CN107469863A - 一种硫掺杂碳酸氧铋催化剂的制备方法 - Google Patents
一种硫掺杂碳酸氧铋催化剂的制备方法 Download PDFInfo
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- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 title claims abstract description 17
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000003054 catalyst Substances 0.000 title claims abstract description 17
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 17
- 239000011593 sulfur Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 238000005516 engineering process Methods 0.000 claims abstract description 12
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical class OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000013019 agitation Methods 0.000 claims abstract description 6
- 238000005119 centrifugation Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 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 claims abstract description 6
- 239000000428 dust Substances 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 239000000376 reactant Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000004042 decolorization Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- YYYARFHFWYKNLF-UHFFFAOYSA-N 4-[(2,4-dimethylphenyl)diazenyl]-3-hydroxynaphthalene-2,7-disulfonic acid Chemical compound CC1=CC(C)=CC=C1N=NC1=C(O)C(S(O)(=O)=O)=CC2=CC(S(O)(=O)=O)=CC=C12 YYYARFHFWYKNLF-UHFFFAOYSA-N 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- GUZOHYPCAAYGEN-UHFFFAOYSA-N carbonic acid;oxobismuth Chemical compound [Bi]=O.OC(O)=O GUZOHYPCAAYGEN-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000005686 electrostatic field Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 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 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000031068 symbiosis, encompassing mutualism through parasitism Effects 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0215—Sulfur-containing compounds
- B01J31/0218—Sulfides
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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
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- 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
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Abstract
本发明公开了一种硫掺杂碳酸氧铋催化剂的制备方法，步骤如下：将5g硝酸铋溶解于100～500mL质量百分浓度为10％～30％的稀硝酸中，在搅拌下逐滴滴入80～160mL浓度为20～150g/L的β‑巯基丙酸，滴加完成后继续搅拌10～20min，将所有反应物一起转移到聚四氟乙烯衬底的水热反应釜中，放入烘箱中在160～180℃下反应18～24h后自然冷却，离心后得到固体物经过去离子水洗涤、干燥，即得到一种硫掺杂碳酸氧铋催化剂。通过硫掺杂得到的催化剂，可分散性良好，催化效果有了较大提高。
Description
技术领域
本发明涉及环境污染控制新材料领域，尤其涉及一种硫掺杂碳酸氧铋催化剂的制备方法。
背景技术
随着科技的发展，来自工农业生产中产生的毒害有机污染物严重威胁着环境和人类的健康，寻求一种新型高效的环境治理技术具有重要的意义。光催化技术因其节能、高效、污染物降解彻底、无二次污染优点，目前已成为一种具有重要应用前景的新兴环境治理技术。近年来，新型高效的可见光光催化剂的研制成为光催化技术中的一个重要研究内容，其中具有表面等离子共振效应的光催化材料，因其独特的表面物理化学性质和高效的可见光光催化性能，成为研究的热点之一。
近年来，铋系半导体材料因其在光照下对难降解污染物具有良好的催化作用而成为新型光催化材料的研究热点之一。其中，碳酸氧铋的结构由于是层与层的交错共生，形成了内静电场，有利于光生电子空穴的分离，减少了电子空穴的复合几率，从而表现出优异的光催化性能。但据报道，未改性的碳酸氧铋禁带宽度在3.1-3.5eV之间，只能被紫外光激发。可利用率较低。
发明内容
本发明的目的是为克服现有技术的不足，提供一种硫掺杂碳酸氧铋催化剂的制备方法。
本发明采用的技术方案是依次包括如下步骤：
将5g硝酸铋溶解于100～500mL质量百分浓度为10％～30％的稀硝酸中，在搅拌下逐滴滴入80～160mL浓度为20～150g/L的β-巯基丙酸，滴加完成后继续搅拌10～20min，将所有反应物一起转移到聚四氟乙烯衬底的水热反应釜中，放入烘箱中在160～180℃下反应18～24h后自然冷却，离心后得到固体物经过去离子水洗涤、干燥，即得到一种硫掺杂碳酸氧铋催化剂。
本发明的优点是：通过硫掺杂得到的催化剂，可分散性良好，催化效果有了较大提高。
具体实施方式
以下进一步提供本发明的3个实施例：
实施例1
将5g硝酸铋溶解于500mL质量百分浓度为30％的稀硝酸中，在搅拌下逐滴滴入160mL浓度为150g/L的β-巯基丙酸，滴加完成后继续搅拌20min，将所有反应物一起转移到聚四氟乙烯衬底的水热反应釜中，放入烘箱中在180℃下反应24h后自然冷却，离心后得到固体物经过去离子水洗涤、干燥，即得到一种硫掺杂碳酸氧铋催化剂。
0.5g硫掺杂碳酸氧铋催化剂加入到100mL浓度为35mg/L的亚甲基蓝废水中，在120W的LED灯照射下，反应70min，脱色率为93.4％。
利用市售的碳酸氧铋，在同样的条件下，去除率仅21.3％。
实施例2
将5g硝酸铋溶解于100mL质量百分浓度为10％的稀硝酸中，在搅拌下逐滴滴入80mL浓度为20g/L的β-巯基丙酸，滴加完成后继续搅拌10min，将所有反应物一起转移到聚四氟乙烯衬底的水热反应釜中，放入烘箱中在160℃下反应18h后自然冷却，离心后得到固体物经过去离子水洗涤、干燥，即得到一种硫掺杂碳酸氧铋催化剂。
0.5g硫掺杂碳酸氧铋催化剂加入到100mL浓度为25mg/L的酸性大红废水中，在120W的LED灯照射下，反应85min，脱色率为94.1％。
实施例3
将5g硝酸铋溶解于200mL质量百分浓度为20％的稀硝酸中，在搅拌下逐滴滴入120mL浓度为130g/L的β-巯基丙酸，滴加完成后继续搅拌20min，将所有反应物一起转移到聚四氟乙烯衬底的水热反应釜中，放入烘箱中在180℃下反应24h后自然冷却，离心后得到固体物经过去离子水洗涤、干燥，即得到一种硫掺杂碳酸氧铋催化剂。
0.5g硫掺杂碳酸氧铋催化剂加入到100mL浓度为25mg/L的罗丹明B废水中，在120W的LED灯照射下，反应85min，脱色率为93.9％。
Claims (1)
1.一种硫掺杂碳酸氧铋催化剂的制备方法，其特征是依次包括如下步骤：
将5g硝酸铋溶解于100～500mL质量百分浓度为10％～30％的稀硝酸中，在搅拌下逐滴滴入80～160mL浓度为20～150g/L的β-巯基丙酸，滴加完成后继续搅拌10～20min，将所有反应物一起转移到聚四氟乙烯衬底的水热反应釜中，放入烘箱中在160～180℃下反应18～24h后自然冷却，离心后得到固体物经过去离子水洗涤、干燥，即得到一种硫掺杂碳酸氧铋催化剂。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109174135A (zh) * | 2018-10-22 | 2019-01-11 | 重庆大学 | 一种硫掺杂钼酸铋纳米片状可见光催化剂的制备方法 |
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| US7335622B2 (en) * | 2001-04-02 | 2008-02-26 | Japan Science And Technology Corporation | Manganese/oxygen compound with arsenic adsorption |
| CN103084195A (zh) * | 2013-02-28 | 2013-05-08 | 重庆工商大学 | (BiO)2CO3纳米片光催化剂的制备方法 |
| CN103769185A (zh) * | 2014-02-11 | 2014-05-07 | 南京信息工程大学 | 一种纳米级正方形片状碳酸氧铋光催化剂的制备方法 |
| CN104971761A (zh) * | 2015-07-01 | 2015-10-14 | 杭州臣工环保科技有限公司 | 一种氮/硫掺杂卤化氧铋可见光催化材料及其制备方法 |
| CN106732684A (zh) * | 2016-12-07 | 2017-05-31 | 西南大学 | 复盐水解法制备高活性卤氧化铋光催化材料 |
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- 2017-09-11 CN CN201710812965.4A patent/CN107469863A/zh active Pending
Patent Citations (5)
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| US7335622B2 (en) * | 2001-04-02 | 2008-02-26 | Japan Science And Technology Corporation | Manganese/oxygen compound with arsenic adsorption |
| CN103084195A (zh) * | 2013-02-28 | 2013-05-08 | 重庆工商大学 | (BiO)2CO3纳米片光催化剂的制备方法 |
| CN103769185A (zh) * | 2014-02-11 | 2014-05-07 | 南京信息工程大学 | 一种纳米级正方形片状碳酸氧铋光催化剂的制备方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109174135A (zh) * | 2018-10-22 | 2019-01-11 | 重庆大学 | 一种硫掺杂钼酸铋纳米片状可见光催化剂的制备方法 |
| CN109174135B (zh) * | 2018-10-22 | 2021-08-10 | 重庆大学 | 一种硫掺杂钼酸铋纳米片状可见光催化剂的制备方法 |
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