CN107746078A - A kind of system and method for preparing ammonium metavanadate crystal - Google Patents
A kind of system and method for preparing ammonium metavanadate crystal Download PDFInfo
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- CN107746078A CN107746078A CN201711216761.0A CN201711216761A CN107746078A CN 107746078 A CN107746078 A CN 107746078A CN 201711216761 A CN201711216761 A CN 201711216761A CN 107746078 A CN107746078 A CN 107746078A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
- B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
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Abstract
The invention provides a kind of system and method for preparing ammonium metavanadate, it is characterised in that including being sequentially connected such as lower unit：Turn molten retort (1), horizontal pressure filter (2), filtrate surge tank (3), heat exchanger (4), crystallizer (5), thickener (6), magma storage tank (7) and horizontal pressure filter (8), wherein, mother liquor holding tank (9) is provided between the thickener (6) and the horizontal pressure filter (8), for collecting supernatant.The present invention before crystallizer by setting heat exchanger, accelerate the rate of filtration of sodium metavanadate leaching liquid, avoid granule foreign in filtering and wear filter problem, realize the efficient crystallization of ammonium metavanadate under weak basic condition, effectively control the granularity and moisture of ammonium metavanadate crystal, solve the problems, such as the putty of ammonium metavanadate crystallization, improve the efficiency of crystal system, have a good application prospect.
Description
Technical field
The invention belongs to vanadium chemical technology field, is related to a kind of system and method for preparing ammonium metavanadate crystal.
Background technology
At present, domestic and international vanadium chemical technology field generally use vanadium slag sodium roasting technique carries out the preparation of barium oxide,
Its general principle is with Na2CO3For additive, the vanadium of lower valency is converted into by high temperature sodium roasting technique (750-850 DEG C)
The sodium salt of water miscible pentavalent vanadium, the leaching liquid of sodium metavanadate is obtained after water logging, add ammonium salt and ammonium metavanadate precipitate, warp is made
The oxide of vanadium is obtained after reduction roasting.
In order to ensure to be free of granule foreign in leaching liquid, traditional calcium vanadate is turned molten filtration system and generally filtered from small-bore
Cloth, the rate of filtration is slow, and filtrate cooling is fast, and tailings can not be entered by filter cloth by having ammonium metavanadate precipitate, cause the serious of vanadium
Loss.Meanwhile traditional crystallization processes can not effectively control the granularity and moisture of ammonium metavanadate, it is therefore desirable to develop new system
It is used to prepare barium oxide with method.
CN106435197A discloses a kind of SCR denitration dead catalyst valuable metal alkaline extraction retracting device and technique,
Described device is precipitated to obtain ammonium metavanadate precipitate thing using precipitation reactor to rich vanadium extract, and using dryer to inclined
Ammonium vanadate sediment drying and processing obtains ammonium metavanadate.However, the device does not solve ammonium metavanadate precipitate blocking filtering device
The problem of.
The content of the invention
In view of the shortcomings of the prior art, it is described the invention provides a kind of system and method for preparing ammonium metavanadate crystal
System accelerates the rate of filtration of sodium metavanadate leaching liquid, avoids particle in filtering by setting return line and heat exchanger
Impurity wears filter problem, using clear mother liquor forced circulation mode, realizes the efficient crystallization of ammonium metavanadate under weak basic condition, has
Effect controls the granularity and moisture of ammonium metavanadate crystal, solves the problems, such as the putty of ammonium metavanadate crystallization, improves crystal system
Efficiency.
To use following technical scheme up to this purpose, the present invention：
In a first aspect, prepare the system of ammonium metavanadate crystal the invention provides a kind of, including be sequentially connected as placed an order
Member：Turn molten retort 1, horizontal pressure filter 2, filtrate surge tank 3, heat exchanger 4, crystallizer 5, thickener 6, magma storage tank 7 and crouch
Formula filter press 8, wherein, mother liquor holding tank 9 is provided between the thickener 6 and the horizontal pressure filter 8, for collecting supernatant
Liquid.
In the present invention, heat exchanger is set before crystallizer, the crystallization of ammonium metavanadate is reduced by way of substep cools
Speed, avoid because the rate of filtration is slow, filtrate cooling is fast, ammonium metavanadate precipitate enters tailings and causes asking for the heavy losses of vanadium
Topic, the granularity and moisture of ammonium metavanadate crystal are effectively controlled, the putty for solving the problems, such as ammonium metavanadate crystallization, improve crystallization
The efficiency of system.
Preferably, the described turn of molten bottom discharge mouth of retort 1 is connected by conveying pipeline with the horizontal pressure filter 2, described
Turn the molten upper part discharge port of retort 1 and circulation loop is formed by the first return line and the conveying pipeline.
Preferably, it is provided with the second return line between the horizontal pressure filter 2 and first return line.
In the present invention, by setting return line in systems, in Cleaning pipes before crystallization starts eliminate pipeline
Residue, accelerate the rate of filtration of sodium metavanadate leaching liquid.
Preferably, the aperture of the filter cloth of the horizontal pressure filter 2 is 5-20 μm, for example, can be 5 μm, 6 μm, 7 μm, 8 μm,
9 μm, 10 μm, 11 μm, 12 μm, 13 μm, 14 μm, 15 μm, 16 μm, 17 μm, 18 μm, 19 μm or 20 μm, preferably 10 μm.
Preferably, it is provided with delivery pump between the filtrate surge tank 3 and the heat exchanger 4.
In the present invention, the slurry provides conveying power by delivery pump in systems.
Preferably, the heat exchanger 4 is pipe heat exchanger.
Preferably, the medium in the heat exchanger 4 is softened water.
Preferably, the crystallizer 5 is continuous crystalizer.
In the present invention, by way of using clear mother liquor forced circulation in continuous crystalizer, crystallization process is realized
Cooling, makes crystalline solid be sunken to crystalliser feet.
Preferably, the horizontal pressure filter 8 is wire netting filter press.
In the present invention, the workflow of the system for preparing ammonium metavanadate is：
The slurry turned in molten retort 1 is circulated into 1-5min in conveying pipeline and the first return line, in Cleaning pipes
Residue, close the first return line and enter the passage of filtrate surge tank, open the second return line, enter slurry horizontal
Filter press 2 keeps 1-3min to form cake layer, closes the second return line, filtrate is entered filtrate surge tank 3；Filtrate is buffered
Slurry in tank 3 is delivered in heat exchanger 4 by delivery pump, is delivered to after cooling in crystallizer 5 and is crystallized precipitation, in crystallizer 5
Bottom obtain magma；Magma is delivered in thickener 6, thickening obtains enrichment magma and supernatant, and supernatant is stored to mother
In flow container 9；Enrichment magma is transported in magma storage tank 7, it is then brilliant by the isolated ammonium metavanadate of the press filtration of horizontal pressure filter 8
Body and separating liquid, gained separating liquid is stored into mother liquor tank 9.
Second aspect, it is used to prepare ammonium metavanadate crystal the invention provides a kind of system as described in relation to the first aspect.
The third aspect, the invention provides a kind of method for preparing ammonium metavanadate crystal, comprise the following steps：
1) slurry turned in molten retort 1 is circulated in the first return line, filtered in horizontal pressure filter 2, collected extremely
In filtrate surge tank 3；
2) obtained filtrate is delivered in crystallizer 5 by heat exchanger 4, obtains magma；
3) magma described in step 2) is delivered to thickener 6, obtains enrichment magma and supernatant, reclaim supernatant；
4) it is isolated described inclined by horizontal pressure filter 8 after step 3) the enrichment magma being delivered into magma storage tank 7
Ammonium vanadate crystal.
Preferably, the step 1) slurry includes calcium vanadate turn solution and/or ammonium metavanadate solution.
Preferably, the temperature of the step 1) slurry is 90-100 DEG C, for example, can be 90 DEG C, 91 DEG C, 92 DEG C, 93 DEG C,
94 DEG C, 95 DEG C, 96 DEG C, 97 DEG C, 98 DEG C, 99 DEG C or 100 DEG C, preferably 95 DEG C.
Preferably, the time of the step 1) circulation is 1-5min, for example, can be 1min, 2min, 3min, 4min or
5min, preferably 3min.
Preferably, the time that the step 1) slurry filters in the horizontal pressure filter 2 is 1-3min, such as can be
1min, 2min or 3min, preferably 2min.
Preferably, the temperature of the step 2) heat exchanger 4 is 50-60 DEG C, for example, can be 50 DEG C, 51 DEG C, 52 DEG C, 53
DEG C, 54 DEG C, 55 DEG C, 56 DEG C, 57 DEG C, 58 DEG C, preferably 59 DEG C or 60 DEG C, 55 DEG C.
Preferably, 30-40 DEG C of the temperature of the step 2) crystallizer 5, for example, can be 30 DEG C, 31 DEG C, 32 DEG C, 33 DEG C,
34 DEG C, 35 DEG C, 36 DEG C, 37 DEG C, 38 DEG C, 39 DEG C or 40 DEG C, preferably 35 DEG C.
Preferably, the solid content in step 3) the enrichment magma is 15-25wt%, for example, can be 15wt%,
16wt%, 17wt%, 18wt%, 19wt%, 20wt%, 21wt%, 22wt%, 23wt%, 24wt% or 25wt%, it is preferably
20wt%.
In the present invention, the solid content refers to the mass fraction of solid in magma.
Preferably, the step 3) supernatant is delivered in mother liquor holding tank 9.
As optimal technical scheme, the invention provides a kind of method for preparing ammonium metavanadate crystal, comprise the following steps：
1) slurry that temperature is 90-100 DEG C in molten retort 1 will be turned and circulates 1-5min in the first return line, and close the
One return line, the second return line is opened, make the horizontal pressure filter 2 that slurry is 5-20 μm in aperture keep 1-3min to form filter
Cake layer, closes the second return line, and filtrate is collected into filtrate surge tank 3；
2) obtained filtrate is transported to the pipe heat exchanger that temperature is 50-60 DEG C by delivery pump from filtrate surge tank 3
4, after carrying out first time cooling, it is delivered in the continuous crystalizer 5 that temperature is 30-40 DEG C, carries out second and cool, obtain crystalline substance
Slurry；
3) magma described in step 2) is delivered to thickener 6, the solid content for the enrichment magma for thickening to obtain is 15-
25wt%, supernatant collection is into mother liquor holding tank 9；
4) after step 3) the enrichment magma being delivered into magma storage tank 7, separated by the press filtration of wire netting horizontal pressure filter 8
The ammonium metavanadate crystal is obtained, supernatant collection is into mother liquor holding tank 9.
Compared with prior art, the invention has the advantages that：
(1) present invention sets return line in systems, in pipeline is eliminated before crystallization starts by Cleaning pipes
Residue, accelerate the rate of filtration of sodium metavanadate leaching liquid；
(2) present invention sets heat exchanger before crystallizer, and the crystallization of ammonium metavanadate is reduced by way of substep cools
Speed, avoid because the rate of filtration is slow, filtrate cooling is fast, ammonium metavanadate precipitate enters tailings and causes asking for the heavy losses of vanadium
Topic；
(3) present invention realizes the cooling of crystallization process in continuous crystalizer by the way of clear mother liquor forced circulation,
The granularity and moisture of ammonium metavanadate crystal are effectively controlled, the putty for solving the problems, such as ammonium metavanadate crystallization, improves system of crystallization
The efficiency of system；
(4) particle diameter of the ammonium metavanadate crystal prepared using the present invention is not less than 0.6mm, water content 17-20%.
Brief description of the drawings
Fig. 1 is the system structure diagram provided by the invention for preparing ammonium metavanadate crystal, wherein, 1- turns molten retort,
2- horizontal pressure filters, 3- filtrate surge tanks, 4- heat exchangers, 5- crystallizers, 6- thickeners, 7- magma storage tanks, 8- horizontal pressure filters,
9- mother liquor holding tanks.
Embodiment
For the technological means and its effect that the present invention is taken is expanded on further, with reference to embodiments with accompanying drawing to this hair
It is bright to be further described.It is understood that embodiment described herein is used only for explaining the present invention, rather than
Limitation of the invention.
In the examples where no specific technique or condition is specified, according to the technology or condition described by document in the art,
Or carried out according to product description.Agents useful for same or the unreceipted production firm person of instrument, be can be by regular channel commercially available from
The conventional products of acquisition.
Embodiment 1
The structural representation of the system for preparing ammonium metavanadate of the present embodiment is as shown in Figure 1.
The system is including being sequentially connected such as lower unit：Turn molten retort 1, horizontal pressure filter 2, filtrate surge tank 3, change
Hot device 4, crystallizer 5, thickener 6, magma storage tank 7 and horizontal pressure filter 8, wherein, the thickener 6 and the horizontal pressure filter
Mother liquor holding tank 9 is provided between 8, for collecting supernatant；
The described turn of molten bottom discharge mouth of retort 1 is connected by conveying pipeline with the horizontal pressure filter 2, described turn of molten reaction
The upper part discharge port of tank 1 forms circulation loop by the first return line and the conveying pipeline；
The second return line is provided between the horizontal pressure filter 2 and first return line；
The aperture of the filter cloth of the horizontal pressure filter 2 is 10 μm；
Delivery pump is provided between the filtrate surge tank 3 and the heat exchanger 4；
The heat exchanger 4 is pipe heat exchanger；
Medium in the heat exchanger 4 is softened water；
The crystallizer 5 is continuous crystalizer；
The horizontal pressure filter 8 is wire netting filter press.
The workflow of the system for preparing ammonium metavanadate is：
The slurry turned in molten retort 1 is circulated into 1-5min in conveying pipeline and the first return line, in Cleaning pipes
Residue, close the first return line and enter the passage of filtrate surge tank, open the second return line, enter slurry horizontal
Filter press 2 keeps 1-3min to form cake layer, closes the second return line, filtrate is entered filtrate surge tank 3；Filtrate is buffered
Slurry in tank 3 is delivered in heat exchanger 4 by delivery pump, is delivered to after cooling in crystallizer 5 and is crystallized precipitation, in crystallizer 5
Bottom obtain magma；Magma is delivered in thickener 6, thickening obtains enrichment magma and supernatant, and supernatant is stored to mother
In flow container 9；Enrichment magma is transported in magma storage tank 7, it is then brilliant by the isolated ammonium metavanadate of the press filtration of horizontal pressure filter 8
Body and separating liquid, gained separating liquid is stored into mother liquor tank 9.
Embodiment 2
The present embodiment carries out the preparation of ammonium metavanadate using system as described in Example 1, concretely comprises the following steps：
1) calcium vanadate that temperature is 95 DEG C in molten retort 1 will be turned and turn the mixed liquor of solution and ammonium metavanadate solution the
One return line circulates 3min, closes the first return line, opens the second return line, makes slurry in aperture be 15 μm horizontal
Filter press 2 keeps 2min to form cake layer, closes the second return line, and filtrate is collected into filtrate surge tank 3；
2) obtained filtrate is transported to the pipe heat exchanger 4 that temperature is 55 DEG C from filtrate surge tank 3 by delivery pump, entered
After row cools for the first time, it is delivered in the continuous crystalizer 5 that temperature is 35 DEG C, carries out second and cool, obtain magma；
3) magma described in step 2) being delivered to thickener 6, the solid content for the enrichment magma for thickening to obtain is 20wt%,
Supernatant collection is into mother liquor holding tank 9；
4) after step 3) the enrichment magma being delivered into magma storage tank 7, separated by the press filtration of wire netting horizontal pressure filter 8
The ammonium metavanadate crystal is obtained, supernatant collection is into mother liquor holding tank 9.
The particle diameter of ammonium metavanadate crystal manufactured in the present embodiment is 0.9mm, water content 20%.
Embodiment 3
The present embodiment carries out the preparation of ammonium metavanadate using system as described in Example 1, concretely comprises the following steps：
1) calcium vanadate that temperature is 90 DEG C in molten retort 1 will be turned and turn solution in the first return line circulation 5min, pass
The first return line is closed, opens the second return line, makes the horizontal pressure filter 2 that slurry is 5 μm in aperture keep 3min to form filter
Cake layer, closes the second return line, and filtrate is collected into filtrate surge tank 3；
2) obtained filtrate is transported to the pipe heat exchanger 4 that temperature is 50 DEG C from filtrate surge tank 3 by delivery pump, entered
After row cools for the first time, it is delivered in the continuous crystalizer 5 that temperature is 40 DEG C, carries out second and cool, obtain magma；
3) magma described in step 2) being delivered to thickener 6, the solid content for the enrichment magma for thickening to obtain is 15wt%,
Supernatant collection is into mother liquor holding tank 9；
4) after step 3) the enrichment magma being delivered into magma storage tank 7, separated by the press filtration of wire netting horizontal pressure filter 8
The ammonium metavanadate crystal is obtained, supernatant collection is into mother liquor holding tank 9.
The particle diameter of ammonium metavanadate crystal manufactured in the present embodiment is 0.8mm, water content 18%.
Embodiment 4
The present embodiment carries out the preparation of ammonium metavanadate using system as described in Example 1, concretely comprises the following steps：
1) ammonium metavanadate solution that temperature in molten retort 1 is 100 DEG C will be turned and circulates 1min in the first return line, closed
First return line, the second return line is opened, make the horizontal pressure filter 2 that slurry is 20 μm in aperture keep 1min to form filter cake
Layer, closes the second return line, and filtrate is collected into filtrate surge tank 3；
2) obtained filtrate is transported to the pipe heat exchanger 4 that temperature is 60 DEG C from filtrate surge tank 3 by delivery pump, entered
After row cools for the first time, it is delivered in the continuous crystalizer 5 that temperature is 30 DEG C, carries out second and cool, obtain magma；
3) magma described in step 2) being delivered to thickener 6, the solid content for the enrichment magma for thickening to obtain is 25wt%,
Supernatant collection is into mother liquor holding tank 9；
4) after step 3) the enrichment magma being delivered into magma storage tank 7, separated by the press filtration of wire netting horizontal pressure filter 8
The ammonium metavanadate crystal is obtained, supernatant collection is into mother liquor holding tank 9.
The particle diameter of ammonium metavanadate crystal manufactured in the present embodiment is 0.6mm, water content 17%.
In summary, the present invention sets return line in systems, and pipe is eliminated by Cleaning pipes before crystallization starts
Residue in road, the rate of filtration of sodium metavanadate leaching liquid is accelerated, heat exchanger is set before crystallizer, cooled by substep
Mode reduce the crystallization rate of ammonium metavanadate, avoid because the rate of filtration is slow, filtrate cooling is fast, ammonium metavanadate precipitate enters
Tailings and the problem of cause the heavy losses of vanadium；In continuous crystalizer by the way of clear mother liquor forced circulation, realization finishes
The cooling of brilliant process, the granularity and moisture of ammonium metavanadate crystal are effectively controlled, the putty for solving the problems, such as ammonium metavanadate crystallization,
The efficiency of crystal system is improved, the particle diameter of the ammonium metavanadate crystal prepared using the present invention is not less than 0.6mm, and water content is
17-20%.
Applicant states that the present invention illustrates the method detailed of the present invention, but not office of the invention by above-described embodiment
It is limited to above-mentioned method detailed, that is, does not mean that the present invention has to rely on above-mentioned method detailed and could implemented.Art
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and disclosing.
Claims (10)
1. a kind of system for preparing ammonium metavanadate crystal, it is characterised in that including being sequentially connected such as lower unit：Turn molten retort
(1), horizontal pressure filter (2), filtrate surge tank (3), heat exchanger (4), crystallizer (5), thickener (6), magma storage tank (7) and sleeping
Formula filter press (8), wherein, mother liquor holding tank (9) is provided between the thickener (6) and the horizontal pressure filter (8), for receiving
Collect supernatant.
2. system according to claim 1, it is characterised in that described turn of molten retort (1) bottom discharge mouth passes through conveying
Pipe be connected with the horizontal pressure filter (2), described turn of molten retort (1) upper part discharge port by the first return line with it is described defeated
Expects pipe forms circulation loop；
Preferably, it is provided with the second return line between the horizontal pressure filter (2) and first return line.
3. system according to claim 1 or 2, it is characterised in that the aperture of the filter cloth of the horizontal pressure filter (2) is 5-
20 μm, preferably 10 μm；
Preferably, it is provided with delivery pump between the filtrate surge tank (3) and the heat exchanger (4)；
Preferably, the heat exchanger (4) is pipe heat exchanger；
Preferably, the medium in the heat exchanger (4) is softened water.
4. according to the system described in claim any one of 1-3, it is characterised in that the crystallizer (5) is continuous crystalizer；
Preferably, the horizontal pressure filter (8) is wire netting filter press.
5. a kind of system as described in claim any one of 1-4 is used to prepare ammonium metavanadate crystal.
A kind of 6. method for preparing ammonium metavanadate crystal, it is characterised in that comprise the following steps：
1) slurry that will turn in molten retort (1) circulates in the first return line, is filtered in horizontal pressure filter (2), collects extremely
In filtrate surge tank (3)；
2) obtained filtrate is delivered in crystallizer (5) by heat exchanger (4), obtains magma；
3) magma described in step 2) is delivered to thickener (6), obtains enrichment magma and supernatant, reclaim supernatant；
4) it is isolated described inclined by horizontal pressure filter (8) after step 3) the enrichment magma being delivered into magma storage tank (7)
Ammonium vanadate crystal.
7. according to the method for claim 6, it is characterised in that the step 1) slurry include calcium vanadate turn solution and/
Or ammonium metavanadate solution；
Preferably, the temperature of the step 1) slurry is 90-100 DEG C, preferably 95 DEG C；
Preferably, the time of the step 1) circulation is 1-5min, preferably 3min；
Preferably, step 1) slurry time of filtering in the horizontal pressure filter (2) is 1-3min, preferably 2min.
8. the method according to claim 6 or 7, it is characterised in that the temperature of the step 2) heat exchanger (4) is 50-60
DEG C, preferably 55 DEG C；
Preferably, 30-40 DEG C of the temperature of the step 2) crystallizer (5), preferably 35 DEG C.
9. according to the method described in claim any one of 6-8, it is characterised in that the solid content in step 3) the enrichment magma
For 15-25wt%, preferably 20wt%；
Preferably, the step 3) supernatant collection is into mother liquor holding tank (9).
10. according to the method described in claim any one of 6-9, it is characterised in that comprise the following steps：
1) slurry that temperature in molten retort (1) is 90-100 DEG C will be turned and circulate 1-5min in the first return line, close first
Return line, the second return line is opened, make the horizontal pressure filter (2) that slurry is 5-20 μm in aperture keep 1-3min to form filter
Cake layer, closes the second return line, and filtrate is collected into filtrate surge tank (3)；
2) obtained filtrate is transported to the pipe heat exchanger that temperature is 50-60 DEG C by delivery pump from filtrate surge tank (3)
(4) after, carrying out first time cooling, it is delivered in the continuous crystalizer (5) that temperature is 30-40 DEG C, carries out second and cool, obtain
Magma；
3) magma described in step 2) is delivered to thickener (6), the solid content for the enrichment magma for thickening to obtain is 15-
25wt%, in supernatant collection to mother liquor holding tank (9)；
4) after step 3) the enrichment magma being delivered into magma storage tank (7), separated by wire netting horizontal pressure filter (8) press filtration
The ammonium metavanadate crystal is obtained, in supernatant collection to mother liquor holding tank (9).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108517424A (en) * | 2018-04-08 | 2018-09-11 | 河钢股份有限公司承德分公司 | A method of being ultrasonically treated precipitation |
| CN109179504A (en) * | 2018-10-19 | 2019-01-11 | 河钢股份有限公司承德分公司 | A method of preparing big granularity ammonium metavanadate |
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| CN104775041A (en) * | 2015-03-31 | 2015-07-15 | 河北钢铁股份有限公司承德分公司 | Clean vanadium extraction method for self-circulation utilization of vanadium-solution-calcium-process precipitated vanadium, mother liquor and solid waste |
| CN105800689A (en) * | 2016-03-02 | 2016-07-27 | 河北钢铁股份有限公司承德分公司 | Preparation method of ultra-pure vanadium pentoxide |
| CN107376399A (en) * | 2017-08-17 | 2017-11-24 | 河钢股份有限公司承德分公司 | A kind of method for crystallising of sodium vanadate crystal system and sodium vanadate |
| CN107381637A (en) * | 2017-09-04 | 2017-11-24 | 河钢股份有限公司承德分公司 | A kind of method of preventing scaring in ammonium metavanadate crystallization process |
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| CN108517424A (en) * | 2018-04-08 | 2018-09-11 | 河钢股份有限公司承德分公司 | A method of being ultrasonically treated precipitation |
| CN109179504A (en) * | 2018-10-19 | 2019-01-11 | 河钢股份有限公司承德分公司 | A method of preparing big granularity ammonium metavanadate |
| CN109179504B (en) * | 2018-10-19 | 2020-12-04 | 河钢股份有限公司承德分公司 | Method for preparing large-particle-size ammonium metavanadate |
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