CN105800648A - Application method of ammonium sulfate prepared from smelting offgas - Google Patents
Application method of ammonium sulfate prepared from smelting offgas Download PDFInfo
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- CN105800648A CN105800648A CN201610128537.5A CN201610128537A CN105800648A CN 105800648 A CN105800648 A CN 105800648A CN 201610128537 A CN201610128537 A CN 201610128537A CN 105800648 A CN105800648 A CN 105800648A
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- ammonium sulfate
- ammonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
-
- 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
- C22B34/22—Obtaining vanadium
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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 relates to an application method of ammonium sulfate prepared from smelting offgas, belongs to the field of chemical industry and metallurgy and aims at providing an application method of ammonium sulfate prepared from smelting offgas. The method comprises the following steps: (a) preparation of a vanadium precipitator liquid dissolving the ammonium sulfate prepared from smelting offgas in a solvent with a temperature higher than or equal to 85 DEG C to obtain an ammonium sulfate solution with a mass percentage concentration of 40-50%; filtering and removing water insoluble matters; and adding an oxidizing agent to obtain a vanadium precipitator solution; and (b) vanadium precipitation: adjusting the pH value of vanadium liquid using sulfuric acid, and adding the vanadium precipitator solution for ammonium salt vanadium precipitation to obtain ammonium polyvanadate or ammonium metavanadate; and washing and purifying to obtain vanadium products such as vanadium oxide. The method provided by the invention has the characteristics of simple flow, good reaction activity, efficient resource utilization and the like and can widen the application field of the smelting offgas ammonium sulfate product, reduce the production cost of vanadium products and enhance the core competitiveness of the vanadium products.
Description
Technical field
The present invention relates to the Application way of the ammonium sulfate that a kind of flue gas during smelting is produced, belong to chemical industry and field of metallurgy.
Background technology
Steel smelting procedure needs use the high-valence state Fe in substantial amounts of reductive coke Ore, containing substantial amounts of SO in the blast furnace tail gas of generation2, take desulfurizing agent adsorption and enrichment SO at present2、SO2Parsing catalytic oxidation is SO3, dilute sulfuric acid or water absorb SO3Prepare the SO in the PROCESS FOR TREATMENT tail gas of sulphuric acid2；Meanwhile, in the Coal Chemical Industry process of producing product being closely related with smelting iron and steel, produce substantial amounts of containing ammonia coal gas, containing ammonia coal gas through containing SO2Generating ammonium sulfate after the sulfuric acid absorption enrichment that tail gas is produced, solution degree of reaching capacity precipitates out ammonium sulfate product.The blast furnace tail gas etc. produced in v-bearing titanomagnetite smelting process can be prepared by ammonium sulfate after above-mentioned purified treatment.The apparent blackout of this type of ammonium sulfate product, color and luster is uneven, and N content (in butt) is about 21%, substantially conforms to GB535-1995 technical conditions, but Fe and water is insoluble exceeds standard, especially water-insoluble is higher than GB535-1995 technical conditions about 10 times；It addition, containing the C of about 0.2%；This type of ammonium sulfate overall qualities is on the low side, and industrial application value is low, and sales promotion is difficult and on the low side.
In tradition ammonium salt precipitation technique, it is typically in vanadium solution being directly added into ammonium sulfate carrying out precipitation as precipitant.And the ammonium sulfate that flue gas during smelting is produced, owing to its product ammonium sulfate overall qualities is on the low side, not only can bring impurity into when precipitation, affect the purity of the products such as vanadium oxide, precipitation rate also can be made simultaneously to reduce, time serious, even be difficult to precipitation.Therefore, at present, the industrial ammonium sulfate not adopting flue gas during smelting to produce is to carry out precipitation.
Summary of the invention
Present invention solves the technical problem that the Application way being to provide the ammonium sulfate that flue gas during smelting is produced.
The Application way of the ammonium sulfate that flue gas during smelting of the present invention is produced, comprises the following steps:
A, precipitation agent solution preparation: the ammonium sulfate produced by flue gas during smelting is dissolved in the solvent of temperature >=85 DEG C, produces and obtains the ammonium sulfate that mass percentage concentration is 40～50%, filter, add oxidant, obtain precipitation agent solution；
B, precipitation: regulate the pH value of vanadium liquid, add precipitation agent solution and carry out ammonium salt precipitation, produce and obtain ammonium poly-vanadate or ammonium metavanadate.
Further, in a step, in mass ratio, oxidant: ammonium sulfate=1:5～20 that flue gas during smelting is produced；It is preferably oxidant: ammonium sulfate=1:8～12 that flue gas during smelting is produced, more preferably oxidant: ammonium sulfate=1:9.28 that flue gas during smelting is produced.
Further, in a step, described oxidant is Ammonium persulfate. or hydrogen peroxide.
Wherein, in a step, described solvent is water or Upper-liquor of Precipitating Vanadate Process.
The ammonium sulfate that flue gas during smelting of the present invention is produced is: in steel smelting procedure produce containing SO2The sulphuric acid that tail gas is produced, absorb Coal Chemical Industry process of producing product produces containing ammonia coal gas, generate ammonium sulfate, the ammonium sulfate product that ammonium sulfate degree of reaching capacity precipitates out after enrichment.
The essence of the inventive method is that water-soluble for low-quality ammonium sulfate filtration is removed water-insoluble to realize purifying, ammonium sulfate after purification adds the oxidants such as Ammonium persulfate. and carries out the ammonium salt precipitation of vanadium liquid as adjuvant, ammonium persulfate oxidizing agent suppresses the reducing substances in the ammonium sulfate that flue gas during smelting is produced that the high price vanadium in vanadium liquid is reduced to Low Valent Vanadium, Low Valent Vanadium not with ammonium in conjunction with Precipitation, the mixed solution of the flue gas during smelting ammonium sulfate after purification and Ammonium persulfate. produces ammonium vanadate as precipitation adjuvant, and the technique of precipitation is mainly ammonium salt precipitation；Purification process is the water solublity principle of applied material, and the water-insoluble impurity in ammonium sulfate is separated by filtration removal, and solvent can use water for industrial use or Upper-liquor of Precipitating Vanadate Process, uses Upper-liquor of Precipitating Vanadate Process then to may utilize acid therein and ammonium, reaches joint acid and the purpose of joint ammonium；The principle of precipitation process is that vanadium solution polymerized form when different acid degree is different, and can be combined the enrichment producing the precipitation of ammonium vanadate polymer and realize vanadium with ammonium salt, and the ammonium vanadate produced is for producing the vanadium products such as vanadium oxide；Meanwhile, ammonium sulfate is used to replace the directly interpolation solid ammonium sulfate precipitation in traditional handicraft, enhance reactivity and the uniformity of vanadic acid root and ammonium ion, optimize the dynamic condition that ammonium ion reacts with vanadic acid radical ion, have and react feature rapidly and uniformly.
In whole technical process, take full advantage of the water solublity of material and separation principle achieves the purification of water-insoluble of flue gas during smelting ammonium sulfate, use the oxidants such as Ammonium persulfate. to inhibit the generation of Low Valent Vanadium, make precipitation reaction more thorough, and optimize the dynamic conditions that ammonium ion reacts with vanadic acid radical ion.It is more than 48.7% by TV content in the ammonium poly-vanadate that the inventive method obtains, Na2O+K2O content is not higher than 0.9%, and rate of deposition is more than 99.4%.
The inventive method has the features such as technological process is simple, reactivity good, the utilization of resources is efficient, can widen the application of flue gas during smelting ammonium sulfate product, reduces vanadium production cost, improves vanadium product core competitiveness.
Detailed description of the invention
The Application way of the ammonium sulfate that flue gas during smelting of the present invention is produced, comprises the following steps:
A, precipitation agent solution preparation: the ammonium sulfate produced by flue gas during smelting is dissolved in the solvent of temperature >=85 DEG C, produces and obtains the ammonium sulfate that mass percentage concentration is 40～50%, filters, and removes water-insoluble, and adds oxidant, obtains precipitation agent solution；
B, precipitation: use sulphuric acid to regulate the pH value of vanadium liquid, add precipitation agent solution and carry out ammonium salt precipitation, produce the ammonium poly-vanadate or ammonium metavanadate that obtain, be used for producing the vanadium products such as vanadium oxide after scrubbed purification.
Through research find, the ammonium sulfate that flue gas during smelting is produced contains the material of partial reductive, during for precipitation, it is easy to the high price vanadium in vanadium liquid is reduced to Low Valent Vanadium, Low Valent Vanadium not with ammonium in conjunction with Precipitation, thus affecting precipitation rate.Therefore, for improving precipitation rate, in a step, in mass ratio, oxidant: ammonium sulfate=1:5～20 that flue gas during smelting is produced；It is preferably oxidant: ammonium sulfate=1:8～12 that flue gas during smelting is produced, more preferably oxidant: ammonium sulfate=1:9.28 that flue gas during smelting is produced.
In order to ensure Oxidation and not increase additional impurities, described oxidant is preferably Ammonium persulfate. or hydrogen peroxide.Wherein, the quality of hydrogen peroxide is in the hydrogen peroxide of mass fraction 30%.
Described steam solvent is water or Upper-liquor of Precipitating Vanadate Process, uses Upper-liquor of Precipitating Vanadate Process recoverable ammonium therein and acid.Described water can adopt water for industrial use or steam condensate (SC).After vanadium liquid carries out precipitation, solid-liquid separation, solid is ammonium poly-vanadate or ammonium metavanadate, and the liquid of gained is Upper-liquor of Precipitating Vanadate Process.
The ammonium sulfate that flue gas during smelting of the present invention is produced be in steel smelting procedure produce containing SO2In the sulfuric acid absorption Coal Chemical Industry process of producing product that tail gas is produced produce containing ammonia coal gas, after enrichment generate ammonium sulfate, ammonium sulfate degree of reaching capacity precipitate out ammonium sulfate product.
In the Application way of the ammonium sulfate that flue gas during smelting of the present invention is produced, the technique of b step precipitation is the ammonium salt precipitation technique that this area is conventional, and its parameter does not repeat at this.
Concrete, the present invention can adopt following technique:
The ammonium sulfate produced by flue gas during smelting is dissolved in the water of temperature >=85 DEG C, makes the ammonium sulfate that mass percentage concentration is 40～50%, and sucking filtration removal black insoluble matter is standby and adds oxidant；Measure the vanadium solution of metering, according to ammonium salt precipitation technological requirement, (acid ammonium salt precipitation process endpoint pH value is 2～2.5, faintly acid ammonium salt precipitation process endpoint pH value is 4～6, basic ammonium salts precipitation process endpoint pH value is 8～9), add concentrated sulphuric acid or dilute sulfuric acid regulates pH value of solution, add ammonium coefficient 1.2～2.0, precipitated and boiled under rear stirring condition, filtering and washing filter cake after standing sedimentation, filtration cakes torrefaction obtains vanadate；Wherein regulating pH value can the various ways such as a step acid adding and distribution acid adding.
Below in conjunction with embodiment, the specific embodiment of the present invention is further described, does not therefore limit the present invention among described scope of embodiments.
Embodiment 1
Weighing the ammonium sulfate that 325g flue gas during smelting is produced, be dissolved in the water of 425g temperature >=85 DEG C, sucking filtration is removed black insoluble matter and is added 35g Ammonium persulfate., obtains precipitation agent solution, stand-by；(vanadium concentration is 40.1g/L to measure vanadium solution 5L, pH value is 10), adding concentrated sulphuric acid adjustment pH value is 6, add precipitation agent solution 780g stir and heat to 55 DEG C, continuing to heat and drip concentrated sulphuric acid stirring and adjusting mixed liquor pH value is 2.0, after boiling 35min under stirring condition, the cold 30min of standing sedimentation, filters and washing leaching cake；After testing, in APV (ammonium poly-vanadate), TV content is 48.7%, Na2O+K2O content is 0.85%, and rate of deposition is 99.7%.
Embodiment 2
Weighing the ammonium sulfate that 290g flue gas during smelting is produced, be dissolved in the Upper-liquor of Precipitating Vanadate Process of 425g temperature >=85 DEG C, in described Upper-liquor of Precipitating Vanadate Process, liquid containing ammonium sulfate is about 36g, and sucking filtration is removed black insoluble matter and added 35g Ammonium persulfate., obtains precipitation agent solution, stand-by；(vanadium concentration is 40.1g/L to measure vanadium solution 5L, pH value is 10), adding concentrated sulphuric acid adjustment pH value is 6, add precipitation agent solution 785g stir and heat to 55 DEG C, continuing to heat and drip concentrated sulphuric acid stirring and adjusting mixed liquor pH value is 2.0, after boiling 35min under stirring condition, the cold 30min of standing sedimentation, filters and washing leaching cake；After testing, in APV, TV content is 48.9%, Na2O+K2O content is 0.89%, and rate of deposition is 99.6%.And using Upper-liquor of Precipitating Vanadate Process, the treating capacity of recoverable ammonium salt therein and minimizing waste water, final realization reduces cost.
Embodiment 3
Weighing the ammonium sulfate that 290g flue gas during smelting is produced, be dissolved in the water of 340g temperature >=85 DEG C, sucking filtration is removed black insoluble matter and is added 25g Ammonium persulfate., obtains precipitation agent solution, stand-by；(vanadium concentration is 36.2g/L to measure vanadium solution 5L, pH value is 11), adding concentrated sulphuric acid adjustment pH value is 7, add precipitation agent solution 650g stir and heat to 55 DEG C, continuing to heat and drip concentrated sulphuric acid stirring and adjusting mixed liquor pH value is 2.0, after boiling 30min under stirring condition, the cold 30min of standing sedimentation, filters and washing leaching cake；After testing, in APV, TV content is 48.9%, Na2O+K2O content is 0.75%, and rate of deposition is 99.4%.
Embodiment 4
Weighing the ammonium sulfate that 285g flue gas during smelting is produced, be dissolved in the water of 320g temperature >=85 DEG C, sucking filtration is removed black insoluble matter and is added the hydrogen peroxide 14g of 30%, obtains precipitation agent solution, stand-by；Measuring vanadium solution 4L (vanadium concentration is 32.8g/L, and pH value is 10), adding concentrated sulphuric acid adjustment pH value is 8.5, adds precipitation agent solution 620g and stirs and heated and boiled 30min, the cold 40min of standing sedimentation, filters and washing leaching cake；After testing, AMV (ammonium metavanadate) purity reaches more than 99%, precipitates yield more than 97%.
Comparative example 1
(vanadium concentration is 40.1g/L to measure vanadium solution 5L, pH value is 10), adding concentrated sulphuric acid adjustment pH value is 6, add the ammonium sulfate (explanation: employ 35g Ammonium persulfate. in embodiment 1 that 345g flue gas during smelting is produced, Ammonium persulfate. has Oxidation on the one hand, can provide ammonium ion on the other hand；Difference in order to avoid embodiment 1 with comparative example 1 ammonium ion amount, it is ammonium sulfate by the conversion of 35g Ammonium persulfate., therefore, ammonium sulfate addition is 345g), stirring and heat to 55 DEG C, continuing to heat and drip concentrated sulphuric acid stirring and adjusting mixed liquor pH value is 2.0, after boiling 35min under stirring condition, the cold 30min of standing sedimentation, filters and washing leaching cake；After testing, in APV, TV content is 48.4%, Na2O+K2O content is 1.02%, and rate of deposition is 98.4%.
Comparative example 2
(illustrating: employ 35g Ammonium persulfate. in embodiment 1, Ammonium persulfate. has Oxidation on the one hand, can provide ammonium ion on the other hand to weigh the ammonium sulfate that 345g flue gas during smelting produces；In order to avoid the difference of embodiment 1 with comparative example 2 ammonium ion amount, being ammonium sulfate by the conversion of 35g Ammonium persulfate., therefore, ammonium sulfate addition is 345g), it is dissolved in the water of 425g temperature >=85 DEG C, sucking filtration removes black insoluble matter, obtains precipitation agent solution, stand-by；(vanadium concentration is 40.1g/L to measure vanadium solution 5L, pH value is 10), adding concentrated sulphuric acid adjustment pH value is 6, add precipitation agent solution 770g stir and heat to 55 DEG C, continuing to heat and drip concentrated sulphuric acid stirring and adjusting mixed liquor pH value is 2.0, after boiling 35min under stirring condition, the cold 30min of standing sedimentation, filters and washing leaching cake；After testing, in APV, TV content is 48.6%, Na2O+K2O content is 1.05%, and rate of deposition is 97.8%.
Claims (5)
1. the Application way of the ammonium sulfate that flue gas during smelting is produced, it is characterised in that comprise the following steps:
A, precipitation agent solution preparation: the ammonium sulfate produced by flue gas during smelting is dissolved in the solvent of temperature >=85 DEG C, produces and obtains the ammonium sulfate that mass percentage concentration is 40～50%, filter, add oxidant, obtain precipitation agent solution；
B, precipitation: regulate the pH value of vanadium liquid, add precipitation agent solution and carry out ammonium salt precipitation, produce and obtain ammonium poly-vanadate or ammonium metavanadate.
2. the Application way of the ammonium sulfate that flue gas during smelting according to claim 1 is produced, it is characterised in that: in a step, in mass ratio, oxidant: ammonium sulfate=1:5～20 that flue gas during smelting is produced；It is preferably oxidant: ammonium sulfate=1:8～12 that flue gas during smelting is produced, more preferably oxidant: ammonium sulfate=1:9.28 that flue gas during smelting is produced.
3. the Application way of the ammonium sulfate that flue gas during smelting according to claim 1 and 2 is produced, it is characterised in that: in a step, described oxidant is Ammonium persulfate. or hydrogen peroxide.
4. the Application way of the ammonium sulfate that flue gas during smelting according to claim 3 is produced, it is characterised in that: in a step, described solvent is water or Upper-liquor of Precipitating Vanadate Process.
5. the Application way of the ammonium sulfate that the flue gas during smelting according to any one of Claims 1 to 4 is produced, it is characterised in that: the ammonium sulfate that described flue gas during smelting is produced is: in steel smelting procedure produce containing SO2The sulphuric acid that tail gas is produced, absorb Coal Chemical Industry process of producing product produces containing ammonia coal gas, generate ammonium sulfate, the ammonium sulfate product that ammonium sulfate degree of reaching capacity precipitates out after enrichment.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112239806A (en) * | 2020-10-29 | 2021-01-19 | 攀枝花市山青钒业有限公司 | Method for extracting vanadium from acidic high-phosphorus vanadium solution |
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