CN103264167A - Surface modification nanometer copper particle and preparation method thereof - Google Patents
Surface modification nanometer copper particle and preparation method thereof Download PDFInfo
- Publication number
- CN103264167A CN103264167A CN2013102297484A CN201310229748A CN103264167A CN 103264167 A CN103264167 A CN 103264167A CN 2013102297484 A CN2013102297484 A CN 2013102297484A CN 201310229748 A CN201310229748 A CN 201310229748A CN 103264167 A CN103264167 A CN 103264167A
- Authority
- CN
- China
- Prior art keywords
- copper
- preparation
- modified nano
- particulate
- nano copper
- 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.)
- Pending
Links
Abstract
The invention relates to a surface modification nanometer copper particle and a preparation method thereof. The preparation method comprises the following steps of: firstly preparing a copper salt water solution with the concentration of 0.05-0.2 mol/L; adding an ammonia water solution; then sufficiently mixing the copper salt water solution and a mixed solution of a reducing agent, a surface modification agent with anti-emulsification property and an organic solvent to react for 1-3 hours under the condition of alkaline (pH is 8-11); and then concentrating and separating to obtain the surface modification nanometer copper particle. The preparation method has the advantages of simple preparation process, easiness for low-cost raw material obtaining, low cost, high yield and suitability for large-scale production and preparation.
Description
Technical field
The present invention relates to a kind of preparation method, particularly a kind of surface-modified nano copper particulate and preparation method thereof.
Background technology
Nano material shows special advantages because of its special nano effect and high surface in tribological field.Particularly soft metal such as copper and alloy thereof nanoparticle antifriction, wear-resistant and self-repair function is particularly outstanding, selfreparing nano lubricating anti-friction material as the novel high-performance lubricating oil and grease additive uses, can repair automatically the abrading section of plant equipment friction pair, and have significant wear-resistant and energy saving effect.Wherein but poor, the dispersion stabilization in oil medium of nanometer copper product oxidation stability and monodispersity are poor, limited their extensive use, therefore preparation has good chemical stability and the nanometer copper particulate of good dispersion is arranged in oil medium and make its multifunction become the focus of people's research.
At present, the preparation method is in the majority with physical method and chemical method for nanometer copper particulate, physical method mainly contains melt-blending process, gas phase co-electrodeposition method etc., the nanometer copper particulate constituent of these method preparations is pure, but its surface is oxidation deterioration easily, and can't disperse in organic media, disperses even add a large amount of surfactants, still can not realize stable dispersion, sedimentation easily takes place.Chemical method mainly contains co-reducing process, metal ion displacement method etc., but also can't solve the aerial oxidation stability of nanometer copper particulate and the dispersion stabilization problem in organic media.The in-situ surface finishing technology is the key that solves this class problem.
As everyone knows, lubricating oil in use can be subjected to the pollution of water, leak, must spray in order to cool off workpiece situations such as a large amount of cooling waters as plant equipment, all can enter certain moisture in lubricating oil, this just requires lubricating oil to have certain branch water-based and is not changed into W/O(water/oil by water and milk) the type emulsified body.Lubricating oil after emulsification or its resistance to emulsion poor, can lost flowability (the w/o type emulsified body can make oil viscosity increase exponentially) and lose lubricity, also can cause metal erosion and wearing and tearing.All be subject to the pollution of water as industrial gear oil, steam turbine oil, the hydraulic oil oil product of zinc salt (as contain), demulsification performance is had higher requirement.
Summary of the invention:
The object of the invention is to provide a kind of surface-modified nano copper particulate and preparation method thereof, and prepared product demulsification performance is strong, antioxygenic property is strong, oily molten dispersion stabilization is good.
The technical solution used in the present invention is as follows: a kind of surface-modified nano copper particulate and preparation method thereof, may further comprise the steps: at first prepare copper salt solution, add ammonia spirit, then the mixed liquor of copper salt solution with reducing agent, the coating material with demulsification performance, organic solvent fully mixed, make it behind reaction 1-3 h under alkalescence (PH is 8-11) condition, concentrating and separating namely gets described surface-modified nano copper particulate, wherein copper: reducing agent: the amount of substance of coating material is than selecting 1:5-20:0-2; Mantoquita is water-soluble substances, and described water-soluble substances is copper sulphate, hydrochloric acid copper, copper nitrate, copper acetate etc.; Wherein copper salt solution concentration is 0.05-0.2 mol/L; Reducing agent is selected the mixture of hydrazine hydrate, sodium borohydride or hydrazine hydrate and sodium borohydride; Coating material is the mixture of a kind of or any two kinds of solution in alkyl polyoxyethylene ether phosphate, alkyl polyoxyethylene ether phosphate, the isooctanol polyoxyethylene poly-oxygen propylene aether phosphate; Organic solvent is wherein any two kinds mixture of benzene,toluene,xylene or benzene,toluene,xylene, and consumption is the 10%-50% of reaction system cumulative volume.
The present invention compared with prior art has the following advantages:
Stoped the generation of further growing up and reuniting of nanoparticle, thereby particle size and the grain while of nano-particle of copper have been controlled, obtained good oxidation stability, can steady in a long-termly exist, nanometer copper has excellent antifriction, wear-resistant and self-repair function and good demulsification performance concurrently, adopt the in-situ surface finishing technology to prepare nanometer copper particulate, guarantee its excellent antifriction, wear-resistant and self-repair function, strengthened its anti-milkiness energy again, and preparation technology is simple, and raw material is cheap and easy to get, and cost is low, the productive rate height is fit to the large-scale production preparation.
The specific embodiment
Below by preferred embodiment technology of the present invention being described in further detail, but protection scope of the present invention is not limited thereto.
Embodiment 1
0.01 mol copper sulphate is dissolved in the 100 mL distilled water, add 5 mL ammonia spirits, obtain the blue solution of transparent and homogeneous, with 0.1 mol hydrazine hydrate and 0.01 mol alkyl polyoxyethylene ether phosphate, 100 mL benzene mix, and slowly are added drop-wise in the above-mentioned blue solution, there is bubble to produce, stir reaction 1-3 h down, dephlegmate divides and benzene obtains thick liquid, is surface-modified nano copper particulate.
Embodiment 2
With 0.04 mol hydrochloric acid copper dissolution in 500 mL distilled water, add 15 mL ammonia spirits, obtain the blue solution of transparent and homogeneous, with 0.3 mol sodium borohydride and 0.01 mol alkyl polyoxyethylene ether phosphate, 200 mL toluene mix, and slowly are added drop-wise in the above-mentioned blue solution, there is bubble to produce, stir reaction 1-3 h down, dephlegmate divides and benzene obtains thick liquid, is surface-modified nano copper particulate.
Embodiment 3
0.04 mol copper nitrate is dissolved in the 500 mL distilled water, add 15 mL ammonia spirits, obtain the blue solution of transparent and homogeneous, with mixture and the 0.06 mol isooctanol polyoxyethylene poly-oxygen propylene aether phosphate of 0.5 mol hydrazine hydrate and 0.2 mol sodium borohydride, 300 mL dimethylbenzene mix, and slowly are added drop-wise in the above-mentioned blue solution, there is bubble to produce, stir reaction 1-3 h down, dephlegmate divides and benzene obtains thick liquid, is surface-modified nano copper particulate.
Embodiment 4
0.04 mol copper acetate is dissolved in the 500 mL distilled water, add 15 mL ammonia spirits, obtain the blue solution of transparent and homogeneous, 0.5 mol hydrazine hydrate and 0.02 mol alkyl polyoxyethylene ether phosphate and the phosphatic mixture of alkyl polyoxyethylene ether, 100 mL benzene and toluene mixture mix, and slowly are added drop-wise in the above-mentioned blue solution, there is bubble to produce, stir reaction 1-3h down, dephlegmate divides and benzene obtains thick liquid, is surface-modified nano copper particulate.
The present invention is owing to surface when nano-particle of copper just generates coats organic modifier, stoped the generation of further growing up and reuniting of nanoparticle, thereby particle size and the grain while of nano-particle of copper have been controlled, the coating of coating material has also stoped the aerial oxidation of metallic nano-particle, thereby obtained good oxidation stability, can steady in a long-termly exist.Good dispersion and the dispersion stabilization of metallic nano-particle in multiple lubricating base oil also given in the existence of different is organic modifier.
Simultaneously, at the characteristics of easy emulsion deterioration in the lubricating oil use, introduce in the organic modifier by the polyoxyethylene group that will have the emulsion resistance function, make nanometer copper have excellent antifriction, wear-resistant and self-repair function and good demulsification performance concurrently.
The present invention is directed to the characteristics of the easy emulsion deterioration of lubricating oil, introduce in the organic modifier by the polyoxyethylene group that will have the emulsion resistance function, adjust nano copper microparticle surfaces organic modifier structure and dressing agent and copper nuclear percentage, adopt the in-situ surface finishing technology to prepare nanometer copper particulate, guarantee its excellent antifriction, wear-resistant and self-repair function, strengthened its anti-milkiness energy again.
Claims (7)
1. surface-modified nano copper particulate, it is characterized in that: may further comprise the steps: at first prepare copper salt solution, add ammonia spirit, then the mixed liquor of copper salt solution with reducing agent, the coating material with demulsification performance, organic solvent fully mixed, make it behind reaction 1-3 h under alkalescence (PH is 8-11) condition, concentrating and separating.
2. according to the described a kind of surface-modified nano copper particulate of claim 1, it is characterized in that: described mantoquita is water-soluble substances, as copper sulphate, hydrochloric acid copper, copper nitrate, copper acetate.
3. according to the described a kind of surface-modified nano copper particulate of claim 1, it is characterized in that: described copper salt solution concentration is 0.05-0.2 mol/L.
4. according to the described a kind of surface-modified nano copper particulate of claim 1, it is characterized in that: described reducing agent is the mixture of hydrazine hydrate, sodium borohydride or hydrazine hydrate and sodium borohydride.
5. according to the described a kind of surface-modified nano copper particulate of claim 1, it is characterized in that: described coating material is the mixture of a kind of or any two kinds of solution in alkyl polyoxyethylene ether phosphate, alkyl polyoxyethylene ether phosphate, the isooctanol polyoxyethylene poly-oxygen propylene aether phosphate.
6. according to the preparation method of the described a kind of surface-modified nano copper particulate of claim 1, it is characterized in that: the amount of substance of Tong Yuan Su ︰ Hai Yuan Ji ︰ coating material is than being 1:5-20:0-2.
7. according to the preparation method of the described a kind of surface-modified nano copper particulate of claim 1, it is characterized in that: described organic solvent is wherein any two kinds mixture of benzene,toluene,xylene or benzene,toluene,xylene, and described consumption of organic solvent is the 10%-50% of reaction system cumulative volume.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013102297484A CN103264167A (en) | 2013-06-09 | 2013-06-09 | Surface modification nanometer copper particle and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013102297484A CN103264167A (en) | 2013-06-09 | 2013-06-09 | Surface modification nanometer copper particle and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103264167A true CN103264167A (en) | 2013-08-28 |
Family
ID=49007853
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013102297484A Pending CN103264167A (en) | 2013-06-09 | 2013-06-09 | Surface modification nanometer copper particle and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103264167A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103752820A (en) * | 2014-02-19 | 2014-04-30 | 南京林业大学 | Method for preparing modified nanometer cobalt powder |
| CN103769598A (en) * | 2013-10-08 | 2014-05-07 | 东江环保股份有限公司 | Method for stably preparing nano-copper powder |
| CN110744068A (en) * | 2019-10-21 | 2020-02-04 | 河南大学 | Oil-soluble nano copper and preparation method thereof |
| CN115070058A (en) * | 2022-08-16 | 2022-09-20 | 西安锐创微米科技有限公司 | Preparation method of high-crystallinity and high-sphericity palladium powder with strong oxidation resistance |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004315853A (en) * | 2003-04-11 | 2004-11-11 | Ishihara Sangyo Kaisha Ltd | Copper powder, manufacturing method therefor, copper paste using the copper powder, copper paint and electrode |
| JP2005060778A (en) * | 2003-08-13 | 2005-03-10 | Ishihara Sangyo Kaisha Ltd | Copper powder, its production method, and copper paste, paint and electrode obtained by using the same |
| CN1672836A (en) * | 2004-03-22 | 2005-09-28 | 河南大学 | Water soluble nano metal particle and its prepn process |
| JP2006022394A (en) * | 2004-07-09 | 2006-01-26 | Harima Chem Inc | Method for producing metallic copper fine particle |
| CN101259531A (en) * | 2008-03-31 | 2008-09-10 | 河南大学 | Surface finish nano copper/copper alloy particles and preparation thereof |
| JP2009242824A (en) * | 2008-03-28 | 2009-10-22 | Furukawa Electric Co Ltd:The | Manufacturing method of copper particulate dispersion liquid, and copper particulate dispersion liquid |
| CN101612667B (en) * | 2009-05-31 | 2011-01-26 | 河南大学 | Method for preparing surface modification oil solubility nanometer copper |
| CN102554217A (en) * | 2012-02-24 | 2012-07-11 | 河南大学 | Water-soluble nano-copper and preparation method thereof |
-
2013
- 2013-06-09 CN CN2013102297484A patent/CN103264167A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004315853A (en) * | 2003-04-11 | 2004-11-11 | Ishihara Sangyo Kaisha Ltd | Copper powder, manufacturing method therefor, copper paste using the copper powder, copper paint and electrode |
| JP2005060778A (en) * | 2003-08-13 | 2005-03-10 | Ishihara Sangyo Kaisha Ltd | Copper powder, its production method, and copper paste, paint and electrode obtained by using the same |
| CN1672836A (en) * | 2004-03-22 | 2005-09-28 | 河南大学 | Water soluble nano metal particle and its prepn process |
| JP2006022394A (en) * | 2004-07-09 | 2006-01-26 | Harima Chem Inc | Method for producing metallic copper fine particle |
| JP2009242824A (en) * | 2008-03-28 | 2009-10-22 | Furukawa Electric Co Ltd:The | Manufacturing method of copper particulate dispersion liquid, and copper particulate dispersion liquid |
| CN101259531A (en) * | 2008-03-31 | 2008-09-10 | 河南大学 | Surface finish nano copper/copper alloy particles and preparation thereof |
| CN101612667B (en) * | 2009-05-31 | 2011-01-26 | 河南大学 | Method for preparing surface modification oil solubility nanometer copper |
| CN102554217A (en) * | 2012-02-24 | 2012-07-11 | 河南大学 | Water-soluble nano-copper and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王会先: "《润滑油脂生产技术》", 30 April 2005, 中国石化出版社 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103769598A (en) * | 2013-10-08 | 2014-05-07 | 东江环保股份有限公司 | Method for stably preparing nano-copper powder |
| CN103752820A (en) * | 2014-02-19 | 2014-04-30 | 南京林业大学 | Method for preparing modified nanometer cobalt powder |
| CN103752820B (en) * | 2014-02-19 | 2016-03-30 | 南京林业大学 | A kind of preparation method of modified Nano cobalt powder |
| CN110744068A (en) * | 2019-10-21 | 2020-02-04 | 河南大学 | Oil-soluble nano copper and preparation method thereof |
| CN110744068B (en) * | 2019-10-21 | 2021-01-26 | 河南大学 | Oil-soluble nano copper and preparation method thereof |
| CN115070058A (en) * | 2022-08-16 | 2022-09-20 | 西安锐创微米科技有限公司 | Preparation method of high-crystallinity and high-sphericity palladium powder with strong oxidation resistance |
| CN115070058B (en) * | 2022-08-16 | 2022-11-01 | 西安锐创微米科技有限公司 | Preparation method of high-crystallinity and high-sphericity palladium powder with strong oxidation resistance |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103934468B (en) | The supercritical water process for thermosynthesizing of nano metal or metal oxide nano particles | |
| CN100579688C (en) | Surface finish nano copper/copper alloy particles and preparation thereof | |
| CN104058380B (en) | The preparation method of the elliposoidal ion doping type hydroxyapatite micro-sphere of porous surface | |
| CN102133646A (en) | Preparation method of dispersed iron nanoparticles | |
| CN103264167A (en) | Surface modification nanometer copper particle and preparation method thereof | |
| CN103666197B (en) | A kind of steel construction use corrosion-resistant epoxy paint | |
| WO2008084828A1 (en) | Method for producing coenzyme q10 particle | |
| CN100577332C (en) | Preparation of Pd nano particle | |
| CN103113958A (en) | Preparation method of graphene alkenyl nano-copper lubricant additive | |
| CN101612667B (en) | Method for preparing surface modification oil solubility nanometer copper | |
| CN103273077A (en) | Preparing method of [Bmim] BF4 dispersed nano-iron particle | |
| CN103045181A (en) | Copper nanofluid solar cooling liquid and preparation method thereof | |
| CN103769599A (en) | Disperse nano-iron particle preparing method | |
| CN103273076A (en) | HDTMPA K6 nano-iron particle dispersing method | |
| CN102303125A (en) | Method for preparing nano silver powder in viscous medium | |
| CN102719295A (en) | Core-shell metal oxide/titanium oxide compound electrorheological fluid and preparation method thereof | |
| CN108998183A (en) | Smart phone frame synthesis type dia-cutting liquid and preparation method thereof | |
| CN103273075A (en) | HPAA nano-iron particle dispersing method | |
| CN103611944A (en) | Preparation method of ClO3- ionic liquid dispersed iron nanoparticles | |
| CN103694848B (en) | A kind of Water-borne epoxy anticorrosive paint for concrete surface | |
| CN101200667A (en) | Method for preparing nano copper lubricating oil additive | |
| CN103551590A (en) | Method for preparing dispersed iron nanoparticles from caprolactam type ionic liquid | |
| CN103785849A (en) | Preparation method of TH-908 dispersed iron nano-particles | |
| CN102276832A (en) | Preparation method of easily dispersible polyaniline for anti-corrosion coating | |
| Pu et al. | Synthesis of transparent oil dispersion of monodispersed calcium carbonate nanoparticles with high concentration |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20130828 |