CN108531739B - A kind of method of electrodissolution high-temperature alloy waste material - Google Patents
A kind of method of electrodissolution high-temperature alloy waste material Download PDFInfo
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- CN108531739B CN108531739B CN201810540017.4A CN201810540017A CN108531739B CN 108531739 B CN108531739 B CN 108531739B CN 201810540017 A CN201810540017 A CN 201810540017A CN 108531739 B CN108531739 B CN 108531739B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/045—Leaching using electrochemical processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/16—Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
- C22B3/1608—Leaching with acyclic or carbocyclic agents
- C22B3/1658—Leaching with acyclic or carbocyclic agents of different types in admixture, e.g. with organic acids added to oximes
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Abstract
The invention discloses a kind of methods of electrodissolution high-temperature alloy waste material, belong to electrochemical technology field.For this method first using bulk high temperature alloy as anode, graphite carries out electrodissolution high temperature alloy block as cathode, using the solution of n,N-Dimethylformamide and thionyl chloride under the conditions of constant current.It is an advantage of the current invention that the rate of electrodissolution bulk high temperature alloy can be improved, while the removing rate of the alloy surface earth of positive pole is 100% compared with traditional electrolytic method, solve the problems, such as that earth of positive pole attachment alloy surface influences electrodissolution.
Description
Technical field:
The present invention relates to electrochemical technology fields, and in particular to a kind of method of electrodissolution high-temperature alloy waste material.
Background technique:
High temperature alloy, containing alloying elements such as Cr, W, Ta, has excellent high temperature strength usually using Ni or Co as matrix,
Good anti-oxidant and hot corrosion resistance, the comprehensive performances such as good fatigue behaviour, fracture toughness, is widely used in aviation
Space flight and energy field.
With the development of aerospace industry, second generation rhenium-containing single crystal super alloy starts to apply, in the alloy in addition to Ni,
Co, Cr, elements such as w also contain rare metal Re, and Re is one of element most rare in the earth earth's crust, and average content valuation is
Part per billion.Since 21st century, rhenium consumption is respectively as follows: General Electric 28%, Rolls Royce PLC
28%, Pu Hui company 12%, all for producing high temperature alloy.In recent years, since the demand of aero-engine continues to increase, Re's
Dosage increases severely, and storage level is reduced sharply with day.
The components such as high-temperature alloy blades used in aero-engine have complicated structure, what is made and used
Form large batch of waste material in the process, these waste materials can be regenerated by hydrometallurgical mode, extract Re, Co, Ni,
The pure metal element such as Ta, regeneration.Since high temperature alloy has excellent obdurability, it is difficult to be broken into fritter alloy or conjunction
Golden clast, therefore in the regenerative process of high temperature alloy, the high-efficiency dissolution of high-temperature alloy waste material is a crucial technological difficulties.
Currently, the alloyed scrap of the method dissolution bulk using electrochemistry, surface will form indissoluble during dissolution
Passivating film and adhere to the earth of positive pole, dissolution is more difficult, and solution treating capacity is larger.
Summary of the invention:
The purpose of the present invention is to provide a kind of method of electrodissolution high-temperature alloy waste material, this method can be efficiently peeled off
The earth of positive pole of alloy surface, while bulk high temperature alloy is dissolved, rate of dissolution is improved, there is preferable engineering application value and warp
Ji value.
To achieve the above object, the technical solution adopted in the present invention is as follows:
A kind of method of electrodissolution high-temperature alloy waste material, the high-temperature alloy waste material include that bulk high temperature alloy and high temperature close
Golden clast；The process of electrodissolution high-temperature alloy waste material are as follows: using bulk high temperature alloy as anode, graphite as cathode, anode with
The area ratio of cathode is 3:1-50:1, is put into electricity for the mixed liquor of n,N-Dimethylformamide and thionyl chloride as electrodissolution liquid
It is 200-800A/m in current density in dissolving tank2Under the conditions of carry out electrodissolution, to realize the dissolution of bulk high temperature alloy.
The high-temperature alloy waste material is nickel base superalloy and/or cobalt base superalloy, and such as: K417G alloy, DZ40M are closed
Gold, DD5 alloy, DD6 alloy etc..
In the electrodissolution liquid, the volume ratio of n,N-Dimethylformamide and thionyl chloride is (10-30): 1.
During the electrodissolution, thionyl chloride regularly is added into electrodissolution liquid, so that n,N-Dimethylformamide
It is maintained at (10-30) with the volume ratio of thionyl chloride: 1 range.
The bulk high temperature alloy is smoothly put into electrodissolution slot, and the cathode uses purity >=99% of graphite, institute
The distance between cathode and anode are stated greater than 13cm.
Beneficial effects of the present invention are as follows:
1, the present invention is the method for electrodissolution high temperature alloy, and the speed of electrodissolution bulk high temperature alloy can be improved in this method
Rate.
2, the method for the present invention solves the problems, such as that earth of positive pole attachment alloy surface influences electrodissolution, the alloy surface earth of positive pole
Removing rate is 100%, has preferable engineering application value and economic value.
Detailed description of the invention:
Fig. 1 puts figure for anode and cathode in electrodissolution slot before electrodissolution.
Fig. 2 is electrodissolution procedure chart of the present invention.
Fig. 3 is alloy surface after 1 electrodissolution of embodiment.
Fig. 4 is anodic product sediment figure after 1 electrodissolution of embodiment.
Specific embodiment:
It is for a more detailed description to the present invention with reference to embodiments.These embodiments are only to best implementation of the invention
The description of mode, does not have any restrictions to the scope of the present invention.
In following embodiment, anode and cathode puts figure as shown in Figure 1, electrodissolution process is as schemed in electrodissolution slot before electrodissolution
2。
Embodiment 1
Using bulk nickel-base high-temperature single crystal alloy DD5 as anode, anode weight is 1.28kg, is smoothly put into electrodissolution slot
It is interior, the graphite plate that purity is 99% is used as to cathode, the area ratio of anode and cathode is 3:1, and cathode is at a distance from anode
N,N-Dimethylformamide and thionyl chloride are mixedly configured into electrodissolution liquid according to the volume ratio of 28:1 and are put into electric molten by 23cm
It solves in slot, is 500A/m in current density2Under the conditions of carry out electrodissolution, stop test after electrodissolution 72h, take out solution weigh it is surplus
Remaining alloy block weight, calculating difference are computed bulk high temperature alloy electrodissolution 200g, and the removing rate of the alloy surface earth of positive pole is
Shown in 100%, Fig. 3.
Embodiment 2
Using bulk cobalt base superalloy DZ40M as anode, anode weight is 1.35kg, is smoothly put into electrodissolution slot
It is interior, the graphite plate that purity is 99% is used as to cathode, the area ratio of anode and cathode is 3:1, and cathode is at a distance from anode
N,N-Dimethylformamide and thionyl chloride solvent are put into electrodissolution slot according to 15:1 volume ratio configuration electrodissolution liquid by 23cm
In, it is 300A/m in current density2Under the conditions of carry out electrodissolution, stop test after electrodissolution 72h, take out solution and weigh remaining close
Gold bullion weight, calculating difference are computed bulk high temperature alloy electrodissolution 181g, and the removing rate of the alloy surface earth of positive pole is 100%.
Embodiment 3
Using bulk high temperature alloy K417G as anode, anode weight is 1.55kg, is smoothly put into electrodissolution slot, will
The graphite plate that purity is 99% is used as cathode, and the area ratio of anode and cathode is 4:1, and cathode is 23cm, general at a distance from anode
N,N-Dimethylformamide and thionyl chloride are put into electrodissolution slot according to volume ratio 10:1 mixed configuration electrodissolution liquid, in electric current
Density is 500A/m2Under the conditions of carry out electrodissolution, stop test after electrodissolution 72h, take out solution and weigh remaining alloy block weight,
Calculating difference, is computed bulk high temperature alloy electrodissolution 210g, and the removing rate of the alloy surface earth of positive pole is 100%.
Comparative example 1
Using bulky single crystal high temperature alloy DD5 as anode, anode weight is 1.28kg, is smoothly put into electrodissolution slot,
The graphite plate that purity is 99% is used as to cathode, the area ratio of anode and cathode is 3:1, and cathode is 23cm at a distance from anode,
The inorganic chloroazotic acid electrodissolution liquid of configuration is put into electrodissolution slot, is 500A/m in current density2Under the conditions of carry out electrodissolution, electricity
Stop test after dissolving 72h, take out the weight that solution weighs remaining alloy block, calculating difference is computed bulk high temperature alloy electricity
94g is dissolved, the removing rate of the alloy surface earth of positive pole is 44%.
Bulk alloy can be dissolved using electrochemistry it can be seen from meltage in above-described embodiment 1-3, compared to comparison
Example 1, electrodissolution rate of the invention are significantly higher.
High temperature alloy is in n,N-Dimethylformamide and thionyl chloride it can be seen from above-described embodiment 1-3 and comparative example 1
Fissility in solution in the more inorganic chloroazotic acid of electrodissolution is good, and the removing rate of the alloy surface earth of positive pole of the present invention is after dissolving for a long time
100%.
According to the present invention the advantages of, solves the problems, such as that earth of positive pole attachment alloy surface influences electrodissolution, has preferable work
Journey application value and economic value.
Claims (4)
1. a kind of method of electrodissolution high-temperature alloy waste material, it is characterised in that: the high-temperature alloy waste material includes that bulk high temperature closes
Gold；The process of electrodissolution high-temperature alloy waste material are as follows: using bulk high temperature alloy as anode, graphite is as cathode, anode and cathode
Area ratio be 3:1-50:1, be put into electrodissolution for the mixed liquor of n,N-Dimethylformamide and thionyl chloride as electrodissolution liquid
It is 200-800A/m in current density in slot2Under the conditions of carry out electrodissolution, to realize the dissolution of bulk high temperature alloy；
In the electrodissolution liquid, the volume ratio of n,N-Dimethylformamide and thionyl chloride is (10-30): 1.
2. the method for electrodissolution high-temperature alloy waste material according to claim 1, it is characterised in that: the high-temperature alloy waste material
For nickel base superalloy or cobalt base superalloy.
3. the method for electrodissolution high-temperature alloy waste material according to claim 1, it is characterised in that: the electrodissolution process
In, thionyl chloride regularly is added into electrodissolution liquid, so that the volume ratio of n,N-Dimethylformamide and thionyl chloride is protected
It holds at (10-30): 1 range.
4. the method for electrodissolution high-temperature alloy waste material according to claim 1, it is characterised in that: the cathode uses graphite
Purity >=99%, the distance between the cathode and anode be greater than 13cm.
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| CN111394780A (en) * | 2020-03-31 | 2020-07-10 | 中国科学院金属研究所 | Device and method for electrochemically dissolving high-temperature alloy waste by using ultrasonic-assisted rotary electrode |
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