CN103586482A - Method for preparing nanometer nickel under microwave and ultraviolet irradiation - Google Patents
Method for preparing nanometer nickel under microwave and ultraviolet irradiation Download PDFInfo
- Publication number
- CN103586482A CN103586482A CN201310506745.0A CN201310506745A CN103586482A CN 103586482 A CN103586482 A CN 103586482A CN 201310506745 A CN201310506745 A CN 201310506745A CN 103586482 A CN103586482 A CN 103586482A
- Authority
- CN
- China
- Prior art keywords
- ultraviolet irradiation
- reaction liquid
- nickel
- under microwave
- nano
- Prior art date
- 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.)
- Granted
Links
Abstract
The invention relates to a method for preparing nanometer nickel under microwave and ultraviolet irradiation, and belongs to the field of preparation for nanometer materials. The method includes steps of ultrasonically dispersing (5wt%-20wt% of) organic modifiers and oxalic acid nickel for 30 minutes to dissolve the organic modifiers and the oxalic acid nickel in absolute ethyl alcohol; dripping NaOH ethanol solution in reaction mixtures one by one when the temperature of the reaction mixtures is increased and then reaches 60 DEG C, and regulating reaction liquid so that a pH (potential of hydrogen) value of the reaction liquid is 12; dripping 0.04-0.5mol/L of hydrazine hydrate ethanol solution into the reaction liquid one by one under microwave and ultraviolet irradiation, magnetically stirring the reaction liquid, simultaneously heating the reaction liquid until the temperature of the reaction liquid ranges from 80 DEG C to 100 DEG C, and enabling the reaction liquid to react for 30-120 minutes so as to prepare nanometer nickel particles with different sizes. The prepared nanometer nickel particles are cooled until the temperature of the nanometer nickel particles reaches the room temperature, and then the nanometer nickel particles are stored in absolute ethyl alcohol solution. The method has the advantages that the nanometer nickel prepared by the method is small in particle diameter, uniform in size distribution and good in dispersibility; reaction conditions of the method are easy to control, the cost is low, and a manufacturing technology and a process are simple and convenient.
Description
Technical field
The preparation method who the present invention relates to nano nickel under a kind of microwave, ultraviolet irradiation, belongs to field of nano material preparation.
Background technology
Nano metal has at aspects such as catalysis, photochemistry, magnetic, conduction, biologies the physicochemical characteristics that is different from reguline metal material, and the pattern of nano-metal particle directly has influence on these character.The pattern of nano metal is controlled and is synthesized the important directions that belongs to investigation of materials field with application study, utilize surfactant to participate in chemical synthesis, preparation and the application study of carrying out the nano metal of particle size and pattern control have far-reaching theory and using value.The slaine of nickel of take is parent, in the aqueous solution or organic solution, utilizes the organic modifier (as many carboxyls, polyhydroxy organic matter etc.) with different functional groups, at different preparation conditions, carries out the study on the synthesis of the nano nickel that particle size and pattern control.Nano nickel pattern is controlled study on the synthesis and has been disclosed the formation of nano metal crystal face and the relation of preparation condition, and the pattern of nano metal is controlled to the synthetic directive significance that has.
At present, there is the preparation method of many nano nickle granules, as wet-chemical reducing process, microemulsion method and hydrothermal synthesis method.For fear of the oxidation of nano nickle granules, reaction is carried out under organic solvent medium, as oxolane, six decyl amine, ethylene glycol and ethanol, can prepare the nano nickle granules of pure phase.Compare with other organic solvent, ethanol is a kind of being easy to get and green solvent.In addition, conventionally select organic modifier, as: sodium carboxymethylcellulose, sulfonated cis-butadiene rubber, softex kw, tetraethylammonium bromide and TBAB, control size, the pattern of nano particle, induction has generated the nano nickle granules of different size, pattern.At present, utilizing the penetrability of microwave, ultraviolet irradiation, selection heating property is heat source for reaction, selects suitable organic modifier to carry out the synthetic synthetic new direction of nano material that just becoming of the highly concentrated nano metal of pattern, size Control.
Under low-temp reaction condition, utilize microwave, ultraviolet irradiation, we have prepared average grain diameter is that 8-287 nm, Size Distribution are the ball shaped nano nickel particle that 5-363 nm, dispersive property are good.The method reaction condition is easy to control, low cost, the advantage of manufacture craft and simple flow.
Summary of the invention
The present invention proposes a kind of organic modifier that contains different functional groups by interpolation as the template of controlling nano nickel size, at different microwaves, ultraviolet irradiation, under the time, by changing reaction condition parameter, prepare the method for different-grain diameter nano nickel.
Its preparation method is as follows:
By the ultrasonic dispersion of 30 min, organic modifier (5wt%-20wt%) and ethanedioic acid nickel are dissolved in absolute ethyl alcohol.When reactant mixture is warming up to 60 ℃, dropwise drip NaOH (1.0 M, 20 mL) ethanolic solution, regulate reactant liquor pH value to 12.Then, under microwave, ultraviolet irradiation, (microwave power is 500 w; Ultraviolet wavelength is 254 nm, and power is 500 w), dropwise drip 0.04-0.5 mol/L hydrazine hydrate ethanolic solution, under magnetic agitation, be warming up to 80-100 ℃, reaction 30-120 min.The nano nickle granules of preparation is cooled to room temperature and is stored in ethanol solution.
The above-mentioned organic modifier that contains different functional groups refers to two (p-sulfonyl-phenyl) the Phenylphosphine di-potassiums of two hydrations, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane or polyoxyethylene.
Wherein the ratio of organic modifier, ethanedioic acid nickel and absolute ethyl alcohol is (0.006-0.12): (0.12-0.6): 70 (g/g/mL).
Above-mentioned ethanedioic acid nickel is (0.12-0.6) with the ratio of hydrazine hydrate ethanolic solution: 10 g/mL.
The nano nickel of preparing by the method, grain diameter is little, even size distribution, good dispersion, and also the method reaction condition is easy to control, low cost, the advantage of manufacture craft and simple flow.
The specific embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment 1
Weigh the ethanedioic acid nickel of two (p-sulfonyl-phenyl) the Phenylphosphine di-potassiums of 0.015 g bis-hydrations and 0.3 g, 30 min ultrasonic auxiliary under, it is dissolved in 70 mL absolute ethyl alcohols, be then transferred in the three-neck flask of 250 mL.Solution temperature is risen to 60 ℃, dropwise drip NaOH (1.0 M, 20 mL) ethanolic solution, regulate reactant liquor pH value to 12.At microwave irradiation with under stirring, dropwise drip hydrazine hydrate ethanolic solution (0.1 M, 10 mL), be warming up to 80 ℃, react 30 min.After reaction finishes, obtaining average diameter is that 36 nm, Size Distribution are the nano nickle granules of 8 – 59 nm.
Embodiment 2
Weigh the ethanedioic acid nickel of two (p-sulfonyl-phenyl) the Phenylphosphine di-potassiums of 0.07 g bis-hydrations and 0.45 g, 30 min ultrasonic auxiliary under, it is dissolved in 70 mL absolute ethyl alcohols, be then transferred in the three-neck flask of 250 mL.Solution temperature is risen to 60 ℃, dropwise drip NaOH (1.0 M, 20 mL) ethanolic solution, regulate reactant liquor pH value to 12.At microwave irradiation with under stirring, dropwise drip hydrazine hydrate ethanolic solution (0.35 M, 10 mL), be warming up to 80 ℃, react 120 min.After reaction finishes, obtaining average diameter is that 8 nm, Size Distribution are the nano nickle granules of 5 – 41 nm.
Embodiment 3
Weigh the ethanedioic acid nickel of two (p-sulfonyl-phenyl) the Phenylphosphine di-potassiums of 0.05 g bis-hydrations and 0.5 g, 30 min ultrasonic auxiliary under, it is dissolved in 70 mL absolute ethyl alcohols, be then transferred in the three-neck flask of 250 mL.Solution temperature is risen to 60 ℃, dropwise drip NaOH (1.0 M, 20 mL) ethanolic solution, regulate reactant liquor pH value to 12.At microwave irradiation with under stirring, dropwise drip hydrazine hydrate ethanolic solution (0.25 M, 10 mL), be warming up to 80 ℃, react 60 min.After reaction finishes, obtaining average diameter is that 87 nm, Size Distribution are the nano nickle granules of 45 – 103 nm.
Embodiment 4
Weigh the ethanedioic acid nickel of two (p-sulfonyl-phenyl) the Phenylphosphine di-potassiums of 0.03 g bis-hydrations and 0.2 g, 30 min ultrasonic auxiliary under, it is dissolved in 70 mL absolute ethyl alcohols, be then transferred in the three-neck flask of 250 mL.Solution temperature is risen to 60 ℃, dropwise drip NaOH (1.0 M, 20 mL) ethanolic solution, regulate reactant liquor pH value to 12.At microwave irradiation with under stirring, dropwise drip hydrazine hydrate ethanolic solution (0.07 M, 10 mL), be warming up to 80 ℃, react 90 min.After reaction finishes, obtaining average diameter is that 19 nm, Size Distribution are the nano nickle granules of 7 – 46 nm.
Embodiment 5
Weigh the ethanedioic acid nickel of 0.06 g polyoxyethylene and 0.6 g, 30 min ultrasonic auxiliary under, it is dissolved in 70 mL absolute ethyl alcohols, be then transferred in the three-neck flask of 250 mL.Solution temperature is risen to 60 ℃, dropwise drip NaOH (1.0 M, 20 mL) ethanolic solution, regulate reactant liquor pH value to 12.At microwave irradiation with under stirring, dropwise drip hydrazine hydrate ethanolic solution (0.5 M, 10 mL), be warming up to 100 ℃, react 120 min.After reaction finishes, obtaining average diameter is that 69 nm, Size Distribution are the nano nickle granules of 29 – 101 nm.
Embodiment 6
Weigh the ethanedioic acid nickel of 0.12 g γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane and 0.15 g, 30 min ultrasonic auxiliary under, it is dissolved in 70 mL absolute ethyl alcohols, be then transferred in the three-neck flask of 250 mL.Solution temperature is risen to 60 ℃, dropwise drip NaOH (1.0 M, 20 mL) ethanolic solution, regulate reactant liquor pH value to 12.At microwave irradiation with under stirring, dropwise drip hydrazine hydrate ethanolic solution (0.05 M, 10 mL), be warming up to 100 ℃, react 90 min.After reaction finishes, obtaining average diameter is that 43 nm, Size Distribution are the nano nickle granules of 22 – 84 nm.
Embodiment 7
Weigh γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane of 0.016 g and the ethanedioic acid nickel of 0.32 g, 30 min ultrasonic auxiliary under, it is dissolved in 70 mL absolute ethyl alcohols, be then transferred in the three-neck flask of 250 mL.Solution temperature is risen to 60 ℃, dropwise drip NaOH (1.0 M, 20 mL) ethanolic solution, regulate reactant liquor pH value to 12.At microwave irradiation with under stirring, dropwise drip hydrazine hydrate ethanolic solution (0.15 M, 10 mL), be warming up to 90 ℃, react 60 min.After reaction finishes, obtaining average diameter is that 287 nm, Size Distribution are the nano nickle granules of 82 – 363 nm.
Embodiment 8
Weigh the ethanedioic acid nickel of 0.006 g polyoxyethylene and 0.12 g, 30 min ultrasonic auxiliary under, it is dissolved in 70 mL absolute ethyl alcohols, be then transferred in the three-neck flask of 250 mL.Solution temperature is risen to 60 ℃, dropwise drip NaOH (1.0 M, 20 mL) ethanolic solution, regulate reactant liquor pH value to 12.At microwave irradiation with under stirring, dropwise drip hydrazine hydrate ethanolic solution (0.04 M, 10 mL), be warming up to 90 ℃, react 30 min.After reaction finishes, obtaining average diameter is that 72 nm, Size Distribution are the nano nickle granules of 32 – 133 nm.
Claims (4)
1. a preparation method for nano nickel under microwave, ultraviolet irradiation, is characterized in that preparation method is as follows:
By the ultrasonic dispersion of 30 min, the organic modifier of 5wt%-20wt% and ethanedioic acid nickel are dissolved in absolute ethyl alcohol; When reactant mixture is warming up to 60 ℃, dropwise drip 1.0 M, the NaOH ethanolic solution of 20 mL, regulates reactant liquor pH value to 12; Then, at microwave power, be 500 w; Ultraviolet wavelength is 254 nm, and power is under the microwave, ultraviolet irradiation of 500 w, dropwise drips 0.04-0.5 mol/L hydrazine hydrate ethanolic solution, under magnetic agitation, is warming up to 80-100 ℃, reaction 30-120 min; The nano nickle granules of preparation is cooled to room temperature and is stored in ethanol solution.
2. the synthetic method of different-grain diameter nano nickel under microwave according to claim 1, ultraviolet irradiation, it is characterized in that selected organic modifier refers to two (p-sulfonyl-phenyl) the Phenylphosphine di-potassiums of two hydrations, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane or polyoxyethylene.
3. the synthetic method of different-grain diameter nano nickel under microwave according to claim 1, ultraviolet irradiation, is characterized in that wherein the ratio of organic modifier, ethanedioic acid nickel and absolute ethyl alcohol is (0.006-0.12): (0.12-0.6): 70 (g/g/mL).
4. the synthetic method of different-grain diameter nano nickel under microwave according to claim 1, ultraviolet irradiation, is characterized in that wherein ethanedioic acid nickel is (0.12-0.6) with the ratio of hydrazine hydrate ethanolic solution: 10 g/mL.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310506745.0A CN103586482B (en) | 2013-10-25 | 2013-10-25 | The preparation method of nano nickel under a kind of microwave, ultraviolet irradiation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310506745.0A CN103586482B (en) | 2013-10-25 | 2013-10-25 | The preparation method of nano nickel under a kind of microwave, ultraviolet irradiation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103586482A true CN103586482A (en) | 2014-02-19 |
| CN103586482B CN103586482B (en) | 2016-06-15 |
Family
ID=50076918
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310506745.0A Expired - Fee Related CN103586482B (en) | 2013-10-25 | 2013-10-25 | The preparation method of nano nickel under a kind of microwave, ultraviolet irradiation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103586482B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107442134A (en) * | 2017-08-30 | 2017-12-08 | 江苏大学 | A kind of rhodium/nickel alloy nanocatalyst and its preparation method and application |
| CN115582553A (en) * | 2022-10-18 | 2023-01-10 | 德清县浙工大莫干山研究院 | Method for assisting in stimulating growth of silver nanowires through ultraviolet rays |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006336060A (en) * | 2005-06-01 | 2006-12-14 | Sumitomo Metal Mining Co Ltd | Nickel particle powder and production method therefor |
| CN101007357A (en) * | 2007-01-22 | 2007-08-01 | 中山大学 | Nanometer nickel powder and its preparation method |
| CN101147978A (en) * | 2007-10-17 | 2008-03-26 | 江苏大学 | Microwave auxiliary liquid phase reduction method preparing needle-shaped nanometer nickel |
| CN101791704A (en) * | 2010-03-25 | 2010-08-04 | 江苏大学 | Method for preparing nano silver |
| CN102179527A (en) * | 2011-05-10 | 2011-09-14 | 湖南省娄底维亚科技有限公司 | Method for preparing nano nickel powder |
-
2013
- 2013-10-25 CN CN201310506745.0A patent/CN103586482B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006336060A (en) * | 2005-06-01 | 2006-12-14 | Sumitomo Metal Mining Co Ltd | Nickel particle powder and production method therefor |
| CN101007357A (en) * | 2007-01-22 | 2007-08-01 | 中山大学 | Nanometer nickel powder and its preparation method |
| CN101147978A (en) * | 2007-10-17 | 2008-03-26 | 江苏大学 | Microwave auxiliary liquid phase reduction method preparing needle-shaped nanometer nickel |
| CN101791704A (en) * | 2010-03-25 | 2010-08-04 | 江苏大学 | Method for preparing nano silver |
| CN102179527A (en) * | 2011-05-10 | 2011-09-14 | 湖南省娄底维亚科技有限公司 | Method for preparing nano nickel powder |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107442134A (en) * | 2017-08-30 | 2017-12-08 | 江苏大学 | A kind of rhodium/nickel alloy nanocatalyst and its preparation method and application |
| CN115582553A (en) * | 2022-10-18 | 2023-01-10 | 德清县浙工大莫干山研究院 | Method for assisting in stimulating growth of silver nanowires through ultraviolet rays |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103586482B (en) | 2016-06-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105126814B (en) | A kind of CeVO4The preparation method of micron ball photocatalyst | |
| CN104014811B (en) | A kind of octreotide acetate that utilizes is for the method for Template preparation coralloid nano cobalt | |
| CN107662944B (en) | Preparation method of nano zirconia | |
| CN103203232B (en) | High dispersion supported nano noble metal catalyst and preparation method and application thereof | |
| CN105728019A (en) | Application and preparation method of ZSM-5 molecular sieve with mesopores and micropores | |
| CN103817346A (en) | Shape-controlled triangle flaky nano silver powder preparation method | |
| CN104600327B (en) | A kind of preparation method of carbon-supported nano platinum alloy catalyst | |
| CN104190423B (en) | A kind of spherical shape α-Fe2O3Preparation method | |
| CN105964258A (en) | Transition metal nanoparticle catalyst with dual confinement structure as well as application thereof to catalysis of selective hydrogenation reaction of dimethyl terephthalate | |
| CN107651708A (en) | A kind of method that microwave hydrothermal prepares 1T@2H MoS2 | |
| Ruiz-Gómez et al. | Innovative solvo-combustion route for the rapid synthesis of MoO3 and Sm2O3 materials | |
| Yu et al. | Ultrasound-assisted construction of a Z-scheme heterojunction with g-C3N4 nanosheets and flower-like Bi2WO6 microspheres and the photocatalytic activity in the coupling reaction between alcohols and amines under visible light irradiation | |
| CN104415765A (en) | Preparation method of Ru-Ni bimetallic based ordered mesoporous carbon catalyst | |
| CN103586482A (en) | Method for preparing nanometer nickel under microwave and ultraviolet irradiation | |
| CN105800604A (en) | Preparation method of graphene-loaded cobalt ferrite quantum dot | |
| CN105110381A (en) | Method for preparing nanopore alpha-Fe2O3 | |
| CN105502480B (en) | Hydrangea-like strontium titanate nano powder preparation method | |
| CN102974285B (en) | Producing method of magnetic microsphere with hierarchical-pore structure and adjustable uniform grain size | |
| CN104229891B (en) | A kind of method preparing tantalic acid calcium powder body | |
| CN104551002B (en) | Method for preparing quincuncial platinum nanoparticles by taking lanreotide acetate as template | |
| CN103466563A (en) | Method for synthesizing nickel diselenide nanocrystal in polyalcohol-base solution | |
| CN103586054A (en) | Silica-supported lithium phosphate catalyst in eggshell shape, and preparation method and application thereof | |
| CN105439213B (en) | A kind of nano nickel cobalt oxide and preparation method thereof | |
| CN103586485B (en) | A kind of auxiliary method of preparing Nanometer Copper of ultraviolet | |
| CN105565365A (en) | Flower-like zinc oxide crystal preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160615 Termination date: 20161025 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |