CN115744982A - Method for preparing large-particle ammonium polyvanadate from vanadium liquid with low ammonium content - Google Patents
Method for preparing large-particle ammonium polyvanadate from vanadium liquid with low ammonium content Download PDFInfo
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- CN115744982A CN115744982A CN202211425884.6A CN202211425884A CN115744982A CN 115744982 A CN115744982 A CN 115744982A CN 202211425884 A CN202211425884 A CN 202211425884A CN 115744982 A CN115744982 A CN 115744982A
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- vanadium
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 123
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 123
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 title claims abstract description 92
- 239000007788 liquid Substances 0.000 title claims abstract description 61
- 239000002245 particle Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 33
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 28
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 238000009835 boiling Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 150000003863 ammonium salts Chemical class 0.000 abstract description 13
- 238000001556 precipitation Methods 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- CFVBFMMHFBHNPZ-UHFFFAOYSA-N [Na].[V] Chemical compound [Na].[V] CFVBFMMHFBHNPZ-UHFFFAOYSA-N 0.000 description 8
- 230000002776 aggregation Effects 0.000 description 5
- 238000004220 aggregation Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000003723 Smelting Methods 0.000 description 4
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 3
- 150000001413 amino acids Chemical class 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910001935 vanadium oxide Inorganic materials 0.000 description 3
- VWBLQUSTSLXQON-UHFFFAOYSA-N N.[V+5] Chemical compound N.[V+5] VWBLQUSTSLXQON-UHFFFAOYSA-N 0.000 description 2
- 229910000756 V alloy Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000007767 bonding agent Substances 0.000 description 2
- 230000014509 gene expression Effects 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 229910000628 Ferrovanadium Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000015598 salt intake Nutrition 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for preparing large-particle ammonium polyvanadate from vanadium liquid with low ammonium content, which comprises the following steps: s1, dividing a vanadium liquid to be treated into two equal parts; s2, adding ammonium sulfate into the first part of vanadium liquid; and S3, treating the second part of vanadium liquid, wherein the step S3 comprises the following steps in sequence: s31, adjusting the pH value of the second vanadium solution to 2-3; s32, stirring the second part of vanadium solution at the temperature of between 60 and 80 ℃ for preset time; s33, adding ammonium sulfate into the second part of vanadium solution, and stirring for a preset time; s34, preserving the heat of the second part of vanadium liquid at 88-92 ℃ for a preset time; s4, adding the solution obtained in the step S2 into the solution obtained in the step S3 at a constant speed according to preset time; and S5, adjusting the pH value of the solution obtained in the step S4 to 2-2.2, heating the solution after the pH value is adjusted to boiling, and then filtering and washing to obtain ammonium polyvanadate. The invention can obtain large-particle ammonium polyvanadate and can reduce the dosage of ammonium salt.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a method for preparing large-particle ammonium polyvanadate from vanadium liquid with low ammonium content.
Background
In the vanadium slag sodium salt vanadium extraction process, vanadium slag is subjected to roasting, water leaching and impurity removal to obtain qualified sodium salt vanadium liquid, and the qualified vanadium liquid is subjected to an acidic ammonium salt vanadium precipitation process to obtain Ammonium Polyvanadate (APV). One of the main uses of ammonium polyvanadate is in the preparation of vanadium oxide products for ferrovanadium smelting, but generally only at densities of 0.6g/cm 3 The ammonium polyvanadate can meet the requirements of subsequent smelting.
In the conventional acidic ammonium salt vanadium precipitation process, ammonium sulfate is mostly used as a precipitator, the pH is controlled to be 2.0, and ammonium polyvanadate is obtained under the boiling condition. In the process of precipitating ammonium polyvanadate, because sodium-modified qualified liquid contains a large amount of sodium ions, in order to improve the vanadium precipitation rate and ensure the product density and quality, excessive ammonium salt is often added, 70% of the obtained ammonium polyvanadate particles have the diameter of 50-150um, 30% of the obtained ammonium polyvanadate particles have the diameter of less than 50um, and sometimes even 10% of the obtained ammonium polyvanadate particles have the diameter of less than 10um, and the particles have small diameters, so that the ammonium polyvanadate particles are easy to float in supernatant liquid and difficult to precipitate, and enter a wastewater pool along with the supernatant liquid, and the vanadium loss is large. The prior technical method for preparing high-density large-particle ammonium polyvanadate by adopting vanadium liquid comprises the following steps: the low-concentration vanadium solution is combined with a binding agent or amino acid, and then the adjusted high-concentration vanadium solution and sulfuric acid are poured into the low-concentration vanadium solution. The method needs two vanadium liquids with different concentrations and a binding agent or amino acid, has harsh conditions for preparing high-density large-particle ammonium polyvanadate in production,
based on this, there is a need for a technique suitable for improving ammonium polyvanadate particles in production.
Disclosure of Invention
The invention mainly aims to provide a method for preparing large-particle ammonium polyvanadate from vanadium liquid with low ammonium content, so as to solve the problems of harsh preparation conditions, low applicability and high ammonium salt consumption in the prior art when preparing high-density large-particle ammonium polyvanadate.
According to one aspect of the invention, a method for preparing large-particle ammonium polyvanadate from vanadium liquid with low ammonium content is provided, which comprises the following steps:
s1, dividing vanadium liquid to be treated into two equal parts;
s2, adding ammonium sulfate into the first vanadium solution;
and S3, treating the second part of vanadium liquid, wherein the step S3 comprises the following steps in sequence:
s31, adjusting the pH value of the second vanadium solution to 2-3;
s32, stirring the second part of vanadium solution at the temperature of between 60 and 80 ℃ for preset time;
s33, adding ammonium sulfate into the second part of vanadium solution, and stirring for a preset time;
s34, preserving the heat of the second part of vanadium liquid at 88-92 ℃ for a preset time;
s4, adding the solution obtained in the step S2 into the solution obtained in the step S3 according to preset time;
and S5, adjusting the pH value of the solution obtained in the step S4 to 2-2.2, heating the solution after the pH value is adjusted to boiling, and then filtering and washing to obtain ammonium polyvanadate.
According to one embodiment of the invention, in the step S1, the temperature of the vanadium liquid to be treated is controlled within the range of 80 ℃ or lower.
According to one embodiment of the invention, in the step S1, the vanadium content of the vanadium liquid to be treated is 10-65 g/L.
According to one embodiment of the invention, in step S2, ammonium sulfate is added into the first part of vanadium solution according to the ammonium addition coefficient of 0.3-0.4; in step S33, adding ammonium sulfate into the second part of vanadium solution according to the ammonium addition coefficient of 0.3-0.4; wherein the ammonium adding coefficient is the ratio of the mass of the added ammonium sulfate to the total mass of vanadium in the vanadium liquid to be treated.
According to one embodiment of the present invention, in step S32, the stirring time is 30-50 min.
According to one embodiment of the present invention, in step S33, the stirring time is 15 to 30min.
According to an embodiment of the present invention, in step S34, the holding time is 15-30 min.
According to an embodiment of the present invention, in step S4, the predetermined time is 15 to 30min.
According to one embodiment of the invention, in step S5, the solution is kept boiling for 30 to 40min.
According to one embodiment of the present invention, the particle size of the large-particle ammonium polyvanadate is greater than or equal to 150um
According to the method for preparing large-particle ammonium polyvanadate from vanadium liquid with low ammonium content, the vanadium liquid is added in two steps, and the vanadium precipitation with low ammonium coefficient is realized by controlling the temperature of the vanadium liquid, an acid regulation system and an ammonium addition system, so that the large-particle ammonium polyvanadate is obtained.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of a method for preparing large-particle ammonium polyvanadate from vanadium liquid with low ammonium content according to an embodiment of the invention;
FIG. 2 shows a schematic of large particle ammonium polyvanadate prepared by a method according to an embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following embodiments of the present invention are described in further detail with reference to the accompanying drawings.
It should be noted that all expressions using "first" and "second" in the embodiments of the present invention are used for distinguishing two entities with the same name but different names or different parameters, and it should be noted that "first" and "second" are only used for convenience of expression and should not be construed as a limitation to the embodiments of the present invention, and no description is given in the following embodiments.
The inventor of the application realizes that in the prior art, regarding the preparation of high-density large-particle ammonium polyvanadate, two kinds of vanadium solutions with different concentrations are needed, and a bonding agent or amino acid needs to be added, the vanadium concentration of the vanadium solution has a narrow application range, and is only suitable for one kind of dilute vanadium solution and one kind of concentrated vanadium solution, and the dosage of ammonium salt is large. The invention provides a method to be described below to realize low ammonium coefficient vanadium precipitation and obtain large-particle ammonium polyvanadate.
Fig. 1 shows a flow chart of a method for preparing large-particle ammonium polyvanadate from vanadium liquid with low ammonium content according to an embodiment of the invention. As shown in fig. 1, the method comprises the steps of:
s1, dividing a vanadium liquid to be treated into two equal parts;
s2, adding ammonium sulfate into the first part of vanadium liquid;
and S3, treating the second part of vanadium liquid, wherein the step S3 comprises the following steps in sequence:
s31, adjusting the pH value of the second vanadium solution to 2-3;
s32, stirring the second part of vanadium solution at the temperature of between 60 and 80 ℃ for preset time;
s33, adding ammonium sulfate into the second part of vanadium solution, and stirring for a preset time;
s34, preserving the heat of the second part of vanadium liquid at 88-92 ℃ for a preset time;
s4, adding the solution obtained in the step S2 into the solution obtained in the step S3 according to preset time;
and S5, adjusting the pH value of the solution obtained in the step S4 to 2-2.2, heating the solution after the pH value is adjusted to boiling, and then filtering and washing to obtain ammonium polyvanadate.
According to the method for preparing large-particle ammonium polyvanadate from vanadium liquid with low ammonium content, the vanadium liquid is added in two steps, and the vanadium precipitation with low ammonium coefficient is realized by controlling the temperature of the vanadium liquid, an acid regulation system and an ammonium addition system, so that the large-particle ammonium polyvanadate is obtained. Not only can prepare large-particle ammonium polyvanadate, but also can reduce the dosage of ammonium salt and obviously reduce the production cost. In addition, the density of the ammonium polyvanadate prepared by the method is more than or equal to 0.6g/L, and the ammonium polyvanadate can be applied to vanadium alloy smelting. The invention does not limit the sequence of the step S2 and the step S3, and the steps can be carried out sequentially or synchronously.
According to the invention, the vanadium liquid to be treated is divided into two equal parts, and ammonium salt is added to each part of vanadium liquid, so that the ammonium salt can be fully utilized, and the reduction of the ammonium salt dosage is facilitated. And (3) adjusting the pH value of the second part of vanadium liquid to 2-3 in step S31 to enable the vanadium liquid to be in a proper aggregation state, and then performing hydrolysis reaction on part of the aggregation state of vanadium in the vanadium liquid after the treatment in step S32 to generate vanadium pentoxide. After the ammonium sulfate is added in step S33 and the heat preservation is performed in step S34, the aggregation vanadium and the ammonium salt react to form ammonium polyvanadate, part of vanadium pentoxide also reacts with the ammonium salt to form ammonium polyvanadate, the ammonium polyvanadate is converted into ammonium polyvanadate, the formation mechanism is different due to the complex aggregation state of vanadium, the obtained ammonium polyvanadate crystal nucleus is different, and then the ammonium polyvanadate crystal nucleus is continuously wrapped and grown on the periphery of the crystal nucleus under the action of the vanadium liquid further added with the ammonium sulfate after the treatment in step S4 and step S5, so that large-particle ammonium polyvanadate can be obtained by precipitating vanadium.
FIG. 2 shows a schematic of large particle ammonium polyvanadate prepared by a method according to an embodiment of the invention. As shown in FIG. 2, the ammonium polyvanadate appeared to be visibly distinct in particle form. In the invention, the particle size of the large-particle ammonium polyvanadate is larger than or equal to 150um.
In the embodiment of the invention, in the step S1, the temperature of the vanadium liquid to be treated is controlled within the range of 80 ℃ or lower. Thus, the undesirable reaction of the vanadium liquid and the ammonium sulfate at high temperature can be avoided.
In the prior art, the preparation of large-particle ammonium polyvanadate from a sodium vanadium solution needs to combine a low-concentration vanadium solution and a high-concentration vanadium solution, and has special requirements on the concentration of the vanadium solution. The method disclosed by the invention is suitable for a wide vanadium concentration range of the vanadium liquid, and in the embodiment of the invention, the vanadium content of the vanadium liquid to be treated in the step S1 can be 10-65 g/L. The phosphorus content of the vanadium liquid to be treated can be less than or equal to 0.015g/L.
In the embodiment of the invention, in the step S2, ammonium sulfate is added into the first part of vanadium liquid according to the ammonium addition coefficient of 0.3-0.4; in step S33, adding ammonium sulfate into the second part of vanadium solution according to the ammonium addition coefficient of 0.3-0.4; wherein the ammonium adding coefficient is the ratio of the mass of the added ammonium sulfate to the total mass of vanadium in the vanadium liquid to be treated. Therefore, the coefficient K of adding ammonium is 0.6-0.8, the dosage of ammonium salt is reduced by more than 50%, and the production cost can be obviously reduced.
In some embodiments, in step S32, the stirring time is 30-50 min, so as to ensure that all vanadium in the second vanadium solution is fully in a corresponding aggregation state.
In some embodiments, in step S33, the stirring time is 15-30 min, so as to ensure that the ammonium sulfate is fully contacted and reacted with the vanadium solution.
In some embodiments, in step S34, the holding time is 15 to 30min.
In step S4, the solution obtained in step S2 is slowly added to the solution obtained in step S3 according to a predetermined time average rate, so as to avoid the ammonium salt from rapidly contacting with the vanadium solution in a large range to generate a large amount of floccules, which affects the density of the ammonium polyvanadate. In some embodiments, the predetermined time in step S4 is 15-30 min, and the uniform speed is determined by the ratio of the volume of the vanadium liquid to be treated to the predetermined time.
In some embodiments, in step S5, the solution is kept boiling for 30-40 min to ensure sufficient vanadium precipitation.
According to the above description, the present invention has the following advantages: the obtained ammonium polyvanadate has large particles; (2) The density of the obtained ammonium polyvanadate is more than or equal to 0.67g/L, and the ammonium polyvanadate can be applied to vanadium alloy smelting; and (3) the dosage of ammonium salt is small, so that the production cost can be obviously reduced. In addition, the method of the invention is suitable for a wide vanadium concentration range of the vanadium liquid, and does not need to add a bonding agent.
The following description is based on specific examples.
The components of the sodium vanadium solution in each example are shown in table 1.
TABLE 1 sodium vanadium solution composition/g.L -1
Wherein the original pH value of the vanadium solution 1 is 10.75; the original pH value of the vanadium oxide solution 2 is 11.0; the original pH value of vanadium oxide solution 3 was 11.45.
Example 1
100mL of sodium vanadium solution 1 at 60 ℃ is divided into two equal parts; an equal partAdding ammonium sulfate with an ammonium addition coefficient of 0.3 into the vanadium liquid for later use; adjusting another equal part of vanadium solution to pH =2 with sulfuric acid, and stirring for 30min at 60 ℃; then adding ammonium sulfate with the ammonium coefficient of 0.3, and continuing stirring for 15min; after the end, heating to 88 ℃, preserving the heat for 15min, and adding the vanadium solution for later use for 10 min; and adjusting the pH value of the mixed vanadium solution to 2, continuing to heat to boil for 30min, filtering and washing to obtain large-particle ammonium polyvanadate. The vanadium precipitation rate is 99.12 percent, and the bulk density of the ammonium polyvanadate is 0.67g/cm 3 The particle size of the particles is more than or equal to 180um.
Example 2
100mL of sodium vanadium solution 2 at 73 ℃, and dividing into two equal parts; adding ammonium sulfate with the ammonium addition coefficient of 0.35 into one equal part of vanadium liquid for standby; adjusting another equal part of vanadium solution to pH =2.5 with sulfuric acid, and stirring for 380min at 70 ℃; then adding ammonium sulfate with the ammonium coefficient of 0.35, and continuing stirring for 20min; after finishing, heating to 90 ℃, preserving the heat for 20min, and adding the vanadium solution for later use for 13 min; and adjusting the pH value of the mixed vanadium solution to 2.05, continuing to heat to boil for 35min, and filtering and washing to obtain large-particle ammonium polyvanadate. The vanadium deposition rate is 99.33 percent, and the bulk density of the ammonium polyvanadate is 0.71g/cm 3 The particle size is not less than 160um.
Example 3
1000mL of sodium vanadium solution 3 at 80 ℃ is divided into two equal parts; adding ammonium sulfate with the ammonium addition coefficient of 0.4 into one equal part of vanadium liquid for standby; adjusting another equal part of vanadium solution to pH =3 with sulfuric acid, and stirring for 50min at 80 ℃; then adding ammonium sulfate with the ammonium coefficient of 0.4, and continuing stirring for 30min; after the end, heating to 92 ℃, preserving the heat for 30min, and adding the vanadium solution for later use after 15min; and adjusting the pH value of the mixed vanadium solution to 2.2, continuing to heat to boil for 40min, and filtering and washing to obtain large-particle ammonium polyvanadate. The vanadium precipitation rate is 99.55 percent, and the bulk density of the ammonium polyvanadate is 0.72g/cm 3 The particle size is not less than 150um.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, of embodiments of the invention is limited to these examples; within the idea of an embodiment of the invention, also technical features in the above embodiment or in different embodiments may be combined and there are many other variations of the different aspects of an embodiment of the invention as described above, which are not provided in detail for the sake of brevity. Therefore, any omissions, modifications, substitutions, improvements, and the like that may be made without departing from the spirit and principles of the embodiments of the present invention are intended to be included within the scope of the embodiments of the present invention.
Claims (10)
1. A method for preparing large-particle ammonium polyvanadate from vanadium liquid with low ammonium content is characterized by comprising the following steps:
s1, dividing a vanadium liquid to be treated into two equal parts;
s2, adding ammonium sulfate into the first part of vanadium liquid;
and S3, treating the second part of vanadium liquid, wherein the step S3 comprises the following steps in sequence:
s31, adjusting the pH value of the second vanadium solution to 2-3;
s32, stirring the second part of vanadium solution at the temperature of between 60 and 80 ℃ for preset time;
s33, adding ammonium sulfate into the second part of vanadium solution, and stirring for a preset time;
s34, preserving the heat of the second part of vanadium liquid at 88-92 ℃ for a preset time;
s4, adding the solution obtained in the step S2 into the solution obtained in the step S3 according to preset time;
and S5, adjusting the pH value of the solution obtained in the step S4 to 2-2.2, heating the solution after the pH value is adjusted to boiling, and then filtering and washing to obtain ammonium polyvanadate.
2. The method according to claim 1, characterized in that in step S1, the temperature of the vanadium liquid to be treated is controlled within a range of 80 ℃ or less.
3. The method according to claim 1, wherein in step S1, the vanadium content of the vanadium liquid to be treated is 10-65 g/L.
4. The method according to claim 1, wherein in step S2, ammonium sulfate is added to the first portion of vanadium solution according to an ammonium addition coefficient of 0.3 to 0.4; in step S33, adding ammonium sulfate into the second part of vanadium solution according to the ammonium addition coefficient of 0.3-0.4; wherein the ammonium adding coefficient is the ratio of the mass of the added ammonium sulfate to the total mass of vanadium in the vanadium liquid to be treated.
5. The method according to claim 1, wherein the stirring time in step S32 is 30 to 50min.
6. The method according to claim 1, wherein the stirring time in step S33 is 15 to 30min.
7. The method according to claim 1, wherein the holding time in step S34 is 15 to 30min.
8. The method according to claim 1, wherein the predetermined time is 15 to 30min in step S4.
9. The method of claim 1, wherein in step S5, the solution is kept boiling for 30-40 min.
10. The method of claim 1, wherein the large ammonium polyvanadate has particle size of 150um or greater.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN112047379A (en) * | 2020-09-14 | 2020-12-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for precipitating ammonium polyvanadate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN112047379A (en) * | 2020-09-14 | 2020-12-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for precipitating ammonium polyvanadate |
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