CN103966437B - A kind of method containing the dephosphorization of vanadium acidic solution - Google Patents
A kind of method containing the dephosphorization of vanadium acidic solution Download PDFInfo
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- CN103966437B CN103966437B CN201410203151.7A CN201410203151A CN103966437B CN 103966437 B CN103966437 B CN 103966437B CN 201410203151 A CN201410203151 A CN 201410203151A CN 103966437 B CN103966437 B CN 103966437B
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Abstract
The invention provides a kind of method containing the dephosphorization of vanadium acidic solution.Described containing in vanadium acidic solution contains H
2pO
4 -, said method comprising the steps of: regulate pH value to 0.2 ~ 1 containing vanadium acidic solution; To add electrolyzer containing vanadium acidic solution and carry out electrolysis, wherein, described electrolyzer is divided into cathode compartment and anolyte compartment by ion-exchange membrane; After electrolysis completes, the anolyte in described anolyte compartment is shifted out in anolyte compartment, and add dephosphorization agent and carry out dephosphorization; Then, the anolyte after filtering dephosphorization is also mixed to get low-phosphorous vanadium liquid with the catholyte in described cathode compartment.The method that the present invention adopts electrochemistry to combine with general chemistry carries out removing the phosphorus in acidic solution, and the clearance of phosphorus can reach 99%.
Description
Technical field
The present invention relates to vanadium extraction chemical technology field, more particularly, relate to the method for a kind of removing containing phosphorus in vanadium acidic solution.
Background technology
At present mainly contain sodium vanadium extracting method and calcification vanadium extracting method using vanadium slag as the raw material method that industrially large-scale application extracts vanadium.Because the vanadium extraction of sodium method causes severe contamination to environmental problem, along with to the concern of environmental problem and the legislation of environment protection, the limitation of sodium method vanadium extraction becomes increasingly conspicuous.In recent years, environmentally friendly cleaning technique-calcification vanadium extraction technology is more and more subject to people's attention.
In order to reduce phosphorus content in molten steel or mineral resources itself containing high phosphorus, in the vanadium slag of gained or raw material, have higher harmful element phosphorus.When acidleach operation is carried out in calcification vanadium extraction, a large amount of harmful element phosphorus has entered into containing vanadium acidic solution.Same, extracting vanadium from stone coal acidleach vanadium liquid and thick vanadium product dissolve in the acid vanadium liquid of gained and also comprise harmful element phosphor.Therefore a kind of method can effectively removed containing harmful element phosphorus in vanadium acidic solution is needed badly.
Summary of the invention
For the deficiencies in the prior art, an object of the present invention is to solve in above-mentioned prior art the one or more problems existed.
An object of the present invention is to provide a kind of method can effectively removed containing harmful element phosphorus in vanadium acidic solution.
To achieve these goals, the invention provides a kind of method containing the dephosphorization of vanadium acidic solution.Described containing in vanadium acidic solution contains H
2pO
4 -, said method comprising the steps of: regulate pH value to 0.2 ~ 1 containing vanadium acidic solution; To add electrolyzer containing vanadium acidic solution and carry out electrolysis, wherein, described electrolyzer is divided into cathode compartment and anolyte compartment by ion-exchange membrane; Until described complete electromigration containing the ion of v element in vanadium acidic solution and the ion of phosphoric after, the anolyte in described anolyte compartment is shifted out in anolyte compartment, and adds dephosphorization agent and carry out dephosphorization; Then, the anolyte after filtering dephosphorization is also mixed to get low-phosphorous vanadium liquid with the catholyte in described cathode compartment.
According to the embodiment of the present invention containing the method for vanadium acidic solution dephosphorization, described electrolysis step adopts voltage stabilized source and controls electrolysis voltage is 2 ~ 10V, and electrolysis time is 0.5 ~ 2h.
According to the embodiment of the present invention containing the method for vanadium acidic solution dephosphorization, described dephosphorization agent is molysite and/or aluminium salt.
According to the embodiment of the present invention containing the method for vanadium acidic solution dephosphorization, described dephosphorization agent is bodied ferric sulfate and/or polyaluminium sulfate.
According to the embodiment of the present invention containing the method for vanadium acidic solution dephosphorization, add-on and the described mol ratio containing phosphorus content in vanadium acidic solution of described dephosphorization agent are 1 ~ 5.
According to the embodiment of method of the present invention containing the dephosphorization of vanadium acidic solution, the pH value that described dephosphorization step controls described anolyte is 1.5 ~ 4, temperature is 50 ~ 100 DEG C, and the reaction times of described dephosphorization step is 0.5 ~ 2h.
According to the embodiment of the present invention containing the method for vanadium acidic solution dephosphorization, the alkali of oxidizing acid or irreducibility is adopted to regulate described containing the pH value of vanadium acidic solution and the pH value of described anolyte.
According to the embodiment of method of the present invention containing the dephosphorization of vanadium acidic solution, described containing vanadium acidic solution be the vanadium liquid of vanadium slag through calcification baking acidleach gained of vanadium-bearing hot metal vanadium extraction gained, the vanadium liquid of the vanadium liquid that obtains of extracting vanadium from stone coal acidolysis after treatment by extraction or dissolve the vanadium liquid of gained for thick vanadium product.
According to the embodiment of method of the present invention containing the dephosphorization of vanadium acidic solution, be describedly greater than 5g/L containing v element content in vanadium acidic solution.
Compared with prior art, beneficial effect of the present invention comprises: the method that the present invention adopts electrochemistry to combine with general chemistry carries out removing the phosphorus in acidic solution, and the clearance of phosphorus can reach 99%.In addition, present invention process is simple and easy to use, equipment requirements is low, easy to operate, wide accommodation, cost are low, has good Social benefit and economic benefit.
Embodiment
Hereinafter, will describe in detail in conjunction with exemplary embodiment according to the method containing the dephosphorization of vanadium acidic solution of the present invention.
The vanadium liquid of the vanadium liquid that method of the present invention can be applicable to the vanadium liquid of vanadium slag through calcification baking acidleach gained of vanadium-bearing hot metal vanadium extraction gained, extracting vanadium from stone coal acidolysis obtains after treatment by extraction or dissolve gained vanadium liquid for thick vanadium product.
Wherein, mainly exist with pentavalent vanadium form containing the vanadium in vanadium acidic solution.
In one exemplary embodiment, be greater than 5g/L containing v element content in vanadium acidic solution, the pH value containing vanadium acidic solution is 2.8 ~ 3.2.Certainly, the present invention be suitable for be not limited thereto containing vanadium acidic solution, the present invention is applicable to various simultaneously containing pentavalent vanadium and H
2pO
4 -vanadium liquid, in addition, other impurity elements can also be comprised containing in vanadium acidic solution, such as chromium element.
Applicant finds, containing the pH value of vanadium acidic solution under 2.8 ~ 3.2 conditions, phosphorus is mainly with H
2pO
4 -exist, effectively can not remove phosphorus according to general chemistry method (such as, calcium chloride dephosphorization process).In order to solve the problem containing phosphorus difficulty removing in vanadium acidic solution, contriver proposes a kind of technique adopting electrochemistry to combine with general chemistry method in a creative way, thus effective removal harmful element phosphorus.Specifically comprise the following steps:
A, with acid-alkali accommodation containing vanadic acid solution ph be 0.2 ~ 1.Being change vanadium in the performance containing existing forms in vanadium acidic solution and ion by the object being adjusted to 0.2 ~ 1 containing vanadic acid solution ph, particularly, is main with VO under the condition of 0.2 ~ 1 containing vanadium in vanadium acidic solution in pH value
2 +positively charged ion form exist, if pH value is greater than 1, then mainly exist with the anionic state of many vanadic acid root containing the vanadium in vanadium acidic solution, if pH is to being less than 0.2, then acidity is too strong, the seriously corroded of not only antianode plate and negative plate when electrolysis, and easily produce hydrogen, there is certain influence to the movement of ion.And phosphoric is under pH value is 0.2 ~ 1 condition, or main with H
2pO
4 -exist.
B, will add in electrolyzer containing vanadium acidic solution and carry out electrolysis.Wherein, electrolyzer comprises cell body, anode, negative electrode and ion-exchange membrane, and cell body is divided into cathode compartment and anolyte compartment by ion-exchange membrane.Negative electrode and anode adopt the acidproof electrode of inertia, and the acidproof electrode of inertia can be Graphite Electrodes, platinum electrode etc.The object of carrying out electrolysis makes vanadium and phosphorus carry out displacement.Wherein, ion (such as, the VO of v element
2 +) enter cathode compartment, ion (such as, the H of phosphoric
2pO
4 -) enter in anolyte compartment.After completing electromigration containing the ion of v element in vanadium acidic solution and the ion of phosphoric, vanadium is separated with phosphorus, just need not take the loss of vanadium while carrying out dephosphorization into account, therefore can by H
2pO
4 -the phosphorus existed effectively is removed.
After c, electrolysis complete, anolyte (i.e. anolyte) in anolyte compartment is shifted out rapidly in anolyte compartment, the pH value regulating anolyte is 1.5 ~ 4, and add dephosphorization agent and carry out dephosphorization, herein, object anolyte pH value being adjusted to 1.5 ~ 4 is for the ease of forming calcium phosphate precipitation.
D, filter the anolyte after by dephosphorization, be then mixed to get low-phosphorous vanadium liquid with the catholyte (i.e. catholyte) in cathode compartment.
Wherein, in step a, for regulating the acid containing vanadic acid solution ph can be the oxidisability acids such as sulfuric acid, nitric acid, hydrochloric acid, can be the alkali that sodium hydroxide, calcium oxide, calcium hydroxide, calcium carbonate, potassium hydroxide etc. do not have reductibility for regulating the alkali containing vanadic acid solution ph.
In stepb, electrolysis carries out ground under voltage stabilizing state, and namely adopting voltage stabilized source and control electrolysis voltage is 2 ~ 10V, and electrolysis time is 0.5 ~ 2h.Preferably, electrolysis voltage controls as 4.8V, and it is 1 hour that electrolysis time controls.
In step c, dephosphorization agent can select one or both mixtures in molysite and aluminium salt, preferably, and the polymerizability salts such as dephosphorization agent selective polymerization ferric sulfate and polyaluminium sulfate.Add-on and the described mol ratio containing phosphorus content in vanadium acidic solution of dephosphorization agent are 1 ~ 5, and better mol ratio is 3.Temperature except phosphorus reaction controls to be 50 ~ 100 DEG C, and better temperature of reaction is 90 ~ 100 DEG C.Regulate the pH value of anolyte to be preferably 3.5, regulate the alkali of the pH value of anolyte can be the alkali that sodium hydroxide, ammoniacal liquor, calcium oxide, potassium hydroxide, calcium carbonate etc. do not have reductibility.Time except phosphorus reaction is 0.5 ~ 2h, and the better reaction times is 0.5 ~ 1h.Further, after phosphorus reaction completes, ageing is proceeded.
The method that the present invention adopts electrochemistry to combine with general chemistry carries out removing the harmful phosphoric containing in vanadium acidic solution, change vanadium in the performance containing existing forms in vanadium acidic solution and ion, then adopt electrolysis to realize vanadium to be separated with the effective of phosphorus, and involved parameter (such as, temperature, mol ratio, pH value, reaction times etc.) is controlled to limit ground parameter area separately at it, finally make the clearance of phosphorus to reach 99%.If above-mentioned parameter exceedes the separation rate that the higher limit of respective range value or lower value can affect vanadium and phosphorus.
In the operation of aforesaid method, take to extend digestion time, increase cooling, take micro-filtration or ultrafiltration to carry out the measure of filtering etc. all to improve phosphor-removing effect.Wherein, increase cooling and refer to before the filtration treatment of steps d, first the anolyte after dephosphorization is cooled, such as, be cooled to room temperature, and then filter, to improve phosphor-removing effect.
In order to understand above-mentioned exemplary embodiment of the present invention better, below in conjunction with concrete example, it is further described.
Such as, a kind of molten iron each constituent content situation in vanadium vanadium slag calcification baking Leaching Vanadium liquid of blowing is: TV content is 5 ~ 50g/L, P element content is 0.1 ~ 5.0g/L, Mg constituent content is 1 ~ 8g/L, Si constituent content is 0.5 ~ 3.8g/L, TFe content is 1 ~ 5g/L, TCr content is 0.1 ~ 0.2g/L, and its pH value is 2.5 ~ 4.0.
In the vanadium liquid of the vanadium liquid that extracting vanadium from stone coal acidolysis obtains after treatment by extraction, each constituent content situation is: TV content is 5 ~ 150g/L, P element content is 0.1 ~ 10g/L, Mg constituent content is 0.1 ~ 0.2g/L, Si constituent content is 0.5 ~ 20g/L, TFe content is 0.01 ~ 0.05g/L, TCr content is 5 ~ 20g/L, and its pH value is 0.5 ~ 4.0.
A kind of thick vanadium product dissolves each constituent content situation in gained vanadium liquid: TV content is 5 ~ 150g/L, P element content is 0.1 ~ 1.3g/L, Mg constituent content is 0.1 ~ 4g/L, Si constituent content is 0.5 ~ 4.8g/L, TFe content is 0.5 ~ 3g/L, TCr content is 0.5 ~ 5g/L, and its pH value is 0.5 ~ 4.0.
Such as, but be used in the present inventionly not limited thereto containing vanadium acidic solution, the lower limit that each impurity content is less than above-mentioned impurity content or the upper limit being greater than above-mentioned impurity content also can.
Table 1 shows the main chemical compositions containing vanadium acidic solution and pH value thereof that example 1 to 3 below uses.
The main chemical compositions containing vanadium acidic solution that table 1 example 1 to 3 uses and pH value thereof
Example 1
What this example adopted is the vanadium liquid of vanadium slag through calcification baking acidleach gained of vanadium-bearing hot metal vanadium extraction gained containing vanadium acidic solution, its main component and pH value as shown in table 1.
Add in the clean beaker of 2000mL in 1000mL table 1 containing vanadium acidic solution, adopt sulfuric acid to regulate pH value containing vanadium acidic solution to 0.2, then join in electrolyzer.Voltage stabilized source voltage is regulated to be 2V, add electrode and ion-exchange is touched, electrolysis 0.5h, takes out anolyte, and the pH value regulating anolyte with calcium oxide is 4, be heated to 50 DEG C, add 19.3g bodied ferric sulfate and carry out dephosphorization, after reaction 0.5h, after cold filtration, be mixed to get low-phosphorous vanadium liquid with catholyte, after testing, the phosphorus content in low-phosphorous vanadium liquid is less than 0.01g/L.
Example 2
This example adopt containing vanadium acidic solution be the vanadium liquid of vanadium liquid after treatment by extraction that extracting vanadium from stone coal acidolysis obtains, its main component and pH value as shown in table 1.
Add in the clean beaker of 2000mL in 1000mL table 1 containing vanadium acidic solution, adopt hydrochloric acid acid to regulate pH value containing vanadium acidic solution to 1.0, then join in electrolyzer.Voltage stabilized source voltage is regulated to be 10V, add electrode and ion-exchange is touched, electrolysis 2h, takes out anolyte, and the pH value regulating anolyte with sodium hydroxide is 1.5, be heated to 100 DEG C, add 57.9g polyaluminium sulfate, after reaction 2h, after cold filtration, be mixed to get low-phosphorous vanadium liquid with catholyte, after testing, the phosphorus content phosphorus in low-phosphorous vanadium liquid is less than 0.02g/L.
Example 3
What this example adopted is that thick vanadium product dissolves gained vanadium liquid containing vanadium acidic solution, its main component and pH value as shown in table 1.
Add in the clean beaker of 2000mL in 1000mL table 1 containing vanadium acidic solution, adopt nitric acid to regulate pH value containing vanadium acidic solution to 0.8, then join in electrolyzer.Voltage stabilized source voltage is regulated to be 8.0V, add electrode and ion-exchange is touched, electrolysis 2h, takes out anolyte, and the pH value regulating anolyte with calcium oxide is 3.0, heat value 70 DEG C, add 38.6g bodied ferric sulfate, after reaction 0.5h, after cold filtration, be mixed to get low-phosphorous vanadium liquid with catholyte, after testing, the phosphorus content in low-phosphorous vanadium liquid is less than 0.01g/L.
In sum, the method that the present invention adopts electrochemistry to combine with general chemistry carries out removing the phosphorus in acidic solution, and the clearance of phosphorus can reach 99%.In addition, present invention process is simple and easy to use, equipment requirements is low, easy to operate, wide accommodation, cost are low, has good Social benefit and economic benefit.
Although above by describing the present invention in conjunction with exemplary embodiment, it will be apparent to those skilled in the art that when not departing from the spirit and scope that claim limits, various amendment and change can be carried out to exemplary embodiment of the present invention.
Claims (7)
1. containing a method for vanadium acidic solution dephosphorization, it is characterized in that, described containing in vanadium acidic solution contains pentavalent vanadium and H
2pO
4 -, said method comprising the steps of:
Regulate pH value to 0.2 ~ 1 containing vanadium acidic solution;
To add electrolyzer containing vanadium acidic solution and carry out electrolysis, wherein, described electrolyzer is divided into cathode compartment and anolyte compartment by ion-exchange membrane;
Until described complete electromigration containing the ion of v element in vanadium acidic solution and the ion of phosphoric after, the anolyte in described anolyte compartment is shifted out in anolyte compartment, and adds dephosphorization agent and carry out dephosphorization;
Then, filter the anolyte after dephosphorization, and the catholyte in the anolyte obtained after filtration and described cathode compartment be mixed to get low-phosphorous vanadium liquid,
Wherein, the add-on of described dephosphorization agent and described be 1 ~ 5 containing the mol ratio of phosphorus content in vanadium acidic solution, the pH value that described dephosphorization step controls described anolyte is 1.5 ~ 4, temperature is 50 ~ 100 DEG C, and the reaction times of described dephosphorization step is 0.5 ~ 2h.
2. the method containing the dephosphorization of vanadium acidic solution according to claim 1, is characterized in that, described electrolysis step adopts voltage stabilized source and controls electrolysis voltage is 2 ~ 10V, and electrolysis time is 0.5 ~ 2h.
3. the method containing the dephosphorization of vanadium acidic solution according to claim 1, it is characterized in that, described dephosphorization agent is molysite and/or aluminium salt.
4. the method containing the dephosphorization of vanadium acidic solution according to claim 3, it is characterized in that, described dephosphorization agent is bodied ferric sulfate and/or polyaluminium sulfate.
5. the method containing the dephosphorization of vanadium acidic solution according to claim 1 and 2, is characterized in that, adopts the alkali of oxidizing acid or irreducibility to regulate described containing the pH value of vanadium acidic solution and the pH value of described anolyte.
6. the method containing the dephosphorization of vanadium acidic solution according to claim 1, it is characterized in that, described containing vanadium acidic solution be the vanadium liquid of vanadium slag through calcification baking acidleach gained of vanadium-bearing hot metal vanadium extraction gained, the vanadium liquid of the vanadium liquid that obtains of extracting vanadium from stone coal acidolysis after treatment by extraction or dissolve the vanadium liquid of gained for thick vanadium product.
7. the method containing the dephosphorization of vanadium acidic solution according to claim 1, is characterized in that, is describedly greater than 5g/L containing v element content in vanadium acidic solution.
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| CN104480308A (en) * | 2015-01-02 | 2015-04-01 | 重庆大学 | Dephosphorizing method for acid vanadium leached solution |
| CN107620090A (en) * | 2017-11-07 | 2018-01-23 | 攀钢集团攀枝花钢铁研究院有限公司 | The recovery method of vanadium and manganese in vanadium wastewater |
| CN109022786A (en) * | 2018-10-23 | 2018-12-18 | 攀钢集团研究院有限公司 | Except the method for silicon phosphorus in acid solution containing vanadium |
| CN109852820B (en) * | 2019-02-22 | 2021-11-30 | 湖南恒光科技股份有限公司 | Method for producing vanadium pentoxide |
| CN115679125B (en) * | 2022-10-08 | 2023-11-28 | 武汉科技大学 | Method for adjusting pH of vanadium-containing pickle liquor |
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| CN102051486A (en) * | 2010-11-12 | 2011-05-11 | 攀钢集团钢铁钒钛股份有限公司 | Method for preparing low-phosphorus vanadium liquid by using wastewater subjected to vanadium precipitation |
| CN102477493A (en) * | 2010-11-29 | 2012-05-30 | 攀钢集团钢铁钒钛股份有限公司 | Silicon-removing phosphorus-removing purifying method of sodium-modified vanadium-extraction leachate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051486A (en) * | 2010-11-12 | 2011-05-11 | 攀钢集团钢铁钒钛股份有限公司 | Method for preparing low-phosphorus vanadium liquid by using wastewater subjected to vanadium precipitation |
| CN102477493A (en) * | 2010-11-29 | 2012-05-30 | 攀钢集团钢铁钒钛股份有限公司 | Silicon-removing phosphorus-removing purifying method of sodium-modified vanadium-extraction leachate |
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