CN106082332A - A kind of ammonium metavanadate removal of impurities purifying technique - Google Patents
A kind of ammonium metavanadate removal of impurities purifying technique Download PDFInfo
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- CN106082332A CN106082332A CN201610433042.3A CN201610433042A CN106082332A CN 106082332 A CN106082332 A CN 106082332A CN 201610433042 A CN201610433042 A CN 201610433042A CN 106082332 A CN106082332 A CN 106082332A
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- ammonium
- ammonium metavanadate
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- precipitate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
Abstract
The invention discloses a kind of ammonium metavanadate removal of impurities purifying technique, this technique comprises the following steps: S1: make alkali lye, S2: grind ammonium poly-vanadate, S3: preliminarily solubilised and filtration, S4: precipitate away indissoluble impurity, S5: produce ammonium metavanadate and wash, S6: drying and processing.Present invention process is simple, by step S4, can remove the impurity of property hard to tolerate, can be removed the impurity of solubility by step S5, and therefore ammonium metavanadate can effectively be purified by the present invention, and energy consumption is low, has preferable market prospects.
Description
Technical field
The present invention relates to ammonium metavanadate production field, be specially a kind of ammonium metavanadate removal of impurities purifying technique.
Background technology
Ammonium metavanadate is heated to 135 DEG C in a vacuum and begins to decompose, can going back due to produced ammonia during more than 210 DEG C
Original work blackening with the low oxide forming vanadium.Become vanadic anhydride when in air middle calcination completely.
The existing complex process produced for ammonium metavanadate and purify, energy consumption is relatively big, so production cost is high, does not meets
The theme of current society energy-conserving and environment-protective, and the ammonium metavanadate purity that existing ammonium metavanadate reparation technology obtains is relatively low, and this just limits
Make the purposes of the ammonium metavanadate of produced in conventional processes, and the ammonium metavanadate price that this conventional method prepares is relatively low, market
Competitiveness is poor.
Content of the invention
It is an object of the invention to provide a kind of ammonium metavanadate removal of impurities purifying technique, to solve above-mentioned background technology proposes
Problem.
For achieving the above object, the present invention provides following technical scheme: a kind of ammonium metavanadate removal of impurities purifying technique, this technique
Comprise the following steps:
NaOH, according to the ratio determining, is put into equipped with carrying out in the dissolution equipment of pure water molten by S1: make alkali lye
Solving, closing equipment, and be stirred and heat, heating-up temperature is 45-65 degree Celsius, and speed of agitator is 300-420 rev/min,
Reaction pressure is 150-190 kPa, transfers in beaker by alkali lye after completing, and being passed through the ammonia reaction time is 3-5 minute,
Standby with preservative film sealing；
S2: grind ammonium poly-vanadate, weigh ammonium poly-vanadate according to set part by weight, be then transferred into grinding in milling apparatus
Mill, milling time is 10-20 minute, crosses 200 mesh sieves afterwards standby；
S3: preliminarily solubilised and filtration, transfer to the alkali lye that step S1 prepares in consersion unit, and the many vanadium preparing step S2
Acid ammonium powder is put in consersion unit, carries out heating and stirring, and consersion unit is airtight equipment, and heating-up temperature is 60-80
Degree Celsius, mixing plant rotating speed is 500-600 rev/min, and the pressure of consersion unit is 200-220 kPa, and the reaction time is 12-18
Minute, prepare ammonium poly-vanadate aqueous slkali；
The ammonium poly-vanadate aqueous slkali that previous step prepares is transferred to precipitate in airtight equipment by S4: precipitate away indissoluble impurity, quiet
Put 80-100 minute, after the impurity sedimentation in solution, use siphon pipe to draw out solution from upper strata, and transfer in container
Standby；
S5: produce ammonium metavanadate and wash, adds ammonium chloride, prepares ammonium metavanadate precipitate, make in the solution preparing one step up
With filter plant, solution is removed, ammonium metavanadate precipitate is stayed, and transfers in drip washing equipment, use leacheate to drench
Washing, the drip washing time is 10-15 minute, then uses distilled water to wash, and wash time is 5-10 minute；
S6: drying and processing, the ammonium metavanadate precipitate after washing previous step is transferred to carry out in drying plant drying and processing, is made
Obtain high-purity ammonium metavanadate.
Preferably, the leacheate using in described step S5 is the saturated aqueous solution of ammonium chloride.
Preferably, the drying mode using in described step S6 is microwave drying method, and the process time is 2-5 minute.
Compared with prior art, the invention has the beneficial effects as follows: present invention process is simple, by step S4, can be by difficulty
The impurity of capacitive removes, and can be removed the impurity of solubility by step S5, and therefore the present invention can be effectively to metavanadic acid
Ammonium purifies, and energy consumption is low, has preferable market prospects.
Detailed description of the invention
Technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described enforcement
Example is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of not making creative work, broadly falls into the model of present invention protection
Enclose.
Embodiment one
The present invention provides a kind of technical scheme: a kind of ammonium metavanadate removal of impurities purifying technique, and this technique comprises the following steps:
NaOH, according to the ratio determining, is put into equipped with carrying out in the dissolution equipment of pure water molten by S1: make alkali lye
Solving, closing equipment, and be stirred and heat, heating-up temperature is 45 degrees Celsius, and speed of agitator is 300 revs/min, reaction pressure
Being 150 kPas, transferring in beaker by alkali lye after completing, being passed through the ammonia reaction time is 3 minutes, standby with preservative film sealing
With；
S2: grind ammonium poly-vanadate, weigh ammonium poly-vanadate according to set part by weight, be then transferred into grinding in milling apparatus
Mill, milling time is 10 minutes, crosses 200 mesh sieves afterwards standby；
S3: preliminarily solubilised and filtration, transfer to the alkali lye that step S1 prepares in consersion unit, and the many vanadium preparing step S2
Acid ammonium powder is put in consersion unit, carries out heating and stirring, and consersion unit is airtight equipment, and heating-up temperature is 60 Celsius
Degree, mixing plant rotating speed is 500 revs/min, and the pressure of consersion unit is 200 kPas, and the reaction time is 12 minutes, prepares many vanadic acid
Ammonium aqueous slkali；
The ammonium poly-vanadate aqueous slkali that previous step prepares is transferred to precipitate in airtight equipment by S4: precipitate away indissoluble impurity, quiet
Put 80 minutes, after the impurity sedimentation in solution, use siphon pipe to draw out solution from upper strata, and transfer in container standby
With；
S5: produce ammonium metavanadate and wash, adds ammonium chloride, prepares ammonium metavanadate precipitate, make in the solution preparing one step up
With filter plant, solution is removed, ammonium metavanadate precipitate is stayed, and transfers in drip washing equipment, use leacheate to drench
Washing, the leacheate of use is the saturated aqueous solution of ammonium chloride, and the drip washing time is 10 minutes, then uses distilled water to wash,
Wash time is 5 minutes；
S6: drying and processing, the ammonium metavanadate precipitate after washing previous step is transferred to carry out in drying plant drying and processing, is adopted
Drying mode be microwave drying method, the process time is 2 minutes, prepare high-purity ammonium metavanadate.
Embodiment two
The present invention provides a kind of technical scheme: a kind of ammonium metavanadate removal of impurities purifying technique, and this technique comprises the following steps:
NaOH, according to the ratio determining, is put into equipped with carrying out in the dissolution equipment of pure water molten by S1: make alkali lye
Solving, closing equipment, and be stirred and heat, heating-up temperature is 55 degrees Celsius, and speed of agitator is 320 revs/min, reaction pressure
Being 180 kPas, transferring in beaker by alkali lye after completing, being passed through the ammonia reaction time is 4 minutes, standby with preservative film sealing
With；
S2: grind ammonium poly-vanadate, weigh ammonium poly-vanadate according to set part by weight, be then transferred into grinding in milling apparatus
Mill, milling time is 18 minutes, crosses 200 mesh sieves afterwards standby；
S3: preliminarily solubilised and filtration, transfer to the alkali lye that step S1 prepares in consersion unit, and the many vanadium preparing step S2
Acid ammonium powder is put in consersion unit, carries out heating and stirring, and consersion unit is airtight equipment, and heating-up temperature is 70 Celsius
Degree, mixing plant rotating speed is 560 revs/min, and the pressure of consersion unit is 210 kPas, and the reaction time is 16 minutes, prepares many vanadic acid
Ammonium aqueous slkali；
The ammonium poly-vanadate aqueous slkali that previous step prepares is transferred to precipitate in airtight equipment by S4: precipitate away indissoluble impurity, quiet
Put 88 minutes, after the impurity sedimentation in solution, use siphon pipe to draw out solution from upper strata, and transfer in container standby
With；
S5: produce ammonium metavanadate and wash, adds ammonium chloride, prepares ammonium metavanadate precipitate, make in the solution preparing one step up
With filter plant, solution is removed, ammonium metavanadate precipitate is stayed, and transfers in drip washing equipment, use leacheate to drench
Washing, the leacheate of use is the saturated aqueous solution of ammonium chloride, and the drip washing time is 12 minutes, then uses distilled water to wash,
Wash time is 8 minutes；
S6: drying and processing, the ammonium metavanadate precipitate after washing previous step is transferred to carry out in drying plant drying and processing, is adopted
Drying mode be microwave drying method, the process time is 3 minutes, prepare high-purity ammonium metavanadate.
Embodiment three
The present invention provides a kind of technical scheme: a kind of ammonium metavanadate removal of impurities purifying technique, and this technique comprises the following steps:
NaOH, according to the ratio determining, is put into equipped with carrying out in the dissolution equipment of pure water molten by S1: make alkali lye
Solving, closing equipment, and be stirred and heat, heating-up temperature is 65 degrees Celsius, and speed of agitator is 420 revs/min, reaction pressure
Being 190 kPas, transferring in beaker by alkali lye after completing, being passed through the ammonia reaction time is 5 minutes, standby with preservative film sealing
With；
S2: grind ammonium poly-vanadate, weigh ammonium poly-vanadate according to set part by weight, be then transferred into grinding in milling apparatus
Mill, milling time is 20 minutes, crosses 200 mesh sieves afterwards standby；
S3: preliminarily solubilised and filtration, transfer to the alkali lye that step S1 prepares in consersion unit, and the many vanadium preparing step S2
Acid ammonium powder is put in consersion unit, carries out heating and stirring, and consersion unit is airtight equipment, and heating-up temperature is 80 Celsius
Degree, mixing plant rotating speed is 600 revs/min, and the pressure of consersion unit is 220 kPas, and the reaction time is 18 minutes, prepares many vanadic acid
Ammonium aqueous slkali；
The ammonium poly-vanadate aqueous slkali that previous step prepares is transferred to precipitate in airtight equipment by S4: precipitate away indissoluble impurity, quiet
Put 100 minutes, after the impurity sedimentation in solution, use siphon pipe to draw out solution from upper strata, and transfer in container standby
With；
S5: produce ammonium metavanadate and wash, adds ammonium chloride, prepares ammonium metavanadate precipitate, make in the solution preparing one step up
With filter plant, solution is removed, ammonium metavanadate precipitate is stayed, and transfers in drip washing equipment, use leacheate to drench
Washing, the leacheate of use is the saturated aqueous solution of ammonium chloride, and the drip washing time is 15 minutes, then uses distilled water to wash,
Wash time is 10 minutes；
S6: drying and processing, the ammonium metavanadate precipitate after washing previous step is transferred to carry out in drying plant drying and processing, is adopted
Drying mode be microwave drying method, the process time is 5 minutes, prepare high-purity ammonium metavanadate.
Present invention process is simple, by step S4, can remove the impurity of property hard to tolerate, can be by solvable by step S5
Property impurity remove, therefore ammonium metavanadate can effectively be purified by the present invention, and energy consumption is low, has preferable market
Prospect.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, permissible
Understand and multiple change, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention
And modification, the scope of the present invention be defined by the appended.
Claims (3)
1. an ammonium metavanadate removal of impurities purifying technique, it is characterised in that this technique comprises the following steps:
NaOH, according to the ratio determining, is put into equipped with carrying out in the dissolution equipment of pure water molten by S1: make alkali lye
Solving, closing equipment, and be stirred and heat, heating-up temperature is 45-65 degree Celsius, and speed of agitator is 300-420 rev/min,
Reaction pressure is 150-190 kPa, transfers in beaker by alkali lye after completing, and being passed through the ammonia reaction time is 3-5 minute,
Standby with preservative film sealing；
S2: grind ammonium poly-vanadate, weigh ammonium poly-vanadate according to set part by weight, be then transferred into grinding in milling apparatus
Mill, milling time is 10-20 minute, crosses 200 mesh sieves afterwards standby；
S3: preliminarily solubilised and filtration, transfer to the alkali lye that step S1 prepares in consersion unit, and the many vanadium preparing step S2
Acid ammonium powder is put in consersion unit, carries out heating and stirring, and consersion unit is airtight equipment, and heating-up temperature is 60-80
Degree Celsius, mixing plant rotating speed is 500-600 rev/min, and the pressure of consersion unit is 200-220 kPa, and the reaction time is 12-18
Minute, prepare ammonium poly-vanadate aqueous slkali；
The ammonium poly-vanadate aqueous slkali that previous step prepares is transferred to precipitate in airtight equipment by S4: precipitate away indissoluble impurity, quiet
Put 80-100 minute, after the impurity sedimentation in solution, use siphon pipe to draw out solution from upper strata, and transfer in container
Standby；
S5: produce ammonium metavanadate and wash, adds ammonium chloride, prepares ammonium metavanadate precipitate, make in the solution preparing one step up
With filter plant, solution is removed, ammonium metavanadate precipitate is stayed, and transfers in drip washing equipment, use leacheate to drench
Washing, the drip washing time is 10-15 minute, then uses distilled water to wash, and wash time is 5-10 minute；
S6: drying and processing, the ammonium metavanadate precipitate after washing previous step is transferred to carry out in drying plant drying and processing, is made
Obtain high-purity ammonium metavanadate.
2. a kind of ammonium metavanadate removal of impurities purifying technique according to claim 1, it is characterised in that: described step S5 uses
Leacheate be the saturated aqueous solution of ammonium chloride.
3. a kind of ammonium metavanadate removal of impurities purifying technique according to claim 1, it is characterised in that: described step S6 uses
Drying mode be microwave drying method, the process time is 2-5 minute.
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| CN201610433042.3A CN106082332A (en) | 2016-06-18 | 2016-06-18 | A kind of ammonium metavanadate removal of impurities purifying technique |
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| CN201610433042.3A CN106082332A (en) | 2016-06-18 | 2016-06-18 | A kind of ammonium metavanadate removal of impurities purifying technique |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107815547A (en) * | 2017-11-08 | 2018-03-20 | 攀钢集团攀枝花钢铁研究院有限公司 | The clean method of acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique |
| CN114604893A (en) * | 2022-03-14 | 2022-06-10 | 河钢承德钒钛新材料有限公司 | Preparation method of ammonium metavanadate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603000A (en) * | 2012-03-19 | 2012-07-25 | 王远望 | Process for preparing high-purity vanadium pentoxide by adopting ammonium metavanadate as raw material |
| CN102923776A (en) * | 2012-12-03 | 2013-02-13 | 张春雨 | Method for producing high-purity vanadium pentoxide |
| CN104495927A (en) * | 2015-01-07 | 2015-04-08 | 攀钢集团研究院有限公司 | Method for preparing vanadium pentoxide |
-
2016
- 2016-06-18 CN CN201610433042.3A patent/CN106082332A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603000A (en) * | 2012-03-19 | 2012-07-25 | 王远望 | Process for preparing high-purity vanadium pentoxide by adopting ammonium metavanadate as raw material |
| CN102923776A (en) * | 2012-12-03 | 2013-02-13 | 张春雨 | Method for producing high-purity vanadium pentoxide |
| CN104495927A (en) * | 2015-01-07 | 2015-04-08 | 攀钢集团研究院有限公司 | Method for preparing vanadium pentoxide |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107815547A (en) * | 2017-11-08 | 2018-03-20 | 攀钢集团攀枝花钢铁研究院有限公司 | The clean method of acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique |
| CN114604893A (en) * | 2022-03-14 | 2022-06-10 | 河钢承德钒钛新材料有限公司 | Preparation method of ammonium metavanadate |
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Application publication date: 20161109 |
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