CN109516502A - Method for extracting ammonium rhenate from high-risk solid waste copper-arsenic filter cake - Google Patents
Method for extracting ammonium rhenate from high-risk solid waste copper-arsenic filter cake Download PDFInfo
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- CN109516502A CN109516502A CN201710843182.2A CN201710843182A CN109516502A CN 109516502 A CN109516502 A CN 109516502A CN 201710843182 A CN201710843182 A CN 201710843182A CN 109516502 A CN109516502 A CN 109516502A
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- solid waste
- filter cake
- ammonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G47/00—Compounds of rhenium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a method for extracting ammonium rhenate from high-risk solid waste copper-arsenic filter cakes, and belongs to the technical field of rare metal smelting, high-risk solid waste treatment and resource comprehensive recycling. The method comprises four steps of copper-rhenium enrichment, copper-rhenium separation, rhenate solution preparation and rhenate crystallization. The method provided by the invention avoids the defects of acidification leaching in the prior art, utilizes the advantages of the treatment capacity of the traditional roasting process, and simultaneously overcomes the disadvantage of adverse effect on the environment in the traditional process, and the obtained ammonium rhenate has the advantages of extremely high purity, good recovery effect, simplicity and high efficiency in operation, environmental friendliness and low maintenance cost, and has great practical significance for the treatment of solid wastes and the recovery of scarce resources.
Description
Technical field
The invention belongs to dissipated metal field of metallurgy and solid dangerous waste recycling field, and in particular to a kind of high-risk solid waste
The method of rehenic acid ammonium is extracted in copper arsenic filter cake.
Background technique
Rhenium is a kind of metallic element, one of refractory metal, and fusing point is lower than 3410 degrees Celsius of tungsten, can be used to make
The shell of electric lamp filament, artificial satellite and rocket, protective plate of atomic pile etc. are made, catalyst is chemically used as.Rhenium is one
Real rare element.Its content in the earth's crust is all smaller than all rare earth elements, simply greater than protactinium and radium these elements.Again plus
It is upper it does not form fixed mineral, usually with other metal associations.
Rhenium metal and its alloy can Fountain pen nib and pyrometer couple processed, in dehydrogenating alcohol, synthesis ammonia and by titanium dioxide
Catalyst is made in sulphur sulfur trioxide.Tungstenic 90%, vanadium 1%, rhenium 9% alloy can high temperature resistant.Since the presence of rhenium disperses, valence
Lattice are expensive.Rhenium is widely used in modern industry each department, is mainly used as petroleum industry and auto industry catalyst, petroleum reforming catalysis
Agent, electronics industry and aerospace industry rhenium alloys etc..Rhenium can improve the intensity and plasticity of tungsten, molybdenum, chromium simultaneously, and people are this
Phenomenon is known as " rhenium effect ".W-Re and Mo Re alloys have good elevated temperature strength and plasticity, can be processed into plate, piece, line, silk,
Stick, thermal structure part, elastic element, electronic component etc. for space flight and aviation, it may also be used for manufacture heating element, workpiece, lamp
Bubble, X-ray instrument and medical instrument.W-Re-ThO2Alloy can be used as being heated at high temperature workpiece, and W-Re, Mo Re alloys contact have
High erosion and high-temperature electric conduction ability can improve the service life and functional reliability of power supply unit.Such as: platinum rhenium alloys, platinum tungsten
Rhenium alloys, tungsten-rhenium alloy, Mo Re alloys etc..
So far, copper arsenic filter cake is the important source material source for extracting rhenium metal, wherein preparing high-purity rehenic acid ammonium
It is the necessary link for preparing rhenium metal.Can heavy industrialization pass through microwave heating method carry out flue dust desulfurization dearsenification report
Also seldom.Return its reason, mainly to not deep enough and to microwave high-temperature heating equipment the application of understanding of micro-wave heating characteristic
Not enough extensively.
Preparing the main method of rehenic acid ammonium at present is that the technique leached by acid system high pressure is recycled, this method work
Skill long flow path, recovery efficiency be low, high production cost, equipment requirement are high.As mentioned in number of patent application 201610291100.3
A method of rehenic acid ammonium being prepared from rich rhenium slag, using precipitating reagent by low concentration richness rhenium slag in Copper making spent acid, uses NaClO3-
NaCl-H2SO4System leaches rich rhenium slag, adjusts pH value in leachate and clean, removal overwhelming majority bismuths and part copper, arsenic and
Then molybdenum is extracted and is stripped using organic phase, carry out concentration crystallisation by cooling to extract liquor and obtain rehenic acid ammonium crystal, this
Energy consumption is high, the reaction time is long, processing capacity is small for method leaching.
Summary of the invention
It is related to extracting rehenic acid ammonium in high-risk solid waste copper arsenic filter cake in order to solve the above technical problem, the present invention provides a kind of
Method, this method avoid the defect that acidification is leached, the very high purities of gained rehenic acid ammonium, and have efficient, environmental protection easy to operate
The advantages of.
To achieve the goals above, the present invention adopts the following technical scheme that:
A method of extracting rehenic acid ammonium from high-risk solid waste copper arsenic filter cake, this method comprises the following steps:
Step 1: additive being added in copper arsenic filter cake raw material, is stirred, then at 200-400 DEG C
It is roasted, realizes that arsenic, sulphur are detached from, obtain copper-rich richness rhenium intermediate products;
Step 2: obtained copper-rich richness rhenium intermediate products being crushed, are milled to obtain powder, chlorination is added in powder
Agent is granulated, and the volatilization of rhenium is then realized at 600-1200 DEG C, obtains rhenium volatile matter;
Step 3: obtained rhenium volatile matter sprays to obtain rehenic acid salting liquid using alkaline solution, carries out to rehenic acid salting liquid net
Eliminate miscellaneous, ion exchange and classical precipitating;
Step 4: being passed through ammonia for the PH of the rehenic acid salting liquid and be adjusted to 8.0-10.0, then be concentrated, crystallisation by cooling, again
Crystallization obtains high-purity rehenic acid ammonium product, while obtaining the product with high-grade copper.
Preferably, additive is soluble sodium salt and soluble ammonium salt, and soluble sodium salt is sodium chloride, nitric acid
Any one or a few mixing in sodium, sodium sulphate, sodium sulfite, sodium carbonate, sodium bicarbonate and sodium bisulfate, it is soluble
Ammonium salt be ammonium sulfate, ammonium chloride and ammonium nitrate in any one or a few mixing,
Preferably, the additional amount of additive is the mass fraction 2.0-30.0% of the copper arsenic filter cake raw material, it is highly preferred that
The additional amount of additive is the mass fraction 20.0% of the copper arsenic filter cake raw material.
Preferably, the temperature of roasting is 200-400 DEG C, it is highly preferred that the temperature of roasting is 300 DEG C.
Preferably, the granularity control of powder is in 20-200 mesh, it is highly preferred that the granularity of powder is controlled in 100 mesh.
Preferably, chlorinating agent is containing chloride salt, including potassium chloride, sodium chloride, calcium chloride, lead chloride, sodium chlorate and chlorine
One of sour potassium or several mixtures, the adding proportion of chlorinating agent are the mass fraction 10.0-50.0% of the powder,
It is highly preferred that the adding proportion of chlorinating agent is the mass fraction 40.0% of the powder
Preferably, alkaline solution is sodium hydroxide, potassium hydroxide, any one or a few the mixing in sodium bicarbonate.
Preferably, purification and impurity removal is to be precipitated using magnesium salts to micro arsenic impurities.
Preferably, ion exchange uses large aperture resin, and the large aperture resin volume exchange flow velocity is 1.0-3.0m3/
h。
Preferably, the classical precipitation method are that addition mass concentration is 5.0-20.0% ammonium chloride or ammonium hydroxide at 60-80 DEG C
It is static, then Bag filter is carried out after natural subsidence to 7.0-8.0 by addition salt acid for adjusting pH.
Preferably, thickening temperature is 80-105 DEG C, and crystallisation by cooling temperature is 0 DEG C or less.
The beneficial effects of the present invention are:
A kind of method for extracting rehenic acid ammonium from high-risk solid waste copper arsenic filter cake provided by the invention, there is industrialization to clean
The high-risk solid waste of mass disposal has good industrial application value the characteristics of efficiently withdrawal using scarce resource
And prospect.The defect that the acidification that this technique avoids is leached, and the advantages of traditional roasting technique treating capacity is utilized, it improves simultaneously
The unfavorable disadvantage of effect on environment in traditional handicraft, the very high purity of gained rehenic acid ammonium, recovering effect be good, it is easy to operate efficiently,
It is environmental-friendly, maintenance cost is low, the processing and scarce resource to solid waste recycling have great Practical significance.
Specific embodiment
To keep the purpose of the present invention, feature, advantage more obvious and understandable, below in the embodiment of the present invention
Technical solution is clearly and completely described, it is clear that and the embodiments described below are only a part of the embodiment of the present invention,
And not all embodiments.Based on the embodiments of the present invention, those skilled in the art's every other embodiment obtained, all
Belong to the scope of protection of the invention.
Embodiment 1
The sodium bisulfate of mass fraction 2.0% is added in copper arsenic filter cake raw material, is stirred, then will
The material is roasted at 200 DEG C or less, realizes that arsenic, sulphur are detached from;Obtained copper-rich richness rhenium intermediate products are crushed, are milled
Powder is obtained, powder particles control is 20 mesh, and the potassium chloride of mass fraction 15.0% is added in powder, is granulated, then
The volatilization of rhenium is realized at 600 DEG C;Obtained rhenium volatile matter obtains rehenic acid sodium solution by spray using sodium hydroxide solution, to rhenium
The magnesium chloride solution that acid sodium solution adds mass fraction 3.0% carries out purification and impurity removal, and purification and impurity removal is using magnesium salts to micro
The impurity such as arsenic are precipitated, using the large aperture D312 resin in 1.5m3Ion exchange is carried out under the exchange flow velocity of/h, adds ammonium hydroxide
It is static, it is then 8.0 with salt acid for adjusting pH, carries out natural sedimentation;It is passed through ammonia and adjusts pH to 9.0 values, carried out at 90 DEG C dense
Contracting, at -4 DEG C crystallisation by cooling, be recrystallized to give high-purity rehenic acid ammonium product, while obtaining the product with high-grade copper.
Test result shows: high-risk solid waste copper arsenic filter cake is reached by the purity of the rehenic acid ammonium obtained after processing
99.2%, the rate of recovery 98.8%.
Embodiment 2
The ammonium sulfate of mass fraction 15.0% is added in copper arsenic filter cake raw material, is stirred, then will
The material is roasted at 400 DEG C or less, realizes that arsenic, sulphur are detached from;Obtained copper-rich richness rhenium intermediate products are crushed, are milled
To 200 mesh, the potassium chloride of mass fraction 50.0% being added in powder, is granulated, the volatilization of rhenium is then realized at 800 DEG C;
Obtained rhenium volatile matter obtains rehenic acid sodium solution by spray using potassium hydroxide solution, adds mass fraction to rehenic acid sodium solution
5.0% magnesium chloride solution carries out purification and impurity removal to trace impurities such as arsenic, using the large aperture D316 resin in 3.0m3The exchange of/h
Ion exchange is carried out under flow velocity, addition ammonium hydroxide is static, is then 8.0 with salt acid for adjusting pH, carries out natural sedimentation;It is passed through ammonia tune
Save pH10.0 value, be concentrated at 105 DEG C, at -1 DEG C crystallisation by cooling, be recrystallized to give high-purity rehenic acid ammonium product, simultaneously
Obtain the product with high-grade copper.
Test result shows: high-risk solid waste copper arsenic filter cake is reached by the purity of the rehenic acid ammonium obtained after processing
99.8%, the rate of recovery 99.2%.
Embodiment 3
The sodium carbonate of mass fraction 30.0% is added in copper arsenic filter cake raw material, is stirred, then will
The material is roasted at 300 DEG C or less, realizes that arsenic, sulphur are detached from;Obtained copper-rich richness rhenium intermediate products are crushed, are milled
To 100 mesh, the sodium chloride and 10.0% calcium chloride of mass fraction 8.0% are added in powder, is granulated, then at 1200 DEG C
Realize the volatilization of rhenium;Obtained rhenium volatile matter obtains rehenic acid sodium solution by spray using sodium bicarbonate solution, molten to rehenic acid sodium
The magnesium chloride solution that liquid adds mass fraction 10.0% carries out purification and impurity removal to impurity such as micro amount of arsenic, using the large aperture D310 resin
In 1.0m3Ion exchange is carried out under the exchange flow velocity of/h, addition ammonium hydroxide is static, is then 7.0 with salt acid for adjusting pH, carries out nature
Precipitating;Be passed through ammonia adjust pH to 9.0, be concentrated at 80 DEG C, at -5 DEG C crystallisation by cooling, be recrystallized to give high-purity rhenium
Sour ammonium product, while obtaining the product with high-grade copper.
Test result shows: high-risk solid waste copper arsenic filter cake is reached by the purity of the rehenic acid ammonium obtained after processing
99.5%, the rate of recovery 99.0%.
Embodiment 4
The sodium sulfite of mass fraction 20.0% is added in copper arsenic filter cake raw material, is stirred, then
The material is roasted at 200 DEG C or less, realizes that arsenic, sulphur are detached from;Obtained copper-rich richness rhenium intermediate products are crushed, are ground
Powder adds the sodium chlorate of mass fraction 40.0% in powder, is granulated, then realize waving for rhenium at 800 DEG C to 100 mesh
Hair;Obtained rhenium volatile matter obtains rehenic acid sodium solution by spray using potassium hydroxide solution, adds quality to rehenic acid sodium solution
The magnesium chloride solution of score 5.0% carries out purification and impurity removal, using the large aperture D316 resin in 3.0m3It is carried out under the exchange flow velocity of/h
Ion exchange, addition ammonium hydroxide is static, and then adjusting pH7.5 with hydrochloric acid is to carry out natural sedimentation;It is passed through ammonia and adjusts pH to 8.5
Value, be concentrated at 105 DEG C, at -5 DEG C crystallisation by cooling, be recrystallized to give high-purity rehenic acid ammonium product, while being had
The product of high-grade copper.
Test result shows: high-risk solid waste copper arsenic filter cake is reached by the purity of the rehenic acid ammonium obtained after processing
99.4%, the rate of recovery 99.1%.
Embodiment 5
The sodium bisulfate of mass fraction 35.0% is added in copper arsenic filter cake raw material, is stirred, then
The material is roasted at 350 DEG C or less, realizes that arsenic, sulphur are detached from;Obtained copper-rich richness rhenium intermediate products are crushed, are ground
Powder adds the sodium chloride and 10.0% calcium chloride of mass fraction 8.0% in powder, is granulated, then 900 to 150 mesh
DEG C realize rhenium volatilization;Obtained rhenium volatile matter obtains rehenic acid sodium solution by spray using sodium bicarbonate solution, to rehenic acid sodium
The magnesium chloride solution that solution adds mass fraction 10.0% carries out purification and impurity removal to impurity such as micro amount of arsenic, using the large aperture D310 tree
Rouge is in 1.0m3Ion exchange is carried out under the exchange flow velocity of/h, addition ammonium hydroxide is static, is then 7.6 with salt acid for adjusting pH, carries out certainly
So precipitating;Be passed through ammonia adjust pH to 9.5, be concentrated at 80 DEG C, at -6 DEG C crystallisation by cooling, be recrystallized to give it is high-purity
Rehenic acid ammonium product, while obtaining the product with high-grade copper.
Test result shows: high-risk solid waste copper arsenic filter cake is reached by the purity of the rehenic acid ammonium obtained after processing
99.2%, the rate of recovery 99.6%.
Above-mentioned, although specific embodiments of the present invention have been described, not to the limit of the scope of the present invention
System, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art do not need to pay
The various modifications or changes that creative work can be made out are still within the scope of the present invention.
Claims (10)
1. a kind of method for extracting rehenic acid ammonium from high-risk solid waste copper arsenic filter cake, which is characterized in that this method comprises the following steps:
Step 1: additive being added in copper arsenic filter cake raw material, is stirred, is then carried out at 200-400 DEG C
Roasting realizes that arsenic, sulphur are detached from, obtains copper-rich richness rhenium intermediate products;
Step 2: obtained copper-rich richness rhenium intermediate products are crushed, are milled to obtain powder, chlorinating agent is added in powder, into
Row is granulated, and the volatilization of rhenium is then realized at 600-1200 DEG C, obtains rhenium volatile matter;
Step 3: obtained rhenium volatile matter sprays to obtain rehenic acid salting liquid using alkaline solution, carries out purification to rehenic acid salting liquid and removes
Miscellaneous, ion exchange and classical precipitating;
Step 4: being passed through ammonia for the PH of the rehenic acid salting liquid and be adjusted to 8.0-10.0, then be concentrated, crystallisation by cooling, recrystallization
High-purity rehenic acid ammonium product is obtained, while obtaining the product with high-grade copper.
2. the method according to claim 1 for extracting rehenic acid ammonium from high-risk solid waste copper arsenic filter cake, which is characterized in that described
Additive is soluble sodium salt and soluble ammonium salt, and the sodium salt of the solubility is sodium chloride, sodium nitrate, sodium sulphate, Asia
The ammonium salt of any one or a few mixing in sodium sulphate, sodium carbonate, sodium bicarbonate and sodium bisulfate, the solubility is
Any one or a few mixing in ammonium sulfate, ammonium chloride and ammonium nitrate, the additional amount of the additive are copper arsenic filter
The mass fraction 2.0-30.0% of cake raw material.
3. the method according to claim 1 for extracting rehenic acid ammonium from high-risk solid waste copper arsenic filter cake, which is characterized in that described
The temperature of roasting is 200-400 DEG C.
4. the method according to claim 1 for extracting rehenic acid ammonium from high-risk solid waste copper arsenic filter cake, which is characterized in that described
The granularity of powder is controlled in 20-200 mesh.
5. the method according to claim 1 for extracting rehenic acid ammonium from high-risk solid waste copper arsenic filter cake, which is characterized in that described
Chlorinating agent be containing one of chloride salt, including potassium chloride, sodium chloride, calcium chloride, lead chloride, sodium chlorate and potassium chlorate or
Several mixtures, the adding proportion of the chlorinating agent are the mass fraction 10.0-50.0% of the powder.
6. the method according to claim 1 for extracting rehenic acid ammonium from high-risk solid waste copper arsenic filter cake, which is characterized in that described
Alkaline solution is sodium hydroxide, potassium hydroxide, any one or a few the mixing in sodium bicarbonate.
7. the method according to claim 1 for extracting rehenic acid ammonium from high-risk solid waste copper arsenic filter cake, which is characterized in that described
Purification and impurity removal is to be precipitated using magnesium salts to micro arsenic impurities.
8. the method according to claim 1 for extracting rehenic acid ammonium from high-risk solid waste copper arsenic filter cake, which is characterized in that described
Ion exchange uses large aperture resin, and the large aperture resin volume exchange flow velocity is 1.0-3.0m3/h。
9. the method according to claim 1 for extracting rehenic acid ammonium from high-risk solid waste copper arsenic filter cake, which is characterized in that described
The classical precipitation method are that addition mass concentration is that 5.0-20.0% ammonium chloride or ammonium hydroxide are static, then pass through addition at 60-80 DEG C
Salt acid for adjusting pH carries out Bag filter after natural subsidence to 7.0-8.0.
10. the method according to claim 1 for extracting rehenic acid ammonium from high-risk solid waste copper arsenic filter cake, which is characterized in that institute
Stating thickening temperature is 80-105 DEG C, and the crystallisation by cooling temperature is 0 DEG C or less.
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Cited By (1)
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