CN104480308A - Dephosphorizing method for acid vanadium leached solution - Google Patents

Dephosphorizing method for acid vanadium leached solution Download PDF

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Publication number
CN104480308A
CN104480308A CN201510000089.6A CN201510000089A CN104480308A CN 104480308 A CN104480308 A CN 104480308A CN 201510000089 A CN201510000089 A CN 201510000089A CN 104480308 A CN104480308 A CN 104480308A
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component
phosphorus
acid vanadium
leached solution
equal
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Inventor
刘作华
陈嫚丽
陶长元
范兴
杜军
刘仁龙
周小霞
谢昭明
孙大贵
左赵宏
孔令峰
彭浩
黄国平
刘敏
张兴然
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Chongqing University
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Chongqing University
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

The invention provides a dephosphorizing method for an acid vanadium leached solution. The pH value of the acid vanadium leached solution involved in the dephosphorizing method ranges from 2.5 to 4.0, and the phosphorus concentration ranges from 0.6 g/L to 1.5 g/L; the phosphate removing agent adopted in the method is a composite phosphate removing agent composed of a component A and a component B, wherein the component A is one of Al2(SO4)3, MgSO4, CaSO4, SrSO4 and ZnSO4; the component B is [Fe(OH)n(SO4)m]q; in [Fe(OH)n(SO4)m]q, n is greater than or equal to 0.5 and less than or equal to 2, m is greater than or equal to 1 and less than or equal to 3, and q is greater than or equal to 10 and less than or equal to 100000; the molar ratio of the component A to phosphorus in the acid vanadium leached solution and the molar ratio of the component B to the phosphorus in the acid vanadium leached solution are both 0.1-5:1. According to the method, firstly, the composite phosphate removing agent is added into the acid vanadium leached solution for direct phosphorous removal; secondly, reaction liquid is subjected to aging and filtration, and then a dephosphorized vanadium leached solution is obtained. Compared with the prior art, the method has the advantages that the process is simple, and the dephosphorizing rate is high.

Description

Phosphorus removing method in a kind of acid vanadium leachate
Technical field
The present invention relates to the method for the acid vanadium leachate produced by From Converter Vanadium-bearing Slag being carried out to dephosphorization treatment.
Background technology
Vanadium has multiple use, is a kind of important strategic resource.Large is at present that raw material carrys out therefrom vanadium extraction mainly with From Converter Vanadium-bearing Slag, vanadium extracting process is, grog is obtained by after From Converter Vanadium-bearing Slag calcification baking, carry out leaching obtaining acid containing vanadium leachate (acid vanadium leachate) using sulfuric acid as leaching agent, and then the precipitation that is hydrolyzed is to be precipitated thing ammonium poly-vanadate [ (NH 4) 2v 6o 16, eventually pass calcining and obtain vanadium extraction goods Vanadium Pentoxide in FLAKES (V 2o 5).Because some impurity elements contained in acid vanadium leachate can have a negative impact to vanadium extracting process; Especially when phosphorus content is excessive, not only can reduce the output capacity of vanadium extraction goods, even also can affect its purity.Therefore, dephosphorization in acid vanadium leachate (usually also incidentally eliminating other impurity) just becomes the operation of can not ignore together.But, in existing phosphorus removing method, except for phosphorus with more single form (H 2pO 4 -, HPO 4 2-or PO 4 3-) outside the acid vanadium leachate that exists, pH value is not more than to the acid vanadium leachate including complicated form microcosmic salt (tri-polyphosphate, phosphorous heteropolyacid salt etc.) of 4, just there is technique more complicated, or the not high enough deficiency of dephosphorizing rate.
Summary of the invention
The object of the invention is, provide that a kind of technique is comparatively simple and dephosphorizing rate is higher, pH value is not more than the phosphorus removing method included in the acid vanadium leachate of complicated form microcosmic salt of 4.
For realizing described object, provide the phosphorus removing method in a kind of so acid vanadium leachate.The pH value of acid vanadium leachate described in this phosphorus removing method is 2.5 ~ 4.0, and the concentration of phosphorus is 0.6g/L ~ 1.5g/L; Dephosphorization agent used during dephosphorization is the composite dephosphorizing agent be made up of component A and B component, and component A is Al 2(SO 4) 3, MgSO 4, CaSO 4, SrSO 4and ZnSO 4in one, B component is [Fe (OH) n(SO 4) m] q, at [Fe (OH) n(SO 4) m] qin, 0.5≤n≤2,1≤m≤3,10≤q≤100000; The step of this phosphorus removing method is as follows:
(1) add composite dephosphorizing agent at described acid vanadium leaching liquid, temperature controls fully to stir between 80 DEG C at 20 DEG C, to carry out except phosphorus reaction; Wherein, in described component A and B component and acid vanadium leachate, the mol ratio of phosphorus is 0.1 ~ 5: 1;
(2) in step (1) except after phosphorus reaction can not proceed down again, filter after reaction solution ageing, obtain the vanadium leachate after dephosphorization.
As can be seen from scheme, the present invention, when the acid vanadium leachate including complicated form microcosmic salt being not more than 4 for pH value is to carry out dephosphorization process, have employed the composite dephosphorizing agent be made up of two kinds of components.Due to the B component [Fe (OH) in this composite dephosphorizing agent n(SO 4) m] qcan ionize in acid vanadium leachate and produce Fe 3+, and Fe 3+can with PO 4 3-reaction, generates FePO 4precipitation, and Fe 3+strong hydrolysis can be there is, various polyreaction occurs simultaneously, generate the hydroxo complex of iron content, as Fe 2(OH) 2 4+, Fe 3(OH) 4 5+, Fe 5(OH) 9 6+deng, the hydroxo complex of these iron content can reduce or eliminate the electrokinetic potential (zeta-potential) of colloid in water body effectively, makes coacervation of colloid by the volume effect of sweeping of charge neutrality, adsorption bridging and flco, then by precipitate and separate by phosphorus ligands.Component A in this composite dephosphorizing agent, the tri-polyphosphate of the complex constructions such as long-chain shape, ring-type and caged, phosphorous heteropolyacid salt etc. being had to the effect of hydrolysis, depolymerization, can be ortho-phosphoric acid root (PO by the Phosphate hydrolysis that these structures (form) in acid vanadium leachate are complicated 4 3-).So, in composite dephosphorizing agent of the present invention component A and B component synergy under, just can remove phosphorus a large amount of in this kind of acid vanadium leachate.It can also be seen that from scheme, operation of the present invention is extremely simple, does not also introduce the influential impurity of follow-up vanadium extracting process, and reaction conditions is gentle.Therefore, for this kind of acid vanadium leachate, compared with prior art, the method that technique really of the present invention is comparatively simple and dephosphorizing rate is higher.
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment
Phosphorus removing method in a kind of acid vanadium leachate.In the present invention, the pH value of described acid vanadium leachate is 2.5 ~ 4.0, and the concentration of phosphorus is 0.6g/L ~ 1.5g/L; Dephosphorization agent used during dephosphorization is the composite dephosphorizing agent be made up of component A and B component, and component A is Al 2(SO 4) 3(Tai-Ace S 150), MgSO 4(magnesium sulfate), CaSO 4(calcium sulfate), SrSO 4(Strontium Sulphate) and ZnSO 4one in (zinc sulfate), B component is [Fe (OH) n(SO 4) m] q(bodied ferric sulfate), at [Fe (OH) n(SO 4) m] qin, 0.5≤n≤2,1≤m≤3,10≤q≤100000; The step of this phosphorus removing method is as follows:
(1) add composite dephosphorizing agent at described acid vanadium leaching liquid, temperature controls fully to stir between 80 DEG C at 20 DEG C, to carry out except phosphorus reaction; Wherein, in described component A and B component and acid vanadium leachate, the mol ratio of phosphorus is 0.1 ~ 5: 1;
(2) in step (1) except after phosphorus reaction can not proceed down (being generally 0.1 ~ 5 hour) again, filter after reaction solution ageing, obtain the vanadium leachate after dephosphorization (digestion time is generally 0.5 ~ 3h).
The present invention have passed the experimental verification done in laboratory, and verification step is identical with the step of above-mentioned embodiment.The result is shown in proof list.
Before and after checking, the initial phosphorus concentration (being abbreviated as in proof list " first phosphorus concentration ") when all adopting GB/T1515-2002 " the mensuration P-Mo blue spectrophotometry of manganese ore phosphorus content " to measure the non-dephosphorization of acid vanadium leachate and the reacted phosphorus concentration of dephosphorization (being abbreviated as in proof list " residual phosphorus concentration ").In proof list, in composite dephosphorizing agent, the Tai-Ace S 150 of component A, magnesium sulfate, calcium sulfate, zinc sulfate, Strontium Sulphate are in turn represented respectively by " A1 " ~ " A5 ", symbol " " represent that this example selects this component; " A: B: P " be with mole for contrast unit composite dephosphorizing agent in component A: B component: the proportion expression of the phosphorus (P) before dephosphorization in acid vanadium leachate; " dephosphorization time " and " dephosphorization temperature " all refer to be except phosphorus reaction can not proceed down again before time of whole dephosphorization reaction process and temperature (namely not comprising digestion time).
Proof list:
As can be seen from the result described in proof list, employ composite dephosphorizing agent of the present invention and after adopting corresponding phosphorus removing method, really can obtain the effect that technique is comparatively simple and dephosphorizing rate is higher.

Claims (1)

1. the phosphorus removing method in acid vanadium leachate, is characterized in that, the pH value of described acid vanadium leachate is 2.5 ~ 4.0, and the concentration of phosphorus is 0.6g/L ~ 1.5g/L; Dephosphorization agent used during dephosphorization is the composite dephosphorizing agent be made up of component A and B component, and component A is Al 2(SO 4) 3, MgSO 4, CaSO 4, SrSO 4and ZnSO 4in one, B component is [Fe (OH) n(SO 4) m] q, at [Fe (OH) n(SO 4) m] qin, 0.5≤n≤2,1≤m≤3,10≤q≤100000; The step of this phosphorus removing method is as follows:
(1) add composite dephosphorizing agent at described acid vanadium leaching liquid, temperature controls fully to stir between 80 DEG C at 20 DEG C, to carry out except phosphorus reaction; Wherein, in described component A and B component and acid vanadium leachate, the mol ratio of phosphorus is 0.1 ~ 5: 1;
(2) in step (1) except after phosphorus reaction can not proceed down again, filter after reaction solution ageing, obtain the vanadium leachate after dephosphorization.
CN201510000089.6A 2015-01-02 2015-01-02 Dephosphorizing method for acid vanadium leached solution Pending CN104480308A (en)

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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN105603191A (en) * 2016-03-10 2016-05-25 武汉理工大学 Pretreatment method for deacidification and impurity removal of acid leaching liquid of vanadium extracted from stone coal
CN108220600A (en) * 2018-01-19 2018-06-29 重庆大学 The minimizing technology of phosphorus in a kind of acidity vanadium leachate
CN108751280A (en) * 2018-06-06 2018-11-06 四川科尔瑞环保科技有限责任公司 A kind of solid iron magnesium composite dephosphorizing agent and preparation method thereof
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
CN109852820A (en) * 2019-02-22 2019-06-07 梁刘友 A method of producing vanadic anhydride
CN109868365A (en) * 2019-03-22 2019-06-11 攀钢集团攀枝花钢铁研究院有限公司 The method of the vanadium extraction of depth containing vanadium raw materials
CN110423890A (en) * 2019-08-28 2019-11-08 重庆大学 A method of the deep phosphorous removal in acid vanadium extraction solution

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CN103818965A (en) * 2014-03-20 2014-05-28 重庆大学 Phosphorous removal method for manganous sulfate produced from high-phosphorus rhodochrosite
CN103966437A (en) * 2014-05-14 2014-08-06 攀钢集团攀枝花钢铁研究院有限公司 Method for removing phosphorous from acid solution containing vanadium

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CN103818965A (en) * 2014-03-20 2014-05-28 重庆大学 Phosphorous removal method for manganous sulfate produced from high-phosphorus rhodochrosite
CN103966437A (en) * 2014-05-14 2014-08-06 攀钢集团攀枝花钢铁研究院有限公司 Method for removing phosphorous from acid solution containing vanadium

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105603191A (en) * 2016-03-10 2016-05-25 武汉理工大学 Pretreatment method for deacidification and impurity removal of acid leaching liquid of vanadium extracted from stone coal
CN105603191B (en) * 2016-03-10 2017-07-11 武汉理工大学 A kind of method of extracting vanadium from stone coal pickle liquor deacidification removal of impurities pretreatment
CN108220600A (en) * 2018-01-19 2018-06-29 重庆大学 The minimizing technology of phosphorus in a kind of acidity vanadium leachate
CN108751280A (en) * 2018-06-06 2018-11-06 四川科尔瑞环保科技有限责任公司 A kind of solid iron magnesium composite dephosphorizing agent and preparation method thereof
CN108751280B (en) * 2018-06-06 2021-12-10 四川科尔瑞环保科技有限责任公司 Solid iron-magnesium composite phosphorus removal agent and preparation method thereof
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
CN109852820A (en) * 2019-02-22 2019-06-07 梁刘友 A method of producing vanadic anhydride
CN109868365A (en) * 2019-03-22 2019-06-11 攀钢集团攀枝花钢铁研究院有限公司 The method of the vanadium extraction of depth containing vanadium raw materials
CN109868365B (en) * 2019-03-22 2020-07-28 攀钢集团攀枝花钢铁研究院有限公司 Method for deeply extracting vanadium from vanadium-containing raw material
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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Application publication date: 20150401