CN107236866A - A kind of method of v-bearing steel slag pressurization reinforcing vanadium extraction - Google Patents
A kind of method of v-bearing steel slag pressurization reinforcing vanadium extraction Download PDFInfo
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- CN107236866A CN107236866A CN201710480240.XA CN201710480240A CN107236866A CN 107236866 A CN107236866 A CN 107236866A CN 201710480240 A CN201710480240 A CN 201710480240A CN 107236866 A CN107236866 A CN 107236866A
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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
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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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
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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Abstract
The present invention relates to a kind of method of v-bearing steel slag pressurization reinforcing vanadium extraction, methods described is：The mixed solution of sodium carbonate and sodium hydroxide is mixed with v-bearing steel slag, carries out obtaining mixed slurry after the completion of Leach reaction, reaction under conditions of heating pressurization；By obtained mixed slurry separation of solid and liquid, tailings is obtained and containing vanadium leachate.The present invention can realize the efficient vanadium extracting from v-bearing steel slag, and leaching rate >=85% of vanadium reaches as high as more than 95%.The method that the present invention is leached using direct weighting extracts the vanadium in vanadium raw materials, can not only save roasting process energy consumption, and produce without the harmful kiln gas of roasting；It is circularly used for leaching slag, whole process non-wastewater discharge after obtained vanadium extraction containing vanadium leachate.The present invention is a kind of efficient, cleaning extraction vanadium method, it is adaptable to industrialized production, is had a good application prospect.
Description
Technical field
The present invention relates to vanadium field of chemical metallurgical technology, and in particular to a kind of method of v-bearing steel slag pressurization reinforcing vanadium extraction.
Background technology
V-bearing steel slag be smelt vanadium titano-magnetite byproduct, be vanadium-bearing hot metal steel-making formed contain V2O5In 2-10%
Slag (its calcium content is big compared with vanadium slag), its generation process has two kinds of approach, and a kind of is remaining vanadium in half steel through steel-making
Rear oxidation enters in slag, and another is that the molten iron direct steelmaking without the vanadium slag that blows obtains v-bearing steel slag.V-bearing steel slag has such as
Lower feature：(1) CaO and iron content are high, and crystallization is perfect, and quality is closely knit, and degree of dissociation is poor；(2) complicated component, and fluctuate larger；(3)
Content of vanadium is relatively low, and vanadium Dispersed precipitate is in a variety of ore deposit phases, complicated occurrence state.Based on above feature, how v-bearing steel slag is entered
The effective vanadium extraction of row is still a problem of field of metallurgy.
Nearly million tons of the v-bearing steel slag that China discharges every year, not only pollutes environment, and cause the loss of valuable element vanadium.Mesh
Before, v-bearing steel slag vanadium extraction mainly has 2 kinds of approach, and one is that v-bearing steel slag returns to ironmaking Vanadium Concentrationin, produces height and contains vanadium slag, further
Vanadium extraction, i.e., add as flux using v-bearing steel slag and enter blast furnace process in sintering deposit, vanadium is fused in molten iron, and height is obtained through blowing vanadium
Grade vanadium slag, is used as vanadium extraction or the raw material of smelting ferrovanadium alloy.Although the technique can reclaim the valuable elements such as iron, manganese, drop simultaneously
Low iron steel than energy consumption, but easily cause phosphorus circulation collection in molten iron, aggravate slag dephosphorization task；And slag impurity is more, effectively
CaO content is relatively low, can reduce grade of sinter, increases ironmaking processes energy consumption, therefore this method fails to be promoted.It is another
The processing method for planting v-bearing steel slag is direct vanadium extracting method, there is the works such as sodium roasting, calcification baking, the roasting of drop calcium and direct acidleach
Skill.Sodium roasting is the soluble sodium salt that Low Valent Vanadium is oxidized to 5 valency vanadium using salt or soda as additive by being calcined, and is adopted
Leached with water or carbonating.The technique vanadium to turn leaching rate relatively low, sodium salt consumption is big, roasting process pollution air, is difficult to administer, and
The technique is not suitable for V2O5The converter slag that content is low, CaO content is high.Calcification baking is to make roasting flux with lime etc., using carbon
The Leaching Vanadiums such as acidifying leaching.This method has certain selectivity to material, there is relatively low, high expensive of conversion ratio etc. to general slag
Problem, is unsuitable for large-scale production.Drop calcium roasting is proposed that its purpose is to solve CaO in v-bearing steel slag to contain by Amiri
The problem of amount height causes vanadium hardly possible leaching.It is by slag and Na to drop calcium roasting3PO4、Na2CO3It is baking mixed, Na3PO4Combined with CaO
Form Ca3(PO4)2, vanadium and sodium generates water miscible sodium vanadate, and then water logging is leachable vanadium.But the method only rests on laboratory
Conceptual phase, and phosphatic proportioning is big, cost is high, and there is presently no industrialization promotion.Direct acidleach refers to not fired work
Sequence, complete wet method vanadium extraction, but due to CaO content height in slag, acid consumption is larger, and cost is higher；Acidleach process need to be in strong acid solution
Middle to carry out, obtained leachate impurity is more, it is difficult to carry out later separation.
The side for extracting vanadium, chromium from v-bearing steel slag with the potassium hydroxide medium of high alkalinity is proposed in the A of CN 102071321
Method, the method does not need high-temperature roasting, and reaction temperature is reduced to 160-240 DEG C, wet method vanadium extraction chromium, during effectively prevent
C12、HCl、SO2, the atmosphere pollution such as dust, and reduce waste water yield and discharge capacity；Have the disadvantage that KOH media are expensive,
And the mass ratio of KOH and slag is 3:1 to 5:1st, reaction alkali concn is 60%-90%, then the KOH media being lost are more, cause
Production cost is higher, the reduction of product benefit.
The A of CN 102094123 propose the side that a kind of sodium hydroxide medium of use high concentration extracts vanadium from v-bearing steel slag
Method, this method reaction temperature be 180-240 DEG C, wet method vanadium extraction, during without waste gas, dust pollution；Have the disadvantage that alkali concn is higher,
Basicity is 65%-90%, then the heat of evaporation and concentration needs when causing the medium circulation to utilize is higher, then production cost is higher,
And remaining V amounts are higher in finishing slag, leaching rate is not high, and V content is 0.3%-0.5% in finishing slag.
The content of the invention
In view of problems of the prior art, it is an object of the invention to provide a kind of side of v-bearing steel slag pressurization reinforcing vanadium extraction
Method, realizes the efficient vanadium extraction from v-bearing steel slag, and leaching rate >=85% of vanadium reaches as high as nothing in 97%, and vanadium extracting process
Waste water and gas is discharged, and is a kind of efficient, cleaning extraction vanadium method.
For up to this purpose, the present invention uses following technical scheme：
The present invention provides a kind of method of v-bearing steel slag pressurization reinforcing vanadium extraction, the described method comprises the following steps：
(1) mixed solution of sodium carbonate and sodium hydroxide is mixed with v-bearing steel slag, carried out under conditions of heating pressurization
Mixed slurry is obtained after the completion of Leach reaction, reaction；
(2) the mixed slurry separation of solid and liquid for obtaining step (1), obtains tailings and containing vanadium leachate.
V-bearing steel slag main component is calcium silicates, calcium ferrite, iron oxide and titanomagnetite, and wherein vanadium is mainly wrapped in silicic acid
In calcium and calcium ferrite, it is achieved that the key that vanadium is extracted, which is reinforcing, decomposes calcium silicates and calcium ferrite.Silicate is in strong alkali solution
In have a good resolution characteristic, and under same concentration, sodium hydroxide is stronger compared with sodium carbonate basicity, and the decomposability of calcium silicates is more
It is good.Therefore, a certain amount of sodium hydroxide is added in the reaction system of Sodium Carbonate Leaching v-bearing steel slag, medium can be significantly improved
Basicity, improves the decomposability of silicate；The carbonate in sodium carbonate is combined with calcium simultaneously, and sodium carbonate/sodium hydroxide mixing is situated between
Verify and have great importance in raising slag vanadium conversion ratio, reduction sodium salt usage amount, reduction production cost.
According to the present invention, the concentration of sodium carbonate is 10-20wt% in step (1) described mixed solution, for example, can be
10wt%, 11wt%, 12wt%, 13wt%, 14wt%, 15wt%, 16wt%, 17wt%, 18wt%, 19wt% or
Specific point value between 20wt%, and above-mentioned numerical value, as space is limited and for concise consideration, the present invention no longer limit is arranged
Lift.
According to the present invention, the concentration of sodium hydroxide is 5-20wt% in step (1) described mixed solution, for example, can be
5wt%, 8wt%, 10wt%, 12wt%, 15wt%, 18wt%, 20wt%, 23wt%, 25wt%, 27wt% or 30wt%,
And the specific point value between above-mentioned numerical value, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the liquid-solid ratio of step (1) mixed solution and v-bearing steel slag is (3-8):1, for example can be
3:1、3.5:1、4:1、4.5:1、5:1、5.5:1、6:1、6.5:1、7:1、7.5:1 or 8:It is specific between 1, and above-mentioned numerical value
Point value, as space is limited and for concise consideration, the present invention no longer exclusive list.
The unit of liquid-solid ratio of the present invention is ml/g.
According to the present invention, the pressure of step (1) described Leach reaction is 0.3-1.5MPa, for example can be 0.3MPa,
0.4MPa、0.5MPa、0.6MPa、0.7MPa、0.8MPa、0.9MPa、1.0MPa、1.1MPa、1.2MPa、1.3MPa、1.4MPa
Or the specific point value between 1.5MPa, and above-mentioned numerical value, as space is limited and for concise consideration, the present invention no longer limit is arranged
Lift.
According to the present invention, the temperature of step (1) described Leach reaction is 120-200 DEG C, for example, can be 120 DEG C, 130
DEG C, 140 DEG C, 150 DEG C, 160 DEG C, 170 DEG C, 180 DEG C, 190 DEG C or the specific point value between 200 DEG C, and above-mentioned numerical value, be limited to
Length and the consideration for simplicity, the present invention no longer exclusive list.
According to the present invention, the time of step (1) described Leach reaction is 0.5-3h, for example can be 0.5h, 0.8h, 1h,
Specific point value between 1.2h, 1.5h, 1.8h, 2h, 2.3h, 2.5h, 2.7h or 3h, and above-mentioned numerical value, as space is limited and goes out
In concise consideration, the present invention no longer exclusive list.
According to the present invention, the temperature of step (2) described separation of solid and liquid is 60-100 DEG C, for example can be 60 DEG C, 65 DEG C, 70
DEG C, 75 DEG C, 80 DEG C, 85 DEG C, 90 DEG C, 95 DEG C or the specific point value between 100 DEG C, and above-mentioned numerical value, as space is limited and for
Concise consideration, the present invention no longer exclusive list.
Separation of solid and liquid of the present invention from means well known in the art carry out, for example can be filtering, suction filtration and from
The means such as the heart, but non-it is only limitted to this.
According to the present invention, to obtaining carrying out precipitation operation containing vanadium leachate in step (2), obtain vanadium product and contain carbon
Liquid after the precipitation of sour sodium and sodium hydroxide, liquid after gained precipitation is back in step (1) and circulated for being carried out to v-bearing steel slag
Leach.
It is optionally possible to which containing in vanadium leachate for being obtained into step (2) is added after sodium carbonate and sodium hydroxide, returned
It is back in step (1) and circulates for being leached to v-bearing steel slag.When the concentration of V in containing vanadium leachate is more than or equal to 20g/L,
Stop circular treatment, directly to carrying out follow-up precipitation operation containing vanadium leachate, obtain vanadium product.The method, which is conducive to improving, to be leached
V concentration in liquid, the consumption of water is greatlyd save in follow-up precipitation.
As preferred technical scheme, the method for v-bearing steel slag pressurization reinforcing vanadium extraction of the present invention comprises the following steps：
(1) (3-8) is pressed:1 liquid-solid ratio mixes the mixed solution of sodium carbonate and sodium hydroxide with v-bearing steel slag, in 0.3-
Under 1.5MPa pressure, Leach reaction 0.5-3h is carried out at a temperature of 120-200 DEG C, mixed slurry is obtained after the completion of reaction；
(2) mixed slurry for obtaining step (1) separation of solid and liquid at 60-100 DEG C, obtains tailings and containing vanadium leachate；
Containing for obtaining carries out precipitation operation in vanadium leachate, obtain liquid after vanadium product and precipitation containing sodium carbonate and sodium hydroxide,
Liquid after gained precipitation is back in step (1) and circulated for being leached to v-bearing steel slag.
Compared with prior art, the present invention at least has the advantages that：
(1) present invention can realize the efficient vanadium extracting from v-bearing steel slag, and leaching rate >=85% of vanadium reaches as high as 97%.
(2) method that the present invention is leached using direct weighting extracts the vanadium in vanadium raw materials, compared with being calcined the method for vanadium extraction,
Roasting process energy consumption can be not only saved, and is produced without the harmful kiln gas of roasting.
(3) it is circularly used for leaching slag after the obtained vanadium extraction containing vanadium leachate of the present invention, whole process non-wastewater discharge,
It is a kind of extraction vanadium method of cleaning.
Brief description of the drawings
Fig. 1 is the process chart that a kind of embodiment of the invention is provided.
Embodiment
Further illustrate technical scheme below in conjunction with the accompanying drawings and by embodiment.
As shown in figure 1, a kind of technological process of embodiment of the invention can be：By sodium carbonate and sodium hydroxide
Mixed liquor is mixed with v-bearing steel slag, and Leach reaction is carried out under pressure；Obtained mixed slurry progress solid-liquid will be reacted
Separation, obtains tailings and containing vanadium leachate；It will obtain carrying out Crystallization Separation containing vanadium leachate, obtain sodium vanadate product and knot
Liquid after crystalline substance, liquid is circularly used for the leaching of v-bearing steel slag after gained crystallization.
For the present invention is better described, technical scheme is readily appreciated, of the invention is typical but non-limiting
Embodiment is as follows：
Embodiment 1
Sodium hydroxide and sodium carbonate mixture are added in pressure reaction still with v-bearing steel slag, sodium carbonate in mixed solution
Solution concentration is 10%, and naoh concentration is 20%, and the liquid-solid ratio of solution and v-bearing steel slag is 8:1.Compressive reaction kettle is close
Envelope, then heating pressurization carries out Leach reaction, and Leach reaction temperature is 120 DEG C, Leach reaction pressure 0.6MPa, reaction time
0.5h.Reaction cools reactor after terminating, and opens reactor when being cooled to 60 DEG C, mixed slurry is separated by filtration and obtained
Containing vanadium leachate；It will contain and sodium vanadate product is obtained after vanadium leachate Crystallization Separation, liquid is circulated for slag leaching after obtained crystallization
Go out.
By detection, the leaching rate of vanadium in vanadium containing steel slag is 85%.
Embodiment 2
Sodium hydroxide and sodium carbonate mixture are added in pressure reaction still with v-bearing steel slag, sodium carbonate in mixed solution
Solution concentration is 12%, and naoh concentration is 16%, and the liquid-solid ratio of solution and v-bearing steel slag is 7:1.Compressive reaction kettle is close
Envelope, then heating pressurization carries out Leach reaction, and Leach reaction temperature is 140 DEG C, Leach reaction pressure 0.5MPa, reaction time
1.5h.Reaction cools reactor after terminating, and opens reactor when being cooled to 75 DEG C, mixed slurry is separated by filtration and obtained
Containing vanadium leachate；It will contain and sodium vanadate product is obtained after vanadium leachate Crystallization Separation, liquid is circulated for slag leaching after obtained crystallization
Go out.
By detection, the leaching rate of vanadium in vanadium containing steel slag is 91%.
V-bearing steel slag and sodium hydroxide/sodium carbonate mixed solution are added in pressure reaction still, sodium carbonate liquor concentration is
12%, naoh concentration is 16%, and the liquid-solid ratio of solution and vanadium slag is 7:1.Compressive reaction kettle is sealed, then heated anti-
Should, Leach reaction temperature is 140 DEG C, Leach reaction pressure 0.5MPa, reaction time 1.5h.Reaction is cooled down after terminating to reactor
Cooling, opens reactor when being cooled to 75 DEG C, mixed slurry is separated by filtration and obtains leachate, is followed after leachate separation sodium vanadate
Ring is leached for slag.The leaching rate of slag is 91%.
Embodiment 3
Sodium hydroxide and sodium carbonate mixture are added in pressure reaction still with v-bearing steel slag, sodium carbonate in mixed solution
Solution concentration is 18%, and naoh concentration is 18%, and the liquid-solid ratio of solution and v-bearing steel slag is 6:1.Compressive reaction kettle is close
Envelope, then heating pressurization carries out Leach reaction, and Leach reaction temperature is 120 DEG C, Leach reaction pressure 0.4MPa, reaction time
1.8h.Reaction cools reactor after terminating, and opens reactor when being cooled to 60 DEG C, mixed slurry is separated by filtration and obtained
Containing vanadium leachate；It will contain and sodium vanadate product is obtained after vanadium leachate Crystallization Separation, liquid is circulated for slag leaching after obtained crystallization
Go out.
By detection, the leaching rate of vanadium in vanadium containing steel slag is 95%.
Embodiment 4
Sodium hydroxide and sodium carbonate mixture are added in pressure reaction still with v-bearing steel slag, sodium carbonate in mixed solution
Solution concentration is 20%, and naoh concentration is 15%, and the liquid-solid ratio of solution and v-bearing steel slag is 5:1.Compressive reaction kettle is close
Envelope, then heating pressurization carries out Leach reaction, and Leach reaction temperature is 200 DEG C, Leach reaction pressure 1.5MPa, reaction time
2h.Reaction cools reactor after terminating, and opens reactor when being cooled to 95 DEG C, mixed slurry is separated by filtration and contained
Vanadium leachate；It will contain and sodium vanadate product is obtained after vanadium leachate Crystallization Separation, liquid is circulated after obtained crystallization leaches for slag.
By detection, the leaching rate of vanadium in vanadium containing steel slag is 96%.
Embodiment 5
Sodium hydroxide and sodium carbonate mixture are added in pressure reaction still with v-bearing steel slag, sodium carbonate in mixed solution
Solution concentration is 18%, and naoh concentration is 15%, and the liquid-solid ratio of solution and v-bearing steel slag is 8:1.Compressive reaction kettle is close
Envelope, then heating pressurization carries out Leach reaction, and Leach reaction temperature is 190 DEG C, Leach reaction pressure 1.2MPa, reaction time
2.7h.Reaction cools reactor after terminating, and opens reactor when being cooled to 75 DEG C, mixed slurry is separated by filtration and obtained
Containing vanadium leachate；It will contain and sodium vanadate product is obtained after vanadium leachate Crystallization Separation, liquid is circulated for slag leaching after obtained crystallization
Go out.
By detection, the leaching rate of vanadium in vanadium containing steel slag is 94%.
Embodiment 6
Sodium hydroxide and sodium carbonate mixture are added in pressure reaction still with v-bearing steel slag, sodium carbonate in mixed solution
Solution concentration is 20%, and naoh concentration is 10%, and the liquid-solid ratio of solution and v-bearing steel slag is 3:1.Compressive reaction kettle is close
Envelope, then heating pressurization carries out Leach reaction, and Leach reaction temperature is 130 DEG C, Leach reaction pressure 0.3MPa, reaction time
3h.Reaction cools reactor after terminating, and opens reactor when being cooled to 100 DEG C, mixed slurry is separated by filtration and obtained
Containing vanadium leachate；It will contain and sodium vanadate product is obtained after vanadium leachate Crystallization Separation, liquid is circulated for slag leaching after obtained crystallization
Go out.
By detection, the leaching rate of vanadium in vanadium containing steel slag is 95%.
Embodiment 7
Sodium hydroxide and sodium carbonate mixture are added in pressure reaction still with v-bearing steel slag, sodium carbonate in mixed solution
Solution concentration is 16%, and naoh concentration is 9%, and the liquid-solid ratio of solution and v-bearing steel slag is 8:1.Compressive reaction kettle is close
Envelope, then heating pressurization carries out Leach reaction, and Leach reaction temperature is 150 DEG C, Leach reaction pressure 0.6MPa, reaction time
1h.Reaction cools reactor after terminating, and opens reactor when being cooled to 80 DEG C, mixed slurry is separated by filtration and contained
Vanadium leachate；It will contain and sodium vanadate product is obtained after vanadium leachate Crystallization Separation, liquid is circulated after obtained crystallization leaches for slag.
By detection, the leaching rate of vanadium in vanadium containing steel slag is 88%.
Embodiment 8
Sodium hydroxide and sodium carbonate mixture are added in pressure reaction still with v-bearing steel slag, sodium carbonate in mixed solution
Solution concentration is 15%, and naoh concentration is 10%, and the liquid-solid ratio of solution and v-bearing steel slag is 6:1.Compressive reaction kettle is close
Envelope, then heating pressurization carries out Leach reaction, and Leach reaction temperature is 195 DEG C, Leach reaction pressure 1.4MPa, reaction time
3h.Reaction cools reactor after terminating, and opens reactor when being cooled to 80 DEG C, mixed slurry is separated by filtration and contained
Vanadium leachate；It will contain and sodium vanadate product is obtained after vanadium leachate Crystallization Separation, liquid is circulated after obtained crystallization leaches for slag.
By detection, the leaching rate of vanadium in vanadium containing steel slag is 96%.
Embodiment 9
It will obtain adding in pressure reaction still with v-bearing steel slag containing vanadium leachate in embodiment 8, while adding a certain amount of
Sodium carbonate and sodium hydroxide, its concentration of sodium carbonate is reached 14%, naoh concentration is 15%, solution and v-bearing steel slag
Liquid-solid ratio is 4:1.Compressive reaction kettle is sealed, then heating pressurization carries out Leach reaction, and Leach reaction temperature is 170 DEG C, leaching
Go out reaction pressure 0.8MPa, reaction time 2.4h.Reaction cools reactor after terminating, and reaction is opened when being cooled to 80 DEG C
Kettle, mixed slurry is separated by filtration and obtains containing vanadium leachate；It will contain and sodium vanadate product is obtained after vanadium leachate Crystallization Separation, obtain
Crystallization after liquid circulate for slag leach.
By detection, the leaching rate of vanadium in vanadium containing steel slag is 97%.
Comparative example 1
Sodium carbonate liquor and v-bearing steel slag are added in pressure reaction still, sodium carbonate liquor concentration is 15%, and solution is with containing
The liquid-solid ratio of vanadium steel slag is 6:1.Compressive reaction kettle is sealed, then heating pressurization carries out Leach reaction, and Leach reaction temperature is
195 DEG C, Leach reaction pressure 1.4MPa, reaction time 3h.Reaction cools reactor after terminating, and is beaten when being cooled to 80 DEG C
Reactor is driven, mixed slurry is separated by filtration and obtains containing vanadium leachate；It will contain and sodium vanadate production is obtained after vanadium leachate Crystallization Separation
Product, liquid is circulated after obtained crystallization leaches for slag.
By detection, the leaching rate of vanadium in vanadium containing steel slag is only 56%.This comparative example in addition to sodium hydroxide is not added, other
Condition is identical with embodiment 8, but conversion ratio is significantly lower than embodiment 8, it is seen then that the addition of sodium hydroxide is for reinforcing slag
Decompose, the conversion ratio for improving vanadium is most important.
Comparative example 2
Sodium carbonate liquor and v-bearing steel slag are added in pressure reaction still, sodium carbonate liquor concentration is 25%, and solution is with containing
The liquid-solid ratio of vanadium steel slag is 6:1.Compressive reaction kettle is sealed, then heating pressurization carries out Leach reaction, and Leach reaction temperature is
195 DEG C, Leach reaction pressure 1.4MPa, reaction time 3h.Reaction cools reactor after terminating, and is beaten when being cooled to 80 DEG C
Reactor is driven, mixed slurry is separated by filtration and obtains containing vanadium leachate；It will contain and sodium vanadate production is obtained after vanadium leachate Crystallization Separation
Product, liquid is circulated after obtained crystallization leaches for slag.
By detection, the leaching rate of vanadium in vanadium containing steel slag is only 77%.Although this comparative example is carried on the basis of comparative example 1
The high concentration of sodium carbonate, but due to the addition without sodium hydroxide, vanadium conversion ratio still is below embodiment 8, it is seen then that hydroxide
The addition of sodium is decomposed for reinforcing slag, and the conversion ratio for improving vanadium is most important.
Comparative example 3
Sodium hydroxide solution and v-bearing steel slag are added in pressure reaction still, concentration of sodium hydroxide solution is 10%, solution
Liquid-solid ratio with v-bearing steel slag is 6:1.Compressive reaction kettle is sealed, then heating pressurization carries out Leach reaction, Leach reaction temperature
Spend for 195 DEG C, Leach reaction pressure 1.4MPa, reaction time 3h.Reaction cools reactor after terminating, and is cooled to 80 DEG C
When open reactor, mixed slurry is separated by filtration obtain contain vanadium leachate；Vanadic acid will be obtained after vanadium leachate Crystallization Separation will be contained
Sodium product, liquid is circulated after obtained crystallization leaches for slag.
By detection, the leaching rate of vanadium in vanadium containing steel slag is only 40%.This comparative example is leached anti-in addition to sodium carbonate is not added
Answer condition same as Example 8, vanadium conversion ratio is significantly lower than embodiment 8, it is seen then that single sodium hydroxide solution can not effectively soak
Go out v-bearing steel slag, sodium carbonate is the leaching agent that v-bearing steel slag can not or lack.
Comparative example 4
Sodium hydroxide solution and v-bearing steel slag are added in pressure reaction still, concentration of sodium hydroxide solution is 25%, solution
Liquid-solid ratio with v-bearing steel slag is 6:1.Compressive reaction kettle is sealed, then heating pressurization carries out Leach reaction, Leach reaction temperature
Spend for 195 DEG C, Leach reaction pressure 1.4MPa, reaction time 3h.Reaction cools reactor after terminating, and is cooled to 80 DEG C
When open reactor, mixed slurry is separated by filtration obtain contain vanadium leachate；Vanadic acid will be obtained after vanadium leachate Crystallization Separation will be contained
Sodium product, liquid is circulated after obtained crystallization leaches for slag.
By detection, the leaching rate of vanadium in vanadium containing steel slag is only 60%.Although this comparative example is carried on the basis of comparative example 3
The high concentration of sodium hydroxide solution, but due to the addition without sodium carbonate, vanadium conversion ratio is significantly lower than embodiment 8, it is seen then that single
Only sodium hydroxide solution can not effectively leach v-bearing steel slag, and sodium carbonate is the leaching agent that v-bearing steel slag can not or lack.
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (10)
1. a kind of method of v-bearing steel slag pressurization reinforcing vanadium extraction, it is characterised in that the described method comprises the following steps：
(1) mixed solution of sodium carbonate and sodium hydroxide is mixed with v-bearing steel slag, leached under conditions of heating pressurization
Reaction, mixed slurry is obtained after the completion of reaction；
(2) the mixed slurry separation of solid and liquid for obtaining step (1), obtains tailings and containing vanadium leachate.
2. the method as described in claim 1, it is characterised in that the concentration of sodium carbonate is 10- in step (1) described mixed solution
20wt%.
3. method as claimed in claim 1 or 2, it is characterised in that the concentration of sodium hydroxide in step (1) described mixed solution
For 5-20wt%.
4. the method as described in claim any one of 1-3, it is characterised in that step (1) mixed solution and v-bearing steel slag
Liquid-solid ratio be (3-8):1.
5. the method as described in claim any one of 1-4, it is characterised in that the pressure of step (1) described Leach reaction is
0.3-1.5MPa。
6. the method as described in claim any one of 1-5, it is characterised in that the temperature of step (1) described Leach reaction is
120-200℃。
7. the method as described in claim any one of 1-6, it is characterised in that the time of step (1) described Leach reaction is
0.5-3h。
8. the method as described in claim any one of 1-7, it is characterised in that the temperature of step (2) described separation of solid and liquid is 60-
100℃。
9. the method as described in claim any one of 1-8, it is characterised in that enter to what is obtained in step (2) containing vanadium leachate
Row precipitation is operated, and obtains liquid after vanadium product and precipitation containing sodium carbonate and sodium hydroxide, liquid after gained precipitation is back into step
Suddenly circulated in (1) for being leached to v-bearing steel slag.
10. the method as described in claim any one of 1-9, it is characterised in that the described method comprises the following steps：
(1) (3-8) is pressed:1 liquid-solid ratio mixes the mixed solution of sodium carbonate and sodium hydroxide with v-bearing steel slag, in 0.3-
Under 1.5MPa pressure, Leach reaction 0.5-3h is carried out at a temperature of 120-200 DEG C, mixed slurry is obtained after the completion of reaction；
(2) mixed slurry for obtaining step (1) separation of solid and liquid at 60-100 DEG C, obtains tailings and containing vanadium leachate；Will
To contain precipitation operation carried out in vanadium leachate, liquid after vanadium product and precipitation containing sodium carbonate and sodium hydroxide is obtained, by institute
Obtaining liquid after precipitation and being back in step (1) to circulate is used to leach v-bearing steel slag.
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| CN107892317A (en) * | 2017-11-14 | 2018-04-10 | 河钢股份有限公司承德分公司 | A kind of vanadium reclaimed in calcification precipitation tailings and the method for preparing nano-calcium carbonate |
| CN108996547A (en) * | 2018-08-31 | 2018-12-14 | 攀钢集团攀枝花钢铁研究院有限公司 | The method of titanium tetrachloride purification tailings ultrasonic wave added alkaline-leaching and vanadium extraction |
| CN111575490A (en) * | 2020-06-17 | 2020-08-25 | 中国科学院过程工程研究所 | Method for extracting vanadium and chromium from chromium mud |
| CN114318013A (en) * | 2021-12-28 | 2022-04-12 | 中国科学院过程工程研究所 | Method and system device for powder spraying and feeding of vanadium slag pressure leaching reaction kettle |
| CN114318014A (en) * | 2021-12-28 | 2022-04-12 | 中国科学院过程工程研究所 | Method for double-flow feeding of vanadium slag pressure leaching reaction kettle |
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| CN107892317A (en) * | 2017-11-14 | 2018-04-10 | 河钢股份有限公司承德分公司 | A kind of vanadium reclaimed in calcification precipitation tailings and the method for preparing nano-calcium carbonate |
| CN107892317B (en) * | 2017-11-14 | 2020-02-04 | 河钢股份有限公司承德分公司 | Method for recovering vanadium in calcified vanadium precipitation tailings and preparing nano calcium carbonate |
| CN108996547A (en) * | 2018-08-31 | 2018-12-14 | 攀钢集团攀枝花钢铁研究院有限公司 | The method of titanium tetrachloride purification tailings ultrasonic wave added alkaline-leaching and vanadium extraction |
| CN111575490A (en) * | 2020-06-17 | 2020-08-25 | 中国科学院过程工程研究所 | Method for extracting vanadium and chromium from chromium mud |
| CN114318013A (en) * | 2021-12-28 | 2022-04-12 | 中国科学院过程工程研究所 | Method and system device for powder spraying and feeding of vanadium slag pressure leaching reaction kettle |
| CN114318014A (en) * | 2021-12-28 | 2022-04-12 | 中国科学院过程工程研究所 | Method for double-flow feeding of vanadium slag pressure leaching reaction kettle |
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