CN106517119A - Method for preparing nano copper phosphide - Google Patents
Method for preparing nano copper phosphide Download PDFInfo
- Publication number
- CN106517119A CN106517119A CN201610953025.2A CN201610953025A CN106517119A CN 106517119 A CN106517119 A CN 106517119A CN 201610953025 A CN201610953025 A CN 201610953025A CN 106517119 A CN106517119 A CN 106517119A
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- CN
- China
- Prior art keywords
- nanometer
- phosphorized copper
- copper
- nano copper
- phosphorized
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention relates to a method for preparing nano copper phosphide. The method includes the steps that copper sulfate and yellow phosphorus are adopted to be added with ethylene glycol for conducting the liquid reduction reaction process so that nano copper phosphide sol can be prepared; and the microwave heating reaction is adopted and accordingly the nano copper phosphide can be prepared after centrifuging, washing with ethyl alcohol and drying. By the adoption of the method, the nano copper phosphide with the uniform size, good dispersity and the grain size being smaller than 10nm can be obtained, the microwave hydrothermal method is adopted to replace a traditional hydrothermal method to prepare the nano copper phosphide, and the method has the characteristics of being simple in technology, short in production cycle, capable of achieving energy saving and environmental protection, good in safety performance and the like.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, and in particular to the preparation method of a kind of nanometer of phosphorized copper.
Background technology
Nanometer phosphorized copper has excellent conductivity of heat, electric conductivity, surface-active and catalytic performance, in optics, catalysis, micro- electricity
The fields such as son, bio-sensing, antibacterial have huge using value.The nanometer phosphorized copper mealiness of different-shape can be different, such as grain
Footpath is less, the ball shaped nano phosphatization copper powder of narrow particle size distribution has good anti-microbial property and electric conductivity.
The preparation of traditional nanometer phosphorized copper is divided into Physical and chemical method.Physical method can obtain that purity is higher to be received
Rice phosphatization copper powder, but have that production cost is high, investment is big, yield poorly, industrialize difficulty defect, and Physical is set to instrument
It is standby to require higher, producing cost costliness, it is unsuitable for current economic condition and Industry Foundation.Chemical method is prepared by nanometer phosphorized copper
Common method, the method be in dicyandiamide solution or the aqueous solution, by metal ion under the parcel of surfactant with yellow phosphorus also
Original belongs to simple substance into nanometer phosphorized copper, and using the nanometer phosphorized copper stability of the method preparation, favorable dispersibility, but yield is relatively low,
Complex process and it is difficult to control to, industrialized production has certain difficulty.
The content of the invention
The technical problem to be solved in the present invention is to provide the preparation method of a kind of nanometer of phosphorized copper, and the method can be obtained grain
Footpath is evenly distributed, particle diameter less than 10nm nanometer phosphorized copper, and preparation process is simple to operate, is capable of achieving industrialization, mass
Production.
The present invention is achieved by the following technical solutions：
(1) adopting copper sulphate and yellow phosphorus and adding ethylene glycol carries out Liquid reduction reaction process preparation nanometer phosphorized copper for dispersant
Colloidal sol；Reaction temperature is 30 DEG C -45 DEG C；
(2) heating using microwave in confined conditions of nanometer phosphorized copper colloidal sol is reacted, it is first anti-under 250～350W microwave powers
2～2.5min is answered, then 2.5～3min is reacted under 100～150W microwave powers；
(3) by the nanometer phosphorized copper mixed solution in step (2) be placed in supercentrifuge under 1000r/min rotating speeds from
Heart 10min, adds ethanol water to be cleaned, after vacuum drying, obtains the nanometer phosphorized copper of certain particle diameter.
Preferably, in the step (2), the condition of heating using microwave reaction is：First react under 300W microwave powers
2.25min, then 2.75min is reacted under 120W microwave powers.
In the step (3), precipitation adopts ethanol water cyclic washing, such as 3～5 times, to remove unreacted ion and parent
Aqueous tenside.
In the step (3), the condition of drying is：4～6h is vacuum dried at 50～70 DEG C.
Obtained nanometer phosphatization copper powder particle size is less than 10nm.
The present invention has the advantages that：
1. the present invention replaces traditional hydro-thermal method to prepare nanometer phosphorized copper using microwave-hydrothermal method, with process is simple, life
Cycle is short, energy-conserving and environment-protective are produced, the features such as having a safety feature.
2. the nanometer phosphorized copper particle using the method preparation is spherical in shape, uniform in size, good dispersion.
Specific embodiment
The present invention is further illustrated with reference to embodiment.
Embodiment 1
The preparation method of a kind of nanometer of phosphorized copper is realized by procedure below：
(1) adopting copper sulphate and yellow phosphorus and adding ethylene glycol carries out Liquid reduction reaction process preparation nanometer phosphorized copper for dispersant
Colloidal sol；The addition of ethylene glycol is the 3% of tetra chlorauric acid quality；Reaction temperature is 40 DEG C；
(2) a nanometer phosphorized copper colloidal sol stirring 10min is taken, microwave heating treatment (selects the auspicious swan HX- in Beijing under airtight condition
300A computer microwaves ultrasound combinatorial compound instrument is microwave source), 2.25min is reacted under 300W microwave powers first, then it is micro- in 120W
2.75min is reacted under wave power；
(3) reaction is finished and is cooled to room temperature, 10min is centrifuged in being subsequently placed in supercentrifuge under 1000r/min rotating speeds,
Precipitation is washed 3 times using ethanol water, to remove unreacted ion and surfactant, is finally placed in vacuum drying chamber,
5h is dried at a temperature of 60 DEG C, the nanometer phosphatization copper powders of grey black are obtained, the nanometer phosphorized copper particle diameter for obtaining is less than 10nm.
Embodiment 2
The preparation method of a kind of nanometer of phosphorized copper is realized by procedure below：
(1) adopting copper sulphate and yellow phosphorus and adding ethylene glycol carries out Liquid reduction reaction process preparation nanometer phosphorized copper for dispersant
Colloidal sol；The addition of ethylene glycol is the 3% of tetra chlorauric acid quality；Reaction temperature is 30 DEG C；
(2) a nanometer phosphorized copper colloidal sol stirring 10min is taken, microwave heating treatment (selects the auspicious swan HX- in Beijing under airtight condition
300A computer microwaves ultrasound combinatorial compound instrument is microwave source), 2.5min is reacted under 250W microwave powers first, then in 150W microwaves
2.5min is reacted under power, reaction is finished and is cooled to room temperature, be centrifuged under 1000r/min rotating speeds in being subsequently placed in supercentrifuge
10min, precipitation are washed 3 times using ethanol water, to remove unreacted ion and surfactant, are finally placed in vacuum drying
In case, 6h being dried at a temperature of 50 DEG C, obtaining the nanometer phosphatization copper powders of grey black, the nanometer phosphorized copper particle diameter for obtaining is less than
10nm。
Although above-mentioned be described to the specific embodiment of the present invention in conjunction with the embodiments, not to present invention protection
The restriction of scope, one of ordinary skill in the art should be understood that on the basis of technical scheme, those skilled in the art
The various modifications made by creative work need not be paid or deformation are still within protection scope of the present invention.
Claims (3)
1. the preparation method of a kind of nanometer of phosphorized copper, is characterized in that, step is as follows：
(1) copper sulphate and yellow phosphorus are adopted and is added ethylene glycol and is carried out for dispersant Liquid reduction reaction process to prepare nanometer phosphorized copper molten
Glue；Reaction temperature is 30 DEG C -45 DEG C；
(2) heating using microwave in confined conditions of nanometer phosphorized copper colloidal sol is reacted, first 2 are reacted under 250～350W microwave powers
～2.5min, then 2.5～3min is reacted under 100～150W microwave powers；
(3) the nanometer phosphorized copper mixed solution in step (2) is placed in supercentrifuge and is centrifuged under 1000r/min rotating speeds
10min, adds ethanol water to be cleaned, after vacuum drying, obtains the nanometer phosphorized copper of certain particle diameter.
2. the preparation method of a kind of nanometer of phosphorized copper according to claim 1, is characterized in that：Drying in the step (2)
Condition be：4～6h is vacuum dried at 50～70 DEG C.
3. the preparation method of a kind of nanometer of phosphorized copper according to claim 1, is characterized in that：Obtained nanometer phosphorized copper
Particle size is less than 10nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610953025.2A CN106517119A (en) | 2016-11-03 | 2016-11-03 | Method for preparing nano copper phosphide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610953025.2A CN106517119A (en) | 2016-11-03 | 2016-11-03 | Method for preparing nano copper phosphide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106517119A true CN106517119A (en) | 2017-03-22 |
Family
ID=58326696
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610953025.2A Pending CN106517119A (en) | 2016-11-03 | 2016-11-03 | Method for preparing nano copper phosphide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106517119A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110586954A (en) * | 2019-09-05 | 2019-12-20 | 厦门大学 | Preparation method of copper nanoparticles and copper nanoparticles |
-
2016
- 2016-11-03 CN CN201610953025.2A patent/CN106517119A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110586954A (en) * | 2019-09-05 | 2019-12-20 | 厦门大学 | Preparation method of copper nanoparticles and copper nanoparticles |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170322 |
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| WD01 | Invention patent application deemed withdrawn after publication |