CN115626661B - Method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid and low ammonium - Google Patents
Method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid and low ammonium Download PDFInfo
- Publication number
- CN115626661B CN115626661B CN202211425898.8A CN202211425898A CN115626661B CN 115626661 B CN115626661 B CN 115626661B CN 202211425898 A CN202211425898 A CN 202211425898A CN 115626661 B CN115626661 B CN 115626661B
- Authority
- CN
- China
- Prior art keywords
- vanadium
- ammonium
- vanadium liquid
- liquid
- tank
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 223
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 222
- 239000007788 liquid Substances 0.000 title claims abstract description 141
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 title claims abstract description 88
- 238000000034 method Methods 0.000 title claims abstract description 27
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 38
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 38
- 230000001105 regulatory effect Effects 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000009835 boiling Methods 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims description 30
- 239000002253 acid Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 15
- 239000012535 impurity Substances 0.000 claims description 5
- 238000002386 leaching Methods 0.000 claims description 4
- 150000003863 ammonium salts Chemical class 0.000 abstract description 30
- 235000015598 salt intake Nutrition 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 35
- 230000001376 precipitating effect Effects 0.000 description 26
- 239000013078 crystal Substances 0.000 description 16
- CFVBFMMHFBHNPZ-UHFFFAOYSA-N [Na].[V] Chemical group [Na].[V] CFVBFMMHFBHNPZ-UHFFFAOYSA-N 0.000 description 8
- 230000002776 aggregation Effects 0.000 description 5
- 238000004220 aggregation Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- VWBLQUSTSLXQON-UHFFFAOYSA-N N.[V+5] Chemical compound N.[V+5] VWBLQUSTSLXQON-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 230000014509 gene expression Effects 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 150000003388 sodium compounds Chemical class 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000004065 wastewater treatment Methods 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
- JUKIIDKZGXLPGL-UHFFFAOYSA-N [N].N.[V] Chemical compound [N].N.[V] JUKIIDKZGXLPGL-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
- 239000000654 additive Substances 0.000 description 1
- 239000001166 ammonium sulphate Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000000926 separation method Methods 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
- 150000003682 vanadium compounds Chemical class 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid and low ammonium, which comprises the following steps: s1, dividing vanadium liquid to be treated at 60-85 ℃ into three parts; s2, adjusting the pH value of the first vanadium liquid to be 4-5.5; s3, adjusting the pH value of the second part of vanadium liquid to be 4-5.5, and then adding ammonium sulfate into the second part of vanadium liquid according to the ammonium addition coefficient of 0.5-0.8, wherein the volume of the second part of vanadium liquid is 10% -15% of the volume of vanadium liquid to be treated; s4, adding the solution obtained in the step S3 into the solution obtained in the step S2; s5, regulating the pH value of the solution obtained in the step S4 to 2.0-2.05, and then preserving heat at 80-90 ℃; s6, adding ammonium sulfate into the third vanadium liquid; s7, adding the solution obtained in the step S6 into the solution obtained in the step S5; and S8, heating the solution obtained in the step S7 to boiling, filtering and washing to obtain ammonium polyvanadate. The invention can deposit vanadium in high temperature vanadium liquid, reduce the ammonium salt consumption and obtain high density ammonium polyvanadate.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid and 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, the ammonium polyvanadate is extractedHigh vanadium deposition rate and product quality, often with excessive addition of ammonium salt, and in order to obtain high density (ρ > 0.6 g/cm) 3 ) The ammonium salt is generally used in higher amounts. Most of the excessive ammonium salt enters the vanadium precipitation wastewater to obtain high ammonia nitrogen vanadium precipitation wastewater, and the wastewater treatment cost is increased. In addition, in the prior art, vanadium-containing solution mainly used for precipitating vanadium is sodium vanadium solution, the temperature of the sodium vanadium solution is generally 60 ℃ or even up to 75 ℃ through a leaching-impurity removing process, and the high-density ammonium polyvanadate is prepared by generally adopting higher ammonium salt addition amount, so that the effect of preparing the high-density ammonium polyvanadate is achieved, and the high-temperature vanadium solution contacts a large amount of ammonium salt, so that the overflow of ammonium can be caused, the vanadium precipitating environment is influenced, and the health of personnel is endangered.
Disclosure of Invention
The invention mainly aims to provide a method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid and low ammonium, so as to solve the problems that the wastewater treatment cost is increased and the vanadium precipitation environment is influenced by ammonium salt overflow caused by excessively high ammonium salt consumption in the preparation of high-density ammonium polyvanadate.
According to one aspect of the invention, a method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid and low ammonium is provided, which comprises the following steps:
s1, dividing vanadium liquid to be treated at 60-85 ℃ into three parts;
s2, adjusting the pH value of the first vanadium liquid to be 4-5.5;
s3, adjusting the pH value of the second part of vanadium liquid to be 4-5.5, and then adding ammonium sulfate into the second part of vanadium liquid according to the ammonium addition coefficient of 0.5-0.8; 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, and the volume of the second vanadium liquid is 10-15% of the volume of the vanadium liquid to be treated;
s4, adding the solution obtained in the step S3 into the solution obtained in the step S2, and stirring;
s5, regulating the pH value of the solution obtained in the step S4 to 2.0-2.05, and then preserving heat for a preset time at 80-90 ℃;
s6, adding ammonium sulfate into the third vanadium liquid;
s7, adding the solution obtained in the step S6 into the solution obtained in the step S5, and stirring;
and S8, heating the solution obtained in the step S7 to boiling, standing, filtering and washing to obtain ammonium polyvanadate.
According to one embodiment of the invention, the vanadium liquid to be treated is vanadium liquid directly obtained after impurity removal of the vanadium-containing leaching liquid.
According to one embodiment of the invention, in the step S1, the volume of the first part of vanadium liquid and the volume of the third part of vanadium liquid are respectively 70-80% and 10-15% of the volume of vanadium liquid to be treated.
According to one embodiment of the present invention, in step S5, the predetermined time is 20 to 30 minutes.
According to one embodiment of the invention, in step S6, ammonium sulphate is added to the third vanadium liquid with an ammonium addition coefficient of 0.1-0.3.
According to one embodiment of the invention, in step S8, the solution is kept boiling for 30 to 40min and the rest time is 10 to 20min.
According to one embodiment of the invention, the vanadium content of the vanadium liquid to be treated is 15-50 g/L.
According to one embodiment of the invention, in step S2, the first part of vanadium liquid is placed in an acid adjusting tank to adjust the pH value; and after the step S2, transferring the first part of vanadium liquid from the acid regulating tank to a vanadium precipitation tank.
According to one embodiment of the invention, in step S3, the second part of vanadium liquid is placed in an acid adjusting tank to adjust the pH value, and then the second part of vanadium liquid is transferred from the acid adjusting tank to an ammonium adding tank to be added with ammonium sulfate; in step S4, transferring the second part of vanadium liquid from the ammonium adding tank to a vanadium precipitation tank.
According to one embodiment of the invention, in step S6, the third part of vanadium liquid is placed in an ammonium adding tank to add ammonium sulfate; in step S7, the third part of vanadium liquid is transferred from the ammonium adding tank to the vanadium precipitation tank.
In the method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid and low ammonium according to the embodiment of the invention, a part of vanadium liquid is firstly adjusted to a certain value, a small amount of vanadium liquid is taken to adjust the pH value to dissolve most of needed ammonium salt, then the vanadium liquid which is adjusted in the earlier stage is added to be stirred at a certain temperature to form a certain crystal nucleus, and then a small amount of vanadium liquid which is dissolved with ammonium salt is added to induce heating, so that the crystal nucleus grows into crystal grains to precipitate, and the ammonium salt is fully utilized, so that the high-density ammonium polyvanadate is precipitated. Not only can the preparation of high-density ammonium polyvanadate be realized, but also the ammonium salt dosage can be reduced, and the overflow of the ammonium salt is avoided.
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 high-density ammonium polyvanadate from high-temperature vanadium liquid low-ammonium 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 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 the common sodium vanadium solution is above 60 ℃ and even up to 75 ℃, a large amount of ammonium salt is needed to be added in the preparation of high-density ammonium polyvanadate, even seed crystals or other additives are introduced to assist in precipitating vanadium, the operation environment is contacted with a large amount of ammonium salt due to the high temperature of the vanadium solution, the ammonium overflow is caused to different degrees, and the operation environment is bad. Vanadium, which cannot react with ammonium salt at high temperature, instantaneously forms a large amount of hydrolyzed flocculent precipitate product due to low ammonium induction, resulting in density reduction. In view of this, the present application proposes a method as will be described below to achieve the preparation of high density ammonium polyvanadate, while also reducing the use of ammonium salts and avoiding ammonium salt spillage.
FIG. 1 shows a flow chart of a method for preparing high-density ammonium polyvanadate from high-temperature 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 at 60-85 ℃ into three parts;
s2, adjusting the pH value of the first vanadium liquid to be 4-5.5;
s3, adjusting the pH value of the second part of vanadium liquid to be 4-5.5, and then adding ammonium sulfate into the second part of vanadium liquid according to the ammonium addition coefficient of 0.5-0.8; 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, and the volume of the second vanadium liquid is 10-15% of the volume of the vanadium liquid to be treated;
s4, adding the solution obtained in the step S3 into the solution obtained in the step S2, and stirring;
s5, regulating the pH value of the solution obtained in the step S4 to 2.0-2.05, and then preserving heat for a preset time at 80-90 ℃;
s6, adding ammonium sulfate into the third vanadium liquid;
s7, adding the solution obtained in the step S6 into the solution obtained in the step S5, and stirring;
and S8, heating the solution obtained in the step S7 to boiling, standing, filtering and washing to obtain ammonium polyvanadate.
In the method, a part of vanadium liquid is firstly regulated to a certain value, so that the polymerization state of vanadium in the vanadium liquid is maximized, part of sodium is separated out, a small amount of vanadium liquid is taken to regulate the pH value to dissolve most of needed ammonium salt, then the vanadium liquid which is regulated in the earlier stage is added to be stirred at a certain temperature to form a certain crystal nucleus, and then a small amount of vanadium liquid which is dissolved with ammonium salt is added to induce heating, so that the crystal nucleus grows into crystal grains to precipitate, the ammonium salt is fully utilized, and the high-density ammonium polyvanadate is precipitated.
The method is suitable for treating the high-temperature vanadium liquid with the temperature of 60-85 ℃ to obtain the high-density ammonium polyvanadate. At the position ofIn the present invention, "high density ammonium polyvanadate" means a density of 0.8g/cm or more 3 Ammonium polyvanadate. Through the steps of the invention, the high-temperature vanadium liquid can be directly treated (without cooling firstly) to obtain the high-density ammonium polyvanadate. In some embodiments, the vanadium liquid to be treated is a vanadium liquid directly obtained after impurity removal of the vanadium-containing leaching liquid. The vanadium content of the vanadium liquid can be 15-50 g/L, the application range is wider, and the method is not strictly limited. The phosphorus content of the vanadium liquid can be less than or equal to 0.015g/L.
In the steps S2 and S3, the pH value of the vanadium liquid is adjusted to be 4-5.5, so that vanadium is in a proper aggregation state in the solution, sodium is conveniently separated from the vanadium compound in the aggregation state, and vanadium precipitation can be realized by adding a small amount of ammonium salt.
In the step S3, adding ammonium sulfate into the second part of vanadium liquid after the pH value is regulated, wherein the volume of the second part of vanadium liquid is 10-15% of the volume of vanadium liquid to be treated, and the mass of the added ammonium sulfate is 0.5-0.8 of the total mass of vanadium in the vanadium liquid to be treated, so that the addition of excessive ammonium sulfate into the second part of vanadium liquid can be ensured. The ammonium salt is added after the second vanadium liquid with small volume is regulated to be in an aggregation state, and a small amount of flocculent precipitate can be generated, but the flocculent precipitate generated by stirring can be dissolved because the ammonium content is far enough to meet the requirement of vanadium in the vanadium liquid with small volume.
In step S4, the second part of vanadium liquid with less ammonium added into the volume is added into the first part of vanadium liquid and stirred for a certain time to slowly form seed crystals. Then in step S5, the seed crystal is favorably formed stably by adjusting the pH value and preserving heat at 80-90 ℃ for a predetermined time.
In the steps S7 and S8, the vanadium liquid directly added with a small amount of ammonium salt is added into the solution obtained in the step S5 to start heating and precipitating vanadium, crystal nuclei grow up at a proper temperature to form crystal precipitation, so that the ammonium salt is fully utilized, and high-density ammonium polyvanadate is precipitated.
Therefore, through the above-mentioned separate treatment of three parts of vanadium liquid and the mixing and subsequent treatment of different vanadium liquids, the formation of seed crystal and the growth of crystal can be realized, and the high-density ammonium polyvanadate is ensured to be obtained. By adjusting the vanadium liquid to a suitable aggregation state and by fully utilizing the ammonium salt, the amount of ammonium salt can be reduced as a whole.
In some embodiments, in step S1, the volume of the first vanadium liquid and the volume of the third vanadium liquid are respectively 70% -80% and 10% -15% of the volume of the vanadium liquid to be treated. The first part of vanadium liquid has a large volume, so that the treated second part of vanadium liquid is added with the first part of vanadium liquid which is regulated to an aggregation state to form a seed crystal. The third part of vanadium liquid has smaller volume and is mainly used for inducing seed crystal growth after adding ammonium salt.
In some embodiments, in step S5, the predetermined time is 20-30 minutes, ensuring that the seed crystal is sufficiently well formed.
In some embodiments, in step S6, ammonium sulfate is added to the third vanadium fluid at an ammonium addition coefficient of 0.1 to 0.3. By the method, the dosage of ammonium salt can be reduced, and the requirement can be met by only adding ammonium sulfate with the ammonium addition coefficient of 0.1-0.3 in the step S6.
In some embodiments, in step S8, the solution is kept boiling for 30-40 min and the standing time is 10-20 min, so as to ensure sufficient vanadium precipitation and separation of the precipitate from the solution after vanadium precipitation.
The present invention is not limited to the sequence of steps S1 to S8. For example, three parts of vanadium liquid can be treated successively, and three parts of vanadium liquid can be treated synchronously. In some embodiments, continuous operation of multiple steps may be achieved with the aid of an acid conditioning tank, an ammonium addition tank, and a vanadium precipitation tank.
Specifically, in step S2, the first part of vanadium liquid is placed in an acid adjusting tank to adjust the pH value; and S2, transferring the first part of vanadium liquid from the acid regulating tank to a vanadium precipitation tank, wherein the vanadium precipitation tank can be in a stirring state all the time.
In the step S3, the second part of vanadium liquid is placed in an acid regulating tank to regulate the pH value, and then the second part of vanadium liquid is transferred from the acid regulating tank to an ammonium adding tank to be added with ammonium sulfate; in step S4, transferring the second part of vanadium liquid from the ammonium adding tank to a vanadium precipitation tank.
In the step S6, the third part of vanadium liquid is placed in an ammonium adding tank, and ammonium sulfate is added; in step S7, the third part of vanadium liquid is transferred from the ammonium adding tank to the vanadium precipitation tank.
Therefore, different vanadium liquids can sequentially enter the corresponding acid regulating tank, the ammonium adding tank or the vanadium precipitating tank to realize corresponding operation, so that continuous operation of vanadium precipitation is facilitated.
According to the above description, the present invention has the following advantages: (1) the high-temperature vanadium liquid can directly precipitate vanadium; (2) the ammonium salt dosage is small; and (3) continuously operating to precipitate vanadium.
The following description is made with reference to specific examples.
The composition of the vanadium sodium salt solution used in each example is shown in Table 1.
TABLE 1 sodium vanadium solution composition/g.L -1
Wherein the original pH value of the vanadium liquid 1 is 10.75, and the temperature of the vanadium liquid is 60 ℃; the original pH value of the vanadium solution 2 is 11.0, and the temperature of the vanadium solution is 70 ℃; the original pH value of the vanadium liquid 3 is 11.15, and the temperature of the vanadium liquid is 85 ℃.
Example 1
Adding 16L of 80% vanadium liquid of the total vanadium liquid volume into 20L of sodium vanadium liquid 1, adding into an acid adjusting tank to adjust the pH to 4, transferring into a vanadium precipitating tank, and continuously stirring; adding 2L of vanadium liquid accounting for 10% of the total vanadium liquid volume into an acid regulating tank to regulate the pH value to 4, adding 153g of a certain amount of ammonium sulfate into an ammonium adding tank (the ammonium adding coefficient is that the mass of ammonium sulfate is 0.5 in total mass of vanadium in the vanadium precipitating tank), and adding into the vanadium precipitating tank to stir all the time; regulating the pH value of the vanadium precipitation tank to 2.0, heating to 80 ℃ and precipitating for 20min; then adding 2L of 10% vanadium liquid of the total vanadium liquid volume into an ammonium adding tank, adding 91.8g of ammonium sulfate (the ammonium adding coefficient is that the mass of ammonium sulfate is 0.3 of the total mass of vanadium in the vanadium precipitating tank), and directly adding into the vanadium precipitating tank; heating to boiling for 30min while stirring in a vanadium precipitation tank; standing for 10min, filtering, washing to obtain high density ammonium polyvanadate with vanadium precipitation rate of 99.34%, and bulk density of 0.82g/cm 3 。
Example 2
1000L of sodium vanadium solution 2 is firstly added into 700L of 70 percent vanadium solution with the total volume of vanadium solution to be precipitated into an acid adjusting tank to adjust the pH value to 5, and then the solution is transferred into a vanadium precipitating tank to be continuously stirred; 150L of 15 percent vanadium liquid with the volume of the total vanadium liquid is added into an acid adjusting tank to adjust the pH value to 5, then the mixture is transferred into an ammonium adding tank, a certain amount of 27.36kg of ammonium sulfate is added (the ammonium adding coefficient is that the mass of the ammonium sulfate is 0.6 of the total mass of vanadium in the vanadium precipitating tank), and then the mixture is transferred into the vanadium precipitating tank, and the vanadium precipitating tank is stirred all the time; regulating the pH value of the vanadium precipitation tank to 2.02, heating to 85 ℃ and precipitating for 25min; 150L of 15% vanadium liquid of the total vanadium liquid volume is added into an ammonium adding tank, 9.12kg of ammonium sulfate is added (the ammonium adding coefficient is that the mass of ammonium sulfate is 0.2 of the total mass of vanadium in the vanadium precipitating tank), and the mixture is directly added into the vanadium precipitating tank; heating to boiling for 35min while stirring in a vanadium precipitation tank; standing for 15min, filtering, washing to obtain high density ammonium polyvanadate with vanadium precipitation rate of 99.45%, and bulk density of 0.84g/cm 3 。
Example 3
Adding 75% of vanadium solution 375L of the total vanadium solution volume into 500L of sodium vanadium solution 3, adding into an acid adjusting tank to adjust the pH to 5.5, transferring into a vanadium precipitating tank, and continuously stirring; adding 60L of vanadium liquid accounting for 12% of the total vanadium liquid volume into an acid regulating tank to regulate the pH value to 5.5, adding 20kg of ammonium sulfate (the ammonium adding coefficient is that the mass of ammonium sulfate is 0.8 in total mass of vanadium in the vanadium precipitating tank) into an ammonium adding tank, and adding the ammonium sulfate into the vanadium precipitating tank to stir the vanadium precipitating tank all the time; regulating the pH value of the vanadium precipitation tank to 2.05, heating to 90 ℃ and precipitating for 30min; then pumping 65L of 13% vanadium liquid of the total vanadium liquid volume into an ammonium adding tank, adding 2.5kg of ammonium sulfate (the ammonium adding coefficient is that the mass of ammonium sulfate is 0.1 of the total mass of vanadium in the vanadium precipitating tank), and directly entering the vanadium precipitating tank; heating to boiling for 40min while stirring in a vanadium precipitation tank; standing for 20min, filtering, and washing to obtain high density ammonium polyvanadate with vanadium precipitation rate of 99.55%, and bulk density of 0.85g/cm 3 。
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 (8)
1. The method for preparing the high-density ammonium polyvanadate from the high-temperature vanadium liquid and low ammonium is characterized by comprising the following steps of:
s1, dividing vanadium liquid to be treated at 60-85 ℃ into three parts;
s2, adjusting the pH value of the first vanadium liquid to be 4-5.5;
s3, adjusting the pH value of the second part of vanadium liquid to be 4-5.5, and then adding ammonium sulfate into the second part of vanadium liquid according to the ammonium addition coefficient of 0.5-0.8; 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, and the volume of the second vanadium liquid is 10-15% of the volume of the vanadium liquid to be treated;
s4, adding the solution obtained in the step S3 into the solution obtained in the step S2, and stirring;
s5, regulating the pH value of the solution obtained in the step S4 to 2.0-2.05, and then preserving heat for a preset time at 80-90 ℃;
s6, adding ammonium sulfate into the third vanadium liquid;
s7, adding the solution obtained in the step S6 into the solution obtained in the step S5, and stirring;
s8, heating the solution obtained in the step S7 to boiling, standing, filtering and washing to obtain ammonium polyvanadate;
in the step S1, the volume of the first part of vanadium liquid and the volume of the third part of vanadium liquid are respectively 70-80% and 10-15% of the volume of vanadium liquid to be treated; in the step S6, ammonium sulfate is added into the third vanadium liquid according to the ammonium addition coefficient of 0.1-0.3.
2. The method according to claim 1, wherein the vanadium liquid to be treated is a vanadium liquid directly obtained after impurity removal of a vanadium-containing leaching solution.
3. The method according to claim 1, wherein in step S5, the predetermined time is 20 to 30 minutes.
4. The method according to claim 1, wherein in step S8, the solution is kept boiling for 30 to 40 minutes and the standing time is 10 to 20 minutes.
5. The method according to claim 1, wherein the vanadium content of the vanadium liquid to be treated is 15-50 g/L.
6. The method according to claim 1, wherein in step S2, the first part of vanadium liquid is placed in an acid adjusting tank to adjust the pH value; and after the step S2, transferring the first part of vanadium liquid from the acid regulating tank to a vanadium precipitation tank.
7. The method according to claim 6, wherein in step S3, the second part of vanadium liquid is placed in an acid adjusting tank to adjust the pH value, and then the second part of vanadium liquid is transferred from the acid adjusting tank to an ammonium adding tank to be added with ammonium sulfate; in step S4, transferring the second part of vanadium liquid from the ammonium adding tank to a vanadium precipitation tank.
8. The method according to claim 7, wherein in step S6, the third part of vanadium liquid is placed in an ammonium adding tank to add ammonium sulfate; in step S7, the third part of vanadium liquid is transferred from the ammonium adding tank to the vanadium precipitation tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211425898.8A CN115626661B (en) | 2022-11-15 | 2022-11-15 | Method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid and low ammonium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211425898.8A CN115626661B (en) | 2022-11-15 | 2022-11-15 | Method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid and low ammonium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115626661A CN115626661A (en) | 2023-01-20 |
| CN115626661B true CN115626661B (en) | 2024-02-06 |
Family
ID=84910829
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211425898.8A Active CN115626661B (en) | 2022-11-15 | 2022-11-15 | Method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid and low ammonium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115626661B (en) |
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 |
| CN104058456A (en) * | 2013-12-06 | 2014-09-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Ammonium metavanadate preparation method |
-
2022
- 2022-11-15 CN CN202211425898.8A patent/CN115626661B/en active Active
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 |
| CN104058456A (en) * | 2013-12-06 | 2014-09-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Ammonium metavanadate preparation method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115626661A (en) | 2023-01-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106006732A (en) | Method for preparing ammonium polyvanadate from high concentration vanadium liquid | |
| CN108046337A (en) | A kind of method of purification of byproduct ferrous sulfate of titanium dioxide | |
| CN102502823A (en) | Preparation method for preparing high-tap density ammonium poly-vanadate | |
| CN115626661B (en) | Method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid and low ammonium | |
| CN101913647A (en) | Hydrolysis method for producing electronic-grade special titanium white by sulfuric acid process | |
| WO2017092217A1 (en) | Method for producing high-purity vanadium pentoxide by room temperature extraction | |
| CN106044838B (en) | Production technology of low-sulfur lanthanum hydroxide | |
| CN111218572B (en) | Method for preparing high-density ammonium polyvanadate by heat preservation of calcified roasting pickle liquor | |
| CN115744981B (en) | Method for preparing high-density ammonium polyvanadate from vanadium liquid | |
| CN105836866B (en) | The technique of the high fluorine waste water induction crystallization calcirm-fluoride of Rare earth metal metallurgy | |
| CN115744982B (en) | Method for preparing large-particle ammonium polyvanadate from vanadium liquid low ammonium | |
| CN115849444B (en) | Preparation method of low-sodium ammonium polyvanadate | |
| CN115594221B (en) | Method for preparing flaky high-density ammonium polyvanadate from low ammonium content in vanadium liquid | |
| CN113753952A (en) | Method for preparing ammonium polyvanadate from sodium vanadium solution with low ammonium content | |
| CN115676886B (en) | Method for reducing vanadium precipitation wastewater of high-concentration vanadium solution | |
| CN112850778A (en) | Preparation method of basic copper chloride | |
| CN111153540A (en) | Salt separation system and process for ensuring quality of crystallized salt in high-salinity wastewater | |
| CN106219589B (en) | A kind of production technology of low-sulfur cerium hydroxide | |
| CN115636441A (en) | Method for preparing high-density low-sodium ammonium polyvanadate from sodium vanadium solution | |
| US2894814A (en) | Purification of tungstates | |
| CN111099656B (en) | Method for preparing high-density ammonium polyvanadate by using calcification roasting acid leaching solution ammonium hydrogen | |
| CN117919646A (en) | Method for treating high-fluorine ammonia-containing slag | |
| CN109368699B (en) | Method for removing magnesium in ammonium dimolybdate production process | |
| CN117843039A (en) | Purification method of titanium white byproduct copperas for preparing battery-grade iron phosphate raw material | |
| CN108557884B (en) | Method for preparing high-density large-particle ammonium polyvanadate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |