CN108220600A - The minimizing technology of phosphorus in a kind of acidity vanadium leachate - Google Patents

The minimizing technology of phosphorus in a kind of acidity vanadium leachate Download PDF

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Publication number
CN108220600A
CN108220600A CN201810051525.6A CN201810051525A CN108220600A CN 108220600 A CN108220600 A CN 108220600A CN 201810051525 A CN201810051525 A CN 201810051525A CN 108220600 A CN108220600 A CN 108220600A
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vanadium leachate
phosphorus
component
acid vanadium
leachate
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谢昭明
张也可
刘作华
陶长元
杜军
范兴
刘仁龙
吴丙山
孔令峰
唐金晶
何文艺
邓丽
邓容锐
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Chongqing University
Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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Chongqing University
Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/20—Obtaining niobium, tantalum or vanadium
    • C22B34/22—Obtaining vanadium
    • 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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  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a kind of minimizing technologies of phosphorus in acid vanadium leachate；The pH value of acid vanadium leachate that this method is related to is 2.5~4.0, a concentration of 0.3g/L~1.5g/L of phosphorus.Oxidation processes, A NaClO, HClO, H are carried out to acid vanadium leachate using oxidant A in this method2O2、KMnO4Or (NH4)2S2O8In one kind；Dephosphorization agent is composite dephosphorizing agent, is mainly made of two kinds of components of B, C, and B component is [Fe (OH)n(SO4)m]q、FeSO4、Fe2(SO4)3In one kind, wherein 0.5≤n≤2,1≤m≤3,10≤q≤100000；Component C is Al2(SO4)3、MgO、CaO、ZrSO4And PbSO4One kind therein；B component and component C and the molar ratio of phosphorus in acid vanadium leachate are 0.1~3:1；Component C and the molar ratio of phosphorus in acid vanadium leachate are 0.1~3:1.This method is after acid vanadium leachate is added in oxidant progress oxidation processes, to add in composite dephosphorizing agent to carry out dephosphorization.Compared with prior art, the advantages of present invention has simple for process, and dephosphorization efficiency is high and phosphor-removing effect is stablized.

Description

The minimizing technology of phosphorus in a kind of acidity vanadium leachate
Technical field
The present invention relates to dephosphorization treatment field, the minimizing technology of phosphorus in specifically a kind of acidity vanadium leachate.
Background technology
Vanadium is a kind of strategic resources, is widely used in every field, wherein the vanadium for having more than 90% is applied to steel The smelting of iron, it can significantly improve hardness, intensity, abrasion resistance and the ductility of steel, improve the cutting ability of steel.But the world The upper enrichment ore deposit there is no vanadium, therefore mostly vanadium is extracted using Converter Vanadium-bearing Slag as raw material.
" calcification baking-acidleach-precipitation-calcining " technique is a kind of novel cleaning process for extracting vanadium.But in acidleach process In, other impurity also enter acid vanadium leachate while vanadium is leached.In acid condition, especially phosphorus meeting and pickle liquor In vanadium combine form heteropoly acid, so as to influence final vanadium product (V2O5) quality.Therefore, acid vanadium is soaked before precipitation Go out liquid and carry out dephosphorization pretreatment, be necessary process to improve the purity of final vanadium product and quality, the development to following vanadium industry Also it has great significance.
In the prior art, most phosphorus removing method is both for the sanitary sewage of weakly acidic pH or industrial wastewater etc., and needle Dephosphorization to vanadium leachate is also mostly under alkaline system, and for acid vanadium leachate, the form of phosphorus therein has complexity Diversity, the different shape (such as phosphate, pyrophosphate, metaphosphate) not only containing high-valence state phosphorus, and there are lower valencies Phosphorus.
There is complex process, dephosphorization efficiency be not high and phosphor-removing effect is unstable for the phosphorus removing method of existing acidity vanadium leachate The shortcomings of.
Invention content
Present invention aim to address problems of the prior art, provide a kind of removal of phosphorus in acid vanadium leachate Method.
To realize the present invention purpose and the technical solution adopted is that such, the removal side of phosphorus in a kind of acidity vanadium leachate Method, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 2.5~4.0, wherein a concentration of 0.3g/L~1.5g/L of phosphorus；
2) under the conditions of 20 DEG C~80 DEG C, with 0.1M NaOH solutions by the control of the pH value of acid vanadium leachate 2.5~ Between 6.5, oxidant A is added in acid vanadium leachate, stirs, mixing liquid A is obtained after 0.1~3 hour；
The oxidant A is NaClO, HClO, H2O2、KMnO4Or (NH4)2S2O8In one kind；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is (1~30) ︰ 1；
3) under the conditions of 20 DEG C~80 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, is stirred, After 0.5~5 hour, mixing liquid B is obtained；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are (0.1~3) ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are (0.1~3) ︰ 1；
The B component is [Fe (OH)n(SO4)m]q、FeSO4、Fe2(SO4)3In one kind；
Wherein：0.5≤n≤2,1≤m≤3,10≤q≤100000；
The component C is Al2(SO4)3、MgO、CaO、ZrSO4Or PbSO4In one kind；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid；
The digestion time is 0.1~3 hour.
The solution have the advantages that unquestionable, the present invention has the following advantages；
1) present invention when carrying out dephosphorization, is employing oxidant A for the acid vanadium leachate for including complicated form Oxidation processes are carried out to acid vanadium leachate, dephosphorization is carried out by the composite dephosphorizing agent that two kinds of components are formed.
1.1) B component in the composite dephosphorizing agent used is capable of providing Fe in acid vanadium leachate3+With PO4 3-Reaction, it is raw Into FePO4Precipitation；And Fe3+Strong hydrolysis can occur, while polymerisation occurs, generate iron-containing hydroxo complex, such as Fe2(OH)2 4+、Fe3(OH)4 5+Deng can effectively reduce or eliminate the electric potential of colloid in water body, pass through charge neutrality, adsorptive racks The volume effect of sweeping of bridge and flco makes coacervation of colloid, then by precipitating phosphorus ligands.
1.2) metal ion in component C in the composite dephosphorizing agent used has and Fe3+The same effect, and can promote Phosphate hydrolysis is into orthophosphoric acid root (PO4 3-)。
1.3) phosphorus in acid vanadium leachate is converted to orthophosphoric acid root (PO by the oxidant A used4 3-)。
1.4) in the present invention under the oxidation of oxidant A and the synergistic effect of composite dephosphorizing agent B component and component C, It can be by phosphorus ligands a large amount of in a kind of this acid vanadium leachate (involved reaction equation is as shown in annex in reaction).
2) operation of the invention is extremely simple, also without introducing on the influential impurity of subsequent vanadium extracting process, reacts item Part is mild.
Therefore, for a kind of this acid vanadium leachate, compared with prior art compared with present invention process is simple, removes Phosphorus is efficient and phosphor-removing effect is stablized.
Description of the drawings
Fig. 1 the present invention relates to reaction equation.
Specific embodiment
With reference to embodiment, the invention will be further described, but should not be construed the above-mentioned subject area of the present invention only It is limited to following embodiments.Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and used With means, various replacements and change are made, should all be included within the scope of the present invention.
Embodiment 1：
The minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 2.5, the wherein a concentration of 0.723g/L of phosphorus；
2) under the conditions of 30 DEG C, oxidant A is added in acid vanadium leachate, stirs, mixed liquor is obtained after 0.1 hour Body A；
The oxidant A is NaClO；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is 1 ︰ 1；
3) under the conditions of 30 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, stirring, 0.1 is small Shi Hou obtains mixing liquid B；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are 0.1 ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are 0.1 ︰ 1；
The B component is [Fe (OH)n(SO4)m]q；
Wherein：0.5≤n≤2,1≤m≤3,10≤q≤100000；
The component C is Al2(SO4)3；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid；
The digestion time is 0.1 hour.
In the present embodiment, residual phosphorus concentration is 0.015g/L in the vanadium leachate after dephosphorization.
Embodiment 2：
The minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 2.5, the wherein a concentration of 1.294g/L of phosphorus；
2) under the conditions of 20 DEG C, the pH value of acid vanadium leachate is adjusted to 3.0 with 0.1M NaOH solutions, by oxidant A It is added in acid vanadium leachate, stirs, mixing liquid A is obtained after 0.5 hour；
The oxidant A is HClO；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is 5 ︰ 1；
3) under the conditions of 50 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, stirring, 0.5 is small Shi Hou obtains mixing liquid B；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are 0.5 ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are 0.1 ︰ 1；
The B component is FeSO4；
The component C is MgO；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid；
The digestion time is 0.5 hour.
In the present embodiment, residual phosphorus concentration is 0.012g/L in the vanadium leachate after dephosphorization.
Embodiment 3：
The minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 3.0, the wherein a concentration of 0.821g/L of phosphorus；
2) under the conditions of 60 DEG C, the pH value of acid vanadium leachate is adjusted to 4.5 with 0.1M NaOH solutions, by oxidant A It is added in acid vanadium leachate, stirs, mixing liquid A is obtained after 1 hour；
The oxidant A is H2O2；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is 10 ︰ 1；
3) under the conditions of 20 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, is stirred, 1 hour Afterwards, mixing liquid B is obtained；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are 0.1 ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are 0.5 ︰ 1；
The B component is Fe2(SO4)3；
The component C is CaO；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid；
The digestion time is 1 hour.
In the present embodiment, residual phosphorus concentration is 0.016g/L in the vanadium leachate after dephosphorization.
Embodiment 4：
The minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 4.0, the wherein a concentration of 0.523g/L of phosphorus；
2) under the conditions of 50 DEG C, the pH value of acid vanadium leachate is adjusted to 5.0 with 0.1M NaOH solutions, by oxidant A It is added in acid vanadium leachate, stirs, mixing liquid A is obtained after 2 hours；
The oxidant A is KMnO4；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is 15 ︰ 1；
3) under the conditions of 40 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, stirring, 1.5 is small Shi Hou obtains mixing liquid B；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are 1.25 ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are 0.4 ︰ 1；
The B component is FeSO4；
The component C is ZrSO4；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid；
The digestion time is 2 hours.
In the present embodiment, residual phosphorus concentration is 0.010g/L in the vanadium leachate after dephosphorization.
Embodiment 5：
The minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 3.5, the wherein a concentration of 0.746g/L of phosphorus；
2) under the conditions of 40 DEG C, the pH value of acid vanadium leachate is adjusted to 5.5 with 0.1M NaOH solutions, by oxidant A It is added in acid vanadium leachate, stirs, mixing liquid A is obtained after 2.5 hours；
The oxidant A is (NH4)2S2O8；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is 25 ︰ 1；
3) under the conditions of 70 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, is stirred, 3 hours Afterwards, mixing liquid B is obtained；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are 1.5 ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are 0.1 ︰ 1；
The B component is [Fe (OH)n(SO4)m]q；
Wherein：0.5≤n≤2,1≤m≤3,10≤q≤100000；
The component C is PbSO4；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid；
The digestion time is 1.5 hours.
In the present embodiment, residual phosphorus concentration is 0.019g/L in the vanadium leachate after dephosphorization.
Embodiment 6：
The minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 4.0, the wherein a concentration of 1.175g/L of phosphorus；
2) under the conditions of 70 DEG C, the pH value of acid vanadium leachate is adjusted to 6.0 with 0.1M NaOH solutions, by oxidant A It is added in acid vanadium leachate, stirs, mixing liquid A is obtained after 3 hours；
The oxidant A is HClO；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is 20 ︰ 1；
3) under the conditions of 80 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, is stirred, 3 hours Afterwards, mixing liquid B is obtained；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are 2.0 ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are 0.4 ︰ 1；
The B component is FeSO4；
The component C is CaO；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid；
The digestion time is 3 hours.
In the present embodiment, residual phosphorus concentration is 0.015g/L in the vanadium leachate after dephosphorization.
Embodiment 7：
The minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 2.5, the wherein a concentration of 0.783g/L of phosphorus；
2) under the conditions of 80 DEG C, the pH value of acid vanadium leachate is adjusted to 6.5 with 0.1M NaOH solutions, by oxidant A It is added in acid vanadium leachate, stirs, mixing liquid A is obtained after 1 hour；
The oxidant A is NaClO；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is 10 ︰ 1；
3) under the conditions of 20 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, is stirred, 1 hour Afterwards, mixing liquid B is obtained；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are 3.0 ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are 0.4 ︰ 1；
The B component is Fe2(SO4)3；
The component C is Al2(SO4)3；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid；
The digestion time is 2.5 hours.
In the present embodiment, residual phosphorus concentration is 0.016g/L in the vanadium leachate after dephosphorization.
Embodiment 8：
The minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 3.5, the wherein a concentration of 0.953g/L of phosphorus；
2) under the conditions of 50 DEG C, oxidant A is added in acid vanadium leachate, stirs, mixing liquid is obtained after 3 hours A；
The oxidant A is KMnO4；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is 5 ︰ 1；
3) under the conditions of 60 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, stirring, 0.5 is small Shi Hou obtains mixing liquid B；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are 1.0 ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are 0.1 ︰ 1；
The B component is [Fe (OH)n(SO4)m]q；
Wherein：0.5≤n≤2,1≤m≤3,10≤q≤100000；
The component C is Al2(SO4)3；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid；
The digestion time is 0.1 hour.
In the present embodiment, residual phosphorus concentration is 0.017g/L in the vanadium leachate after dephosphorization.
Embodiment 9：
The minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 3.0, the wherein a concentration of 0.481g/L of phosphorus；
2) under the conditions of 40 DEG C, the pH value of acid vanadium leachate is adjusted to 5.0 with 0.1M NaOH solutions, by oxidant A It is added in acid vanadium leachate, stirs, mixing liquid A is obtained after 0.5 hour；
The oxidant A is NaClO；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is 30 ︰ 1；
3) under the conditions of 20 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, is stirred, 2 hours Afterwards, mixing liquid B is obtained；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are 0.1 ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are 0.5 ︰ 1；
The B component is [Fe (OH)n(SO4)m]q；
Wherein：0.5≤n≤2,1≤m≤3,10≤q≤100000；
The component C is MgO；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid.
The digestion time is 0.1 hour.
In the present embodiment, residual phosphorus concentration is 0.013g/L in the vanadium leachate after dephosphorization.
Embodiment 10：
The minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 4.0, the wherein a concentration of 0.851g/L of phosphorus；
2) under the conditions of 70 DEG C, the pH value of acid vanadium leachate is adjusted to 4.5 with 0.1M NaOH solutions, by oxidant A It is added in acid vanadium leachate, stirs, mixing liquid A is obtained after 1 hour；
The oxidant A is (NH4)2S2O8；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is 15 ︰ 1；
3) under the conditions of 50 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, is stirred, 3 hours Afterwards, mixing liquid B is obtained；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are 0.5 ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are 1 ︰ 1；
The B component is Fe2(SO4)3；
The component C is PbSO4；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid.
The digestion time is 1.5 hours.
In the present embodiment, residual phosphorus concentration is 0.019g/L in the vanadium leachate after dephosphorization.
Embodiment 11：
The minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 2.5, the wherein a concentration of 0.963g/L of phosphorus；
2) under the conditions of 60 DEG C, the pH value of acid vanadium leachate is adjusted to 4.0 with 0.1M NaOH solutions, by oxidant A It is added in acid vanadium leachate, stirs, mixing liquid A is obtained after 2.5 hours；
The oxidant A is H2O2；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is 10 ︰ 1；
3) under the conditions of 30 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, is stirred, 5 hours Afterwards, mixing liquid B is obtained；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are 1.25 ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are 0.5 ︰ 1；
The B component is Fe2(SO4)3；
The component C is MgO；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid.
The digestion time is 1.0 hours.
In the present embodiment, residual phosphorus concentration is 0.017g/L in the vanadium leachate after dephosphorization.
Embodiment 12：
The minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 3.0, the wherein a concentration of 1.076g/L of phosphorus；
2) under the conditions of 30 DEG C, the pH value of acid vanadium leachate is adjusted to 6.0 with 0.1M NaOH solutions, by oxidant A It is added in acid vanadium leachate, stirs, mixing liquid A is obtained after 1 hour；
The oxidant A is KMnO4；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is 20 ︰ 1；
3) under the conditions of 60 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, stirring, 0.1 is small Shi Hou obtains mixing liquid B；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are 3 ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are 2 ︰ 1；
The B component is [Fe (OH)n(SO4)m]q；
Wherein：0.5≤n≤2,1≤m≤3,10≤q≤100000；
The component C is PbSO4；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid.
The digestion time is 3 hours.
In the present embodiment, residual phosphorus concentration is 0.015g/L in the vanadium leachate after dephosphorization.
Embodiment 13：
The minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 2.5, the wherein a concentration of 0.592g/L of phosphorus；
2) under the conditions of 50 DEG C, the pH value of acid vanadium leachate is adjusted to 6.5 with 0.1M NaOH solutions, by oxidant A It is added in acid vanadium leachate, stirs, mixing liquid A is obtained after 1 hour；
The oxidant A is NaClO；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is 25 ︰ 1；
3) under the conditions of 40 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, is stirred, 2 hours Afterwards, mixing liquid B is obtained；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are 2 ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are 1 ︰ 1；
The B component is FeSO4；
The component C is CaO；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid.
The digestion time is 2.5 hours.
In the present embodiment, residual phosphorus concentration is 0.016g/L in the vanadium leachate after dephosphorization.
Embodiment 14：
The minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 3.5, the wherein a concentration of 1.457g/L of phosphorus；
2) under the conditions of 60 DEG C, oxidant A is added in acid vanadium leachate, stirs, mixed liquor is obtained after 0.5 hour Body A；
The oxidant A is H2O2；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is 15 ︰ 1；
3) under the conditions of 50 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, is stirred, 3 hours Afterwards, mixing liquid B is obtained；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are 0.5 ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are 3 ︰ 1；
The B component is Fe2(SO4)3；
The component C is Al2(SO4)3；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid.
The digestion time is 0.5 hour.
In the present embodiment, residual phosphorus concentration is 0.018g/L in the vanadium leachate after dephosphorization.
Embodiment 15：
The minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 4.0, the wherein a concentration of 0.658g/L of phosphorus；
2) under the conditions of 20 DEG C, the pH value of acid vanadium leachate is adjusted to 5.5 with 0.1M NaOH solutions, by oxidant A It is added in acid vanadium leachate, stirs, mixing liquid A is obtained after 2 hours；
The oxidant A is (NH4)2S2O8；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is 5 ︰ 1；
3) under the conditions of 80 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, is stirred, 1 hour Afterwards, mixing liquid B is obtained；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are 1.25 ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are 3 ︰ 1；
The B component is [Fe (OH)n(SO4)m]q；
Wherein：0.5≤n≤2,1≤m≤3,10≤q≤100000；
The component C is CaO；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid.
The digestion time is 0.1 hour.
In the present embodiment, residual phosphorus concentration is 0.017g/L in the vanadium leachate after dephosphorization.
Embodiment 16：
The minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 3.0, the wherein a concentration of 0.396g/L of phosphorus；
2) under the conditions of 80 DEG C, the pH value of acid vanadium leachate is adjusted to 4.0 with 0.1M NaOH solutions, by oxidant A It is added in acid vanadium leachate, stirs, mixing liquid A is obtained after 3 hours；
The oxidant A is HClO；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is 15 ︰ 1；
3) under the conditions of 50 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, stirring, 1.5 is small Shi Hou obtains mixing liquid B；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are 3 ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are 3 ︰ 1；
The B component is FeSO4；
The component C is ZrSO4；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the leaching of the vanadium after dephosphorization Liquid.
The digestion time is 1.5 hours.
In the present embodiment, residual phosphorus concentration is 0.010g/L in the vanadium leachate after dephosphorization.

Claims (1)

1. the minimizing technology of phosphorus in a kind of acidity vanadium leachate, which is characterized in that include the following steps：
1) acid vanadium leachate is placed in container；
The pH value of the acidity vanadium leachate is 2.5~4.0, wherein a concentration of 0.3g/L~1.5g/L of phosphorus；
2) under the conditions of 20 DEG C~80 DEG C, with 0.1M NaOH solutions by the control of the pH value of acid vanadium leachate 2.5~6.5 it Between, oxidant A is added in acid vanadium leachate, stirs, mixing liquid A is obtained after 0.1~3 hour；
The oxidant A is NaClO, HClO, H2O2、KMnO4Or (NH4)2S2O8In one kind；
The molar ratio of the oxidant A and phosphorus in acid vanadium leachate is (1~30) ︰ 1.
3) under the conditions of 20 DEG C~80 DEG C, in the mixing liquid A obtained into step 2), composite dephosphorizing agent is added in, is stirred, 0.1 After~5 hours, mixing liquid B is obtained；
The composite dephosphorizing agent includes B component and component C；
The B component and the molar ratio of phosphorus in acid vanadium leachate are (0.1~3) ︰ 1；
The component C and the molar ratio of phosphorus in acid vanadium leachate are (0.1~3) ︰ 1；
The B component is [Fe (OH)n(SO4)m]q、FeSO4、Fe2(SO4)3In one kind；
Wherein：0.5≤n≤2,1≤m≤3,10≤q≤100000；
The component C is Al2(SO4)3、MgO、CaO、ZrSO4Or PbSO4In one kind；
4) it after the obtained mixing liquid B ageings by dephosphorization after reaction, is filtered, obtains the vanadium leachate after dephosphorization； The digestion time is 0.1~3 hour.
CN201810051525.6A 2018-01-19 2018-01-19 The minimizing technology of phosphorus in a kind of acidity vanadium leachate Pending CN108220600A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109022786A (en) * 2018-10-23 2018-12-18 攀钢集团研究院有限公司 Except the method for silicon phosphorus in acid solution containing vanadium
CN109179617A (en) * 2018-10-23 2019-01-11 攀钢集团研究院有限公司 A kind of dephosphorization agent and preparation method thereof and application method
CN109182752A (en) * 2018-10-23 2019-01-11 攀钢集团研究院有限公司 The method that desilication slag removes phosphorus in acid vanadium liquid
CN109234532A (en) * 2018-10-23 2019-01-18 攀钢集团研究院有限公司 Dephosphorization agent and preparation method thereof and application method
CN109399778A (en) * 2018-10-23 2019-03-01 攀钢集团研究院有限公司 Except silicon phosphorus agent and preparation method thereof and application method
CN109852820A (en) * 2019-02-22 2019-06-07 梁刘友 A method of producing vanadic anhydride
CN110423890A (en) * 2019-08-28 2019-11-08 重庆大学 A method of the deep phosphorous removal in acid vanadium extraction solution

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012140668A (en) * 2010-12-28 2012-07-26 Jx Nippon Mining & Metals Corp Method for preparing refined nickel solution, method for manufacturing nickel metal, and method for manufacturing nickel carbonate
CN102943176A (en) * 2012-11-08 2013-02-27 长沙矿冶研究院有限责任公司 Method for removing silicon and phosphorus impurities from rich-vanadium desorption liquid
CN103818965A (en) * 2014-03-20 2014-05-28 重庆大学 Phosphorous removal method for manganous sulfate produced from high-phosphorus rhodochrosite
CN104480308A (en) * 2015-01-02 2015-04-01 重庆大学 Dephosphorizing method for acid vanadium leached solution
CN104894374A (en) * 2015-06-05 2015-09-09 攀钢集团攀枝花钢铁研究院有限公司 Method for carrying out phosphorus removal on acidic vanadium-containing solution
CN106477772A (en) * 2016-11-09 2017-03-08 武汉青江化工黄冈有限公司 A kind of high phosphorus trade effluent dephosphorization and its reclamation of phosphorus resource method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012140668A (en) * 2010-12-28 2012-07-26 Jx Nippon Mining & Metals Corp Method for preparing refined nickel solution, method for manufacturing nickel metal, and method for manufacturing nickel carbonate
CN102943176A (en) * 2012-11-08 2013-02-27 长沙矿冶研究院有限责任公司 Method for removing silicon and phosphorus impurities from rich-vanadium desorption liquid
CN103818965A (en) * 2014-03-20 2014-05-28 重庆大学 Phosphorous removal method for manganous sulfate produced from high-phosphorus rhodochrosite
CN104480308A (en) * 2015-01-02 2015-04-01 重庆大学 Dephosphorizing method for acid vanadium leached solution
CN104894374A (en) * 2015-06-05 2015-09-09 攀钢集团攀枝花钢铁研究院有限公司 Method for carrying out phosphorus removal on acidic vanadium-containing solution
CN106477772A (en) * 2016-11-09 2017-03-08 武汉青江化工黄冈有限公司 A kind of high phosphorus trade effluent dephosphorization and its reclamation of phosphorus resource method

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109022786A (en) * 2018-10-23 2018-12-18 攀钢集团研究院有限公司 Except the method for silicon phosphorus in acid solution containing vanadium
CN109179617A (en) * 2018-10-23 2019-01-11 攀钢集团研究院有限公司 A kind of dephosphorization agent and preparation method thereof and application method
CN109182752A (en) * 2018-10-23 2019-01-11 攀钢集团研究院有限公司 The method that desilication slag removes phosphorus in acid vanadium liquid
CN109234532A (en) * 2018-10-23 2019-01-18 攀钢集团研究院有限公司 Dephosphorization agent and preparation method thereof and application method
CN109399778A (en) * 2018-10-23 2019-03-01 攀钢集团研究院有限公司 Except silicon phosphorus agent and preparation method thereof and application method
CN109179617B (en) * 2018-10-23 2021-08-24 攀钢集团研究院有限公司 Phosphorus removing agent and preparation method and use method thereof
CN109399778B (en) * 2018-10-23 2021-08-31 攀钢集团研究院有限公司 Silicon and phosphorus removing agent and preparation method and use method thereof
CN109852820A (en) * 2019-02-22 2019-06-07 梁刘友 A method of producing vanadic anhydride
CN110423890A (en) * 2019-08-28 2019-11-08 重庆大学 A method of the deep phosphorous removal in acid vanadium extraction solution
CN110423890B (en) * 2019-08-28 2021-06-18 重庆大学 Method for deeply removing phosphorus in acidic vanadium extraction solution

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