CN102477493B - Silicon-removing phosphorus-removing purifying method of sodium-modified vanadium-extraction leachate - Google Patents
Silicon-removing phosphorus-removing purifying method of sodium-modified vanadium-extraction leachate Download PDFInfo
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- CN102477493B CN102477493B CN201010572694.8A CN201010572694A CN102477493B CN 102477493 B CN102477493 B CN 102477493B CN 201010572694 A CN201010572694 A CN 201010572694A CN 102477493 B CN102477493 B CN 102477493B
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Abstract
The invention provides a silicon-removing phosphorus-removing purifying method of a sodium-modified vanadium-extraction leachate. With the method, the phosphorus removing effect is good, and the loss of vanadium is low. The method comprises a step that: the sodium-modified vanadium-extraction leachate contacts soluble magnesium salt, ammonium salt and soluble aluminum salt. With the silicon-removing phosphorus-removing purifying method provided by the invention, the content of phosphorus element in the sodium-modified vanadium-extraction leachate can be reduced to a value below 0.015g/L. The silicon-removing effect is even better, where in the content of silicon element can be reduced to a value below 0.15g/L. Also, the vanadium loss percentage of the purified vanadium-extraction leachate is lower than 0.3wt%.
Description
Technical field
The present invention relates to a kind of silica removal removing phosphorus-removing purifying method of sodium vanadium extraction leach liquor.
Background technology
At present in the world most of vanadium manufacturing enterprise take vanadium titano-magnetite as raw material, obtain thick vanadium slag by blast furnace/converter process, thick Leaching of Vanadium from Vanadium slag adopts sodium process for extracting vanadium conventionally: mainly take sodium carbonate as the thick vanadium slag of roasting additive roasting, product of roasting adopts water logging to obtain vanadium extraction leach liquor, remove after the impurity such as phosphorus and silicon, add ammonium salt, Precipitation ammonium poly-vanadate under acidic conditions, then utilizes ammonium poly-vanadate to produce subsequent product.Phosphorus in vanadium extraction leach liquor and silicon are the important factors that affects precipitation yield and ammonium poly-vanadate quality product, therefore in process of production, conventionally to carry out purifying treatment (dephosphorization, silica removal) to leach liquor, after processing, reach leach liquor phosphorus element content and be less than 0.015g/L, the content of element silicon is less than 0.15g/L.
Tradition vanadium extraction leach liquor phosphorus and silicon removing technique is to adopt CaCl
2solution carries out phosphorus and silicon removing, and being mainly to provide and controlling pH is 8-9, makes phosphorus generate calcium phosphate, destroys colloid simultaneously and makes calcium phosphate suspended substance flocculation sediment to accelerate clarifying speed, therefore CaCl
2solution is fairly simple effective scavenging agent.But calcium chloride adds the loss that too much can form vanadic acid calcium deposit and cause vanadium, and sodium vanadium extraction pH of leaching solution is conventionally between 10-11, and within the scope of this pH value, calcium chloride can be hydrolyzed generation calcium hydroxide, causes calcium chloride consumption large, and affects phosphor-removing effect.
For example patent of invention CN 1298872C proposes to be made into dephosphorization scavenging solution with crystal aluminum chloride and crystallization calcium chloride according to certain weight ratio, adds containing in vanadium leachate, adds polyacrylamide solution to flocculate after reaction, then carries out solid-liquid separation with sheet frame.The method technique is simple, and phosphorus and silicon removing is more complete, but has the defect that vanadium rate of loss is larger.
Summary of the invention
In order to overcome the defect of the existing silica removal removing phosphorus-removing purifying method containing vanadium leachate, the invention provides the silica removal removing phosphorus-removing purifying method of the effective and sodium vanadium extraction leach liquor that vanadium loss is less of a kind of phosphorus and silicon removing.
According to the silica removal removing phosphorus-removing purifying method of sodium vanadium extraction leach liquor provided by the present invention, the method comprises: described sodium vanadium extraction leach liquor is contacted with solubility magnesium salts, ammonium salt and aluminum soluble salt.
Silica removal removing phosphorus-removing purifying method provided by the invention, can be reduced to the content of phosphoric in sodium vanadium extraction leach liquor below 0.015g/L, has better silica removal effect simultaneously, and the content of element silicon can be reduced to below 0.15g/L.And can make the vanadium rate of loss of the vanadium extraction leach liquor after purification lower than 0.3 % by weight.
Embodiment
According to the silica removal removing phosphorus-removing purifying method of sodium vanadium extraction leach liquor provided by the present invention, the method comprises: described sodium vanadium extraction leach liquor is contacted with solubility magnesium salts, ammonium salt and aluminum soluble salt.
Wherein, described sodium vanadium extraction leach liquor can be the leach liquor obtaining in sodium process for extracting vanadium, and particularly, mainly take sodium carbonate as the thick vanadium slag of roasting additive roasting, then water impregnation-calcination product obtains vanadium extraction leach liquor.Described roasting and dipping all carry out according to method well known in the art.
Before silica removal dephosphorization purifies, in described sodium vanadium extraction leach liquor, contain more phosphoric and element silicon, the content of phosphoric can be 0.03-0.05g/L, the content of element silicon can be 0.5-1.5g/L.Meanwhile, the pH value of described sodium vanadium extraction leach liquor can be 10-11; Within the scope of this pH, phosphoric generally exists with the form of phosphate anion, and element silicon generally exists with the form of silicate ion.
According to method provided by the present invention, described contact can be carried out according to method well known in the art, for example, is specifically as follows sodium vanadium extraction leach liquor and solubility magnesium salts, ammonium salt and aluminum soluble salt are uniformly mixed.
The present invention does not have special requirement to sodium vanadium extraction leach liquor with the order that solubility magnesium salts, ammonium salt and aluminum soluble salt contact, can be selected from contact simultaneously, also can be respectively by random order contact, if described sodium vanadium extraction leach liquor is first contacted with the mixture of solubility magnesium salts and ammonium salt, contact with aluminum soluble salt again, can shorten the time of purification, therefore the present invention preferably first contacts with solubility magnesium salts described sodium vanadium extraction leach liquor with ammonium salt, then contacts with aluminum soluble salt.
The present invention has no particular limits the temperature and time of contact, those skilled in the art can select arbitrarily, in order to enhance productivity under the prerequisite guaranteeing fully purification, in the time that sodium vanadium extraction leach liquor contacts with solubility magnesium salts, ammonium salt and aluminum soluble salt simultaneously, preferably the temperature of contact is 50-90 ℃, and the total time of contact is 480-820 minute.
When the present invention preferably first contacts described sodium vanadium extraction leach liquor with the mixture of solubility magnesium salts and ammonium salt, while contact with aluminum soluble salt again, described sodium vanadium extraction leach liquor first contacts 120-180 minute with ammonium salt with solubility magnesium salts at 50-90 ℃, then at 50-90 ℃, contacts 160-240 minute with aluminum soluble salt.After can in advance solubility magnesium salts being mixed with ammonium salt, contact with described sodium vanadium extraction leach liquor, also can directly solubility magnesium salts be contacted with described sodium vanadium extraction leach liquor with ammonium salt without mixing.
Method provided by the present invention can make phosphoric and the content of element silicon in the sodium vanadium extraction leach liquor after contact reduce, in order to improve the efficiency that purifies rear leach liquor vanadium extraction, under preferable case, the condition of contact makes the content of phosphoric in the sodium vanadium extraction leach liquor after contact be less than 0.015g/L, and the content of element silicon is less than 0.15g/L.
In order to meet the condition of above-mentioned contact, with respect to the phosphoric of 1 mole in sodium vanadium extraction leach liquor, in magnesium ion, the consumption of solubility magnesium salts can be 5-20 mole, is preferably 10-15 mole; In ammonium ion, the consumption of ammonium salt can be 10-30 mole, is preferably 15-20 mole; With respect to the element silicon of 1 mole in sodium vanadium extraction leach liquor; In aluminum ion, the consumption of aluminum soluble salt can be 0.5-2.0 mole, is preferably 1-1.5 mole.
The effect of the present invention's solubility magnesium salts used is to provide magnesium ion, therefore the selection of solubility magnesium salts is not had to special requirement, consider the being easy to get property of raw material, preferred described solubility magnesium salts is selected from but is not limited to one or more in magnesium sulfate, magnesium chloride and magnesium nitrate.
The effect of the present invention's ammonium salt used is to provide ammonium ion, therefore the selection of ammonium salt is not had to special requirement, consider the being easy to get property of raw material, preferred described ammonium salt is selected from but is not limited to one or more in ammonium sulfate, volatile salt, bicarbonate of ammonia, ammonium chloride and ammonium nitrate.
The effect of the present invention's aluminum soluble salt used is to provide aluminum ion, therefore the selection of aluminum soluble salt is not had to special requirement, consider the being easy to get property of raw material, preferred described aluminum soluble salt is selected from but is not limited to one or more in Tai-Ace S 150, aluminum chloride and aluminum nitrate.
Because the vanadium extraction leach liquor after method purification provided by the present invention is used in follow-up ammonium salt precipitation technique, and ammonium salt used is generally ammonium sulfate in ammonium salt precipitation technique, therefore in order not introduce hetero-ion, particularly preferably described solubility magnesium salts is Tai-Ace S 150, described ammonium salt is ammonium sulfate, described aluminum soluble salt is Tai-Ace S 150, and under this optimal way, the corrodibility minimum of the vanadium extraction leach liquor after purification to equipment.
According to method provided by the present invention, wherein, described solubility magnesium salts, ammonium salt and aluminum soluble salt can contact with vanadium extraction leach liquor with the form of solid or the aqueous solution, the consumption of also simultaneously saving water in order to reach best dispersion effect, preferred described solubility magnesium salts, ammonium salt and aluminum soluble salt all contact with vanadium extraction leach liquor with the form of saturated aqueous solution.
In the present invention, the content of various elements is measured according to the method for SL394-2007 " mensuration of 34 kinds of elements such as lead, cadmium, vanadium, phosphorus " regulation.
In the present invention, the volume of liquid is 20 ℃, the numerical value that 1 standard atmosphere is depressed.
In the present invention, described vanadium rate of loss is the per-cent that the difference of the total amount of vanadium in the leach liquor before and after purifying accounts for the total amount of vanadium in the leach liquor before purification.
Further illustrate by the following examples method provided by the present invention, but scope of the present invention is not limited in embodiment.In following examples, sodium vanadium extraction leach liquor derives from v-bearing steel slag sodium roasting-water logging operation, specifically obtain by the method in CN101649397A containing vanadium leachate.
Embodiment 1
The present embodiment is for illustrating the silica removal removing phosphorus-removing purifying method of sodium vanadium extraction leach liquor provided by the present invention.
Sodium vanadium extraction leach liquor ([V] is 30g/L, and [P] is 0.05g/L, and [Si] is 1.5g/L) is heated to 90 ℃, then according to NH
4 +: Mg: P=20: the mol ratio of 15: 1, magnesium sulfate and ammonium sulfate are made into respectively to saturated solution and mix after add in vanadium extraction leach liquor, stir, react 180 minutes, obtain suspension liquid, in this suspension liquid, according to Al: Si=1.5: 1 mol ratio adds Tai-Ace S 150 saturated solution, fully stir, then leave standstill after 240 minutes and filter, obtain cleaner liquid, the concentration that records phosphoric in cleaner liquid is 0.008g/L, the concentration of element silicon is 0.05g/L, and vanadium rate of loss is 0.18 % by weight.
Comparative example 1
By sodium vanadium extraction leach liquor, ([V] is 30g/L, [P] is 0.05g/L, [Si] is 1.5g/L) be heated to 90 ℃, then according to Mg: P=15: 1 mol ratio, magnesium sulfate is made into saturated solution to add in vanadium extraction leach liquor, stir, react 180 minutes, obtain suspension liquid, in this suspension liquid, according to Al: Si=1.5: 1 mol ratio adds Tai-Ace S 150 saturated solution, fully stir, then leave standstill after 240 minutes and filter, obtain cleaner liquid, the concentration that records phosphoric in cleaner liquid is 0.028g/L, the concentration of element silicon is 0.05g/L, vanadium rate of loss is 0.19 % by weight.
Comparative example 2
By sodium vanadium extraction leach liquor, ([V] is 30g/L, [P] is 0.05g/L, [Si] is 1.5g/L) be heated to 90 ℃, then according to Ca: P=15: 1 mol ratio, calcium chloride is made into saturated solution to add in vanadium extraction leach liquor, stir, react 180 minutes, obtain suspension liquid, in this suspension liquid, according to Al: Si=1.5: 1 mol ratio adds aluminum chloride saturated solution, fully stir, then leave standstill after 240 minutes and filter, obtain cleaner liquid, the concentration that records phosphoric in cleaner liquid is 0.07g/L, the concentration of element silicon is 0.05g/L, vanadium rate of loss is 0.66 % by weight.
Comparative example 3
Sodium vanadium extraction leach liquor ([V] is 30g/L, and [P] is 0.05g/L, and [Si] is 1.5g/L) is heated to 90 ℃, then according to NH
4 +: Mg: P=20: the mol ratio of 15: 1, magnesium sulfate and ammonium sulfate are made into respectively to saturated solution and mix after add in vanadium extraction leach liquor, stir, react after 180 minutes and filter, obtain cleaner liquid, the concentration that records phosphoric in cleaner liquid is 0.09g/L, and the concentration of element silicon is 1.08g/L, and vanadium rate of loss is 0.18 % by weight.
Embodiment 2
The present embodiment is for illustrating the silica removal removing phosphorus-removing purifying method of sodium vanadium extraction leach liquor provided by the present invention.
Sodium vanadium extraction leach liquor ([V] is 20g/L, and [P] is 0.03g/L, and [Si] is 0.5g/L) is heated to 60 ℃, then according to NH
4 +: Mg: P=15: the mol ratio of 10: 1, magnesium sulfate and ammonium sulfate are made into respectively to saturated solution and mix after add in vanadium extraction leach liquor, stir, react 120 minutes, obtain suspension liquid, in this suspension liquid, according to Al: Si=1.0: 1 mol ratio adds Tai-Ace S 150 saturated solution, fully stir, then leave standstill after 160 minutes and filter, obtain cleaner liquid, the concentration that records phosphoric in cleaner liquid is 0.012g/L, the concentration of element silicon is 0.13g/L, and vanadium rate of loss is 0.2 % by weight.
Embodiment 3
The present embodiment is for illustrating the silica removal removing phosphorus-removing purifying method of sodium vanadium extraction leach liquor provided by the present invention.
Sodium vanadium extraction leach liquor ([V] is 22g/L, and [P] is 0.035g/L, and [Si] is 0.8g/L) is heated to 70 ℃, then according to NH
4 +: Mg: P=17: the mol ratio of 12: 1, magnesium sulfate and ammonium sulfate are made into respectively to saturated solution and mix after add in vanadium extraction leach liquor, stir, react 140 minutes, obtain suspension liquid, in this suspension liquid, according to Al: Si=1.2: 1 mol ratio adds Tai-Ace S 150 saturated solution, fully stir, then leave standstill after 180 minutes and filter, obtain cleaner liquid, the concentration that records phosphoric in cleaner liquid is 0.009g/L, the concentration of element silicon is 0.08g/L, and vanadium rate of loss is 0.15 % by weight.
Embodiment 4
The present embodiment is for illustrating the silica removal removing phosphorus-removing purifying method of sodium vanadium extraction leach liquor provided by the present invention.
Sodium vanadium extraction leach liquor ([V] is 30g/L, and [P] is 0.05g/L, and [Si] is 1.5g/L) is heated to 90 ℃, then according to NH
4 +: Mg: P=20: the mol ratio of 15: 1, magnesium nitrate and bicarbonate of ammonia are made into respectively to saturated solution and mix after add in vanadium extraction leach liquor, stir, react 180 minutes, obtain suspension liquid, in this suspension liquid, according to Al: Si=1.5: 1 mol ratio adds aluminum nitrate saturated solution, fully stir, then leave standstill after 240 minutes and filter, obtain cleaner liquid, the concentration that records phosphoric in cleaner liquid is 0.013g/L, the concentration of element silicon is 0.11g/L, and vanadium rate of loss is 0.28 % by weight.
Embodiment 5
The present embodiment is for illustrating the silica removal removing phosphorus-removing purifying method of sodium vanadium extraction leach liquor provided by the present invention.
Sodium vanadium extraction leach liquor ([V] is 30g/L, and [P] is 0.05g/L, and [Si] is 1.5g/L) is heated to 90 ℃, then according to NH
4 +: Mg: P=20: the mol ratio of 15: 1, magnesium chloride and ammonium chloride are made into respectively to saturated solution and mix after add in vanadium extraction leach liquor, stir, react 180 minutes, obtain suspension liquid, in this suspension liquid, according to Al: Si=1.5: 1 mol ratio adds aluminum chloride saturated solution, fully stir, then leave standstill after 240 minutes and filter, obtain cleaner liquid, the concentration that records phosphoric in cleaner liquid is 0.014g/L, the concentration of element silicon is 0.12g/L, and vanadium rate of loss is 0.29 % by weight.
According to the result of embodiment 1-5 and comparative example 1-3, silica removal removing phosphorus-removing purifying method provided by the invention, can be reduced to the content of phosphoric in sodium vanadium extraction leach liquor below 0.015g/L, and the content of element silicon is reduced to below 0.15g/L.And can make the vanadium rate of loss of the vanadium extraction leach liquor after purification lower than 0.3 % by weight.
Claims (7)
1. the silica removal removing phosphorus-removing purifying method of a sodium vanadium extraction leach liquor, the method comprises: described sodium vanadium extraction leach liquor is first contacted to 120-180 minute with the mixture of solubility magnesium salts and ammonium salt at 50-90 ℃, then at 50-90 ℃, contact 160-240 minute with aluminum soluble salt; With respect to the phosphoric of 1 mole in sodium vanadium extraction leach liquor, in magnesium ion, the consumption of solubility magnesium salts is 5-20 mole; In ammonium ion, the consumption of ammonium salt is 10-30 mole; With respect to the element silicon of 1 mole in sodium vanadium extraction leach liquor; In aluminum ion, the consumption of aluminum soluble salt is 0.5-2.0 mole.
2. method according to claim 1, wherein, the condition of contact makes the content of phosphoric in the sodium vanadium extraction leach liquor after contact be less than 0.015g/L, and the content of element silicon is less than 0.15g/L.
3. method according to claim 1 and 2, wherein, described solubility magnesium salts is selected from one or more in magnesium sulfate, magnesium chloride and magnesium nitrate.
4. method according to claim 1 and 2, wherein, described ammonium salt is selected from one or more in ammonium sulfate, volatile salt, bicarbonate of ammonia, ammonium chloride and ammonium nitrate.
5. method according to claim 1 and 2, wherein, described aluminum soluble salt is selected from one or more in Tai-Ace S 150, aluminum chloride and aluminum nitrate.
6. method according to claim 1 and 2, wherein, described solubility magnesium salts is magnesium sulfate, and described ammonium salt is ammonium sulfate, and described aluminum soluble salt is Tai-Ace S 150.
7. method according to claim 1, wherein, in described sodium vanadium extraction leach liquor, the content of phosphoric is 0.03-0.05g/L, the content of element silicon is 0.5-1.5g/L.
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| CN103966437B (en) * | 2014-05-14 | 2015-11-11 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method containing the dephosphorization of vanadium acidic solution |
| CN104480308A (en) * | 2015-01-02 | 2015-04-01 | 重庆大学 | Dephosphorizing method for acid vanadium leached solution |
| CN106145188A (en) * | 2016-07-05 | 2016-11-23 | 河北钢铁股份有限公司承德分公司 | A kind of method that sodium vanadium extraction liquid prepares V electrolyte high purity vanadic anhydride |
| 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 |
| CN109319910B (en) * | 2018-11-05 | 2022-06-03 | 博天环境集团股份有限公司 | Composite medicament for removing silicon by mine water evaporation crystallization water inflow and application thereof |
| CN110423890B (en) * | 2019-08-28 | 2021-06-18 | 重庆大学 | Method for deeply removing phosphorus in acidic vanadium extraction solution |
| CN113481389A (en) * | 2021-06-02 | 2021-10-08 | 四川星明能源环保科技有限公司 | Method for removing phosphorus from vanadium-containing solution with high phosphorus content |
| CN114315196B (en) * | 2021-11-23 | 2023-01-24 | 攀钢集团研究院有限公司 | Method for recovering silicon-phosphorus thermal insulation material from alkaline vanadium-containing liquid |
| CN115976341B (en) * | 2022-12-30 | 2023-07-25 | 四川省银河化学股份有限公司 | Method for removing silicon and phosphorus in vanadium slag sodium roasting production system |
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