CN105671324A - Method for preparing ammonium rhenate from rhenium-enriched slags - Google Patents
Method for preparing ammonium rhenate from rhenium-enriched slags Download PDFInfo
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- CN105671324A CN105671324A CN201610126621.3A CN201610126621A CN105671324A CN 105671324 A CN105671324 A CN 105671324A CN 201610126621 A CN201610126621 A CN 201610126621A CN 105671324 A CN105671324 A CN 105671324A
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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
- C22B7/04—Working-up slag
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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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- 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
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Abstract
The invention discloses a method for preparing ammonium rhenate from rhenium-enriched slags. The method comprises the following operation steps that pure water is added to the rhenium-enriched slags for slurry mixing according to a liquid-solid ratio of (4-8):1; a hot-pressure leaching method is utilized at the leaching temperature of 100-200 DEG C and the oxygen partial pressure of 0.3-1.5 MPa, so that a rhenium-enriched liquid with the rhenium concentration of 3-10g/L is obtained after 1-5 hours of leaching; after filtering and washing treatment, 98% concentrated sulfuric acid is added to a filtrate till the acidity reaches 130-160 g/L; then the mixture obtained in the previous step is mixed with a no-load organic phase which comprises 20%-50% N235, 25%-40% octanol and 25%-40% kerosene, wherein the phase ratio O/A is (7-10):1; the mixture obtained in the previous step is fiercely vibrated and mixed uniformly for 5-10 minutes, and then is clarified for 10-20 minutes to obtain a loaded organic phase; finally, after the loaded organic phase is washed with pure water, reverse extraction is performed with 1-5 mol/L ammonium hydroxide, and the reverse extraction phase ratio is 5:1; and the reverse extraction liquid is subjected to evaporation and concentration at 70-90 DEG C, and then is subjected to freezing crystallization to obtain an ammonium rhenate product. According to the method for leaching rhenium for the rhenium-enriched slags and preparing the ammonium rhenate, the method has the characteristics of being clean and pollution-free, and being simple and high-efficient for operation, high in yield and purity and low in manufacture cost.
Description
Technical field
The invention belongs to dissipated metal field of metallurgy, be specifically related to leach rhenium the method preparing rehenic acid ammonium product from rich rhenium slag.
Background technology
Rhenium is a kind of valuable rare metal, does not have independent mineral deposit in nature, can only association in other metalliferous minerals such as copper-sulphide ores. In Copper making process, rhenium oxidation forms Re2O7Enter flue gas, exist in waste acid with the form of perrhenic acid after dynamic wave system is washed. Thus, solid slag and arsenic filter cake that waste acid and waste acid subsequent treatment produce are all the important source material extracting rhenium metal.
At present, adopt arsenic filter cake to extract rhenium metal as raw material to have been reported that repeatly, main technique is to pass into oxygen pressing under sulfuric acid system to leach, leachate utilizes extraction to extract rhenium metal, just belongs to this type of method as the bibliographical information such as Sun Wenda Jiangxi Copper group Guixi Smelter adopts " acid system high pressure leaching arsenic filter cake-extracting and enriching rhenium-prepare rehenic acid ammonium " technique to reclaim rhenium. The method can the multiple valuable metal of synthetical recovery, but due in technological process length and arsenic filter cake rhenium accumulation rate low, cause production process material quantity big, whole process Rhenium recovery rate is on the low side, separately owing to arsenic filter cake pressure leaching is acid medium, requiring height to equipment is corrosion-resistant, production cost is high.
For the problem that rhenium grade in arsenic filter cake is low, utilize targeting precipitant that waste acid is processed, make rhenium in waste acid enter rich rhenium slag and have been reported. Rhenium-containing 0.5% ~ 3.5% in rich rhenium slag, the method of existing " rich rhenium slag and logical oxygen heating oxidizing roasting-pressurized, heated alkali leaching in a certain amount of sulphur-fixing agent profit mill-tube furnace " prepares the expensive liquid of rhenium-containing, this method rhenium leaching rate is high, but relating to roasting and leach multistage technology, oxidizing roasting energy consumption is high, big for environment pollution; High pressure base caustic dip consumption is big, and the response time is long, and disposal ability is little. Therefore, the method has yet to be improved and developed.
CN102433439A " a kind of method reclaiming rhenium from arsenic filter cake " proposes to adopt " one section of alkali leaching-two-stage nitration Oxidation Leaching-sulfur dioxide method or the lime method arsenic removal-extract and separate rhenium-potassium chloride sedimentation method-recrystallization method " to prepare high-purity potassium perrhenate technique.This method relates to two sections of leachings, and flow process is complicated, and after leaching, in liquid, rhenium-containing is low, cannot directly sink rhenium containing arsenic height, the shortcomings such as Rhenium recovery rate is low.
CN104404277A discloses " in a kind of Strengthen education richness rhenium slag the method for rhenium and rhenium leachate ", it is primarily related to the technique of one " rich rhenium slag and sulphur-fixing agent profit mill-dioxygen oxidation roasting-pressurized, heated alkali leaching ", is not directed to how further rhenium in your liquid to be prepared into rhenium product.
Summary of the invention
It is an object of the invention to provide a kind of cleanliness without any pollution when leaching rhenium from rich rhenium slag and prepare rehenic acid ammonium, simple to operate efficiently, product yield and purity is high, cost of manufacture is low method.
For realizing object above, the present invention prepares the method for rehenic acid ammonium from rich rhenium slag and includes following operating procedure:
A. being added water by liquid-solid ratio 4 ~ 8:1 by richness rhenium slag and size mixing, utilize hot-pressure leaching method to process, control extraction temperature 100 ~ 200 DEG C, partial pressure of oxygen is 0.3 ~ 1.5MPa, and extraction time is 1 ~ 5h, and through filtering, to obtain rich rhenium liquid rhenium content be 3 ~ 10g/L in washing;
B. with addition of sulphuric acid, Controlled acidity 130 ~ 160g/L in rich rhenium liquid, it being mixed with unloaded organic facies, comparing O/A is 7 ~ 10:1, and vibrate mixing 5 ~ 10min, clarifies 10 ~ 20min, obtains load organic phases; Wherein, unloaded organic facies consists of 20% ~ 50%N235+ 25% ~ 40% sec-octyl alcohol+25% ~ 40% kerosene;
C. load organic phases is after water washing, carries out back extraction with 1 ~ 5mol/L ammonia, and 5:1 is compared in back extraction, and strip liquor is evaporation and concentration freezing and crystallizing at 70 ~ 90 DEG C, obtains rehenic acid ammonium product.
The present invention prepares the method for rehenic acid ammonium from rich rhenium slag and has techniques below feature:
(1) adopting hot-pressure oxidation extract technology to process rich rhenium slag, with aqueous solution for medium, oxygen is oxidant, still belongs to the first time in rich rhenium Slag treatment field;
(2) adopt extraction means to reach remove impurity purpose for high pressure richness rhenium leachate, still belong to the first time in field;
(3) adopt extraction means, extractant proportioning is improved with comparing, under short extraction progression (1 ~ 2 grade), realizes the purpose of remove impurity Sync enrichment rhenium, alleviate subsequent evaporation concentration amount, reduce production cost, reduce labor intensity.
The present invention prepares the method for rehenic acid ammonium from rich rhenium slag and has the advantages that
(1) adopting the rhenium in hot-pressure oxidation method Strengthen education richness rhenium slag, process is not introduced into any impurity, and rhenium leaching rate is more than 99%;
(2) after improving extraction conditions, under short extraction progression (1 ~ 2 grade), impurity-eliminating effect is notable, and copper, separating by extraction are more than 98%, and process energy consumption is low, and operational approach is simple;
(3) extraction process makes rhenium be enriched with further, and the concentration of strip liquor rhenium is greatly improved, and reduces evaporation and concentration treating capacity, reduces production cost.
The present invention proposes a kind of from rich rhenium slag hot-pressure oxidation--the process of solvent extraction remove impurity-prepare rehenic acid ammonium, forms one leaching rhenium prepare the complete technique with industrial application value of rehenic acid ammonium from rich rhenium slag. This technique adopts hot-pressure oxidation technology, proposes first to adopt High Temperature High Pressure to leach rich rhenium copper ashes with water for medium, and rhenium copper leaching rate is more than 98%, and leaching rhenium is effective, and energy consumption is low; Solvent extraction means remove impurity is adopted first for high pressure richness rhenium leachate, the elimination impurity such as arsenic, copper, process object, extraction conditions and operation and be all different from conventional extraction processes, impurity removal percentage is more than 98%, gained potassium perrhenate purity is more than 99.5%, there is good impurity removing effect, rhenium product yield and purity height, cleanliness without any pollution, simple to operate efficiently, feature that cost of manufacture is low, rhenium recycling and rhenium industry chain are improved and are significant.
Accompanying drawing explanation
Fig. 1 is the method process flow diagram that the present invention prepares rehenic acid ammonium from rich rhenium slag.
Accompanying drawing labelling: rich rhenium slag 1, pure water 2, filtering residue 3, unloaded organic facies 4, rhenium-containing filtrate 5, concentrated sulphuric acid 6, ammonia 7, strip liquor 8, rehenic acid ammonium product 9.
Detailed description of the invention
The method present invention being prepared rehenic acid ammonium from rich rhenium slag below in conjunction with the drawings and specific embodiments is described in further detail.
The process conditions that the present invention need to control include:
In the operation of A pressure leaching, need to controlling liquid-solid ratio 4 ~ 8:1, extraction temperature 130 ~ 170 DEG C, partial pressure of oxygen is 0.3 ~ 1.5MPa, and extraction time is 1 ~ 5h, to obtain good leaching rate;
In B extracting operation, needing Controlled acidity is 130 ~ 160g/L, by its with consist of 40%N235The unloaded organic facies mixing of+30% sec-octyl alcohol+30% kerosene, comparing O/A is 7 ~ 10:1, biphase mixing 5 ~ 10min, static clarification 10 ~ 20min so that in rich rhenium solution, rhenium can enter in organic facies as far as possible;
In C back extraction operation, control ammonia concn is 1 ~ 5mol/L, and is evaporated condensing crystallizing at 70 ~ 90 DEG C, obtains rehenic acid ammonium product.
It is exemplified below five embodiments:
Embodiment 1:In this instance processes richness rhenium slag, rhenium-containing 2.5%, containing arsenic 28.9%, process technique, effect are as follows:
Weigh rich rhenium slag 100g, add 800mL pure water, stirring and evenly mixing; Being positioned in autoclave and carry out hot-pressure oxidation leaching by raw material after mixing, partial pressure of oxygen is 1.5MPa, response time 3h, reaction temperature 130 DEG C, after reaction terminates, is filtered by rhenium-containing leachate, washs, and now, the leaching rate of rhenium is 99.3%; The concentrated sulphuric acid 44mL of also middle addition 98% after filtration, acidity is adjusted 160g/L, rhenium-containing leachate after acidity being adjusted mixes with unloaded organic facies, being in a ratio of 10:1, concussion mixing 5min, clarifies 10min on the oscillator, release load organic phases, with pure water, then carrying out back extraction with 5mol/L ammonia, back extraction is in a ratio of 5:1; After back extraction, organic facies returns and uses, and strip liquor is evaporated condensing crystallizing at 70 DEG C, obtains rehenic acid ammonium product. Rehenic acid ammonium product purity is 99.6%, and the response rate of rhenium is 99.1%.
Embodiment 2:In this instance processes richness rhenium slag, rhenium-containing 2.5%, containing arsenic 28.9%, process technique, effect are as follows:
Weigh rich rhenium slag 120g, add 480mL pure water, stirring and evenly mixing; Being positioned in autoclave and carry out hot-pressure oxidation leaching by raw material after mixing, partial pressure of oxygen is 0.8MPa, response time 5h, reaction temperature 150 DEG C, after reaction terminates, is filtered by rhenium-containing leachate, washs, and now, the leaching rate of rhenium is 99.6%; The concentrated sulphuric acid 35mL of also middle addition 98% after filtration, acidity is adjusted 130g/L, rhenium-containing leachate after acidity being adjusted mixes with unloaded organic facies, being in a ratio of 8:1, concussion mixing 10min, clarifies 20min on the oscillator, release load organic phases, with pure water, then carrying out back extraction with 2.5mol/L ammonia, back extraction is in a ratio of 5:1; After back extraction, organic facies returns and uses, and strip liquor is evaporating, concentrating and crystallizing at 80 DEG C, obtains rehenic acid ammonium product. Rehenic acid ammonium product purity is 99.7%, and the response rate of rhenium is 99.4%.
Embodiment 3:In this instance processes richness rhenium slag, rhenium-containing 2.5%, containing arsenic 28.9%, process technique, effect are as follows:
Weigh rich rhenium slag 150g, add 750mL pure water, stirring and evenly mixing; Being positioned in autoclave and carry out hot-pressure oxidation leaching by raw material after mixing, partial pressure of oxygen is 0.3MPa, response time 1h, reaction temperature 170 DEG C, after reaction terminates, is filtered by rhenium-containing leachate, washs, and now, the leaching rate of rhenium is 99.1%;The concentrated sulphuric acid 50mL of also middle addition 98% after filtration, acidity is adjusted 150g/L, rhenium-containing leachate after acidity being adjusted mixes with unloaded organic facies, being in a ratio of 9:1, concussion mixing 5min, clarifies 10min on the oscillator, release load organic phases, with pure water, then carrying out back extraction with 1mol/L ammonia, back extraction is in a ratio of 5:1; After back extraction, organic facies returns and uses, and strip liquor is evaporating, concentrating and crystallizing at 90 DEG C, obtains rehenic acid ammonium product. Rehenic acid ammonium product purity is 99.5%, and the response rate of rhenium is 98.9%.
Embodiment 4:In this instance processes richness rhenium slag, rhenium-containing 3.0%, containing arsenic 29.5%, process technique, effect are as follows:
Weigh rich rhenium slag 120g, add 600mL pure water, stirring and evenly mixing; Being positioned in autoclave and carry out hot-pressure oxidation leaching by raw material after mixing, partial pressure of oxygen is 1.5MPa, response time 3h, reaction temperature 140 DEG C, after reaction terminates, is filtered by rhenium-containing leachate, washs, and now, the leaching rate of rhenium is 99.2%; The concentrated sulphuric acid 60mL of also middle addition 98% after filtration, acidity is adjusted 160g/L, rhenium-containing leachate after acidity being adjusted mixes with unloaded organic facies, being in a ratio of 7:1, concussion mixing 5min, clarifies 15min on the oscillator, release load organic phases, with pure water, then carrying out back extraction with 2.5mol/L ammonia, back extraction is in a ratio of 5:1; After back extraction, organic facies returns and uses, and strip liquor is evaporating, concentrating and crystallizing at 70 DEG C, obtains rehenic acid ammonium product. Rehenic acid ammonium product purity is 99.5%, and the response rate of rhenium is 98.6%.
Embodiment 5:In this instance processes richness rhenium slag, rhenium-containing 3.0%, containing arsenic 29.5%, process technique, effect are as follows:
Weigh rich rhenium slag 150g, add 600mL pure water, stirring and evenly mixing; Being positioned in autoclave and carry out hot-pressure oxidation leaching by raw material after mixing, partial pressure of oxygen is 0.8MPa, response time 1.5h, reaction temperature 160 DEG C, after reaction terminates, is filtered by rhenium-containing leachate, washs, and now, the leaching rate of rhenium is 99.6%; The concentrated sulphuric acid 50mL of also middle addition 98% after filtration, acidity is adjusted 150g/L, rhenium-containing leachate after acidity being adjusted mixes with unloaded organic facies, being in a ratio of 8:1, concussion mixing 5min, clarifies 10min on the oscillator, release load organic phases, with pure water, then carrying out back extraction with 3mol/L ammonia, back extraction is in a ratio of 5:1; After back extraction, organic facies returns and uses, and strip liquor is evaporating, concentrating and crystallizing at 80 DEG C, obtains rehenic acid ammonium product. Rehenic acid ammonium product purity is 99.4%, and the response rate of rhenium is 99.2%.
The all technical of above five embodiments is to such as table 1.
Rhenium yield and purity in each embodiment of table 1
Relatively above five embodiments, it can be seen that recovery rate and the purity of embodiment 2 rhenium are the highest, are most preferred embodiments.
In above example, rich rhenium slag adopts autoclave hot-pressure oxidation to leach rhenium, and the major effect parameter in rule of operation includes liquid-solid ratio, extraction temperature, partial pressure of oxygen and extraction time; When liquid-solid ratio is lower than lower limit, being unfavorable for medium and oxidising agent, affect leaching rate, during higher than the upper limit, leachate volume increases difficulty to greatly your follow-up liquid concentration; When lower than lowest temperature, leaching rate reduces, and during higher than temperature upper limit, causes energy consumption high, and autoclave temperature restriction is unsuitable too high; When pressing in limited time lower than oxygen, reaction rate is slow, and oxidation is not exclusively.
The application of the present invention is not limited to above-mentioned citing; for those of ordinary skills; under the premise without departing from the principles of the invention, it is also possible to improved according to the above description or modify, all these improve or modify in the protection domain that all should fall into the claims in the present invention.
Claims (3)
1. the method preparing rehenic acid ammonium from rich rhenium slag, is characterized in that: it includes following operating procedure:
A. being added water by liquid-solid ratio 4 ~ 8:1 by richness rhenium slag and size mixing, utilize hot-pressure leaching method to process, control extraction temperature 100 ~ 200 DEG C, partial pressure of oxygen is 0.3 ~ 1.5MPa, and extraction time is 1 ~ 5h, and through filtering, to obtain rich rhenium liquid rhenium content be 3 ~ 10g/L in washing;
B. with addition of sulphuric acid, Controlled acidity 130 ~ 160g/L in rich rhenium liquid, it being mixed with unloaded organic facies, comparing O/A is 7 ~ 10:1, and vibrate mixing 5 ~ 10min, clarifies 10 ~ 20min, obtains load organic phases; Wherein, unloaded organic facies consists of 20% ~ 50%N235+ 25% ~ 40% sec-octyl alcohol+25% ~ 40% kerosene;
C. load organic phases is after water washing, carries out back extraction with 1 ~ 5mol/L ammonia, and 5:1 is compared in back extraction, and strip liquor is evaporation and concentration freezing and crystallizing at 70 ~ 90 DEG C, obtains rehenic acid ammonium product.
2. the method preparing as claimed in claim 1 rehenic acid ammonium from rich rhenium slag, is characterized in that: in described operating procedure A, extraction temperature scope more preferably is 130 ~ 170 DEG C.
3. the method preparing as claimed in claim 1 rehenic acid ammonium from rich rhenium slag, is characterized in that: in described operating procedure B, unloaded organic facies more preferably consists of 40%N235+ 30% sec-octyl alcohol+30% kerosene.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107236872A (en) * | 2017-05-26 | 2017-10-10 | 金川集团股份有限公司 | A kind of method that rhenium is reclaimed in the difficult poor rhenium slag from high-sulfur high-arsenic |
| CN108677010A (en) * | 2018-06-14 | 2018-10-19 | 中核通辽铀业有限责任公司 | A kind of ground-dipping uranium extraction comprehensive recycling process |
| CN114058854A (en) * | 2021-11-29 | 2022-02-18 | 铜陵铜冠优创特种材料有限公司 | Wet process for recovering rhenium-containing material |
| CN115724471A (en) * | 2022-11-30 | 2023-03-03 | 龙岩市宇恒环保科技有限公司 | Process for producing high-purity ammonium rhenate from rhenium-containing sulfide slag by full-wet method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107236872A (en) * | 2017-05-26 | 2017-10-10 | 金川集团股份有限公司 | A kind of method that rhenium is reclaimed in the difficult poor rhenium slag from high-sulfur high-arsenic |
| CN108677010A (en) * | 2018-06-14 | 2018-10-19 | 中核通辽铀业有限责任公司 | A kind of ground-dipping uranium extraction comprehensive recycling process |
| CN114058854A (en) * | 2021-11-29 | 2022-02-18 | 铜陵铜冠优创特种材料有限公司 | Wet process for recovering rhenium-containing material |
| CN115724471A (en) * | 2022-11-30 | 2023-03-03 | 龙岩市宇恒环保科技有限公司 | Process for producing high-purity ammonium rhenate from rhenium-containing sulfide slag by full-wet method |
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Application publication date: 20160615 |