CN104294323B - Integrated treatment device and method for cleaning, reducing and drying electrolytic copper powder - Google Patents
Integrated treatment device and method for cleaning, reducing and drying electrolytic copper powder Download PDFInfo
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- CN104294323B CN104294323B CN201410553896.6A CN201410553896A CN104294323B CN 104294323 B CN104294323 B CN 104294323B CN 201410553896 A CN201410553896 A CN 201410553896A CN 104294323 B CN104294323 B CN 104294323B
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- copper powder
- electrolytic copper
- processing unit
- integrated processing
- drying integrated
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Abstract
The invention belongs to the technical field of electrolysis and particularly relates to an integrated treatment device and a method for cleaning, reducing and drying electrolytic copper powder. According to the integrated treatment device for cleaning, reducing and drying electrolytic copper powder, a filtering layer is arranged inside a cavity of the integrated treatment device, and the cavity is divided into two parts, namely, an upper part and a lower part, by virtue of the filtering layer; a material charging opening, a liquid charging opening, a gas outlet and a material outlet are respectively formed in the upper part of the cavity; and a compressed gas inlet, a liquid outlet and a filtration-suction opening are respectively formed in the lower part of the cavity. By combining a plurality of treatment processes of electrolytic copper powder into the integrated treatment device, production devices can be decreased, the labor strength of operators is reduced, the energy consumption and the loss of the product are reduced and the yield and the quality of the product are improved.
Description
Technical field
The invention belongs to electrolysis tech field, more particularly to a kind of electrolytic copper powder cleaning drying integrated processing unit of reduction
And method.
Background technology
In electrolytic copper powder production process, electrolytically generated copper powder needs many through over cleaning, drying, reduction, drying, classification etc.
Road treatment process could turn into product, and most uses is all independent unit process at present, and electrolytic copper powder is used in cleaning machine
Deionized water multipass cleaning depickling saponification after, in batches send into centrigugal swing dryer slough most of moisture, be then fed into reduction furnace after
It is continuous to dry to water content less than 0.1% and the oxygen in reduction removing copper powder under a hydrogen atmosphere, copper powder by reduction furnace it is latter as meeting
Caking closes batch packaging, it is necessary to can just proceed classification after broken, and such product needs to transmit many between multiple working procedure
It is secondary, single equipment is required for per procedure, the amount of labour is not only increased, energy resource consumption is increased, and in transmittance process
Easily there are the phenomenons such as evaporating, emitting, dripping or leaking of liquid or gas.Which part operation is merged into an equipment to be carried out, it will is reduced equipment consumption, is subtracted
Few amount of labour, there is provided productivity ratio.
The content of the invention
It is an object of the invention to provide a kind of electrolytic copper powder drying integrated processing unit of cleaning reduction and method, by multiple tracks
Treatment process merging into a single whole processing procedure, reduces the amount of labour, reduces equipment amount, and the reduction energy disappears with other auxiliary materials
Consumption, reduces the loss of product, improves productivity ratio.
To achieve these goals, the invention provides a kind of electrolytic copper powder cleaning drying integrated processing unit of reduction,
The operations such as common cleaning, drying, reduction, drying are merged into an equipment to be carried out, and this equipment has cleaning, reduction, does
The function such as dry.
A kind of electrolytic copper powder cleaning drying integrated processing unit of reduction, the device inside cavity sets one layer of filter layer,
Cavity is divided into upper and lower two parts by filter layer；Charge door, filling opening are respectively provided with the upper part of cavity, exhaust outlet, are gone out
Material mouth；Compressed gas entrance, leakage fluid dram, suction filtration mouth are respectively provided with the lower part of cavity.
Valve is respectively provided with the charge door, filling opening, exhaust outlet, discharging opening, compressed gas entrance, leakage fluid dram and suction filtration mouth
Door.
It is molten that the common nitrogen atmosphere high temperature drying reduction that electrolytic copper powder is carried out in reduction furnace is changed to reducing agent by the present invention
The chemical reduction process and fluidization dry air-flow process of immersion bubble, increase antioxidant solution immersion treatment, remove centrifugal drying
The drying process of dry machine, so cleaning reduction drying process can be carried out within one device.
A kind of application method of the electrolytic copper powder cleaning drying integrated processing unit of reduction, from the electrolysis that electrolytic cell is collected into
Copper powder is cleaned, is dehydrated, is reduced, is surface-treated and drying process respectively successively in the device cavity.
During the cleaning, electrolytic copper powder is cleaned using deionized water in the apparatus, removing institute band sulphur
Acid.
The dehydration uses suction filtration or filter-pressing process.
Copper powder is soaked using reductant solution in the reduction process.
The reducing agent is hydrazine hydrate or glucose.
Electrolytic copper powder is soaked using antioxidant solution in the surface treatment process.
The antioxidant is BTA (BTA) or aliphatic acid.
The drying process uses gas flow pattern fluidized drying technology, electrolytic copper powder is added fluidization shape with compressed gas
State, reaches the purpose for dehydrating.
The compressed gas are hot-air or inert gas.
When carrying out reduction and surface treatment process, to the electrolytic copper powder cleaning drying integrated processing unit inside cavity of reduction
Inert gas is filled with to protect electrolytic copper powder.
The present invention provide technical process be：The electrolytic copper powder product and electrolyte collected in electrolytic cell are put into electrolysis together
In the copper powder cleaning drying integrated processing unit of reduction, electrolyte is excluded by filter layer therein returns to electrolyte reservoir
In, electrolytic copper powder is stayed on filtering layer, and multipass cleaning is carried out to electrolytic copper powder using deionized water, cleans sulfuric acid therein, electricity
The solution copper powder cleaning drying integrated processing unit of reduction has suction filtration or press filtration function, and suction filtration is carried out after drained cleaning fluid is cleaned every time
Or filter-press dehydration, can reduce water consumption, improve cleaning performance.Reductant solution immersion electrolytic copper powder one is added after the completion of cleaning
Fix time, remove oxygen contained therein.Reductant solution is discharged after the completion of reduction, antioxidant solution immersion cathode copper is added
Powder certain hour, carries out anti-oxidant surface treatment.Antioxidant solution is discharged after the completion of surface treatment, from electrolytic copper powder cleaning also
Former drying integrated processing unit bottom is passed through hot compressed gas makes electrolytic copper powder enter fluidized state, carries out fluidized drying and takes off
Water, upper gas outlet connection cyclone separator and dust arrester installation, collects the dust discharged with gas.Dry certain hour electricity
Solution copper powder water content is discharged after reaching requirement from the electrolytic copper powder cleaning drying integrated side outlet of processing unit one of reduction, Zhi Houke
Classification packaging is carried out to enter sieve division and combination batch facility.
Beneficial effects of the present invention are：
The multiple working procedure of electrolytic copper powder product processing procedure is incorporated into one by the new technology and implementation that the present invention is provided
Carried out in platform equipment, the multiple devices such as original cleaning machine, drier, reduction furnace, disintegrating machine instead of by an equipment, and
The auxiliary equipment of electrolytic copper powder is transported between individual device, technical process is simplified, equipment amount is reduced, work is reduced
Amount, reduces the consumption of the energy and other auxiliary materials, reduces the loss of product, improves productivity ratio.What the present invention was provided
New technology and implementation chemical reduction procedure and fluidized drying process substitution drier and high temperature hydrogen atmosphere reduction furnace
Dry and reduction process, eliminate electrolytic copper powder by caking phenomenon and shattering process after high temperature reduction, maintain cathode copper
The dendritic structure of powder, is conducive to the production of low-apparent-density copper powder to realize.The new technology and implementation that the present invention is provided are adopted
With the method for antioxidant solution immersion treatment electrolytic copper powder surface state, the antioxygenic property of electrolytic copper powder product is improved,
Improve the quality of product.
Brief description of the drawings
Fig. 1 is the electrolytic copper powder of the present invention cleaning drying integrated processing device structure diagram of reduction；
Label in figure：1- charge doors, 2- filling openings, 3- exhaust outlets, 4- filter layers, 5- discharging openings, 6- compressed gas entrances, 7-
Leakage fluid dram, 8- suction filtration mouths.
Specific embodiment
Drying integrated processing unit and method are reduced the invention provides a kind of cleaning of electrolytic copper powder, below in conjunction with the accompanying drawings
The present invention will be further described with specific embodiment.
A kind of electrolytic copper powder cleaning drying integrated processing unit of reduction, its structure is as shown in figure 1, the device inside cavity
One layer of filter layer 4 is set, and cavity is divided into upper and lower two parts by filter layer 4；Charge door is respectively provided with the upper part of cavity
1st, filling opening 2, exhaust outlet 3, discharging opening 5；Compressed gas entrance 6, leakage fluid dram 7, suction filtration mouth are respectively provided with the lower part of cavity
8。
Divide in the charge door 1, filling opening 2, exhaust outlet 3, discharging opening 5, compressed gas entrance 6, leakage fluid dram 7 and suction filtration mouth 8
Valve is not set.
Embodiment 1
General electrolytic copper powder is divided into two batches, a collection of to be processed by common process process, and 7 times, saponification are cleaned in powder-clean machine
Clean three times afterwards, centrigugal swing dryer dries 30min, dries reductase 12 hour in reduction furnace in 480 DEG C, then by crusher in crushing,
After gas flow sizing machine classification, -200 mesh copper powder bulk loading densities of screening are 1.78g/cm3, oxygen content 565ppm, water content 0.04%；
Another batch is cleaned 5 times in the electrolytic copper powder cleaning drying integrated processing unit of reduction, mass fraction be 3% hydrazine hydrate it is water-soluble
Immersion is steeped 30min and reduces deoxygenation to copper powder, then carries out surface oxidation-resistant treatment with the BTA aqueous solution that mass fraction is 0.3%, is soaked
The bubble time is 40min.Be dehydrated once by suction filtration mode after drained liquid, then pass to 180 DEG C of hot-air make it is powder fluidising
It is dried within 20 minutes, -200 mesh products is got through sieving after copper powder material discharge, detects that its apparent density is 1.36g/
cm3, oxygen content 871ppm, water content 0.06%, by oxygen content after anti-aging experiment 20 hours be 892ppm, and existing process
Production a kind of electrolytic copper powder initial oxygen content 654ppm, by it is anti-aging experiment 20 hours after oxygen content be 1115ppm.
Embodiment 2
Low-apparent-density electrolytic copper powder is divided into two batches, a collection of to be processed by common process process, and 10 are cleaned in powder-clean machine
Cleaned three times after secondary, saponification, centrigugal swing dryer is dried reductase 12 .5 hours in drying 40min, reduction furnace in 430 DEG C, then by broken
After broken crusher machine, gas flow sizing machine classification, -200 mesh copper powder bulk loading densities of screening are 1.18g/cm3, oxygen content 765ppm, water contains
Amount 0.07%；Another batch is cleaned 5 times in the electrolytic copper powder cleaning drying integrated processing unit of reduction, and mass fraction is 3%
Hydrazine hydrate aqueous solution soak 40min to copper powder reduce deoxygenation, then carried out with the BTA aqueous solution that mass fraction is 0.3% surface resist
Oxidation processes, soak time is 60min.It is dehydrated once by suction filtration mode after drained liquid, then passes to 210 DEG C of hot-air
Make be dried within powder fluidising 40 minutes, -200 mesh products are got through sieving after copper powder material discharge, detect its apparent density
It is 0.86g/cm3, oxygen content 1023ppm, water content 0.09%, by it is anti-aging experiment 20 hours after oxygen content be 1038ppm,
And a kind of low-apparent-density electrolytic copper powder initial oxygen content 981ppm of existing technique productions, by oxygen after anti-aging experiment 20 hours
Content is 1426ppm.
Claims (12)
1. a kind of electrolytic copper powder cleaning reduces drying integrated processing unit, it is characterised in that：The device inside cavity sets one
Cavity is divided into upper and lower two parts by layer filter layer (4), filter layer (4)；Charge door is respectively provided with the upper part of cavity
(1), filling opening (2), exhaust outlet (3), discharging opening (5)；Compressed gas entrance (6), discharge opeing are respectively provided with the lower part of cavity
Mouth (7), suction filtration mouth (8).
2. a kind of electrolytic copper powder cleaning according to claim 1 reduces drying integrated processing unit, it is characterised in that：Institute
State charge door (1), filling opening (2), exhaust outlet (3), discharging opening (5), compressed gas entrance (6), leakage fluid dram (7) and suction filtration mouth (8)
On be respectively provided with valve.
3. a kind of electrolytic copper powder cleaning as claimed in claim 1 or 2 reduces the application method of drying integrated processing unit, its
It is characterised by：The electrolytic copper powder being collected into from electrolytic cell is cleaned, is dehydrated, being reduced respectively successively in the device cavity, table
Face is processed and drying process.
4. a kind of electrolytic copper powder cleaning according to claim 3 reduces the application method of drying integrated processing unit, its
It is characterised by：During the cleaning, electrolytic copper powder is cleaned using deionized water in the apparatus, removing institute band sulphur
Acid.
5. a kind of electrolytic copper powder cleaning according to claim 3 reduces the application method of drying integrated processing unit, its
It is characterised by：The dehydration uses suction filtration or filter-pressing process.
6. a kind of electrolytic copper powder cleaning according to claim 3 reduces the application method of drying integrated processing unit, its
It is characterised by：Copper powder is soaked using reductant solution in the reduction process.
7. a kind of electrolytic copper powder cleaning according to claim 3 reduces the application method of drying integrated processing unit, its
It is characterised by：Electrolytic copper powder is soaked using antioxidant solution in the surface treatment process.
8. a kind of electrolytic copper powder cleaning according to claim 3 reduces the application method of drying integrated processing unit, its
It is characterised by：The drying process uses gas flow pattern fluidized drying technology, electrolytic copper powder is added fluidization shape with compressed gas
State, reaches the purpose for dehydrating.
9. a kind of electrolytic copper powder cleaning according to claim 3 reduces the application method of drying integrated processing unit, its
It is characterised by：When carrying out reduction and surface treatment process, in the electrolytic copper powder cleaning drying integrated processing unit cavity of reduction
Portion is filled with inert gas and electrolytic copper powder is protected.
10. a kind of electrolytic copper powder cleaning according to claim 6 reduces the application method of drying integrated processing unit, its
It is characterised by：The reducing agent is hydrazine hydrate or glucose.
A kind of 11. application methods of the electrolytic copper powder cleaning drying integrated processing unit of reduction according to claim 7, its
It is characterised by：The antioxidant is BTA or aliphatic acid.
A kind of 12. application methods of the electrolytic copper powder cleaning drying integrated processing unit of reduction according to claim 8, its
It is characterised by：The compressed gas are hot-air or inert gas.
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| CN201410553896.6A CN104294323B (en) | 2014-10-17 | 2014-10-17 | Integrated treatment device and method for cleaning, reducing and drying electrolytic copper powder |
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| CN201410553896.6A CN104294323B (en) | 2014-10-17 | 2014-10-17 | Integrated treatment device and method for cleaning, reducing and drying electrolytic copper powder |
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| CN104294323B true CN104294323B (en) | 2017-05-24 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106521533B (en) * | 2016-12-07 | 2019-01-01 | 有研粉末新材料（北京）有限公司 | A kind of electrolytic copper powder continuous cleaning device and method |
| CN112808996B (en) * | 2020-12-30 | 2023-03-14 | 重庆宇泰金属材料有限公司 | Copper powder washing process |
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| US5882502A (en) * | 1992-04-01 | 1999-03-16 | Rmg Services Pty Ltd. | Electrochemical system and method |
| CN201746597U (en) * | 2010-05-10 | 2011-02-16 | 北京有色金属研究总院 | Cleaning device for electrolytic powder |
| CN102950283A (en) * | 2012-11-06 | 2013-03-06 | 昆明舒扬科技有限公司 | Preparation method for superfine silver plating copper powder used for electronic paste |
| CN103464774A (en) * | 2012-06-07 | 2013-12-25 | 荆门市格林美新材料有限公司 | Preparation method for low-agglomeration antioxidant copper nanoparticle powder |
| CN203507654U (en) * | 2013-10-23 | 2014-04-02 | 陕西天沐新材料有限公司 | Electrolyte filtering device for nickel hydrometallurgy |
| CN103768844A (en) * | 2012-10-22 | 2014-05-07 | 南京恒安树脂化学有限公司 | Suction filtration tank |
| CN203678063U (en) * | 2014-01-09 | 2014-07-02 | 安徽理工大学 | Laboratory suction filtration device |
| CN204224727U (en) * | 2014-10-17 | 2015-03-25 | 有研粉末新材料（北京）有限公司 | The drying integrated treatment unit of a kind of electrolytic copper powder cleaning reduction |
-
2014
- 2014-10-17 CN CN201410553896.6A patent/CN104294323B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5882502A (en) * | 1992-04-01 | 1999-03-16 | Rmg Services Pty Ltd. | Electrochemical system and method |
| CN201746597U (en) * | 2010-05-10 | 2011-02-16 | 北京有色金属研究总院 | Cleaning device for electrolytic powder |
| CN103464774A (en) * | 2012-06-07 | 2013-12-25 | 荆门市格林美新材料有限公司 | Preparation method for low-agglomeration antioxidant copper nanoparticle powder |
| CN103768844A (en) * | 2012-10-22 | 2014-05-07 | 南京恒安树脂化学有限公司 | Suction filtration tank |
| CN102950283A (en) * | 2012-11-06 | 2013-03-06 | 昆明舒扬科技有限公司 | Preparation method for superfine silver plating copper powder used for electronic paste |
| CN203507654U (en) * | 2013-10-23 | 2014-04-02 | 陕西天沐新材料有限公司 | Electrolyte filtering device for nickel hydrometallurgy |
| CN203678063U (en) * | 2014-01-09 | 2014-07-02 | 安徽理工大学 | Laboratory suction filtration device |
| CN204224727U (en) * | 2014-10-17 | 2015-03-25 | 有研粉末新材料（北京）有限公司 | The drying integrated treatment unit of a kind of electrolytic copper powder cleaning reduction |
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Address after: 101407 No. 12 Yanqi Nansi Street, Yanqi Economic Development Zone, Huairou District, Beijing Patentee after: Youyan Powder New Materials Co., Ltd. Address before: 101407 No. 12 Yanqi Nansi Street, Yanqi Economic Development Zone, Huairou District, Beijing Patentee before: Gripm Advanced Materials (Beijing) Co., Ltd. |
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