CN108328655A - 一种羟基硝酸氧铋及其制备方法和用作光催化剂的用途 - Google Patents
一种羟基硝酸氧铋及其制备方法和用作光催化剂的用途 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- OSVNMCFQQBBOLQ-UHFFFAOYSA-M O[Bi] Chemical compound O[Bi] OSVNMCFQQBBOLQ-UHFFFAOYSA-M 0.000 title claims abstract description 12
- 229960001482 bismuth subnitrate Drugs 0.000 title claims abstract description 12
- 239000011941 photocatalyst Substances 0.000 title abstract description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000004202 carbamide Substances 0.000 claims abstract description 4
- 239000012153 distilled water Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims description 3
- 230000015556 catabolic process Effects 0.000 abstract description 8
- 238000006731 degradation reaction Methods 0.000 abstract description 8
- 229940043267 rhodamine b Drugs 0.000 abstract description 4
- 230000000694 effects Effects 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 239000000975 dye Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- -1 Hydroxyl nitric acid Oxygen bismuth Chemical compound 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000007281 self degradation Effects 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000701 toxic element Toxicity 0.000 description 1
- 238000005406 washing Methods 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
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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
- B01J27/24—Nitrogen compounds
- B01J27/25—Nitrates
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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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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
本发明公开了一种羟基硝酸氧铋及其制备方法和用作光催化剂的用途，该羟基硝酸氧铋的制备方法包括如下步骤：步骤S1，在蒸馏水中于搅拌条件下加入至尿素、五水合硝酸铋至9g/L、36g/L；步骤S2，将混合液放入水浴锅中90‑110℃搅拌0.25‑0.35h，离心、洗涤、干燥即得。本发明提供了一种[Bi6O6(OH)3](NO3)3·5H2O，以其作为光催化剂时30分钟就可以把罗丹明b降解95％以上，具有良好的应用前景，可用于制备光催化剂。本发明还提供了[Bi6O6(OH)3](NO3)3·5H2O的制备方法，步骤简单、可控，成本低廉，可推广性强。
Description
技术领域
本发明属于化学领域，具体涉及一种[Bi6O6(OH)3](NO3)3·5H2O及其制备方法和用作光催化剂的用途。
背景技术
进入21世纪，人类面临着能源和环境两个非常严峻的问题，特别是有毒且难降解有机污染物(如多环芳烃、多氯联苯、农药、染料等)引起的环境问题，已成为影响人类生存与健康的重大问题。利用半导体氧化物材料在太阳光照射下表面能受激活化的特性，可有效地氧化分解有机污染物。与传统的净化环境处理方法相比，半导体光催化技术拥有反应条件温和、无二次污染、操作简单和降解效果显著等优势。自光催化技术开发以来，研究和应用最多的光催化剂是TiO2。但其产生的光生电子空穴对很容易复合，导致电子和空穴不能及时迁移至表面参与氧化还原反应，从而光转化效率较低。因此寻找性能优异的新型光催化材料以获得具有高效光催化活性的光催化剂非常有意义。含铋系列复合物有着广泛的用途，不仅可以用于医药行业，还可应用于半导体。由于铋元素相对是一种无毒绿色的金属，近年来在光催化剂的制备上，日益取代含铅、锑、镉、汞等有毒元素的化合物。羟基硝酸氧铋作为一种功能材料，在光催化方面有较好的性能。已报道的羟基硝酸氧铋相关专利中，张莉莉等发明的五水合硝酸铋和有机醇反应生成的Bi6O5(OH)3(NO3)5·2H2O(JCPDS 54-0627)(专利号CN200910182646.5)，李志华等发明的Bi2O2(OH)(NO3)(专利号CN201110004735.8)，有滕飞等发明的片状羟基硝酸氧铋光催化剂Bi6O5(OH)3(NO3)5·1.5H2O(专利号CN201510484340.0)。
发明内容
本发明目的是提供一种[Bi6O6(OH)3](NO3)3·5H2O及其制备方法和用作光催化剂的用途。
本发明的上述目的是通过下面的技术方案得以实现的：
一种羟基硝酸氧铋化学式为[Bi6O6(OH)3](NO3)3·5H2O。
上述羟基硝酸氧铋的制备方法，包括如下步骤：
步骤S1，在蒸馏水中于搅拌条件下加入至尿素、五水合硝酸铋至9g/L、36g/L；
步骤S2，将混合液放入水浴锅中90-110℃搅拌0.25-0.35h，离心、洗涤、干燥即得。
优选地，100℃搅拌0.3h。
上述羟基硝酸氧铋用于制备光催化剂的用途。
有益效果：
本发明提供了一种[Bi6O6(OH)3](NO3)3·5H2O，以其作为光催化剂时30分钟就可以把罗丹明b降解95％以上，具有良好的应用前景，可用于制备光催化剂。本发明还提供了[Bi6O6(OH)3](NO3)3·5H2O的制备方法，步骤简单、可控，成本低廉，可推广性强。
附图说明
图1为实施例1制备的[Bi6O6(OH)3](NO3)3·5H2O光催化剂的扫面电子显微镜(SEM)图；由图1可见本发明制备的[Bi6O6(OH)3](NO3)3·5H2O光催化剂为棒状结构
图2为实施例1制备的[Bi6O6(OH)3](NO3)3·5H2O的X射线衍射(XRD)图；由图2可以看出，[Bi6O6(OH)3](NO3)3·5H2O光催化剂是纯相的标准卡(JCPDS：7012-26)，实施例一制备的是[Bi6O6(OH)3](NO3)3·5H2O光催化剂。
图3为测试例1制备的[Bi6O6(OH)3](NO3)3·5H2O光催化剂在降解含有罗丹明b(RhB)染料废水溶液的活性对比图。其中C0为RhB的初始浓度，C为经过可见光照射一段时间后测量的RhB浓度，t为时间；由图3可以看出，[Bi6O6(OH)3](NO3)3·5H2O光催化剂能高效催化降解RhB染料废水溶液，并且活性远高于RhB的自降解性能。
具体实施方式
下面结合附图和实施例具体介绍本发明实质性内容，但并不以此限定本发明的保护范围。
实施例1：
在烧杯中加入100ml蒸馏水后，在搅拌条件下，加入0.9g尿素和3.6g五水合硝酸铋；将混合液放入水浴锅中100摄氏度度搅拌0.3h，离心洗涤、干燥，得样品。其扫面电子显微镜(SEM)图如图1所示，其X射线衍射(XRD)图如图2所示。
测试例：
测试过程如下：
将实施例一制得到的[Bi6O6(OH)3](NO3)3·5H2O光催化剂，降解含有RhB的废水溶液。
称取样品0.1g，分别加入200ml RhB水溶液，其中RhB浓度都10mg/L，先避光搅拌30min，使染料在催化剂表面达到吸附/脱附平衡。然后开启氙灯光源在可见外光照射下进行光催化反应，上清液用分光光度计检测。根据Lambert–Beer定律，有机物特征吸收峰强度的变化，可以定量计算其浓度变化。当吸光物质相同、厚度相同时，可以用吸光度的变化直接表示溶液浓度的变化。因为RhB在554nm处有一个特征吸收峰，所以可以利用吸光度的变化来衡量溶液中RHB的浓度变化。从图上(横坐标：紫外光照射时间；纵坐标：经过紫外光照射一段时间后测量的RhB浓度值与RhB的初始浓度的比值。)可以看出光照30min后，[Bi6O6(OH)3](NO3)3·5H2O光催化剂降解RhB高达95％，与RhB自降解相比，[Bi6O6(OH)3](NO3)3·5H2O光催化剂对RhB具有显著的催化活性(图3)。
综上，本发明提供了一种[Bi6O6(OH)3](NO3)3·5H2O，以其作为光催化剂时30分钟就可以把罗丹明b降解95％以上，具有良好的应用前景，可用于制备光催化剂。本发明还提供了[Bi6O6(OH)3](NO3)3·5H2O的制备方法，步骤简单、可控，成本低廉，可推广性强。
上述实施例的作用在于具体介绍本发明的实质性内容，但本领域技术人员应当知道，不应将本发明的保护范围局限于该具体实施例。
Claims (4)
1.一种羟基硝酸氧铋，其特征在于：化学式为[Bi6O6(OH)3](NO3)3·5H2O。
2.权利要求1所述羟基硝酸氧铋的制备方法，其特征在于，包括如下步骤：
步骤S1，在蒸馏水中于搅拌条件下加入至尿素、五水合硝酸铋至9g/L、36g/L；
步骤S2，将混合液放入水浴锅中90-110℃搅拌0.25-0.35h，离心、洗涤、干燥即得。
3.根据权利要求2所述的制备方法，其特征在于：100℃搅拌0.3h。
4.权利要求1所述羟基硝酸氧铋用于制备光催化剂的用途。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110302826A (zh) * | 2019-06-21 | 2019-10-08 | 长沙学院 | 碱式硝酸铋和碘氧铋复合光催化剂及其制备方法和应用 |
| CN114832850A (zh) * | 2022-03-16 | 2022-08-02 | 武汉轻工大学 | 一种层状羟基硝酸氧铋纳米片及制备方法和应用 |
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| JPH02294354A (ja) * | 1989-05-08 | 1990-12-05 | Toagosei Chem Ind Co Ltd | 半導体封止用エポキシ樹脂組成物 |
| JP2012169041A (ja) * | 2011-02-09 | 2012-09-06 | Toyota Central R&D Labs Inc | 電解質及び固体高分子型燃料電池 |
| CN105056986A (zh) * | 2015-08-10 | 2015-11-18 | 南京信息工程大学 | 一种制备片状羟基硝酸氧铋光催化剂的方法及催化剂用途 |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH02294354A (ja) * | 1989-05-08 | 1990-12-05 | Toagosei Chem Ind Co Ltd | 半導体封止用エポキシ樹脂組成物 |
| JP2012169041A (ja) * | 2011-02-09 | 2012-09-06 | Toyota Central R&D Labs Inc | 電解質及び固体高分子型燃料電池 |
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Non-Patent Citations (1)
| Title |
|---|
| JIAWEI PANG ET.AL: "Two basic bismuth nitrates: [Bi6O6(OH)2](NO3)4 2H2O with superior photodegradation activity for rhodamine B and[Bi6O5(OH)3](NO3)5•3H2O with ultrahigh adsorption capacity for methyl orange,", 《APPLIED SURFACE SCIENCE 》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110302826A (zh) * | 2019-06-21 | 2019-10-08 | 长沙学院 | 碱式硝酸铋和碘氧铋复合光催化剂及其制备方法和应用 |
| CN110302826B (zh) * | 2019-06-21 | 2022-04-15 | 长沙学院 | 碱式硝酸铋和碘氧铋复合光催化剂及其制备方法和应用 |
| CN114832850A (zh) * | 2022-03-16 | 2022-08-02 | 武汉轻工大学 | 一种层状羟基硝酸氧铋纳米片及制备方法和应用 |
| CN114832850B (zh) * | 2022-03-16 | 2023-12-01 | 武汉轻工大学 | 一种层状羟基硝酸氧铋纳米片及制备方法和应用 |
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