CN108359804A - A method of it being enriched with tungsten tantalum hafnium from high-temperature alloy waste material - Google Patents
A method of it being enriched with tungsten tantalum hafnium from high-temperature alloy waste material Download PDFInfo
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- CN108359804A CN108359804A CN201810286888.8A CN201810286888A CN108359804A CN 108359804 A CN108359804 A CN 108359804A CN 201810286888 A CN201810286888 A CN 201810286888A CN 108359804 A CN108359804 A CN 108359804A
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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
- C22B7/007—Wet processes by acid leaching
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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
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/14—Obtaining zirconium or hafnium
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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
- C22B34/36—Obtaining tungsten
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The method that the invention discloses a kind of to be enriched with tungsten tantalum hafnium from high-temperature alloy waste material, this method include：One, respectively using two titanium baskets as the anode and cathode of the molten equipment of electricity, then block-like high-temperature alloy waste material is fitted into anode titanium basket, and acid solution is added into electrolytic cell and carries out acidleach processing, it is then turned on DC power supply and carries out the molten reaction of electricity, obtain the slurry containing precipitation；Two, slurry is separated by solid-liquid separation, discards supernatant liquid, collected deposit and obtain the earth of positive pole；Three, acid solution is added into the earth of positive pole and oxidant carries out oxidation acid leaching processing, tungsten tantalum hafnium enriched substance is obtained through being separated by solid-liquid separation collection deposit.The invention is directly handled high-temperature alloy waste material, pass through the selectivity efficient dissolving of the molten reaction of electricity and oxidation acid leaching, miscellaneous element and difficult separating element are removed to greatest extent, it is simultaneously effective enriched tungsten, tantalum, hafnium, method is simple, and operation is flexible, it is low for equipment requirements, process conditions are mild, and acid consumption is small, efficient and environmentally friendly.
Description
Technical field
The invention belongs to metallurgical technology fields, and in particular to a method of it being enriched with tungsten tantalum hafnium from high-temperature alloy waste material.
Background technology
High temperature alloy be manufacture aerospace engine thermal end pieces critical material, mainly by nickel, chromium, cobalt, molybdenum, aluminium,
The metallic elements such as titanium, tantalum, niobium, tungsten, ruthenium, zirconium, hafnium, platinum and iridium form, while being also large-sized power plant, such as industrial combustion gas wheel
The core material of the devices such as machine, high temperature gas-cooled nuclear reactor.The high-temperature alloy waste material of tungstenic tantalum hafnium is mainly derived from：(1) high temperature
Riser, shavings, vehicle bits for being generated in alloy preparation process etc.；(2) casting such as superalloy components, parts and forging processing production
Raw waste material；(3) superalloy components, the parts of service life are reached.With China's space flight, aviation, gas turbine, atomic energy
The rapid development in equal fields, it is increasing to the demand of high temperature alloy, while the waste material generated is also very huge, there is an urgent need for carry out
Recycling comprehensive utilization.To high temperature alloy utilization rate up to 70% or more, use is stored up or degraded to most domestic waste material, is made for foreign countries
At the huge wasting of resources and economic loss.
It is mainly wet processing that the method for high-temperature alloy waste material is handled in production.Wet processing is that high-temperature alloy waste material is pre-
Acidleach and alkali leaching are carried out after processing, make have the metal of recovery value to enter solution in the form of ion, then using chemical precipitation, electricity
One or more of solution deposition, organic solvent extraction, displacement method, ion-exchange separate mode detach Determination of Rare-Expensive Elements
Chemical method out.
Enrichment tungsten, tantalum, the research of hafnium are seldom from high-temperature alloy waste material at present, the enriching and recovering method almost all of report
It is " powder by atomization-leaching-out technique " that there are powder by atomization for this method to equipment requirement height, high energy consumption, of high cost, and is closed after powder processed
The activity at bronze end greatly improves, and leads to the shortcomings of tungsten, tantalum, hafnium are easy dispersion when leaching.Therefore from high-temperature alloy waste material
Recycling tungsten, tantalum, hafnium key be how to make tungsten, tantalum, hafnium in high-temperature alloy waste material are effectively enriched with not disperseing, and and its
The metallic elements such as its metal such as nickel, cobalt, chromium, aluminium detach.
Invention content
It is a kind of from high temperature conjunction technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, providing
The method that tungsten tantalum hafnium is enriched in golden waste material.This method is directly handled high-temperature alloy waste material, passes through the selection of the molten reaction of electricity
Property high-efficiency dissolution and oxidation acid leaching, remove miscellaneous element and difficult separating element to greatest extent, be simultaneously effective enriched tungsten, tantalum,
Hafnium, method is simple, and operation is flexible, and low for equipment requirements, process conditions are mild, and acid consumption is small, efficient and environmentally friendly.
In order to solve the above technical problems, the technical solution adopted by the present invention is：One kind being enriched with tungsten from high-temperature alloy waste material
The method of tantalum hafnium, which is characterized in that this approach includes the following steps：
Step 1: then block-like high temperature alloy is given up using two titanium baskets as the anode and cathode of the molten equipment of electricity respectively
Material is fitted into anode titanium basket, and acid solution is added into electrolytic cell and carries out acidleach processing to high-temperature alloy waste material, is then turned on direct current
Source carries out the molten reaction of electricity, obtains the slurry containing precipitation；
Step 2: the slurry obtained in step 1 is separated by solid-liquid separation, liquid is discarded supernatant, deposit is collected and obtains anode
Mud；
It is 1MPa~1.2MPa in pressure Step 3: acid solution and oxidant are added in the earth of positive pole obtained into step 2
Under conditions of carry out oxidation acid leaching processing, be then separated by solid-liquid separation, discard supernatant liquid, collected deposit and obtain the enrichment of tungsten tantalum hafnium
Object.
A kind of above-mentioned method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material, which is characterized in that high described in step 1
Contain nickel or cobalt in the ingredient of temperature alloy waste material, also contains aluminium, chromium, tungsten, tantalum and hafnium.
A kind of above-mentioned method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material, which is characterized in that sour described in step 1
Liquid is salpeter solution, a concentration of 1mol/L of the salpeter solution, the volume of the acid solution and the quality of high-temperature alloy waste material it
Than being 4:1, the unit of volume is mL, and the unit of quality is g.
A kind of above-mentioned method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material, which is characterized in that step 2 neutralization procedure
The method being separated by solid-liquid separation described in three is vacuum filtration, plate compression or natural subsidence.
A kind of above-mentioned method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material, which is characterized in that filtered described in step 2
Tungsten concentration, tantalum concentration and hafnium concentration in liquid are respectively less than 40mg/L.
A kind of above-mentioned method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material, which is characterized in that sour described in step 3
Liquid is salpeter solution, a concentration of 1.85mol/L of the salpeter solution, and the volume of the acid solution and the mass ratio of the earth of positive pole are
2:1, the unit of volume is mL, and the unit of quality is g.
A kind of above-mentioned method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material, which is characterized in that oxygen described in step 3
Agent is sodium peroxydisulfate solution, ammonium persulfate solution or sodium chlorate solution, the addition of the oxidant and the quality of the earth of positive pole
The ratio between be 1:2.4~1:3, a concentration of 200g/L~300g/L of the oxidant..
A kind of above-mentioned method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material, which is characterized in that oxygen described in step 3
The temperature for changing acidleach processing is 60 DEG C~90 DEG C, and the time is 1h~4h.
A kind of above-mentioned method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material, which is characterized in that filtered described in step 3
Tungsten concentration, tantalum concentration and hafnium concentration in liquid are respectively less than 40mg/L, the quality of nickel, cobalt, chromium and aluminium in the tungsten tantalum hafnium enriched substance
Content is respectively less than 0.4%.
Compared with the prior art, the present invention has the following advantages：
1, the present invention carries out the molten reaction of electricity to high-temperature alloy waste material first, by high-temperature alloy waste material in acid solution electrolyte
In miscellaneous element dissolution, to make the object elements such as tungsten, tantalum, hafnium be enriched in the earth of positive pole, then to the earth of positive pole carry out oxidizing acid
Leaching is handled, and is removed the difficult separating element such as nickel, cobalt, chromium and aluminium, is obtained tungsten tantalum hafnium enriched substance, made without being atomized to high-temperature alloy waste material
Powder removes miscellaneous element and difficult separation member to greatest extent directly by the selectivity efficient dissolving of the molten reaction of electricity and oxidation acid leaching
Element is simultaneously effective enriched tungsten, tantalum, hafnium, and avoids the dispersion of tungsten, tantalum, hafnium；It is equal additionally, due to the technical process of the present invention
It carries out in the solution, tungsten, tantalum, the loss consume of hafnium are less, further improve the degree of enrichment of tungsten, tantalum, hafnium.
2, tungsten, tantalum, hafnium are not only enriched in the earth of positive pole by the molten reaction process of electricity of the invention, and block-like high temperature is closed
Golden converting waste material is the granuliform earth of positive pole, promotes each element and acid solution and oxidation in oxidation acid leaching processing procedure Anodic mud
Agent comes into full contact with, and improves the dissolution efficiency of the difficult separating element such as nickel, cobalt, chromium and aluminium, improve indirectly tungsten in filter residue, tantalum,
The purity of hafnium.
3, the present invention combines the molten reaction process of electricity and oxidation acid leaching technique, can be useless to the high temperature alloy containing multiple element
Material is handled, and object element is obtained step by step by control technological parameter for the property of different elements, adaptable and suitable
It is wider with range, it is easy to spread.
4, method of the invention is simple, and operation is flexible, and low for equipment requirements, process conditions are mild, and acid consumption is small, it is efficient and
It is environmentally friendly.
Technical scheme of the present invention is described in further detail below by drawings and examples.
Description of the drawings
Fig. 1 is the process flow chart of the present invention.
Specific implementation mode
Embodiment 1
As shown in Figure 1, the present embodiment includes the following steps：
Step 1: respectively using two titanium baskets as the anode and cathode of the molten equipment of electricity, it is then that 300kg is in irregular shape
Blocky high-temperature alloy waste material is fitted into anode titanium basket, and the salpeter solution pair of a concentration of 1mol/L of 1200L is added into electrolytic cell
High-temperature alloy waste material carries out acidleach processing, is then turned on DC power supply and carries out the molten reaction of electricity, obtains the slurry containing precipitation；The height
Contain nickel, aluminium, chromium, tungsten, tantalum and hafnium in the ingredient of temperature alloy waste material；
Step 2: the slurry obtained in step 1 is carried out plate compression, filtrate is discarded, filter residue is collected and obtains the earth of positive pole；
Tungsten concentration, tantalum concentration and hafnium concentration are respectively 35mg/L, 12mg/L, 9mg/L in the filtrate；
Step 3: the salpeter solution of a concentration of 1.85mol/L of 240L is added in the 120kg earth of positive pole obtained into step 2
It is 1.0MPa in pressure, oxidation acid leaching handles 2h under conditions of temperature is 80 DEG C, then carries out true with 50kg sodium peroxydisulfate solution
Sky filters, and discards filtrate, collects filter residue and obtains tungsten tantalum hafnium enriched substance；Tungsten concentration, tantalum concentration and hafnium concentration difference in the filtrate
For 38mg/L, 18mg/L, 13mg/L, nickel in the tungsten tantalum hafnium enriched substance, cobalt, chromium, aluminium mass content be respectively 0.18%,
0.25%, 0.08%；The molten a concentration of 300g/L of the sodium peroxydisulfate.
Embodiment 2
As shown in Figure 1, the present embodiment includes the following steps：
Step 1: respectively using two titanium baskets as the anode and cathode of the molten equipment of electricity, it is then that 300kg is in irregular shape
Blocky high-temperature alloy waste material is fitted into anode titanium basket, and the salpeter solution pair of a concentration of 1mol/L of 1200L is added into electrolytic cell
High-temperature alloy waste material carries out acidleach processing, is then turned on DC power supply and carries out the molten reaction of electricity, obtains the slurry containing precipitation；The height
Contain cobalt, aluminium, chromium, tungsten, tantalum and hafnium in the ingredient of temperature alloy waste material；
Step 2: the slurry obtained in step 1 is carried out natural subsidence, liquid is discarded supernatant, deposit is collected and obtains anode
Mud；Tungsten concentration, tantalum concentration and hafnium concentration are respectively 38mg/L, 10mg/L, 11mg/L in the supernatant；
Step 3: the salpeter solution of a concentration of 1.85mol/L of 244L is added in the 122kg earth of positive pole obtained into step 2
With 40.67kg sodium chlorate solutions, oxidation acid leaching handles 1h under the conditions of pressure is 1.2MPa, is at a temperature of 90 °C, then carries out
Plate compression discards filtrate, collects filter residue and obtains tungsten tantalum hafnium enriched substance；Tungsten concentration, tantalum concentration and hafnium concentration point in the filtrate
Not Wei 37mg/L, 23mg/L, 16mg/L, cobalt in the tungsten tantalum hafnium enriched substance, chromium, aluminium mass content be respectively 0.26%,
0.30%, 0.14%；A concentration of 200g/L of the sodium chlorate solution.
Embodiment 3
As shown in Figure 1, the present embodiment includes the following steps：
Step 1: respectively using two titanium baskets as the anode and cathode of the molten equipment of electricity, it is then that 300kg is in irregular shape
Blocky high-temperature alloy waste material is fitted into anode titanium basket, and the salpeter solution pair of a concentration of 1mol/L of 1200L is added into electrolytic cell
High-temperature alloy waste material carries out acidleach processing, is then turned on DC power supply and carries out the molten reaction of electricity, obtains the slurry containing precipitation；The height
Contain nickel, aluminium, chromium, tungsten, tantalum and hafnium in the ingredient of temperature alloy waste material；
Step 2: the slurry obtained in step 1 is carried out vacuum press filtration, filtrate is discarded, filter residue is collected and obtains the earth of positive pole；
Tungsten concentration, tantalum concentration and hafnium concentration are respectively 33mg/L, 14mg/L, 7mg/L in the filtrate；
Step 3: the salpeter solution of a concentration of 1.85mol/L of 238L is added in the 119kg earth of positive pole obtained into step 2
It is 1.1MPa in pressure, oxidation acid leaching handles 4h under conditions of temperature is 60 DEG C, then carries out with 42.5kg ammonium persulfate solutions
Natural subsidence discards supernatant liquid, collects deposit and obtains tungsten tantalum hafnium enriched substance；Tungsten concentration, tantalum concentration and hafnium in the supernatant
Concentration is respectively 37mg/L, 19mg/L, 10mg/L, nickel in the tungsten tantalum hafnium enriched substance, chromium, aluminium mass content be respectively
0.35%, 0.15%, 0.12%；A concentration of 250g/L of the ammonium persulfate solution.
The above is only presently preferred embodiments of the present invention, is not imposed any restrictions to the present invention.It is every according to invention skill
Art essence still falls within technical solution of the present invention to any simple modification, change and equivalence change made by above example
Protection domain in.
Claims (9)
1. a kind of method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material, which is characterized in that this approach includes the following steps：
Step 1: then block-like high-temperature alloy waste material is filled using two titanium baskets as the anode and cathode of the molten equipment of electricity respectively
Enter in anode titanium basket, and into electrolytic cell be added acid solution to high-temperature alloy waste material carry out acidleach processing, be then turned on DC power supply into
The molten reaction of row electricity, obtains the slurry containing precipitation；
Step 2: the slurry obtained in step 1 is separated by solid-liquid separation, liquid is discarded supernatant, deposit is collected and obtains the earth of positive pole；
Step 3: acid solution and oxidant are added in the earth of positive pole obtained into step 2, in the item that pressure is 1MPa~1.2MPa
Oxidation acid leaching processing is carried out under part, is then separated by solid-liquid separation, liquid is discarded supernatant, and is collected deposit and is obtained tungsten tantalum hafnium enriched substance.
2. a kind of method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material according to claim 1, which is characterized in that step
Contain nickel or cobalt in the ingredient of high-temperature alloy waste material described in one, also contains aluminium, chromium, tungsten, tantalum and hafnium.
3. a kind of method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material according to claim 1, which is characterized in that step
Acid solution described in one is salpeter solution, and a concentration of 1mol/L of the salpeter solution, volume and the high temperature alloy of the acid solution give up
The mass ratio of material is 4:1, the unit of volume is mL, and the unit of quality is g.
4. a kind of method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material according to claim 1, which is characterized in that step
The method being separated by solid-liquid separation described in two neutralization procedures three is vacuum filtration, plate compression or natural subsidence.
5. a kind of method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material according to claim 1, which is characterized in that step
Tungsten concentration, tantalum concentration and hafnium concentration in filtrate described in two are respectively less than 40mg/L.
6. a kind of method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material according to claim 1, which is characterized in that step
Acid solution described in three is salpeter solution, a concentration of 1.85mol/L of the salpeter solution, the volume of the acid solution and the earth of positive pole
Mass ratio is 2:1, the unit of volume is mL, and the unit of quality is g.
7. a kind of method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material according to claim 1, which is characterized in that step
Oxidant described in three is sodium peroxydisulfate solution, ammonium persulfate solution or sodium chlorate solution, addition and the sun of the oxidant
The mass ratio of pole mud is 1:2.4~1:3, a concentration of 200g/L~300g/L of the oxidant.
8. a kind of method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material according to claim 1, which is characterized in that step
The temperature of the processing of oxidation acid leaching described in three is 60 DEG C~90 DEG C, and the time is 1h~4h.
9. a kind of method being enriched with tungsten tantalum hafnium from high-temperature alloy waste material according to claim 1, which is characterized in that step
Tungsten concentration, tantalum concentration and hafnium concentration in filtrate described in three are respectively less than 40mg/L, nickel, cobalt, chromium in the tungsten tantalum hafnium enriched substance
It is respectively less than 0.4% with the mass content of aluminium.
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| CN111057882A (en) * | 2019-12-31 | 2020-04-24 | 厦门钨业股份有限公司 | Method for recovering tungsten from nickel-tungsten-based alloy powder |
| CN111286617A (en) * | 2020-03-31 | 2020-06-16 | 中国科学院金属研究所 | Method for extracting ruthenium and rhenium products by using high-temperature alloy waste |
| 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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Cited By (3)
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| CN111057882A (en) * | 2019-12-31 | 2020-04-24 | 厦门钨业股份有限公司 | Method for recovering tungsten from nickel-tungsten-based alloy powder |
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