CN107115878A - 磷化钯光解水材料及其制备方法 - Google Patents
磷化钯光解水材料及其制备方法 Download PDFInfo
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- CN107115878A CN107115878A CN201710462384.2A CN201710462384A CN107115878A CN 107115878 A CN107115878 A CN 107115878A CN 201710462384 A CN201710462384 A CN 201710462384A CN 107115878 A CN107115878 A CN 107115878A
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000000463 material Substances 0.000 title claims abstract description 23
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 230000001699 photocatalysis Effects 0.000 title abstract description 9
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000005855 radiation Effects 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract 2
- 239000002243 precursor Substances 0.000 claims description 6
- UQMZPFKLYHOJDL-UHFFFAOYSA-N zinc;cadmium(2+);disulfide Chemical compound [S-2].[S-2].[Zn+2].[Cd+2] UQMZPFKLYHOJDL-UHFFFAOYSA-N 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 claims description 2
- 239000007789 gas 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
- 239000007788 liquid Substances 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 229910003445 palladium oxide Inorganic materials 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
- 238000003786 synthesis reaction Methods 0.000 claims 1
- 238000005516 engineering process Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 101150003085 Pdcl gene Proteins 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
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011109 contamination Methods 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
- 238000006303 photolysis reaction Methods 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
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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
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1856—Phosphorus; Compounds thereof with iron group metals or platinum group metals with platinum group metals
-
- 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
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- 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
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- 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
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/025—Processes for making hydrogen or synthesis gas containing a partial oxidation step
- C01B2203/0261—Processes for making hydrogen or synthesis gas containing a partial oxidation step containing a catalytic partial oxidation step [CPO]
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- 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
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- 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
- C01B2203/1076—Copper or zinc-based catalysts
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- 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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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钯及磷化钯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
光解水产氢技术是利用光催化剂分解水产生氢气的技术。该技术具有节省能源、清洁、无污染的特点，近几年已经成为新的氢能制备方法。目前需要开发新的光催化剂，提高产氢活性和稳定性是亟待解决的关键科学问题。因此，寻找优秀的光催化材料仍然是一个巨大的挑战。磷化钯具有很好的稳定性，催化性能也十分优秀。本专利就是解决如何合成高效稳定的磷化钯光解水催化材料。
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钯光催化材料。
本发明提供的磷化钯光催化材料的制备方法如下：
将一定量的氯化钯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，保持钯和磷的摩尔比为0.1-10之间。继续搅拌一段时间，然后将此混合溶液经水浴蒸干，得到前体。前体焙烧后放入管式炉中，通入氢气，升温到500-900℃，还原一定时间获得磷化钯光催化剂。
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钯或磷化钯和其它光催化材料。在持续地搅拌下每隔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0.75g PdCl2和(NH4)2HPO4(Pd∶P摩尔比为1∶1)溶解于60mL去离子水中，搅拌10min，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3h，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750℃，保持3h，反应结束后，自然冷却，磷化钯样品保存在真空干燥器中。
实施方案2
将总计1.13mg磷化钯和硫化锌镉(磷化钯的质量比为1-50％)加入到40mL去离子水中，再加入10mL L-乳酸作为牺牲剂，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5W Led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Pd∶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Pd∶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Pd∶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Pd∶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2中的硫化锌镉变为硫化铋，其它条件不变。
实施方案8
将实施方案1中的硫化锌镉变为二氧化钛，其它条件不变。
实施方案9
将实施方案1中的硫化锌镉变为氮化碳，其它条件不变。
本发明不限于以上实施方案。
Claims (3)
1.磷化钯光催化材料，其特征在于包括如下合成步骤：
将一定量的氯化钯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，保持钯和磷的摩尔比为0.1-10之间；继续搅拌一段时间，然后将此混合溶液经水浴蒸干，得到前体；前体焙烧后放入管式炉中，通入氢气，升温到500-900℃，还原一定时间获得磷化钯光催化剂。
2.磷化钯光催化材料包括磷化钯和硫化锌镉，磷化钯和二氧化钛，磷化钯和氮化碳的混合物。
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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| CN201710462384.2A CN107115878A (zh) | 2017-06-16 | 2017-06-16 | 磷化钯光解水材料及其制备方法 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110560089A (zh) * | 2019-08-16 | 2019-12-13 | 南京理工大学 | 锌镉硫-铋掺杂埃洛石复合光催化剂及其制备方法 |
| CN113546652A (zh) * | 2020-04-26 | 2021-10-26 | 中国科学院理化技术研究所 | 一种光催化Suzuki偶联反应用催化剂及其制备方法和应用 |
-
2017
- 2017-06-16 CN CN201710462384.2A patent/CN107115878A/zh active Pending
Non-Patent Citations (2)
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|---|
| S. TED OYAMA 等: "The active site of nickel phosphide catalysts for the hydrodesulfurization of 4,6-DMDBT", 《JOURNAL OF CATALYSIS》 * |
| ZIJUN SUN 等: "Enhanced photocatalytic hydrogen production in water under visible light using noble metal-free ferrous phosphide as an active cocatalyst", 《CATALYSIS SCIENCE & TECHNOLOGY》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110560089A (zh) * | 2019-08-16 | 2019-12-13 | 南京理工大学 | 锌镉硫-铋掺杂埃洛石复合光催化剂及其制备方法 |
| CN110560089B (zh) * | 2019-08-16 | 2022-06-28 | 南京理工大学 | 锌镉硫-铋掺杂埃洛石复合光催化剂及其制备方法 |
| CN113546652A (zh) * | 2020-04-26 | 2021-10-26 | 中国科学院理化技术研究所 | 一种光催化Suzuki偶联反应用催化剂及其制备方法和应用 |
| CN113546652B (zh) * | 2020-04-26 | 2023-09-05 | 中国科学院理化技术研究所 | 一种光催化Suzuki偶联反应用催化剂及其制备方法和应用 |
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