CN111302396A - Preparation method of vanadium pentoxide - Google Patents
Preparation method of vanadium pentoxide Download PDFInfo
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- CN111302396A CN111302396A CN202010310875.7A CN202010310875A CN111302396A CN 111302396 A CN111302396 A CN 111302396A CN 202010310875 A CN202010310875 A CN 202010310875A CN 111302396 A CN111302396 A CN 111302396A
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- vanadium pentoxide
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- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000007787 solid Substances 0.000 claims abstract description 23
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 22
- 238000002844 melting Methods 0.000 claims abstract description 22
- 230000008018 melting Effects 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 239000003513 alkali Substances 0.000 claims abstract description 15
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 15
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000008394 flocculating agent Substances 0.000 claims description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 7
- 235000019270 ammonium chloride Nutrition 0.000 claims description 7
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 7
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 7
- 238000011010 flushing procedure Methods 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 5
- 229910052720 vanadium Inorganic materials 0.000 abstract description 20
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical group [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract description 20
- 239000012535 impurity Substances 0.000 abstract description 17
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract description 7
- 238000009776 industrial production Methods 0.000 abstract description 7
- 238000001556 precipitation Methods 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 45
- 238000007792 addition Methods 0.000 description 19
- 238000004519 manufacturing process Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 5
- 150000003682 vanadium compounds Chemical class 0.000 description 5
- 238000001914 filtration Methods 0.000 description 4
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229910001935 vanadium oxide Inorganic materials 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000009615 deamination Effects 0.000 description 1
- 238000006481 deamination reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- IBYSTTGVDIFUAY-UHFFFAOYSA-N vanadium monoxide Chemical compound [V]=O IBYSTTGVDIFUAY-UHFFFAOYSA-N 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
- C01G31/02—Oxides
-
- 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
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a preparation method of vanadium pentoxide, which comprises the following steps: (1) dissolving ammonium vanadate in an alkali solution, adding an auxiliary agent, and heating to obtain a treatment solution; (2) adding ammonium salt into the treatment liquid obtained in the step (1) and carrying out solid-liquid separation to obtain a solid; (3) and (3) washing the solid obtained in the step (2), and then melting to obtain high-purity vanadium pentoxide. According to the method provided by the invention, through reasonable selection of the steps, the polyaluminium chloride is used for removing impurities, the operation of the impurity removing process is simple, secondary vanadium precipitation is only needed for washing ammonium metavanadate, ammonia water is not needed, the large-scale industrial production is easy to realize, and the cost is lower.
Description
Technical Field
The invention relates to the field of high-purity vanadium, and particularly relates to a preparation method of vanadium pentoxide.
Background
The high-purity vanadium compound is widely applied to the fields of aviation, electronic materials, fluorescent powder, vanadium-oxygen batteries and the like. Following the advance of skill, some vanadium downstream produced commercial production of high end-of-skill products, with higher demands on vanadium compound quality. China has rich vanadium resources, and the production of high-purity vanadium compounds has wide prospect in China. Because the high-purity vanadium compound has high production skill, although more suppliers exist in China, the production skill level is mostly laggard and the product quality is not high. The production skill development of high-purity vanadium compounds has serious skill and social value.
At present, various impurity removing agents are commonly used in a high-purity vanadium production process, ammonia water is used as a washing liquid after vanadium precipitation, the production cost is high, the vanadium loss is large, and the smell is large in the production process. CN104692461A discloses a preparation method of high-purity powdery vanadium oxide, belonging to the technical field of vanadium chemical metallurgy. The technical scheme is as follows: adding an adsorbent, an acid-base regulator and an impurity removing agent into vanadium liquid serving as a raw material, mixing and stirring, and filtering to obtain purified vanadium liquid; supplementing NH4+ to the purified vanadium liquid, adjusting the concentration of NH4+ in the purified vanadium liquid, cooling, crystallizing and filtering to obtain ammonium metavanadate; the ammonium metavanadate is subjected to heating decomposition deamination at the temperature of 300-650 ℃ to obtain powdery vanadium oxide, and the obtained high-purity powdery vanadium oxide is suitable for producing vanadium electrolyte. The invention adopts the process of controlling the impurity content of the leachate from the source, simplifies the subsequent impurity removal process steps, reduces the medicament consumption, has low production cost and clean process, and is beneficial to industrial production. CN101456587A discloses a production method of high-purity vanadium pentoxide, which comprises the following steps: dissolving: adding crude ammonium metavanadate into the aqueous solution, heating to 80-90 ℃, adding ammonia water, and stirring while adding until the ammonium metavanadate is completely dissolved; adding different impurity removal reagents to separate impurities; filtering the solution with the impurities separated out; putting the filtered solution into a reaction kettle, adding an oxidant, and oxidizing bivalent vanadium into pentavalent vanadium; acidifying the completely oxidized solution to separate out brown vanadium pentoxide; vacuum filtering brown vanadium pentoxide, and dehydrating and drying; placing the dried brown vanadium pentoxide into a rotary furnace for calcining; the production method comprises the equipment such as a disc type vacuum filter, a reaction kettle, a rotary furnace and the like; the vanadium pentoxide produced by the method has high purity and few impurities, is used for the fields of organic synthesis catalysts and aerospace, has simple production equipment and high production benefit, and is suitable for large-scale industrial production.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a preparation method of vanadium pentoxide, which has the advantages of simple operation of impurity removal process, no need of ammonia water for secondary vanadium precipitation and ammonium metavanadate washing, easiness in realization of large-scale industrial production and low cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of vanadium pentoxide, which comprises the following steps:
(1) dissolving ammonium vanadate in an alkali solution, adding an auxiliary agent, and heating to obtain a treatment solution;
(2) adding ammonium salt into the treatment liquid obtained in the step (1) and carrying out solid-liquid separation to obtain a solid;
(3) and (3) washing the solid obtained in the step (2), and then melting to obtain high-purity vanadium pentoxide.
According to the method provided by the invention, through reasonable selection of the steps, the polyaluminium chloride is used for removing impurities, the operation of the impurity removing process is simple, secondary vanadium precipitation is only needed for washing ammonium metavanadate, ammonia water is not needed, the large-scale industrial production is easy to realize, and the cost is lower.
As a preferred technical solution of the present invention, the ammonium vanadate salt in step (1) comprises ammonium metavanadate and/or ammonium polyvanadate.
Preferably, the alkali solution of step (1) comprises a sodium hydroxide solution and/or a potassium hydroxide solution.
Preferably, the pH of the solution after dissolution in step (1) is 8.5-9.5, for example, 8.5, 8.6, 8.7, 8.8, 8.9, 9, 9.1, 9.2, 9.3, 9.4 or 9.5, but not limited to the recited values, and other values not recited in this range are also applicable.
As a preferable technical scheme of the invention, the auxiliary agent in the step (1) comprises polyaluminium chloride and a flocculating agent.
In a preferred embodiment of the present invention, the amount of the polyaluminum oxide added is 4.5 to 6%, for example, 4.5%, 4.6%, 4.7%, 4.8%, 4.9%, 5%, 5.1%, 5.2%, 5.3%, 5.4%, 5.5%, 5.6%, 5.7%, 5.8%, 5.9% or 6% of the solution mass, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
Preferably, the addition amount of the flocculant is 0.0008 to 0.001%, for example, 0.0008%, 0.00081%, 0.00082%, 0.00083%, 0.00084%, 0.00085%, 0.00086%, 0.00087%, 0.00088%, 0.0009%, 0.00091%, 0.00092%, 0.00093%, 0.00094%, 0.00095%, 0.00096%, 0.00097%, 0.00098%, 0.00099% or 0.001%, etc., of the solution mass, but is not limited to the enumerated values, and other unrecited values in this range are also applicable.
As a preferred embodiment of the present invention, the temperature at the end of the heating in step (1) is 90 to 100 ℃ and may be, for example, 90 ℃, 91 ℃, 92 ℃, 93 ℃, 94 ℃, 95 ℃, 96 ℃, 97 ℃, 98 ℃, 99 ℃ or 100 ℃, but is not limited to the recited values, and other values not recited in the range are also applicable.
Preferably, the heat-preserving time of the step (1) is 30-45min, such as 30min, 31min, 32min, 33min, 34min, 35min, 36min, 37min, 38min, 39min, 40min, 41min, 42min, 43min, 44min or 45min, but not limited to the recited values, and other values not recited in the range are also applicable.
As a preferred technical scheme of the invention, the ammonium salt in the step (2) comprises ammonium sulfate and/or ammonium chloride.
Preferably, the ammonium salt is added with an addition ratio of 3 to 4, such as 3, 3.1, 3.2, 3.3, 3.4, 3.5, 3.6, 3.7, 3.8, 3.9 or 4, but not limited to the recited values, and other values not recited in this range are also applicable.
In a preferred embodiment of the present invention, the flushing medium is water.
Preferably, the water has a mass 4 to 5.5 times the mass of the solid, for example, 4 times, 4.1 times, 4.2 times, 4.3 times, 4.4 times, 4.5 times, 4.6 times, 4.7 times, 4.8 times, 4.9 times, 5 times, 5.1 times, 5.2 times, 5.3 times, 5.4 times, or 5.5 times, etc., but is not limited to the recited values, and other values not recited in the range are also applicable.
As a preferred embodiment of the present invention, the melting temperature in the step (3) is 1000 ℃ or 1200 ℃, for example, 1000 ℃, 1010 ℃, 1020 ℃, 1030 ℃, 1040 ℃, 1050 ℃, 1060 ℃, 1070 ℃, 1080 ℃, 1090 ℃, 1100 ℃, 1110 ℃, 1120 ℃, 1130 ℃, 1140 ℃, 1150 ℃, 1160 ℃, 1170 ℃, 1180 ℃, 1190 ℃ or 1200 ℃, but is not limited to the recited values, and other values not recited in the range are also applicable.
Preferably, the melting time is 30-60min, such as 30min, 32min, 34min, 36min, 38min, 40min, 42min, 44min, 46min, 48min, 50min, 52min, 54min, 56min, 58min or 60min, but not limited to the recited values, and other values not recited in this range are also applicable.
In a preferred embodiment of the present invention, the purity of the high-purity vanadium pentoxide in step (3) is 99.6% or more, and may be, for example, 99.6%, 99.62%, 99.64%, 99.66%, 99.68%, 99.7%, 99.72%, 99.74%, 99.76%, 99.78%, 99.8%, 99.82%, 99.84%, 99.86%, 99.88%, 99.9%, 99.92%, 99.94%, 99.96%, 99.98%, or 100%, but is not limited to the above-mentioned values, and other values not listed in this range are also applicable.
As a preferred technical scheme of the invention, the method comprises the following steps:
(1) dissolving ammonium vanadate in an alkali solution, adding an auxiliary agent, and heating to obtain a treatment solution; wherein the ammonium vanadate salt comprises ammonium metavanadate and/or ammonium polyvanadate; the alkali solution comprises a sodium hydroxide solution and/or a potassium hydroxide solution; the pH value of the dissolved solution is 8.5-9.5; the auxiliary agent comprises polyaluminium chloride and a flocculating agent; the addition amount of the polymeric alumina is 4.5-6 per mill of the mass of the solution; the addition amount of the flocculating agent is 0.0008-0.001 per mill of the mass of the solution; the heating end point temperature is 90-100 ℃; the heating and heat preservation time is 30-45 min;
(2) adding ammonium salt into the treatment liquid obtained in the step (1) and carrying out solid-liquid separation to obtain a solid; wherein the ammonium salt comprises ammonium sulfate and/or ammonium chloride; the coefficient of adding ammonium in the addition of the ammonium salt is 3-4;
(3) washing the solid obtained in the step (2), and then melting to obtain high-purity vanadium pentoxide; the flushing medium is water; the mass of the water is 4-5.5 times of the mass of the solid; the melting temperature is 1000-1200 ℃; the melting time is 30-60 min; the purity of the high-purity vanadium pentoxide is more than or equal to 99.6%.
Compared with the prior art, the invention has the following beneficial effects:
according to the method provided by the invention, through reasonable selection of the steps, the polyaluminium chloride is used for removing impurities, the operation of the impurity removing process is simple, secondary vanadium precipitation is only needed for washing ammonium metavanadate, ammonia water is not needed, the large-scale industrial production is easy to realize, and the cost is lower. The grade of the produced vanadium pentoxide can reach more than 99.6 percent.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
This example 1 provides a method for preparing high-purity vanadium pentoxide, which includes the following steps:
(1) dissolving ammonium vanadate in an alkali solution, adding an auxiliary agent, and heating to obtain a treatment solution; wherein the ammonium vanadate salt comprises ammonium metavanadate and/or ammonium polyvanadate; the alkali solution comprises a sodium hydroxide solution and/or a potassium hydroxide solution; the pH value of the dissolved solution is 8.5; the auxiliary agent comprises polyaluminium chloride and a flocculating agent; the addition amount of the polymeric alumina is 4.5 per mill of the mass of the solution; the addition amount of the flocculant is 0.0008 per mill of the mass of the solution; the heating end point temperature is 90 ℃; the heating heat preservation time is 30 min;
(2) adding ammonium salt into the treatment liquid obtained in the step (1) and carrying out solid-liquid separation to obtain a solid; wherein the ammonium salt comprises ammonium sulfate and/or ammonium chloride; the coefficient of ammonium addition in the addition of the ammonium salt is 3;
(3) washing the solid obtained in the step (2), and then melting to obtain high-purity vanadium pentoxide; the flushing medium is water; the mass of the water is 4 times of that of the solid; the melting temperature is 1000 ℃; the melting time is 30 min;
the purity of the obtained high-purity vanadium pentoxide is 99.65%.
Example 2
This example 1 provides a method for preparing high-purity vanadium pentoxide, which includes the following steps:
(1) dissolving ammonium vanadate in an alkali solution, adding an auxiliary agent, and heating to obtain a treatment solution; wherein the ammonium vanadate salt comprises ammonium metavanadate and/or ammonium polyvanadate; the alkali solution comprises a sodium hydroxide solution and/or a potassium hydroxide solution; the pH value of the dissolved solution is 9; the auxiliary agent comprises polyaluminium chloride and a flocculating agent; the addition amount of the polymeric alumina is 5.5 per mill of the mass of the solution; the addition amount of the flocculant is 0.0009 per mill of the mass of the solution; the heating end point temperature is 95 ℃; the heating heat preservation time is 38 min;
(2) adding ammonium salt into the treatment liquid obtained in the step (1) and carrying out solid-liquid separation to obtain a solid; wherein the ammonium salt comprises ammonium sulfate and/or ammonium chloride; the coefficient of ammonium addition in the addition of the ammonium salt is 3.5;
(3) washing the solid obtained in the step (2), and then melting to obtain high-purity vanadium pentoxide; the flushing medium is water; the mass of the water is 5 times of that of the solid; the melting temperature is 1100 ℃; the time for the melting was 45 ℃;
the purity of the obtained high-purity vanadium pentoxide is 99.82%.
Example 3
This example 1 provides a method for preparing high-purity vanadium pentoxide, which includes the following steps:
(1) dissolving ammonium vanadate in an alkali solution, adding an auxiliary agent, and heating to obtain a treatment solution; wherein the ammonium vanadate salt comprises ammonium metavanadate and/or ammonium polyvanadate; the alkali solution comprises a sodium hydroxide solution and/or a potassium hydroxide solution; the pH value of the dissolved solution is 9.5; the auxiliary agent comprises polyaluminium chloride and a flocculating agent; the adding amount of the polymeric alumina is 6 per mill of the mass of the solution; the addition amount of the flocculating agent is 0.001 per mill of the mass of the solution; the heating end point temperature is 100 ℃; the heating heat preservation time is 45 min;
(2) adding ammonium salt into the treatment liquid obtained in the step (1) and carrying out solid-liquid separation to obtain a solid; wherein the ammonium salt comprises ammonium sulfate and/or ammonium chloride; the coefficient of ammonium addition in the addition of the ammonium salt is 4;
(3) washing the solid obtained in the step (2), and then melting to obtain high-purity vanadium pentoxide; the flushing medium is water; the mass of the water is 5.5 times of the mass of the solid; the melting temperature is 1200 ℃; the time for melting is 60 ℃;
the purity of the obtained high-purity vanadium pentoxide is 99.73%.
Comparative example 1
The only difference from example 1 is that the pH of the solution after dissolution is 7, and the purity of the obtained high-purity vanadium pentoxide is 99.6%. But the vanadium loss is increased by 30-50%
Comparative example 2
The only difference from example 1 is that the pH of the solution after dissolution is 11 and the purity of the obtained high-purity vanadium pentoxide is 99.32%. The purity is slightly reduced, but the material consumption is increased.
Comparative example 3
The difference from the embodiment 1 is only that the addition amount of the polymeric alumina is 3 per mill of the solution mass, and the purity of the obtained high-purity vanadium pentoxide is 98.94%.
Comparative example 4
The difference from the example 1 is only that the addition amount of the polymeric alumina is 10 per mill of the solution mass, and the purity of the obtained high-purity vanadium pentoxide is 99.3%.
According to the results of the above examples and comparative examples, the method provided by the invention has the advantages that through reasonable selection of the steps, the polyaluminium chloride is used for impurity removal, the operation of the impurity removal process is simple, secondary vanadium precipitation is only needed for washing ammonium metavanadate, ammonia water is not needed, the large-scale industrial production is easy to realize, and the cost is low. The grade of the produced vanadium pentoxide can reach more than 99.6 percent.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. A preparation method of vanadium pentoxide is characterized by comprising the following steps:
(1) dissolving ammonium vanadate in an alkali solution, adding an auxiliary agent, and heating to obtain a treatment solution;
(2) adding ammonium salt into the treatment liquid obtained in the step (1) and carrying out solid-liquid separation to obtain a solid;
(3) and (3) washing the solid obtained in the step (2), and then melting to obtain high-purity vanadium pentoxide.
2. The method of claim 1, wherein the ammonium vanadate of step (1) comprises ammonium metavanadate and/or ammonium polyvanadate;
preferably, the alkali solution of step (1) comprises a sodium hydroxide solution and/or a potassium hydroxide solution;
preferably, the pH value of the solution after dissolving in the step (1) is 8.5-9.5.
3. The method of claim 1 or 2, wherein the auxiliary agent of step (1) comprises polyaluminium chloride and a flocculating agent.
4. The method of claim 3, wherein the polymeric alumina is added in an amount of 4.5 to 6% o by mass of the solution;
preferably, the addition amount of the flocculating agent is 0.0008-0.001 per mill of the solution mass.
5. The method of any one of claims 1-4, wherein the end temperature of the heating of step (1) is 90-100 ℃;
preferably, the heating in the step (1) is kept for 30-45 min.
6. The method of any one of claims 1 to 5, wherein the ammonium salt of step (2) comprises ammonium sulfate and/or ammonium chloride;
preferably, the ammonium salt is added with an ammonium addition coefficient of 3-4.
7. The method of any one of claims 1-6, wherein the flushing medium of step (3) is water;
preferably, the mass of the water is 4 to 5.5 times the mass of the solid.
8. The method according to any one of claims 1 to 7, wherein the melting temperature in step (3) is 1000-1200 ℃;
preferably, the time for melting is 30-60 min.
9. The method according to any one of claims 1 to 8, wherein the purity of the high-purity vanadium pentoxide in the step (3) is 99.6% or more.
10. A method according to any one of claims 1-9, characterized in that the method comprises the steps of:
(1) dissolving ammonium vanadate in an alkali solution, adding an auxiliary agent, and heating to obtain a treatment solution; wherein the ammonium vanadate salt comprises ammonium metavanadate and/or ammonium polyvanadate; the alkali solution comprises a sodium hydroxide solution and/or a potassium hydroxide solution; the pH value of the dissolved solution is 8.5-9.5; the auxiliary agent comprises polyaluminium chloride and a flocculating agent; the addition amount of the polymeric alumina is 4.5-6 per mill of the mass of the solution; the addition amount of the flocculating agent is 0.0008-0.001 per mill of the mass of the solution; the heating end point temperature is 90-100 ℃; the heating and heat preservation time is 30-45 min;
(2) adding ammonium salt into the treatment liquid obtained in the step (1) and carrying out solid-liquid separation to obtain a solid; wherein the ammonium salt comprises ammonium sulfate and/or ammonium chloride; the coefficient of adding ammonium in the addition of the ammonium salt is 3-4;
(3) washing the solid obtained in the step (2), and then melting to obtain high-purity vanadium pentoxide; the flushing medium is water; the mass of the water is 4-5.5 times of the mass of the solid; the melting temperature is 1000-1200 ℃; the melting time is 30-60 min; the purity of the high-purity vanadium pentoxide is more than or equal to 99.6%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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