CN110066927A - A kind of hydrometallurgic recovery method of bulk high-temperature alloy waste material - Google Patents
A kind of hydrometallurgic recovery method of bulk high-temperature alloy waste material Download PDFInfo
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- CN110066927A CN110066927A CN201910445356.9A CN201910445356A CN110066927A CN 110066927 A CN110066927 A CN 110066927A CN 201910445356 A CN201910445356 A CN 201910445356A CN 110066927 A CN110066927 A CN 110066927A
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
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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
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/24—Obtaining niobium or tantalum
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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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/32—Obtaining chromium
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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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
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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
- C22B59/00—Obtaining rare earth metals
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- 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
- C22B7/007—Wet processes by acid leaching
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Abstract
The invention discloses a kind of hydrometallurgic recovery methods of bulk high-temperature alloy waste material, belong to field of hydrometallurgy.Bulk high-temperature alloy waste material is machined into high temperature alloy clast first by this method, it is then placed into the mixed solution of hydrochloric acid, nitric acid and distilled water, liquid-solid ratio is (5~10) mL:(1~2) g, add 2~20mL reagent A, the reagent A is one or more of oxalic acid solution, citric acid solution and hydrogen peroxide, 1~5h is dissolved under stirring condition, is further separated by solid-liquid separation after dissolution, and different element classification separation are realized.The rate of dissolution of bulk high temperature alloy can be improved in the present invention, solves passivating film to the obstruction in high temperature alloy course of dissolution and greatly improves the contact area of high temperature alloy and leachate.Meanwhile raw material of the present invention is waste and old high temperature alloy, oxalic acid, citric acid etc. are cheap and easy to get, and removal process is simply controllable, convenient for large-scale production, have good practicability and economic prospect.
Description
Technical field:
The present invention relates to technical field of wet metallurgy, and in particular to a kind of hydrometallurgic recovery side of bulk high-temperature alloy waste material
Method.
Background technique:
Currently, nearly 300,000 tons of high-temperature alloy material are consumed on international market every year, China's high-temperature alloy material annual output about 1
Ten thousand tons or so, for every annual requirement up to 20,000 tons or more, market capacity is more than 8,000,000,000 yuan.High temperature alloy is mainly used in aviation, boat
It and navigational field, and gradually expand to atomic energy, glass manufacture, petrochemical industry, metallurgy, automobile charging turbine, gas turbine
Etc. industries.
Global high temperature alloy aerospace demand surpasses 55%, and the military high temperature alloy accounting in China is up to 80%.External advanced
Aero-engine in, the dosage of high temperature alloy accounts for the ratio of total weight 40%~60%.In recent years, China's Aeronautics and Astronautics,
The fast development of navigation and power field, on the one hand increasing to the demand of high temperature alloy, high temperature alloy annual requirement is protected
Hold 15% or more growth rate.On the other hand higher and higher to the high temperature resistance requirement of high temperature alloy, often require that high temperature
Alloy uses in the environment of being higher than 1000 DEG C, in order to reach this requirement, adds refractory metal usually into high temperature alloy and closes
Gold element, such as W, Mo, Re, Ta, Nb, Zr, Hf, Ru.
High temperature alloy development is very fast, experienced the development from polycrystalline alloy, directionally solidified alloy to single crystal alloy, and monocrystalline is high
Containing 3%Re alloy without Re alloy to the second generation of the temperature alloy from the first generation, alloy of the developing deeply to the third generation containing 6%Re, with
And the forth generation alloy of 3%Ru is added on the basis of high Re.With the increase of high temperature resistant degree, the additive amount of refractory element is being held
Continuous to increase, the mass fraction of refractory element (W, Mo, Re, Ta) is 14.6% in first generation single crystal alloy in high temperature alloy, the
It is 16.4% in two generation single crystal alloys, and is then up to 20.7% in third generation single crystal alloy.Therefore high-temperature alloy waste material has
Very high comprehensive reutilization value, the especially elements such as Re, Ru, Hf are Determination of Rare-Expensive Elements, scarcity of resources, and price is high
It is expensive, seriously restrict the development of China's advanced hightemperature and aerospace cause.China is at present to dilute in high-temperature alloy waste material
The recycling consciousness of precious metal element falls behind relatively, and external rare metal returns to material utilization rate intimate 100%, and domestic utilization rate is not
To 30%, the high-temperature alloy waste material recovery processing technology and technique of actively researching and developing scientific and reasonable economy are needed.
Since high temperature alloy has excellent obdurability, it is difficult to it is broken, it is small with leachate contact area.Therefore it is closed in high temperature
During the regeneration of gold, the high-efficiency dissolution of high-temperature alloy waste material is a crucial technological difficulties.Currently, using electrochemistry
Method dissolution bulk high-temperature alloy waste material, surface will form the passivating film of indissoluble and adhere to the earth of positive pole in course of dissolution,
Dissolution is more difficult, and recovery efficiency is low and at high cost.Therefore, new technique is needed, bulk high temperature alloy rate of dissolution is being improved
While, passivating film is solved to the obstruction in high temperature alloy removal process, in favor of further isolating and purifying.
Summary of the invention:
The purpose of the present invention is to provide a kind of method of bulk high-temperature alloy waste material hydrometallurgic recovery, this method can be effective
Ground improves the contact area of high temperature alloy and leachate, while high-efficiency dissolution bulk high temperature alloy, has preferable engineer application
Value and economic value.
To achieve the above object, the technical solution adopted in the present invention is as follows:
A kind of hydrometallurgic recovery method of bulk high-temperature alloy waste material, this method are adopted using bulk high-temperature alloy waste material as raw material
Alloyed scrap is dissolved with leachate；Specifically comprise the following steps:
(1) bulk high-temperature alloy waste material is processed by clast using the method for turning；
(2) it is cleaned by ultrasonic:
It will be cleaned by ultrasonic in high temperature alloy clast ethanol solution, it is broken to obtain free of contamination high temperature alloy after vacuum dried
Bits；
(3) it leaches:
15~20g high temperature alloy clast is weighed, is dissolved in hydrochloric acid, nitric acid and distilled water under the action of magnetic agitation auxiliary
Mixed solution in, liquid-solid ratio be (5~10) mL:(1~2) g, mixing speed be 150~200r/min, then be added 2~
20mL reagent A, the reagent A are one or more of oxalic acid solution, citric acid solution and hydrogen peroxide, are dissolved under stirring condition
1~5h is filtered separation after dissolution.
The high-temperature alloy waste material is nickel base superalloy or cobalt base superalloy.
In above-mentioned steps (1), in turning process, lathe spindle revolving speed be 100~200r/min, the amount of feeding be 0.1~
0.5mm, 0.02~0.06mm/r of feed speed.
The detailed process of above-mentioned steps (2) ultrasonic cleaning are as follows: surpass high temperature alloy clast in 95vol.% ethanol solution
Sound cleaning, scavenging period are 10~20min, are put into dry 30~60min in the vacuum oven that temperature is 40~60 DEG C later,
Obtain free of contamination high temperature alloy clast.
In above-mentioned steps (3), the hydrochloric acid, oxalic acid solution and citric acid solution are complexant, the nitric acid and hydrogen peroxide
For oxidant；The concentration of the hydrogen peroxide is 20-40wt.%, and the concentration of oxalic acid solution is 2-10wt.%, citric acid solution
Concentration is 2-10wt.%.
In above-mentioned steps (3), the mixed solution is by hydrochloric acid, nitric acid and distilled water according to (3~5): (1~2): (5~
7) it is obtained after volume ratio mixing；The nitric acid that nitric acid used in mixed solution is concentration 60-70wt.% is prepared, hydrochloric acid used is
The hydrochloric acid of concentration 30-40wt.%.
Beneficial effects of the present invention are as follows:
1, bulk high temperature alloy turning is high temperature alloy clast by the present invention, and this method can greatly improve high temperature alloy
Rate of dissolution and recovery rate.
2, the method for the present invention solves the problems, such as that passivating film hinders high temperature alloy dissolution, and alloy rate of dissolution is 10g/min,
With preferable engineering application value and economic value.
3, the present invention solves passivating film and recycled to high temperature alloy while improving bulk high temperature alloy rate of dissolution
Obstruction in journey greatly improves the contact area of high temperature alloy and leachate.In leachate used in the present invention, hydrochloric acid, grass
Acid and citric acid are complexant, and the nitric acid and hydrogen peroxide are oxidant.Hydrochloric acid and nitric acid there must be, and contain oxalic acid, lemon
At least one of lemon acid and hydrogen peroxide, the complexant being added and oxidant cooperate, on the one hand can be with part metals ion shape
At stable complex, it on the other hand can promote the dissolution of the elements such as Ni, Co, Cr and Re well, further to isolate and purify
Convenience is provided.
4, the hydrometallurgy that the inventive method can also be used for the processing scrap generated in high temperature alloy part process is returned
It receives.
Detailed description of the invention:
Fig. 1 is comparison diagram before and after the turning of bulk high temperature alloy；Wherein: (a) before turning；(b) after turning.
Fig. 2 is dissolution figure after the turning of bulk high temperature alloy.
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.
The hydrometallurgic recovery method of bulk high-temperature alloy waste material of the present invention, the present invention in " bulk " refer to weight be greater than 0.1Kg
Alloy block, the high-temperature alloy waste material be nickel base superalloy or cobalt base superalloy,
The process of hydrometallurgic recovery high-temperature alloy waste material are as follows: by bulk high-temperature alloy waste material turning be high temperature alloy clast, claim
A certain amount of high temperature alloy clast being taken, with liquid-solid ratio for (5~10) mL:(1~2) ratio of g is dissolved in hydrochloric acid, nitric acid and distillation
In the mixed liquor of water, and other complexants (oxalic acid solution, citric acid solution) and oxidant (hydrogen peroxide) is added, in magnetic agitation
Under the action of make it completely dissolved, be finally separated by filtration, the dissolution rate of alloy reaches 95% or more after measured.
In following embodiment, the concentration of used oxalic acid solution is 2-10wt.%, and the concentration of citric acid solution is 2-
10wt.%；Nitric acid used is the nitric acid of concentration 60-70wt.%, and hydrochloric acid used is the hydrochloric acid of concentration 30-40wt.%.
Embodiment 1
It with revolving speed is 150r/min by 350g bulk high temperature alloy (DD5), amount of feeding 0.3mm, feed speed is
The technique turning of 0.04mm/r is high temperature alloy clast (Fig. 1), and clast is put into 95vol.% ethanol solution and is cleaned by ultrasonic 3
Secondary, each 30min is put into 40 DEG C of vacuum oven dry 30min later.
It weighs 20g high temperature alloy clast (mixing speed 180r/min) under the action of magnetic agitation auxiliary and is placed in salt
Acid, nitric acid and distilled water mixed solution in, mixed solution be by hydrochloric acid 30mL, nitric acid 10mL and water 60mL mixed preparing and
At；Then citric acid solution 6mL is added, dissolves 5h (Fig. 2) under stirring condition, filter and weigh filter residue is 5.2g, ingredient point
Analysis is as shown in table 1.
Table 1
| Element | Cr | Co | Ni | Re | Ta | W | Filter residue/g |
| Wt (%) | 5.03 | 3.90 | 16.00 | 0.60 | 38.79 | 26.58 | 5.2 |
Embodiment 2
It with revolving speed is 150r/min by 350g bulk high temperature alloy (DD5), amount of feeding 0.3mm, feed speed is
The technique turning of 0.04mm/r is high temperature alloy clast, and clast is put into 95% ethanol solution and is cleaned by ultrasonic 3 times, every time
30min is put into 40 DEG C of vacuum oven dry 30min later.
It weighs 20g superalloy powder (mixing speed 180r/min) under the action of magnetic agitation auxiliary and is placed in salt
Acid, nitric acid and distilled water mixed solution in, mixed solution be by being prepared after hydrochloric acid 36mL, nitric acid 12mL and water 72mL mixing and
At；Then oxalic acid solution 10mL is added, dissolves 5h under stirring condition, filter and weigh filter residue is 4.5g, constituent analysis such as table 2
It is shown.
Table 2
| Element | Cr | Co | Ni | Re | Ta | W | Filter residue/g |
| Wt (%) | 5.94 | 4.00 | 18.06 | 2.25 | 31.71 | 23.62 | 4.5 |
Embodiment 3
It with revolving speed is 150r/min by 350g bulk high temperature alloy (DD5), amount of feeding 0.3mm, feed speed is
The technique turning of 0.04mm/r is high temperature alloy clast, and clast is put into 95% ethanol solution and is cleaned by ultrasonic 3 times, every time
30min is put into 40 DEG C of vacuum oven dry 30min later.
It weighs 20g superalloy powder (mixing speed 180r/min) under the action of magnetic agitation auxiliary and is placed in salt
Acid, nitric acid and distilled water mixed solution in, mixed solution be by being prepared after hydrochloric acid 30mL, nitric acid 10mL and water 60mL mixing and
At；Then hydrogen peroxide 10mL and oxalic acid solution 10mL is added, dissolves 5h under stirring condition, filter and weigh filter residue is 3.2g,
Constituent analysis is as shown in table 3.
Table 3
Comparative example 1
It with revolving speed is 150r/min by 350g bulk high temperature alloy (DD5), amount of feeding 0.3mm, feed speed is
The technique turning of 0.04mm/r is high temperature alloy clast, and clast is put into 95% ethanol solution and is cleaned by ultrasonic 3 times, every time
30min is put into 40 DEG C of vacuum oven dry 30min later, weighs 20g superalloy powder in hydrochloric acid 30mL, nitric acid
Dissolve 5h in the leachate that 10mL and water 60mL are mixed, filter and weigh filter residue be 9.6g, constituent analysis such as 4 institute of table
Show.
Table 4
| Element | Cr | Co | Ni | Re | Ta | W | Filter residue/g |
| Wt (%) | 5.55 | 4.23 | 25.08 | 2.20 | 38.25 | 20.38 | 9.6 |
Bulk high-temperature alloy waste material is containing after being turned into clast it can be seen from above-described embodiment 1-3 and comparative example 1
Hydrochloric acid and nitric acid, and it is at least high containing the dissolution in a kind of leachate, the rate of recovery in oxalic acid, hydrogen peroxide and citric acid, be
Further element, which further isolates and purifies, provides simple and reliable method.
According to the present invention the advantages of solve high temperature alloy easily formed in leachate passivating film and with leachate contact surface
The small problem of product, has preferable engineering application value and economic value.
Claims (7)
1. a kind of hydrometallurgic recovery method of bulk high-temperature alloy waste material, it is characterised in that: this method is with bulk high-temperature alloy waste material
For raw material, alloyed scrap is dissolved using leachate；Specifically comprise the following steps:
(1) bulk high-temperature alloy waste material is processed by clast using the method for turning；
(2) it is cleaned by ultrasonic:
It will be cleaned by ultrasonic in high temperature alloy clast ethanol solution, obtain free of contamination high temperature alloy clast after vacuum dried；
(3) it leaches:
15~20g high temperature alloy clast is weighed, is placed in the mixed of hydrochloric acid, nitric acid and distilled water under the action of magnetic agitation auxiliary
Close in solution, liquid-solid ratio is (5~10) mL:(1~2) g, mixing speed is 150~200r/min, and 2~20mL examination is then added
Agent A, the reagent A are one or more of oxalic acid solution, citric acid solution and hydrogen peroxide, and 1~5h is dissolved under stirring condition,
It is separated by filtration after dissolution.
2. the hydrometallurgic recovery method of bulk high-temperature alloy waste material according to claim 1, it is characterised in that: the high temperature closes
Golden waste material is nickel base superalloy or cobalt base superalloy.
3. the hydrometallurgic recovery method of bulk high-temperature alloy waste material according to claim 1, it is characterised in that: in step (1),
In turning process, lathe spindle revolving speed be 100~200r/min, the amount of feeding be 0.1~0.5mm, feed speed 0.02~
0.06mm/r。
4. the hydrometallurgic recovery method of bulk high-temperature alloy waste material according to claim 1, it is characterised in that: step (2) is super
Sound cleaning detailed process are as follows: high temperature alloy clast is cleaned by ultrasonic in 95vol.% ethanol solution, scavenging period be 10~
20min is put into dry 30~60min in the vacuum oven that temperature is 40~60 DEG C later, obtains free of contamination high temperature alloy
Clast.
5. the hydrometallurgic recovery method of bulk high-temperature alloy waste material according to claim 1, it is characterised in that: in step (3),
The hydrochloric acid, oxalic acid solution and citric acid solution are complexant, and the nitric acid and hydrogen peroxide are oxidant.
6. the hydrometallurgic recovery method of bulk high-temperature alloy waste material according to claim 1 or 5, it is characterised in that: described double
The concentration of oxygen water is 20-40wt.%, and the concentration of oxalic acid solution is 2-10wt.%, and the concentration of citric acid solution is 2-10wt.%.
7. the hydrometallurgic recovery method of bulk high-temperature alloy waste material according to claim 1, it is characterised in that: in step (3),
The mixed solution is by hydrochloric acid, nitric acid and distilled water according to (3~5): (1~2): being obtained after the volume ratio mixing of (5~7)
?；The nitric acid that nitric acid used in mixed solution is concentration 60-70wt.% is prepared, hydrochloric acid used is the hydrochloric acid of concentration 30-40wt.%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111304446A (en) * | 2020-03-31 | 2020-06-19 | 中国科学院金属研究所 | Method for comprehensively utilizing high-temperature alloy waste through segmented leaching |
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| CN103233125A (en) * | 2013-04-22 | 2013-08-07 | 贵研铂业股份有限公司 | Method for extracting tungsten, molybdenum and rhenium from waste high-temperature alloy |
| CN103506018A (en) * | 2012-06-27 | 2014-01-15 | 成都光明光电股份有限公司 | Platinum-rhodium alloy dissolving reagent and method |
| CN109750167A (en) * | 2019-03-20 | 2019-05-14 | 东北大学 | A method of recycling nickel from nickel base superalloy waste cut materials |
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2019
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103506018A (en) * | 2012-06-27 | 2014-01-15 | 成都光明光电股份有限公司 | Platinum-rhodium alloy dissolving reagent and method |
| CN103233125A (en) * | 2013-04-22 | 2013-08-07 | 贵研铂业股份有限公司 | Method for extracting tungsten, molybdenum and rhenium from waste high-temperature alloy |
| CN109750167A (en) * | 2019-03-20 | 2019-05-14 | 东北大学 | A method of recycling nickel from nickel base superalloy waste cut materials |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111304446A (en) * | 2020-03-31 | 2020-06-19 | 中国科学院金属研究所 | Method for comprehensively utilizing high-temperature alloy waste through segmented leaching |
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