CN106299361A - A kind of preparation method of vanadyl phosphate - Google Patents
A kind of preparation method of vanadyl phosphate Download PDFInfo
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- CN106299361A CN106299361A CN201610992605.2A CN201610992605A CN106299361A CN 106299361 A CN106299361 A CN 106299361A CN 201610992605 A CN201610992605 A CN 201610992605A CN 106299361 A CN106299361 A CN 106299361A
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- phosphate
- electrolyte
- vanadium ion
- vanadyl phosphate
- preparation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides the preparation method of a kind of vanadyl phosphate, the method is by being electrolysed the vanadium ion in inefficacy V electrolyte as pentavalent vanadium ion；Pentavalent vanadium ion electrolyte after electrolysis adds the phosphate of excess, stirring, produces yellow-green precipitate；Filter and precipitate with organic solvent washing, being dried in atmosphere, obtain vanadyl phosphate solid.The present invention uses inefficacy V electrolyte to prepare vanadyl phosphate, it is achieved that to the recovery of vanadium ion in electrolyte of vanadium redox battery and utilization, has reached the comprehensive utilization of refuse, has avoided the problems such as vanadic anhydride dissolubility in phosphoric acid is relatively low, the response time is longer simultaneously.This method is simple to operate, and the response time is shorter, and economic benefit increases, and is easily achieved industrialized production.
Description
Technical field
The invention belongs to chemical field, specifically, relate to the preparation method of a kind of vanadyl phosphate.
Background technology
Generally, vanadium cell has output because of it and capacity is separate, power and capacity big, service life cycle
Long, energy efficiency high, degree of depth charge-discharge performance is good, security performance advantages of higher is it is considered to be most one of application prospect big
Scale energy-storage battery, is increasingly paid close attention to by people.But, along with the continuous charge and discharge cycle of vanadium cell, it may appear that positive and negative
The problem that in the electrolyte of pole, the concentration of vanadium ion and valence state do not match that, causes vanadium cell normally to use.When electrolyte
Utilization rate does not reaches design when requiring, it is necessary to the V electrolyte more renewed, and therefore, creates the electrolyte of inefficacy.Along with vanadium
The extensive utilization of battery, creates the V electrolyte of a large amount of inefficacy, accordingly, it would be desirable to carry out the V electrolyte lost efficacy at recovery
Reason.
Same, vanadio phosphate has the construction features of complexity because of it, therefore, by as a kind of compound catalyst material
Material, is widely used in paraffin selectivity oxidation reaction, and at butane, butylene and the butadiene with four carbon atom, (summary is especially
" C4 hydrocarbon ") it is that raw material is prepared in the technique of maleic anhydride and had important application.And vanadyl phosphate (VOPO4) it is to prepare vanadio phosphoric acid
The persursor material of salt catalyst.At present, vanadyl phosphate (VOPO4) side that is heated to reflux of commonly used phosphoric acid and vanadic anhydride
Prepared by method.But the method is less due to vanadic anhydride dissolubility in phosphoric acid solution, and the response time is longer, is unfavorable for work
Industry metaplasia is produced.
Summary of the invention
It is an object of the invention to solve at least one in deficiencies of the prior art.
Such as, an object of the present invention is to solve the recovery problem of inefficacy V electrolyte and vanadic anhydride at phosphoric acid
The problem that dissolubility in solution is little.
To achieve these goals, one aspect of the present invention provides the preparation method of a kind of vanadyl phosphate.Described method bag
Include following steps: be electrolysed the vanadium ion in inefficacy V electrolyte for pentavalent vanadium ion；Pentavalent vanadium ion electrolysis after electrolysis
Liquid adds the phosphate of excess, obtains vanadyl phosphate solid.
In one exemplary embodiment of the present invention, the inefficacy V electrolyte that the described present invention uses is vanadium cell anode
Electrolyte (V5+/V4+) waste liquid and/or vanadium cell catholyte (V3+/V2+) waste liquid.
In one exemplary embodiment of the present invention, described phosphate be a kind of in potassium phosphate, sodium phosphate, ammonium phosphate or
Two or more combinations.
In one exemplary embodiment of the present invention, the detergent of described washing yellow-green precipitate is organic solvent.
In one exemplary embodiment of the present invention, described organic solvent is one or both in ethanol, acetone
Combination.
Compared with prior art, the Advantageous Effects of the application includes: the present invention utilizes inefficacy V electrolyte to prepare
Vanadyl phosphate, it is achieved that to the recovery of vanadium ion in electrolyte of vanadium redox battery and utilization, reached the comprehensive utilization of refuse.This method
Simple to operate, the response time is shorter, increases economic benefit, and is easily achieved industrialized production.
Detailed description of the invention
Hereinafter, exemplary embodiment will be combined describe in detail the preparation method of the vanadyl phosphate according to the present invention.
Generally speaking, the present invention mainly utilizes the electrolyte of vanadium redox battery of inefficacy to carry out preparing phosphoric acid vanadyl (VOPO4)。
In one exemplary embodiment of the present invention, the preparation method of vanadyl phosphate comprises the following steps:
First, the vanadium ion electrolysis in the V electrolyte that will lose efficacy is pentavalent vanadium ion.
Secondly, the pentavalent vanadium ion electrolyte after electrolysis adds the phosphate of excess, stirring, produce yellow green and sink
Form sediment.Here, phosphate can be one or more combination in potassium phosphate, sodium phosphate, ammonium phosphate.
Finally, filter and with the above-mentioned yellow-green precipitate of organic solvent washing, be dried in atmosphere, i.e. can get vanadyl phosphate
Solid.Here, organic solvent can be one or both the combination in ethanol, acetone.
The exemplary embodiment of the present invention is described in further detail below in conjunction with concrete example.
Embodiment 1:
First, being V (V) electrolyte by the electrolyte of vanadium redox battery electrolysis lost efficacy, sampling liquid carries out UV-Visible absorption light
Spectrum test, without the absworption peak of tetravalent vanadium ion in spectrogram.Then, it is 1.6mol/ by chemical titration vanadium ion concentration
L.Take above-mentioned solution 500mL, add the sodium phosphate of excess.Constantly it is stirred, solution produces rapidly yellow-green precipitate.?
After, filter and use washing with acetone yellow-green precipitate, then the solid after washing is placed in drying baker, obtain vanadyl phosphate
(VOPO4) solid.
Embodiment 2:
First, being V (V) electrolyte by the electrolyte of vanadium redox battery electrolysis lost efficacy, sampling liquid carries out UV-Visible absorption light
Spectrum test, without the absworption peak of tetravalent vanadium ion in spectrogram.Then, it is 1.5mol/ by chemical titration vanadium ion concentration
L.Take above-mentioned solution 500mL, add the ammonium phosphate of excess.Constantly it is stirred, solution produces rapidly yellow-green precipitate.?
After, filter and use washing with alcohol yellow-green precipitate, then the solid after washing is placed in drying baker, obtain vanadyl phosphate
(VOPO4) solid.
The present invention uses inefficacy vanadium electrode solution to prepare vanadyl phosphate, it is achieved that return vanadium ion in electrolyte of vanadium redox battery
Receive and utilize, having reached the comprehensive utilization of refuse, avoiding that vanadic anhydride dissolubility in phosphoric acid is relatively low, the response time simultaneously
The problem such as longer.This method is simple to operate, and the response time is shorter, and economic benefit increases, and is easily achieved industrialized production.
Although describing the present invention already in connection with exemplary embodiment above, but those of ordinary skill in the art should be clear
Chu, in the case of without departing from spirit and scope by the claims, can carry out various amendment to above-described embodiment.
Claims (5)
1. the preparation method of a vanadyl phosphate, it is characterised in that said method comprising the steps of:
Vanadium ion in inefficacy V electrolyte is electrolysed as pentavalent vanadium ion；
Pentavalent vanadium ion electrolyte after electrolysis adds the phosphate of excess, obtains vanadyl phosphate solid.
The preparation method of vanadyl phosphate the most according to claim 1, it is characterised in that described inefficacy V electrolyte is vanadium
Galvanic anode electrolyte waste liquid and/or catholyte waste liquid.
The preparation method of vanadyl phosphate the most according to claim 1, it is characterised in that described phosphate is potassium phosphate, phosphorus
One or more combination in acid sodium, ammonium phosphate.
The preparation method of vanadyl phosphate the most according to claim 1, it is characterised in that described method also includes with organic molten
Agent washing vanadyl phosphate solid.
The preparation method of vanadyl phosphate the most according to claim 4, it is characterised in that described organic solvent be ethanol, third
One or both combination in ketone.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610992605.2A CN106299361A (en) | 2016-11-11 | 2016-11-11 | A kind of preparation method of vanadyl phosphate |
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| CN201610992605.2A CN106299361A (en) | 2016-11-11 | 2016-11-11 | A kind of preparation method of vanadyl phosphate |
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| CN201610992605.2A Pending CN106299361A (en) | 2016-11-11 | 2016-11-11 | A kind of preparation method of vanadyl phosphate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108408707A (en) * | 2018-02-09 | 2018-08-17 | 清华大学 | A kind of lithium ion anode material nanometer ω-VOPO4Preparation method |
| CN111646452A (en) * | 2020-06-17 | 2020-09-11 | 广东工业大学 | Nano flaky hydrated sodium vanadyl phosphate cathode material and preparation method and application thereof |
| CN116081687A (en) * | 2022-12-14 | 2023-05-09 | 成都先进金属材料产业技术研究院股份有限公司 | Bismuth vanadate powder based on ultrasonic and/or microwave dispersion and preparation method thereof |
| CN116081687B (en) * | 2022-12-14 | 2024-05-10 | 成都先进金属材料产业技术研究院股份有限公司 | Bismuth vanadate powder based on ultrasonic and/or microwave dispersion and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05115783A (en) * | 1991-10-24 | 1993-05-14 | Mitsui Toatsu Chem Inc | Catalyst for producing maleic anhydride and preparation of the same |
| CN102600875A (en) * | 2012-01-13 | 2012-07-25 | 中南民族大学 | Nanometer vanadyl phosphate as well as preparation method and application thereof |
| CN102983346A (en) * | 2012-12-04 | 2013-03-20 | 中国科学院金属研究所 | Method for preparing vanadyl sulfate from electrolyte for failure vanadium cell |
| CN103972506A (en) * | 2014-05-16 | 2014-08-06 | 中南大学 | Preparation method of nano sheet negative electrode material, phosphoric acid oxygen vanadium, of lithium ion battery |
| CN105457665A (en) * | 2014-09-09 | 2016-04-06 | 中国石油化工股份有限公司 | Preparation method for vanadium-phosphorus catalyst with high specific surface area |
-
2016
- 2016-11-11 CN CN201610992605.2A patent/CN106299361A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05115783A (en) * | 1991-10-24 | 1993-05-14 | Mitsui Toatsu Chem Inc | Catalyst for producing maleic anhydride and preparation of the same |
| CN102600875A (en) * | 2012-01-13 | 2012-07-25 | 中南民族大学 | Nanometer vanadyl phosphate as well as preparation method and application thereof |
| CN102983346A (en) * | 2012-12-04 | 2013-03-20 | 中国科学院金属研究所 | Method for preparing vanadyl sulfate from electrolyte for failure vanadium cell |
| CN103972506A (en) * | 2014-05-16 | 2014-08-06 | 中南大学 | Preparation method of nano sheet negative electrode material, phosphoric acid oxygen vanadium, of lithium ion battery |
| CN105457665A (en) * | 2014-09-09 | 2016-04-06 | 中国石油化工股份有限公司 | Preparation method for vanadium-phosphorus catalyst with high specific surface area |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108408707A (en) * | 2018-02-09 | 2018-08-17 | 清华大学 | A kind of lithium ion anode material nanometer ω-VOPO4Preparation method |
| CN111646452A (en) * | 2020-06-17 | 2020-09-11 | 广东工业大学 | Nano flaky hydrated sodium vanadyl phosphate cathode material and preparation method and application thereof |
| CN116081687A (en) * | 2022-12-14 | 2023-05-09 | 成都先进金属材料产业技术研究院股份有限公司 | Bismuth vanadate powder based on ultrasonic and/or microwave dispersion and preparation method thereof |
| CN116081687B (en) * | 2022-12-14 | 2024-05-10 | 成都先进金属材料产业技术研究院股份有限公司 | Bismuth vanadate powder based on ultrasonic and/or microwave dispersion and preparation method thereof |
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Application publication date: 20170104 |