CN110343880A - A method of utilizing v-bearing steel slag reduction melting vanadium alloy - Google Patents
A method of utilizing v-bearing steel slag reduction melting vanadium alloy Download PDFInfo
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- CN110343880A CN110343880A CN201910769740.4A CN201910769740A CN110343880A CN 110343880 A CN110343880 A CN 110343880A CN 201910769740 A CN201910769740 A CN 201910769740A CN 110343880 A CN110343880 A CN 110343880A
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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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
- C22C27/025—Alloys based on vanadium, niobium, or tantalum alloys based on vanadium
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Abstract
The present invention provides a kind of method using v-bearing steel slag reduction melting vanadium alloy, which comprises mixes v-bearing steel slag and reducing agent, and binder is added and is prepared into pelletizing；The pelletizing is heated into reduction under vacuum conditions, obtains reduzate；After reduzate is melted, cooling obtains vanadium alloy product under protective atmosphere.The method can restore barium oxide most in v-bearing steel slag and ferriferous oxide, both take full advantage of waste resource, save Solid state fermentation cost, in turn avoid problem of environmental pollution caused by waste residue is stacked, economic benefit and environmental benefit are significant.
Description
Technical field
The invention belongs to vanadium field of metallurgy, in particular to a kind of method of v-bearing steel slag reduction melting vanadium alloy.
Background technique
V-bearing steel slag is the byproduct for smelting vanadium titano-magnetite, and generating process, there are two types of approach, and one is residual in half steel
The vanadium deposited enters v-bearing steel slag obtained in slag through oxidation after steel-making, and another way is that the molten iron without the vanadium slag that blows is straight
Nearly million tons of v-bearing steel slag that China v-bearing steel slag that steel-making obtains is discharged every year are connect, this not only causes environmental pollution, but also right
Vanadium resource is also a kind of greatly waste.
Currently, there are mainly two types of approach for v-bearing steel slag vanadium extraction.First is that v-bearing steel slag returns to ironmaking Vanadium Concentrationin, high vanadium is produced
Slag, further the processing method of vanadium extraction another kind v-bearing steel slag is direct vanadium extracting method, and the method for direct vanadium extraction has sodium roasting
The techniques such as burning, calcification baking, the roasting of drop calcium and direct acidleach.It is low, at high cost that such generally existing vanadium of technique turns leaching rate, and is difficult to
The problem of large-scale production, fails the recycling for really solving the problems, such as vanadium in steel slag.
1320142 C of CN discloses a kind of enrichment method of vanadium in vanadium containing steel slag, and the patent in v-bearing steel slag by adding
Enter additive, under the conditions of logical oxygen, melt processed, it is then cooling, keep the temperature after v-bearing steel slag is taken out and quenching in air, from
And make the vanadium of Dispersed precipitate in v-bearing steel slag be transferred to be enriched with and crystallize in the cenotype rich in vanadium precipitation obtain rich vanadium phase grade
Rich vanadium phase is conducive to vanadium from the separation and Extraction in steel slag.But the patent is only by the V in vanadium slag2O5Enrichment obtains rich vanadium slag.
103484590 A of CN discloses a kind of method of rich vanadium pig iron of v-bearing steel slag smelting, by 63~67 parts of V-alloyed steels
Slag, 14~18 parts of iron powders, 8~12 parts of silicas, 4~6 parts of carbon dusts and 3~4 parts of aluminum shots are added in smelting furnace, by resulting mixture
Heating melts and to separate clinker and molten iron after reaction, is the rich vanadium pig iron after molten iron is cooling, wherein the v-bearing steel slag
For vanadium-bearing hot metal slag remaining after converter smelting.
Summary of the invention
To solve the technical problems existing in the prior art, the present invention provides a kind of utilization v-bearing steel slag reduction melting vanadium conjunction
Barium oxide most in v-bearing steel slag and ferriferous oxide can be restored, both be taken full advantage of by the method for gold, the method
Waste resource saves Solid state fermentation cost, in turn avoids problem of environmental pollution, economic benefit and environmental protection caused by waste residue is stacked
Remarkable benefit.
In order to achieve the above object, the invention adopts the following technical scheme:
The present invention a kind of method using v-bearing steel slag reduction melting vanadium alloy is provided the described method includes:
V-bearing steel slag and reducing agent are mixed, and binder is added and is prepared into pelletizing；Under vacuum conditions by the pelletizing
Heating reduction, obtains reduzate；After reduzate is melted, cooling obtains vanadium alloy product under protective atmosphere.
As currently preferred technical solution, the v-bearing steel slag is the generation of aluminiferous molten iron-steelmaking.
As currently preferred technical solution, the mass fraction of TFe is 15~25%, V in the v-bearing steel slag2O5's
Mass fraction is 1~4%.Wherein, the mass fraction of TFe can be 16%, 17%, 18%, 19%, 20%, 21%, 22%,
23% or 24% etc., V2O5Mass fraction can be 1.5%, 2%, 2.5%, 3% or 3.5% etc., it is not limited to listed
The numerical value of act, other interior unlisted numerical value of above-mentioned each numberical range are equally applicable.
As currently preferred technical solution, the reducing agent is carbonaceous reducing agent.
As currently preferred technical solution, the carbonaceous reducing agent includes semi-coke, graphite, carbon black, active carbon, coke
In organic carbon any one or at least two combination, the combination is typical but non-limiting example has: semi-coke and graphite
Combination, the combination of graphite and carbon black, the combination of carbon black and active carbon, the combination of active carbon and coke, coke and organic carbon
Combination, the combination or graphite of organic carbon and semi-coke, the combination of carbon black and active carbon etc..
As currently preferred technical solution, the mass ratio of the v-bearing steel slag and reducing agent is 1:0.15~0.40,
Such as 1:0.20,1:0.25,1:0.30 or 1:0.35, it is not limited to cited numerical value, in the numberical range, other are not
The numerical value enumerated is equally applicable.
In the present invention, due to removing ferro element and vanadium in v-bearing steel slag, there is also other elements, and are not at its highest
Valence state, thus when the mass ratio of the v-bearing steel slag and reducing agent be greater than 1:0.15 when at this time reducing agent can with other oxidisability compared with
Strong element reacts, and the rate that is reduced of vanadium is caused sharply to decline, the vanadium in v-bearing steel slag cannot be completely reduced for+
Trivalent state；It is some weak while vanadium is reduced when the mass ratio of the v-bearing steel slag and reducing agent is less than 1:0.40
The compound of oxidisability can be reduced, and the content of vanadium in finally obtained vanadium alloy is caused to decline.
As currently preferred technical solution, the binder includes polyethanol and/or amylan.
Preferably, the mass ratio of the v-bearing steel slag and binder is 1:0.02~0.05, such as 1:0.02,1:0.025,1:
0.03,1:0.035,1:0.04,1:0.045 or 1:0.05 etc., it is not limited to cited numerical value, in the numberical range its
His unlisted numerical value is equally applicable.
As currently preferred technical solution, the temperature of the heating reduction reaction is 1250~1600 DEG C, such as 1300
DEG C, 1350 DEG C, 1400 DEG C, 1450 DEG C, 1500 DEG C or 1550 DEG C etc., it is not limited to cited numerical value, the numberical range
Other interior unlisted numerical value are equally applicable.
In the present invention, due to removing ferro element and vanadium in v-bearing steel slag, there is also other elements, when the reduction temperature
It has when less than 1250 DEG C or a large amount of side reactions when former temperature is greater than 1600 DEG C to generate, although as long as the addition of reducing agent at this time
The enough reduction rates for ensuring that vanadium greatly of amount, but will cause the content decline for finally obtaining vanadium in vanadium alloy.
Preferably, it is described heating reduction reaction time be 55~75min, as 55min, 56min, 58min, 60min,
62min, 65min, 68min, 70min, 72min or 75min etc., it is not limited to cited numerical value, in the numberical range
Other unlisted numerical value are equally applicable.
Preferably, pressure is no more than 26700Pa in the heating reaction process.
It is described to be cooled to 135~155 DEG C as currently preferred technical solution, such as 136 DEG C, 138 DEG C, 140 DEG C, 142
DEG C, 145 DEG C, 148 DEG C, 150 DEG C or 152 DEG C etc., it is not limited to cited numerical value, other are unlisted in the numberical range
Numerical value it is equally applicable.
Preferably, the protective atmosphere includes argon gas and/or helium.
As currently preferred technical solution, the above-mentioned method using v-bearing steel slag reduction melting vanadium alloy includes:
V-bearing steel slag and reducing agent are mixed according to mass ratio 1:0.15~0.40, and binder is added and is prepared into pelletizing；
By the pelletizing 1250~1600 DEG C of heating reduction under vacuum conditions, reduzate is obtained；After reduzate is melted, protecting
135~155 DEG C, which are cooled to, under shield atmosphere obtains vanadium alloy product.
Compared with prior art, the present invention at least has the advantages that
The present invention provides a kind of method using v-bearing steel slag reduction melting vanadium alloy, and the method can will be in v-bearing steel slag
Most barium oxide and ferriferous oxide reduction, both take full advantage of waste resource, save Solid state fermentation cost, and keep away
Problem of environmental pollution caused by waste residue is stacked is exempted from, economic benefit and environmental benefit are significant.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is only to aid in the understanding present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
The present embodiment provides a kind of methods of v-bearing steel slag reduction melting vanadium alloy, which comprises
By 1000kg v-bearing steel slag, (TFe content is 18%, V2O5Content is 2%) to be put into 150kg semi-coke, 50kg ethyl alcohol
Vacuum drying oven is evacuated to pressure in 23Pa by pressure ball after batch mixer mixes, and vacuum drying oven is added after dry screening in pelletizing, and temperature exists
Reduction reaction is carried out at 1550 DEG C, furnace pressure is no more than 26700Pa and melts product after reaction 5 hours in reaction process,
It is then injected into ingot mould, under helium protection, is come out of the stove when being cooled to 150 DEG C, obtains vanadium alloy through broken.
In the above-mentioned vanadium alloy being prepared, the content of vanadium is 2.6%；Take the iron slag sample analysis after smelting, V2O5Content is
0.48%, TFe content are 0.86%, and such smelting process is by V most in v-bearing steel slag2O5It is restored with FeO, to obtain
The rich vanadium pig iron.
Embodiment 2
The present embodiment provides a kind of methods of v-bearing steel slag reduction melting vanadium alloy, which comprises
By 1000kg v-bearing steel slag, (TFe content is 22%, V in production process2O5Content be 3.5%) with 160kg graphite,
35kg starch is put into pressure ball after batch mixer mixes, and vacuum drying oven is evacuated to pressure in 23Pa, pelletizing is added after dry screening
Vacuum drying oven, temperature carry out reduction reaction at 1450 DEG C, and furnace pressure is no more than 26700Pa in reaction process, react 5 hours
Afterwards, product is melted, is then injected into ingot mould, under helium protection, come out of the stove when being cooled to 140 DEG C, obtain vanadium alloy through broken.
In the above-mentioned vanadium alloy being prepared, the content of vanadium is 4%；Take the iron slag sample analysis after smelting, V2O5Content is
0.39%, TFe content are 0.91%, and such smelting process is by V most in v-bearing steel slag2O5It is restored with FeO, to obtain
The rich vanadium pig iron.
Embodiment 3
The present embodiment provides a kind of methods of v-bearing steel slag reduction melting vanadium alloy, which comprises
By 1000kg v-bearing steel slag, (TFe content is 15%, V in production process2O5Content be 1%) with 400kg carbon black,
45kg ethyl alcohol is put into pressure ball after batch mixer mixes, and vacuum drying oven is evacuated to pressure in 23Pa, pelletizing is added after dry screening
Vacuum drying oven, temperature carry out reduction reaction at 1600 DEG C, and furnace pressure is no more than 26700Pa in reaction process, react 5 hours
Afterwards, product is melted, is then injected into ingot mould, under helium protection, come out of the stove when being cooled to 155 DEG C, obtain vanadium alloy through broken.
In the above-mentioned vanadium alloy being prepared, the content of vanadium is 3.8%；Take the iron slag sample analysis after smelting, V2O5Content
0.41%, TFe content are 0.92%, and such smelting process is by V most in v-bearing steel slag2O5It is restored with FeO, to obtain
The rich vanadium pig iron.
Embodiment 4
The present embodiment provides a kind of methods of v-bearing steel slag reduction melting vanadium alloy, which comprises
By 1000kg v-bearing steel slag, (TFe content is 25%, V in production process2O5Content be 4%) with 400kg coke,
25kg starch is put into pressure ball after batch mixer mixes, and vacuum drying oven is evacuated to pressure in 23Pa, pelletizing is added after dry screening
Vacuum drying oven, temperature carry out reduction reaction at 1250 DEG C, and furnace pressure is no more than 26700Pa in reaction process, react 5 hours
Afterwards, product is melted, is then injected into ingot mould, under helium protection, come out of the stove when being cooled to 135 DEG C, obtain vanadium alloy through broken.
In the above-mentioned vanadium alloy being prepared, the content of vanadium is 3.5%；Take the iron slag sample analysis after smelting, V2O5Content is
0.425%, TFe content are 0.89%, and such smelting process is by V most in v-bearing steel slag2O5It is restored with FeO, to obtain
The rich vanadium pig iron.
Embodiment 5
The present embodiment provides a kind of methods of v-bearing steel slag reduction melting vanadium alloy, which comprises
By 1000kg v-bearing steel slag, (TFe content is 18%, V in production process2O5Content be 2%) with 200kg coke,
22kg ethyl alcohol is put into pressure ball after batch mixer mixes, and vacuum drying oven is evacuated to pressure in 23Pa, pelletizing is added after dry screening
Vacuum drying oven, temperature carry out reduction reaction at 1500 DEG C, and furnace pressure is no more than 26700Pa in reaction process, react 5 hours
Afterwards, product is melted, is then injected into ingot mould, under helium protection, come out of the stove when being cooled to 150 DEG C, obtain vanadium alloy through broken.
In the above-mentioned vanadium alloy being prepared, the content of vanadium is 3%；Take the iron slag sample analysis after smelting, V2O5Content is
0.44%, TFe content are 0.886%, and such smelting process is by V most in v-bearing steel slag2O5It is restored with FeO, to obtain
The rich vanadium pig iron.
Comparative example 1
This comparative example provides a kind of method of v-bearing steel slag reduction melting vanadium alloy, and the method is in addition to semi-coke additional amount
Outside 50kg, aluminiferous steel slag additional amount is outside 1070kg, and other conditions are same as Example 1.
In the above-mentioned vanadium alloy being prepared, the content of vanadium is 1.7%；Take the iron slag sample analysis after smelting, V2O5Content is
3.16%, TFe content are 1.33%.
Comparative example 2
This comparative example provides a kind of method of v-bearing steel slag reduction melting vanadium alloy, and the method is in addition to semi-coke additional amount
Outside 500kg, aluminiferous steel slag additional amount is outside 620kg, and other conditions are same as Example 1.
In the above-mentioned vanadium alloy being prepared, the content of vanadium is 2.1%；Take the iron slag sample analysis after smelting, V2O5Content is
0.51%, TFe content are 0.86%.
Comparative example 3
This comparative example provides a kind of method of v-bearing steel slag reduction melting vanadium alloy, temperature of the method in addition to reduction reaction
Degree is outer for 800 DEG C, and other conditions are same as Example 1.
In the above-mentioned vanadium alloy being prepared, the content of vanadium is 1.5%；Take the iron slag sample analysis after smelting, V2O5Content is
2.62%, TFe content are 1.13%.
Comparative example 4
This comparative example provides a kind of method of v-bearing steel slag reduction melting vanadium alloy, temperature of the method in addition to reduction reaction
Degree is outer for 1800 DEG C, and other conditions are same as Example 1.
In the above-mentioned vanadium alloy being prepared, the content of vanadium is 2.2%；Take the iron slag sample analysis after smelting, V2O5Content is
0.46%, TFe content are 0.81%.
It is can be seen that compared with comparative example 1-4 according to embodiment 1 when the quality of reducing agent and aluminiferous steel slag is relatively low
When, V compared with Example 1 in the scum after reduction reaction2O5Content it is higher, and finally obtain in vanadium alloy the content of vanadium with
Embodiment 1 is compared and is declined slightly；When the quality of reducing agent and aluminiferous steel slag is relatively high, V in the scum after reduction reaction2O5's
Content is basically unchanged compared with Example 1, and the content with embodiment 1 for finally obtaining vanadium in vanadium alloy decline it is more.Work as reduction
Reaction it is too high or too low for temperature when, will lead to finally obtain vanadium in vanadium alloy content with embodiment 1 generate be decreased obviously.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (10)
1. a kind of method using v-bearing steel slag reduction melting vanadium alloy, which is characterized in that the described method includes:
V-bearing steel slag and reducing agent are mixed, and binder is added and is prepared into pelletizing；The pelletizing is heated under vacuum conditions
Reduction, obtains reduzate；After reduzate fusing, cooling obtains vanadium alloy product under protective atmosphere.
2. the method according to claim 1, wherein the v-bearing steel slag is the generation of aluminiferous molten iron-steelmaking.
3. method according to claim 1 or 2, which is characterized in that in the v-bearing steel slag mass fraction of TFe be 15~
25%, V2O5Mass fraction be 1~4%.
4. method according to claim 1-3, which is characterized in that the reducing agent is carbonaceous reducing agent.
5. according to the method described in claim 4, it is characterized in that, the carbonaceous reducing agent includes semi-coke, graphite, carbon black, work
In property charcoal, coke or organic carbon any one or at least two combination.
6. method according to claim 1-5, which is characterized in that the mass ratio of the v-bearing steel slag and reducing agent
For 1:0.15~0.40.
7. method according to claim 1-6, which is characterized in that the binder includes polyethanol and/or shallow lake
Arogel；
Preferably, the mass ratio of the v-bearing steel slag and binder is 1:0.02~0.05.
8. method according to claim 1-7, which is characterized in that it is described heating reaction temperature be 1250~
1600℃；
Preferably, the time of the heating reaction is 55~75min；
Preferably, pressure is no more than 26700Pa in the heating reaction process.
9. method according to claim 1-8, which is characterized in that described to be cooled to 135~155 DEG C；
Preferably, the protective atmosphere includes argon gas and/or helium.
10. method according to claim 1-8, which is characterized in that the described method includes:
V-bearing steel slag and reducing agent are mixed according to mass ratio 1:0.15~0.40, and binder is added and is prepared into pelletizing；By institute
Pelletizing 1250~1600 DEG C of heating reduction under vacuum conditions are stated, reduzate is obtained；After reduzate is melted, in protection gas
It is cooled to 135~155 DEG C under atmosphere and obtains vanadium alloy product.
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| CN111621686A (en) * | 2020-05-21 | 2020-09-04 | 中冶东方工程技术有限公司 | Method for producing silicon vanadium nitride by smelting vanadium-rich slag |
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Application publication date: 20191018 |