CN109913661A - A method of from extraction sulphur and vanadium in desulfurization slag containing vanadium - Google Patents
A method of from extraction sulphur and vanadium in desulfurization slag containing vanadium Download PDFInfo
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- CN109913661A CN109913661A CN201910339909.2A CN201910339909A CN109913661A CN 109913661 A CN109913661 A CN 109913661A CN 201910339909 A CN201910339909 A CN 201910339909A CN 109913661 A CN109913661 A CN 109913661A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The method that the present invention relates to a kind of to extract sulphur and vanadium from desulfurization slag containing vanadium, the method are as follows: vanadium desulfurization slag will be contained and carry out blank roasting, obtain roasting clinker；Roasting clinker is mixed with water and is leached, tailings and leachate are obtained after separation of solid and liquid；Gained leachate crystallisation by cooling obtains sodium sulfate crystal after separation of solid and liquid and containing liquid after vanadium crystallization.The present invention, which realizes, utilizes the resource utilization of valuable element in desulfurization slag containing vanadium, wherein the rate of recovery of sulphur is greater than 93%, and the rate of recovery of vanadium is greater than 85%, and has obtained sodium sulphate product of the purity 94% or more.Method provided by the invention alleviates the adverse effect containing the desuifurized accumulation of vanadium for environment, good economic benefit is achieved simultaneously, and whole processing technology process is simple, production process does not have discharge of wastewater, economy and obvious environment benefit are suitable for industrialization promotion.
Description
Technical field
The invention belongs to vanadium metallurgy and solid waste recycling fields, and in particular to one kind is extracted from desulfurization slag containing vanadium
The method of sulphur and vanadium.
Background technique
Vanadium is a kind of accompanying element for being present in vanadium titano-magnetite, since its important physicochemical properties becomes one kind
Important strategic resource is widely used in the fields such as national defence, chemical industry, metallurgy.Smelting iron and steel industry changes steel by addition vanadium
Intensity, vanadium also increasing year by year in the dosage of steel industry.
Since China's low-grade vanadium titano-magnetite content is larger, in steel-making, petroleum refining, alumina producing, and power generation
In many industrial processes of power generation etc. of standing, a large amount of solid waste containing vanadium can be all generated.Desulfurization slag containing vanadium is a kind of refining
The solid waste containing vanadium generated in iron process production.Contain a small amount of vanadium (1-5%) in the desulfurization slag containing vanadium of Cheng Gang company production
And a large amount of sulphur (15-25%) and sodium (20-35%).On the one hand, these desulfurization slags containing vanadium are such as not added disposition and arbitrarily bank up
If, both occupied a large amount of land resource, and increased the management cost of enterprise, and can due to vanadium toxicity and brought to human and environment
Grievous injury；On the other hand, part valuable resource is contained in desulfurization slag containing vanadium, it should positive is recycled, change give up into
Treasured changes evil for benefit, to create considerable economic benefit and social benefit.Therefore, have to the recycling of the desulfurization slag containing vanadium
Very important meaning.
Currently, Some Enterprises realize the recycling to desulfurization slag.For example, by the desulfurization slag sphere of powder in CN101491780A
Magnetic separation is carried out after mill, efficiently separates iron in desulphurizing slag powder, slag, to improve the ferrous grade of desulphurizing slag powder.
By the processes such as compounding, milling, suppressing and drying with binder bentonite in CN102560082A, desulphurizing slag powder is prepared into balling-up
As electric furnace steel making raw material.CN102586537A carries out magnetic separation or refinement by the desulfurization slag obtained after desulfurization to vanadium-bearing hot metal
Magnetic separation obtains granulated iron afterwards, then it is compounded with steel-making iron scale and bonding agent, uses as vanadium-raising cooling agent.
But the above method only realizes the secondary use to desulfurization slag, for the valuable vanadium in desulfurization slag containing vanadium without
Method is effectively recycled, and the significant wastage to valuable resource is caused.And traditional wet processing processing (acidleach, alkali leaching) although
It can be realized effective extraction to vanadium, but extraction process generates a large amount of waste water again needs secondary treatment, energy consumption is also high, economical
Benefit is also undesirable.Therefore, for recycling valuable resource, the raising performance of enterprises and environmental protection the purpose of, need exploitation one
Kind can in resource utilization desulfurization slag containing vanadium valuable element method.
Summary of the invention
In order to solve the above technical problems, the method that the present invention provides a kind of to extract sulphur and vanadium from desulfurization slag containing vanadium, real
Show the resource utilization utilization to valuable element in desulfurization slag containing vanadium (sulphur and vanadium), achieves good economic benefit and society
Benefit is suitable for industrialization promotion.
In order to achieve the above objectives, the invention adopts the following technical scheme:
The method that the present invention provides a kind of to extract sulphur and vanadium from desulfurization slag containing vanadium, the described method comprises the following steps:
(1) vanadium desulfurization slag will be contained and carry out blank roasting, obtain roasting clinker；
(2) the roasting clinker that step (1) obtains is mixed with water and is leached, tailings and leaching are obtained after separation of solid and liquid
Liquid；
(3) by leachate crystallisation by cooling obtained by step (2), liquid after sodium sulfate crystal and crystallization is obtained after separation of solid and liquid.
According to the present invention, based on mass percentage, contain in desulfurization slag containing vanadium described in step (1): S15-25%,
Na20-35%, V1-5%.
According to the present invention, desulfurization slag containing vanadium described in step (1) is crushed and is ground before roasting, is typically chosen and is ground
150 mesh are milled to hereinafter, being more advantageous to subsequent recovery.
According to the present invention, the temperature of step (1) described roasting is 600-900 DEG C, such as can be 600 DEG C, 650 DEG C, 700
DEG C, 750 DEG C, 800 DEG C, 850 DEG C or the specific point value between 900 DEG C and above-mentioned numerical value, the present invention no longer exclusive list.
According to the present invention, the time of step (1) described roasting be 0.5-3h, such as can be 0.5h, 1h, 1.5h, 2h,
Specific point value between 2.5h or 3h and above-mentioned numerical value, the present invention no longer exclusive list.
According to the present invention, the mass ratio of step (2) water and roasting clinker is (2-6): 1, such as can be 2:1,3:
1, the specific point value between 4:1,5:1 or 6:1 and above-mentioned numerical value, the present invention no longer exclusive list.
According to the present invention, the temperature of step (2) described leaching be 60-100 DEG C, such as can be 60 DEG C, 65 DEG C, 70 DEG C,
Specific point value between 75 DEG C, 80 DEG C, 85 DEG C, 90 DEG C, 95 DEG C or 100 DEG C and above-mentioned numerical value, the no longer exhaustive column of the present invention
It lifts.
According to the present invention, the time of step (2) described leaching be 0.5-2h, such as can be 0.5h, 0.8h, 1h, 1.2h,
Specific point value between 1.5h, 1.8h or 2h and above-mentioned numerical value, the present invention no longer exclusive list.
According to the present invention, the temperature of step (3) described crystallisation by cooling is 10-30 DEG C, such as can be 10 DEG C, 15 DEG C, 20
DEG C, 25 DEG C or the specific point value between 30 DEG C and above-mentioned numerical value, the present invention no longer exclusive list.
After step (3) the of the present invention separation of solid and liquid, the concentration of vanadium in liquid after gained crystallizes is detected, as vanadium concentration < 10g/
When L, roasting clinker will be leached in liquid return step (2) after crystallization, repetitive operation to after crystallizing in liquid vanadium build up to it is dense
Degree >=10g/L.
After gained crystallization when vanadium concentration >=10g/L in liquid, vanadium product is converted by processing by liquid after crystallization.
The conventional means that this field can be used in the above-mentioned operation for converting vanadium product for liquid after crystallization carry out, and the present invention is to it
Do not do particular determination.
Illustratively, liquid after vanadium concentration >=10g/L crystallization can be returned directly to vanadium slag sodium roasting process, and passed through
The obtained vanadium solution that contains is leached after sodium-salt calcination to mix, and is then converted to vanadium product；It can also be adsorbed and be tied with spent ion exchange resin
Liquid carries out vanadium extraction after crystalline substance；Calcium precipitation can also be added into liquid after crystallization, turn molten with sulfuric acid solution, adjust pH and precipitated, obtained
Vanadium product.
Only the present invention enumerates " liquid is converted into vanadium product after crystallization " available method to the above method, and
It is not limited only to this.
The mode of separation of solid and liquid commonly used in the art is suitable for the present invention, it is preferred to use the mode of filtering carries out, but non-
It is only limitted to this.
The method of extraction sulphur and vanadium of the present invention from desulfurization slag containing vanadium includes following step as a preferred technical solution,
It is rapid:
(1) vanadium desulfurization slag will be contained to be crushed, grind, blank is carried out at 600-900 DEG C and roasts 0.5-3h, obtains roasting ripe
Material；
(2) the roasting clinker that step (1) obtains is mixed with water, control water and the mass ratio for roasting clinker are (2-6): 1,
0.5-2h is leached at 60-100 DEG C, obtains tailings and leachate after separation of solid and liquid；
(3) by leachate crystallisation by cooling at 10-30 DEG C obtained by step (2), obtained after separation of solid and liquid sodium sulfate crystal and
Liquid after crystallization；
(4) after the crystallization obtained by the step (3) in liquid when vanadium concentration < 10g/L, to roasting in liquid return step (2) after crystallization
Clinker is leached；After gained crystallization when vanadium concentration >=10g/L in liquid, vanadium product is converted by processing by liquid after crystallization.
Compared with prior art, the present invention at least has the advantages that
(1) present invention, which realizes, utilizes the resource utilization of valuable element in desulfurization slag containing vanadium, wherein the rate of recovery of sulphur
Greater than 93%, the rate of recovery of vanadium is greater than 85%, and has obtained sodium sulphate product of the purity 94% or more.
(2) simple process of offer of the invention, entire production process do not have discharge of wastewater, and economy and environmental benefit are aobvious
It writes, is suitable for industrialization promotion.
(3) method provided by the invention alleviates the desuifurized accumulation containing vanadium for the adverse effect of environment, obtains simultaneously
Good economic benefit, has a extensive future.
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.
Desulfurization slag containing vanadium used in various embodiments of the present invention is the waste residue obtained in iron-smelting process of company containing Cheng Gang, institute
The content for stating vanadium in desulfurization slag containing vanadium is 1-5wt%, and the content of sulphur is 15-25wt%, the content 20-35wt% of sodium.
The following are typical but non-limiting specific embodiments of the invention:
Embodiment 1
A kind of method that sulphur and vanadium are extracted from desulfurization slag containing vanadium is present embodiments provided, the method includes following steps
It is rapid:
(1) vanadium desulfurization slag will be contained to be crushed, be finely ground to 150 mesh hereinafter, being subsequently placed in Muffle furnace, blank roasts at 700 DEG C
2h is burnt, roasting clinker is obtained after roasting；
(2) the roasting clinker that step (1) obtains is mixed with water 1:6 in mass ratio, the leaching 1.5h at 80 DEG C, instead
It should filter after the completion, obtain tailings and leachate；
(3) leachate that step (2) obtains is cooled to 25 DEG C to crystallize, sodium sulphate crystalline substance is obtained by filtration after the completion of crystallization
Liquid after body and crystallization；
(4) vanadium concentration is 2g/L in liquid after crystallization obtained by step (3), is returned it into step (2) for roasting clinker
Leaching；
(5) repeat aforesaid operations to after crystallizing in liquid vanadium concentration be >=10g/L when, liquid after crystallization is returned into vanadium slag sodium
Calcining process is converted into vanadium product.
After testing, the recovery rate of sulphur is 94.2% in the present embodiment, and sodium sulfate crystal purity is 95.2%, the extraction of vanadium
Rate is 86.2%.
Embodiment 2
A method of from sulphur and vanadium is extracted in desulfurization slag containing vanadium, described method includes following steps:
(1) vanadium desulfurization slag will be contained to be crushed, be finely ground to 150 mesh hereinafter, being subsequently placed in Muffle furnace, blank roasts at 800 DEG C
1.5h is burnt, roasting clinker is obtained after roasting；
(2) the roasting clinker that step (1) obtains is mixed, the leaching 1h at 95 DEG C with water 1:3 in mass ratio, is reacted
It filters after the completion, obtains tailings and leachate；
(3) leachate that step (2) obtains is cooled to 20 DEG C to crystallize, sodium sulphate crystalline substance is obtained by filtration after the completion of crystallization
Liquid after body and crystallization；
(4) vanadium concentration is 10g/L in liquid after crystallization obtained by step (3), returns it to vanadium slag sodium roasting process, is converted
For vanadium product.
After testing, the recovery rate of sodium sulphate is 93.3% in the present embodiment, and sodium sulfate crystal purity is 95.8%, vanadium
Recovery rate is 85.6%.
Embodiment 3
A method of from sulphur and vanadium is extracted in desulfurization slag containing vanadium, described method includes following steps:
(1) vanadium desulfurization slag will be contained to be crushed, be finely ground to 150 mesh hereinafter, being subsequently placed in Muffle furnace, blank roasts at 750 DEG C
2.5h is burnt, roasting clinker is obtained after roasting；
(2) the roasting clinker that step (1) obtains is mixed with water 1:5 in mass ratio, the leaching 0.5h at 100 DEG C,
It filters after the reaction was completed, obtains tailings and leachate；
(3) leachate that step (2) obtains is cooled to 22 DEG C to crystallize, sodium sulphate crystalline substance is obtained by filtration after the completion of crystallization
Liquid after body and crystallization；
(4) vanadium concentration is 5g/L in liquid after crystallization obtained by step (3), is returned it into step (2) for roasting clinker
Leaching；
(5) repeat aforesaid operations to after crystallizing in liquid vanadium concentration be >=10g/L when, liquid after crystallization is returned into vanadium slag sodium
Calcining process is converted into vanadium product.
After testing, the recovery rate of sodium sulphate is 94.8% in the present embodiment, and sodium sulfate crystal purity is 96.1%, vanadium
Recovery rate is 85.2%.
Embodiment 4
A method of from sulphur and vanadium is extracted in desulfurization slag containing vanadium, described method includes following steps:
(1) vanadium desulfurization slag will be contained to be crushed, be finely ground to 150 mesh hereinafter, being subsequently placed in Muffle furnace, blank roasts at 850 DEG C
1h is burnt, roasting clinker is obtained after roasting；
(2) the roasting clinker that step (1) obtains is mixed with water 1:2 in mass ratio, the leaching 1.5h at 95 DEG C, instead
It should filter after the completion, obtain tailings and leachate；
(3) leachate that step (2) obtains is cooled to 24 DEG C to crystallize, sodium sulphate crystalline substance is obtained by filtration after the completion of crystallization
Liquid after body and crystallization；
(4) vanadium concentration is 12g/L in liquid after crystallization obtained by step (3), returns it to vanadium slag sodium roasting process, is converted
For vanadium product.
After testing, the recovery rate of sodium sulphate is 95.1% in the present embodiment, and sodium sulfate crystal purity is 94.5%, vanadium
Recovery rate is 86.7%.
Embodiment 5
A kind of method that sulphur and vanadium are extracted from desulfurization slag containing vanadium is present embodiments provided, the method includes following steps
It is rapid:
(1) vanadium desulfurization slag will be contained to be crushed, be finely ground to 150 mesh hereinafter, being subsequently placed in Muffle furnace, blank roasts at 600 DEG C
3h is burnt, roasting clinker is obtained after roasting；
(2) the roasting clinker that step (1) obtains is mixed, the leaching 2h at 70 DEG C with water 1:4 in mass ratio, is reacted
It filters after the completion, obtains tailings and leachate；
(3) leachate that step (2) obtains is cooled to 10 DEG C to crystallize, sodium sulphate crystalline substance is obtained by filtration after the completion of crystallization
Liquid after body and crystallization；
(4) vanadium concentration is 8g/L in liquid after crystallization obtained by step (3), is returned it into step (2) for roasting clinker
Leaching；
(5) repeat aforesaid operations to after crystallizing in liquid vanadium concentration be >=10g/L when, liquid after crystallization is returned into vanadium slag sodium
Calcining process is converted into vanadium product.
After testing, the recovery rate of sulphur is 94.5% in the present embodiment, and sodium sulfate crystal purity is 96.0%, the extraction of vanadium
Rate is 87.4%.
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 (9)
1. a kind of method for extracting sulphur and vanadium from desulfurization slag containing vanadium, which is characterized in that the described method comprises the following steps:
(1) vanadium desulfurization slag will be contained and carry out blank roasting, obtain roasting clinker；
(2) the roasting clinker that step (1) obtains is mixed with water and is leached, tailings and leachate are obtained after separation of solid and liquid；
(3) by leachate crystallisation by cooling obtained by step (2), liquid after sodium sulfate crystal and crystallization is obtained after separation of solid and liquid.
2. the method as described in claim 1, which is characterized in that based on mass percentage, desulfurization slag containing vanadium described in step (1)
In contain: S15-25%, Na20-35%, V1-5%.
3. method according to claim 1 or 2, which is characterized in that desulfurization slag containing vanadium described in step (1) carries out brokenly before roasting
Broken and grinding.
4. the method according to claim 1, which is characterized in that the temperature of step (1) described roasting is 600-900
℃；
Preferably, the time of step (1) described roasting is 0.5-3h.
5. method according to any of claims 1-4, which is characterized in that the quality of step (2) water and roasting clinker
Than for (2-6): 1.
6. the method according to claim 1 to 5, which is characterized in that the temperature of step (2) described leaching is 60-100
℃；
Preferably, the time of step (2) described leaching is 0.5-2h.
7. as the method according to claim 1 to 6, which is characterized in that the temperature of step (3) described crystallisation by cooling is 10-
30℃。
8. the method according to claim 1 to 7, which is characterized in that the vanadium concentration in liquid after step (3) gained crystallizes
When < 10g/L, roasting clinker is leached in liquid return step (2) after crystallization；Vanadium is dense in liquid after step (3) gained crystallizes
When degree >=10g/L, vanadium product is converted by processing by liquid after crystallization.
9. the method according to claim 1, which is characterized in that the described method comprises the following steps:
(1) vanadium desulfurization slag will be contained to be crushed, grind, blank is carried out at 600-900 DEG C and roasts 0.5-3h, obtain roasting clinker；
(2) the roasting clinker that step (1) obtains is mixed with water, control water and the mass ratio for roasting clinker are (2-6): 1,
0.5-2h is leached at 60-100 DEG C, obtains tailings and leachate after separation of solid and liquid；
(3) by leachate crystallisation by cooling at 10-30 DEG C obtained by step (2), sodium sulfate crystal and crystallization are obtained after separation of solid and liquid
Liquid afterwards；
(4) after the crystallization obtained by the step (3) in liquid when vanadium concentration < 10g/L, to roasting clinker in liquid return step (2) after crystallization
It is leached；After gained crystallization when vanadium concentration >=10g/L in liquid, vanadium product is converted by processing by liquid after crystallization.
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| CN201910339909.2A CN109913661A (en) | 2019-04-25 | 2019-04-25 | A method of from extraction sulphur and vanadium in desulfurization slag containing vanadium |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110983051A (en) * | 2019-12-24 | 2020-04-10 | 河钢股份有限公司承德分公司 | Backwashing enrichment method for low-concentration vanadium liquid |
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| CN103572063A (en) * | 2013-11-04 | 2014-02-12 | 中国科学院过程工程研究所 | Method for cleanly and efficiently recovering vanadium from vanadium slag by employing sodium-free roasting |
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