合钨酸铋（AgBr@Bi2WO6）的制备方法。其特征在于采用水热‑离子交换‑原位复合相结合法，制备异质结AgBr@Bi2WO6纳米复合材料。首先制备高分散的纳米Bi2WO6纳米片球，纳米片的厚度为15nm左右；将其分散到符合化学计量比的溴化钾水溶液中，进行离子交换反应；再将一定量的硝酸银水溶液缓慢滴加到上述溶剂中，通过搅拌使溴化银缓慢均匀的原位生长到钨酸铋薄片表面。然后在光照条件下反应1小时，在溴化银表面形成一种银膜，促进电子传输。最终得到一种具备高稳定性和分散性的高效复合光催化剂，Xe灯下对RhB降解30min后，降解率达到90.7%。所得到的AgBr@Bi2WO6可广泛应用于污染物降解、废水处理、光水解产氢等领域。
Description
技术领域
本发明属于环境材料制备技术领域，具体涉及到一种纳米溴化银复合钨酸铋的制备方法及其产品和应用。
背景技术
四环素类抗生素水溶性较好,经体内代谢大部分以原形排出,最终进入城市的污水处理系统中,而各种污水处理过程对污水中的这些物质不起作用或作用很少最终被排放到环境中,对环境污染构成潜在威胁,它们在环境中不易发生生物降解,因而容易在水环境中储存和蓄积,它们在地表水中已被频繁检出。因此,对环境中四环素的去除显得尤为重要。在众多治理水污染的方法中,光催化技术由于其自身的优点而显得较为突出,利用光催化技术不仅降低处理水污染成本,而且可以有效的将水体中的酚类污染物降解为对环境无害的小分子物质。
Bi2WO6光催化剂由于禁带宽度仅为2.7eV，具备可见光吸收。与此同时，通过水热法合成的Bi2WO6纳米材料易于成片，具有较大的比表面积，利于污染物的吸附。因此，Bi2WO6被认为是具备发展潜力的可见光光催化剂。但由于Bi2WO6光生电子-空穴容易复合，限制了Bi2WO6光催化应用的潜力，因此对Bi2WO6进行改性以改善其光催化性能是亟待解决的问题。AgBr的禁带宽度仅为2.65eV，也是具备可见光响应的半导体光催化材料。另外，由于AgBr材料容易光还原生成Ag纳米颗粒，因此将AgBr与Bi2WO6复合，不仅能够利用异质结结构提高载流子分离效率，同时也能够利用Ag纳米颗粒的等离子共振效应，大幅度提高Bi2WO6对可见光的利用率。所以,在Bi2WO6的基础上加入AgBr，并通过紫外光照条件在AgBr颗粒表面还原出一层Ag，可以有效提升Bi2WO6光催化剂的活性。
发明内容
为克服现有技术的不足，本发明的目的在于提供一种纳米溴化银复合钨酸铋的制备方法。
本发明的再一目的在于：提供一种上述方法制备的纳米溴化银复合钨酸铋产品。
本发明的又一目的在于：提供一种上述产品的应用。
本发明目的通过下述方案实现：一种纳米溴化银复合钨酸铋的制备方法，采用水热-离子交换-原位复合法相结合，制备异质结AgBr@Bi2WO6纳米复合材料，包括以下步骤：
a、在去离子水中加入五水硝酸铋（Bi(NO3)3﹒5H2O）和0.330g二水钨酸钠（Na2WO4﹒2H2O），至所述的五水硝酸铋（Bi(NO3)3﹒5H2O）和0.330g二水钨酸钠（Na2WO4﹒2H2O）摩尔比为2:1~2:2，搅拌60min形成均匀的溶液；
b、将该溶液转移到一个100mL聚四氟乙烯内衬的不锈钢高压釜中，水热合成，得到样品；
c、将得到的样品洗涤，随后在60~80℃真空烘箱中烘干，得到纳米片球Bi2WO6；
d、将得到纳米片球Bi2WO6分散到溴化钾水溶液中，进行离子交换，超声分散后将一定量的硝酸银溶液逐滴加入，搅拌一定时间原位生成溴化银混合溶液；
e、将所得混合溶液放置在紫外灯下，光照一定时间，洗涤干燥，得到纳米AgBr@Bi2WO6。
所述的水热反应温度为120~200℃，反应时间为8~24 h。
所述的紫外光灯为汞灯，光照功率为300W，光照时间为1.5~2.5 h。
所述的纳米片球有多个纳米片组成，纳米片的厚度为15nm。
本发明提供一种纳米溴化银复合钨酸铋，根据上述任一所述方法制备得到。
本发明提供一种纳米溴化银复合钨酸铋在降解四环素中作为复合光催化剂的应用。
本发明通过将溴化银复合到纳米钨酸铋表面的方法，既能使溴化银与钨酸铋形成异质结结构，提高光催化剂的光生电子-空穴对的分离效率，并且通过光照的手段，在溴化银表面还原出一层银单质薄膜，促进电子的转移，不仅使得催化剂的吸附能力和分散性提高，并且能够大幅度提高钨酸铋的光催化活性。Xe灯下对RhB降解30min后，降解率达到90.7%。所得到的AgBr@Bi2WO6可广泛应用于污染物降解、废水处理、光水解产氢等领域。
附图说明
图1为本发明实施例1合成的纳米级AgBr@Bi2WO6的XRD图。
图2为本发明实施例2合成的纳米级AgBr@Bi2WO6的SEM图。
图3为本发明实施例3合成的纳米级AgBr@Bi2WO6对RhB的降解曲线。
具体实施方式
本发明下面通过具体实例进行详细的描述，但是本发明的保护范围不受限于这些实施例子。
实施例1
一种纳米溴化银复合钨酸铋的制备方法，采用水热-离子交换-原位复合法相结合，制备异质结AgBr@Bi2WO6纳米复合材料，包括以下步骤：
a、在80mL的去离子水中加入硝酸，将pH调整到3，加入2mmol的五水硝酸铋（Bi(NO3)3﹒5H2O）和1mmol的二水钨酸钠（Na2WO4﹒2H2O），搅拌1小时形成均匀的溶液；
b、将该溶液转移到一个100mL聚四氟乙烯衬底中不锈钢高压釜中，水热反应在180℃下进行24小时，反应结束后，等待反应釜自然冷却，之后将所得样品取出；
c、将得到的样品用水和乙醇交换洗涤三次，在60℃的真空烘箱中烘干得到纳米片球Bi2WO6固体；
d、将所得固体用玛瑙研钵研磨成细小均匀的粉末，取0.2g粉末将其分散到60mL的溴化钾（0.44g/L）溶液中，进行离子交换，超声分散15分钟,再将60mL的0.628g/L硝酸银溶液缓慢滴加到上述分散液中，搅拌2 h原位生成溴化银混合溶液；
e、将所得混合溶液放置在300 W紫外汞灯下光照1 h，洗涤烘干后得到浅棕色纳米AgBr@Bi2WO6粉末。
合成的纳米AgBr@Bi2WO6的XRD图如图1所示。
实施例2
一种纳米溴化银复合钨酸铋的制备方法，其特征在于，采用水热-离子交换-原位复合法相结合，制备异质结AgBr@Bi2WO6纳米复合材料，包括以下步骤：
a、在80mL中去离子水加入0.1 g的表面活性剂十六烷基三甲基溴化铵（CTAB），搅拌20min形成均匀的混合胶束分散体系；再加入2mmol的五水硝酸铋和1mmol的二水钨酸钠到上述胶束分散体系中，搅拌1小时转n形成均匀的溶液；
b、将该溶液转移到一个100mL聚四氟乙烯内衬的不锈钢高压釜中，水热反应在180℃下进行24小时，反应结束后，等待反应釜自然冷却，之后将所得样品取出；
c、将得到的样品用水和乙醇交换洗涤三次，在60℃的真空烘箱中烘干得到纳米片球Bi2WO6固体；
d、将所得固体用玛瑙研钵研磨成细小均匀的粉末，取0.4g粉末将其分散到100mL的溴化钾（0.44g/L）溶液中，进行离子交换，超声分散15分钟，再将100mL的硝酸银（0.628g/L）溶液缓慢滴加到上诉分散液中，搅拌2 h后原位生成溴化银混合溶液；
e、将所得混合溶液放置在300 W紫外汞灯下光照0.5 h，洗涤烘干后得到浅棕色纳米AgBr@Bi2WO6粉末。
合成的纳米AgBr@Bi2WO6的SEM图如图2所示。
实施例3
一种纳米溴化银复合钨酸铋的制备方法，其特征在于，采用水热-离子交换-原位复合法相结合，制备异质结AgBr@Bi2WO6纳米复合材料，包括以下步骤：
a、在80mL中去离子水加入0.5 g的表面活性剂十六烷基三甲基溴化铵（CTAB），搅拌20min形成均匀的混合胶束分散体系；再加入2mmol的五水硝酸铋和1mmol的二水钨酸钠到上述胶束分散体系中，搅拌1小时形成均匀的溶液；
b、将该溶液转移到一个100mL聚四氟乙烯内衬的不锈钢高压釜中，水热反应在180℃下进行24小时，反应结束后，等待反应釜自然冷却之后，将所得样品取出；
c、将得到的样品用水和乙醇交换洗涤三次，在60℃的真空烘箱中烘干纳米片球Bi2WO6固体。
d、将所得固体用玛瑙研钵研磨成细小均匀的粉末，取0.4g粉末将其分散到100mL的溴化钾（0.44g/L）溶液中，进行离子交换，超声分散15分钟，再将100mL的硝酸银（0.628g/L）溶液缓慢滴加到上述分散液中，搅拌2 h后原位生成溴化银混合溶液；
e、将所得混合溶液放置在300 W紫外汞灯下光照0.5 h，洗涤烘干后得到浅棕色AgBr@Bi2WO6粉末。
取AgBr@Bi2WO6粉末60mg加入80mL RhB（10mg/L）污染物溶液中，在300W Xe灯可见光照下反应，30分钟RhB降解率达到90.7%，浓度变化如图3所示。
Claims (8)
1.一种纳米溴化银复合钨酸铋的制备方法，其特征在于，采用水热-离子交换-原位复合法相结合，制备异质结AgBr@Bi2WO6纳米复合材料，包括以下步骤：
a、在去离子水中加入五水硝酸铋（Bi(NO3)3﹒5H2O）和0.330g二水钨酸钠（Na2WO4﹒2H2O），至所述的五水硝酸铋（Bi(NO3)3﹒5H2O）和0.330g二水钨酸钠（Na2WO4﹒2H2O）摩尔比为2:1~2:2，搅拌60min形成均匀的溶液；
b、将该溶液转移到一个100mL聚四氟乙烯内衬的不锈钢高压釜中，水热合成，得到样品；
c、将得到的样品洗涤，随后在60~80℃真空烘箱中烘干，得到纳米片球Bi2WO6；
d、将得到纳米片球Bi2WO6分散到溴化钾水溶液中，进行离子交换，超声分散后将一定量的硝酸银溶液逐滴加入，搅拌一定时间原位生成溴化银混合溶液；
e、将所得混合溶液放置在紫外灯下，光照一定时间，洗涤干燥，得到纳米AgBr@Bi2WO6。
2.根据权利要求1所述的纳米溴化银复合钨酸铋的制备方法，其特征在于所述的水热反应的反应温度为120~200℃，反应时间为8~24 h。
3.根据权利要求1所述的纳米溴化银复合钨酸铋的制备方法，其特征在于步骤a中用硝酸调节去离子水到pH3。
4.根据权利要求1所述的纳米溴化银复合钨酸铋的制备方法，其特征在于步骤a中在80mL中去离子水加入0.1-0.5 g的表面活性剂十六烷基三甲基溴化铵（CTAB），搅拌形成均匀的混合胶束分散体系。
5.根据权利要求1所述的纳米溴化银复合钨酸铋的制备方法，其特征在于所述的紫外光灯为汞灯，光照功率为300W，光照时间为1.5~2.5 h。
6.根据权利要求1所述的纳米溴化银复合钨酸铋的制备方法，其特征在于所述的纳米片球有多个纳米片组成，纳米片的厚度为15nm。
7.一种纳米溴化银复合钨酸铋，其特征在于根据权利要求1-6任一所述方法制备得到。
8.一种根据权利要求7所述纳米溴化银复合钨酸铋在降解四环素中作为复合光催化剂的应用。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111036243A (zh) * | 2019-12-31 | 2020-04-21 | 福州大学 | 含氧空缺的过渡金属掺杂的BiOBr纳米片光催化剂及其制备方法和应用 |
| CN113769768A (zh) * | 2021-09-08 | 2021-12-10 | 中国科学院海洋研究所 | 一种双功能复合纳米材料及其制备方法和用途 |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102009044926A1 (de) * | 2009-09-23 | 2011-03-31 | Schott Ag | Photokatalysatoreinrichtung |
| CN102489298A (zh) * | 2011-12-15 | 2012-06-13 | 江南大学 | 一种贵金属负载型Bi2WO6可见光催化剂的制备方法 |
| CN102764653A (zh) * | 2011-05-06 | 2012-11-07 | 中国科学院合肥物质科学研究院 | 银修饰的钨酸铋复合光催化剂及其制备方法和用途 |
| CN104117355A (zh) * | 2014-07-14 | 2014-10-29 | 王丹军 | 一种纳米银表面修饰钨酸铋光催化剂及其制备方法 |
| CN106345534A (zh) * | 2016-09-23 | 2017-01-25 | 安徽师范大学 | 一种Bi2WO6/Ag异质纳米结构材料、制备方法及其应用 |
| CN106732683A (zh) * | 2016-12-06 | 2017-05-31 | 江苏大学 | 一种合成等离子体复合光催化剂的方法 |
-
2018
- 2018-11-14 CN CN201811353263.5A patent/CN109331846A/zh active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102009044926A1 (de) * | 2009-09-23 | 2011-03-31 | Schott Ag | Photokatalysatoreinrichtung |
| CN102764653A (zh) * | 2011-05-06 | 2012-11-07 | 中国科学院合肥物质科学研究院 | 银修饰的钨酸铋复合光催化剂及其制备方法和用途 |
| CN102489298A (zh) * | 2011-12-15 | 2012-06-13 | 江南大学 | 一种贵金属负载型Bi2WO6可见光催化剂的制备方法 |
| CN104117355A (zh) * | 2014-07-14 | 2014-10-29 | 王丹军 | 一种纳米银表面修饰钨酸铋光催化剂及其制备方法 |
| CN106345534A (zh) * | 2016-09-23 | 2017-01-25 | 安徽师范大学 | 一种Bi2WO6/Ag异质纳米结构材料、制备方法及其应用 |
| CN106732683A (zh) * | 2016-12-06 | 2017-05-31 | 江苏大学 | 一种合成等离子体复合光催化剂的方法 |
Non-Patent Citations (2)
| Title |
|---|
| PENG ZHANG ET AL.: "Preparation and photocatalytic application of AgBr modified Bi2WO6 nanosheets with high adsorption capacity", 《J. MATER. RES.》 * |
| SHUANGLONG LIN ET AL.: "Nano Ag@AgBr surface-sensitized Bi2WO6 photocatalyst: oil-in-water synthesis and enhanced photocatalytic degradation", 《APPLIED SURFACE SCIENCE》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111036243A (zh) * | 2019-12-31 | 2020-04-21 | 福州大学 | 含氧空缺的过渡金属掺杂的BiOBr纳米片光催化剂及其制备方法和应用 |
| CN111036243B (zh) * | 2019-12-31 | 2021-08-31 | 福州大学 | 含氧空缺的过渡金属掺杂的BiOBr纳米片光催化剂及其制备方法和应用 |
| CN113769768A (zh) * | 2021-09-08 | 2021-12-10 | 中国科学院海洋研究所 | 一种双功能复合纳米材料及其制备方法和用途 |
| CN113769768B (zh) * | 2021-09-08 | 2023-05-26 | 中国科学院海洋研究所 | 一种双功能复合纳米材料及其制备方法和用途 |
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