CN104760996A - Low-temperature crystallization method of ammonium polyvanadate - Google Patents
Low-temperature crystallization method of ammonium polyvanadate Download PDFInfo
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Abstract
The invention discloses a low-temperature crystallization method of ammonium polyvanadate. The low-temperature crystallization method includes following steps: (1) adding a crystallization initiator to vanadium liquid and stirring the vanadium liquid to dissolve the crystallization initiator; (2) adding acid to regulate the pH of the vanadium liquid to 1.0-7.0; and (3) continuously stirring the vanadium liquid to precipitate-out ammonium polyvanadate crystal, and performing filtration to obtain the ammonium polyvanadate crystal. The crystallization initiator is a mixture composed of one or more from water-soluble organic amine compounds and derivatives thereof. The method can effectively achieve high-concentration vanadium precipitation, can reduce the production amount of vanadium precipitation waste water by many times, can crystallize the ammonium polyvanadate crystal at room temperature, can effectively reduce energy consumption of steam and the like, can reduce the clean production cost and can increase yield rate. In the invention, the ammonium polyvanadate is precipitated-out in the form of a large-granular crystal being complete in structure. The method can reduce the entrainment of harmful impurities such as NH4<+>, Na<+>, K<+>, Fe<3+>, SO4<2->, SiO3<2-> and the like and can improve product quality.
Description
Technical field
The present invention relates to a kind of precipitation method, especially a kind of method of low temperature crystallization ammonium poly-vanadate.
Background technology
Industrial, comprise following key step containing vanadium material for the technical process of raw material production barium oxide (comprising vanadous oxide, Vanadium Pentoxide in FLAKES etc.) with vanadium titano-magnetite, vanadium slag, bone coal, spent catalyst etc.:
(1) activate: through roasting or acidization, the v element in Solid raw materials is converted into soluble vanadium hydrochlorate or vanadic acid;
(2) leach: by acid, in or alkaline aqueous solution soluble vanadium hydrochlorate is leached to liquid phase;
(3) precipitation (crystallization): obtain vanadium leachate after purification and impurity removal, adds precipitation medicament, makes vanadate be converted into insolubles, departs from liquid phase;
(4) finished product: barium oxide product is prepared in drying, deamination or reduction.
Wherein, precipitation technique adopts following several mode usually:
(1) acid ammonium salt precipitation: patent publication No. CN102351245A discloses a kind of continuous production method of ammonium vanadate, the method by vanadium liquid (vanadium leachate) with being steam heated to 50 ~ 80 DEG C, first time acid adding adjustment vanadium liquid pH=4 ~ 6, in vanadium liquid, add ammonium sulfate, the quality coefficient added is (NH
4)
2sO
4/ V=0.8 ~ 1.5, vanadium liquid continue stir and by steam heating to 80 ~ 100 DEG C; Second time adds acid and regulates vanadium liquid pH value 1.8 ~ 2.5 vanadium liquid with being steam heated to boiling, keeps boiling state; Be delivered in thickening pond after the supernatant liquor V≤0.1g/L of solid-liquid slip, final obtained ammonium poly-vanadate product.
(2) weakly alkaline ammonium salt precipitation: patent publication No. CN103146930A discloses a kind of method preparing barium oxide.The method, by after vanadium leachate silica removal, adds ammonium oxalate in vanadium leachate, regulates NH
4 +the mol ratio of/TV precipitates ammonium meta-vanadate in 2 ~ 3.5 scopes.
(3) calcium method precipitation: namely add the precipitation such as calcium chloride, calcium hydroxide medicament in vanadium liquid, make the v element in vanadium liquid be converted into calcium vanadate Precipitation.
In aforesaid method, there is the residual vanadium of liquid high (V >=2g/L) after precipitation in the precipitation of weakly alkaline ammonium salt, and ammonium meta-vanadate is higher containing ammonia, the defects such as deamination process energy consumption is large; The precipitation of calcium method exists with the calcium vanadate of output for barium oxide flow process chain length prepared by raw material, and technique is more complicated, the bottleneck that cost is high, limits the prospect of its industrial application.
Acid ammonium salt precipitation is because having the residual vanadium of liquid low (V≤0.08g/L) after its precipitation, and the advantages such as technological process of production chain is shorter, and production cost is lower are domestic and international each main manufacturer widespread use.But still there is a series of very important problem in acid ammonium salt precipitation technique:
(1) precipitation process remains that, between 80 ~ 100 DEG C, need consume a large amount of steam, energy consumption cost is higher.
(2) high temperature precipitation process requires that v element concentration in vanadium liquid≤30g/L(vanadium excessive concentration causes the ammonium poly-vanadate of output to be unformed shape usually, and short texture, is easy to solubility NH
4 +, Na
+, K
+, Fe
3+, SO
4 2-, SiO
3 2-deng detrimental impurity, be difficult to remove, conforming product rate), make a large amount of high salt of precipitation output, high ammonia-nitrogen wastewater.
(3) owing to adopting steam direct heating, steam condenses in the liquid phase, dilutes the v element concentration in liquid phase, vanadium wastewater quantum of output must be caused to raise, add subsequent wastewater treatment pressure.
(4) processing parameter requires harsh, and secondary acid adding must strictly between control pH=1.8 ~ 2.5, and slight fluctuations just easily produces " sizing ", " stock " phenomenon.
(5) the precipitation time is long, and certainly start to be warming up to the residual vanadium≤0.2g/L of liquid after precipitation, industrial production needs to react more than 3h usually, greatly constrains the raising of production efficiency.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method of low temperature crystallization ammonium poly-vanadate of efficient, environmental protection.
For solving the problems of the technologies described above, the technical solution used in the present invention is: in vanadium liquid, add seed content, stirring and dissolving; Then acid adding regulates pH value to 1.0 ~ 7.0 of vanadium liquid; Continuing stirring makes ammonium poly-vanadate crystal separate out, and filters and obtains ammonium poly-vanadate crystal; Described seed content is the mixing of one or more of water-soluble organic amine class and derivative thereof.
The preferred organic amine of the present invention is primary amine, secondary amine, tertiary amine, quaternary ammonium salt or polyamine.
The preferred seed content of the present invention is the mixture of one or more of methylamine, quadrol, piperazine, hexamethylenetetramine and diethylamide.
The add-on of seed content of the present invention is 2% ~ 40% of ammonium salt quality.
The acid of adjustment vanadium liquid pH value of the present invention is one or more mixtures in sulfuric acid, nitric acid, hydrochloric acid, oxalic acid and acetic acid.
The present invention makes ammonium poly-vanadate crystal separate out-5 ~ 50 DEG C of stirrings.
Ammonium poly-vanadate crystal of the present invention is separated out and is filtered to the crystalline mother solution V≤1g/L of solid-liquid slip.
Vanadium liquid of the present invention adopts following technique to obtain: (1) activated containing vanadium material, leach after obtain containing vanadium solution;
(2) containing adding aluminium salt and magnesium salts in vanadium solution, stirring reaction at 40 ~ 100 DEG C, filters and obtains filtrate; Aluminium salt add-on is by aluminium in aluminium salt: the amount of substance ratio=1:1 ~ 3:1 containing silicon in vanadium solution adds, and magnesium salts add-on is by magnesium in magnesium salts: the amount of substance ratio=1:1 ~ 2.5:1 containing phosphorus in vanadium solution adds;
(3) add ammonium salt in described filtrate, leach and obtain vanadium liquid; Charging capacity is ammonium salt: the mass ratio=0.6:1 ~ 1.3:1 of v element in filtrate.
Ammonium salt in step of the present invention (3) is one or more mixtures of ammonium sulfate, ammonium chloride, ammonium acetate, ammonium nitrate, ammonium oxalate.
Design of the present invention is as follows: under acidic conditions, and in ammonium poly-vanadate water, solubleness is very little, but containing after adding ammonium salt, acid adjustment in vanadium solution, the ammonium poly-vanadate supersaturated solution but quite stable of formation, unsuitable crystallization.Common process adopts the method for heating to destroy its meta structure, makes it at high temperature separate out.Under high temperature action, separate out a large amount of nucleus simultaneously, make ammonium poly-vanadate be difficult to be generated as the macrobead crystal of structural integrity, but separate out with loosely organized unformed shape, in precipitation process, carry great amount of soluble NH secretly
4 +, Na
+, K
+, Fe
3+, SO
4 2-, SiO
3 2-deng detrimental impurity.The present invention by introducing a small amount of seed content in system, such seed content can with V(V) forms stable complex, preferentially separate out as nucleus, induce ammonium poly-vanadate centered by nucleus, be grown to macrobead crystal.When ammonium poly-vanadate Study of Deamination is for oxyvanadium compound, such seed content can be analyzed to the gaseous fraction such as ammonia, carbonic acid gas, can not have any impact to barium oxide quality.
The beneficial effect adopting technique scheme to produce is: (1) the present invention effectively can realize high dense precipitation, reduces vanadium wastewater quantum of output at double.
(2) the present invention can crystallization ammonium poly-vanadate crystal under room temperature, effectively reduces the consumption of steam equal energy source, reduces cleaner production cost; Effective solution directly passes into the vanadium liquid density loss that steam causes, the problem increasing wastewater treatment capacity.
(3) process of the present invention has wider pH value, temperature window, and precipitation process condition is more easily manipulated, and reduces " stock " " sizing " and occurs, improve yield rate.
(4) product ammonium poly-vanadate of the present invention is separated out with the macrobead crystal state of structural integrity, decreases the solubility NH in liquid phase
4 +, Na
+, K
+, Fe
3+, SO
4 2-, SiO
3 2-carry secretly Deng detrimental impurity, improve the quality of products.
(5) when ammonium poly-vanadate Study of Deamination is for oxyvanadium compound, such seed content can be analyzed to the gaseous fraction such as ammonia, carbonic acid gas, can not have any impact to barium oxide quality.
In sum, the present invention can reduce vanadium wastewater quantum of output at double, effectively reduces the consumption of steam equal energy source, reduces cleaner production cost, decreases detrimental impurity and carry secretly, improve quality product; Have that energy-saving and environmental protection, production cost are low, the feature of good product quality.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is process flow diagram of the present invention.
Embodiment
Shown in Fig. 1, the method for this low temperature crystallization ammonium poly-vanadate adopts following processing step:
(1) containing the silicon, the phosphorus impurities that add in vanadium solution in aluminium salt, magnesium salts removal solution, at 40 ~ 100 DEG C, filter after stirring reaction 0.5 ~ 2h; Aluminium salt add-on: by aluminium in aluminium salt with the amount of substance containing silicon in vanadium solution than calculating, aluminium: silicon=1:1 ~ 3:1(mol); Magnesium salts add-on: by magnesium in magnesium salts with the amount of substance containing phosphorus in vanadium solution than calculating, magnesium: phosphorus=1:1 ~ 2.5:1(mol).Described aluminium salt can select the conventional aluminium salt such as Tai-Ace S 150, aluminum chloride, aluminum nitrate; Magnesium salts can select the conventional magnesium salts such as magnesium sulfate, magnesium chloride, magnesium nitrate.
Described is the solution containing soluble vanadium hydrochlorate that vanadium titano-magnetite, vanadium slag, bone coal, spent catalyst etc. obtain containing methods such as vanadium material sodium roasting, calcification baking, acidleach, alkali leachings containing vanadium solution, v element concentration 5 ~ 100g/L.
(2) containing in vanadium solution after removal of impurities adds ammonium salt, leaches and obtains vanadium liquid (vanadium leachate); Charging capacity: calculate with containing the mass ratio of v element in vanadium solution by ammonium salt, ammonium salt: v element=0.6:1 ~ 1.3:1(quality); Described ammonium salt is one or more mixtures in ammonium sulfate, ammonium chloride, ammonium acetate, ammonium nitrate and ammonium oxalate.
(3) add seed content, the quality added is containing v element quality in vanadium solution 2% ~ 40%, is constantly stirred to it and dissolves completely; Described seed content be water-soluble organic amine class (comprising primary amine, secondary amine, tertiary amine, quaternary ammonium salt, polyamine) and derivative thereof one or more mixing, it is at V(V) acidic aqueous solution in, stable complex can be formed with it, separate out as nucleus; One or more mixtures in the preferred methylamine of seed content, quadrol, piperazine, hexamethylenetetramine and diethylamide.
(4) acid adding regulates the pH value 1.0 ~ 7.0 of vanadium liquid; Add acid for one or more mixtures in sulfuric acid, nitric acid, hydrochloric acid, oxalic acid and acetic acid.
(5) stir at-5 ~ 50 DEG C, ammonium poly-vanadate crystal constantly separate out until solid-liquid slip crystalline mother solution V≤1g/L after, filter and obtain liquid after ammonium poly-vanadate crystal and precipitation; Wherein, stir speed (S.S.) controls at 30 ~ 150 turns/min, crystallization time >=0.1 hour.
Embodiment 1: with somewhere, Chengde vanadium slag sodium roasting water-leach liquor (containing vanadium solution, V=24.5g/l) for example, the concrete technology of the method for this low temperature crystallization ammonium poly-vanadate is as described below.
(1) containing adding Tai-Ace S 150, magnesium chloride in vanadium solution, filter after 50 DEG C of stirring reaction 1h; Tai-Ace S 150 add-on is: by aluminium in aluminium salt: containing silicon=1.5:1(mol in vanadium solution) add, magnesium chloride add-on: by magnesium in magnesium salts: containing phosphorus=1.2:1(mol in vanadium solution) add.
(2) ammonium sulfate is added, ammonium sulfate: v element=1.1:1(quality in solution).
(3) add seed content piperazine, the quality added is 10% of ammonium salt quality, is constantly stirred to it and dissolves completely.
(4) adding sulfuric acid regulates the pH value of vanadium liquid to be 2.0.
(5) continue to stir, at 30 DEG C, stir speed (S.S.) controls at 80 ~ 100 turns/min, crystallization time 1h.Ammonium poly-vanadate crystal constantly separate out until solid-liquid slip supernatant liquor V≤0.15g/L after, filter obtain ammonium poly-vanadate crystal, ammonium vanadate yield reaches 99%.
After gained ammonium poly-vanadate crystal 500 DEG C of deaminations, obtain Vanadium Pentoxide in FLAKES product; Gained Vanadium Pentoxide in FLAKES: purity >=99%; Foreign matter content Na≤0.5wt%, Si≤0.3wt%, Fe≤0.5wt%, P≤0.1wt%.
Embodiment 2: with Certain District, Hunan district bone coal pickling liquor (containing vanadium solution, V=45.6g/l) for example, the concrete technology of the method for this low temperature crystallization ammonium poly-vanadate is as described below.
(1) containing adding aluminum chloride, magnesium nitrate in vanadium solution, filter after 80 DEG C of stirring reaction 0.5h; Aluminum chloride add-on: by aluminium in aluminium salt: containing silicon=1.5:1(mol in vanadium solution) add, magnesium nitrate add-on: by magnesium in magnesium salts: containing phosphorus=1.2:1(mol in vanadium solution) add.
(2) ammonium chloride is added, ammonium chloride to containing in vanadium solution: v element=0.8:1(quality in solution).
(3) add seed content quadrol, the quality added is 5% of v element quality in solution, is constantly stirred to it and dissolves completely.
(4) adding acetic acid regulates the pH value of vanadium liquid to be 1.6;
(5) continue to stir, at 30 DEG C, stir speed (S.S.) controls at 30 ~ 50 turns/min, crystallization time 0.5h.Ammonium poly-vanadate crystal constantly separate out until solid-liquid slip supernatant liquor V≤0.15g/L after, filter obtain ammonium poly-vanadate crystal, ammonium vanadate yield reaches 98%.
After gained ammonium poly-vanadate crystal 500 DEG C of deaminations, obtain Vanadium Pentoxide in FLAKES product; Gained Vanadium Pentoxide in FLAKES: purity >=99%; Foreign matter content Na≤0.2%, Si≤0.2%, Fe≤0.2%, P≤0.4%.
Embodiment 3: with somewhere, the Sichuan pickling liquor of vanadium slag calcification baking (containing vanadium solution, V=32.1g/l) for example, the concrete technology of the method for this low temperature crystallization ammonium poly-vanadate is as described below.
(1) containing adding aluminum nitrate, magnesium chloride in vanadium solution, filter after 60 DEG C of stirring reaction 0.6h; Aluminum chloride add-on: by aluminium in aluminium salt: containing silicon=1.2:1(mol in vanadium solution) add, magnesium nitrate add-on: by magnesium in magnesium salts: containing phosphorus=1.0:1(mol in vanadium solution) add.
(2) ammonium nitrate is added, ammonium nitrate to containing in vanadium solution: v element=0.9:1(quality in solution).
(3) add seed content hexamethylenetetramine, the quality added is 20% of v element quality in solution, is constantly stirred to it and dissolves completely.
(4) adding acetic acid regulates the pH value of vanadium liquid to be 3.0.
(5) continue to stir, at 25 DEG C, stir speed (S.S.) controls at 60 ~ 80 turns/min, crystallization time 0.5h; Ammonium poly-vanadate crystal constantly separate out until solid-liquid slip supernatant liquor V≤0.1g/L after, filter obtain ammonium poly-vanadate crystal, ammonium vanadate yield reaches 98%.
After gained ammonium poly-vanadate crystal 500 DEG C of deaminations, obtain Vanadium Pentoxide in FLAKES product; Gained Vanadium Pentoxide in FLAKES: purity >=99%; Foreign matter content Na≤0.3%, Si≤0.1%, Fe≤0.4%, P≤0.1%.
Embodiment 4: with spent catalyst alkali immersion liquid (containing vanadium solution, V=52.7g/l) for example, the concrete technology of the method for this low temperature crystallization ammonium poly-vanadate is as described below.
(1) containing adding Tai-Ace S 150, magnesium sulfate in vanadium solution, filter after 40 DEG C of stirring reaction 1.5h; Tai-Ace S 150 add-on: by aluminium in aluminium salt: containing silicon=1.0:1(mol in vanadium solution) add, magnesium sulfate add-on: by magnesium in magnesium salts: containing phosphorus=2.0:1(mol in vanadium solution) add.
(2) ammonium acetate is added, ammonium acetate to containing in vanadium solution: v element=0.6:1(quality in solution).
(3) add seed content methylamine, the quality added is 2% of v element quality in solution, is constantly stirred to it and dissolves completely.
(4) adding oxalic acid regulates the pH value of vanadium liquid to be 5.0.
(5) continue to stir, at-5 DEG C, stir speed (S.S.) controls at 100 ~ 150 turns/min, crystallization time 0.1h; Ammonium poly-vanadate crystal constantly separate out until solid-liquid slip supernatant liquor V≤1g/L after, filter obtain ammonium poly-vanadate crystal, ammonium vanadate yield reaches 99%.
After gained ammonium poly-vanadate crystal 500 DEG C of deaminations, obtain Vanadium Pentoxide in FLAKES product; Gained Vanadium Pentoxide in FLAKES: purity >=99%; Foreign matter content Na≤0.3%, Si≤0.1%, Fe≤0.4%, P≤0.1%.
Embodiment 5: with vanadium titano-magnetite sodium roasting immersion liquid (containing vanadium solution, V=16.3g/l) for example, the concrete technology of the method for this low temperature crystallization ammonium poly-vanadate is as described below.
(1) containing adding aluminum chloride, magnesium nitrate in vanadium solution, filter after 100 DEG C of stirring reaction 1.2h; Aluminum chloride add-on: by aluminium in aluminium salt: containing silicon=2.0:1(mol in vanadium solution) add, magnesium nitrate add-on: by magnesium in magnesium salts: containing phosphorus=2.5:1(mol in vanadium solution) add.
(2) ammonium oxalate is added, ammonium oxalate to containing in vanadium solution: v element=1.3:1(quality in solution).
(3) add seed content diethylamide, the quality added is 40% of v element quality in solution, is constantly stirred to it and dissolves completely.
(4) adding hydrochloric acid regulates the pH value of vanadium liquid to be 7.0.
(5) continue to stir, at 15 DEG C, stir speed (S.S.) controls at 70 ~ 90 turns/min, crystallization; Ammonium poly-vanadate crystal constantly separate out until solid-liquid slip supernatant liquor V≤0.5g/L after, filter obtain ammonium poly-vanadate crystal, ammonium vanadate yield reaches 98%.
After gained ammonium poly-vanadate crystal 500 DEG C of deaminations, obtain Vanadium Pentoxide in FLAKES product; Gained Vanadium Pentoxide in FLAKES: purity >=99%; Foreign matter content Na≤0.3%, Si≤0.1%, Fe≤0.4%, P≤0.1%.
Embodiment 6: contain vanadium solution for identical with embodiment 1, the concrete technology of the method for this low temperature crystallization ammonium poly-vanadate is as described below.
(1) containing adding aluminum nitrate, magnesium sulfate in vanadium solution, filter after 60 DEG C of stirring reaction 2.0h; Aluminum nitrate add-on: by aluminium in aluminium salt: containing silicon=3:1(mol in vanadium solution) add, magnesium sulfate add-on: by magnesium in magnesium salts: containing phosphorus=1.5:1(mol in vanadium solution) add.
(2) ammonium chloride and ammonium nitrate (mass ratio 1:1) is added, (ammonium chloride+ammonium nitrate) to containing in vanadium solution: v element=1.3:1(quality in solution).
(3) quality that interpolation seed content methylamine and piperazine (mass ratio 1:1) add is 15% of v element quality in solution, is constantly stirred to it and dissolves completely.
(4) the pH value adding nitric acid and acetic acid adjustment vanadium liquid is 1.0.
(5) continue to stir, at 50 DEG C, stir speed (S.S.) controls at 40 ~ 50 turns/min, crystallization; Ammonium poly-vanadate crystal constantly separate out until solid-liquid slip supernatant liquor V≤0.2g/L after, filter obtain ammonium poly-vanadate crystal.
After gained ammonium poly-vanadate crystal 500 DEG C of deaminations, obtain Vanadium Pentoxide in FLAKES product; In gained Vanadium Pentoxide in FLAKES: foreign matter content Na≤0.3%, Si≤0.1%, Fe≤0.4%, P≤0.1%.
Claims (9)
1. a method for low temperature crystallization ammonium poly-vanadate, is characterized in that: in vanadium liquid, add seed content, stirring and dissolving; Then acid adding regulates pH value to 1.0 ~ 7.0 of vanadium liquid; Continuing stirring makes ammonium poly-vanadate crystal separate out, and filters and obtains ammonium poly-vanadate crystal; Described seed content is the mixing of one or more of water-soluble organic amine class and derivative thereof.
2. the method for a kind of low temperature crystallization ammonium poly-vanadate according to claim 1, is characterized in that: described organic amine is primary amine, secondary amine, tertiary amine, quaternary ammonium salt or polyamine.
3. the method for a kind of low temperature crystallization ammonium poly-vanadate according to claim 2, is characterized in that: described seed content is the mixture of one or more of methylamine, quadrol, piperazine, hexamethylenetetramine and diethylamide.
4. the method for a kind of low temperature crystallization ammonium poly-vanadate according to claim 1, is characterized in that: the add-on of described seed content is 2% ~ 40% of ammonium salt quality.
5. the method for a kind of low temperature crystallization ammonium poly-vanadate according to claim 1, is characterized in that: the acid of described adjustment vanadium liquid pH value is one or more mixtures in sulfuric acid, nitric acid, hydrochloric acid, oxalic acid and acetic acid.
6. the method for a kind of low temperature crystallization ammonium poly-vanadate according to claim 1, is characterized in that :-5 ~ 50 DEG C of stirrings, ammonium poly-vanadate crystal is separated out.
7. the method for a kind of low temperature crystallization ammonium poly-vanadate according to claim 1, is characterized in that: described ammonium poly-vanadate crystal is separated out and filtered to the crystalline mother solution V≤1g/L of solid-liquid slip.
8. the method for a kind of low temperature crystallization ammonium poly-vanadate according to claim 1-7 any one, is characterized in that, described vanadium liquid adopts following technique to obtain: (1) activated containing vanadium material, leach after obtain containing vanadium solution;
(2) containing adding aluminium salt and magnesium salts in vanadium solution, stirring reaction at 40 ~ 100 DEG C, filters and obtains filtrate; Aluminium salt add-on is by aluminium in aluminium salt: the amount of substance ratio=1:1 ~ 3:1 containing silicon in vanadium solution adds, and magnesium salts add-on is by magnesium in magnesium salts: the amount of substance ratio=1:1 ~ 2.5:1 containing phosphorus in vanadium solution adds;
(3) add ammonium salt in described filtrate, leach and obtain vanadium liquid; Charging capacity is ammonium salt: the mass ratio=0.6:1 ~ 1.3:1 of v element in filtrate.
9. the method for a kind of low temperature crystallization ammonium poly-vanadate according to claim 8, is characterized in that: the ammonium salt in described step (3) is one or more mixtures of ammonium sulfate, ammonium chloride, ammonium acetate, ammonium nitrate, ammonium oxalate.
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| CN105236485B (en) * | 2015-10-20 | 2016-12-14 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of preparation method of ammonium poly-vanadate |
| CN106241871A (en) * | 2016-07-15 | 2016-12-21 | 攀钢集团攀枝花钢铁研究院有限公司 | High vanadium concentrations liquid acid ammonium salt precipitation method |
| CN107010667A (en) * | 2017-04-01 | 2017-08-04 | 攀钢集团研究院有限公司 | A kind of method for preparing vanadic anhydride |
| CN107010667B (en) * | 2017-04-01 | 2019-03-19 | 攀钢集团研究院有限公司 | A method of preparing vanadic anhydride |
| CN109207721A (en) * | 2018-10-17 | 2019-01-15 | 中国科学院过程工程研究所 | A method of the Crystallization Separation ammonium metavanadate from containing vanadium raw materials roasting clinker infusion solution |
| CN110438347A (en) * | 2019-09-11 | 2019-11-12 | 攀钢集团攀枝花钢铁研究院有限公司 | Sodium cleans extraction vanadium method |
| CN111455186A (en) * | 2020-06-08 | 2020-07-28 | 江苏美东环境科技有限公司 | Method for preparing vanadium pentoxide by treating vanadium-containing waste sulfuric acid catalyst through two-step method |
| CN111455186B (en) * | 2020-06-08 | 2022-08-30 | 江苏美东环境科技有限公司 | Method for preparing vanadium pentoxide by treating vanadium-containing waste sulfuric acid catalyst through two-step method |
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