CN101857207A - Preparation method and application of transition metal phosphide Co2P - Google Patents
Preparation method and application of transition metal phosphide Co2P Download PDFInfo
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- CN101857207A CN101857207A CN201010193860A CN201010193860A CN101857207A CN 101857207 A CN101857207 A CN 101857207A CN 201010193860 A CN201010193860 A CN 201010193860A CN 201010193860 A CN201010193860 A CN 201010193860A CN 101857207 A CN101857207 A CN 101857207A
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- transition metal
- preparation
- metal phosphide
- hypophosphite
- deionized water
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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
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- 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
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a preparation method of transition metal phosphide Co2P, which includes the following steps that: (1) cobalt salt and hypophosphite as mixing precursors are dissolved in deionized water, and are stirred until the cobalt salt and the hypophosphite are completely dissolved; (2) the produced precursor solution is dried; (3) the dried precursor powder is loaded into a tube furnace, and is calcined under the argon atmosphere; (4) the precursor powder is cooled to the room temperature, the produced product is washed by deionized water and then dried under vacuum, and thereby the transition metal phosphide Co2P is produced. The invention has the following advantages that: the sources of the main materials needed by preparation are rich, the prices are low, and therefore the cost is low; the technique is simple, steps, such as high temperature and high pressure and temperature programming, are not needed, consequently, the preparation flow is simplified, and energy consumption is reduced; in the process of preparation, the environment cannot be polluted, and therefore the invention is suitable for mass production; and when being used for simulating the nickel-metal hydride battery, the prepared product can show good electrochemical invertibility.
Description
[technical field]
The present invention relates to the transition metal phosphide synthetic technology, particularly a kind of transition metal phosphide Co
2The preparation method of P and application.
[background technology]
Transition metal phosphide is as a kind of good catalyzer, is widely used in hydro-desulfurization and dehydrogenation adds nitrogen, and serious day by day energy dilemma and environmental problem have been made huge contribution.Simultaneously, transition metal phosphide is widely used in the plated material owing to having good resistance to corrosion.Some transition metal phosphides are owing to have strong hydrogen adsorption ability, and it is active and caused people's very big interest to show good electrochemical catalysis in the electrochemical oxidation of hydrogen, and the potential value as nickel-hydrogen battery negative pole material is arranged.
The traditional preparation process method of transition metal phosphide comprises: the direct reduction of phosphuret-(t)ed hydrogen or phosphorus pentachloride and cobalt or cobalt salt; Metal organic chemical vapor deposition; Phosphoric acid salt is temperature-programmed reduction method etc. in hydrogen atmosphere.Recently, collosol and gel, methods such as solvent thermal also are used to synthetic phosphide.But, above-mentioned reaction method or temperature of reaction (generally more than 1000 °) that need be higher, or the long crystal of reaction times to obtain, exist raw materials cost height, working condition harshness, complex process, controllable factor less and can't form shortcomings such as batch process, be unfavorable for the widespread production and the application of transition metal phosphide.
[summary of the invention]
The objective of the invention is at above-mentioned existing problems, a kind of transition metal phosphide Co is provided
2The preparation method of P and application, this method technology simply, does not need complicated operations such as High Temperature High Pressure and temperature programming, and cost of material is low, energy consumption is low, preparation cost is low, non-environmental-pollution; The product of preparation is applied to simulate nickel metal hydride battery, shows excellent electrochemical reversibility.
Technical scheme of the present invention:
A kind of transition metal phosphide Co
2The preparation method of P, step is as follows:
1) serves as to mix precursor with cobalt salt and hypophosphite, it is dissolved in the deionized water, be stirred to dissolving fully; 2) gained precursor solution is dried; 3) the precursor powder of oven dry is packed in the tube furnace, under argon atmosphere, calcine; 4) be cooled to room temperature, products therefrom with the laggard capable vacuum-drying of deionized water wash, can be made transition metal phosphide Co
2P.
Described cobalt salt is cobalt oxalate, cobalt chloride, rose vitriol, cobaltous carbonate, cobaltous acetate, cobaltous dihydroxycarbonate or cobaltous hydroxide.
Described hypophosphite is ammonium hypophosphite, potassium hypophosphite, sodium hypophosphite or Hypophosporous Acid, 50.
The mixing quality of described cobalt salt and hypophosphite is than being Co
2+: H
2PO
2 -=1: 1～5, the consumption of deionized water is cobalt salt and hypophosphite total mass 25-40 a times.
The bake out temperature of described precursor solution is (20～100) ℃.
The calcining temperature of described precursor powder is (400～800) ℃, and calcination time is (3～6) hour.
Described deionized water wash is three times, and vacuum-drying is carried out in the electric vacunm drying case, and vacuum tightness is-0.1MPa.
A kind of described transition metal phosphide Co
2The simulation nickel metal hydride battery is made in the application of P.
The present invention has following advantage: prepare required main raw material source and enrich, cheap, cost is lower; Technology is simple, does not need High Temperature High Pressure, and the step that temperature programming etc. are complicated has been simplified preparation flow, has reduced energy consumption; Can not pollute by environment in the preparation process, be fit to scale operation; The product of preparation is applied to simulate nickel metal hydride battery, shows excellent electrochemical reversibility.
[description of drawings]
Fig. 1 is the prepared Co of embodiment 1
2The XRD figure of P.
Fig. 2 is the prepared Co of embodiment 2
2The SEM figure of P.
Fig. 3 is the prepared Co of embodiment 3
2The CV figure of P.
[embodiment]
Embodiment 1:
Take by weighing 0.562g Cobalt monosulfate heptahydrate, 0.332g ammonium hypophosphite (Co
2+: H
2PO
2 -=1: 2), in the deionized water of adding 25ml water it is dissolved fully, stir half an hour down, put into baking oven then to dry at 65 ℃; Precursor powder after the oven dry is put into tube furnace (the Tianjin ring experimental electric furnace ZK-1BS of company limited), under the argon atmospher protection, calcined 6 hours in 550 ℃; Be cooled to room temperature, products therefrom is carried out vacuum-drying with behind the deionized water wash three times in the electric vacunm drying case, vacuum tightness is-0.1MPa to make transition metal phosphide Co
2P.
Fig. 1 is the XRD figure of gained material, adopts Rigaku D/Max Ш type X-ray diffractometer (Cu target k
αRay, wavelength X=0.15418nm).The reference standard card as can be seen, the synthetic material is rhombic system (spacer Pnam 62).
Embodiment 2:
Take by weighing 0.595g cobalt chloride hexahydrate, 0.652g sodium hypophosphite (Co
2+: H
2PO
2 -=1: 2.46), add 30ml water, stir half an hour down, put into baking oven then to dry at 65 ℃; Precursor powder after the oven dry is put into tube furnace (the Tianjin ring experimental electric furnace ZK-1BS of company limited), under the argon atmospher protection, calcined 4 hours in 600 ℃; Be cooled to room temperature, products therefrom is carried out vacuum-drying with behind the deionized water wash three times in the electric vacunm drying case, vacuum tightness is-0.1MPa to make transition metal phosphide Co
2P.
Fig. 2 is prepared Co
2The SEM figure of P.
Embodiment 3:
Take by weighing 0.562g Cobalt monosulfate heptahydrate, 0.326g sodium hypophosphite (Co
2+: H
2PO
2 -=1: 1.54), add 30ml water, stir half an hour down, put into baking oven then to dry at 65 ℃; Precursor powder after the oven dry is put into tube furnace (the Tianjin ring experimental electric furnace ZK-1BS of company limited), under protection of inert gas, calcined 3 hours in 650 ℃; Be cooled to room temperature, products therefrom is carried out vacuum-drying with behind the deionized water wash three times in the electric vacunm drying case, vacuum tightness is-0.1MPa to make transition metal phosphide Co
2P.
Accurately take by weighing Co
2P mixes according to 1: 3 mass ratio with carbonyl Ni powder; Depress to the disk that diameter is 1cm at 30MPa pressure then; Be about two nickel foam clamping wafers of 2cm with diameter, and with the pressure compacting of 20MPa; At last make nickel-hydrogen battery negative pole material, sintered type NiOOH/Ni (OH) at the Bian Shangdian of the nickel foam metallic nickel sheet of burn-oning
2As positive pole, Hg/HgO is that reference electrode is made the simulation nickel metal hydride battery.
Fig. 3 is the cyclic voltammetry curve of prepared simulation nickel metal hydride battery, and probe temperature is a room temperature.As can be seen from the figure: the redox peak area of material is equal substantially, shows excellent electrochemical reversibility.
Claims (8)
1. transition metal phosphide Co
2The preparation method of P is characterized in that step is as follows:
1) serves as to mix precursor with cobalt salt and hypophosphite, it is dissolved in the deionized water, be stirred to dissolving fully; 2) gained precursor solution is dried; 3) the precursor powder of oven dry is packed in the tube furnace, under argon atmosphere, calcine; 4) be cooled to room temperature, products therefrom with the laggard capable vacuum-drying of deionized water wash, can be made transition metal phosphide Co
2P.
2. according to the described transition metal phosphide Co of claim 1
2The preparation method of P is characterized in that: described cobalt salt is cobalt oxalate, cobalt chloride, rose vitriol, cobaltous carbonate, cobaltous acetate, cobaltous dihydroxycarbonate or cobaltous hydroxide.
3. according to the described transition metal phosphide Co of claim 1
2The preparation method of P is characterized in that: described hypophosphite is ammonium hypophosphite, potassium hypophosphite, sodium hypophosphite or Hypophosporous Acid, 50.
4. according to the described transition metal phosphide Co of claim 1
2The preparation method of P is characterized in that: the mixing quality of described cobalt salt and hypophosphite is than being Co
2+: H
2PO
2 -=1: 1～5, the consumption of deionized water is cobalt salt and hypophosphite total mass 25-40 a times.
5. according to the described transition metal phosphide Co of claim 1
2The preparation method of P is characterized in that: the bake out temperature of described precursor solution is (20～100) ℃.
6. according to the described transition metal phosphide Co of claim 1
2The preparation method of P is characterized in that: the calcining temperature of described precursor powder is (400～800) ℃, and calcination time is (3～6) hour.
7. according to the described transition metal phosphide Co of claim 1
2The preparation method of P is characterized in that: described deionized water wash is three times, and vacuum-drying is carried out in the electric vacunm drying case, and vacuum tightness is-0.1MPa.
8. transition metal phosphide Co according to claim 1
2The application of P is characterized in that: make the simulation nickel metal hydride battery.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102173400A (en) * | 2011-03-16 | 2011-09-07 | 天津工业大学 | Method for preparing metal phosphide based on mechanical mixture of dihydrogen phosphate and metal salt |
| CN102607988A (en) * | 2012-03-31 | 2012-07-25 | 苏州大学 | Method for measuring content of impurities in phosphoric acid lithium cobalt |
| CN104118852A (en) * | 2014-08-06 | 2014-10-29 | 济南大学 | Method for preparing transition metal phosphide Co2P |
| CN104445116A (en) * | 2014-11-19 | 2015-03-25 | 中国科学院长春应用化学研究所 | Preparation method of transition metal phosphide with good morphology |
| CN104803365A (en) * | 2015-05-07 | 2015-07-29 | 陕西科技大学 | Preparation method of cobalt phosphide three-dimensional sheet flower |
| CN105016319A (en) * | 2015-08-04 | 2015-11-04 | 中国科学院苏州纳米技术与纳米仿生研究所 | Three-dimensional porous urchin-like cobalt phosphide as well as preparation method and application thereof |
| CN106276830A (en) * | 2015-05-20 | 2017-01-04 | 南开大学 | A kind of preparation method of microwave synthesis metal phosphide |
| CN106672928A (en) * | 2017-01-12 | 2017-05-17 | 南京师范大学 | CoxPy porous nanometer sheet, and synthesis method and application thereof |
| CN108658053A (en) * | 2018-06-28 | 2018-10-16 | 安徽工程大学 | A kind of open structure CoP two-dimensional nano piece preparation methods |
| CN109160501A (en) * | 2018-11-06 | 2019-01-08 | 中山大学 | The method for preparing transition metal phosphide with microwave plasma CVD |
| CN109841422A (en) * | 2019-03-20 | 2019-06-04 | 武汉理工大学 | Co3O4/Co2P coaxial heterogeneous structure material and its preparation method and application |
| CN109967099A (en) * | 2019-03-11 | 2019-07-05 | 浙江大学 | A kind of Co with hollow nanostructures2P@C composite and its preparation method and application |
| CN111266122A (en) * | 2018-12-04 | 2020-06-12 | 中国科学院上海硅酸盐研究所 | Surface modified Co (OH)xNanoparticle CoP nanosheet hydrogen evolution reaction catalyst and preparation method thereof |
| CN115770597A (en) * | 2022-11-22 | 2023-03-10 | 廊坊师范学院 | Metal phosphide catalyst for boron-based hydride dehydrogenation and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101574663A (en) * | 2009-06-11 | 2009-11-11 | 南开大学 | Preparation method of copper phosphide (Cu3P) catalyst with hypophosphite by prosoma pyrolytic process |
-
2010
- 2010-06-08 CN CN201010193860A patent/CN101857207A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101574663A (en) * | 2009-06-11 | 2009-11-11 | 南开大学 | Preparation method of copper phosphide (Cu3P) catalyst with hypophosphite by prosoma pyrolytic process |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102173400A (en) * | 2011-03-16 | 2011-09-07 | 天津工业大学 | Method for preparing metal phosphide based on mechanical mixture of dihydrogen phosphate and metal salt |
| CN102173400B (en) * | 2011-03-16 | 2013-01-30 | 天津工业大学 | Method for preparing metal phosphide based on mechanical mixture of dihydrogen phosphate and metal salt |
| CN102607988A (en) * | 2012-03-31 | 2012-07-25 | 苏州大学 | Method for measuring content of impurities in phosphoric acid lithium cobalt |
| CN104118852A (en) * | 2014-08-06 | 2014-10-29 | 济南大学 | Method for preparing transition metal phosphide Co2P |
| CN104118852B (en) * | 2014-08-06 | 2016-02-03 | 济南大学 | A kind of transition metal phosphide Co 2the preparation method of P |
| CN104445116A (en) * | 2014-11-19 | 2015-03-25 | 中国科学院长春应用化学研究所 | Preparation method of transition metal phosphide with good morphology |
| CN104803365A (en) * | 2015-05-07 | 2015-07-29 | 陕西科技大学 | Preparation method of cobalt phosphide three-dimensional sheet flower |
| CN104803365B (en) * | 2015-05-07 | 2017-01-25 | 陕西科技大学 | Preparation method of cobalt phosphide three-dimensional sheet flower |
| CN106276830A (en) * | 2015-05-20 | 2017-01-04 | 南开大学 | A kind of preparation method of microwave synthesis metal phosphide |
| CN105016319A (en) * | 2015-08-04 | 2015-11-04 | 中国科学院苏州纳米技术与纳米仿生研究所 | Three-dimensional porous urchin-like cobalt phosphide as well as preparation method and application thereof |
| CN106672928A (en) * | 2017-01-12 | 2017-05-17 | 南京师范大学 | CoxPy porous nanometer sheet, and synthesis method and application thereof |
| CN106672928B (en) * | 2017-01-12 | 2019-10-01 | 南京师范大学 | A kind of CoxPyPorous nano-sheet and its synthetic method and application |
| CN108658053A (en) * | 2018-06-28 | 2018-10-16 | 安徽工程大学 | A kind of open structure CoP two-dimensional nano piece preparation methods |
| CN109160501A (en) * | 2018-11-06 | 2019-01-08 | 中山大学 | The method for preparing transition metal phosphide with microwave plasma CVD |
| CN111266122A (en) * | 2018-12-04 | 2020-06-12 | 中国科学院上海硅酸盐研究所 | Surface modified Co (OH)xNanoparticle CoP nanosheet hydrogen evolution reaction catalyst and preparation method thereof |
| CN109967099A (en) * | 2019-03-11 | 2019-07-05 | 浙江大学 | A kind of Co with hollow nanostructures2P@C composite and its preparation method and application |
| CN109841422A (en) * | 2019-03-20 | 2019-06-04 | 武汉理工大学 | Co3O4/Co2P coaxial heterogeneous structure material and its preparation method and application |
| CN115770597A (en) * | 2022-11-22 | 2023-03-10 | 廊坊师范学院 | Metal phosphide catalyst for boron-based hydride dehydrogenation and preparation method thereof |
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Open date: 20101013 |