CN107354300A - A kind of method of enriching rhenium in spent acid from Copper making - Google Patents
A kind of method of enriching rhenium in spent acid from Copper making Download PDFInfo
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- CN107354300A CN107354300A CN201710588106.1A CN201710588106A CN107354300A CN 107354300 A CN107354300 A CN 107354300A CN 201710588106 A CN201710588106 A CN 201710588106A CN 107354300 A CN107354300 A CN 107354300A
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- rhenium
- spent acid
- copper
- copper making
- solution
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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
- C22B61/00—Obtaining metals not elsewhere provided for in this subclass
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
Abstract
The invention discloses a kind of method of enriching rhenium in spent acid from Copper making.The technical scheme of use is：Into the Copper making spent acid containing low concentration rhenium, it is 8 ~ 12 to add precipitating reagent to pH value of solution, press filtration separation, collect filtrate, pH to 1 ~ 8 is adjusted, filtrate is pre-processed by charcoal adsorption tower, further removes interfering ion, then solution is passed through into copper-loaded charcoal adsorption tower Adsorption of Rhenium, after absorption reaches saturation, stop absorption, eluted with alkali lye, concentration, obtains rhenium-containing pregnant solution.Present invention process is reasonable, pollution-free, and operating condition is gentle, and the rate of recovery is up to more than 99%, and maximal absorptive capacity is 100 mg rheniums/g adsorbents, and rhenium enrichment is improved up to more than 100 times, it is possible to achieve the rapidly and efficiently recovery of low concentration rhenium in Copper making spent acid.
Description
Technical field
The invention belongs to chemical separating field, and in particular to a kind of method of enriching rhenium in spent acid from Copper making.
Background technology
The independent deposit of dissipated metal rhenium is very rare, and it is mainly with ReS2Form association in molybdenite, copper-sulphide ores
In porphyry copper.In copper concentrate, rhenium is mainly with copper rhenium ore deposit (CuReS4) and brightness rhenium ore deposit (ReS2) form exist, copper mine exists
During pyrometallurgical smelting, most rheniums are with Re2O7Form is volatized into flue gas, rhenium-containing flue gas after eluting column pickling, rhenium with
HReO4Form is present in Copper making spent acid.The mg/L of rhenium-containing 3 ~ 30 in spent acid, by removing in arsenic, heavy metal and alkaline matter
And processing, most rheniums enter arsenic filter cake or neutralized in slag, small part (0.5 ~ 10 mg/L) is damaged with discharge of wastewater up to standard
Lose.
Mainly there are precipitation-oxidizing roasting method, neutralization precipitation-ion-exchange and molten from method that rhenium is extracted in spent acid is smelted
Agent extraction.
Precipitation-oxidizing roasting method reclaims rhenium from Copper making spent acid, take into leacheate add ammonium thiocyanate solution and
Poly- propionyl amine aqueous solution, precipitate rhenium and arsenic, sediment in 200,430 DEG C of 1 h of each calcining and 5 h desulfurization, is calcined at 500 DEG C respectively
5 h dearsenifications, finally 850 DEG C of oxidizing roastings volatilize Re in rotary furnace2O7, with ammonia absorption, obtain ammonium perrhenate.The technique
Rhenium recovery rate is up to 65%, but precipitating reagent dosage is big, and rhenium, arsenic, the separation of sulphur are difficult, and the rhenium purity and yield of acquisition are relatively low.
Domestic patent of invention CN102173457B discloses a kind of side that ammonium perrhenate is prepared from the waste liquid containing molybdenum-rhenium
Method, first into the waste liquid containing molybdenum-rhenium, it is in yellow to add hydrogen peroxide to solution, and it is 6 ~ 7 to add mixed agent to pH value of solution, pressure
Filter separation, collects filtrate, and filtrate Adsorption of Rhenium, is finally eluted with ammoniacal liquor by ion exchange resin column, prepares ammonium perrhenate.Should
Neutralization precipitation-ion-exchange, rhenium enrichment improve nearly 20 times, and the rate of recovery is more than 93%, and ammonium perrhenate purity is made up to 99.5%
More than, but used resin price is expensive and spent resin processing is difficult.
Solvent extraction is the main method of enrichment extraction rhenium in industrial production, and this method is widely used, process conditions phase
To maturation.Rhenium-containing spent acid absorbing liquid amine, ketone, phosphine or quaternary ammonium salt extractant extraction extraction rhenium.Then using 10%
Ammoniacal liquor is stripped, and obtains ammonium perrhenate strip liquor.By repeatedly extraction, purity can be obtained up to 99.6% ammonium perrhenate.The technique is returned
The speed of receiving rhenium is fast, purity is high, mild condition, but extraction process is mostly amine extractant using extractant so that extraction is selected
Selecting property is poor, salt-forming reaction easily occurs, and has that loading capacity is big, extractant is volatile, reagent consumption is big, processing cost is high, easy
The problems such as causing secondary environmental pollution.
In summary, extraction low concentration rhenium difficulty, processing cost be present in the prior art that rhenium is reclaimed from Copper making spent acid
The shortcomings of high, easy pollution environment.Therefore, the process route of science, efficient precipitating reagent, the strippant of high-efficiency low-toxicity, place are developed
Reason cost is low, environmental pollution is small, is whether extraction low concentration rhenium technology is successfully crucial.
The content of the invention
It is an object of the invention to for above-mentioned technical deficiency, there is provided a kind of rational technology, pollution-free, mild condition, effect
The method of enriching rhenium in the high spent acid from Copper making of rate.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of method of enriching rhenium in spent acid from Copper making：Into the Copper making spent acid containing low concentration rhenium, precipitating reagent is added extremely
PH value of solution is 8 ~ 12, press filtration separation, collects filtrate, adds sulphur acid for adjusting pH to 1 ~ 8, filtrate is located in advance by charcoal adsorption tower
Reason, further removes interfering ion, when each interfering ion concentration is less than 5 mg/L, solution is passed through into copper-loaded charcoal adsorption tower
Adsorption of Rhenium, after absorption reaches saturation, eluted with alkali lye, ammoniacal liquor is added in most backward eluent, concentrated, obtain rhenium-containing pregnant solution.
The mg/L of rhenium-containing 4.0 ~ 100 in described Copper making spent acid.
Described precipitating reagent is by weight 4 ~ 6 by calcium hydroxide and calcium oxide:1 mixing.
Described biological carbon feedstock is large agriculture and forestry organic waste materials such as stalk, rice husk, peanut shell, bamboo shoot shell, bagasse, coffee bean
In one or more.
Described interfering ion is mainly copper, iron and arsenic, is less than by precipitation and preprocessing process, each interfering ion concentration
5 mg/L。
Described alkali lye is KOH solution, and its concentration is 0.1 ~ 1.0 mol/L, and dosage is that 2 ~ 10 g adsorbents coordinate 1L to wash
De- liquid.
Described precipitation, pretreatment, Adsorption of Rhenium and alkali lye elution process is all carried out at normal temperatures.
The present invention principle be：A kind of method of enriching rhenium in spent acid from Copper making：To the Copper making containing low concentration rhenium
In spent acid, calcium hydroxide and calcium oxide are added by weight mixing, as interfering ion and the precipitating reagent of rhenium initial gross separation, is added
Precipitating reagent to pH value of solution is 8 ~ 12, precipitates interfering ion, press filtration separation, collects filtrate, and filtrate pH to 5 ~ 7 is adjusted with hydrochloric acid,
And pre-process filtrate by charcoal adsorption tower, with further adsorbing and removing interfering ion, when interfering ion concentration is less than 5
During mg/L, by solution by copper-loaded charcoal adsorption tower, adsorption and enrichment rhenium, after absorption reaches saturation, stop absorption.Will absorption
The copper-loaded charcoal of saturation, is eluted with alkali lye, concentration, obtains rhenium-containing pregnant solution.
Beneficial effects of the present invention and outstanding advantage are：
1. achievement of the present invention, which is the recovery utilization of rhenium in China's Copper making roasting industry, has founded a new clean manufacturing
Technology；
2. the biological carbon feedstock that the present invention uses is large agriculture and forestry organic waste material, its wide material sources, cost is cheap, for from copper smelting
Refine enriching rhenium in spent acid, the purpose for reach the treatment of wastes with processes of wastes against one another, turning waste into wealth；
3. the present invention is using KOH solution desorption rhenium, by 4 ~ 8 adsorption-desorption cycles, desorption efficiency desorbs bar still greater than 92%
Part is gentle, at normal temperatures；
4. the present invention is using the low concentration rhenium in neutralization precipitation-biomass absorbent method enrichment Copper making spent acid, the rate of recovery is up to 99%
More than, maximal absorptive capacity is 100 mg rheniums/g adsorbents, and enriching rhenium is up to more than 100 times, can realize rhenium in Copper making spent acid
Efficiently separate and high efficiente callback.
Brief description of the drawings
Fig. 1 is the process flow diagram of the present invention；
Fig. 2 is present invention process flow and equipment drawing, wherein：1. sedimentation basin；2. pressure filter；3. pH regulating tanks；4. charcoal
Adsorption tower；5. copper-loaded charcoal adsorption tower；6. liquid waste tank；7. switching valve；8. copper-loaded charcoal desorber；9. liquid waste tank；
10. concentrator；Rhenium-containing is enriched with liquid storage tank.
Embodiment
With reference to case study on implementation, the present invention will be further described, and case study on implementation will facilitate a better understanding of the present invention,
But the present invention is not limited only to following embodiments.
Embodiment 1
The Copper making spent acid provided using certain company A is detected, in copper smelting as raw material using inductive coupling plasma emission spectrograph
The mg/L of cupric 1260 in spent acid is refined, containing the mg/L of arsenic 394, the mg/L of iron content 604, the mg/L of rhenium-containing 65, the mg/L of sulfur acid 79440.
Into the sedimentation basin equipped with Copper making spent acid, calcium hydroxide is added with calcium oxide by weight 4 ~ 6:1 mixing is sunk
Shallow lake agent to pH value of solution is 8, press filtration separation, collects filtrate in reservoir（PH regulating tanks）, sulfuric acid regulation filter is passed through into reservoir
Liquid pH is pre-processed to 5, and by rhenium-containing filtrate by charcoal adsorption tower, when each interfering ion concentration is less than 5 mg/L, will be contained
Rhenium solution adsorption and enrichment rhenium, after absorption reaches saturation, stops absorption by copper-loaded charcoal adsorption tower.After adsorption saturation
Copper-loaded charcoal, eluted with 0.1 mol/L KOH solutions, the eluting rate of rhenium is 96.34%, the rate of recovery 99.12%, enriching Cu smelting
Low concentration rhenium in refining spent acid is up to 105 times.
Embodiment 2
The Copper making spent acid provided using certain company B is detected, in copper smelting as raw material using inductive coupling plasma emission spectrograph
The mg/L of cupric 952 in spent acid is refined, containing the mg/L of arsenic 586, the mg/L of iron content 814, the mg/L of rhenium-containing 76, the mg/L of sulfur acid 56870.
Into the sedimentation basin equipped with Copper making spent acid, calcium hydroxide is added with calcium oxide by weight 4 ~ 6:1 mixing is sunk
Shallow lake agent to pH value of solution is 12, press filtration separation, collects filtrate in reservoir（PH regulating tanks）, sulfuric acid regulation filter is passed through into reservoir
Liquid pH is pre-processed to 6, and by rhenium-containing filtrate by charcoal adsorption tower, when each interfering ion concentration is less than 5 mg/L, by rhenium-containing
Solution adsorption and enrichment rhenium, after absorption reaches saturation, stops absorption by copper-loaded charcoal adsorption tower.Load after adsorption saturation
Copper charcoal, eluted with 0.5 mol/L KOH solutions, the eluting rate of rhenium is 94.69%, the rate of recovery 99.35%, is enriched with Copper making
Low concentration rhenium in spent acid is up to 50 times.
Embodiment 3
The Copper making spent acid provided using certain company C is detected, in copper smelting as raw material using inductive coupling plasma emission spectrograph
The mg/L of cupric 1380 in spent acid is refined, containing the mg/L of arsenic 471, the mg/L of iron content 985, the mg/L of rhenium-containing 49, the mg/L of sulfur acid 58640.
Into the sedimentation basin equipped with Copper making spent acid, calcium hydroxide is added with calcium oxide by weight 4 ~ 6:1 mixing is sunk
Shallow lake agent to pH value of solution is 10, press filtration separation, collects filtrate in reservoir（PH regulating tanks）, sulfuric acid regulation filter is passed through into reservoir
Liquid pH is pre-processed to 7, and by rhenium-containing filtrate by charcoal adsorption tower, when each interfering ion concentration is less than 5 mg/L, by rhenium-containing
Solution adsorption and enrichment rhenium, after absorption reaches saturation, stops absorption by copper-loaded charcoal adsorption tower.Load after adsorption saturation
Copper charcoal, eluted with 1.0 mol/L KOH solutions, the eluting rate of rhenium is 93.85%, the rate of recovery 99.55%, is enriched with Copper making
Low concentration rhenium in spent acid is up to 80 times.
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, it should all belong to the covering scope of the present invention.
Claims (6)
1. a kind of method of enriching rhenium in spent acid from Copper making, it is characterised in that：Into the Copper making spent acid containing low concentration rhenium,
It is 8 ~ 12 to add precipitating reagent to pH value of solution, press filtration separation, collects filtrate, adds sulphur acid for adjusting pH to 1 ~ 8, filtrate is passed through into biology
Charcoal adsorption tower pre-processes, and further removes interfering ion, when each interfering ion concentration is less than 5 mg/L, solution is passed through copper-loaded
Charcoal adsorption tower Adsorption of Rhenium, after absorption reaches saturation, stop absorption, eluted with alkali lye, concentrate, obtain rhenium-containing pregnant solution.
2. the method for enriching rhenium in a kind of spent acid from Copper making according to claim 1, it is characterised in that：Described copper
Smelt the mg/L of rhenium-containing 4.0 ~ 100 in spent acid.
3. the method for enriching rhenium in a kind of spent acid from Copper making according to claim 1, it is characterised in that：Described precipitation
Agent is by weight 4 ~ 6 by calcium hydroxide and calcium oxide:1 mixing.
4. the method for enriching rhenium in a kind of spent acid from Copper making according to claim 1, it is characterised in that：Described biology
The raw material of charcoal is large agriculture and forestry organic waste material.
5. the method for enriching rhenium in a kind of spent acid from Copper making according to claim 4, it is characterised in that：Described biology
The raw material of charcoal is the one or more in stalk, rice husk, peanut shell, bamboo shoot shell, bagasse, coffee bean.
6. the method for enriching rhenium in a kind of spent acid from Copper making according to claim 1, it is characterised in that：Described alkali
Liquid is KOH solution, and concentration is 0.1 ~ 1.0 mol/L, and dosage is：2 ~ 10 g adsorbents coordinate 1L eluents.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109518014A (en) * | 2018-10-30 | 2019-03-26 | 金川集团股份有限公司 | The enrichment method of rhenium in a kind of copper blast furnace off-gas purification system acid waste water |
| CN110501327A (en) * | 2019-05-29 | 2019-11-26 | 金川集团股份有限公司 | The method for separating and detecting of rhenium in a kind of high Copper substrate solid material and liquid material |
| CN111413288A (en) * | 2020-03-31 | 2020-07-14 | 安徽工业大学 | Accurate detection method for rhenium in copper smelting multi-element mixed waste acid |
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| CN106011487A (en) * | 2016-06-28 | 2016-10-12 | 阳谷祥光铜业有限公司 | Method for recycling rhenium from copper smelting smoke washing waste acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109518014A (en) * | 2018-10-30 | 2019-03-26 | 金川集团股份有限公司 | The enrichment method of rhenium in a kind of copper blast furnace off-gas purification system acid waste water |
| CN110501327A (en) * | 2019-05-29 | 2019-11-26 | 金川集团股份有限公司 | The method for separating and detecting of rhenium in a kind of high Copper substrate solid material and liquid material |
| CN110501327B (en) * | 2019-05-29 | 2022-11-11 | 金川集团股份有限公司 | Separation detection method for rhenium in high-copper matrix solid material and liquid material |
| CN111413288A (en) * | 2020-03-31 | 2020-07-14 | 安徽工业大学 | Accurate detection method for rhenium in copper smelting multi-element mixed waste acid |
| CN111413288B (en) * | 2020-03-31 | 2023-06-30 | 安徽工业大学 | Accurate detection method for rhenium in copper smelting multielement mixed waste acid |
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