CN102897834A - Vanadium-precipitating method and preparation method for vanadium pentoxide - Google Patents
Vanadium-precipitating method and preparation method for vanadium pentoxide Download PDFInfo
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- CN102897834A CN102897834A CN2011102157032A CN201110215703A CN102897834A CN 102897834 A CN102897834 A CN 102897834A CN 2011102157032 A CN2011102157032 A CN 2011102157032A CN 201110215703 A CN201110215703 A CN 201110215703A CN 102897834 A CN102897834 A CN 102897834A
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Abstract
The invention provides a vanadium-precipitating method. The method comprises the steps of heating an acidic vanadium acid radical ion solution in a sealing condition, with a heating temperature of 90-250 DEG C and heating time of 0.5-5 h. The invention also provides a preparation method for vanadium pentoxide. The preparation method employs the vanadium-precipitating method provided by the invention to precipitate the acidic vanadium acid radical ions, and bakes the obtained solid from vanadium precipitation after the solid is dried. Compared hydrolysis vanadium precipitation in a conventional vanadium-precipitating process, the method provided by the invention has easily realizable vanadium precipitation conditions, high vanadium precipitation rate and fast vanadium precipitation speed. Compared with a vanadium precipitation by ammonium salts, the method provided by the invention reduces difficult-to-be treated salt content in precipitation waste water, has important environmental significance, can complete the vanadium precipitation process with no need of adding the ammonium salts, and reduces cost. The vanadium-precipitating method provided by the invention is simple in process and can be widely used for industrial production.
Description
Technical field
The present invention relates to a kind of method of precipitation and the preparation method of the Vanadium Pentoxide in FLAKES of the method that comprises this precipitation.
Background technology
Precipitation mainly contains hydrolysis precipitation method and two kinds of methods of ammonium salt precipitation method.
Hydrolysis precipitation method is that sodium vanadate solution is along with the solution acidic increase progressively is hydrolyzed, generate the process of many vanadic acid sodiums, this is the industrial method of using the earliest, the method is to add hot sulfuric acid in sodium vanadate solution, regulate the pH value to 1.7-1.9, be settled out many vanadic acid sodiums of reddish-brown under the condition of heated and boiled and stirring, the method precipitation condition is harsh, need to expend the pH value that a large amount of acid just can reach 1.7-1.9, and the precipitation rate is lower.
Therefore, precipitation method commonly used is ammonium salt precipitation method in the present industrial production.Namely add water miscible ammonium salt in the vanadium leachate to containing under certain condition, comprise ammonium chloride, ammonium sulfate and ammonium nitrate etc., vanadium is separated out from solution with ammonium meta-vanadate or ammonium poly-vanadate form.Then through calcining to get V
2O
5Difference according to the pH value of precipitation, ammonium salt precipitation method can be divided into the precipitation of weakly alkaline ammonium salt, the precipitation of slightly acidic ammonium salt and highly acid ammonium salt precipitation, but the interior the most frequently used ammonium salt precipitation technique of world wide mainly contains weakly alkaline ammonium salt precipitation technique and highly acid ammonium salt precipitation technique at present.
Weakly alkaline ammonium salt precipitation method generates ammonium meta-vanadate (NH based on weakly alkaline metavanadate solution and ammonium salt effect
4VO
3) reaction, and crystallization at low temperatures is so this method claims again ammonium meta-vanadate precipitation method.PH=8～9 o'clock, the vanadium in the solution mainly (is reduced to VO with the metavanadic acid root
3 -) the form existence.When in vanadium solution, adding water miscible ammonium salt, replacement(metathesis)reaction will occur, generate ammonium meta-vanadate, the solubleness of ammonium meta-vanadate sharply reduces and crystallization at low temperatures.The precipitin reaction of weakly alkaline ammonium salt precipitation method is chronic; High ammonium salt consumption is conducive to the abundant Precipitation of vanadium.
Highly acid ammonium salt precipitation technique is that vanadate solution is added acid for adjusting pH value 2.0-2.5, then adds water miscible ammonium salt, and at high temperature precipitation generates saffron ammonium poly-vanadate ((NH
4)
2V
6O
16) precipitation.This technique and ammonium meta-vanadate precipitated phase ratio, the ammonium salt consumption that needs is lower, but needs higher service temperature.
In the ammonium salt precipitation process, except generating the ammonium vanadate precipitation, also generated simultaneously a large amount of salinities, such as ammonium sulfate etc., the salinity of generation enters in the precipitation waste water, and environmental pollution is serious, brought great difficulty for the processing of waste water, and the ammonium consumption is also larger, energy consumption is high.
Summary of the invention
The objective of the invention is in order to overcome the precipitation condition harshness of hydrolysis precipitation in the existing precipitation technique, the precipitation waste water of ammonium salt precipitation contains the salinities such as ammonium sulfate, and waste water is difficult to process, and the defective that environmental pollution is serious provides a kind of new precipitation method.
The present inventor is unexpected the discovery under study for action, in confined conditions with acidic conditions under, improve the temperature of vanadic acid radical ion solution to 90-250 ℃, the vanadium hydrolytic precipitation is separated out with the form of vanadate.Therefore, to achieve these goals, the invention provides a kind of method of precipitation, it is characterized in that, the method comprises carries out heat treated in confined conditions with acid vanadic acid radical ion solution, and the temperature of heat treated is 90-250 ℃, and the time is 0.5-5h.
The method of precipitation provided by the invention, if in confined conditions with acidic conditions under, under 90-250 ℃ of temperature, carry out, can realize precipitation, with in the existing precipitation technique hydrolysis precipitation compare, the precipitation condition easily realizes; The precipitation rate is high, and precipitation speed is fast; The inventive method is compared with ammonium salt precipitation method, has reduced the salt content that is difficult to process in the precipitation waste water, has important environment protection significance, and need not add ammonium salt and can finish the precipitation process, has reduced cost; The method of precipitation provided by the invention, technique is simple, can be widely used in industrial production.
Other features and advantages of the present invention will partly be described in detail in embodiment subsequently.
Embodiment
Below the specific embodiment of the present invention is elaborated.Should be understood that, embodiment described herein only is used for description and interpretation the present invention, is not limited to the present invention.
On the one hand, the invention provides a kind of method of precipitation, the method comprises carries out heat treated in confined conditions with acid vanadic acid radical ion solution, and the temperature of heat treated is 90-250 ℃, and the time is 0.5-5h.
According to the present invention, although the temperature of heat treated is 90-250 ℃, the time is that 0.5-5h can realize purpose of the present invention, and under the preferable case, the temperature of heat treated is 100-200 ℃, and the time is 1-2h, can further improve the precipitation rate.
In order to make the vanadate that is settled out more even, further reduce foreign matter content, heat treated is preferably thermostatically heating and processes.In order further to accelerate precipitation speed, heat treated is preferably carried out under agitation condition.
The pH value of acid vanadic acid radical ion solution is preferably 0.5-5.5.Without particular requirement, can adopt this area the whole bag of tricks commonly used to make vanadic acid radical ion solution be acid for the preparation method of acid vanadic acid radical ion solution, for example can adopt the method that adds acid solution in the vanadic acid radical ion solution.Acid solution for adding can be the various various acid solutions that can make vanadic acid radical ion solution reach above-mentioned pH value and the precipitation effect not had a negative impact, and is preferably sulphuric acid soln.The concentration of described acid solution is not particularly limited, as long as the pH value can be adjusted to above-mentioned scope.
Among the present invention, the concentration of vanadic acid radical ion is preferably the 0.5-0.68 mol/L in the vanadic acid radical ion solution.It will be understood by those skilled in the art that the vanadic acid radical ion solution among the present invention is the precipitation qualifying liquid, be preferably sodium vanadate solution.Described sodium vanadate solution for example can obtain by sodium roasting technique, as can being that the bone coal of 106-180 μ m and sodium-chlor mix and puts into fluid bed furnace with grinding particle size, the consumption of sodium-chlor is the 10-20 % by weight of bone coal consumption, make vanadic acid sodium at 800-850 ℃ of lower roasting 2-2.5h, then with filtering behind the deionized water dissolving, be prepared into again the sodium vanadate solution of different concns.
Adopt aforesaid method provided by the invention, when described vanadic acid radical ion solution was sodium vanadate solution, the solid of gained was many vanadic acid sodiums after the precipitation, will can obtain Vanadium Pentoxide in FLAKES after this solid roasting.The solid of gained also is commonly called as " red cake " after the precipitation, generally uses general formula xNa
2OyV
2O
5NH
2O represents, Na
2The content of O is lower to be that x is relatively less, and the purity of the Vanadium Pentoxide in FLAKES that then obtains after the follow-up roasting is higher, usually thinks Na
2It is acceptable that the content of O is lower than 5 % by weight.Therefore, on the other hand, the invention provides a kind of preparation method of Vanadium Pentoxide in FLAKES, the method comprises and adopts the method for above-mentioned precipitation that acid vanadic acid radical ion is carried out precipitation, then with roasting behind the precipitation gained solid drying.
The present invention with precipitation gained solid drying after the roasting concrete grammar that makes Vanadium Pentoxide in FLAKES do not have special requirement, can adopt this area the whole bag of tricks commonly used, for example precipitation gained solid can be washed with deionized water, at 60-100 ℃ of lower dry 3-5h, then make the Vanadium Pentoxide in FLAKES solid at 360-600 ℃ of lower roasting 3-5h after the washing.
More than describe preferred implementation of the present invention in detail; but the present invention is not limited to the detail in the above-mentioned embodiment, in technical conceive scope of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
Need to prove in addition, each concrete technical characterictic described in above-mentioned embodiment in reconcilable situation, can make up by any suitable mode, for fear of unnecessary repetition, the present invention is to the no longer separately explanation of various possible array modes.
In addition, also can carry out arbitrary combination between the various embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Embodiment
The present invention is further illustrated for following embodiment, but therefore do not limit the present invention.The precipitation rate refers to that the content of vanadium in the precipitation gained solid accounts for the ratio of the content of vanadium in the vanadic acid radical ion solution among the present invention.
Embodiment 1
This embodiment is used for illustrating the preparation method of precipitation method provided by the invention and Vanadium Pentoxide in FLAKES.
With sulfuric acid the pH value of sodium vanadate solution (vanadic acid radical ion concentration is 0.6 mol/L) is transferred to 2.5, then pour in the reactor, whipping appts is equipped with in the reactor, tight a bolt make reactor airtight after, reactor is placed 150 ℃ of baking oven thermostatically heating 1.5h, and constantly stir, filter subsequently, precipitation gained solid is taken out, use deionized water wash, put into 80 ℃ of dry 4h of baking oven after the washing, then make the Vanadium Pentoxide in FLAKES solid at 480 ℃ of lower roasting 4h.The precipitation rate sees Table 1 with the purity of the Vanadium Pentoxide in FLAKES that makes.
Embodiment 2
This embodiment is used for illustrating the preparation method of precipitation method provided by the invention and Vanadium Pentoxide in FLAKES.
With sulfuric acid the pH value of sodium vanadate solution (vanadic acid radical ion concentration is 0.5 mol/L) is transferred to 0.5, then pour in the reactor, whipping appts is equipped with in the reactor, tight a bolt make reactor airtight after, reactor is placed 200 ℃ of baking oven thermostatically heating 1h, and constantly stir, filter subsequently, precipitation gained solid is taken out, use deionized water wash, put into 100 ℃ of dry 3h of baking oven after the washing, then make the Vanadium Pentoxide in FLAKES solid at 600 ℃ of lower roasting 3h.The precipitation rate sees Table 1 with the purity of the Vanadium Pentoxide in FLAKES that makes.
Embodiment 3
This embodiment is used for illustrating the preparation method of precipitation method provided by the invention and Vanadium Pentoxide in FLAKES.
With sulfuric acid the pH value of sodium vanadate solution (vanadic acid radical ion concentration is 0.68 mol/L) is transferred to 5.5, then pour in the reactor, whipping appts is equipped with in the reactor, tight a bolt make reactor airtight after, reactor is placed 100 ℃ of baking oven thermostatically heating 2h, and constantly stir, filter subsequently, precipitation gained solid is taken out, use deionized water wash, put into 60 ℃ of dry 5h of baking oven after the washing, then make the Vanadium Pentoxide in FLAKES solid at 360 ℃ of lower roasting 5h.The precipitation rate sees Table 1 with the purity of the Vanadium Pentoxide in FLAKES that makes.
Comparative Examples 1
With sulfuric acid the pH value of sodium vanadate solution (vanadic acid radical ion concentration is 0.6 mol/L) is transferred to 2.5, then press ammonium vanadium mol ratio and add ammoniumsulphate soln at 1: 3, then thermostatically heating backflow 1.5h, and constantly stir, filter subsequently, precipitation gained solid is taken out, use deionized water wash, put into 80 ℃ of dry 4h of baking oven after the washing, then make the Vanadium Pentoxide in FLAKES solid at 480 ℃ of lower roasting 4h.The precipitation rate sees Table 1 with the purity of the Vanadium Pentoxide in FLAKES that makes.
Comparative Examples 2
With sodium hydroxide the pH value of sodium vanadate solution (vanadic acid radical ion concentration is 0.68 mol/L) is transferred to 8, then press ammonium vanadium mol ratio and add ammoniumsulphate soln at 1: 1, then at 20 ℃ of lower 3h that place, and constantly stir, filter subsequently, precipitation gained solid is taken out, use deionized water wash, put into 80 ℃ of dry 4h of baking oven after the washing, then make the Vanadium Pentoxide in FLAKES solid at 550 ℃ of lower roasting 2h.The precipitation rate sees Table 1 with the purity of the Vanadium Pentoxide in FLAKES that makes.
Comparative Examples 3
With sulfuric acid the pH value of sodium vanadate solution (vanadic acid radical ion concentration is 0.6 mol/L) is transferred to 1.8, then under the condition that constantly stirs with solution heated and boiled backflow 1.5h, filter subsequently, precipitation gained solid is taken out, use deionized water wash, put into 80 ℃ of dry 4h of baking oven after the washing, then make the Vanadium Pentoxide in FLAKES solid at 480 ℃ of lower roasting 4h.The precipitation rate sees Table 1 with the purity of the Vanadium Pentoxide in FLAKES that makes.
Table 1
| Embodiment | Precipitation rate (%) | Vanadium Pentoxide in FLAKES purity (%) |
| 1 | 99.1 | 96.8 |
| 2 | 98.7 | 96.5 |
| 3 | 99.4 | 98.2 |
| Comparative Examples 1 | 98.4 | 98.8 |
| Comparative Examples 2 | 97.8 | 99.5 |
| Comparative Examples 3 | 97.6 | 96.2 |
Embodiment 1-3 is compared and can find out with Comparative Examples 1 and Comparative Examples 2 respectively, although employing the inventive method is high not as the purity of the Vanadium Pentoxide in FLAKES that ammonium salt precipitation method makes, but the precipitation rate of the inventive method is high, and the inventive method do not have the salinity such as ammonium sulfate to produce, and reduced the salt content that is difficult to process in the precipitation waste water; Embodiment 1-3 and Comparative Examples 3 are compared and can find out, adopt the inventive method ratio under open state, the precipitation condition of sodium vanadate solution coctoprecipitinogen easily to be realized, as long as in confined conditions with acidic conditions under, under 90-250 ℃ of temperature, carry out, can realize precipitation, and the precipitation rate is higher.
The method of precipitation provided by the invention, if in confined conditions with acidic conditions under, under 90-250 ℃ of temperature, carry out, can realize precipitation, with in the existing precipitation technique hydrolysis precipitation compare, the precipitation condition easily realizes; The precipitation rate is high, and precipitation speed is fast; The inventive method is compared with ammonium salt precipitation method, has reduced the salt content that is difficult to process in the precipitation waste water, has important environment protection significance, and need not add ammonium salt and can finish the precipitation process, has reduced cost; The method of precipitation provided by the invention, technique is simple, can be widely used in industrial production.
Claims (10)
1. the method for a precipitation is characterized in that, the method comprises carries out heat treated in confined conditions with acid vanadic acid radical ion solution, and the temperature of heat treated is 90-250 ℃, and the time is 0.5-5h.
2. method according to claim 1, wherein, the temperature of heat treated is 100-200 ℃, the time is 1-2h.
3. method according to claim 1 and 2, wherein, described heat treated is that thermostatically heating is processed.
4. the described method of any one according to claim 1-3, wherein, described heat treated is carried out under agitation condition.
5. the described method of any one according to claim 1-4, wherein, the pH value of described acid vanadic acid radical ion solution is 0.5-5.5.
6. the described method of any one according to claim 1-5, wherein, the preparation method of described acid vanadic acid radical ion solution comprises in vanadic acid radical ion solution and adds acid solution.
7. method according to claim 6, wherein, described acid solution is sulphuric acid soln.
8. the described method of any one according to claim 1-7, wherein, the concentration of vanadic acid radical ion is the 0.5-0.68 mol/L in the described vanadic acid radical ion solution.
9. the described method of any one according to claim 1-8, wherein, described vanadic acid radical ion solution is sodium vanadate solution.
10. the preparation method of a Vanadium Pentoxide in FLAKES is characterized in that, described method comprises that the described method of any one is carried out precipitation with acid vanadic acid radical ion among the employing claim 1-9, then with roasting behind the precipitation gained solid drying.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145187A (en) * | 2013-03-22 | 2013-06-12 | 中南大学 | Production technology of harmless high-purity vanadium pentoxide |
| CN103803649A (en) * | 2014-02-28 | 2014-05-21 | 重庆大学 | Method for settling vanadium by using acidic vanadium solution |
| CN104004926A (en) * | 2014-06-11 | 2014-08-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing high-purity vanadium pentoxide through sodium polyvanadate |
| CN104058457A (en) * | 2013-10-31 | 2014-09-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing vanadium pentoxide from low purity vanadium containing compound |
| CN106587150A (en) * | 2016-12-19 | 2017-04-26 | 攀枝花卓越钒业科技股份有限公司 | Method for preheating sodium vanadate to carry out vanadium precipitation |
| CN107512734A (en) * | 2017-08-01 | 2017-12-26 | 洛阳理工学院 | A kind of method that tungsten vanadium and titanium dioxide are reclaimed from discarded SCR denitration |
| CN107739825A (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 | It is a kind of to utilize the method that vanadium product is prepared containing vanadium leachate |
| CN109279653A (en) * | 2018-12-07 | 2019-01-29 | 攀钢集团攀枝花钢铁研究院有限公司 | The method for preparing high purity vanadic anhydride |
| CN112047379A (en) * | 2020-09-14 | 2020-12-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for precipitating ammonium polyvanadate |
| CN115611310A (en) * | 2022-10-08 | 2023-01-17 | 武汉科技大学 | Method for preparing high-purity vanadium pentoxide by using vanadium-containing solution |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145187A (en) * | 2013-03-22 | 2013-06-12 | 中南大学 | Production technology of harmless high-purity vanadium pentoxide |
| CN104058457A (en) * | 2013-10-31 | 2014-09-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing vanadium pentoxide from low purity vanadium containing compound |
| CN104058457B (en) * | 2013-10-31 | 2016-02-03 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method being produced Vanadium Pentoxide in FLAKES by low-purity vanadium-containing compound |
| CN103803649A (en) * | 2014-02-28 | 2014-05-21 | 重庆大学 | Method for settling vanadium by using acidic vanadium solution |
| CN104004926A (en) * | 2014-06-11 | 2014-08-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing high-purity vanadium pentoxide through sodium polyvanadate |
| CN104004926B (en) * | 2014-06-11 | 2016-04-27 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method utilizing many vanadic acid sodiums to prepare high-purity vanadium pentoxide |
| CN106587150A (en) * | 2016-12-19 | 2017-04-26 | 攀枝花卓越钒业科技股份有限公司 | Method for preheating sodium vanadate to carry out vanadium precipitation |
| CN107512734A (en) * | 2017-08-01 | 2017-12-26 | 洛阳理工学院 | A kind of method that tungsten vanadium and titanium dioxide are reclaimed from discarded SCR denitration |
| CN107739825A (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 | It is a kind of to utilize the method that vanadium product is prepared containing vanadium leachate |
| CN107739825B (en) * | 2017-10-31 | 2019-05-17 | 成都先进金属材料产业技术研究院有限公司 | A method of vanadium product is prepared using containing vanadium leachate |
| CN109279653A (en) * | 2018-12-07 | 2019-01-29 | 攀钢集团攀枝花钢铁研究院有限公司 | The method for preparing high purity vanadic anhydride |
| CN112047379A (en) * | 2020-09-14 | 2020-12-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for precipitating ammonium polyvanadate |
| CN115611310A (en) * | 2022-10-08 | 2023-01-17 | 武汉科技大学 | Method for preparing high-purity vanadium pentoxide by using vanadium-containing solution |
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Application publication date: 20130130 |