CN105836720A - Cross-shaped nickel-cobalt-phosphorus compound and synthesis method of same - Google Patents
Cross-shaped nickel-cobalt-phosphorus compound and synthesis method of same Download PDFInfo
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- CN105836720A CN105836720A CN201610177335.XA CN201610177335A CN105836720A CN 105836720 A CN105836720 A CN 105836720A CN 201610177335 A CN201610177335 A CN 201610177335A CN 105836720 A CN105836720 A CN 105836720A
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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
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/08—Other phosphides
- C01B25/088—Other phosphides containing plural metal
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A cross-shaped nickel-cobalt-phosphorus compound and a synthesis method of the same. The synthesis method includes the steps of: (1) respectively adding a nickel salt water solution, a cobalt salt water solution and a complexing agent into a reaction kettle, fully stirring the mixture, adding a hypophosphite or a phosphite water solution, continuously stirring and mixing the components, sealing the reaction kettle, and increasing the temperature to 150-200 DEG C to perform a reaction; (2) when the reaction is finished, cooling the reaction kettle to room temperature, and centrifugally washing a precipitate for several times with ultrapure water, and finally washing the precipitate with alcohol and vacuum-drying the precipitate to prepare the grey-white cross-shaped nickel-cobalt-phosphorus compound. According to the method, the hypophosphite or the phosphite is employed for simultaneously reducing the nickel and cobalt ions, wherein the ratio of Ni/Co is controlled and the sustained release of the complexing agent is achieved to synthesize the compound. The method is simple and convenient. The compound has a perfect cross-shaped crystal structure, and has special optical, magnetic and electrochemical properties.
Description
Technical field
This patent disclosure relates generally to the synthetic method of metal-powder, be specifically related to a kind of crossed nano
Nickel cobalt phosphorus compound and synthetic method thereof.
Background technology
Nano material has and differs markedly from individual material and the peculiar property of individual molecule, as little
Dimensional effect, skin effect, bulk effect, quantum size effect, macroscopic quantum tunneling are imitated
Should, have in electricity, optics, chemical industry, pottery, biology and medicine and other fields and widely should
With.On nanoscale, material morphology on the impact of its performance clearly, nano-cluster, is received
Rice grain, nano wire, nanometer rods, nanosphere, nanometer film, nano flower, nanotube, nanometer
The material of the various pattern such as cage all shows different features and application.
Nickel phosphorus, nickel cobalt compound have the magnetic of uniqueness, optical, electrical, sensitive and catalytic performance, extensively
General it is applied to corrosion-inhibiting coating, magnetic material, function ceramics, gas sensor, electrode material, urges
The fields such as agent, electrochemical capacitor, photoelectric device, electrochromic material.And, element
Nickel, cobalt have abundant reserves, convenient sources, the batch of low price, beneficially product
Metaplasia is produced.Synthesis crossed nano nickel cobalt phosphorus compound has important using value.
Summary of the invention
The invention aims to obtain the nickel cobalt phosphorus compound of special nature, and provide a kind of
The synthetic method of cross nickel cobalt phosphorus compound, the method is by using hypophosphites in the solution
Reduced nickel ion, cobalt ion simultaneously, thus prepare cross nickel cobalt phosphorus compound, it is special to have
Optics, magnetics and electrochemical properties.
According to the first aspect of the invention, it is provided that the synthesis side of a kind of cross nickel cobalt phosphorus compound
Method, comprises the steps:
(1) in reactor, it is separately added into nickel salt aqueous solution, cobalt saline solution and chelating agent, fills
After dividing stirring, add hypophosphites or phosphite aqueous solution, after continuation stirring mixes, will be anti-
Answer still to be warming up to 150-200 DEG C after sealing to react；
(2), after reaction terminates, it is cooled to room temperature, by many for precipitate ultra-pure water centrifuge washing
Secondary, finally it is vacuum dried with after washing with alcohol, obtains grey black cross nickel cobalt phosphatization and close
Thing.
Specifically, during described nickel salt is selected from nickel sulfate, nickel nitrate, Nickel dichloride. and nickel acetate
Plant or several mixture.
Specifically, described cobalt salt is selected from cobalt nitrate, cobaltous chloride, cobalt acetate, cobaltous sulfate and chlorination
One or more mixture in sub-cobalt.
Specifically, described chelating agent is selected from sodium tartrate, EDTA, aminoacid, polyvinyl alcohol
With one or more mixture in triethylamine.
Specifically, described hypophosphites is sodium hypophosphite.
Under preferable case, described nickel salt, described cobalt salt, described chelating agent and described hypophosphorous acid
Salt or phosphite by the amount proportioning of material be: (2-6): 1:(2-6): (10-20).
Use this optimum ratio, obtained nickel cobalt phosphorus compound cross crystallization perfection.
According to the second aspect of the invention, it is provided that the cross prepared according to above-mentioned synthetic method
Nickel cobalt phosphorus compound.
The synthetic method of the cross nickel cobalt phosphorus compound according to the present invention, utilize hypophosphites or
Phosphite reduced nickel ion and cobalt ion simultaneously, by controlling nickel cobalt ratio and using chelating agent
Slow release, thus synthesis prepares cross nickel cobalt phosphorus compound.Method is simple, convenient, cross
Crystallization perfection, has special optics, magnetic and electrochemical properties.
Accompanying drawing explanation
Fig. 1-4: the scanning electron microscope (SEM) photograph of the cross nickel cobalt phosphorus compound synthesized by the present invention.
Fig. 5: the ultraviolet-visible absorption spectroscopy of the cross nickel cobalt phosphorus compound synthesized by the present invention
Figure.
Fig. 6: the magnetic hysteresis loop of the cross nickel cobalt phosphorus compound synthesized by the present invention.
Fig. 7: the cross nickel cobalt phosphorus compound synthesized by the present invention is in 0.5M sulfuric acid solution
Electrocatalytic hydrogen evolution polarization curve.
Detailed description of the invention
Below by specific embodiment and combine accompanying drawing the present invention is expanded on further, but do not limit
The present invention processed.
Embodiment 1
The synthetic method of a kind of cross nickel cobalt phosphorus compound, specifically includes following steps:
Add 10mL 0.6mM nickel sulfate solution, 10mL 0.6mM wine in a kettle.
Stone acid sodium aqueous solution, the cobalt chloride aqueous solution of 10mL 0.15mM, be sufficiently stirred for half little
Time.Half an hour again it is sufficiently stirred for after adding 30mL 0.8mM sodium hypophosphite aqueous solution.Will
Reactor sealing is put into baking oven 1h and is warming up to 180 DEG C, keeps 24h, naturally cools to room temperature,
40 DEG C of vacuum constant temperatures are put into after 4 last washing with alcohol of precipitate ultra-pure water centrifuge washing
Drying baker is dried 10h, obtains dark gray powder shape cross nickel cobalt phosphorus compound.
Seeing Fig. 1-4, scanning electron microscope is it is observed that above-mentioned products therefrom is perfect cross
Shape.
Seeing Fig. 5, ultraviolet-visible absorption spectroscopy characterizes and finds above-mentioned cross nickel cobalt phosphorus compound
There is in visible region broad absorption characteristic, ultraviolet light is had superabsorbent characteristic.
Seeing Fig. 6, hysteresis curve research shows that above-mentioned cross nickel cobalt phosphorus compound has super suitable
Magnetic.
Seeing Fig. 7, the electrocatalytic hydrogen evolution polarization curve research in 0.5M sulfuric acid solution shows
Cross nickel cobalt phosphorus compound has more preferable electro-catalysis analysis than corresponding nickel phosphorus, cobalt phosphorus compound
Hydrogen performance.
Embodiment 2
The synthetic method of a kind of cross nickel cobalt phosphorus compound, specifically includes following steps:
Add 10mL 0.3mM nickel chloride aqueous solution, 10mL 0.3mM in a kettle.
EDTA aqueous solution, the cobalt nitrate aqueous solution of 10mL 0.15mM, be sufficiently stirred for half an hour.
Half an hour again it is sufficiently stirred for after adding 30mL 0.6mM sodium hypophosphite aqueous solution.Will reaction
Still sealing is put into baking oven 1h and is warming up to 150 DEG C, keeps 24h, naturally cools to room temperature, will be heavy
Put into 40 DEG C of vacuum constant temperatures after 4 the last washing with alcohol of thing ultra-pure water centrifuge washing of shallow lake to be dried
Case is dried 10h, obtains dark gray powder shape cross nickel cobalt phosphorus compound.
Embodiment 3
The synthetic method of a kind of cross nickel cobalt phosphorus compound, specifically includes following steps:
Add 10mL 0.9mM nickel nitrate aqueous solution, 10mL 0.9mM ammonia in a kettle.
Base aqueous acid, the cobalt sulfate solution of 10mL 0.15mM, be sufficiently stirred for half an hour.Add
Half an hour again it is sufficiently stirred for after 30mL 1.0mM sodium phosphite aqueous solution.Reactor is close
Envelope is put into baking oven 1h and is warming up to 180 DEG C, keeps 24h, naturally cools to room temperature, by precipitate
Do with putting into 40 DEG C of vacuum constant temperature drying baker after 4 last washing with alcohol of ultra-pure water centrifuge washing
Dry 10h, obtains dark gray powder shape cross nickel cobalt phosphorus compound.
Embodiment 4
The synthetic method of a kind of cross nickel cobalt phosphorus compound, specifically includes following steps:
Add 10mL 0.8mM nickel acetate aqueous solution in a kettle., 10mL 0.8mM gathers
Vinyl alcohol aqueous solution, the cobalt acetate aqueous solution of 10mL 0.15mM, be sufficiently stirred for half an hour.Add
Half an hour again it is sufficiently stirred for after entering 30mL 0.8mM sodium hypophosphite aqueous solution.By reactor
Sealing is put into baking oven 1h and is warming up to 200 DEG C, keeps 24h, naturally cools to room temperature, will precipitation
40 DEG C of vacuum constant temperature drying baker are put into after 4 last washing with alcohol of thing ultra-pure water centrifuge washing
It is dried 10h, obtains dark gray powder shape cross nickel cobalt phosphorus compound.
Foregoing is only the basic explanation under present inventive concept, and according to the technical side of the present invention
Any equivalent transformation that case is made, all should belong to protection scope of the present invention.
Claims (6)
1. a synthetic method for cross nickel cobalt phosphorus compound, comprises the steps:
(1) in reactor, nickel salt aqueous solution, cobalt saline solution and chelating agent it are separately added into,
After being sufficiently stirred for, add hypophosphites or phosphite aqueous solution, after continuing stirring mixing, will
Reactor is warming up to 150-200 DEG C after sealing and reacts；
(2), after reaction terminates, it is cooled to room temperature, by many for precipitate ultra-pure water centrifuge washing
Secondary, finally it is vacuum dried with after washing with alcohol, obtains grey black cross nickel cobalt phosphatization and close
Thing.
Synthetic method the most according to claim 1, described nickel salt is selected from nickel sulfate, nitre
One or more mixture in acid nickel, Nickel dichloride. and nickel acetate.
Synthetic method the most according to claim 1, described cobalt salt is selected from cobalt nitrate, chlorine
Change one or more mixture in cobalt, cobalt acetate, cobaltous sulfate and cobalt chloride.
Synthetic method the most according to claim 1, described chelating agent is selected from tartaric acid
One or more mixture in sodium, EDTA, aminoacid, polyvinyl alcohol and triethylamine.
Synthetic method the most according to claim 1, described hypophosphites is hypophosphorous acid
Sodium.
6. the cross nickel prepared according to the arbitrary described synthetic method of claim 1-5
Cobalt phosphorus compound.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610177335.XA CN105836720B (en) | 2016-03-25 | 2016-03-25 | A kind of cross nickel cobalt phosphorus compound and its synthetic method |
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| CN201610177335.XA CN105836720B (en) | 2016-03-25 | 2016-03-25 | A kind of cross nickel cobalt phosphorus compound and its synthetic method |
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| CN105836720B CN105836720B (en) | 2017-08-25 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108543541A (en) * | 2018-03-12 | 2018-09-18 | 华南理工大学 | A kind of nickel cobalt phosphorus/amino carbon nano-tube catalyst and its preparation method and application |
| CN108573818A (en) * | 2018-04-18 | 2018-09-25 | 安阳师范学院 | Natrium doping " bowknot " shape pyrophosphoric acid nickel-cobalt combination electrode material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006339104A (en) * | 2005-06-06 | 2006-12-14 | Toyota Central Res & Dev Lab Inc | Active material for lithium secondary battery, and its manufacturing method as well as the lithium secondary battery |
| CN103962162A (en) * | 2014-05-06 | 2014-08-06 | 安徽理工大学 | Micro-nanometer composite, preparing method and application thereof |
| CN104743533A (en) * | 2015-03-23 | 2015-07-01 | 陕西科技大学 | Preparation method for NiCoP nano material |
| CN105152149A (en) * | 2015-07-09 | 2015-12-16 | 中国科学技术大学 | Nickel-cobalt-phosphorus crystal, and preparation method and application thereof |
-
2016
- 2016-03-25 CN CN201610177335.XA patent/CN105836720B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006339104A (en) * | 2005-06-06 | 2006-12-14 | Toyota Central Res & Dev Lab Inc | Active material for lithium secondary battery, and its manufacturing method as well as the lithium secondary battery |
| CN103962162A (en) * | 2014-05-06 | 2014-08-06 | 安徽理工大学 | Micro-nanometer composite, preparing method and application thereof |
| CN104743533A (en) * | 2015-03-23 | 2015-07-01 | 陕西科技大学 | Preparation method for NiCoP nano material |
| CN105152149A (en) * | 2015-07-09 | 2015-12-16 | 中国科学技术大学 | Nickel-cobalt-phosphorus crystal, and preparation method and application thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108543541A (en) * | 2018-03-12 | 2018-09-18 | 华南理工大学 | A kind of nickel cobalt phosphorus/amino carbon nano-tube catalyst and its preparation method and application |
| CN108543541B (en) * | 2018-03-12 | 2021-01-19 | 华南理工大学 | Nickel-cobalt-phosphorus/amino carbon nanotube catalyst and preparation method and application thereof |
| CN108573818A (en) * | 2018-04-18 | 2018-09-25 | 安阳师范学院 | Natrium doping " bowknot " shape pyrophosphoric acid nickel-cobalt combination electrode material and preparation method thereof |
| CN108573818B (en) * | 2018-04-18 | 2019-12-06 | 安阳师范学院 | Sodium-doped bowtie-shaped nickel pyrophosphate-cobalt composite electrode material and preparation method thereof |
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