CN108941539A - A kind of preparation method and equipment of the silver-coated copper powder of low discharging of waste liquid - Google Patents
A kind of preparation method and equipment of the silver-coated copper powder of low discharging of waste liquid Download PDFInfo
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- CN108941539A CN108941539A CN201810652424.4A CN201810652424A CN108941539A CN 108941539 A CN108941539 A CN 108941539A CN 201810652424 A CN201810652424 A CN 201810652424A CN 108941539 A CN108941539 A CN 108941539A
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- copper powder
- silver
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- solution
- pickling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
Abstract
The invention discloses the preparation methods and equipment of a kind of silver-coated copper powder of low discharging of waste liquid.The step of preparation method, has: 1, flake copper powder pickling；2, flake copper powder is mediated, and obtains wicker copper slurry；3, wicker copper slurry squeezed, filtered；4, the wicker copper filtered is starched and is dried, the silver-coated copper powder is made.The industrialized production of silver-coated copper powder may be implemented in preparation method provided by the invention；Using atomization charging and kneading cladding when producing silver-coated copper powder, it can reduce the usage amount of solvent, realize low discharging of waste liquid and reduce the loss of copper material；Preparation process is simple, saves manpower and time, substantially increases production efficiency.
Description
Technical field
The present invention relates to the preparation process of wicker copper conductive powder more particularly to another can realize large-scale production, simultaneously
The preparation method and equipment of low discharging of waste liquid wicker copper conductive powder can be realized again.
Background technique
Industrialized production is substantially also not implemented in the production of current wicker copper conductive powder, i.e., most of still using reaction
A small amount of production of kettle progress chemical plating.Using reaction kettle carry out chemical plating production efficiency it is low, need to expend a large amount of manpower and
Time.Since reaction kettle capacity is limited, and need to be added a large amount of solution in reaction process, therefore each product amount is not
Greatly, production capacity is not caught up with.It is carried out along with reaction, there is a large amount of waste liquid to generate.Contain a certain amount of copper ion in waste liquid, in waste liquid
Copper ion be difficult to recycle, cause to waste, meanwhile, the discharging of waste liquid containing copper ion comes out, and can cause environmental pollution.
Therefore, how to overcome lacking for the low production efficiency of the preparation process of existing wicker copper, waste of material and environmental pollution
Falling into is industry urgent problem to be solved.
Summary of the invention
The present invention is in order to which the production efficiency for solving the preparation process of existing wicker copper is low, waste of material and environmental pollution are asked
Topic, propose a kind of achievable industrialized production, low discharging of waste liquid silver-coated copper powder preparation method and equipment.
A kind of preparation method of the silver-coated copper powder of low discharging of waste liquid proposed by the present invention, steps are as follows:
Step 1: flake copper powder pickling
Flake copper powder is put into the pickling tube equipped with acid solution, after stirring and pickling, waste acid liquor is discharged；Place into deionized water
After stirring and washing, waste water is discharged in the submergence flake copper powder；
Step 2: flake copper powder is mediated
The good flake copper powder of pickling is placed in kneader, revolving speed and the unlatching of built-in temperature and agitating paddle are mediated in setting,
Silver-colored solution and reducing agent solution atomization are sprayed into the kneader, so that reducing agent solution, silver-colored solution and the sheet
Copper powder mediates cladding completely, obtains wicker copper slurry；
Step 3: the wicker copper slurry being expressed in suction funnel, then the wicker copper slurry is filtered；
Step 4: the wicker copper filtered being starched and is dried, the silver-coated copper powder is made.
The invention also provides a kind of equipment of the preparation method of silver-coated copper powder using low discharging of waste liquid comprising: it is interior
Portion is equipped with the kneader of agitating paddle, and the pickling tube with movable floor, silver ammino solution charging above the kneader are spraying
Bucket and the reducing agent solution spray tank that feeds are set to set on the top inlet of pickling tube and the leakage fluid dram equipped with pickling tube lower part
Double blades blender in pickling tube, the screw extrusion apparatus with kneader outlet connection, goes out with the screw extrusion apparatus
The suction funnel that mouth connects and the vacuum pump for suction filtration, further include the baking oven for toasting the material that the suction funnel filters out.
The industrial metaplasia of silver-coated copper powder may be implemented in the preparation method of the silver-coated copper powder of low discharging of waste liquid provided by the invention
It produces, solves the problems, such as large-scale production silver-coated copper powder, can once produce the wicker copper powder of 100kg or more；Conventional wicker copper
Powder preparation process can generate a large amount of waste liquid, recycle containing a large amount of copper ion because being difficult to and cause to waste and pollute in waste liquid, this
Invention using atomization charging and mediates cladding when producing silver-coated copper powder, can reduce the usage amount of solvent, realizes low waste liquid row
Copper material loss is put and reduces, the waste discharge amount of this preparation method is the 1/4-1/2 for having reaction kettle to carry out chemical plating；Using the present invention
Preparation method prepare wicker copper powder, preparation process is fairly simple, saves manpower and time, substantially increases production efficiency.
Detailed description of the invention
Fig. 1 is the schematic diagram of silver-coated copper powder Preparation equipment proposed by the present invention.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described further.
As shown in Figure 1, the schematic diagram of the silver-coated copper powder Preparation equipment of low discharging of waste liquid proposed by the present invention.The use
The equipment of the silver-coated copper powder preparation of low discharging of waste liquid comprising: inside is equipped with the kneader 1 of agitating paddle 11, is set to the kneader 1
The pickling tube 2 with movable floor, silver ammino solution charging spray tank 3 and the reducing agent solution charging spray tank 4 of top, are set to acid
The top inlet 8 of wash pool 2 and leakage fluid dram 9 equipped with 2 lower part of pickling tube, the double blades blender in the pickling tube 2
10, the screw extrusion apparatus 5 with the kneader 1 outlet connection, the suction funnel 6 with the screw extrusion apparatus 5 outlet connection
And the vacuum pump 12 for suction filtration.It further include one for toasting the baking oven 7 for the material that the suction funnel 6 filters out.
The silver-coated copper powder Preparation equipment of low discharging of waste liquid provided by the invention is a kind of low discharging of waste liquid, efficiently preparation is set
It is standby, it is big
Generally it is divided into three parts:
1. pickling region.By two double blades blenders open pickling tubes to the stearic acid on flake copper powder surface and oxide into
Row pickling, after the residual acid on flake copper powder is rinsed with deionized water again；
2. silver ion solution and copper powder mediate conversion zone.Under conditions of high concentration, by displacement reduction method in flake copper powder
Surface grows one layer of silver layer, realizes the cladding to copper powder；
3. filtering drying area.After being covered to complete, product is filtered by filter paper and funnel, and reaction is generated a small amount of waste liquid and is filtered
Fall, finally dries.
A kind of preparation method of the silver-coated copper powder of low discharging of waste liquid provided by the invention, specific embodiment it is following (incorporated by reference to
Fig. 1):
Embodiment 1:
Step 1: flake copper powder pickling
The concentrated sulfuric acid of 0.35kg is added in the deionized water of 150kg, is configured to dilution heat of sulfuric acid.Prepared dilute sulfuric acid is molten
Liquid is added in pickling tube 2 by inlet 8.
The flake copper powder of 70kg is put into pickling tube 2, is stirred using double blades blender 10 with the revolving speed of 200-400rmp
20 minutes.The leakage fluid dram 9 of pickling tube 2 is opened, waste acid liquor is discharged.
Leakage fluid dram 9 is closed, inlet 8 is opened, with the residual acid solution on deionized water developing sheet shape copper powder.Then make
Deionized water submerged flake copper powder, after ten minutes with the revolving speed stirring of 200-400rmp, opened leakage fluid dram 9, discharge cleaning is useless
Water.
Step 2: flake copper powder is mediated
47kg silver nitrate is dissolved in 40kg deionized water, 42kg ammonium hydroxide, which is added, makes solution become clear.By prepared silver
Ammonia solution is added in silver ammino solution charging spray tank 3.
The glucose of 35kg is dissolved in the deionized water of 80kg.Prepared glucose reducing solution is added to reduction
Agent feeds in spray tank 4.
The bottom plate of 2 bottom of pickling tube twitched is opened, so that cleaned flake copper powder falls into the kneader 1 of lower section
It is interior.It adjusts kneader temperature to 50-70 DEG C and to open, agitating paddle 11 is adjusted to suitable revolving speed, flake copper powder is pinched
Close stirring.
Air compressor is adjusted, the silver ammino solution in silver ammino solution charging spray tank 3 is uniformly sprayed onto the piece in kneader 1
On shape copper powder, silver ion carries out displacement reaction on clean smooth flake copper powder surface, so that copper sheet surface grows silver-colored nucleus, silver
The mist spray time of ammonia solution controlled within half an hour.Glucose reducing solution in reducing agent charging spray tank 4 is uniformly sprayed onto
In kneader 1, to silver ammino solution carry out reduction reaction so that silver ion on flake copper powder surface along silver-colored nucleus growth, to copper sheet
It is coated.Glucose reducing solution can also spray into kneader 1 simultaneously with silver ammino solution, the mist spray of glucose reducing solution
Time controlled within 1 hour.
After the completion of silver ammino solution, the spray of glucose reducing solution mist, the silver ammino solution and glucose reducing solution and sheet
Copper powder continues stirring and mediates reaction 1 hour, so that flake copper powder kneading cladding is complete.
Step 3: the wicker copper after being covered to complete will be mediated and starched, wicker copper slurry is expressed to pumping using screw extrusion apparatus 5
It filters in funnel 6, opens vacuum pump and wicker copper slurry is filtered.
Step 4: the wicker copper filtered slurry being finally put into baking oven 7,65-85 DEG C is dried 2 hours.
The present embodiment finally obtains the silver-coated copper powder of about 100kg, generates waste liquid about 400kg, is conventional wet lay preparation silver packet
The 1/3 of the waste liquid discharging amount of copper powder.
Embodiment 2:
Step 1: flake copper powder pickling
The concentrated sulfuric acid of 0.4kg is added in the deionized water of 200kg, is configured to dilution heat of sulfuric acid.Prepared dilute sulfuric acid is molten
Liquid is added in pickling tube 2 by inlet 8.
The flake copper powder of 100kg is put into pickling tube 2, is stirred using double blades blender 10 with the revolving speed of 200-400rmp
20 minutes.The leakage fluid dram 9 of pickling tube 2 is opened, waste acid liquor is discharged.
Leakage fluid dram 9 is closed, inlet 8 is opened, with the residual acid solution on deionized water developing sheet shape copper powder.Then make
Deionized water submerged flake copper powder, after ten minutes with the revolving speed stirring of 200-400rmp, opened leakage fluid dram 9, discharge cleaning is useless
Water.
Step 2: flake copper powder is mediated
79kg silver nitrate is dissolved in 75kg deionized water, 72kg ammonium hydroxide, which is added, makes solution become clear.By prepared silver
Ammonia solution is added in silver ammino solution charging spray tank 3.
The glucose of 53kg is dissolved in the deionized water of 95kg.Prepared glucose reducing solution is added to reduction
Agent feeds in spray tank 4.
The bottom plate of 2 bottom of pickling tube twitched is opened, so that cleaned flake copper powder falls into the kneader 1 of lower section
It is interior.It adjusts kneader temperature to 50-70 DEG C and to open, agitating paddle 11 is adjusted to suitable revolving speed, flake copper powder is pinched
Close stirring.
Air compressor is adjusted, the silver ammino solution in silver ammino solution charging spray tank 3 is uniformly sprayed onto the piece in kneader 1
On shape copper powder, silver ion carries out displacement reaction on clean smooth flake copper powder surface, so that copper sheet surface grows silver-colored nucleus, silver
The mist spray time of ammonia solution controlled within half an hour.Glucose reducing solution in reducing agent charging spray tank 4 is uniformly sprayed onto
In kneader 1, to silver ammino solution carry out reduction reaction so that silver ion on flake copper powder surface along silver-colored nucleus growth, to copper sheet
It is coated.Glucose reducing solution can also spray into kneader 1 simultaneously with silver ammino solution, the mist spray of glucose reducing solution
Time controlled within 1 hour.
After the completion of silver ammino solution, the spray of glucose reducing solution mist, the silver ammino solution and glucose reducing solution and sheet
Copper powder continues stirring and mediates reaction 1 hour, so that flake copper powder kneading cladding is complete.
Step 3: the wicker copper after being covered to complete will be mediated and starched, wicker copper slurry is expressed to pumping using screw extrusion apparatus 5
It filters in funnel 6, opens vacuum pump and wicker copper slurry is filtered.
Step 4: the wicker copper filtered slurry being finally put into baking oven 7,65-85 DEG C is dried 2 hours.
The present embodiment finally obtains the silver-coated copper powder of about 150kg, generates waste liquid about 600kg, is conventional wet lay preparation silver packet
The 1/2-1/3 of the waste liquid discharging amount of copper powder.
Embodiment 3:
Step 1: flake copper powder pickling
The concentrated sulfuric acid of 0.5kg is added in the deionized water of 230kg, is configured to dilution heat of sulfuric acid.Prepared dilute sulfuric acid is molten
Liquid is added in pickling tube 2 by inlet 8.
The flake copper powder of 140kg is put into pickling tube 2, is stirred using double blades blender 10 with the revolving speed of 200-400rmp
20 minutes.The leakage fluid dram 9 of pickling tube 2 is opened, waste acid liquor is discharged.
Leakage fluid dram 9 is closed, inlet 8 is opened, with the residual acid solution on deionized water developing sheet shape copper powder.Then make
Deionized water submerged flake copper powder, after ten minutes with the revolving speed stirring of 200-400rmp, opened leakage fluid dram 9, discharge cleaning is useless
Water.
Step 2: flake copper powder is mediated
95kg silver nitrate is dissolved in 90kg deionized water, 88kg ammonium hydroxide, which is added, makes solution become clear.By prepared silver
Ammonia solution is added in silver ammino solution charging spray tank 3.
The glucose of 70kg is dissolved in the deionized water of 130kg.Prepared glucose reducing solution is added to also
In former agent charging spray tank 4.
The bottom plate of 2 bottom of pickling tube twitched is opened, so that cleaned flake copper powder falls into the kneader 1 of lower section
It is interior.It adjusts kneader temperature to 50-70 DEG C and to open, agitating paddle 11 is adjusted to suitable revolving speed, flake copper powder is pinched
Close stirring.
Air compressor is adjusted, the silver ammino solution in silver ammino solution charging spray tank 3 is uniformly sprayed onto the piece in kneader 1
On shape copper powder, silver ion carries out displacement reaction on clean smooth flake copper powder surface, so that copper sheet surface grows silver-colored nucleus, silver
The mist spray time of ammonia solution controlled within half an hour.Glucose reducing solution in reducing agent charging spray tank 4 is uniformly sprayed onto
In kneader 1, to silver ammino solution carry out reduction reaction so that silver ion on flake copper powder surface along silver-colored nucleus growth, to copper sheet
It is coated.Glucose reducing solution can also spray into kneader 1 simultaneously with silver ammino solution, the mist spray of glucose reducing solution
Time controlled within 1 hour.
After the completion of silver ammino solution, the spray of glucose reducing solution mist, the silver ammino solution and glucose reducing solution and sheet
Copper powder continues stirring and mediates reaction 1 hour, so that flake copper powder kneading cladding is complete.
Step 3: the wicker copper after being covered to complete will be mediated and starched, wicker copper slurry is expressed to pumping using screw extrusion apparatus 5
It filters in funnel 6, opens vacuum pump and wicker copper slurry is filtered.
Step 4: the wicker copper filtered slurry being finally put into baking oven 7,65-85 DEG C is dried 2 hours.
The present embodiment finally obtains the silver-coated copper powder of about 200kg, generates waste liquid about 700kg, is conventional wet lay preparation silver packet
The 1/3-1/4 of the waste liquid discharging amount of copper powder.
As needed, the dilution heat of sulfuric acid that acid content is 0.25-0.4% can be selected in acid solution of the invention.Silver ammino solution by
The weight ratio of following raw materials according is formulated: silver nitrate 47-50kg: deionized water 35-40kg: ammonium hydroxide 45-50kg.Reducing agent by
The weight ratio of following raw materials according is formulated: glucose 12-16kg: deionized water 20-30kg.In flake copper powder acid pickling step, acid
The revolving speed for washing stirring and cleaning stirring is 200-400rmp；Pickling mixing time is 15-30 minutes.Kneader temperature is adjusted to
40-70℃.The mist spray time of silver ammino solution is 0.5-1 hours；Reducing agent mist sprays the time in 1 hour.Silver ammino solution, reduction
After the completion of the spray of agent mist, the silver ammino solution, reducing agent continue to mediate with the flake copper powder reacts 1 hour.
Industrialized production may be implemented in the preparation method of silver-coated copper powder provided by the invention；It is used when producing silver-coated copper powder
Atomization charging and kneading cladding, can reduce the usage amount of solvent, realize low discharging of waste liquid and reduce the loss of copper material；Preparation
Simple process saves manpower and time, substantially increases production efficiency.
Embodiment described above is primarily to illustrate creating conception of the invention, it is noted that for this field
Those of ordinary skill for, without departing from the inventive concept of the premise, various modifications and improvements can be made, these are all
It belongs to the scope of protection of the present invention.
Claims (10)
1. a kind of preparation method of the silver-coated copper powder of low discharging of waste liquid comprising following steps:
Step 1: flake copper powder pickling
Flake copper powder is put into the pickling tube equipped with acid solution, after stirring and pickling, waste acid liquor is discharged；Place into deionized water
After stirring and washing, waste water is discharged in the submergence flake copper powder；
Step 2: flake copper powder is mediated
The good flake copper powder of pickling is placed in kneader, the revolving speed of the temperature and agitating paddle in kneader is set and is opened
It opens, silver-colored solution and reducing agent solution atomization is sprayed into the kneader, so that reducing agent solution, silver-colored solution and the piece
Shape copper powder mediates cladding completely, obtains wicker copper slurry；
Step 3: the wicker copper slurry being expressed in suction funnel, then the wicker copper slurry is filtered；
Step 4: the wicker copper filtered being starched and is dried, the silver-coated copper powder is made.
2. preparation method as described in claim 1, which is characterized in that the acid solution is that acid content is 0.25-0.4%
Dilution heat of sulfuric acid.
3. preparation method as described in claim 1, which is characterized in that the silver ammino solution is matched by the weight ratio of following raw materials according
It makes: silver nitrate 47-50kg: deionized water 35-40kg: ammonium hydroxide 45-50kg.
4. preparation method as described in claim 1, which is characterized in that the reducing agent is prepared by the weight ratio of following raw materials according
It forms: glucose 12-16kg: deionized water 20-30kg.
5. preparation method as described in claim 1, which is characterized in that in the flake copper powder acid pickling step, pickling stirring
Revolving speed with cleaning stirring is 200-400rmp；Pickling mixing time is 15-30 minutes.
6. preparation method as described in claim 1, which is characterized in that the kneader temperature is adjusted to 40-70 DEG C.
7. preparation method as described in claim 1, which is characterized in that the mist spray time of the silver ammino solution is 0.5-1 hours；
Reducing agent mist sprays the time in 1 hour.
8. preparation method as described in claim 1, which is characterized in that described after the completion of the silver ammino solution, the spray of reducing agent mist
Silver ammino solution, reducing agent and the flake copper powder continue to mediate and react 1 hour.
9. preparation method as described in claim 1, which is characterized in that the wicker copper is starched at 70 DEG C, is dried 2 hours.
10. a kind of equipment using the preparation method of low discharging of waste liquid described in claim 1, which is characterized in that set including inside
There is the kneader (1) of agitating paddle (11), pickling tube (2), the silver ammino solution with movable floor being set to above the kneader (1)
It feeds spray tank (3) and reducing agent solution feeds spray tank (4), be set to the top inlet (8) of the pickling tube (2), be set to
The leakage fluid dram (9) of pickling tube (2) lower part；
Double blades blender (10) in the pickling tube (2) is filled with the Screw Extrusion of the kneader (1) outlet connection
(5) are set, further include one with the suction funnel (6) of the screw extrusion apparatus (5) outlet connection and for the vacuum pump (12) of suction filtration
For toasting the baking oven (7) for the material that the suction funnel (6) filters out.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810652424.4A CN108941539B (en) | 2018-06-22 | 2018-06-22 | Preparation method and equipment of silver-coated copper powder with low waste liquid discharge |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810652424.4A CN108941539B (en) | 2018-06-22 | 2018-06-22 | Preparation method and equipment of silver-coated copper powder with low waste liquid discharge |
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| Publication Number | Publication Date |
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| CN108941539A true CN108941539A (en) | 2018-12-07 |
| CN108941539B CN108941539B (en) | 2020-09-15 |
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| CN201810652424.4A Active CN108941539B (en) | 2018-06-22 | 2018-06-22 | Preparation method and equipment of silver-coated copper powder with low waste liquid discharge |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114101665A (en) * | 2021-11-15 | 2022-03-01 | 深圳市绚图新材科技有限公司 | Preparation method of silver-coated copper conductive powder |
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| CN202343938U (en) * | 2011-12-14 | 2012-07-25 | 华中科技大学 | Continuous manufacturing and original-position wrapping device for metal nanometer materials apt to be oxidized |
| CN102825258A (en) * | 2012-08-27 | 2012-12-19 | 淮北五星铝业有限公司 | Manufacturing method of electroplating aluminum paste |
| JP2013204050A (en) * | 2012-03-27 | 2013-10-07 | Hitachi Zosen Corp | Method for producing metal sintered compact |
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| CN102328076A (en) * | 2011-06-20 | 2012-01-25 | 宁波广博纳米新材料股份有限公司 | Preparation method of silver coated copper powder for electronic slurry |
| CN202343938U (en) * | 2011-12-14 | 2012-07-25 | 华中科技大学 | Continuous manufacturing and original-position wrapping device for metal nanometer materials apt to be oxidized |
| JP2013204050A (en) * | 2012-03-27 | 2013-10-07 | Hitachi Zosen Corp | Method for producing metal sintered compact |
| CN102825258A (en) * | 2012-08-27 | 2012-12-19 | 淮北五星铝业有限公司 | Manufacturing method of electroplating aluminum paste |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114101665A (en) * | 2021-11-15 | 2022-03-01 | 深圳市绚图新材科技有限公司 | Preparation method of silver-coated copper conductive powder |
| CN114101665B (en) * | 2021-11-15 | 2023-08-29 | 深圳市绚图新材科技有限公司 | Preparation method of silver-coated copper conductive powder |
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| CN108941539B (en) | 2020-09-15 |
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