CN103191778A - Preparation method of metal organic framework loaded Pt-base catalyst - Google Patents
Preparation method of metal organic framework loaded Pt-base catalyst Download PDFInfo
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- CN103191778A CN103191778A CN2013100630590A CN201310063059A CN103191778A CN 103191778 A CN103191778 A CN 103191778A CN 2013100630590 A CN2013100630590 A CN 2013100630590A CN 201310063059 A CN201310063059 A CN 201310063059A CN 103191778 A CN103191778 A CN 103191778A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000012621 metal-organic framework Substances 0.000 title abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000006185 dispersion Substances 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract 2
- 238000001291 vacuum drying Methods 0.000 claims abstract 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 8
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 5
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 4
- 235000019253 formic acid Nutrition 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052711 selenium Inorganic materials 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 239000013384 organic framework Substances 0.000 claims 9
- 230000001476 alcoholic effect Effects 0.000 claims 2
- 235000011187 glycerol Nutrition 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 230000010355 oscillation Effects 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract description 14
- 239000011865 Pt-based catalyst Substances 0.000 abstract description 9
- 239000011943 nanocatalyst Substances 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 5
- 238000003756 stirring Methods 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract 3
- 229910000428 cobalt oxide Inorganic materials 0.000 abstract 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- -1 NaBH 4 Substances 0.000 description 1
- 239000004280 Sodium formate Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 239000008098 formaldehyde solution Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 1
- 235000019254 sodium formate Nutrition 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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Abstract
本发明公开了一种金属有机骨架负载的Pt基催化剂的制备方法，将金属有机骨架加入醇溶液中，超声振荡，然后滴加氯铂酸和氧化钴混合溶液，再加入NaOH，搅拌后，置于微波炉中间歇加热，冷却抽滤，真空烘干，得到金属有机骨架负载的Pt基纳米催化剂。本发明催化剂颗粒小、不易团聚，分散性好、电化学催化活性高。The invention discloses a preparation method of a metal-organic framework-supported Pt-based catalyst. The metal-organic framework is added into an alcohol solution, ultrasonically oscillated, and then a mixed solution of chloroplatinic acid and cobalt oxide is added dropwise, and then NaOH is added. After stirring, the Heating intermittently in a microwave oven, cooling, suction filtering, and vacuum drying to obtain a Pt-based nanocatalyst supported by a metal-organic framework. The catalyst of the invention has small particles, is not easy to agglomerate, has good dispersion and high electrochemical catalytic activity.
Description
技术领域 technical field
本发明涉及一种金属有机骨架负载Pt催化剂的制备方法。 The invention relates to a preparation method of a Pt catalyst supported by a metal organic framework. the
背景技术 Background technique
目前在燃料电池和锂空气电池中常用的氧气还原催化剂是碳负载Pt基催化剂，但是由于Pt资源短缺，价格昂贵，必须采取合适的制备方法和工艺条件，提高Pt的分散性，减少Pt颗粒大小，减少Pt在催化剂中的负载量，降低催化剂的成本。目前制备单元和多元催化剂的方法很多，如，浸渍一液相还原法：将Pt的前驱体溶解后，与活性碳载体混合，再加入还原剂，如NaBH4、甲醛溶液、柠檬酸钠、甲酸钠、肼等，使Pt还原、沉积到活性碳上，干燥后，得到Pt/C催化剂。这种方法的优点是方法简便，缺点是制得的催化剂分散性较差，平均粒径较大。但是制备具有高分散性的Pt基催化剂一个较难解决的问题。 Oxygen reduction catalysts commonly used in fuel cells and lithium-air batteries are carbon-supported Pt-based catalysts. However, due to the shortage of Pt resources and high prices, appropriate preparation methods and process conditions must be adopted to improve the dispersion of Pt and reduce the particle size of Pt. , reduce the load of Pt in the catalyst, and reduce the cost of the catalyst. At present, there are many methods for preparing unit and multi-component catalysts, such as impregnation-liquid phase reduction method: dissolve the Pt precursor, mix it with activated carbon carrier, and then add reducing agent, such as NaBH 4 , formaldehyde solution, sodium citrate, sodium formate , hydrazine, etc., to reduce Pt, deposit it on activated carbon, and obtain a Pt/C catalyst after drying. The advantage of this method is that the method is simple, and the disadvantage is that the prepared catalyst has poor dispersion and large average particle size. However, the preparation of Pt-based catalysts with high dispersion is a difficult problem to solve.
发明内容 Contents of the invention
本发明提供了一种金属有机骨架负载的Pt基催化剂的制备方法，制备的催化剂的活性组分高度分散，不易团聚，克服了现有技术缺陷。 The invention provides a method for preparing a Pt-based catalyst supported by a metal-organic framework. The active components of the prepared catalyst are highly dispersed and difficult to agglomerate, thereby overcoming the defects of the prior art. the
一种金属有机骨架负载的Pt基催化剂的制备方法是按下述步骤进行的： A kind of preparation method of the Pt-based catalyst supported by metal-organic framework is carried out according to the following steps:
将金属有机骨架加入醇溶液中，用超声振荡至形成均匀分散液，然后逐滴滴加氯铂酸和氯化钴混合溶液，搅拌30分钟，然后置于微波炉中间歇加热，冷却抽滤，真空烘干10小时，得到金属有机骨架负载Pt基纳米催化剂。 Add the metal-organic framework into the alcohol solution, vibrate with ultrasound until a uniform dispersion is formed, then add the mixed solution of chloroplatinic acid and cobalt chloride drop by drop, stir for 30 minutes, then heat intermittently in a microwave oven, cool and filter, vacuum After drying for 10 hours, the Pt-based nanocatalyst supported by the metal-organic framework was obtained. the
一种金属有机骨架负载的Pt基催化剂的制备方法，所述Pt元素和Co元素摩尔比为1：1。 A method for preparing a Pt-based catalyst supported by a metal-organic framework, wherein the molar ratio of the Pt element to the Co element is 1:1. the
一种金属有机骨架负载的Pt基催化剂的制备方法，所述金属有机骨架在催化剂中的比例为85-99.5%。 A method for preparing a Pt-based catalyst supported by a metal-organic framework, wherein the proportion of the metal-organic framework in the catalyst is 85-99.5%. the
一种金属有机骨架负载的Pt基催化剂的制备方法，所述的醇为：乙二醇，乙醇和丙三醇。 A method for preparing a Pt-based catalyst supported by a metal-organic framework, wherein the alcohols are: ethylene glycol, ethanol and glycerol. the
一种金属有机骨架负载的Pt基催化剂的制备方法，所述金属有机骨架的金属离子为：V，Cr，Mn，Fe，Co，Ni，Ti，Zr，Mo，Sn，Se，Ca中的一种或两种及以上元素任意比例的混合物。 A method for preparing a Pt-based catalyst supported by a metal-organic framework, the metal ion of the metal-organic framework is one of V, Cr, Mn, Fe, Co, Ni, Ti, Zr, Mo, Sn, Se, and Ca A mixture of one or two or more elements in any proportion. the
本发明提供一种简单快速的制备方法，应用微波调控技术和还原性能较温和的还原剂，将催化剂的活性成分快速均匀地还原到载体的表面。本发明方法制备得到的催化剂颗粒小、不易团聚，分布均匀、电化学催化活性高。本发明采用微波加热、还原剂和分散剂的选择将产品颗粒大小控制在1.5～l0nm之间。本发明适合制备金属有机骨架载一元和多元纳米金属材料电催化剂，可用于醇类燃料电池，锂空气电池和电化学传感器电极的高分散的纳米催化。 The invention provides a simple and fast preparation method, which uses microwave control technology and a reducing agent with mild reducing performance to quickly and uniformly reduce the active components of the catalyst to the surface of the carrier. The catalyst particles prepared by the method of the invention are small, difficult to agglomerate, evenly distributed and high in electrochemical catalytic activity. The invention adopts microwave heating, selection of reducing agent and dispersing agent to control product particle size between 1.5-10nm. The invention is suitable for the preparation of metal-organic framework-loaded single-element and multi-element nano-metal material electrocatalysts, and can be used for highly dispersed nano-catalysis of alcohol fuel cells, lithium-air batteries and electrochemical sensor electrodes. the
具体实施方式 Detailed ways
实施例1 Example 1
将1g金属有机骨架（中心离子为Co，比表面积为534.3m2/g）加入20mL乙二醇中，用超声振荡至形成均匀分散液，然后逐滴滴加2mL含有0.01M氯铂酸和0.01M氯化钴混合溶液，再加入甲酸在25℃条件下搅拌30分钟，然后置于微波炉中在1000W功率下加热10s间歇50s的方式加热10min，冷却抽滤，真空烘干10小时，得到金属有机骨架负载Pt基纳米催化剂，用于锂空气电池的充放电效率为89.7%。 Add 1g of metal-organic framework (the central ion is Co, specific surface area is 534.3m 2 /g) into 20mL of ethylene glycol, vibrate with ultrasonic to form a uniform dispersion, then add 2mL containing 0.01M chloroplatinic acid and 0.01 M cobalt chloride mixed solution, then added formic acid and stirred at 25°C for 30 minutes, then placed in a microwave oven and heated for 10s at 1000W with intermittent 50s for 10 minutes, cooled and filtered, and vacuum dried for 10 hours to obtain metal organic Skeleton-loaded Pt-based nanocatalysts for lithium-air batteries have a charge-discharge efficiency of 89.7%.
实施例2 Example 2
将0.5g金属有机骨架（中心离子为Mn，比表面积为3981.2m2/g）加入20mL乙二醇中，用超声振荡 至形成均匀分散液，然后逐滴滴加5mL含有0.2M氯铂酸和0.2M氯化钴混合溶液，再加入甲酸在25℃条件下搅拌30分钟，然后置于微波炉中在700W功率下加热10s间歇50s的方式加热10min，冷却抽滤，真空烘干10小时，制备得到金属有机骨架载Pt基纳米催化剂，用于锂空气电池的充放电效率为83.6%。 Add 0.5g metal-organic framework (the central ion is Mn, the specific surface area is 3981.2m 2 /g) into 20mL ethylene glycol, vibrate with ultrasonic until a uniform dispersion is formed, then add 5mL containing 0.2M chloroplatinic acid and 0.2M cobalt chloride mixed solution, then add formic acid and stir at 25°C for 30 minutes, then place it in a microwave oven and heat it for 10s at 700W power for 10s with intermittent heating for 10s, cool and filter, and vacuum dry for 10 hours to prepare Metal-organic framework-supported Pt-based nanocatalysts for lithium-air batteries with a charge-discharge efficiency of 83.6%.
实施例3 Example 3
将0.7g金属有机骨架（中心离子为Fe，比表面积为2353.8m2/g）加入20mL乙二醇中，用超声振荡至形成均匀分散液，然后逐滴滴加4mL含有0.2M氯铂酸和0.2M氯化钴混合溶液，再加入甲酸在25℃条件下搅拌30分钟，然后置于微波炉中在1500W功率下加热10s间歇50s的方式加热10min，冷却抽滤，真空烘干10小时，制备得到金属有机骨架载Pt基纳米催化剂，用于锂空气电池的充放电效率为84.1%。 Add 0.7g metal-organic framework (the central ion is Fe, the specific surface area is 2353.8m 2 /g) into 20mL ethylene glycol, vibrate with ultrasonic until a uniform dispersion is formed, then add 4mL containing 0.2M chloroplatinic acid and 0.2M cobalt chloride mixed solution, then add formic acid and stir at 25°C for 30 minutes, then place in a microwave oven and heat for 10s at 1500W power for 10s with intermittent heating for 10s, cool and filter, and vacuum dry for 10 hours to prepare Metal-organic framework-supported Pt-based nanocatalysts for lithium-air batteries with a charge-discharge efficiency of 84.1%.
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Cited By (8)
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| CN105633418A (en) * | 2015-12-25 | 2016-06-01 | 华南理工大学 | Pt/UIO-66 composite material for lithium air battery negative electrode and preparation method for Pt/UIO-66 composite material |
| CN105958085A (en) * | 2016-05-09 | 2016-09-21 | 北京化工大学常州先进材料研究院 | Preparation method for metal-organic-framework-loaded platinum-based catalyst |
| CN106229524A (en) * | 2016-07-19 | 2016-12-14 | 青岛大学 | The preparation method of metallic organic framework cladding PtNi/ ionic liquid/grapheme material |
| CN106582857A (en) * | 2016-12-16 | 2017-04-26 | 昆明理工大学 | Preparation method of metal organic framework for loading nano silver |
| CN109301264A (en) * | 2017-07-24 | 2019-02-01 | 北京大学 | Catalyst for cathode reaction of fuel cell and preparation method thereof |
| CN111359671A (en) * | 2020-03-12 | 2020-07-03 | 长春工业大学 | Preparation method of palladium-loaded or platinum-loaded zirconium-based microporous coordination polymer composite material |
| CN112675913A (en) * | 2019-10-18 | 2021-04-20 | 南京理工大学 | Palladium-loaded titanium-based metal organic framework catalyst, preparation method and application |
| CN115490213A (en) * | 2022-08-30 | 2022-12-20 | 华东师范大学 | Metal organic framework derived VSe 2 Material, preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105633418A (en) * | 2015-12-25 | 2016-06-01 | 华南理工大学 | Pt/UIO-66 composite material for lithium air battery negative electrode and preparation method for Pt/UIO-66 composite material |
| CN105958085A (en) * | 2016-05-09 | 2016-09-21 | 北京化工大学常州先进材料研究院 | Preparation method for metal-organic-framework-loaded platinum-based catalyst |
| CN106229524A (en) * | 2016-07-19 | 2016-12-14 | 青岛大学 | The preparation method of metallic organic framework cladding PtNi/ ionic liquid/grapheme material |
| CN106229524B (en) * | 2016-07-19 | 2018-05-18 | 青岛大学 | The preparation method of metal organic framework cladding PtNi/ ionic liquids/grapheme material |
| CN106582857A (en) * | 2016-12-16 | 2017-04-26 | 昆明理工大学 | Preparation method of metal organic framework for loading nano silver |
| CN109301264A (en) * | 2017-07-24 | 2019-02-01 | 北京大学 | Catalyst for cathode reaction of fuel cell and preparation method thereof |
| CN109301264B (en) * | 2017-07-24 | 2021-10-01 | 北京大学 | Catalyst for cathode reaction of fuel cell and preparation method thereof |
| CN112675913A (en) * | 2019-10-18 | 2021-04-20 | 南京理工大学 | Palladium-loaded titanium-based metal organic framework catalyst, preparation method and application |
| CN111359671A (en) * | 2020-03-12 | 2020-07-03 | 长春工业大学 | Preparation method of palladium-loaded or platinum-loaded zirconium-based microporous coordination polymer composite material |
| CN111359671B (en) * | 2020-03-12 | 2023-01-24 | 长春工业大学 | Preparation method of palladium-loaded or platinum-loaded zirconium-based microporous coordination polymer composite material |
| CN115490213A (en) * | 2022-08-30 | 2022-12-20 | 华东师范大学 | Metal organic framework derived VSe 2 Material, preparation method and application thereof |
| CN115490213B (en) * | 2022-08-30 | 2023-08-18 | 华东师范大学 | VSe derived from metal-organic frameworks 2 Material, preparation method and application thereof |
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Application publication date: 20130710 |