CN103303961A - 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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- CN103303961A CN103303961A CN2013101934112A CN201310193411A CN103303961A CN 103303961 A CN103303961 A CN 103303961A CN 2013101934112 A CN2013101934112 A CN 2013101934112A CN 201310193411 A CN201310193411 A CN 201310193411A CN 103303961 A CN103303961 A CN 103303961A
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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
The cupric oxide powder that is used on the electroplating technology at present need to possess higher requirement, as requires cupric oxide powder can dissolve fast stable performance etc. in electroplate liquid.
The technique of tradition preparation plating-grade copper oxide powder mainly may further comprise the steps: (1) splashes into or puts into sodium carbonate solution in copper-bath or copper sulphate powder, and reacted product after filtration, washing, drying make ventilation breather (unformed random crystal particle); (2) the above-mentioned ventilation breather that makes is placed rotary kiln be heated under 450 ℃ ~ 600 ℃ temperature and calcine, grind, make cupric oxide powder.
Adopting the cupric oxide powder of aforesaid method preparation is a kind of not regulation shape powder granule, when electroplating, cupric oxide powder easily forms arch formation in electroplating lysate, cause dissolution rate slow, and need artificial periodic cleaning, to such an extent as to cupric oxide powder can not fully dissolve the drawbacks such as waste 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 kind of preparation method of spherical plating-grade copper oxide powder, it may further comprise the steps:
(1) adding cupric sulfate pentahydrate and ultrapure water and the two weight ratio in reactor is 1:2 ~ 3, then is heated to 65 ℃ ~ 75 ℃ and stir it is fully dissolved, and makes copper-bath;
(2) described copper-bath is injected atomisation tower by the high-pressure atomization nozzle, after the high pressure gas atomizing, obtain spherical copper sulfate crystal drop;
(3) described spherical copper sulfate crystal drop directly enters in the reactor that aqueous sodium carbonate is housed after naturally cooling in atomisation tower, and stir, temperature of reaction is controlled between 50 ℃ ~ 80 ℃, restir reaction 10min ~ 20min after the material in described spray tower all enters reactor;
(4) with the material after step (3) reaction kettle for reaction after filtration, washing, drying, make spherical basic carbonate copper crystal, wherein, the waste water that produces after the waste water that produces after filtering and the washing all enters Waste Water Treatment;
(5) the spherical basic carbonate copper crystal that step (4) is made is transferred in the calcining furnace to be calcined, and makes spherical plating-grade copper oxide powder, discharges simultaneously containing water vapor, CO
2The tail gas of gas, described tail gas is processed by washing tower.
Particularly, in the step (1), described cupric sulfate pentahydrate is Powdered.
Particularly, in the 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 the more generation of the harmful shock wave of establishment, obviously increase the kinetic energy of gas, make nebulization efficiency higher; What select in the described high pressure gas atomization process is that gaseous tension is the high pressure gas of 3kg ~ 5kg.
Particularly, the calcining temperature of the employing of the calcination process in the described step (5) is 300 ℃ ~ 500 ℃.
Because the enforcement of technique scheme, the present invention compared with prior art has following advantage:
The cupric oxide powder of the present invention's preparation 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, can dissolves fast and dissolve fully in electroplating lysate.
The copper sulfate crystal drop that forms after the high pressure gas atomizing among the 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, and is easy to operate.
Description of 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
The invention will be further described below in conjunction with Figure of description.
A kind of preparation method of spherical plating-grade copper oxide powder specifically may further comprise the steps:
(1) in the reactor of 500L, adds 255kg ultrapure water and the Powdered cupric sulfate pentahydrate of 127.5kg, then be heated to 70 ℃ and stir it is fully dissolved, make copper-bath;
(2) copper-bath is injected atomisation tower by the high-pressure atomization nozzle with folding structure spray orifice 1, the high-pressure atomization nozzle is to obtain spherical copper sulfate crystal drop after the high pressure gas atomizing of 4kg through gaseous tension as shown in Figure 2;
(3) spherical copper sulfate crystal drop directly enters in the 3000L reactor that the 1700L aqueous sodium carbonate is housed in atomisation tower after naturally cooling, and stir, temperature of reaction is controlled at 75 ℃, restir reacted 15min after material in spray tower all entered reactor, wherein, the concentration of aqueous sodium carbonate is 0.3mol/L;
(4) with the material after step (3) reaction kettle for reaction after filtration, washing, drying, make spherical basic carbonate copper crystal, wherein, the waste water that produces after the waste water that produces after filtering and the washing all enters Waste Water Treatment;
(5) the spherical basic carbonate copper crystal that step (4) is made is transferred in the calcining furnace to be calcined, calcining temperature is 350 ℃, make spherical plating-grade copper oxide powder, discharge simultaneously the tail gas of containing water vapor, CO2 gas in the calcination process, tail gas is processed by washing tower.
Embodiment 2
A kind of preparation method of spherical plating-grade copper oxide powder specifically may further comprise the steps:
(1) in the reactor of 1500L, adds 700kg ultrapure water and the Powdered cupric sulfate pentahydrate of 280kg, then be heated to 70 ℃ and stir it is fully dissolved, make copper-bath;
(2) copper-bath is injected atomisation tower by the high-pressure atomization nozzle with folding structure spray orifice 1, the high-pressure atomization nozzle is to obtain spherical copper sulfate crystal drop after the high pressure gas atomizing of 5kg through gaseous tension as shown in Figure 2;
(3) spherical copper sulfate crystal drop directly enters in the 5000L reactor that the 2800L aqueous sodium carbonate is housed in atomisation tower after naturally cooling, and stir, temperature of reaction is controlled at 65 ℃, restir reacted 20min after material in spray tower all entered reactor, wherein, the concentration of aqueous sodium carbonate is 0.4mol/L;
(4) with the material after step (3) reaction kettle for reaction after filtration, washing, drying, make spherical basic carbonate copper crystal, wherein, the waste water that produces after the waste water that produces after filtering and the washing all enters Waste Water Treatment;
(5) the spherical basic carbonate copper crystal that step (4) is made is transferred in the calcining furnace to be calcined, calcining temperature is 400 ℃, make spherical plating-grade copper oxide powder, discharge simultaneously the tail gas of containing water vapor, CO2 gas in the calcination process, tail gas is processed by washing tower.
Above the present invention has been done detailed description; its purpose is to allow the personage that is familiar with this art can understand content of the present invention and is implemented; can not limit protection scope of the present 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, and all should be encompassed within protection scope of the present invention.
Claims (5)
1. the preparation method of a spherical plating-grade copper oxide powder, it is characterized in that: described preparation method may further comprise the steps:
(1) adding cupric sulfate pentahydrate and ultrapure water and the two weight ratio in reactor is 1:2 ~ 3, then is heated to 65 ℃ ~ 75 ℃ and stir it is fully dissolved, and makes copper-bath;
(2) described copper-bath is injected atomisation tower by the high-pressure atomization nozzle, after the high pressure gas atomizing, obtain spherical copper sulfate crystal drop;
(3) described spherical copper sulfate crystal drop directly enters in the reactor that aqueous sodium carbonate is housed after naturally cooling in atomisation tower, and stir, temperature of reaction is controlled between 50 ℃ ~ 80 ℃, restir reaction 10min ~ 20min after the material in described spray tower all enters reactor;
(4) with the material after step (3) reaction kettle for reaction after filtration, washing, drying, make spherical basic carbonate copper crystal, wherein, the waste water that produces after the waste water that produces after filtering and the washing all enters Waste Water Treatment;
(5) the spherical basic carbonate copper crystal that step (4) is made is transferred in the calcining furnace to be calcined, and makes spherical plating-grade copper oxide powder, discharges simultaneously containing water vapor, CO
2The tail gas of gas, described tail gas is processed by washing tower.
2. the preparation method of spherical plating-grade copper oxide powder according to claim 1, it is characterized in that: in the step (1), described cupric sulfate pentahydrate is Powdered.
3. the preparation method of spherical plating-grade copper oxide powder according to claim 1, it is characterized in that: in the 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, it is characterized in that: in the step (2), what select in the described high pressure gas atomization process 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 the described step (5) adopts is 300 ℃ ~ 500 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103739000A (en) * | 2013-12-25 | 2014-04-23 | 广州科城环保科技有限公司 | Production method of high-purity electroplating grade copper oxide |
| 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 |
| 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 |
| CN107311220A (en) * | 2017-07-07 | 2017-11-03 | 盛洪超 | A kind of cupric oxide powder and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001335320A (en) * | 2000-05-24 | 2001-12-04 | Sumitomo Metal Mining Co Ltd | Basic copper carbonate and its preparing method |
| 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 |
| JP2010143809A (en) * | 2008-12-22 | 2010-07-01 | Rasa Ind Ltd | Method for producing basic copper carbonate and basic copper carbonate |
| 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 |
-
2013
- 2013-05-23 CN CN201310193411.2A patent/CN103303961B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001335320A (en) * | 2000-05-24 | 2001-12-04 | Sumitomo Metal Mining Co Ltd | Basic copper carbonate and its preparing method |
| 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 |
| US20020053518A1 (en) * | 2000-09-04 | 2002-05-09 | Tsurumi Soda Co., Ltd. | Material for copper electroplating, method for manufacturing same and copper electroplating method |
| JP2010143809A (en) * | 2008-12-22 | 2010-07-01 | Rasa Ind Ltd | Method for producing basic copper carbonate and basic copper carbonate |
| 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 |
|---|
| GUOXING ZHU ET AL.: "Facile Fabrication and Enhanced Sensing Properties of Hierarchically Porous CuO Architectures", 《APPL. MATER. INTERFACES》 * |
| 苏黎宁等: "不同粒度纳米碱式碳酸铜的制备", 《应用化工》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103739000A (en) * | 2013-12-25 | 2014-04-23 | 广州科城环保科技有限公司 | Production method of high-purity electroplating grade 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 |
| CN107311220A (en) * | 2017-07-07 | 2017-11-03 | 盛洪超 | A kind of cupric oxide powder and preparation method thereof |
| 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 |
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