CN107059009A - The method for moving back copper solution and recovery permalloy of permalloy - Google Patents
The method for moving back copper solution and recovery permalloy of permalloy Download PDFInfo
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- CN107059009A CN107059009A CN201710114114.2A CN201710114114A CN107059009A CN 107059009 A CN107059009 A CN 107059009A CN 201710114114 A CN201710114114 A CN 201710114114A CN 107059009 A CN107059009 A CN 107059009A
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- Prior art keywords
- permalloy
- copper
- solution
- copper solution
- nitric acid
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/44—Compositions for etching metallic material from a metallic material substrate of different composition
Abstract
Copper solution and the method for reclaiming permalloy are moved back the invention discloses copper plating permalloy, belong to alloy recovery technology field, comprise the steps of, that prepares permalloy in proportion moves back copper solution, copper plating permalloy is soaked in and moved back in copper solution, temperature control reacts, while the content of concentrated nitric acid in copper solution is moved back in control；After reaction terminates, the surface of permalloy is rinsed with saturated limewater, and dries preservation.The present invention provides a kind of method for quickly and efficiently reclaiming copper plating permalloy.
Description
Technical field
Copper solution and the method for reclaiming permalloy are moved back the present invention relates to a kind of permalloy, belongs to alloy recycling
Technical field.
Background technology
Permalloy refers to iron-nickel alloy, and the scope of its nickel content is very wide, between 35%~90%.The maximum of permalloy
Feature is that, with very high low-intensity magnetic field permeability, their saturation induction density is general between 0.6~1.0T.Due to perm
Alloy activity is stronger, therefore, and permalloy part is general in permalloy piece surface needs when being used after processing
One layer of copper is plated, to prevent it from aoxidizing, and the copper coating of outside is often stripped in waste and old permalloy removal process, so that
Recycling is subject to iron-nickel alloy in internal layer.
Copper coating stripping on permalloy matrix, generally using mechanical grinding method or chemical method such as：M-nitro
Sodium sulfonate and Cymag, concentrated nitric acid.Mechanical grinding method is difficult to hold the copper coating that the dynamics polished often not only polishes off outer layer,
And alloy bulk has also been worn and torn；And under chemical method, boil under strongly alkaline conditions move back, anode process or concentrated nitric acid method stripping
The reaction rate of copper coating is difficult to control, while can also produce corrosiveness to matrix metal itself, is caused on alloy substrate not
Produce the corrosion of pockmarks shape with can avoiding, moving back after the alloy after copper will be polished again can just be continuing with.
The content of the invention
The technical problem to be solved in the invention is how to provide a kind of quick, effective and do not interfere with inner alloy time
Receive the method used.
In order to solve the above technical problems, the technical solution adopted in the present invention is：
6~15mol/L concentrated nitric acid is added in saturation copper nitrate solution.
Technical solution of the present invention further improvement is that：Concentrated nitric acid is controlled between 7~15mol/L.
Technical solution of the present invention further improvement is that：The volume ratio of concentrated nitric acid and saturation copper nitrate is 2:1~3:1.
Technical solution of the present invention further improvement is that：Comprise the steps of, for preparing permalloy in proportion moves back copper
Solution, copper plating permalloy is soaked in and moved back in copper solution, temperature control reaction, while the content of concentrated nitric acid in copper solution is moved back in control；
After reaction terminates, the surface of permalloy is rinsed with saturated limewater, and dries preservation.
Technical solution of the present invention further improvement is that：The copper of addition plates volume ratio of the permalloy with moving back copper solution
1:25~1:40.
Technical solution of the present invention further improvement is that：It is 5 that copper, which plates reaction temperature of the permalloy in copper solution is moved back,
~30 DEG C.
Technical solution of the present invention further improvement is that：The consumption speed of copper plating permalloy copper coating in copper solution is moved back
Rate is 0.01~0.03mm/h.
Technical solution of the present invention further improvement is that：Reaction time is 10~40min.
Technical solution of the present invention further improvement is that：The temperature of the drying of permalloy is 100~120 DEG C, drying
Time is 2~3h.
By adopting the above-described technical solution, the technological progress that the present invention is obtained is：
Copper plating permalloy is soaked in special one kind and moved back in copper solution by the present invention, by control concentrated nitric acid concentration and
The temperature of reaction, ensure that permalloy outer layer copper coating dissolves；Meanwhile, the alloy substrate shape and performance of nexine are not broken
It is bad.The technique recovery permalloy method of the present invention is simple, unique, and permalloy outer layer can be easily stripped using this method
Copper coating.
Using the chemical reaction property of copper and concentrated nitric acid in the present invention, while the copper nitrate that saturation is added in system is molten
Liquid, it is to avoid the excessive velocities that simple concentrated nitric acid solution reacts with copper coating, reacts uppity phenomenon.Concentrated nitric acid it is dense
Degree is in 7~15mol/L, and the temperature control of reaction enables to concentrated nitric acid to corrode perm completely within the scope of 5~30 DEG C
Copper coating outside alloy, without having corrosion to internal iron-nickel alloy.Therefore, the copper coating of permalloy had both been stripped,
It ensure that the shape and performance of permalloy all obtain intact reservation.
What the present invention was prepared moves back the copper nitrate for depositing to get off in the copper nitrate solution containing saturation, course of reaction in copper solution
All it is to be obtained by the copper coating reaction of permalloy.By the collection to reaction product copper nitrate, weigh, can shift onto and obtain
The quality of the middle copper coating of permalloy, the forward and backward volume vs of association reaction, it can be deduced that the copper coating thickness consumed.
The control by the nitric acid copper mass to precipitating is facilitated, and then it is expected that the thickness of consumption copper coating, adds and reclaimed
To the controllability of the extent of reaction in journey.
The present invention periodically takes out in removal process and is deposited on the copper nitrate of bottom, and these copper nitrates can be again as moving back copper
Solution allocation raw material；Meanwhile, the copper nitrate purity deposited is very high can to reach HG/T3443-2014 chemical reagent standards,
By-product sale can be used as.
Embodiment
The present invention is described in further details below：
Moving back in copper solution containing the concentrated nitric acid and saturation copper nitrate solution that concentration is 6~15mol/L, dense nitre in the present invention
Acid is 2 with the volume ratio that saturation copper nitrate is added:1~3:1.
The method that permalloy is reclaimed in the present invention is as follows：First, plate permalloy according to copper and move back copper solution volume ratio
For 1:25~1:40, it is ensured that copper plating permalloy can be completely soaked in moving back in copper solution, temperature control reaction temperature is 5~30 DEG C
React 10~40min；Then, permalloy is taken out, the surface of permalloy is rinsed with water and dries preservation.The baking of permalloy
Dry temperature is 100~120 DEG C, and drying time is 2~3h.According to the size of reaction system, periodically take out and be deposited on reactor
The copper nitrate of bottom, copper nitrate can continue to serve as preparing the raw material for moving back copper solution；Meanwhile, produced according to the method for the present invention
Copper nitrate can reach HG/T3443-2014 chemical reagent standards, can also be sold as chemical reagent, produce certain economic effect
Benefit.The present invention is absorbed the nitrogen dioxide gas generated in reaction system using absorption tower, it is to avoid pollution to environment.
The copper coating thickness consumed can be released in the present invention by weighing the nitric acid copper mass deposited.
It can be calculated and obtained according to following step：
1) the copper mass m for participating in reaction is extrapolated by the copper nitrate depositedCopper, due to moving back in copper solution containing saturation
Copper nitrate, depositing obtained copper nitrate is obtained by the copper coating reaction of permalloy outer layer；
2) by following relational expressions, the thickness for the copper coating that can be reacted away：
mCopper=ρCopper(VBefore-VAfterwards)
VBeforeCopper plates the volume of permalloy before-reaction；
VAfterwardsThe volume of permalloy after-reaction；
According to calculate copper coating depletion rate be 0.01~0.03mm/h.
The present invention is described in further details with reference to embodiment：
Embodiment 1,
Prepare in the saturation copper nitrate solution containing 6mol/L nitric acid, the concentrated nitric acid of addition and the volume ratio of saturation copper nitrate
For 2:1, the volume V that copper before reaction plates permalloy is measured in advanceBefore, will be 1 with moving back copper solution volume ratio:25 permalloy leaching
Steep and moved back in above-mentioned in copper solution；The temperature of reaction is controlled at 5 DEG C, to take out alloy after reaction 40min, rinsed well with water
It is placed in drying 3 hours at 100 DEG C, measures the volume V of permalloy after reactionAfterwards, the consumption speed of copper coating is obtained according to calculating
Rate is 0.01mm/h.
The copper coating of alloy surface is completely dissolved, and alloy shape and performance all obtain intact reservation, reacts output nitre
Sour copper reaches HG/T 3443-2014 chemical reagent standards.
Embodiment 2,
Prepare in the saturation copper nitrate solution containing 7mol/L nitric acid, the concentrated nitric acid of addition and the volume ratio of saturation copper nitrate
For 3:1, the volume V that copper before reaction plates permalloy is measured in advanceBefore, will be 1 with moving back copper solution volume ratio:28 permalloy leaching
Steep and moved back in above-mentioned in copper solution；Control the temperature of reaction at 10 DEG C, to take out alloy after reaction 30min, rinse dry with water
It is net to be placed in drying 2.5 hours at 110 DEG C, measure the volume V of permalloy after reactionAfterwards, disappearing for copper coating is obtained according to calculating
Consumption speed is 0.02mm/h.
The copper coating of alloy surface is completely dissolved, and alloy shape and performance all obtain intact reservation, reacts output nitre
Sour copper reaches HG/T 3443-2014 chemical reagent standards.
Embodiment 3,
Prepare in the saturation copper nitrate solution containing 8mol/L nitric acid, the concentrated nitric acid of addition and the volume ratio of saturation copper nitrate
For 2:1, the volume V that copper before reaction plates permalloy is measured in advanceBefore, will be 1 with moving back copper solution volume ratio:30 permalloy leaching
Steep and moved back in above-mentioned in copper solution；Control the temperature of reaction at 20 DEG C, to take out alloy after reaction 30min, rinse dry with water
It is net to be placed in drying 2 hours at 110 DEG C, measure the volume V of permalloy after reactionAfterwards, the consumption of copper coating is obtained according to calculating
Speed is 0.02mm/h.
The copper coating of alloy surface is completely dissolved, and alloy shape and performance all obtain intact reservation, reacts output nitre
Sour copper reaches HG/T 3443-2014 chemical reagent standards.
Embodiment 4,
Prepare in the saturation copper nitrate solution containing 10mol/L nitric acid, the concentrated nitric acid of addition and the volume of saturation copper nitrate
Than for 3:1, the volume V that copper before reaction plates permalloy is measured in advanceBefore, will be 1 with moving back copper solution volume ratio:35 permalloy
It is soaked in above-mentioned move back in copper solution；The temperature of reaction is controlled at 30 DEG C, to take out alloy after reaction 20min, rinsed with water
It is clean to be placed in drying 2.5 hours at 115 DEG C, measure the volume V of permalloy after reactionAfterwards, copper coating is obtained according to calculating
Wear rate is 0.03mm/h.
The copper coating of alloy surface is completely dissolved, and alloy shape and performance all obtain intact reservation, reacts output nitre
Sour copper reaches HG/T 3443-2014 chemical reagent standards.
Embodiment 5,
Prepare in the saturation copper nitrate solution containing 15mol/L nitric acid, the concentrated nitric acid of addition and the volume of saturation copper nitrate
Than for 3:1, the volume V that copper before reaction plates permalloy is measured in advanceBefore, will be 1 with moving back copper solution volume ratio:40 permalloy
It is soaked in above-mentioned move back in copper solution；The temperature of reaction is controlled at 25 DEG C, to take out alloy after reaction 10min, rinsed with water
It is clean to be placed in drying 2.5 hours at 120 DEG C, measure the volume V of permalloy after reactionAfterwards, copper coating is obtained according to calculating
Wear rate is 0.02mm/h.
The copper coating of alloy surface is completely dissolved, and alloy shape and performance all obtain intact reservation, reacts output nitre
Sour copper reaches HG/T 3443-2014 chemical reagent standards.
Claims (9)
1. permalloy moves back copper solution, it is characterised in that：6~15mol/L concentrated nitric acid is added in saturation copper nitrate solution.
2. permalloy according to claim 1 moves back copper solution, it is characterised in that：Concentrated nitric acid is controlled in 7~15mol/L
Between.
3. permalloy according to claim 1 moves back copper solution, it is characterised in that：Concentrated nitric acid and saturation copper nitrate solution
Volume ratio be 2:1~3:1.
4. utilize the method that copper solution reclaims permalloy of moving back of the permalloy described in claim 3, it is characterised in that：Comprising
Following steps, permalloy is prepared in proportion moves back copper solution, and copper plating permalloy is soaked in and moved back in copper solution, temperature control is anti-
Should, while the content of concentrated nitric acid in copper solution is moved back in control；After reaction terminates, the surface of permalloy is rinsed with saturated limewater,
And dry preservation.
5. the method according to claim 4 for reclaiming permalloy, it is characterised in that：The copper of addition plates permalloy with moving back
The volume ratio of copper solution is 1:25~1:40.
6. the method according to claim 4 for reclaiming permalloy, it is characterised in that：Copper plating permalloy is moving back copper solution
In reaction temperature be 5~30 DEG C.
7. the method according to claim 6 for reclaiming permalloy, it is characterised in that：Copper plating permalloy is moving back copper solution
The wear rate of middle copper coating is 0.01~0.03mm/h.
8. the method according to claim 7 for reclaiming permalloy, it is characterised in that：Reaction time is 10~40min.
9. the method according to claim 8 for reclaiming permalloy, it is characterised in that：The temperature of the drying of permalloy is
100~120 DEG C, drying time is 2~3h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710114114.2A CN107059009B (en) | 2017-02-28 | 2017-02-28 | The method for moving back copper solution and recycle permalloy of permalloy |
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| CN201710114114.2A CN107059009B (en) | 2017-02-28 | 2017-02-28 | The method for moving back copper solution and recycle permalloy of permalloy |
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| CN107059009A true CN107059009A (en) | 2017-08-18 |
| CN107059009B CN107059009B (en) | 2019-10-29 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108188146A (en) * | 2017-12-28 | 2018-06-22 | 京磁材料科技股份有限公司 | Sintered NdFeB plates the recycling technique of Zn scrap returns |
| CN109576717A (en) * | 2018-11-29 | 2019-04-05 | 广东工业大学 | Move back copper agent and its preparation method and application in a kind of permalloy silk table face |
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| US4497687A (en) * | 1983-07-28 | 1985-02-05 | Psi Star, Inc. | Aqueous process for etching cooper and other metals |
| US4767661A (en) * | 1986-09-15 | 1988-08-30 | Psi Star | Copper etching process and product |
| CN101748408A (en) * | 2008-12-11 | 2010-06-23 | 长沙铂鲨环保设备有限公司 | Acidic copper dissolution solution |
| CN104131283A (en) * | 2014-07-15 | 2014-11-05 | 烟台恒迪克能源科技有限公司 | Electronic printed circuit board etching solution |
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Patent Citations (4)
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| US4497687A (en) * | 1983-07-28 | 1985-02-05 | Psi Star, Inc. | Aqueous process for etching cooper and other metals |
| US4767661A (en) * | 1986-09-15 | 1988-08-30 | Psi Star | Copper etching process and product |
| CN101748408A (en) * | 2008-12-11 | 2010-06-23 | 长沙铂鲨环保设备有限公司 | Acidic copper dissolution solution |
| CN104131283A (en) * | 2014-07-15 | 2014-11-05 | 烟台恒迪克能源科技有限公司 | Electronic printed circuit board etching solution |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108188146A (en) * | 2017-12-28 | 2018-06-22 | 京磁材料科技股份有限公司 | Sintered NdFeB plates the recycling technique of Zn scrap returns |
| CN109576717A (en) * | 2018-11-29 | 2019-04-05 | 广东工业大学 | Move back copper agent and its preparation method and application in a kind of permalloy silk table face |
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| CN107059009B (en) | 2019-10-29 |
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