CN101343695A - Method for reducing content of kalium and sodium in vanadium solvent extraction circulation liquid - Google Patents
Method for reducing content of kalium and sodium in vanadium solvent extraction circulation liquid Download PDFInfo
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- CN101343695A CN101343695A CNA2008102130220A CN200810213022A CN101343695A CN 101343695 A CN101343695 A CN 101343695A CN A2008102130220 A CNA2008102130220 A CN A2008102130220A CN 200810213022 A CN200810213022 A CN 200810213022A CN 101343695 A CN101343695 A CN 101343695A
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- solvent extraction
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Abstract
The invention discloses a method for reducing the potassium and sodium content in a vanadium extraction leaching circulating liquid, which comprises the following steps: the pH value in the vanadium extraction leaching circulating liquid is adjusted with acid to maintain the vanadium extraction leaching circulating liquid within the acidic range; the vanadium extraction leaching circulating liquid is heated and stirred; when the vanadium extraction leaching circulating liquid reaches a reaction temperature, a potassium and sodium removing agent is added in the vanadium extraction leaching circulating liquid to make the potassium and sodium in the vanadium extraction leaching circulating liquid react with the potassium and sodium removing agent; and when the reaction is ended, the vanadium extraction leaching circulating liquid is filtrated.
Description
Technical field
The present invention relates to a kind of potassium in the vanadium solvent extraction circulation liquid, method of sodium content of reducing, relate in particular to a kind of potassium in low taste vanadium raw materials acidleach-ion-exchange circulation fluid, method of sodium content of reducing.
Background technology
At present, the vanadium product that the vanadium extraction of domestic low taste vanadium raw materials is obtained has occupied certain market share, and this has produced bigger influence to domestic vanadium output.Since comparatively serious when low taste vanadium raw materials is produced the vanadium product to the pollution of environment, be greatly limited so produce the vanadium product with low taste vanadium raw materials.In the problem of environmental pollution that production vanadium product causes, contaminated wastewater is wherein comparatively serious problem, and the waste water more than 90% is the surplus liquid of leach liquor after ion-exchange.When low taste vanadium raw materials adopted acidleach-ion exchange method to produce the vanadium product, the potassium in the solution, the enrichment of sodium content were to influence the one of the main reasons that the surplus liquid of ion-exchange recycles.
Potassium in the vanadium extraction leach liquor, sodium mainly contain two sources: potassium, sodium element that the low taste of first vanadium raw materials itself contains enter leach liquor in the process of acidleach, and it two is sodium elements that the sodium hydroxide that adds in the process of the impurity in removing leach liquor is introduced.When containing a large amount of potassium, sodium ion in the surplus liquid of ion-exchange, can't recycle because the viscosity of vanadium extraction leach liquor is too big; In addition, the vanadium extraction leach liquor that will contain a large amount of potassium, sodium ion directly discharges, and can cause problem of environmental pollution again.Therefore, need to remove potassium, sodium ion in the vanadium extraction leach liquor, perhaps reduce the potassium in the vanadium extraction leach liquor, the concentration of sodium ion, make its leaching that can circulate.
Summary of the invention
The present invention is directed to potassium in the vanadium solvent extraction circulation liquid, sodium content is too high and problem that solution that cause can not be recycled provides a kind of potassium in the vanadium solvent extraction circulation liquid, method of sodium content of reducing.This method can reduce potassium, the sodium content in the vanadium solvent extraction circulation liquid greatly, for the recycle of waste water provides favourable condition, has avoided the emission pollution problem of a large amount of vanadium extracting waste waters.
May further comprise the steps according to the potassium in the reduction vanadium solvent extraction circulation liquid of the present invention, the method for sodium content: the pH value with vanadium solvent extraction circulation liquid is regulated in acid makes vanadium solvent extraction circulation liquid in acid range; The heating vanadium solvent extraction circulation liquid also stirs; After vanadium solvent extraction circulation liquid reaches temperature of reaction, in vanadium solvent extraction circulation liquid, add to remove potassium, sodium agent, make in the vanadium solvent extraction circulation liquid potassium, sodium and remove potassium, the sodium agent is reacted; After reaction finishes, filter vanadium solvent extraction circulation liquid.
Aforesaid method is further comprising the steps of: the potassium in vanadium solvent extraction circulation liquid, sodium and remove potassium, sodium agent reaction and finish after, the pH value of vanadium solvent extraction circulation liquid is adjusted in 3.6～7.0 the scope, make excessive remove potassium, the sodium agent precipitates.
The method according to this invention before the heating vanadium solvent extraction circulation liquid, is adjusted to the pH value of vanadium solvent extraction circulation liquid with sulfuric acid in 1.5～2.3 the scope.
Preferably, described temperature of reaction is 90 a ℃～vanadium solvent extraction circulation liquid ebullient temperature.
The method according to this invention after vanadium solvent extraction circulation liquid reaches temperature of reaction, uses a kind of in calcium oxide, calcium hydroxide and the lime carbonate or their mixture the pH value of vanadium solvent extraction circulation liquid to be controlled in 1.4～1.9 the scope.
Preferably, describedly remove potassium, the sodium agent is the compound that contains iron ion; More preferably, describedly remove potassium, the sodium agent is a ferric sulfate.
The ratio of the potassium that contains in the amount of removing potassium, sodium agent that preferably, adds in vanadium solvent extraction circulation liquid and the vanadium solvent extraction circulation liquid, the amount of sodium is: remove potassium, the contained Fe of sodium agent
3+Molar weight and Na
+Or K
+The ratio of molar weight in 2.5～3.0 scope.
Preferably, the reaction times except that potassium, sodium is 60 minutes～120 minutes.
Description of drawings
Fig. 1 is the schema that illustrates according to the method for the potassium in the reduction vanadium solvent extraction circulation liquid of the present invention, sodium content.
Embodiment
The invention provides a kind of potassium in the vanadium solvent extraction circulation liquid, method of sodium content of reducing.With reference to Fig. 1, the potassium in the reduction vanadium solvent extraction circulation liquid of the present invention, the method for sodium content may further comprise the steps: the pH value with vanadium solvent extraction circulation liquid is regulated in acid makes vanadium solvent extraction circulation liquid in acid range; The heating vanadium solvent extraction circulation liquid also stirs; After vanadium solvent extraction circulation liquid reaches temperature of reaction, in vanadium solvent extraction circulation liquid, add to remove potassium, sodium agent, make in the vanadium solvent extraction circulation liquid potassium, sodium and remove potassium, the sodium agent is reacted; After reaction finishes, filter vanadium solvent extraction circulation liquid.
Preferably, may further comprise the steps according to the potassium in the reduction vanadium solvent extraction circulation liquid of the present invention, the method for sodium: the first step is adjusted in the pH value of vanadium solvent extraction circulation liquid with sulfuric acid in 1.5～2.3 the scope; In second step, the heating vanadium solvent extraction circulation liquid also stirs; The 3rd step, when vanadium solvent extraction circulation liquid reaches 90 ℃～solution ebullient temperature, add the potassium that removes that contains iron ion, the sodium agent, preferably remove potassium, the sodium agent is a ferric sulfate, wherein, the amount of the ferric sulfate that adds satisfies following equation, promptly, molar weight/the sodium ion of the iron ion that adds or molar weight=2.5～3.0 of potassium ion, after adding ferric sulfate, potassium in ferric sulfate and the vanadium solvent extraction circulation liquid, sodium reacts according to following equation, and in this reaction process, use calcium oxide, a kind of in calcium hydroxide and the lime carbonate or their mixture are controlled at the pH value of vanadium solvent extraction circulation liquid in 1.4～1.9 the scope, and entire reaction needs 60 minutes～120 minutes; The 4th step after reaction finishes, was adjusted to the pH value of solution in 3.6～7.0 the scope, made excessive ferric sulfate precipitate; The 5th step, filter vanadium solvent extraction circulation liquid, filtrate is returned extract technology reuse.
Equation
K
++3Fe
3++2SO
4 2-+6H
2O→KFe
3(SO
4)
2(OH)
6+6H
+
Na
++3Fe
3++2SO
4 2-+6H
2O→NaFe
3(SO
4)
2(OH)
6+6H
+
By aforesaid equation as can be known, potassium ion in the vanadium extraction leach liquor and the reaction of the ferric sulfate of adding generate the complex compound jarosite KFe that is insoluble in water
3[SO
4]
2(OH)
6Thereby, removed potassium ion in the vanadium extraction leach liquor by easily separating jarosite.
Based on similar principle, sodium ion in the vanadium extraction leach liquor and the reaction of the ferric sulfate of adding generate the yellow modumite NaFe of the complex compound that is insoluble in water
3[SO
4]
2(OH)
6Thereby, removed sodium ion in the vanadium extraction leach liquor by easily separating yellow modumite.
Below, by detailed example the present invention is described.
Example 1
Get the vanadium extraction leach liquor (Na in the solution of 1200mL
+Concentration is 20.7g/L, K
+Concentration is 3.1g/L, SO
4 2-Concentration is 34.2g/L), with the vitriol oil pH value of solution is adjusted to 1.7; Heating in water bath to 95 ℃ adds 580g ferric sulfate under stirring condition, and with calcium hydroxide the pH value of solution is controlled at 1.4～1.9; After the isothermal reaction 60 minutes, the pH value of solution is adjusted to 3.8; Filter, obtain filtrate 962mL.By analysis, the main component of filtrate is: Na
+Concentration be 2.4g/L, K
+Concentration be 0.3g/L, SO
4 2-Concentration 1.7g/L.Filtrate is returned extract technology and is recycled.
Example 2
Get the vanadium extraction leach liquor (Na in the solution of 1600mL
+Concentration is 34.5g/L, SO
4 2-Concentration is 53.1g/L), with the vitriol oil pH value of solution is adjusted to 2.2; Heating in water bath to 92 ℃ adds 1290g ferric sulfate under stirring condition, and with calcium hydroxide the pH value of solution is controlled at 1.4～1.9; After the isothermal reaction 120 minutes, the pH value of solution is adjusted to 6.0; Filter, obtain filtrate 1076mL.By analysis, the main component of filtrate is: Na
+Concentration be 2.7g/L, SO
4 2-Concentration 0.3g/L.Filtrate is returned extract technology and is recycled.
Example 3
Get the vanadium extraction leach liquor (Na in the solution of 2000mL
+Concentration is 30.8g/L, SO
4 2-Concentration is 49.8g/L), with the vitriol oil pH value of solution is adjusted to 2.0; Heating in water bath to 95 ℃ adds 1550g ferric sulfate under stirring condition, and with calcium hydroxide the pH value of solution is controlled at 1.4～1.9; After the isothermal reaction 90 minutes, the pH value of solution is adjusted to 4.0; Filter, obtain filtrate 1320mL.By analysis, the main component of filtrate is: Na
+Concentration be 2.5g/L, SO
4 2-Concentration 1.5g/L.Filtrate is returned extract technology and is recycled.
Example 4
Get the vanadium extraction leach liquor (Na in the solution of 2000mL
+Concentration is 20.7g/L, K
+Concentration is 3.1g/L, SO
4 2-Concentration is 34.2g/L), with the vitriol oil pH value of solution is adjusted to 1.5; Heating in water bath to 90 ℃ adds 970g ferric sulfate under stirring condition, and with calcium oxide the pH value of solution is controlled at 1.4～1.9; After the isothermal reaction 80 minutes, the pH value of solution is adjusted to 3.6; Filter, obtain filtrate 1460mL.By analysis, the main component of filtrate is: Na
+Concentration be 2.2g/L, K
+Concentration be 0.3g/L, SO
4 2-Concentration 1.6g/L.Filtrate is returned extract technology and is recycled.
Example 5
Get the vanadium extraction leach liquor (Na in the solution of 2000mL
+Concentration is 30.8g/L, SO
4 2-Concentration is 49.8g/L), with the vitriol oil pH value of solution is adjusted to 2.3; Heating in water bath to solution seethes with excitement, and adds 1450g ferric sulfate under stirring condition, and with calcium hydroxide the pH value of solution is controlled at 1.4～1.9; After the isothermal reaction 60 minutes, the pH value of solution is adjusted to 7.0; Filter, obtain filtrate 1350mL.By analysis, the main component of filtrate is: Na
+Concentration be 2.9g/L, SO
4 2-Concentration 1.5g/L.Filtrate is returned extract technology and is recycled.
Clearly show that effect in the table 1 below according to the method for potassium, sodium content in the reduction vanadium solvent extraction circulation liquid of the present invention.
Table 1
| Potassium content (g/L) before the reaction in the solution | Potassium content (g/L) in the solution of reaction back | Potassium reduces ratio (%) | Sodium content (g/L) before the reaction in the solution | Sodium content (g/L) in the solution of reaction back | Sodium reduces ratio (%) | |
| Example 1 | 3.1 | 0.3 | 90.3 | 20.7 | 2.4 | 88.4 |
| Example 2 | - | - | - | 34.5 | 2.7 | 92.2 |
| Example 3 | - | - | - | 30.8 | 2.5 | 91.9 |
| Example 4 | 3.1 | 0.3 | 90.3 | 20.7 | 2.2 | 89.4 |
| Example 5 | - | - | - | 30.8 | 2.9 | 90.6 |
From top table 1 as can be seen, by the potassium in the reduction vanadium solvent extraction circulation liquid according to the present invention, the method for sodium, the potassium, the sodium content that contain in the solution obviously reduce, make the vanadium extraction leach liquor to be recycled, solved the contaminated wastewater problem of environment that produces in the low taste vanadium raw materials vanadium extraction process.
Claims (9)
1, a kind of potassium in the vanadium solvent extraction circulation liquid, method of sodium content of reducing, this method may further comprise the steps:
PH value with vanadium solvent extraction circulation liquid is regulated in acid makes vanadium solvent extraction circulation liquid in acid range;
The heating vanadium solvent extraction circulation liquid also stirs;
After vanadium solvent extraction circulation liquid reaches temperature of reaction, in vanadium solvent extraction circulation liquid, add to remove potassium, sodium agent, make in the vanadium solvent extraction circulation liquid potassium, sodium and remove potassium, the sodium agent is reacted;
After reaction finishes, filter vanadium solvent extraction circulation liquid.
2, method according to claim 1, described method is further comprising the steps of: the potassium in vanadium solvent extraction circulation liquid, sodium and remove potassium, sodium agent reaction and finish after, the pH value of vanadium solvent extraction circulation liquid is adjusted in 3.6～7.0 the scope, makes excessive potassium, the sodium agent precipitation removed.
3, method according to claim 1 wherein, before the heating vanadium solvent extraction circulation liquid, is adjusted to the pH value of vanadium solvent extraction circulation liquid with sulfuric acid in 1.5～2.3 the scope.
4, method according to claim 1, wherein, described temperature of reaction is 90 a ℃～vanadium solvent extraction circulation liquid ebullient temperature.
5, method according to claim 1, wherein, after vanadium solvent extraction circulation liquid reaches temperature of reaction, use a kind of in calcium oxide, calcium hydroxide and the lime carbonate or their mixture the pH value of vanadium solvent extraction circulation liquid to be controlled in 1.4～1.9 the scope.
6, method according to claim 1 wherein, is describedly removed potassium, the sodium agent is the compound that contains iron ion.
7, method according to claim 6 wherein, is describedly removed potassium, the sodium agent is a ferric sulfate.
8, method according to claim 1, wherein, the ratio of the potassium that contains in the amount of removing potassium, sodium agent that adds in vanadium solvent extraction circulation liquid and the vanadium solvent extraction circulation liquid, the amount of sodium is: remove potassium, the contained Fe of sodium agent
3+Molar weight and Na
+Or K
+The ratio of molar weight in 2.5～3.0 scope.
9, method according to claim 1, wherein, the reaction times of removing potassium, sodium is 60 minutes～120 minutes.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102130220A CN101343695A (en) | 2008-08-20 | 2008-08-20 | Method for reducing content of kalium and sodium in vanadium solvent extraction circulation liquid |
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|---|---|---|---|
| CNA2008102130220A CN101343695A (en) | 2008-08-20 | 2008-08-20 | Method for reducing content of kalium and sodium in vanadium solvent extraction circulation liquid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950999A (en) * | 2014-03-28 | 2014-07-30 | 北京中凯宏德科技有限公司 | Sodium sulfate-containing wastewater sodium removal method |
| CN107739826A (en) * | 2017-10-31 | 2018-02-27 | 成都先进金属材料产业技术研究院有限公司 | A kind of method of the reduction containing sodium content in vanadium leachate |
| CN108675498A (en) * | 2018-05-25 | 2018-10-19 | 中国科学院过程工程研究所 | A kind of method of bone coal acid waste water recycling |
| CN109336138A (en) * | 2018-12-21 | 2019-02-15 | 中国科学院过程工程研究所 | The separation method of potassium sodium in a kind of mixed sulfate containing potassium and sodium |
| CN109881019A (en) * | 2019-04-25 | 2019-06-14 | 河钢股份有限公司承德分公司 | A kind of method of resource utilization desulfurization slag containing vanadium |
-
2008
- 2008-08-20 CN CNA2008102130220A patent/CN101343695A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950999A (en) * | 2014-03-28 | 2014-07-30 | 北京中凯宏德科技有限公司 | Sodium sulfate-containing wastewater sodium removal method |
| CN107739826A (en) * | 2017-10-31 | 2018-02-27 | 成都先进金属材料产业技术研究院有限公司 | A kind of method of the reduction containing sodium content in vanadium leachate |
| CN108675498A (en) * | 2018-05-25 | 2018-10-19 | 中国科学院过程工程研究所 | A kind of method of bone coal acid waste water recycling |
| CN108675498B (en) * | 2018-05-25 | 2021-04-06 | 中国科学院过程工程研究所 | Method for resource utilization of stone coal acidic wastewater |
| CN109336138A (en) * | 2018-12-21 | 2019-02-15 | 中国科学院过程工程研究所 | The separation method of potassium sodium in a kind of mixed sulfate containing potassium and sodium |
| CN109336138B (en) * | 2018-12-21 | 2020-11-10 | 中国科学院过程工程研究所 | Method for separating potassium and sodium in mixed sulfate containing potassium and sodium |
| CN109881019A (en) * | 2019-04-25 | 2019-06-14 | 河钢股份有限公司承德分公司 | A kind of method of resource utilization desulfurization slag containing vanadium |
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Open date: 20090114 |