CN115626661A - Method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid with low ammonium content - Google Patents
Method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid with low ammonium content Download PDFInfo
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- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 236
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 235
- 239000007788 liquid Substances 0.000 title claims abstract description 104
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 title claims abstract description 89
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000001556 precipitation Methods 0.000 claims abstract description 61
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 37
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 37
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000009835 boiling Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 15
- 239000012535 impurity Substances 0.000 claims description 5
- 238000002386 leaching Methods 0.000 claims description 3
- 150000003863 ammonium salts Chemical class 0.000 abstract description 30
- 239000013078 crystal Substances 0.000 description 16
- CFVBFMMHFBHNPZ-UHFFFAOYSA-N [Na].[V] Chemical compound [Na].[V] CFVBFMMHFBHNPZ-UHFFFAOYSA-N 0.000 description 10
- 239000002244 precipitate Substances 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 5
- 238000004220 aggregation Methods 0.000 description 5
- 230000001376 precipitating effect Effects 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 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 3
- 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
- 239000000047 product Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 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
- 238000003723 Smelting Methods 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000002893 slag Substances 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
- 239000000654 additive Substances 0.000 description 1
- 238000006243 chemical reaction Methods 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
- 230000014509 gene expression Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000003301 hydrolyzing effect 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
- 238000000926 separation method Methods 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
- 150000003682 vanadium compounds Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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- 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
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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 high-density ammonium polyvanadate from high-temperature vanadium liquid with low ammonium content, which comprises the following steps: s1, dividing vanadium liquid to be treated at the temperature of 60-85 ℃ into three parts; s2, adjusting the pH value of the first part of vanadium liquid to 4-5.5; s3, adjusting the pH value of the second vanadium liquid to 4-5.5, and then adding ammonium sulfate into the second vanadium liquid according to the ammonium addition coefficient of 0.5-0.8, wherein the volume of the second vanadium liquid is 10-15% of that of the vanadium liquid to be treated; s4, adding the solution obtained in the step S3 into the solution obtained in the step S2; s5, adjusting 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 solution; 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 method can carry out vanadium precipitation on the high-temperature vanadium liquid, can reduce the using amount of ammonium salt, and can 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 with low ammonium content.
Background
In the vanadium slag sodium salt vanadium extraction process, vanadium slag is roasted, soaked in water and subjected to 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 subsequent smelting requirements.
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 the qualified sodium treatment solution contains a large amount of sodium ions, in order to improve the vanadium precipitation rate and ensure the product quality, excessive ammonium salt is often added, and in order to obtain high density (rho is more than 0.6 g/cm) 3 ) Ammonium polyvanadate, the amount of ammonium salt used is generally higher. Most of excessive ammonium salt can enter the vanadium precipitation wastewater to obtain the high-ammonia-nitrogen vanadium precipitation wastewater, and the wastewater treatment cost is increased. In addition, in the prior art, the vanadium-containing solution mainly used for vanadium precipitation is a sodium vanadium solution, the sodium vanadium solution is subjected to a leaching-impurity removal process, the temperature is generally 60 ℃ and even reaches 75 ℃, high-density ammonium polyvanadate is prepared, a higher ammonium salt addition amount is generally adopted, 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 ammonium overflow is caused, the vanadium precipitation environment is influenced, and the health of personnel is harmed.
Disclosure of Invention
The invention mainly aims to provide a method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid with low ammonium content, so as to solve the problems that the use amount of ammonium salt is too high when the high-density ammonium polyvanadate is prepared, the wastewater treatment cost is increased, and the vanadium deposition environment is influenced by the overflow of the ammonium salt.
According to one aspect of the invention, a method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid with low ammonium content is provided, which comprises the following steps:
s1, dividing vanadium liquid to be treated at the temperature of 60-85 ℃ into three parts;
s2, adjusting the pH value of the first part of vanadium liquid to 4-5.5;
s3, adjusting the pH value of the second part of vanadium solution to 4-5.5, and then adding ammonium sulfate into the second part of vanadium solution according to the ammonium addition coefficient of 0.5-0.8; 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, and the volume of the second part of 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, adjusting the pH value of the solution obtained in the step S4 to 2.0-2.05, and then preserving the temperature at 80-90 ℃ for a preset time;
s6, adding ammonium sulfate into the third vanadium solution;
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 a vanadium liquid directly obtained after the vanadium-containing leaching solution is subjected to impurity removal.
According to an embodiment of the invention, in 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 the vanadium liquid to be treated.
According to an embodiment of the present invention, in step S5, the predetermined time is 20 to 30min.
According to an embodiment of the invention, in step S6, ammonium sulfate is added into the third part of vanadium solution according to the ammonium addition coefficient of 0.1-0.3.
According to one embodiment of the invention, in step S8, the solution is kept boiling for 30-40 min and standing for 10-20 min.
According to one embodiment of the invention, the vanadium content of the vanadium liquid to be treated is 15-50 g/L.
According to an embodiment of the invention, in step S2, the first portion of vanadium solution is placed in an acid adjusting tank to adjust the pH value; after the step S2, transferring the first part of vanadium liquid from the acid adjusting tank to a vanadium precipitation tank.
According to an 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 add ammonium sulfate; and in the step S4, transferring the second part of vanadium liquid from the ammonium adding tank to a vanadium precipitation tank.
According to an embodiment of the invention, in step S6, the third vanadium solution is placed in an ammonium adding tank, and ammonium sulfate is added; and in the step S7, transferring the third part of vanadium liquid from the ammonium adding tank to the vanadium precipitation tank.
According to the method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid and low ammonium, disclosed by the embodiment of the invention, the pH value of a part of vanadium liquid is adjusted to a certain value, then a small amount of vanadium liquid is taken to adjust the pH value to dissolve most of required ammonium salt, the obtained solution is added into the vanadium liquid which is adjusted in the early stage and stirred at a certain temperature to form a certain crystal nucleus, and then a small amount of vanadium liquid which dissolves ammonium salt is added to induce temperature rise so that the crystal nucleus grows into crystal grains to precipitate, so that the ammonium salt is fully utilized, and the high-density ammonium polyvanadate is precipitated. The preparation of high-density ammonium polyvanadate can be realized, the dosage of ammonium salt can be reduced, and the overflow of 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 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 shows a flow chart of a method for preparing high-density ammonium polyvanadate from high-temperature vanadium liquid with low ammonium content 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 merely for convenience of description and should not be construed as limitations of the embodiments of the present invention, and they are not described in any more detail in the following embodiments.
The inventor of the application realizes that the preparation of high-density ammonium polyvanadate from general sodium vanadium solution at the temperature of more than 60 ℃ and even up to 75 ℃ needs to add a large amount of ammonium salt, even introduces seed crystals or other additives to assist in vanadium precipitation, and the operating environment is severe because the vanadium solution temperature is high and contacts a large amount of ammonium salt, and the ammonium overflows due to different degrees. At the moment that vanadium which can not obtain ammonium salt reaction under the high temperature is induced by low ammonium, a large amount of hydrolytic flocculent precipitate products are formed, and the density is reduced. In view of this, the present application proposes the following method to realize the preparation of high density ammonium polyvanadate, while reducing the use of ammonium salt and avoiding the overflow of ammonium salt.
Fig. 1 shows a flow chart of a method for preparing high-density ammonium polyvanadate from high-temperature 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 vanadium liquid to be treated at the temperature of 60-85 ℃ into three parts;
s2, adjusting the pH value of the first part of vanadium liquid to 4-5.5;
s3, adjusting the pH value of the second part of vanadium solution to 4-5.5, and then adding ammonium sulfate into the second part of vanadium solution according to the ammonium addition coefficient of 0.5-0.8; 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, and the volume of the second part of 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, adjusting the pH value of the solution obtained in the step S4 to 2.0-2.05, and then preserving the temperature at 80-90 ℃ for a preset time;
s6, adding ammonium sulfate into the third vanadium solution;
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, firstly, the pH value of a part of vanadium liquid is adjusted to a certain value, so that the vanadium polymerization state in the vanadium liquid is maximized, part of sodium is separated out, then a small amount of vanadium liquid is taken to adjust the pH value to dissolve most of required ammonium salt, then the vanadium liquid adjusted in the early stage is added to be stirred at a certain temperature to form a certain crystal nucleus, and then a small amount of vanadium liquid dissolving ammonium salt is added to induce temperature rise, so that the crystal nucleus grows up to form crystal grains to be precipitated, the ammonium salt is fully utilized, and the high-density ammonium polyvanadate is precipitated.
The method is suitable for treating high-temperature vanadium liquid with the temperature of 60-85 ℃ to obtain high-density ammonium polyvanadate. In 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 in advance) to obtain high-density ammonium polyvanadate. In some embodiments, the vanadium solution to be treated is a vanadium solution directly obtained after removing impurities from a vanadium-containing leaching solution. The vanadium content of the vanadium liquid can be 15-50 g/L, the application range is wide, and no strict limitation is imposed. The phosphorus content of the vanadium liquid can be less than or equal to 0.015g/L.
In steps S2 and S3, the pH of the vanadium solution is adjusted to 4 to 5.5, so that the vanadium is in a suitable aggregation state in the solution, in which aggregation state sodium is conveniently separated from the vanadium compound, and subsequently a small amount of ammonium salt is added to achieve vanadium precipitation.
In the step S3, ammonium sulfate is added into the second part of vanadium liquid after the pH value is adjusted, wherein the volume of the second part of vanadium liquid is 10-15% of the volume of the 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 second part of vanadium liquid can be ensured to be added with excessive ammonium sulfate. And adding ammonium salt after the second small-volume vanadium liquid is adjusted to be in an aggregation state, although a small amount of flocculent precipitate can be generated, the ammonium content far meets the requirement of vanadium in the small-volume vanadium liquid, and the flocculent precipitate generated by stirring can be dissolved again.
In step S4, the second part of vanadium solution with small volume added with ammonium is added into the first part of vanadium solution and stirred for a certain time, and seed crystals are slowly formed. Then in step S5, the stable formation of the seed crystal is facilitated by adjusting the pH value and maintaining the temperature at 80-90 ℃ for a predetermined time.
In steps S7 and S8, adding vanadium liquid directly added with a small amount of ammonium salt into the solution obtained in step S5, starting to heat up to precipitate vanadium, and growing crystal nuclei at a proper temperature to form crystal precipitate, so that the ammonium salt is fully utilized, and high-density ammonium polyvanadate is precipitated.
Therefore, through the respective treatment of the three vanadium liquids, the mixing and subsequent treatment of different vanadium liquids, the formation of crystal seeds and the growth of crystals can be realized, and the high-density ammonium polyvanadate can be obtained. By adjusting the vanadium solution to a suitable aggregation state and by making full use of the ammonium salt, the amount of ammonium salt used can be reduced as a whole.
In some embodiments, in step S1, the volume of the first vanadium solution and the volume of the third vanadium solution are 70% to 80% and 10% to 15% of the volume of the vanadium solution to be treated, respectively. The first part of vanadium liquid is more in volume, and the second part of vanadium liquid after treatment is added into the first part of vanadium liquid which is adjusted to an aggregation state to form seed crystals. The third part of vanadium liquid has less volume and is mainly used for inducing seed crystal growth after ammonium salt is added.
In some embodiments, the predetermined time is 20 to 30min in step S5, which ensures that the seed crystal is sufficiently well formed.
In some embodiments, in step S6, ammonium sulfate is added to the third portion of vanadium solution according to an ammonium addition coefficient of 0.1 to 0.3. By the method, the consumption of ammonium salt can be reduced, and the requirement can be met only by 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 standing for 10-20 min, so as to ensure sufficient vanadium precipitation and separation of the precipitate from the solution after vanadium precipitation.
The present invention does not limit the sequence of the steps S1 to S8. For example, three parts of vanadium solution may be treated sequentially, or three parts of vanadium solution may be treated simultaneously. In some embodiments, continuous operation of the multiple steps may be achieved by means of an acid adjustment tank, an ammonium addition tank, and a vanadium precipitation tank.
Specifically, in step S2, the first portion of vanadium liquid is placed in an acid adjusting tank to adjust the pH value; after the step S2, transferring the first portion of vanadium solution from the acid adjusting tank to a vanadium precipitation tank, where the vanadium precipitation tank may be in a stirring state all the time.
In the 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 add ammonium sulfate; and in the step S4, transferring the second part of vanadium liquid from the ammonium adding tank to a vanadium precipitation tank.
Step S6, placing the third vanadium liquid into an ammonium adding tank, and adding ammonium sulfate; and in the step S7, transferring the third part of vanadium liquid from the ammonium adding tank to the vanadium precipitation tank.
Therefore, different vanadium liquids can sequentially enter corresponding acid adjusting tanks, ammonium adding tanks or vanadium precipitating tanks to realize corresponding operation, and continuous operation 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 dosage of ammonium salt is less; and (3) continuously operating to precipitate vanadium.
The following description is given with reference to specific examples.
The components of the sodium vanadium solution used 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, and the temperature of the vanadium solution 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 oxide solution 3 is 11.15, and the temperature of the vanadium oxide solution is 85 ℃.
Example 1
Adding 16L of vanadium solution with the volume being 80% of the total vanadium precipitation solution into 20L of sodium vanadium solution 1, adding the vanadium solution into an acid adjusting tank to adjust the pH value to 4, transferring the vanadium solution into a vanadium precipitation tank, and continuously stirring; then 2L of vanadium liquid with the volume of 10 percent of the total vanadium precipitation liquid is added into an acid adjusting tank to adjust the pH value to 4, then the vanadium liquid is transferred into an ammonium adding tank to add a certain amount of ammonium sulfate 153g (the ammonium addition coefficient is the mass of the ammonium sulfate/the total mass of vanadium in the vanadium precipitation tank = 0.5), and then the vanadium liquid is transferred into a vanadium precipitation tank, and the vanadium precipitation tank is stirred all the time; adjusting the pH value of the vanadium precipitation tank to 2.0, heating to 80 ℃, and precipitating for 20min; 2L of vanadium liquid with the volume being 10% of the total vanadium precipitation liquid is thrown into the vanadium precipitation tank, and the vanadium precipitation tank is directly filled with 91.8g of ammonium sulfate (the ammonium addition coefficient is the mass of ammonium sulfate/the total mass of vanadium in the vanadium precipitation tank = 0.3); heating to boil for 30min while stirring in a vanadium precipitation tank; standing for 10min, filtering, and washing to obtain high density ammonium polyvanadate with vanadium precipitation rate of 99.34% and ammonium polyvanadate bulk density of 0.82g/cm 3 。
Example 2
Adding 700L of vanadium solution with the volume of 70 percent of the total vanadium precipitation solution into 1000L of sodium vanadium solution 2, adding the vanadium solution into an acid adjusting tank to adjust the pH value to 5, transferring the vanadium solution into a vanadium precipitation tank, and continuously stirring the vanadium solution; then adding 150L of vanadium solution with the volume being 15% of the total vanadium precipitation solution, putting the vanadium solution into an acid adjusting tank, adjusting the pH value to 5, then transferring the vanadium solution into an ammonium adding tank, adding 27.36kg of a certain amount of ammonium sulfate (the ammonium addition coefficient is the mass of the ammonium sulfate/the total mass of vanadium in the vanadium precipitation tank = 0.6), transferring the vanadium solution into a vanadium precipitation tank, and stirring the vanadium precipitation tank all the time; adjusting the pH value of the vanadium precipitation tank to 2.02, heating to 85 ℃, and precipitating for 25min; then 150L of vanadium liquid with the volume being 15% of the total vanadium precipitation liquid is added into the vanadium adding tank, and the vanadium adding tank directly enters the vanadium precipitation tank after 9.12kg of ammonium sulfate is added (the ammonium addition coefficient is the mass of ammonium sulfate/the total mass of vanadium in the vanadium precipitation tank = 0.2); heating to boil for 35min while stirring in a vanadium precipitation tank; standing for 15min, filtering, and 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 375L of vanadium solution with the volume of 75 percent of the total vanadium precipitation solution into 500L of sodium vanadium solution 3, adding into an acid adjusting tank, adjusting the pH value to 5.5, transferring into a vanadium precipitation tank, and continuously stirring; then drive into60L of vanadium liquid with the volume being 12 percent of the total vanadium precipitation liquid enters an acid adjusting tank to adjust the pH value to 5.5, then the vanadium liquid is transferred into an ammonium adding tank to be added with a certain amount of ammonium sulfate by 20kg (the ammonium addition coefficient is the mass of the ammonium sulfate/the total mass of vanadium in the vanadium precipitation tank = 0.8), and then the vanadium liquid is transferred into a vanadium precipitation tank, and the vanadium precipitation tank is stirred all the time; adjusting the pH value of the vanadium precipitation tank to 2.05, heating to 90 ℃, and precipitating for 30min; then adding 65L of 13 percent vanadium liquid of the total vanadium precipitation liquid volume into an ammonium adding tank directly, and after 2.5kg of ammonium sulfate is added (the ammonium addition coefficient is the mass of ammonium sulfate/the total mass of vanadium in the vanadium precipitation tank = 0.1), directly entering the vanadium precipitation tank; heating to boil 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 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 high-density ammonium polyvanadate from high-temperature vanadium liquid with low ammonium content is characterized by comprising the following steps:
s1, dividing vanadium liquid to be treated at the temperature of 60-85 ℃ into three parts;
s2, adjusting the pH value of the first part of vanadium liquid to 4-5.5;
s3, adjusting the pH value of the second part of vanadium liquid to 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 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, and the volume of the second part of 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, adjusting the pH value of the solution obtained in the step S4 to 2.0-2.05, and then preserving the temperature at 80-90 ℃ for a preset time;
s6, adding ammonium sulfate into the third vanadium solution;
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.
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 S1, the volume of the first vanadium solution and the volume of the third vanadium solution are respectively 70-80% and 10-15% of the volume of the vanadium solution to be treated.
4. The method according to claim 1, wherein the predetermined time is 20 to 30min in step S5.
5. The method according to claim 1, wherein in step S6, ammonium sulfate is added to the third vanadium solution according to an ammonium addition coefficient of 0.1-0.3.
6. The method of claim 1, wherein in step S8, the solution is kept boiling for 30-40 min and standing for 10-20 min.
7. The method according to claim 1, characterized in that the vanadium content of the vanadium liquid to be treated is 15-50 g/L.
8. 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 adjusting tank to a vanadium precipitation tank.
9. The method of claim 8, 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 add ammonium sulfate; and in the step S4, transferring the second part of vanadium liquid from the ammonium adding tank to a vanadium precipitation tank.
10. The method of claim 9, wherein in step S6, the third vanadium solution is placed in an ammonium adding tank to which ammonium sulfate is added; and S7, transferring the third part of vanadium solution from the ammonium adding tank to the vanadium precipitation tank.
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| 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 |
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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 |
| 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 |
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