CN107059009B - The method for moving back copper solution and recycle permalloy of permalloy - Google Patents
The method for moving back copper solution and recycle permalloy of permalloy Download PDFInfo
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- CN107059009B CN107059009B CN201710114114.2A CN201710114114A CN107059009B CN 107059009 B CN107059009 B CN 107059009B CN 201710114114 A CN201710114114 A CN 201710114114A CN 107059009 B CN107059009 B CN 107059009B
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- permalloy
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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
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Abstract
The invention discloses the methods for moving back copper solution and recycle permalloy of copper plating permalloy, belong to alloy recovery technology field, it comprises the steps of, that prepares permalloy in proportion moves back copper solution, copper plating permalloy is soaked in and is 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, the surface of permalloy is rinsed with saturated limewater, and dries preservation.The present invention provides a kind of method of quickly and efficiently recycling copper plating permalloy.
Description
Technical field
The present invention relates to a kind of methods for moving back copper solution and recycle permalloy of permalloy, belong to alloy recovery processing
Technical field.
Background technique
Permalloy refers to iron-nickel alloy, and the range of nickel content is very wide, between 35%~90%.The maximum of permalloy
Feature is that have very high low-intensity magnetic field magnetic permeability, their saturation induction density is generally between 0.6~1.0T.Due to perm
Alloy activity is stronger, and therefore, permalloy part after processing when using generally in permalloy piece surface needs
One layer of copper is plated, to prevent its oxidation, and often to strip the copper coating of outside in waste and old permalloy removal process, thus
Recycling and reusing is subject to iron-nickel alloy in internal layer.
Copper coating stripping on permalloy matrix, generallys use mechanical grinding method or chemical method such as: m-nitro
Sodium sulfonate and Cymag, concentrated nitric acid.Mechanical grinding method is not easy to hold the copper coating that the dynamics polished often not only polishes off outer layer,
And alloy bulk is also worn；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 not easy to control, while can also generate corrosiveness to matrix metal itself, causes on alloy substrate not
The corrosion of pockmarks shape is generated avoidablely, and the alloy after moving back copper can just continue to use after polishing again.
Summary of the invention
The technical problem to be solved in the invention be how to provide it is a kind of quickly, effectively and will not influence inner alloy and return
Receive the method used.
In order to solve the above technical problems, the technical scheme adopted by the invention is that:
The concentrated nitric acid of 6~15mol/L is added in saturation copper nitrate solution.
Technical solution of the present invention further improvement lies in that: concentrated nitric acid control between 7~15mol/L.
Technical solution of the present invention further improvement lies in that: concentrated nitric acid and saturation copper nitrate volume ratio be 2:1~3:1.
Technical solution of the present invention further improvement lies in that: comprise the steps of, prepare permalloy in proportion and move back copper
Copper plating permalloy is soaked in and moves back in copper solution by solution, temperature control reaction, while the content of concentrated nitric acid in copper solution is moved back in control；
After reaction, the surface of permalloy is rinsed with saturated limewater, and dries preservation.
Technical solution of the present invention further improvement lies in that: the copper of addition plating permalloy is with the volume ratio for moving back copper solution
1:25~1:40.
Technical solution of the present invention further improvement lies in that: copper plate permalloy move back the reaction temperature in copper solution be 5
~30 DEG C.
Technical solution of the present invention further improvement lies in that: copper plate permalloy copper coating in moving back copper solution consumption speed
Rate is 0.01~0.03mm/h.
Technical solution of the present invention further improvement lies in that: the reaction time be 10~40min.
Technical solution of the present invention further improvement lies in that: the temperature of the drying of permalloy be 100~120 DEG C, drying
Time is 2~3h.
By adopting the above-described technical solution, the technological progress achieved by the present invention 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 can guarantee that permalloy outer layer copper coating dissolves；Meanwhile the alloy substrate shape and performance of inner layer are not broken
It is bad.Technique recycling permalloy method of the invention is simple, unique, can easily strip permalloy outer layer using this method
Copper coating.
The chemical reaction property of copper and concentrated nitric acid is utilized in the present invention, while the copper nitrate that joined in system saturation is molten
Liquid avoids the excessive velocities that simple concentrated nitric acid solution is reacted with copper coating, reacts phenomenon not easy to control.Concentrated nitric acid it is dense
Degree controls within the scope of 5~30 DEG C in 7~15mol/L, the temperature of reaction, enables to concentrated nitric acid that can corrode perm completely
Copper coating outside alloy, without having corrosion to internal iron-nickel alloy.Therefore, the copper coating of permalloy had both been stripped,
The shape and performance that ensure that permalloy all obtain intact reservation.
What the present invention prepared moves back the copper nitrate solution containing saturation in copper solution, deposits the copper nitrate to get off in reaction process
It is all to react to obtain by the copper coating of permalloy.By collection, the weighing to reaction product copper nitrate, can shift onto 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.
Facilitate through the control to the nitric acid copper mass to precipitate, and then it is expected that consumption copper coating thickness, increase and recycled
To the controllability of the extent of reaction in journey.
The present invention periodically takes out the copper nitrate for being deposited on bottom in removal process, these copper nitrates can be again as moving back copper
Solution allocation raw material；Meanwhile depositing that the copper nitrate purity got off is very high can to reach HG/T3443-2014 chemical reagent standard,
It can be used as by-product sale.
Specific 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
The volume ratio that acid is added with saturation copper nitrate is 2:1~3:1.
The method that permalloy is recycled in the present invention is as follows: firstly, according to copper plating permalloy and moving back copper solution volume ratio
For 1:25~1:40, guarantee for copper plating permalloy to 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 takes 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 the method according to the invention generation
Copper nitrate can reach HG/T3443-2014 chemical reagent standard, can also be used as chemical reagent sale, generate certain economic effect
Benefit.The present invention absorbs the nitrogen dioxide gas generated in reaction system using absorption tower, avoids the pollution to environment.
In the present invention copper coating thickness consumed can be released by weighing the nitric acid copper mass deposited.
It can be calculated 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, the copper nitrate deposited are reacted by the copper coating of permalloy outer layer；
2) by following relational expressions, the thickness of the available copper coating reacted away:
mCopper=ρCopper(VBefore-VAfterwards)
VBefore- react the volume that preceding copper plates permalloy；
VAfterwardsThe volume of permalloy after-reaction；
It is 0.01~0.03mm/h according to the depletion rate that copper coating is calculated.
The present invention is described in further details below with reference to embodiment:
Embodiment 1,
It prepares 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 of copper plating permalloy before reacting is measured in advanceBefore, by with move back copper solution volume ratio be 1:25 permalloy soak
It steeps and is moved back in copper solution in above-mentioned；The temperature of control reaction is to take out alloy after reacting 40min at 5 DEG C, is rinsed with water clean
It is placed at 100 DEG C and dries 3 hours, measure the volume V of permalloy after reactionAfterwards, according to the consumption speed that copper coating is calculated
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 standard.
Embodiment 2,
It prepares 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 of copper plating permalloy before reacting is measured in advanceBefore, by with move back copper solution volume ratio be 1:28 permalloy soak
It steeps and is moved back in copper solution in above-mentioned；The temperature of control reaction is to take out alloy at 10 DEG C after reacting 30min, be rinsed with water dry
Only it is placed at 110 DEG C and dries 2.5 hours, measure the volume V of permalloy after reactionAfterwards, according to disappearing for copper coating is calculated
Consumption 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 standard.
Embodiment 3,
It prepares 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 of copper plating permalloy before reacting is measured in advanceBefore, by with move back copper solution volume ratio be 1:30 permalloy soak
It steeps and is moved back in copper solution in above-mentioned；The temperature of control reaction is to take out alloy at 20 DEG C after reacting 30min, be rinsed with water dry
Only it is placed at 110 DEG C and dries 2 hours, measure the volume V of permalloy after reactionAfterwards, according to the consumption that copper coating is calculated
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 standard.
Embodiment 4,
It prepares 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, measure in advance react before copper plating permalloy volume VBefore, by with move back copper solution volume ratio be 1:35 permalloy
It is soaked in above-mentioned move back in copper solution；The temperature of control reaction is to take out alloy at 30 DEG C after reacting 20min, be rinsed with water
It is completely placed at 115 DEG C and dries 2.5 hours, measure the volume V of permalloy after reactionAfterwards, according to copper coating is calculated
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 standard.
Embodiment 5,
It prepares 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, measure in advance react before copper plating permalloy volume VBefore, by with move back copper solution volume ratio be 1:40 permalloy
It is soaked in above-mentioned move back in copper solution；The temperature of control reaction is to take out alloy at 25 DEG C after reacting 10min, be rinsed with water
It is completely placed at 120 DEG C and dries 2.5 hours, measure the volume V of permalloy after reactionAfterwards, according to copper coating is calculated
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 standard.
Claims (4)
1. a kind of method for recycling permalloy, it is characterised in that: move back copper solution recycling permalloy, institute using permalloy
The copper solution of moving back for stating permalloy is the concentrated nitric acid that 6~15mol/L is added in saturation copper nitrate solution, concentrated nitric acid and saturation nitre
The volume ratio of sour copper solution is 2:1~3:1；
It is comprised the steps of using the method for moving back copper solution recycling permalloy of permalloy, prepares permalloy in proportion
Copper solution is moved back, copper plating permalloy is soaked in and moves back in copper solution, temperature control reaction, while containing for concentrated nitric acid in copper solution is moved back in control
Amount；After reaction, the surface of permalloy is rinsed with saturated limewater, and dries preservation；
It is 5~25 DEG C that copper, which plates permalloy moving back the reaction temperature in copper solution, and the reaction time is 10~40min, permalloy
Drying temperature be 100~120 DEG C, drying time be 2~3h.
2. a kind of method for recycling permalloy according to claim 1, it is characterised in that: concentrated nitric acid control 7~
Between 15mol/L.
3. a kind of method for recycling permalloy according to claim 1, it is characterised in that: the copper of addition plates permalloy
It is 1:25~1:40 with the volume ratio for moving back copper solution.
4. a kind of method for recycling permalloy according to claim 1, it is characterised in that: copper plating permalloy is moving back copper
The wear rate of copper coating is 0.01~0.03mm/h in solution.
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| 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 |
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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2017
- 2017-02-28 CN CN201710114114.2A patent/CN107059009B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 硝酸型酸性蚀刻液蚀刻工艺的研究;李佳等;《表面技术》;20100630;第39卷(第3期);全文 * |
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