CN115744982B - Method for preparing large-particle ammonium polyvanadate from vanadium liquid low ammonium - Google Patents
Method for preparing large-particle ammonium polyvanadate from vanadium liquid low ammonium Download PDFInfo
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- CN115744982B CN115744982B CN202211425884.6A CN202211425884A CN115744982B CN 115744982 B CN115744982 B CN 115744982B CN 202211425884 A CN202211425884 A CN 202211425884A CN 115744982 B CN115744982 B CN 115744982B
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- vanadium
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 127
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 127
- 239000007788 liquid Substances 0.000 title claims abstract description 91
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 title claims abstract description 87
- 239000002245 particle Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 32
- 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
- 230000001105 regulatory effect Effects 0.000 claims abstract description 15
- 238000009835 boiling Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000011534 incubation Methods 0.000 claims description 3
- 150000003863 ammonium salts Chemical class 0.000 abstract description 13
- 239000000243 solution Substances 0.000 description 31
- 238000001556 precipitation Methods 0.000 description 10
- 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 6
- 230000008569 process Effects 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000003723 Smelting Methods 0.000 description 4
- 239000011230 binding agent Substances 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
- 239000002253 acid Substances 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
- 150000001413 amino acids Chemical class 0.000 description 3
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 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
- 230000001276 controlling effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000014509 gene expression Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 150000003388 sodium compounds Chemical class 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
- 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 1
- 230000002378 acidificating effect Effects 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
- 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
- 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
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 235000015598 salt intake Nutrition 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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 low ammonium, which comprises the following steps: s1, dividing vanadium liquid to be treated into two equal parts; s2, adding ammonium sulfate into the first part of vanadium liquid; s3, treating a second part of vanadium liquid, wherein the step S3 comprises the following steps in sequence: s31, regulating the pH value of the second vanadium liquid to 2-3; s32, stirring the second part of vanadium liquid at 60-80 ℃ for a preset time; s33, adding ammonium sulfate into the second vanadium liquid, and stirring for a preset time; s34, preserving the temperature of the second part of vanadium liquid at 88-92 ℃ for a preset time; s4, uniformly and rapidly adding the solution obtained in the step S2 into the solution obtained in the step S3 according to preset time; and S5, regulating the pH value of the solution obtained in the step S4 to 2-2.2, heating the solution with the regulated pH value to boiling, and then filtering and washing to obtain ammonium polyvanadate. The invention can obtain large-particle ammonium polyvanadate and reduce the ammonium salt dosage.
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 low ammonium.
Background
In the vanadium extraction process of the sodium salt of the vanadium slag, roasting, leaching and impurity removing are carried out on the vanadium slag to obtain sodium compound lattice 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 for the preparation of vanadium oxide products for ferrovanadium smelting, but generally only with a density of 0.6g/cm 3 The ammonium polyvanadate can meet the subsequent smelting requirement.
In the conventional acid ammonium salt vanadium precipitation process, ammonium sulfate is mostly used as a precipitator, the pH value is controlled to be 2.0, and ammonium polyvanadate is obtained under the boiling condition. In the process of precipitating ammonium polyvanadate, since sodium compound lattice liquid contains a large amount of sodium ions, in order to improve the vanadium precipitation rate and ensure the density and quality of products, excessive ammonium salt is often added, 70% of ammonium polyvanadate particles with the diameter of 50-150 um,30% of ammonium polyvanadate particles with the diameter of less than 50um, and sometimes even 10% of ammonium polyvanadate particles with the diameter of less than 10um are obtained, the particle diameters are small, the floating in supernatant is difficult to settle, the supernatant enters a wastewater tank, and vanadium loss is large. The prior technical method for preparing high-density large-particle ammonium polyvanadate by adopting vanadium liquid comprises the following steps: combining the low-concentration vanadium liquid with a binding agent or amino acid, and pouring the prepared high-concentration vanadium liquid and sulfuric acid into the low-concentration vanadium liquid. The method needs two vanadium liquids with different concentrations, needs binding agents or amino acids, has harsh conditions when being applied to the production of preparing high-density large-particle ammonium polyvanadate,
based on this, there is a need for techniques 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, which aims to solve the problems of harsh preparation conditions, low applicability and high ammonium salt dosage in the preparation of high-density large-particle ammonium polyvanadate in the prior art.
According to one aspect of the invention, a method for preparing large-particle ammonium polyvanadate from vanadium liquid low ammonium is provided, comprising the following steps:
s1, dividing vanadium liquid to be treated into two equal parts;
s2, adding ammonium sulfate into the first part of vanadium liquid;
s3, treating a second part of vanadium liquid, wherein the step S3 comprises the following steps in sequence:
s31, regulating the pH value of the second vanadium liquid to 2-3;
s32, stirring the second part of vanadium liquid at 60-80 ℃ for a preset time;
s33, adding ammonium sulfate into the second vanadium liquid, and stirring for a preset time;
s34, preserving the temperature 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, regulating the pH value of the solution obtained in the step S4 to 2-2.2, heating the solution with the regulated pH value to boiling, and then filtering and washing to obtain ammonium polyvanadate.
According to one embodiment of the present invention, in step S1, the temperature of the vanadium liquid to be treated is controlled to be within a range of 80 ℃ or less.
According to one embodiment of the invention, in 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 to the first vanadium liquid according to an ammonium addition coefficient of 0.3-0.4; in the step S33, adding ammonium sulfate into the second vanadium liquid according to the ammonium addition coefficient of 0.3-0.4; wherein the ammonium addition coefficient is the ratio of the mass of ammonium sulfate added 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 to 50 minutes.
According to one embodiment of the present invention, in step S33, the stirring time is 15 to 30 minutes.
According to one embodiment of the present invention, in step S34, the incubation time is 15 to 30 minutes.
According to one embodiment of the present invention, in step S4, the predetermined time is 15 to 30 minutes.
According to one embodiment of the invention, in step S5, the solution is kept boiling for a period of 30 to 40 minutes.
According to one embodiment of the invention, the particle size of the large-particle ammonium polyvanadate is 150um or more
In the method for preparing large-particle ammonium polyvanadate from the vanadium liquid with low ammonium content, according to the embodiment of the invention, the vanadium liquid is added in two steps, and the large-particle ammonium polyvanadate is obtained by controlling the temperature, the acid regulation and the ammonium addition of the vanadium liquid and realizing low-ammonium-coefficient vanadium precipitation.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 shows a flow chart of a method for preparing large-particle ammonium polyvanadate from vanadium liquid low ammonium according to an embodiment of the invention;
fig. 2 shows a schematic representation of large particle ammonium polyvanadate prepared using the method of the examples 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 will be described in further detail with reference to the accompanying drawings.
It should be noted that, in the embodiments of the present invention, all the expressions "first" and "second" are used to distinguish two entities with the same name but different entities or different parameters, and it is noted that the "first" and "second" are only used for convenience of expression, and should not be construed as limiting the embodiments of the present invention, and the following embodiments are not described one by one.
The inventor of the application realizes that in the prior art, regarding the preparation of high-density large-particle ammonium polyvanadate, two concentrations of vanadium solution are needed, and a binding agent or amino acid is needed to be added, the application range of the vanadium concentration of the vanadium solution is narrow, the vanadium solution is only suitable for one dilute vanadium solution and one concentrated vanadium solution, and the ammonium salt dosage is more. The invention proposes a method to achieve low ammonium coefficient vanadium precipitation to obtain large-particle ammonium polyvanadate as will be described below.
FIG. 1 shows a flow chart of a method for preparing large-particle ammonium polyvanadate from vanadium liquid low ammonium according to an embodiment of the invention. As shown in fig. 1, the method comprises the steps of:
s1, dividing vanadium liquid to be treated into two equal parts;
s2, adding ammonium sulfate into the first part of vanadium liquid;
s3, treating a second part of vanadium liquid, wherein the step S3 comprises the following steps in sequence:
s31, regulating the pH value of the second vanadium liquid to 2-3;
s32, stirring the second part of vanadium liquid at 60-80 ℃ for a preset time;
s33, adding ammonium sulfate into the second vanadium liquid, and stirring for a preset time;
s34, preserving the temperature 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, regulating the pH value of the solution obtained in the step S4 to 2-2.2, heating the solution with the regulated pH value to boiling, and then filtering and washing to obtain ammonium polyvanadate.
In the method for preparing large-particle ammonium polyvanadate from the vanadium liquid with low ammonium content, according to the embodiment of the invention, the vanadium liquid is added in two steps, and the large-particle ammonium polyvanadate is obtained by controlling the temperature, the acid regulation and the ammonium addition of the vanadium liquid and realizing low-ammonium-coefficient vanadium precipitation. Not only can large-particle ammonium polyvanadate be prepared, but also the dosage of ammonium salt can be reduced, and the production cost is obviously reduced. In addition, the density of 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 is not limited to the sequence of the step S2 and the step S3, and the two steps can be sequentially performed or synchronously performed.
According to the invention, the vanadium liquid to be treated is divided into two equal parts, and the ammonium salt is added to each part of vanadium liquid, so that the full utilization of the ammonium salt can be ensured, and the use amount of the ammonium salt is reduced. And for the second part of vanadium liquid, the pH value of the second part of vanadium liquid is adjusted to be 2-3 in the step S31, so that the vanadium liquid is in a proper aggregation state, and then after the treatment in the step S32, the vanadium aggregation state part in the vanadium liquid is subjected to hydrolysis reaction, so that vanadium pentoxide is generated. Then, adding ammonium sulfate in the step S33 and carrying out heat preservation in the step S34, reacting the aggregated vanadium with ammonium salt to form ammonium polyvanadate, reacting part of vanadium pentoxide with ammonium salt to form ammonium polyvanadate, converting the ammonium polyvanadate into ammonium polyvanadate, and obtaining ammonium polyvanadate crystal nuclei with different mechanisms due to the fact that the aggregated vanadium is complex and different in formation mechanisms, and then, continuously wrapping and growing at the periphery of the crystal nuclei under the action of vanadium liquid added with ammonium sulfate after the treatment of the step S4 and the step S5, so that vanadium can be precipitated to obtain large-particle ammonium polyvanadate.
Fig. 2 shows a schematic representation of large particle ammonium polyvanadate prepared using the method of the examples of the invention. As shown in fig. 2, ammonium polyvanadate appears to the naked eye to be visibly particulate. In the invention, the particle size of the large-particle ammonium polyvanadate is more than or equal to 150um.
In the embodiment of the present invention, in step S1, the temperature of the vanadium liquid to be treated is controlled to be in the range of 80 ℃ or lower. Thus, the vanadium liquid can be prevented from generating unwanted reaction with the ammonium sulfate at high temperature.
In the prior art, the sodium vanadium solution is used for preparing large-particle ammonium polyvanadate, and the low-concentration vanadium solution and the high-concentration vanadium solution are required to be combined, so that special requirements on the concentration of the vanadium solution are met. The vanadium concentration range 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 the step S33, adding ammonium sulfate into the second vanadium liquid according to the ammonium addition coefficient of 0.3-0.4; wherein the ammonium addition coefficient is the ratio of the mass of ammonium sulfate added to the total mass of vanadium in the vanadium liquid to be treated. Therefore, the ammonium addition coefficient K of the invention is 0.6-0.8, the ammonium salt consumption 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 the vanadium in the second part of vanadium liquid is fully and 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 and the vanadium solution are fully contacted and reacted.
In some embodiments, in step S34, the incubation time is 15-30 minutes.
In the step S4, the solution obtained in the step S2 is slowly added into the solution obtained in the step S3 according to the preset time, so that the phenomenon that the density of ammonium polyvanadate is influenced due to the fact that ammonium salt and vanadium liquid are quickly and widely contacted to generate a large amount of floccules can be avoided. In some embodiments, the predetermined time in step S4 is 15-30 min, and the average speed is determined by the ratio of the volume of vanadium liquid to be treated to the predetermined time.
In some embodiments, in step S5, the solution is kept boiling for 30-40 min, ensuring sufficient vanadium precipitation.
According to the above description, the present invention has the following advantages: the ammonium polyvanadate obtained in the step (1) 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 ammonium salt dosage is small, so that the production cost can be obviously reduced. In addition, the method provided by the invention is suitable for a wider concentration range of vanadium in the vanadium liquid, and no binding agent is needed.
The following description is made with reference to specific examples.
The composition of the vanadium sodium salt solution in each example is shown in table 1.
TABLE 1 sodium vanadium solution composition/g.L -1
Wherein the original pH value of vanadium vanadate solution 1 is 10.75; the original pH value of vanadium vanadate solution 2 is 11.0; the original pH value of the vanadium vanadate solution 3 is 11.45.
Example 1
100mL of sodium vanadium solution 1 at 60 ℃ and divided into two equal parts; adding ammonium sulfate with an ammonium addition coefficient of 0.3 into an equal part of vanadium liquid for standby; adjusting another equal part of vanadium liquid to pH=2 by sulfuric acid, and stirring for 30min at 60 ℃; adding ammonium sulfate with the ammonium addition coefficient of 0.3, and continuously stirring for 15min; heating to 88 ℃ after the completion of the process, preserving the heat for 15min, and adding vanadium liquid for later use after 10 min; and regulating the pH value of the mixed vanadium liquid to 2, continuously heating to boiling for 30min, and filtering and washing to obtain the large-particle ammonium polyvanadate. The vanadium precipitation rate is 99.12 percent, and the ammonium polyvanadate bulk density is 0.67g/cm 3 The particle size is more than or equal to 180um.
Example 2
100mL of sodium vanadium solution 2 at 73 ℃ and divided into two equal parts; adding ammonium sulfate with an ammonium addition coefficient of 0.35 into an equal part of vanadium liquid for standby; adjusting another equal part of vanadium liquid to pH=2.5 by sulfuric acid, and stirring at 70 ℃ for 380min; adding ammonium sulfate with the ammonium addition coefficient of 0.35, and continuously stirring for 20min; heating to 90 ℃ after the completion of the process, preserving heat for 20min, and adding vanadium liquid for later use after 13 min; and regulating the pH value of the mixed vanadium liquid to 2.05, continuously heating to boiling for 35min, and filtering and washing to obtain the large-particle ammonium polyvanadate. The vanadium precipitation rate is 99.33 percent, and the poly-vanadateAmmonium bulk Density 0.71g/cm 3 The particle size is more than or equal to 160um.
Example 3
1000mL of sodium vanadium solution 3 at 80 ℃ and divided into two equal parts; adding ammonium sulfate with an ammonium addition coefficient of 0.4 into an equal part of vanadium liquid for standby; adjusting another equal part of vanadium liquid to pH=3 by sulfuric acid, and stirring for 50min at 80 ℃; adding ammonium sulfate with the ammonium addition coefficient of 0.4, and continuously stirring for 30min; heating to 92 ℃ after the completion of the process, preserving the heat for 30min, and adding vanadium liquid for later use after 15min; and regulating the pH value of the mixed vanadium liquid to 2.2, continuously heating to boiling for 40min, and filtering and washing to obtain the large-particle ammonium polyvanadate. The vanadium precipitation rate is 99.55 percent, and the bulk density of ammonium polyvanadate is 0.72g/cm 3 The particle size is more than or equal to 150um.
Those of ordinary skill in the art will appreciate that: the above discussion of any embodiment is merely exemplary and is not intended to imply that the scope of the disclosure of embodiments of the invention, including the claims, is limited to such examples; combinations of features of the above embodiments or in different embodiments are also possible within the idea of an embodiment of the invention, and there are many other variations of the different aspects of the embodiments of the invention as described above, which are not provided in detail for the sake of brevity. Therefore, any omissions, modifications, equivalent substitutions, improvements, and the like, which are made within the spirit and principles of the embodiments of the invention, are included within the scope of the embodiments of the invention.
Claims (7)
1. The method for preparing large-particle ammonium polyvanadate from low ammonium content vanadium liquid is characterized by comprising the following steps of:
s1, dividing vanadium liquid to be treated into two equal parts;
s2, adding ammonium sulfate into the first part of vanadium liquid;
s3, treating a second part of vanadium liquid, wherein the step S3 comprises the following steps in sequence:
s31, regulating the pH value of the second vanadium liquid to 2-3;
s32, stirring the second part of vanadium liquid at 60-80 ℃ for a preset time;
s33, adding ammonium sulfate into the second vanadium liquid, and stirring for a preset time;
s34, preserving the temperature 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;
s5, regulating the pH value of the solution obtained in the step S4 to 2-2.2, heating the solution with the regulated pH value to boiling, and then filtering and washing to obtain ammonium polyvanadate;
in the step S2, adding ammonium sulfate into the first part of vanadium liquid according to the ammonium addition coefficient of 0.3-0.4; in the step S33, adding ammonium sulfate into the second vanadium liquid according to the ammonium addition coefficient of 0.3-0.4; wherein the ammonium addition coefficient is the ratio of the mass of ammonium sulfate added to the total mass of vanadium in the vanadium liquid to be treated;
the particle size of the large-particle ammonium polyvanadate is more than or equal to 150 mu m;
in the step S1, the temperature of the vanadium liquid to be treated is controlled to be within the range of 80 ℃ or lower.
2. 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.
3. The method according to claim 1, wherein the stirring time is 30 to 50 minutes in step S32.
4. The method according to claim 1, wherein in step S33, the stirring time is 15 to 30 minutes.
5. The method according to claim 1, wherein in step S34, the incubation time is 15 to 30min.
6. The method according to claim 1, wherein in step S4, the predetermined time is 15-30 min.
7. The method according to claim 1, wherein in step S5, the solution is kept boiling for a period of 30 to 40 minutes.
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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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