CN103303961B - Preparation method of spherical electroplating-level copper oxide powder - Google Patents
Preparation method of spherical electroplating-level copper oxide powder Download PDFInfo
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- CN103303961B CN103303961B CN201310193411.2A CN201310193411A CN103303961B CN 103303961 B CN103303961 B CN 103303961B CN 201310193411 A CN201310193411 A CN 201310193411A CN 103303961 B CN103303961 B CN 103303961B
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Abstract
The invention relates to a preparation method of spherical electroplating-level copper oxide powder. The preparation method comprises the preparation steps of: (1) dissolving powdered copper sulfate pentahydrate into super-pure water to prepare a copper sulfate solution; (2) carrying out gas atomization on the copper sulfate solution to form spherical copper sulfate crystal drops; (3) naturally cooling the spherical copper sulfate crystal drops and then directly flowing in a reaction kettle containing a sodium carbonate aqueous solution, controlling the reaction temperature to range from 50 DEG C to 80 DEG C, and reacting for 10min to 20min under the stirring state; (4) filtering, washing and drying reacted materials to obtain spherical basic copper carbonate crystals; and (5) transferring the spherical basic copper carbonate crystals into a calcining furnace for calcining to prepare spherical electroplating-level copper oxide powder. The prepared copper oxide powder is irregularly spherical micro-fine powder, large in specific surface area, good in dispersity, and has the advantages of being high in purity and stable in product performance, and when being applied in electroplating technique, the copper oxide powder can be fast dissolved sufficiently in the electroplating dissolved solution.
Description
Technical field
The present invention relates to gas atomization chemical reaction technology, particularly a kind of preparation method who adopts gas atomization to prepare spherical plating-grade copper oxide powder.
Background technology
At present need to possess higher requirement for the cupric oxide powder on electroplating technology, as require cupric oxide powder can dissolve fast in electroplate liquid, stable performance etc.
The technique that tradition is prepared plating-grade copper oxide powder mainly comprises the following steps: (1) splashes into or put into sodium carbonate solution in copper-bath or copper sulphate powder, reacted product after filtration, washing, the dry ventilation breather (unformed random crystal particle) that makes; (2) the above-mentioned ventilation breather making is placed in to rotary kiln and is heated to calcine, grind at 450 DEG C ~ 600 DEG C temperature, make cupric oxide powder.
The cupric oxide powder that adopts aforesaid method to prepare is not regulation shape powder granule of one, in the time electroplating, cupric oxide powder, electroplating the easy arch formation that forms in lysate, causes dissolution rate slow, and needing artificial periodic cleaning, cupric oxide powder can not fully dissolve to such an extent as to waste the drawbacks such as material.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, and a kind of preparation method who adopts gas atomization to prepare spherical plating-grade copper oxide powder is provided.
For solving above technical problem, the present invention adopts following technical scheme:
A preparation method for spherical plating-grade copper oxide powder, it comprises the following steps:
(1) in reactor, adding cupric sulfate pentahydrate and ultrapure water and the two weight ratio is 1:2 ~ 3, is then heated to 65 DEG C ~ 75 DEG C and also stirs it is fully dissolved, and makes copper-bath;
(2) described copper-bath is injected to atomisation tower by high-pressure atomization nozzle, after high pressure gas atomization, obtain spherical copper sulfate crystal drop;
(3) described spherical copper sulfate crystal drop directly enters in the reactor that aqueous sodium carbonate is housed in atomisation tower after naturally cooling, and stir, temperature of reaction is controlled between 50 DEG C ~ 80 DEG C, stirring reaction 10min ~ 20min again after the material in described spray tower all enters reactor;
(4) by the material after step (3) reaction kettle for reaction after filtration, washing, dry, make spherical basic carbonate copper crystal, wherein, the waste water producing after the waste water producing after filtering and washing all enters Waste Water Treatment;
(5) spherical basic carbonate copper crystal step (4) being made is transferred in calcining furnace to be calcined, and makes spherical plating-grade copper oxide powder, discharges containing water vapor, CO simultaneously
2the tail gas of gas, described tail gas is by washing tower processing.
Particularly, in step (1), described cupric sulfate pentahydrate is Powdered.
Particularly, in step (2), the spray orifice of described high-pressure atomization nozzle is folding structure formula spray orifice, folding structure formula spray orifice can produce higher Supersonic air-flow and uniform gas velocity field under lower air pressure, thereby more effectively suppress the generation of harmful shock wave, the kinetic energy that obviously increases gas, makes nebulization efficiency higher; What in described high pressure gas atomization process, select is that gaseous tension is the high pressure gas of 3kg ~ 5kg.
Particularly, the calcining temperature that the calcination process in described step (5) adopts is 300 DEG C ~ 500 DEG C.
Due to the enforcement of technique scheme, the present invention compared with prior art tool has the following advantages:
Cupric oxide powder prepared by the present invention is that regular spherical fines, specific surface area are large, good dispersity, and has advantages of that purity is high, product performance are stable, when this cupric oxide powder is applied to electroplating technology, in plating lysate, can dissolves fast and dissolve fully.
The copper sulfate crystal drop forming after high pressure gas atomization in preparation method of the present invention directly enters in the reactor that aqueous sodium carbonate is housed, and has simplified technical process, has reduced cost, easy to operate.
Brief description of the drawings
Fig. 1 is production process flow process figure of the present invention;
Fig. 2 is the structural representation of high-pressure atomization nozzle;
Wherein: 1, spray orifice.
Embodiment
Below in conjunction with Figure of description, the invention will be further described.
Embodiment 1
A preparation method for spherical plating-grade copper oxide powder, specifically comprises the following steps:
(1) in the reactor of 500L, add 255kg ultrapure water and the Powdered cupric sulfate pentahydrate of 127.5kg, be then heated to 70 DEG C and also stir it is fully dissolved, make copper-bath;
(2) copper-bath is injected to atomisation tower by the high-pressure atomization nozzle with folding structure spray orifice 1, high-pressure atomization nozzle as shown in Figure 2, obtains spherical copper sulfate crystal drop through gaseous tension after the high pressure gas atomization that is 4kg;
(3) spherical copper sulfate crystal drop directly enters in the 3000L reactor that 1700L aqueous sodium carbonate is housed in atomisation tower after naturally cooling, and stir, temperature of reaction is controlled at 75 DEG C, stirring reaction 15min again after the material in spray tower all enters reactor, wherein, the concentration of aqueous sodium carbonate is 0.3mol/L;
(4) by the material after step (3) reaction kettle for reaction after filtration, washing, dry, make spherical basic carbonate copper crystal, wherein, the waste water producing after the waste water producing after filtering and washing all enters Waste Water Treatment;
(5) spherical basic carbonate copper crystal step (4) being made is transferred in calcining furnace to be calcined, calcining temperature is 350 DEG C, make spherical plating-grade copper oxide powder, discharge the tail gas of containing water vapor, CO2 gas in calcination process simultaneously, tail gas is by washing tower processing.
Embodiment 2
A preparation method for spherical plating-grade copper oxide powder, specifically comprises the following steps:
(1) in the reactor of 1500L, add 700kg ultrapure water and the Powdered cupric sulfate pentahydrate of 280kg, be then heated to 70 DEG C and also stir it is fully dissolved, make copper-bath;
(2) copper-bath is injected to atomisation tower by the high-pressure atomization nozzle with folding structure spray orifice 1, high-pressure atomization nozzle as shown in Figure 2, obtains spherical copper sulfate crystal drop through gaseous tension after the high pressure gas atomization that is 5kg;
(3) spherical copper sulfate crystal drop directly enters in the 5000L reactor that 2800L aqueous sodium carbonate is housed in atomisation tower after naturally cooling, and stir, temperature of reaction is controlled at 65 DEG C, stirring reaction 20min again after the material in spray tower all enters reactor, wherein, the concentration of aqueous sodium carbonate is 0.4mol/L;
(4) by the material after step (3) reaction kettle for reaction after filtration, washing, dry, make spherical basic carbonate copper crystal, wherein, the waste water producing after the waste water producing after filtering and washing all enters Waste Water Treatment;
(5) spherical basic carbonate copper crystal step (4) being made is transferred in calcining furnace to be calcined, calcining temperature is 400 DEG C, make spherical plating-grade copper oxide powder, discharge the tail gas of containing water vapor, CO2 gas in calcination process simultaneously, tail gas is by washing tower processing.
Above the present invention is described in detail; its object is to allow the personage who is familiar with this art can understand content of the present invention and be implemented; can not limit the scope of the invention with this; and the invention is not restricted to the embodiments described; the equivalence that all spirit according to the present invention are done changes or modifies, within all should being encompassed in protection scope of the present invention.
Claims (5)
1. a preparation method for spherical plating-grade copper oxide powder, is characterized in that: described preparation method comprises the following steps:
(1) in reactor, adding cupric sulfate pentahydrate and ultrapure water and the two weight ratio is 1:2 ~ 3, is then heated to 65 DEG C ~ 75 DEG C and also stirs it is fully dissolved, and makes copper-bath;
(2) described copper-bath is injected to atomisation tower by high-pressure atomization nozzle, after high pressure gas atomization, obtain spherical copper sulfate crystal drop;
(3) described spherical copper sulfate crystal drop directly enters in the reactor that aqueous sodium carbonate is housed in atomisation tower after naturally cooling, and stir, temperature of reaction is controlled between 50 DEG C ~ 80 DEG C, stirring reaction 10min ~ 20min again after the material in described atomisation tower all enters reactor;
(4) by the material after step (3) reaction kettle for reaction after filtration, washing, dry, make spherical basic carbonate copper crystal, wherein, the waste water producing after the waste water producing after filtering and washing all enters Waste Water Treatment;
(5) spherical basic carbonate copper crystal step (4) being made is transferred in calcining furnace to be calcined, and makes spherical plating-grade copper oxide powder, discharges containing water vapor, CO simultaneously
2the tail gas of gas, described tail gas is by washing tower processing.
2. the preparation method of spherical plating-grade copper oxide powder according to claim 1, is characterized in that: in step (1), described cupric sulfate pentahydrate is Powdered.
3. the preparation method of spherical plating-grade copper oxide powder according to claim 1, is characterized in that: in step (2), the spray orifice of described high-pressure atomization nozzle is folding structure formula spray orifice.
4. the preparation method of spherical plating-grade copper oxide powder according to claim 1, is characterized in that: in step (2), what in described high pressure gas atomization process, select is that gaseous tension is the high pressure gas of 3kg ~ 5kg.
5. the preparation method of spherical plating-grade copper oxide powder according to claim 1, is characterized in that: the calcining temperature that the calcination process in described step (5) adopts is 300 DEG C ~ 500 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104108739A (en) * | 2013-04-22 | 2014-10-22 | 广东致卓精密金属科技有限公司 | Preparation method of particle size-controllable spherical copper oxide |
| CN103739000B (en) * | 2013-12-25 | 2015-11-18 | 广州科城环保科技有限公司 | A kind of production method of high-purity plating-grade copper oxide |
| CN104445360A (en) * | 2014-12-03 | 2015-03-25 | 金川集团股份有限公司 | Production method of high-purity active copper oxide powder |
| CN107311220B (en) * | 2017-07-07 | 2019-07-09 | 苏州昆腾威新材料科技有限公司 | A kind of cupric oxide powder and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1342787A (en) * | 2000-09-04 | 2002-04-03 | 鹤见曹达株式会社 | Copper plated material, its manufacturing method and method for copper plating |
| CN101885506A (en) * | 2010-07-17 | 2010-11-17 | 天津市化学试剂研究所 | Method for preparing analytically pure basic cupric carbonate |
| CN103073039A (en) * | 2013-03-01 | 2013-05-01 | 兰州理工大学 | Method for preparing superfine carbonate powder material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2001335320A (en) * | 2000-05-24 | 2001-12-04 | Sumitomo Metal Mining Co Ltd | Basic copper carbonate and its preparing method |
| JP5259375B2 (en) * | 2008-12-22 | 2013-08-07 | ラサ工業株式会社 | Method for producing basic copper carbonate |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1342787A (en) * | 2000-09-04 | 2002-04-03 | 鹤见曹达株式会社 | Copper plated material, its manufacturing method and method for copper plating |
| CN101885506A (en) * | 2010-07-17 | 2010-11-17 | 天津市化学试剂研究所 | Method for preparing analytically pure basic cupric carbonate |
| CN103073039A (en) * | 2013-03-01 | 2013-05-01 | 兰州理工大学 | Method for preparing superfine carbonate powder material |
Non-Patent Citations (2)
| Title |
|---|
| Facile Fabrication and Enhanced Sensing Properties of Hierarchically Porous CuO Architectures;Guoxing Zhu et al.;《Appl. Mater. Interfaces》;20120118;第4卷;第744-751页 * |
| 不同粒度纳米碱式碳酸铜的制备;苏黎宁等;《应用化工》;20120131;第41卷(第1期);第23-25页 * |
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