CN108658126A - A method of extracting vanadium from calcium phosphorus slag - Google Patents
A method of extracting vanadium from calcium phosphorus slag Download PDFInfo
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- CN108658126A CN108658126A CN201810696718.7A CN201810696718A CN108658126A CN 108658126 A CN108658126 A CN 108658126A CN 201810696718 A CN201810696718 A CN 201810696718A CN 108658126 A CN108658126 A CN 108658126A
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- phosphorus slag
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- calcium phosphorus
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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
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Abstract
The present invention relates to a kind of method for extracting vanadium in phosphorus slag from calcium, the method is：Calcium phosphorus slag is mixed with lye, then heats, pressurize and leached, obtain containing vanadium leachate and leached mud after separation of solid and liquid.The present invention selects the condition of low-temperature low-alkali and high pressure to leach calcium phosphorus slag, realizes the efficient leaching to v element in calcium phosphorus slag, leaching rate is 80% or more.And entire production process does not have discharge of wastewater, economy and obvious environment benefit, has a good application prospect.
Description
Technical field
The present invention relates to vanadium recycling fields, and in particular to a kind of method for being related to extracting vanadium in the phosphorus slag from calcium.
Background technology
Vanadium is a kind of accompanying element 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 adding 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.On the one hand, these solids containing vanadium are useless
Gurry had both occupied a large amount of land resource as being not added with disposition if arbitrarily banking up, and increased the management cost of enterprise, and can be due to
The toxicity of vanadium and bring grievous injury to human and environment；On the other hand, containing in solid waste containing vanadium much has Important Economic
The metal of value, it should positive is recycled, and is turned waste into wealth, and changes evil as benefit, to create considerable economic benefit and
Social benefit.Therefore the extraction of v element is of great significance in research waste containing vanadium.
Calcium phosphorus slag is that the steel-making of Cheng Gang companies removes generated solid waste when silicon dephosphorization, wherein containing about 2% V.At present
Generally directly (calcium) phosphorus slag is utilized directly as waste industrially, and is applied in building field, and seldom to its into
Row secondary recovery vanadium extraction.Such as CN106082723A discloses a kind of method producing high-quality high-dopant phosphorus slag cement using phosphorus slag
And its production method, using shale, phosphorus slag, sandstone, lime stone, five component dispensing of iron ore, using sandstone as siliceous compared with Zhengyuan
Material obtains raw material through grinding, using pre- thermal decomposition, cools down to obtain phosphoric slag cement clinker through high-temperature calcination, then with gypsum, stone
It is mixed with phosphoric slag cement after the separate compilings such as lime stone, phosphorus slag.CN103351530A discloses a kind of modified phosphorous slag and waste and old modeling
Composite plate and its production method, use waste and old polypropylene, vinyon and industrial residue phosphorus slag for primary raw material made of material,
Using suitable preparation method, high-strength composite board is made, has not only alleviated waste plastic and pollution of the phosphorus slag to environment, but also to build
It builds engineering and increases new material, widely used bamboo plywood and Wood construction formwork in alternative construction.
CN104803646A discloses a kind of phosphorus slag powder microdilatancy grouting material and its application method, utilizes portland cement, river sand, phosphorus
Ground-slag, slag powders, phosphorus slag powder activity excitant, calcined magnesia, adipose membrane calcium oxide, polypropylene fibre, wood-fibred, modified bumps
Phosphorus slag powder microdilatancy grouting material is prepared in stick soil, antifoaming agent and water-reducing agent, after building-site directly adds water to stir evenly
It can be used.
Since V content is not high, and complicated component in calcium phosphorus slag, the processing of traditional wet processing are difficult to effectively carry it
It takes, improved technique is again excessively complicated, and process generates a large amount of waste water again needs after-treatment, and energy consumption is also high, and economic benefit is simultaneously
It is undesirable.For the dual purpose increased economic efficiency with environmental protection, it is necessary to develop it is a kind of it is efficient, low energy consumption and technique letter
The technique that vanadium is extracted in single slave calcium phosphorus slag, efficiently uses vanadium resource with realizing.
Invention content
In order to solve the above technical problems, the present invention provides a kind of method for extracting vanadium in the phosphorus slag from calcium, low-temperature low-alkali is selected
And the condition of high pressure leaches calcium phosphorus slag, realizes the efficient leaching to v element in calcium phosphorus slag, leaching rate is 80%
More than.Entire production process does not have discharge of wastewater, economy and obvious environment benefit, has a good application prospect.
In order to achieve the above objectives, the present invention uses following technical scheme：
The present invention provides the clean preparation method for extracting vanadium in a kind of phosphorus slag from calcium, the method is：By calcium phosphorus slag with
Lye mixes, and then heats, pressurizes and leached, obtains containing vanadium leachate and leached mud after separation of solid and liquid.
According to the present invention, the calcium phosphorus slag is subjected to broken and fine grinding before being mixed with lye, to calcium phosphorus slag after fine grinding
Granularity and without particular determination, is worn into the particle of granularity equalization.
According to the present invention, the lye is sodium hydroxide solution and/or potassium hydroxide solution.
Preferably, a concentration of 0.1-3mol/L of the lye, for example, can be 0.1mol/L, 0.5mol/L, 1mol/L,
Specific point value between 1.5mol/L, 2mol/L, 2.5mol/L or 3mol/L and above-mentioned numerical value, as space is limited and for letter
Bright consideration, the present invention no longer exclusive list.
According to the present invention, the calcium phosphorus slag is 1 with the mass ratio of sodium hydroxide and/or potassium hydroxide in lye:(0.5-
1.2), such as can be 1:0.5、1:0.6、1:0.7、1:0.8、1:0.9、1:1、1:1.1 or 1:1.2 and above-mentioned numerical value it
Between specific point value, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the temperature of the leaching is 90-130 DEG C, for example, can be 90 DEG C, 95 DEG C, 100 DEG C, 105 DEG C,
Specific point value between 110 DEG C, 115 DEG C, 120 DEG C, 125 DEG C or 130 DEG C and above-mentioned numerical value, as space is limited and for simplicity
The considerations of, the present invention no longer exclusive list.
According to the present invention, time of the leaching is 1-4h, for example, can be 1h, 1.5h, 2h, 2.5h, 3h, 3.5h or
Specific point value between 4h and 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 pressure of the leaching is 0.1-1MPa, for example, can be 0.1MPa, 0.2MPa, 0.3MPa,
Specific point value between 0.4MPa, 0.5MPa, 0.6MPa, 0.7MPa, 0.8MPa, 0.9MPa or 1MPa and above-mentioned numerical value, limit
In length and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the Leach reaction carries out preferably in autoclave.
According to the present invention, after the completion of leaching, the operation being separated by solid-liquid separation again after being diluted to gained reaction paste, institute
Stating dilution can be carried out with the cleaning solution that water or washing leached mud obtain.
According to the present invention, in order to be conducive to vanadium extraction, gained is returned containing vanadium leachate and is mixed with lye with calcium phosphorus slag by the present invention
It closes, continues Leach reaction, until containing when vanadium concentration >=8g/L, vanadium extraction is carried out in vanadium leachate.
Means well known in the art can be selected in the present invention illustratively can be right containing vanadium leachate progress vanadium extraction to gained
Gained is crystallized to obtain sodium vanadate containing vanadium leachate, but it is non-be only limitted to this, other suitable extraction vanadium methods are equally applicable to this
Invention.
Liquid return is mixed with calcium phosphorus slag and lye after the present invention will crystallize crystallization obtained by vanadium extraction after the completion, and water is greatly saved
Dosage, realize recycling for water.
Of the present invention be separated by solid-liquid separation selects means commonly used in the art to carry out, such as can be filtering, filter, centrifugation
Deng, but it is non-be only limitted to this, other suitable solid-liquid separation means are equally applicable to the present invention.
The method of the invention includes the following steps as a preferred technical solution,：
(1) calcium phosphorus slag mix with sodium hydroxide solution and/or potassium hydroxide solution after broken and fine grinding, control calcium
Phosphorus slag is 1 with the mass ratio of sodium hydroxide and/or potassium hydroxide in lye:(0.5-1.2), is then heated to 90-130 DEG C,
1-4h is leached under 0.1-1MPa；
(2) reaction paste obtained to leaching is diluted, and is then separated by solid-liquid separation, and obtains containing vanadium leachate and leaching
Slag washs leached mud, by gained cleaning solution for being diluted to reaction paste after separation of solid and liquid；
(3) it will mix, continue with calcium phosphorus slag and lye in return to step containing vanadium leachate (1) that step (2) obtains
Leach reaction, until containing when vanadium concentration >=8g/L, vanadium extraction is carried out containing vanadium leachate to gained in vanadium leachate.
Compared with prior art, the present invention at least has the advantages that：
(1) present invention selects the condition of low-temperature low-alkali and high pressure to leach calcium phosphorus slag, realizes in calcium phosphorus slag
The efficient leaching of v element, leaching rate is 80% or more.
(2) present invention, which realizes, recycles the recycling of v element in calcium phosphorus slag, and entire production process does not have waste water row
It puts, economy and obvious environment benefit have a good application prospect.
Specific implementation mode
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
(1) calcium phosphorus slag mix with the sodium hydroxide solution of 0.5mol/L after broken and fine grinding, control calcium phosphorus slag and
The mass ratio of sodium hydroxide is 1 in lye:1, then mixed material is placed in autoclave, is heated to 105 DEG C,
3h is leached under 0.8MPa；
(2) reaction paste obtained after being leached to step (1) is diluted, and is then separated by solid-liquid separation, and obtains soaking containing vanadium
Go out liquid and leached mud, leached mud washed with 80 DEG C of water, after separation of solid and liquid by gained cleaning solution be used for reaction paste into
Row dilution.
By detection, the leaching rate of vanadium is 82.1% in calcium phosphorus slag.
Embodiment 2
(1) calcium phosphorus slag mix with the sodium hydroxide solution of 0.8mol/L after broken and fine grinding, control calcium phosphorus slag and
The mass ratio of sodium hydroxide is 1 in lye:1.2, then mixed material is placed in autoclave, is heated to 95 DEG C,
4h is leached under 0.6MPa；
(2) reaction paste obtained after being leached to step (1) is diluted, and is then separated by solid-liquid separation, and obtains soaking containing vanadium
Go out liquid and leached mud, leached mud washed with 70 DEG C of water, after separation of solid and liquid by gained cleaning solution be used for reaction paste into
Row dilution；
(3) it will mix, continue with calcium phosphorus slag and lye in return to step containing vanadium leachate (1) that step (2) obtains
Leach reaction carries out crystallization vanadium extraction containing vanadium leachate to gained, obtains vanadic acid until when 10g/L a concentration of containing vanadium in vanadium leachate
Sodium, liquid is back in step (1) for the leaching to calcium phosphorus slag after gained crystallization.
By detection, the leaching rate of vanadium is 85.6% in calcium phosphorus slag.
Embodiment 3
(1) calcium phosphorus slag mix with the sodium hydroxide solution of 0.5mol/L after broken and fine grinding, control calcium phosphorus slag and
The mass ratio of sodium hydroxide is 1 in lye:0.5, then mixed material is placed in autoclave, is heated to 120 DEG C,
2h is leached under 1MPa；
(2) reaction paste obtained after being leached to step (1) is diluted, and is then separated by solid-liquid separation, and obtains soaking containing vanadium
Go out liquid and leached mud, leached mud washed with 75 DEG C of water, after separation of solid and liquid by gained cleaning solution be used for reaction paste into
Row dilution；
(3) it will mix, continue with calcium phosphorus slag and lye in return to step containing vanadium leachate (1) that step (2) obtains
Leach reaction carries out crystallization vanadium extraction containing vanadium leachate to gained, obtains vanadic acid until when 8g/L a concentration of containing vanadium in vanadium leachate
Sodium, liquid is back in step (1) for the leaching to calcium phosphorus slag after gained crystallization.
By detection, the leaching rate of vanadium is 83.4% in calcium phosphorus slag.
Embodiment 4
(1) calcium phosphorus slag mix with the potassium hydroxide solution of 1mol/L after broken and fine grinding, control calcium phosphorus slag and alkali
The mass ratio of potassium hydroxide is 1 in liquid:1.1, mixed material is then heated to 130 DEG C, 1h is leached at 0.9MPa；
(2) reaction paste obtained after being leached to step (1) is diluted, and is then separated by solid-liquid separation, and obtains soaking containing vanadium
Go out liquid and leached mud, leached mud washed with 85 DEG C of water, after separation of solid and liquid by gained cleaning solution be used for reaction paste into
Row dilution；
(3) it will mix, continue with calcium phosphorus slag and lye in return to step containing vanadium leachate (1) that step (2) obtains
Leach reaction carries out crystallization vanadium extraction containing vanadium leachate to gained, obtains vanadic acid until when 9g/L a concentration of containing vanadium in vanadium leachate
Sodium, liquid is back in step (1) for the leaching to calcium phosphorus slag after gained crystallization.
By detection, the leaching rate of vanadium is 84.8% in calcium phosphorus slag.
Embodiment 5
(1) calcium phosphorus slag mix with the potassium hydroxide solution of 2mol/L after broken and fine grinding, control calcium phosphorus slag and alkali
The mass ratio of potassium hydroxide is 1 in liquid:0.8, mixed material is then heated to 110 DEG C, 3.5h is leached at 0.5MPa；
(2) reaction paste obtained after being leached to step (1) is diluted, and is then separated by solid-liquid separation, and obtains soaking containing vanadium
Go out liquid and leached mud, leached mud washed with 80 DEG C of water, after separation of solid and liquid by gained cleaning solution be used for reaction paste into
Row dilution；
(3) it will mix, continue with calcium phosphorus slag and lye in return to step containing vanadium leachate (1) that step (2) obtains
Leach reaction carries out crystallization vanadium extraction containing vanadium leachate to gained, obtains vanadic acid until when 8.5g/L a concentration of containing vanadium in vanadium leachate
Sodium, liquid is back in step (1) for the leaching to calcium phosphorus slag after gained crystallization.
By detection, the leaching rate of vanadium is 83.1% in calcium phosphorus slag.
Embodiment 6
(1) calcium phosphorus slag mix with the sodium hydroxide solution of 2.5mol/L after broken and fine grinding, control calcium phosphorus slag and
The mass ratio of sodium hydroxide is 1 in lye:0.5, mixed material is then heated to 90 DEG C, 4h is leached at 0.3MPa；
(2) reaction paste obtained after being leached to step (1) is diluted, and is then separated by solid-liquid separation, and obtains soaking containing vanadium
Go out liquid and leached mud, leached mud washed with 80 DEG C of water, after separation of solid and liquid by gained cleaning solution be used for reaction paste into
Row dilution.
By detection, the leaching rate of vanadium is 82.7% in calcium phosphorus slag.
Embodiment 7
(1) calcium phosphorus slag mix with the sodium hydroxide solution of 1.5mol/L after broken and fine grinding, control calcium phosphorus slag and
The mass ratio of sodium hydroxide is 1 in lye:0.6, mixed material is then heated to 100 DEG C, 2.5h is leached at 0.8MPa；
(2) reaction paste obtained after being leached to step (1) is diluted, and is then separated by solid-liquid separation, and obtains soaking containing vanadium
Go out liquid and leached mud, leached mud washed with 75 DEG C of water, after separation of solid and liquid by gained cleaning solution be used for reaction paste into
Row dilution；
(3) it will mix, continue with calcium phosphorus slag and lye in return to step containing vanadium leachate (1) that step (2) obtains
Leach reaction carries out crystallization vanadium extraction containing vanadium leachate to gained, obtains vanadic acid until when 11g/L a concentration of containing vanadium in vanadium leachate
Sodium, liquid is back in step (1) for the leaching to calcium phosphorus slag after gained crystallization.
By detection, the leaching rate of vanadium is 85.0% in calcium phosphorus slag.
Comparative example 1
Compared with Example 4, outer in addition to being not pressurized in the heating leaching process in the step (1), other steps and condition and
Embodiment 4 is identical, i.e., mixed material is leached 1h at 130 DEG C.
By detection, the leaching rate of vanadium is 56.3% in calcium phosphorus slag in this comparative example.
Comparative example 2
Compared with Example 4, in addition to the temperature of step (1) described leaching process is 70 DEG C outer, other steps and condition and
Embodiment 4 is identical, i.e., mixed material is heated to 70 DEG C, and 1h. is leached at 0.9MPa
By detection, the leaching rate of vanadium is 43.7% in calcium phosphorus slag in this comparative example.
Applicant states that the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological processes, that is, it is above-mentioned detailed not mean that the present invention has to rely on
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The addition of equivalence replacement and auxiliary element to each raw material of product of the present invention, the selection etc. of concrete mode all fall within the present invention's
Within protection domain and the open scope.
Claims (10)
1. a kind of method for extracting vanadium in phosphorus slag from calcium, which is characterized in that the method is：Calcium phosphorus slag is mixed with lye, so
It heats afterwards, pressurize and leached, obtain containing vanadium leachate and leached mud after separation of solid and liquid.
2. the method as described in claim 1, which is characterized in that carry out the calcium phosphorus slag before mixed with lye broken and carefully
Mill.
3. method as claimed in claim 1 or 2, which is characterized in that the lye is sodium hydroxide solution and/or potassium hydroxide
Solution；
Preferably, a concentration of 0.1-3mol/L of the lye.
4. method as described in any one of claims 1-3, which is characterized in that in the calcium phosphorus slag and lye sodium hydroxide and/
Or the mass ratio of potassium hydroxide is 1:(0.5-1.2).
5. method according to any one of claims 1-4, which is characterized in that the temperature of the leaching is 90-130 DEG C；
Preferably, the time of the leaching is 1-4h.
6. method as described in any one in claim 1-5, which is characterized in that the pressure of the leaching is 0.1-1MPa.
7. method as claimed in any one of claims 1 to 6, which is characterized in that the Leach reaction in autoclave into
Row.
8. such as claim 1-7 any one of them methods, which is characterized in that after the completion of leaching, carried out to gained reaction paste
The operation being separated by solid-liquid separation again after dilution；
Preferably, leached mud is washed, by gained cleaning solution for being diluted to reaction paste after separation of solid and liquid.
9. such as claim 1-8 any one of them methods, which is characterized in that by gained containing vanadium leachate return with calcium phosphorus slag with
Lye mixes, and continues Leach reaction, until containing when vanadium concentration >=8g/L, vanadium extraction is carried out in vanadium leachate.
10. such as claim 1-9 any one of them methods, which is characterized in that the described method comprises the following steps：
(1) calcium phosphorus slag mix with sodium hydroxide solution and/or potassium hydroxide solution after broken and fine grinding, control calcium phosphorus slag
It is 1 with the mass ratio of sodium hydroxide in lye and/or potassium hydroxide:(0.5-1.2), is then heated to 90-130 DEG C, in 0.1-
1-4h is leached under 1MPa；
(2) reaction paste obtained to leaching is diluted, and is then separated by solid-liquid separation, and obtains containing vanadium leachate and leached mud,
Leached mud is washed, by gained cleaning solution for being diluted to reaction paste after separation of solid and liquid；
(3) it will be mixed with calcium phosphorus slag and lye in return to step containing vanadium leachate (1) that step (2) obtains, continue to leach
Reaction, until containing when vanadium concentration >=8g/L, vanadium extraction is carried out containing vanadium leachate to gained in vanadium leachate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810696718.7A CN108658126A (en) | 2018-06-29 | 2018-06-29 | A method of extracting vanadium from calcium phosphorus slag |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586613A (en) * | 2012-03-20 | 2012-07-18 | 河北钢铁股份有限公司承德分公司 | Method for recycling vanadium from vanadium-containing steel slag |
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2018
- 2018-06-29 CN CN201810696718.7A patent/CN108658126A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586613A (en) * | 2012-03-20 | 2012-07-18 | 河北钢铁股份有限公司承德分公司 | Method for recycling vanadium from vanadium-containing steel slag |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Application publication date: 20181016 |