CN104294323A - 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 PDF

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Publication number
CN104294323A
CN104294323A CN201410553896.6A CN201410553896A CN104294323A CN 104294323 A CN104294323 A CN 104294323A CN 201410553896 A CN201410553896 A CN 201410553896A CN 104294323 A CN104294323 A CN 104294323A
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copper powder
electrolytic copper
integrated treatment
treatment unit
drying integrated
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CN201410553896.6A
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CN104294323B (en
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王跃发
戴赫
刘勇
张景怀
汪礼敏
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Youyan Powder New Materials Co., Ltd.
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GRIPM ADVANCED MATERIALS (BEIJING) CO Ltd
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  • Manufacture And Refinement Of Metals (AREA)
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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

A kind of electrolytic copper powder cleaning drying integrated treatment unit of reduction and method
Technical field
The invention belongs to electrolysis tech field, particularly a kind of electrolytic copper powder cleaning drying integrated treatment unit of reduction and method.
Background technology
In electrolytic copper powder production process, the copper powder that electrolysis generates needs through cleaning, dry, reduction, dry, the multiple tracks treatment process such as classification just can become product, what current majority adopted is all independently unit process, after electrolytic copper powder cleans depickling saponification with deionized water multipass in cleaning machine, send into centrigugal swing dryer in batches and slough most of moisture, then send into reduction furnace and continue to be dried to the oxygen of water-content lower than 0.1% and under a hydrogen atmosphere in reduction removing copper powder, copper powder generally can lump after reduction furnace, need after fragmentation, just can proceed classification and close batch packaging, such product needs to transmit between multiple working procedure repeatedly, every procedure all needs independent equipment, not only increase labor capacity, add energy consumption, and easily there is the phenomenons such as evaporating, emitting, dripping or leaking of liquid or gas in transmittance process.Wherein process portion is merged in an equipment and carries out, equipment consumption will be reduced, reduce labor capacity, productivity is provided.
Summary of the invention
The object of this invention is to provide a kind of electrolytic copper powder cleaning drying integrated treatment unit of reduction and method, by merging into a single whole of multiple tracks treatment process treating processes, reduce labor capacity, reduce equipment amount, reduce the consumption of the energy and other subsidiary material, reduce the loss of product, boost productivity.
To achieve these goals, the invention provides the drying integrated treatment unit of a kind of electrolytic copper powder cleaning reduction, the operations such as common cleaning, drying, reduction, drying be merged in an equipment and carry out, this equipment has the functions such as cleaning, reduction, drying.
The drying integrated treatment unit of a kind of electrolytic copper powder cleaning reduction, this device inside cavity arranges one deck filtering layer, and cavity is divided into upper and lower two parts by filtering layer; The upper part of cavity arranges charging opening, liquid adding hole, venting port, discharge port respectively; The lower part of cavity arranges compressed gas entrance, leakage fluid dram, suction filtration mouth respectively.
Described charging opening, liquid adding hole, venting port, discharge port, compressed gas entrance, leakage fluid dram and suction filtration mouth arrange valve respectively.
The present invention changes the common nitrogen atmosphere high temperature drying reduction carrying out electrolytic copper powder in reduction furnace chemical reduction process and the fluidization dry air-flow process of reductant solution immersion into, increase antioxidant solution immersion treatment, remove the drying process of centrigugal swing dryer, cleaning reduction drying process can be carried out within one device like this.
A using method for the drying integrated treatment unit of electrolytic copper powder cleaning reduction, the electrolytic copper powder collected from electrolyzer carries out respectively successively cleaning in this device cavity, dewater, reduce, surface treatment and drying process.
In described cleaning process, electrolytic copper powder uses deionized water to clean in the apparatus, removes be with sulfuric acid.
Described dehydration adopts suction filtration or filter-pressing process.
Reductant solution is adopted to soak copper powder in described reduction process.
Described reductive agent is hydrazine hydrate or glucose.
Antioxidant solution is adopted to soak electrolytic copper powder in described surface treatment process.
Described antioxidant is benzotriazole (BTA) or lipid acid.
Described drying process adopts gas flow pattern fluidized drying technology, makes electrolytic copper powder add fluidized state, reach the object dehydrated with pressurized gas.
Described pressurized gas is warm air or rare gas element.
When carrying out reduction and surface treatment process, be filled with rare gas element to the drying integrated treatment unit inside cavity of electrolytic copper powder cleaning reduction and electrolytic copper powder is protected.
Technological process provided by the invention is: the electrolytic copper powder product collected in electrolyzer puts into the drying integrated treatment unit of electrolytic copper powder cleaning reduction together with electrolytic solution, by filtering layer wherein, electrolytic solution eliminating is turned back in electrolyte reservoir, electrolytic copper powder is stayed on filtering layer, deionized water is used to carry out multipass cleaning to electrolytic copper powder, clean sulfuric acid wherein, the drying integrated treatment unit of electrolytic copper powder cleaning reduction has suction filtration or press filtration function, suction filtration or filter-press dehydration is carried out after the drained scavenging solution of each cleaning, can reduce water consumption, improve cleaning performance.Add reductant solution after having cleaned and soak electrolytic copper powder certain hour, the oxygen that removing is wherein contained.Reduce rear discharge reductant solution, then added antioxidant solution and soak electrolytic copper powder certain hour, carry out anti-oxidant surface treatment.Discharge antioxidant solution after surface treatment completes, bottom the drying integrated treatment unit of electrolytic copper powder cleaning reduction, pass into hot compressed gas makes electrolytic copper powder enter fluidized state, carry out fluidized drying dehydration, upper gas relief outlet connects cyclonic separator and dust arrester installation, collects the dust of discharging with gas.Discharge from drying integrated treatment unit one side outlet of electrolytic copper powder cleaning reduction after dry certain hour electrolytic copper powder water-content reaches requirement, sieve division and combination batch facility can be entered afterwards and carry out point grade packaged.
Beneficial effect of the present invention is:
The multiple working procedure of electrolytic copper powder product treatment process is incorporated in an equipment and carries out by novel process provided by the invention and device for carrying out said, instead of the multiple devices such as original cleaning machine, drier, reduction furnace, crusher by an equipment, and between individual device, transport the utility appliance of electrolytic copper powder, simplify technological process, decrease equipment amount, decrease labor capacity, reduce the consumption of the energy and other subsidiary material, decrease the loss of product, improve productivity.The drying of novel process provided by the invention and device for carrying out said chemical reduction procedure and fluidized drying process replacement drier and high temperature hydrogen atmosphere reduction furnace and reduction process, eliminate the caking phenomenon of electrolytic copper powder after high temperature reduction and shattering process, maintain the dendritic structure of electrolytic copper powder, the production being conducive to low-apparent-density copper powder realizes.Novel process provided by the invention and device for carrying out said adopt the method for antioxidant solution immersion treatment electrolytic copper powder condition of surface, improve the antioxidant property of electrolytic copper powder product, improve the quality of product.
Accompanying drawing explanation
Fig. 1 is the drying integrated treatment unit structural representation of electrolytic copper powder of the present invention cleaning reduction;
Number in the figure: 1-charging opening, 2-liquid adding hole, 3-venting port, 4-filtering layer, 5-discharge port, 6-compressed gas entrance, 7-leakage fluid dram, 8-suction filtration mouth.
Embodiment
The invention provides a kind of electrolytic copper powder cleaning drying integrated treatment unit of reduction and method, below in conjunction with the drawings and specific embodiments, the present invention will be further described.
The drying integrated treatment unit of a kind of electrolytic copper powder cleaning reduction, as shown in Figure 1, this device inside cavity arranges one deck filtering layer 4 to its structure, and cavity is divided into upper and lower two parts by filtering layer 4; The upper part of cavity arranges charging opening 1, liquid adding hole 2, venting port 3, discharge port 5 respectively; The lower part of cavity arranges compressed gas entrance 6, leakage fluid dram 7, suction filtration mouth 8 respectively.
Described charging opening 1, liquid adding hole 2, venting port 3, discharge port 5, compressed gas entrance 6, leakage fluid dram 7 and suction filtration mouth 8 arrange valve respectively.
Embodiment 1
General electrolytic copper powder is divided into two batches, a collection of through the process of common process process, clean three times after cleaning 7 times, saponification in powder-clean machine, centrigugal swing dryer dries in 30min, reduction furnace in 480 DEG C of dry reductase 12s hour, again after crusher in crushing, air classifier classification, screening-200 order copper powder bulk loading densities are 1.78g/cm 3, oxygen level 565ppm, water-content 0.04%; Another batch is cleaned 5 times in the drying integrated treatment unit of electrolytic copper powder cleaning reduction, massfraction be 3% hydrazine hydrate aqueous solution soak 30min deoxygenation reduced to copper powder, carry out surface oxidation-resistant process with the BTA aqueous solution that massfraction is 0.3% again, soak time is 40min.Dewater once by suction filtration mode after drained liquid, the warm air then passing into 180 DEG C makes powder fluidising 20 minutes to carry out drying, and copper powder material point obtains-200 order products through sieving after discharging, and detecting its loose density is 1.36g/cm 3, oxygen level 871ppm, water-content 0.06%, through anti-aging test after 20 hours oxygen level be 892ppm, and a kind of electrolytic copper powder initial oxygen content 654ppm of existing explained hereafter, through anti-aging test after 20 hours oxygen level be 1115ppm.
Embodiment 2
Low-apparent-density electrolytic copper powder is divided into two batches, a collection of through the process of common process process, clean three times after cleaning 10 times, saponification in powder-clean machine, centrigugal swing dryer dries in 40min, reduction furnace in 430 DEG C of dry reductase 12 .5 hour, again after crusher in crushing, air classifier classification, screening-200 order copper powder bulk loading densities are 1.18g/cm 3, oxygen level 765ppm, water-content 0.07%; Another batch is cleaned 5 times in the drying integrated treatment unit of electrolytic copper powder cleaning reduction, massfraction be 3% hydrazine hydrate aqueous solution soak 40min deoxygenation reduced to copper powder, carry out surface oxidation-resistant process with the BTA aqueous solution that massfraction is 0.3% again, soak time is 60min.Dewater once by suction filtration mode after drained liquid, the warm air then passing into 210 DEG C makes powder fluidising 40 minutes to carry out drying, and copper powder material point obtains-200 order products through sieving after discharging, and detecting its loose density is 0.86g/cm 3, oxygen level 1023ppm, water-content 0.09%, through anti-aging test after 20 hours oxygen level be 1038ppm, and a kind of low-apparent-density electrolytic copper powder initial oxygen content 981ppm of existing explained hereafter, through anti-aging test after 20 hours oxygen level be 1426ppm.

Claims (12)

1. the drying integrated treatment unit of electrolytic copper powder cleaning reduction, it is characterized in that: this device inside cavity arranges one deck filtering layer (4), cavity is divided into upper and lower two parts by filtering layer (4); The upper part of cavity arranges charging opening (1), liquid adding hole (2), venting port (3), discharge port (5) respectively; The lower part of cavity arranges compressed gas entrance (6), leakage fluid dram (7), suction filtration mouth (8) respectively.
2. the drying integrated treatment unit of a kind of electrolytic copper powder cleaning reduction according to claim 1, is characterized in that: described charging opening (1), liquid adding hole (2), venting port (3), discharge port (5), compressed gas entrance (6), leakage fluid dram (7) and suction filtration mouth (8) arrange valve respectively.
3. the using method of the drying integrated treatment unit of a kind of electrolytic copper powder cleaning reduction as claimed in claim 1 or 2, is characterized in that: the electrolytic copper powder collected from electrolyzer carries out respectively successively cleaning in this device cavity, dewater, reduce, surface treatment and drying process.
4. the using method of the drying integrated treatment unit of a kind of electrolytic copper powder cleaning reduction according to claim 3, it is characterized in that: in described cleaning process, electrolytic copper powder uses deionized water to clean in the apparatus, removes be with sulfuric acid.
5. the using method of the drying integrated treatment unit of a kind of electrolytic copper powder cleaning reduction according to claim 3, is characterized in that: described dehydration adopts suction filtration or filter-pressing process.
6. the using method of the drying integrated treatment unit of a kind of electrolytic copper powder cleaning reduction according to claim 3, is characterized in that: adopt reductant solution to soak copper powder in described reduction process.
7. the using method of the drying integrated treatment unit of a kind of electrolytic copper powder cleaning reduction according to claim 6, is characterized in that: described reductive agent is hydrazine hydrate or glucose.
8. the using method of the drying integrated treatment unit of a kind of electrolytic copper powder cleaning reduction according to claim 3, is characterized in that: adopt antioxidant solution to soak electrolytic copper powder in described surface treatment process.
9. the using method of the drying integrated treatment unit of a kind of electrolytic copper powder cleaning reduction according to claim 8, is characterized in that: described antioxidant is benzotriazole or lipid acid.
10. the using method of the drying integrated treatment unit of a kind of electrolytic copper powder cleaning reduction according to claim 3, it is characterized in that: described drying process adopts gas flow pattern fluidized drying technology, make electrolytic copper powder add fluidized state with pressurized gas, reach the object dehydrated.
The using method of the drying integrated treatment unit of 11. a kind of electrolytic copper powder cleaning reduction according to claim 10, is characterized in that: described pressurized gas is warm air or rare gas element.
The using method of the drying integrated treatment unit of 12. a kind of electrolytic copper powder cleaning reduction according to claim 3; it is characterized in that: when carrying out reduction and surface treatment process, be filled with rare gas element to the drying integrated treatment unit inside cavity of electrolytic copper powder cleaning reduction and electrolytic copper powder is protected.
CN201410553896.6A 2014-10-17 2014-10-17 Integrated treatment device and method for cleaning, reducing and drying electrolytic copper powder Active CN104294323B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106521533A (en) * 2016-12-07 2017-03-22 有研粉末新材料(北京)有限公司 Continuous washing device and method for electrolytic copper powder
CN112808996A (en) * 2020-12-30 2021-05-18 重庆宇泰金属材料有限公司 Copper powder washing process

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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
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

Patent Citations (8)

* Cited by examiner, † Cited by third party
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

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106521533A (en) * 2016-12-07 2017-03-22 有研粉末新材料(北京)有限公司 Continuous washing device and method for electrolytic copper powder
CN112808996A (en) * 2020-12-30 2021-05-18 重庆宇泰金属材料有限公司 Copper powder washing process
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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Address after: 101407 No. 12 Yanqi Nansi Street, Yanqi Economic Development Zone, Huairou District, Beijing

Patentee after: Youyan Powder New Materials Co., Ltd.

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