CN108557884A - A method of preparing high-density large-particle ammonium poly-vanadate - Google Patents
A method of preparing high-density large-particle ammonium poly-vanadate Download PDFInfo
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- CN108557884A CN108557884A CN201810084264.8A CN201810084264A CN108557884A CN 108557884 A CN108557884 A CN 108557884A CN 201810084264 A CN201810084264 A CN 201810084264A CN 108557884 A CN108557884 A CN 108557884A
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- vanadate
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- C01G31/00—Compounds of vanadium
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a kind of methods preparing high-density large-particle ammonium poly-vanadate, belong to chemical field.A method of high-density large-particle ammonium poly-vanadate is prepared, including：Bonding agent is mixed, addition sulfuric acid with low concentration vanadium liquid, after heating and thermal insulation, inorganic ammonium salt is added, reaction finishes, and obtains solution A；High concentration vanadium liquid and sulfuric acid are added in solution A, after completion of the reaction, through being filtered, washed, drying, obtain ammonium poly-vanadate.The method of the present invention prepares high-density large-particle ammonium poly-vanadate using low concentration vanadium liquid and high concentration vanadium liquid simultaneously, improve the utilization rate of vanadium liquid, precipitation rate is up to 99.0% or more, the method of the present invention has that easy to use, equipment requirement is low, easy to operate, wide adaptability, the advantages such as at low cost, has good social benefit.
Description
Technical field
The invention belongs to chemical fields, and in particular to a method of preparing high-density large-particle ammonium poly-vanadate.
Background technology
Ammonium poly-vanadate, light yellow crystalline powder are slightly soluble in cold water, hot ethanol and ether, are dissolved in hot water and dilute ammonium hydroxide,
Become vanadic anhydride in air when calcination, it is toxic；It is mainly used as chemical reagent, catalyst, drier, mordant etc., pottery
Porcelain industry is widely used as glaze, it can also be used to produce vanadic anhydride, vanadium trioxide.
《High density ammonium polyvanadate Study on Preparation Technology》Middle introduction can a kind of preparation method of high density ammonium polyvanadate,
TV concentration, pH, mixing speed, dosing and sour temperature plus ammonium coefficient and crystal seed are had studied to the heap density of ammonium poly-vanadate and is sunk
The influence of vanadium rate.Result of study shows：It is added at 60~85 DEG C with the solution of 20~30g/L containing vanadium and is more than 1/50 times of full vanadium matter
After the crystal seed of amount and the ammonium sulfate of 1.5~2.5 times of full vanadium quality, with sulphur acid for adjusting pH to 2.1~2.4,95 DEG C of boiling water bath according to
It is secondary to precipitate 40min and 20min respectively under 350r/min and 200r/min rotating speeds, 98.5% or more precipitation rate is can get, is dried
APV heap density after dry is more than 0.95g/cm3, APV roasting after powder vanadium in contain V2O5More than 98.5%, Na2O is less than 0.10%.
Above method reaction temperature is higher, complicated for operation, and to equipment requirement height, and it is only applicable to low concentration vanadium liquid, office
It is sex-limited larger, it is unfavorable for promoting and applying.
Invention content
For deficiencies of the prior art, a kind of method preparing high-density large-particle ammonium poly-vanadate of the invention,
This approach includes the following steps：
A, bonding agent is mixed, addition sulfuric acid with low concentration vanadium liquid, after heating and thermal insulation, soluble inorganic ammonium salt is added, instead
It should finish, obtain solution A；The bonding agent is amino acid；
B, high concentration vanadium liquid and sulfuric acid are added in solution A, after completion of the reaction, through being filtered, washed, drying, much vanadic acid
Ammonium.
Wherein, in the method for preparing high-density large-particle ammonium poly-vanadate described above, in step a, the low concentration vanadium
A concentration of 1~10g/L of TV of liquid, phosphorus content are no more than 0.01g/L.
Preferably, in the method for preparing high-density large-particle ammonium poly-vanadate described above, in step a, the bonding agent
For glycine.
Wherein, in the method for preparing high-density large-particle ammonium poly-vanadate described above, in step a, the bonding agent with
The mass ratio of total vanadium is 0.01~0.07 in low concentration vanadium liquid and high concentration vanadium liquid.
Wherein, in the method for preparing high-density large-particle ammonium poly-vanadate described above, in step a, the sulfuric acid it is dense
Degree is 10~50%.
Wherein, in the method for preparing high-density large-particle ammonium poly-vanadate described above, in step a, the sulfuric acid adds
Entering amount, system pH is 1.5~2.8 in order to control.
Wherein, in the method for preparing high-density large-particle ammonium poly-vanadate described above, in step a, the heating and thermal insulation
Temperature be 40 DEG C~60 DEG C, the time be 40~60min.
Wherein, in the method for preparing high-density large-particle ammonium poly-vanadate described above, in step a, the inorganic ammonium salt
For at least one of ammonium sulfate, ammonium hydrogen sulfate, ammonium chloride, ammonium oxalate, ammonium carbonate, ammonium hydrogen carbonate；The soluble inorganic ammonium
NH in salt4 +Molar ratio with total vanadium in low concentration vanadium liquid and high concentration vanadium liquid is 1~2.
Wherein, in the method for preparing high-density large-particle ammonium poly-vanadate described above, in step a, the reaction when
Between be 40min~120min.
Wherein, in the method for preparing high-density large-particle ammonium poly-vanadate described above, in step b, the high vanadium concentrations
The TV concentration of liquid is not less than 40g/L, and phosphorus content is no more than 0.01g/L.
Wherein, in the method for preparing high-density large-particle ammonium poly-vanadate described above, in step b, the high vanadium concentrations
The volume ratio of liquid and low concentration vanadium liquid in step a is 1：1~3.
Wherein, in the method for preparing high-density large-particle ammonium poly-vanadate described above, in step b, the sulfuric acid it is dense
Degree is 10%~50%.
Wherein, in the method for preparing high-density large-particle ammonium poly-vanadate described above, in step b, the sulfuric acid adds
Entering amount, system pH is 2.0~3.0 in order to control.
Wherein, in the method for preparing high-density large-particle ammonium poly-vanadate described above, in step b, the reaction when
Between be 20min~100min, temperature be 80 DEG C~95 DEG C.
Wherein, in the method for preparing high-density large-particle ammonium poly-vanadate described above, in step b, the temperature of the drying
Degree is 40 DEG C~60 DEG C, and the time is 10~13h.
The beneficial effects of the invention are as follows：
The method of the present invention prepares high-density large-particle ammonium poly-vanadate using low concentration vanadium liquid and high concentration vanadium liquid simultaneously, improves
The utilization rate of vanadium liquid, up to 99.0% or more, the density for preparing gained ammonium poly-vanadate is 1.5~2.0g/cm for precipitation rate3, average
A diameter of 0.2~0.6mm, impurity content are respectively less than 0.002%, can be used for that high density powdery vanadium trioxide and five oxygen can be prepared
Change two vanadium, and then improves the vanadium yield of vanadium iron；The method of the present invention is with easy to use, equipment requirement is low, easy to operate, suitable
The advantages such as Ying Xingguang, at low cost have good Social benefit and economic benefit.
Specific implementation mode
Specifically, a kind of method preparing high-density large-particle ammonium poly-vanadate, includes the following steps：
A, bonding agent is mixed, addition sulfuric acid with low concentration vanadium liquid, after heating and thermal insulation, soluble inorganic ammonium salt is added, instead
It should finish, obtain solution A；The bonding agent is amino acid；
B, high concentration vanadium liquid and sulfuric acid are added in solution A, after completion of the reaction, through being filtered, washed, drying, much vanadic acid
Ammonium.
The method of the present invention prepares high-density large-particle ammonium poly-vanadate using low concentration vanadium liquid and high concentration vanadium liquid simultaneously, improves
The utilization rate of vanadium liquid, a concentration of 1~10g/L of TV of the low concentration vanadium liquid, phosphorus content is no more than 0.01g/L, described highly concentrated
The TV concentration for spending vanadium liquid is not less than 40g/L, and phosphorus content is no more than 0.01g/L
It is bonding agent that amino acid is added in the method for the present invention, and the addition for controlling bonding agent is low concentration vanadium liquid and highly concentrated
1%~7% of the quality of total vanadium in vanadium liquid is spent, is conducive to uniformity nucleus and is formed, it is fixed to be easy in two kinds of concentration crystallization process
To growth, make that the density of ammonium poly-vanadate is higher, particle is larger；Preferably, the bonding agent is glycine.
In the method for the present invention step a, system pH is adjusted to 1.5~2.8 by the sulfuric acid for being added a concentration of 10~50%, is conducive to
Sweet acid vanadium is formed, 40 DEG C~60 DEG C is then heated to, and keep the temperature 40~60min, nucleus can be made to be easy to grow up.
In the method for the present invention step a, soluble inorganic ammonium salt may be selected ammonium sulfate, ammonium hydrogen sulfate, ammonium chloride, ammonium oxalate,
At least one of ammonium carbonate, ammonium hydrogen carbonate；NH in the soluble inorganic ammonium salt4 +, with low concentration vanadium liquid and high vanadium concentrations
The molar ratio of total vanadium is 1~2 in liquid, ensures precipitation rate and ammonium poly-vanadate yield.
In step a, after soluble inorganic ammonium salt is added, then 40min~120min is reacted, obtain midbody solution A.
Since the method for the present invention utilizes two kinds of vanadium liquids of low concentration and high concentration simultaneously, it is therefore desirable to be controlled to the two dosage
System, makes the moderate concentration of vanadium in system, avoids in ammonium poly-vanadate forming process, the reunion of ammonium poly-vanadate, therefore, the method for the present invention
In step b, the volume ratio of high concentration vanadium liquid and low concentration vanadium liquid in step a is 1：1~3.
In step b, the addition control of sulfuric acid is regulation system pH to 2.0~3.0, which advantageously forms more vanadic acid
Root is easy to precipitation；Then 20min~100min is reacted at 80 DEG C~95 DEG C, is filtered, washed to obtain wet ammonium poly-vanadate, it is wet
The fully dry 10~13h of 40 DEG C~60 DEG C of ammonium poly-vanadate are to get to high-density large-particle ammonium poly-vanadate.
The density that the present invention prepares gained ammonium poly-vanadate is 1.5~2.0g/cm3, average diameter is 0.2~0.6mm.
Heretofore described content is mass content, and total vanadium indicates total TV in low concentration vanadium liquid and high concentration vanadium liquid
It measures (quality or mole).
Below by embodiment, invention is further described in detail, but does not therefore limit the scope of the present invention
Among the embodiment described range.
The leading indicator of low concentration vanadium liquid used in the embodiment of the present invention is shown in Table 1, and the leading indicator of high concentration vanadium liquid is shown in
Table 2.
1 low concentration vanadium liquid main chemical compositions table of table/gL-1
2 high concentration vanadium liquid main chemical compositions table of table/gL-1
| TV | P | Mg2+ | Na+ | Si | TFe | TCr | Mn | Al3+ | Ca2+ | pH |
| 50.86 | 0.005 | 0.002 | 45.04 | 1.19 | 0.010 | 1.51 | 0.001 | 0.002 | 0.22 | 10.45 |
Embodiment 1
A, the low concentration vanadium liquid in 1000mL tables 1 is added into 2000mL cleaning beakers, according to glycine and low concentration vanadium
The mass ratio of total vanadium is 0.01 in liquid and high concentration vanadium liquid, and glycine is added in beaker, is adjusted with a concentration of 25% sulfuric acid
PH value is heated to 40 DEG C to 2.5, after keeping the temperature 40min, ammonium sulfate is added, the addition of ammonium sulfate is according to NH4 +/ V=1 (mole
Than V indicates total vanadium in low concentration vanadium liquid and high concentration vanadium liquid), stirring and dissolving obtains solution A after reacting 40min；
B, the sulfuric acid of the high concentration vanadium liquid 1000mL and a concentration of 25% in table 2 is added slowly in solution A simultaneously,
The addition of sulfuric acid is to adjust pH value to 2.5, is finished, and after 90~95 DEG C of reaction 75min, is filtered washing, obtains wet more
Wet ammonium poly-vanadate is put into drying in 40 DEG C of baking ovens by ammonium vanadate, and drying time is 12 hours, obtains the more vanadium of high-density large-particle
Sour ammonium.
It is 0.34g/L to detect content of vanadium in Upper-liquor of Precipitating Vanadate Process, and precipitation rate is 99.0%, measures the apparent density of ammonium poly-vanadate
For 1.5g/cm3, ammonium poly-vanadate average diameter of particles 0.2mm is scanned, ammonium poly-vanadate butt is 99.5, and impurity silicon, chromium, potassium, sodium contain
Amount is respectively less than 0.002%.
Embodiment 2
A, the low concentration vanadium liquid in 1000mL tables 1 is added into 2000mL cleaning beakers, according to glycine and low concentration vanadium
The mass ratio of total vanadium in liquid and high concentration vanadium liquid is 0.05, glycine is added in beaker, with a concentration of 35% sulfuric acid tune
PH value is saved to 2.5, is heated to 40 DEG C, after keeping the temperature 60min, ammonium sulfate is added, the addition of ammonium sulfate is according to NH4 +/ V=2 (mole
Than V indicates total vanadium in low concentration vanadium liquid and high concentration vanadium liquid), stirring and dissolving obtains solution A after reacting 40min；
B, the sulfuric acid of the high concentration vanadium liquid 1000mL and a concentration of 35% in table 2 is added slowly in a solution simultaneously,
The addition of sulfuric acid is to adjust pH value to 3.0, is finished, and after 85~93 DEG C of reaction 85min, is filtered washing, obtains wet more
Wet ammonium poly-vanadate is put into drying in 40 DEG C of baking ovens by ammonium vanadate, and drying time is 12 hours, obtains the more vanadium of high-density large-particle
Sour ammonium.
It is 0.26g/L to detect content of vanadium in Upper-liquor of Precipitating Vanadate Process, and precipitation rate is 99.2%, measures the apparent density of ammonium poly-vanadate
For 1.7g/cm3, ammonium poly-vanadate average diameter of particles 0.3mm is scanned, ammonium poly-vanadate butt is 99.6, miscellaneous, matter silicon, chromium, potassium, sodium
Content is respectively less than 0.002%.
Embodiment 3
A, the low concentration vanadium liquid in 1000mL tables 1 is added into 2000mL cleaning beakers, according to glycine and low concentration vanadium
The mass ratio of total vanadium in liquid and high concentration vanadium liquid is 0.05, glycine is added in beaker, with a concentration of 50% sulfuric acid tune
PH value is saved to 1.5, is heated to 40 DEG C, after keeping the temperature 40min, ammonium sulfate is added, the addition of ammonium sulfate is according to NH4 +/ V=1 (mole
Than V indicates total vanadium in low concentration vanadium liquid and high concentration vanadium liquid), solvent is stirred, after reacting 40min, obtains solution A；
B, the sulfuric acid of the high concentration vanadium liquid 1000mL and a concentration of 50% in table 2 is added slowly in a solution simultaneously,
The addition of sulfuric acid is to adjust pH value to 2.0, is finished, and after 80~90 DEG C of reaction 65min, is filtered washing, obtains wet more
Wet ammonium poly-vanadate is put into drying in 40 DEG C of baking ovens by ammonium vanadate, and drying time is 12 hours, obtains the more vanadium of high-density large-particle
Sour ammonium.
It is 0.16g/L to detect content of vanadium in Upper-liquor of Precipitating Vanadate Process, and precipitation rate is 99.5%, measures the apparent density of ammonium poly-vanadate
For 1.8g/cm3, ammonium poly-vanadate average diameter of particles 0.4mm is scanned, ammonium poly-vanadate butt is 99.7, and impurity silicon, chromium, potassium, sodium contain
Amount is respectively less than 0.002%.
By Examples 1 to 3 it is found that invention significantly improves the utilization rate of high concentration vanadium liquid, precipitation rate up to 99.0% with
On, the density for preparing gained ammonium poly-vanadate is 1.5~1.8g/cm3, average diameter is 0.2~0.4mm, and impurity content is respectively less than
0.002%；The method of the present invention has that easy to use, equipment requirement is low, easy to operate, wide adaptability, the advantages such as at low cost, has
Good Social benefit and economic benefit.
Claims (10)
1. the method for preparing high-density large-particle ammonium poly-vanadate, it is characterised in that：Include the following steps：
A, bonding agent is mixed, addition sulfuric acid with low concentration vanadium liquid, after heating and thermal insulation, soluble inorganic ammonium salt is added, has reacted
Finish, obtains solution A；The bonding agent is amino acid；
B, high concentration vanadium liquid and sulfuric acid are added in solution A, after completion of the reaction, through being filtered, washed, drying, obtain ammonium poly-vanadate.
2. the method according to claim 1 for preparing high-density large-particle ammonium poly-vanadate, it is characterised in that：In step a, institute
A concentration of 1~10g/L of TV of low concentration vanadium liquid are stated, phosphorus content is no more than 0.01g/L.
3. the method according to claim 1 for preparing high-density large-particle ammonium poly-vanadate, it is characterised in that：In step a, institute
It is glycine to state bonding agent；In step a, the mass ratio of the bonding agent and total vanadium in low concentration vanadium liquid and high concentration vanadium liquid is
0.01~0.07.
4. the method according to claim 1 for preparing high-density large-particle ammonium poly-vanadate, it is characterised in that：In step a, institute
State a concentration of the 10~50% of sulfuric acid；In step a, system pH is 1.5~2.8 to the addition of the sulfuric acid in order to control.
5. the method according to claim 1 for preparing high-density large-particle ammonium poly-vanadate, it is characterised in that：In step a, institute
The temperature for stating heating and thermal insulation is 40 DEG C~60 DEG C, and the time is 40~60min.
6. the method according to claim 1 for preparing high-density large-particle ammonium poly-vanadate, it is characterised in that：In step a, institute
It is at least one of ammonium sulfate, ammonium hydrogen sulfate, ammonium chloride, ammonium oxalate, ammonium carbonate, ammonium hydrogen carbonate to state soluble inorganic ammonium salt；
NH in the soluble inorganic ammonium salt4 +Molar ratio with total vanadium in low concentration vanadium liquid and high concentration vanadium liquid is 1~2.
7. the method according to claim 1 for preparing high-density large-particle ammonium poly-vanadate, it is characterised in that：In step a, institute
The time for stating reaction is 40min~120min.
8. the method according to claim 1 for preparing high-density large-particle ammonium poly-vanadate, it is characterised in that：In step b, institute
The TV concentration for stating high concentration vanadium liquid is not less than 40g/L, and phosphorus content is no more than 0.01g/L；In step b, the high concentration vanadium liquid with
The volume ratio of low concentration vanadium liquid is 1 in step a：1~3.
9. the method according to claim 1 for preparing high-density large-particle ammonium poly-vanadate, it is characterised in that：In step b, institute
State a concentration of the 10~50% of sulfuric acid；In step b, system pH is 2.0~3.0 to the addition of the sulfuric acid in order to control.
10. the method for preparing high-density large-particle ammonium poly-vanadate according to claim 1~9 any one of them, it is characterised in that：
In step b, the time of the reaction is 20min~100min, and temperature is 80 DEG C~95 DEG C.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502823A (en) * | 2011-10-21 | 2012-06-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method for preparing high-tap density ammonium poly-vanadate |
| CN105236484A (en) * | 2015-10-20 | 2016-01-13 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of ammonium polyvanadate |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502823A (en) * | 2011-10-21 | 2012-06-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method for preparing high-tap density ammonium poly-vanadate |
| CN105236484A (en) * | 2015-10-20 | 2016-01-13 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of ammonium polyvanadate |
Non-Patent Citations (1)
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| 殷兆迁: "常温制备高密度多钒酸铵的技术研究", 《2015年中国化工学会年会论文集 》 * |
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