CN107126968A - 磷化铁基光催化剂及其合成方法 - Google Patents
磷化铁基光催化剂及其合成方法 Download PDFInfo
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- VAKIVKMUBMZANL-UHFFFAOYSA-N iron phosphide Chemical compound P.[Fe].[Fe].[Fe] VAKIVKMUBMZANL-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 239000011941 photocatalyst Substances 0.000 title claims description 3
- 238000010189 synthetic method Methods 0.000 title description 2
- 239000000463 material Substances 0.000 claims abstract description 21
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 14
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000005855 radiation Effects 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 20
- 239000002243 precursor Substances 0.000 claims description 6
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 claims description 5
- 229910052980 cadmium sulfide Inorganic materials 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 230000003197 catalytic effect Effects 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 150000002505 iron Chemical class 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 238000000354 decomposition reaction Methods 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 claims 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims 1
- 239000010452 phosphate Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- NNLOHLDVJGPUFR-UHFFFAOYSA-L calcium;3,4,5,6-tetrahydroxy-2-oxohexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(=O)C([O-])=O.OCC(O)C(O)C(O)C(=O)C([O-])=O NNLOHLDVJGPUFR-UHFFFAOYSA-L 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 229910000388 diammonium phosphate Inorganic materials 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- 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
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1853—Phosphorus; Compounds thereof with iron group metals or platinum group metals with iron, cobalt or nickel
-
- 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
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
- B01J37/18—Reducing with gases containing free hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/08—Other phosphides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1047—Group VIII metal catalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Catalysts (AREA)
Abstract
本发明涉及一种光催化材料及其制备方法，属于无机光催化材料领域。这种光催化材料包括磷化铁及磷化铁和其它光催化材料的混合物。本发明制备的光催化材料在400到1000nm波长范围内具有光催化活性，能够在可见光或自然光辐射下光催化水分解产生氢气。
Description
技术领域
本发明涉及一种新型光催化材料。
本发明还涉及上述光催化材料的制备方法。
本发明还涉及上述光催化材料的用途。
背景技术
光解水产氢的技术具有节省能源、清洁、无污染而成为新的氢能制备方法。但是寻找优秀的光催化材料仍然是一个巨大的挑战。最近发现硫化物、氮化物、碳化物、磷化物有很高的光解水产氢气能力。尤其是磷化物，对光比较敏感、在酸碱条件下很稳定，具备作为光催化材料的本征属性。而且磷化物可以替代贵金属作为共催化剂，在光辐射下产生氢气，这个专利主要研究的是高活性但是很廉价的磷化铁作为可见光响应的光解水产氢材料。
发明内容
本发明的意义在于提供一种高效稳定的新型光催化材料，这种光催化材料能够被可见光激发，并且有非常好的光催化分解水产生氢气的活性，同时制备过程简便、成本很低。
本发明提供的光催化材料是磷化铁基光催化材料。
本发明提供的磷化铁基光催化材料的制备方法如下：
将一定量的铁盐溶解到一定量的溶剂中，持续搅拌一定时间，再将一定量的磷酸盐加入上述溶液中，保持铁和磷的摩尔比为0.1-10之间。继续搅拌一段时间，然后将此混合溶液水浴蒸干，得到前体。将前体放入管式炉中，通入氢气，升温到500-800℃，还原一定时间获得磷化铁催化剂。
在可见光辐射下光解水产生氢气活性测试具体方法和条件如下：
光催化材料的活性测试是在自制的50mL密封石英反应器中进行的。采用Led灯(λ＞450nm)为辐射光源，反应液为含有一定量的牺牲剂，用来消耗光生空穴。然后加入一定量的磷化铁或磷化铁和其它光催化材料。在持续的搅拌下每隔60min抽取少量反应器中的气体，通过气相色谱确定产生氢气的量。
具体实施方案
实施方案1
将总计0.85g Fe(NO3)3·6H2O和(NH4)2HPO4(Fe∶P摩尔比为1∶1)溶解于80mL去离子水中，搅拌30min，在95℃水浴蒸干，将蒸干的物质磨细，放在坩埚中，以10℃/min的速率升温至500℃，保持4h，获得前体。将前体磨细后装在瓷舟中，以300mL/min的速率通入氢气，1℃/min的速率升温至650℃，保持2h，反应结束后，自然冷却，磷化铁样品保存在真空干燥器中。
实施方案2
将总计1.13mg磷化铁和硫化镉(磷化铁的质量比为1-50％)加入到40mL去离子水中，再加入10mL L-乳酸，然后密封后用循环水泵抽真空30min，在反应管的周围放置10个5WLed灯，溶液在搅拌下产生氢气，产生的氢气用气相色谱分析。
实施方案3
将实施方案1中的Fe∶P摩尔比为1∶1改为1∶0.5，其它条件不变。
实施方案4
将实施方案1中的Fe∶P摩尔比为1∶1改为1∶1.5，其它条件不变。
实施方案5
将实施方案1中的Fe∶P摩尔比为1∶1改为1∶2.5，其它条件不变。
实施方案6
将实施方案1中的Fe∶P摩尔比为1∶1改为1∶2，其它条件不变。
实施方案7
将实施方案1中的Fe∶P摩尔比为1∶1改为1∶3，其它条件不变。
实施方案8
将实施方案1中的Fe∶P摩尔比为1∶1改为1∶4，其它条件不变。
实施方案9
将实施方案1中的Fe∶P摩尔比为1∶1改为0.1∶1，其它条件不变。
实施方案10
将实施方案1中的Fe∶P摩尔比为1∶1改为0.2∶1，其它条件不变。
实施方案11
将实施方案2中的硫化镉变为硫化铋，其它条件不变。
实施方案12
将实施方案1中的硫化镉变为二氧化钛，其它条件不变。
实施方案13
将实施方案1中的硫化镉变为氮化碳，其它条件不变。
本发明不限于以上实施方案。
Claims (3)
1.磷化铁基光催化剂，其特征在于包括如下合成步骤：
一定量的铁盐溶解到一定量的溶剂中，持续搅拌一定时间，再将一定量的磷酸盐加入上述溶液中，保持铁和磷的摩尔比为0.1-10之间；继续搅拌一段时间，然后将此混合溶液水浴蒸干，得到前体；将前体放入管式炉中，通入氢气，升温到一定500-800℃，还原一定时间获得磷化铁催化剂；
2.磷化铁基光催化材料包括磷化铁和硫化镉，磷化铁和二氧化钛，磷化铁和氮化碳的混合物；
3.根据权利要求1和2的光催化材料，其特征在于在可见光的辐射下能够分解水产生氢气。
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107552083A (zh) * | 2017-10-11 | 2018-01-09 | 肇庆市华师大光电产业研究院 | 一种FeP/C3N4复合光催化剂及其制备方法和应用 |
| CN107737604A (zh) * | 2017-11-21 | 2018-02-27 | 宁波科邦华诚技术转移服务有限公司 | 一种纳米级金属磷化物复合光催化剂的制备方法 |
| CN109107597A (zh) * | 2018-08-31 | 2019-01-01 | 华南农业大学 | 一种过渡金属磷化物/g-C3N4复合材料及其制备方法与应用 |
| CN109267094A (zh) * | 2018-10-19 | 2019-01-25 | 温州大学 | 一种杂原子掺杂多孔碳/磷化铁复合材料 |
| CN112619675A (zh) * | 2020-12-09 | 2021-04-09 | 中山大学 | 复合压电催化剂的制备方法及制备双氧水的方法 |
| CN114957321A (zh) * | 2022-06-08 | 2022-08-30 | 北京建筑材料科学研究总院有限公司 | 一种铁配合物及其制备方法和应用 |
| CN115869973A (zh) * | 2023-01-15 | 2023-03-31 | 陕西科技大学 | 一种Fe-Fe3O4-FeP/g-C3N4光催化剂及其制备方法和应用 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107552083A (zh) * | 2017-10-11 | 2018-01-09 | 肇庆市华师大光电产业研究院 | 一种FeP/C3N4复合光催化剂及其制备方法和应用 |
| CN107737604A (zh) * | 2017-11-21 | 2018-02-27 | 宁波科邦华诚技术转移服务有限公司 | 一种纳米级金属磷化物复合光催化剂的制备方法 |
| CN109107597A (zh) * | 2018-08-31 | 2019-01-01 | 华南农业大学 | 一种过渡金属磷化物/g-C3N4复合材料及其制备方法与应用 |
| CN109267094A (zh) * | 2018-10-19 | 2019-01-25 | 温州大学 | 一种杂原子掺杂多孔碳/磷化铁复合材料 |
| CN112619675A (zh) * | 2020-12-09 | 2021-04-09 | 中山大学 | 复合压电催化剂的制备方法及制备双氧水的方法 |
| CN114957321A (zh) * | 2022-06-08 | 2022-08-30 | 北京建筑材料科学研究总院有限公司 | 一种铁配合物及其制备方法和应用 |
| CN115869973A (zh) * | 2023-01-15 | 2023-03-31 | 陕西科技大学 | 一种Fe-Fe3O4-FeP/g-C3N4光催化剂及其制备方法和应用 |
| CN115869973B (zh) * | 2023-01-15 | 2024-05-28 | 陕西科技大学 | 一种Fe-Fe3O4-FeP/g-C3N4光催化剂及其制备方法和应用 |
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Application publication date: 20170905 |