CN107974557A - A kind of method that rhenium is extracted from rich rhenium slag - Google Patents
A kind of method that rhenium is extracted from rich rhenium slag Download PDFInfo
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- CN107974557A CN107974557A CN201711260095.0A CN201711260095A CN107974557A CN 107974557 A CN107974557 A CN 107974557A CN 201711260095 A CN201711260095 A CN 201711260095A CN 107974557 A CN107974557 A CN 107974557A
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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
- C22B1/02—Roasting 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
- C22B61/00—Obtaining metals not elsewhere provided for in this subclass
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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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- 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 present invention provides a kind of method that rhenium is extracted from rich rhenium slag, comprise the following steps：A) rich rhenium slag is mixed with sodium hydrate aqueous solution, obtains mixed material, the mixed material is roasted, obtains fired slags；B the fired slags) are subjected to water logging, obtain leachate and leached mud；By the leachate and the substance reaction containing calcium ion, filter residue A and filtrate A are obtained after filtering；C calcium remover) is added in the filtrate A, filter residue B and liquor B are obtained after filtering；D) liquor B is concentrated, is crystallized, obtains rehenic acid ammonium.The method that rhenium is extracted from rich rhenium slag that the application provides is simple, and Rhenium recovery is high, and the effective separation for realizing arsenic and copper, rhenium, avoids the secondary pollution caused by arsenic.
Description
Technical field
The present invention relates to the technical field of dissipated metal extraction, more particularly to a kind of method that rhenium is extracted from rich rhenium slag.
Background technology
Rhenium belongs to dissipated metal, its content in the earth's crust very low-about 10-9.Due to the high dispersion of rhenium, end mesh
It is preceding not find self-existent rhenium mineral in nature.The rhenium-containing mineral having now found that are mainly molybdenite and sulphur copper mine,
Also there is minimal amount of distribution in some platinum ores, columbite and uranium mineral.Since rhenium has high temperature resistant, high density, high resistivity etc.
Physical property and good chemical property, have highlighted the excellent specific property such as the catalytic of rhenium, high temperature resistant, corrosion-resistant, therefore in stone
Oil refines the fields such as catalytic cracking, electrothermal alloy, electronic tubular construction material, aerospace specific alloy material and environmental protection
Have a wide range of applications.
In order to effectively recycle rhenium metal, successively have been reported that from molybdenum and smelt and recycle rhenium during Copper making；Publication No.
The Chinese patent of CN102628110A discloses a kind of method that rhenium is recycled in spent acid from Copper making, it is to add thiosulfate
Enter in Copper making spent acid, filter after reaction, filter residue is rich rhenium concentrate.And how from the material of rhenium-containing to extract valuable metal
Rhenium becomes the object of domestic and international researcher concern；The Chinese patent of Application No. 201210099836.2 discloses a kind of from rhenium essence
The method that rhenium is recycled in ore deposit；The patent is to carry out calcification to the rhenium in rhenium concentrate, arsenic etc. using addition quick lime roasting, is allowed to become
Into rehenic acid calcium soluble easily in water and calcium arsenate not soluble in water, to reach the separation of rhenium and copper, arsenic in rhenium concentrate, but this method
Since the quick lime of use does not have volatility, the arsenic to volatilize during roasting can not react and enter flue gas, easily make
Into smoke pollution.Therefore, a kind of better method processing rhenium-containing material how is provided, it is the present invention to be specifically similar to rhenium concentrate
Problem to be solved.
The content of the invention
Present invention solves the technical problem that in a kind of method that rhenium is extracted from rich rhenium slag of offer, the side that the application provides
Method can realize the extraction of rhenium, and can avoid the secondary pollution of arsenic.
In view of this, this application provides a kind of method that rhenium is extracted from rich rhenium slag, comprise the following steps：
A), rich rhenium slag is mixed with sodium hydrate aqueous solution, obtains mixed material, the mixed material is roasted, is obtained
Fired slags；
B), the fired slags are subjected to water logging, obtain leachate and leached mud；By the leachate and contain calcium ion
Substance reaction, obtains filter residue A and filtrate A after filtering；
C), calcium remover is added in the filtrate A, filter residue B and liquor B are obtained after filtering；
D), the liquor B concentrated, crystallized, obtain rehenic acid ammonium.
Preferably, step A) in, further included before the mixing：
The rich rhenium slag is washed, makes pH >=6 of the rich rhenium slag after washing.
Preferably, the mass ratio of the rich rhenium slag and the sodium hydroxide in the sodium hydrate aqueous solution is 1：(0.6~
0.8)。
Preferably, the temperature of the roasting is 450~750 DEG C, and the time is 3~5h.
Preferably, the liquid-solid ratio of the water logging is (2~5)：1, the time of the water logging is 1.5~3h, the water logging
Temperature is 120~150 DEG C.
Preferably, step B) in, the quality of arsenic and calcium ion in the material containing calcium ion in the leachate
Mass ratio is 1：(1~1.2).
Preferably, the material containing calcium ion is calcium hydroxide.
Preferably, the calcium remover is ammonium carbonate or ammonium hydrogen carbonate.
Preferably, the addition of the calcium remover is according to carbonate matter in calcium ion in the filtrate A and the calcium remover
Amount is than being 1：(2~3) add.
Preferably, the rich rhenium slag includes the Re of 0.8~10wt%, the As of 0.5~20wt%, the Cu of 8~30wt%
With the S of 20~70wt%.
This application provides a kind of method that rhenium is extracted from rich rhenium slag, it is first by rich rhenium slag and sodium hydrate aqueous solution
Mixing, to improve mixed effect so that the element in rich rhenium slag reacts more abundant with sodium hydroxide, then passes through follow-up roasting
Burn, the arsenic in rich rhenium slag is converted into arsenate soluble easily in water, rhenium is converted into rhenate soluble easily in water, and copper is converted into insoluble
Precipitated in the Kocide SD of water；Then by water logging, copper is made to stay in leached mud, arsenic enters in solution with rhenium, in leached mud
The content of arsenic is extremely low, avoids the return copper metallurgy industry arsenic of slag containing arsenic and pollutes；Added again in leachate and contain calcium ion
Material, make arsenate generation arsenic acid calcium precipitate separated with rhenate, the fabulous separation for realizing arsenic and rhenium, obtains pole containing arsenic
High calcium arsenate slag；Then add calcium remover in the solution after arsenic removal, generate precipitation of calcium carbonate, with remove calcium therein from
Son, obtains the Ammonium rhenate solution of very high purity；Condensing crystallizing is finally carried out, that is, obtains the very high rehenic acid ammonium of purity.In the application
State that the technique of recycling rhenium is simple, and the recycling of rhenium is high, and effectively realize the separation of arsenic and copper, rhenium, avoid two caused by arsenic
Secondary pollution.
Embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, still
It should be appreciated that these descriptions are simply further explanation the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
During rhenium being recycled for the prior art, the problem of arsenic is volatile to cause secondary pollution, and Rhenium recovery is relatively low, this
Inventive embodiments disclose a kind of method that rhenium is extracted from rich rhenium slag, and this method can realize the separation of arsenic, copper and rhenium, and arsenic is formed
A kind of arsenic acid calcium precipitate of stabilization, copper precipitation return to copper metallurgy industry, thus avoid the evil that arsenic is again introduced into copper metallurgy industry
Property circulation, calcium arsenate can open a way as the material of arsenic, the content of arsenic in reduction system, and not cause secondary pollution, realize
Effective recycling of rhenium.Specifically, this application provides a kind of method that rhenium is extracted in concentrate from rhenium, comprise the following steps：
A), rich rhenium slag is mixed with sodium hydrate aqueous solution, obtains mixed material, the mixed material is roasted, is obtained
Fired slags；
B), the fired slags are subjected to water logging, obtain leachate and leached mud；By the leachate and contain calcium ion
Substance reaction, obtains filter residue A and filtrate A after filtering；
C), calcium remover is added in the filtrate A, filter residue B and liquor B are obtained after filtering；
D), the liquor B concentrated, crystallized, obtain rehenic acid ammonium.
During said extracted rhenium, the application first mixes the rich rhenium slag with sodium hydrate aqueous solution, obtains
Mixed material；, it is necessary to which the rich rhenium slag is washed before above-mentioned mixing, to lower the acidity of the rich rhenium slag, make institute
State pH >=6 of rich rhenium slag；Sodium hydroxide is added to the water at the same time, forms sodium hydrate aqueous solution.The sodium hydroxide with it is described
The mass ratio of rich rhenium slag is (0.6~0.8)：1.The application first mixes sodium hydrate aqueous solution with the rich rhenium slag, favorably
It is uniformly mixed in both, to improve the reaction rate and reaction efficiency of element and sodium hydroxide in rich rhenium slag.In the richness rhenium slag
The S of the As of Re, 0.5~20wt%, the Cu of 8~30wt% and 20~70wt% including 0.8~10wt%.
According to the present invention, then the mixed material is roasted, obtains fired slags；During roasting, rich rhenium
The elements such as arsenic, rhenium and copper in slag react, and are specifically that sodium hydroxide is reacted with rhenium concentrate solid, while sodium hydroxide
Aqueous solution volatilizees with arsenic, the two can also be reacted in volatilization process, and arsenic is oxidized to 5 valency arsenic, react raw rapidly with NaOH
Produce natrium arsenicum, belong to material soluble easily in water, and effectively prevent arsenic volatilize in roasting process and caused by arsenic pollution；Rhenium is same
Sample is aoxidized, and becomes rhenate；Copper is also aoxidized, and produces Kocide SD precipitation not soluble in water.So enter next step water logging
During process, it is possible to achieve the separation of arsenic, rhenium and copper.Above-mentioned reaction process is specially：
As2S+OH-+O2=(As2O4)3-+SO4 2-+H2O；
Re2S7+OH-+O2=(ReO4)4-+SO4 2-+H2O；
Cu2S+OH-+O2=Cu (OH)2+SO4 2-。
During above-mentioned roasting, the temperature of the roasting is 450~750 DEG C, and the time of the roasting is 3~5h；
In specific embodiment, the temperature of the roasting is 500~700 DEG C, and the time of the roasting is 4~5h.
According to the present invention, fired slags are then subjected to water logging, obtain leachate and leached mud；After water logging, the leaching
Go out liquid for rhenium-containing acid group and the solution of arsenate, since leachate is strong alkali solution, then copper entered in filter residue, effectively
The copper that realizes separated with arsenic, reduce the content of arsenic in leached mud, avoid filter residue and made when returning to copper metallurgy industry
Into arsenic closed cycle and secondary pollution.The liquid-solid ratio of the water logging is (2~5)：1, the time of the water logging is 1.5~3h,
The temperature of the water logging is 120~150 DEG C.
Then the application by the leachate and the substance reaction containing calcium ion, obtains filter residue A and filtrate A after filtering；
In the process, the material containing calcium ion is preferably calcium hydroxide, and above-mentioned reaction makes arsenate and calcium in leachate
Ionic reaction generates arsenic acid calcium precipitate not soluble in water, and the main component of filter residue A is calcium arsenate, and the material is more stable, can be with
As a kind of mode of arsenic fixing process, placed for storing up, avoid the pollution of secondary arsenic；The filtrate A is rhenium-containing acid group
Solution, can as generation rehenic acid ammonium raw material.The addition of the material containing calcium ion is according in the leachate
The ratio of the quality of arsenic and the quality of calcium ion in the material containing calcium ion is 1：(1~1.2) add.
In order to make rehenic acid root in above-mentioned leachate and arsenate and calcium ion reaction abundant, the above-mentioned thing containing calcium ion
The addition of matter is excessive, causes calcium ion in filtrate A excessive, in order to put forward the quality of ammonium perrhenate, therefore the application needs
The filtrate A is subjected to removing calcium ion, i.e. the application adds calcium remover in the filtrate A, filters, that is, is filtered after reaction
Slag B and liquor B.The calcium remover is ammonium carbonate or ammonium hydrogen carbonate；The addition of the calcium remover presses calcium ion quality in filtrate A
It is 1 with carbonic acid root mass ratio in the calcium remover：(2~3) add.Above-mentioned filter residue B is calcium carbonate slag, and liquor B is molten for rehenic acid ammonium
Liquid.
The application is finally concentrated Ammonium rhenate solution, then crystallization is placed at -5 DEG C, and filtering obtains rehenic acid crystalline ammonium
Body, extraction raffinate return to condensing crystallizing.
This application provides a kind of method that rhenium is extracted in concentrate from rhenium, this method is due to anti-using sodium hydrate aqueous solution
Should, arsenic is entered solution, realize arsenic and separated with the copper in leached mud, be mainly copper in leached mud, arsenic content is extremely low, is leaching
Calcium ion is added in liquid, forms arsenic acid calcium precipitate, it is a kind of material of stabilization, and copper returns to copper metallurgy industry, avoids arsenic
The vicious circle of copper metallurgy industry is again introduced into, calcium arsenate can open a way as the material of arsenic, reduce the amount of arsenic in system, and
Do not cause secondary pollution.
For a further understanding of the present invention, with reference to embodiment to the side provided by the invention that rhenium is extracted from rich rhenium slag
Method is described in detail, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
A) material mixes
1kg richness rhenium slags are taken to be washed, pH≤6 of rich rhenium slag after washing, take 0.6kgNaOH to add in 1L water and dissolve, obtain
To NaOH solution, then NaOH solution is uniformly mixed with rich rhenium slag；Rich rhenium slag ingredient is (dry) Re：3.8%, As：8.6%,
Cu：12.9%, S：68%；
B) roast
Mixed material is added in Muffle furnace, temperature control when heating 5 is small, obtains fired slags at 500 DEG C；Roasting
Slag ingredient：Re:2.7%, As:5.2%, Cu:8%, S:45%；
C) water logging
Fired slags are added in 3L water and are leached, when the water logging time is 2 small, water soaking temperature is 150 DEG C, is obtained by filtration
Filtrate A and excessively filter residue B；Filtered fluid A components are：Re:9.5g/L, As:19.65g/L；
D) infusion dearsenification
Take added in 1L filtered fluids A 20g calcium hydroxide reactions 1 it is small when, after completion of the reaction, filtered fluid B and mistake is obtained by filtration
Filter residue B；The component of filtered fluid B is：Re:9.3g/L, As:0.013g/L, Ca:0.12g/L；
E) infusion decalcification
Take step D) obtained filtered fluid B1L, add 0.3g ammonium carbonates reaction 30min, filtering, obtain Ammonium rhenate solution and
Cross filter residue；
F) condensing crystallizing
By Ammonium rhenate solution heating evaporation, 5h at a temperature of being then placed in -5 DEG C, it is 99.5%, yield to filter up to purity
For 92% rehenic acid ammonium crystal.
Embodiment 2
A) material mixes
1kg richness rhenium slags are taken to be washed, pH >=6 of rich rhenium slag after washing, take 0.9kgNaOH to add in 1L water and dissolve, obtain
To NaOH solution, then NaOH solution is uniformly mixed with rich rhenium slag；Rich rhenium slag ingredient is (dry) Re:1.2%, As:10.5%,
Cu:19.8%, S:68%；
B) roast
Mixed material is added into Muffle kiln roasting, temperature control when heating 4 is small, obtains fired slags at 600 DEG C；
Roast slag ingredient：Re:0.8%, As:7.3%, Cu:13.2%, S:47%；
C) water logging
Fired slags are added in 3L water and are leached, when the water logging time is 3 small, water soaking temperature is 120 DEG C, is obtained by filtration
Filtrate A and excessively filter residue B；Filtered fluid A components are：Re:4.2g/L, As:36.2g/L；
D) infusion dearsenification
Take added in 1L filtered fluids A 80g calcium hydroxide reactions 1 it is small when, after completion of the reaction, filtered fluid B and mistake is obtained by filtration
Filter residue B；The component of filtered fluid B is：Re:4g/L, As:0.012g/L, Ca:0.14g/L；
E) infusion decalcification
Take step D) obtained filtered fluid B1L, 0.35g ammonium carbonates reaction 30min is added, filtering, obtains Ammonium rhenate solution
With filter residue excessively；
F) condensing crystallizing
By Ammonium rhenate solution heating evaporation, 5h at a temperature of being then placed in -5 DEG C, it is 99.2%, yield to filter up to purity
For 90% rehenic acid ammonium crystal.
Embodiment 3
A) material mixes
1kg richness rhenium slags are taken to be washed, pH >=6 of rich rhenium slag after washing, take 0.8kgNaOH to add in 1L water and dissolve, obtain
To NaOH solution, then NaOH solution is uniformly mixed with rich rhenium slag；Rich rhenium slag ingredient is (dry) Re:6.0%, As:5.8%,
Cu:11.8%, S:65%；
B) roast
Mixed material is added in Muffle furnace, temperature control when heating 5 is small, obtains fired slags at 500 DEG C；Roasting
Slag ingredient：Re:3.75%, As:3.6%, Cu:7.38%, S:43%；
C) water logging
Fired slags are added in 3L water and are leached, when the water logging time is 3 small, water soaking temperature is 150 DEG C, and filtered fluid is obtained by filtration
A and excessively filter residue B；Filtered fluid A components are：Re:12.4g/L As:12g/L；
D) infusion dearsenification
Take added in 1L filtered fluids A 24g calcium hydroxide reactions 1 it is small when, after completion of the reaction, filtered fluid B and mistake is obtained by filtration
Filter residue B；The component of filtered fluid B is：Re:12g/L, As:0.011g/L, Ca:0.15g/L；
E) infusion decalcification
Take step D) obtained filtered fluid B1L, add 0.4g ammonium carbonates reaction 30min, filtering, obtain Ammonium rhenate solution and
Cross filter residue；
F, condensing crystallizing
By Ammonium rhenate solution heating evaporation, 5h at a temperature of being then placed in -5 DEG C, it is 99.6%, yield to filter up to purity
For 94% rehenic acid ammonium crystal.
The explanation of above example is only intended to help to understand method and its core concept of the invention.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvement and modification, these are improved and modification is also fallen into the protection domain of the claims in the present invention.
The foregoing description of the disclosed embodiments, enables professional and technical personnel in the field to realize or use the present invention.
A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and the principles and novel features disclosed herein phase one
The most wide scope caused.
Claims (10)
1. a kind of method that rhenium is extracted from rich rhenium slag, comprises the following steps：
A), rich rhenium slag is mixed with sodium hydrate aqueous solution, obtains mixed material, the mixed material is roasted, is roasted
Slag；
B), the fired slags are subjected to water logging, obtain leachate and leached mud；By the leachate and the material containing calcium ion
Reaction, obtains filter residue A and filtrate A after filtering；
C), calcium remover is added in the filtrate A, filter residue B and liquor B are obtained after filtering；
D), the liquor B concentrated, crystallized, obtain rehenic acid ammonium.
2. according to the method described in claim 1, it is characterized in that, step A) in, further included before the mixing：
The rich rhenium slag is washed, makes pH >=6 of the rich rhenium slag after washing.
3. method according to claim 1 or 2, it is characterised in that in the richness rhenium slag and the sodium hydrate aqueous solution
Sodium hydroxide mass ratio be 1：(0.6~0.8).
4. method according to claim 1 or 2, it is characterised in that the temperature of the roasting is 450~750 DEG C, and the time is
3~5h.
5. method according to claim 1 or 2, it is characterised in that the liquid-solid ratio of the water logging is (2~5)：1, the water
The time of leaching is 1.5~3h, and the temperature of the water logging is 120~150 DEG C.
6. method according to claim 1 or 2, it is characterised in that step B) in, the quality of arsenic and institute in the leachate
The mass ratio for stating calcium ion in the material containing calcium ion is 1：(1~1.2).
7. method according to claim 1 or 2, it is characterised in that the material containing calcium ion is calcium hydroxide.
8. method according to claim 1 or 2, it is characterised in that the calcium remover is ammonium carbonate or ammonium hydrogen carbonate.
9. according to the method described in claim 8, it is characterized in that, the addition of the calcium remover is according to calcium in the filtrate A
Ion is 1 with carbonic acid root mass ratio in the calcium remover：(2~3) add.
10. according to claim 1~9 any one of them method, it is characterised in that the richness rhenium slag includes 0.8~
The Re of 10wt%, the As of 0.5~20wt%, the S of the Cu of 8~30wt% and 20~70wt%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110715903A (en) * | 2019-10-25 | 2020-01-21 | 铜陵有色金属集团股份有限公司 | Method for determining rhenium in molybdenum ore |
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