CN104325154A - Preparation technology of ultrafine copper powder - Google Patents
Preparation technology of ultrafine copper powder Download PDFInfo
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- CN104325154A CN104325154A CN201410715478.2A CN201410715478A CN104325154A CN 104325154 A CN104325154 A CN 104325154A CN 201410715478 A CN201410715478 A CN 201410715478A CN 104325154 A CN104325154 A CN 104325154A
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- copper
- ethylene glycol
- mixed solution
- copper powder
- powder
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Abstract
The invention provides a preparation technology of ultrafine copper powder. The preparation technology comprises the steps of mixing copper salt and ethylene glycol, and adding alkaline liquid to prepare a mixed solution with the copper concentration being 10-100g/L; heating the mixed solution to 150-250 DEG C, performing condensing backflow on volatilized ethylene glycol steam at the temperature of 100-150 DEG C, performing condensing recycling on residual ethylene glycol steam at the temperature of 20-30 DEG C for reaction for 1-10 hours; and performing solid-liquid separation and washing on reactants, and performing vacuum drying at the temperature of 50-100 DEG C to prepare the ultrafine copper powder. The technology is low in cost and simple in flow; the obtained ultrafine copper powder is small in particle size, the particle size is 0.3-1.5 microns, and the particle size distribution is narrow.
Description
Technical field
The present invention relates to a kind of preparation method of powder body material, particularly relate to a kind of preparation technology of superfine cupper powder.
Technical background
Superfine cupper powder, owing to having higher surface-active and good conduction, heat conductivility, is therefore essential industry raw material, is mainly used in the fields such as powder metallurgy, catalyst, lubricant, electrically-conducting paint and electromagnetic shielding material.
As superfine cupper powder have that resistivity is little, electromigration speed is little, the excellent advantage such as honest and clean of price, be one of ideal substitute of silver-palladium inner electrode, can be used in MLCC on electrode.
The application of superfine cupper powder in electrically-conducting paint.The filler of current electrically-conducting paint mainly contains carbon system, silver system, copper system and nickel system and compound system etc.As the conductive filler in electromagnetic wave shielding coating, copper powder is high with electrical conductivity, and price is relatively cheap, and material is easy to get, and there is not silver powder and " silver migration " occurs in the coating and affects the advantages such as coating performance and gain great popularity.
The application of copper powder on lubricant.Superfine cupper powder is scattered in an adequate manner in various lubricating oil and forms a kind of stable suspension; a kind of lubricant of function admirable can be become; significantly can reduce wearing and tearing and friction; especially act on more remarkable in heavy duty, low speed and high-temperature vibrating situation, material and equipment are played to the effect of protection.
Copper powder application on a catalyst.The particle of superfine cupper powder is thin and evenly, specific surface activity is very large, and this characteristic can be utilized to manufacture effective catalyst.As in purifying vehicle exhaust processing procedure, superfine cupper powder can be used as catalyst and is used for partly replacing noble metal platinum and ruthenium, makes the carbon monoxide of toxicity change carbon dioxide into, makes nitric oxide change nitrogen dioxide into; The catalyst in the course of reaction such as carbon dioxide and hydrogen synthesizing methanol can also be used for, there is higher catalytic activity.The polymerization of nanometer copper particle catalyzing acetylene also achieves satisfied effect.
Copper nanoparticle can be used for preparing Nanometer Copper material, and the copper product of gained has good ductility, and intensity and plasticity also improve significantly, and this processing to material, micromachine manufacture have important value.In addition, because the fusing point of copper is low, also can be used for space industry, as rocket nozzle etc.Secondly, superfine cupper powder even may be used for treating osteoporosis, fracture etc.
The preparation method of superfine cupper powder has gas phase vapor method, gamma-rays method, plasma method, mechanochemical reaction, liquid phase reduction etc., generally speaking can be summed up as Physical and chemical method, and gas phase steam method equipment is complicated, cost is high; Gamma-radiation method product is difficult to collect; Plasma method capacity usage ratio is low; Product granularity prepared by water atomization is large, and formability is poor.With regard to chemical method, copper powder prepared by mechanochemical reaction is uneven, and domain size distribution is wide, easily introduces impurity; Electrolysis energy consumption is large, and cost is high; Ammonium salt discrimination method productive rate is too low; Although solution phase chemical reduction equipment is simple, easy suitability for industrialized production, current used reducing agent or have severe toxicity, or high cost.Just because of above shortcoming, the application of these preparation methods is restricted.
Summary of the invention
The object of the present invention is to provide a kind of preparation technology of superfine cupper powder, in the present invention, reducing agent ethylene glycol is cheap, and the byproduct glyoxal generated can reclaim completely and sell, thus production cost is reduced greatly, technological process is simple, and the copper powder particle size of preparation is 0.3-1.5um, narrow particle size distribution, is easy to realize large-scale production.
Concrete technical scheme is as follows:
Prepare a method for spherical cobalt powder, comprise the following steps:
1). get mantoquita and mix with ethylene glycol, add alkali lye, be mixed with the mixed solution that copper concentration is 10 ~ 100g/L.
2). mixed solution is heated to 150 ~ 250 DEG C, the glycol steam of volatilization is through 100-150 DEG C of condensing reflux, and remaining glyoxal steam reclaims through 20-30 DEG C of condensation, reaction 1-10 hour.
3). reactant is through Separation of Solid and Liquid, and washing, vacuum drying at 50-100 DEG C of temperature, obtains superfine cupper powder.
Described mantoquita is one or more in copper sulphate, copper nitrate, copper chloride, Schweinfurt green.
The concentration of described ethylene glycol in mixed solution is 8 ~ 80g/L.
Described alkali lye is one or more in NaOH, potassium hydroxide, ammoniacal liquor.
N (OH in described alkali lye
-) and n (Cu
2+) ratio be 3 ~ 6: 1.
The described vacuum drying time is 1-6 hour.
Its chemical equation is as follows:
C
2H
6O
2+Cu(OH)
2＝C
2H
4O
2+Cu+2H
2O
C
2h
6o
2the boiling point of (ethylene glycol) is 197 DEG C, and C
2h
4o
2the boiling point of (glyoxal) is 45 DEG C, and in course of reaction, because reaction temperature is far above the boiling point of glyoxal, then the glyoxal generated evaporates completely, reclaims obtain glyoxal product through 20-30 DEG C of condensation.Can be used as product to sell.The surface that simultaneously can be adsorbed on copper powder due to ethylene glycol defines the electronegative film of one deck and prevents the reunion of copper powder particle to stop new nucleus to generate simultaneously, thus makes the particle of copper powder thinner, and size distribution is narrower.Dry under vacuum conditions, avoid the oxidation of copper powder, greatly reduce the oxygen content of copper powder.
A kind of preparation technology preparing superfine cupper powder provided by the invention, has following beneficial effect:
(1) superfine cupper powder is prepared in direct mantoquita and reduction of ethylene glycol reaction, and flow process is short, and technique is simple;
(2) the accessory substance glyoxal obtained due to reduction of ethylene glycol is recyclable to be sold as product, reduce the three wastes and produce, and cost reduces greatly;
(3) due to the peptizaiton of ethylene glycol, finally the copper powder particle size prepared of this technique is comparatively thin, is generally 0.3-1.5um, and narrow particle size distribution.
Detailed description of the invention
The following stated is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Embodiment one
1). get copper sulphate and mix with ethylene glycol, add sodium hydroxide solution, be mixed with the mixed solution that copper concentration is 65g/L, the concentration of ethylene glycol is 75g/l, n (OH in system
-) and n (Cu
2+) ratio be 4: 1.
2). mixed solution is heated to 185 DEG C, the glycol steam of volatilization is through 110 DEG C of condensing refluxes, and remaining glyoxal steam reclaims through 25 DEG C of condensations, reacts 5 hours.
3). reactant is through Separation of Solid and Liquid, and washing, vacuum drying 3 hours at 75 DEG C of temperature, obtained superfine cupper powder granularity is 0.8um, (D90-D10)/D50=0.75.
Embodiment two
1). get copper sulphate and mix with ethylene glycol, add sodium hydroxide solution, be mixed with the mixed solution that copper concentration is 65g/L, the concentration of ethylene glycol is 75g/l, n (OH in system
-) and n (Cu
2+) ratio be 5: 1.
2). mixed solution is heated to 200 DEG C, the glycol steam of volatilization is through 110 DEG C of condensing refluxes, and remaining glyoxal steam reclaims through 25 DEG C of condensations, reacts 6 hours.
3). reactant is through Separation of Solid and Liquid, and washing, vacuum drying 3 hours at 75 DEG C of temperature, obtained superfine cupper powder granularity is 1.0um, (D90-D10)/D50=0.70.
Embodiment three
1). get copper sulphate and mix with ethylene glycol, add sodium hydroxide solution, be mixed with the mixed solution that copper concentration is 40g/L, the concentration of ethylene glycol is 50g/l, n (OH in system
-) and n (Cu
2+) ratio be 5: 1.
2). mixed solution is heated to 200 DEG C, the glycol steam of volatilization is through 110 DEG C of condensing refluxes, and remaining glyoxal steam reclaims through 25 DEG C of condensations, reacts 6 hours.
3). reactant is through Separation of Solid and Liquid, and washing, vacuum drying 6 hours at 50 DEG C of temperature, obtained superfine cupper powder granularity is 0.65um, (D90-D10)/D50=0.80.
Claims (6)
1. a preparation technology for superfine cupper powder, is characterized in that, comprises the following steps:
1). get mantoquita and mix with ethylene glycol, add alkali lye, be mixed with the mixed solution that copper concentration is 10 ~ 100g/L.
2). mixed solution is heated to 150 ~ 250 DEG C, the glycol steam of volatilization is through 100-150 DEG C of condensing reflux, and remaining glyoxal steam reclaims through 20-30 DEG C of condensation, reaction 1-10 hour.
3). reactant is through Separation of Solid and Liquid, and washing, vacuum drying at 50-100 DEG C of temperature, obtains superfine cupper powder.
2. the method for claim 1, is characterized in that, described mantoquita is one or more in copper sulphate, copper nitrate, copper chloride, Schweinfurt green.
3. the method for claim 1, is characterized in that, the concentration of described ethylene glycol in mixed solution is 8 ~ 80g/L.
4. the method for claim 1, is characterized in that, described alkali lye is one or more in NaOH, potassium hydroxide, ammoniacal liquor.
5. the method for claim 1, is characterized in that, the n (OH-) in described alkali lye and n (Cu
2+) ratio be 3 ~ 6: 1.
6. the method for claim 1, is characterized in that, the described vacuum drying time is 1-6 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410715478.2A CN104325154A (en) | 2014-11-28 | 2014-11-28 | Preparation technology of ultrafine copper powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410715478.2A CN104325154A (en) | 2014-11-28 | 2014-11-28 | Preparation technology of ultrafine copper powder |
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| Publication Number | Publication Date |
|---|---|
| CN104325154A true CN104325154A (en) | 2015-02-04 |
Family
ID=52400025
Family Applications (1)
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|---|---|---|---|
| CN201410715478.2A Pending CN104325154A (en) | 2014-11-28 | 2014-11-28 | Preparation technology of ultrafine copper powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104475750A (en) * | 2014-12-02 | 2015-04-01 | 广西大学 | Preparation method of superfine copper powder |
| CN110039069A (en) * | 2019-05-30 | 2019-07-23 | 江西省科学院能源研究所 | A kind of spongy Micron Copper Powder and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101376174A (en) * | 2008-09-27 | 2009-03-04 | 浙江华友钴业股份有限公司 | Method for preparing superfine spherical cobalt powder |
| CN101474678A (en) * | 2008-11-28 | 2009-07-08 | 中国兵器工业第五二研究所 | Method for preparing antioxidated superfine copper powder |
| CN102240813A (en) * | 2010-05-10 | 2011-11-16 | 中国科学院过程工程研究所 | Preparing method for cubic crystallized copper micro powder |
| US20130192423A1 (en) * | 2012-01-27 | 2013-08-01 | Blue Nano Inc. | Method of producing silver nanowires |
| CN103691967A (en) * | 2014-01-09 | 2014-04-02 | 李泽国 | Novel large-scale simple preparation method of nano-silver hydrosol |
-
2014
- 2014-11-28 CN CN201410715478.2A patent/CN104325154A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101376174A (en) * | 2008-09-27 | 2009-03-04 | 浙江华友钴业股份有限公司 | Method for preparing superfine spherical cobalt powder |
| CN101474678A (en) * | 2008-11-28 | 2009-07-08 | 中国兵器工业第五二研究所 | Method for preparing antioxidated superfine copper powder |
| CN102240813A (en) * | 2010-05-10 | 2011-11-16 | 中国科学院过程工程研究所 | Preparing method for cubic crystallized copper micro powder |
| US20130192423A1 (en) * | 2012-01-27 | 2013-08-01 | Blue Nano Inc. | Method of producing silver nanowires |
| CN103691967A (en) * | 2014-01-09 | 2014-04-02 | 李泽国 | Novel large-scale simple preparation method of nano-silver hydrosol |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104475750A (en) * | 2014-12-02 | 2015-04-01 | 广西大学 | Preparation method of superfine copper powder |
| CN110039069A (en) * | 2019-05-30 | 2019-07-23 | 江西省科学院能源研究所 | A kind of spongy Micron Copper Powder and preparation method thereof |
| CN110039069B (en) * | 2019-05-30 | 2021-05-14 | 江西省科学院能源研究所 | Spongy micron copper powder and preparation method thereof |
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Application publication date: 20150204 |