CN101264876B - Method for preparing ferric lithium phosphate precursor by comprehensive utilization of ilmenite - Google Patents
Method for preparing ferric lithium phosphate precursor by comprehensive utilization of ilmenite Download PDFInfo
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- CN101264876B CN101264876B CN200810031119XA CN200810031119A CN101264876B CN 101264876 B CN101264876 B CN 101264876B CN 200810031119X A CN200810031119X A CN 200810031119XA CN 200810031119 A CN200810031119 A CN 200810031119A CN 101264876 B CN101264876 B CN 101264876B
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Abstract
The invention discloses a preparation method for lithium iron phosphate precursor by comprehensively utilizing ilmenite, comprising a plurality of steps: leach the ilmenite in acid and filtrate is obtained by filtering; dissolve a certain amount of other iron sources in the filtrate to make the Fe concentration in the mixed solution as 0.01-3mol/L and the molar ratio of Ti and Fe as 0.0005-0.5; add appropriate amount of oxidant to the mixed solution; use alkali aqueous solution to regulate the system pH as 4.0-14.0; react for 10min to 24h at 10-90 DEG Cin a stir reactor; filter, wash and dry the sedimentation at 50-159 DEG C; after drying, calcine the sedimentation in air at 300-800 DEG C for 1-24h; lithium iron phosphate precursor for the lithium-ion battery cathode material, which is also the ferric oxide of doped-metal elements, can be obtained. The preparation method has the advantages of wide material source, simple technological process, good and stable product quality and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion battery anode material lithium iron phosphate presoma, particularly a kind ofly fully utilize the method that ilmenite prepares the lithium ion battery anode material lithium iron phosphate presoma.
Technical background
The iron lithium phosphate of olivine structural becomes one of the most promising anode material for lithium-ion batteries because of it has theoretical specific capacity height (170mAh/g), good cycle, Heat stability is good, cheap, advantages of environment protection.But, as main raw material-molysite of producing iron lithium phosphate but because of unstable product quality, density is low, the not high shortcoming of purity is seriously restricting iron lithium phosphate large-scale commercial production.
The source of iron of preparation iron lithium phosphate mostly is chemical pure or analytically pure molysite greatly at present, mainly contains Ferrox, Iron diacetate, ferrous sulfate, ferric sulfate, iron nitrate, tertiary iron phosphate, ferric oxide etc.These molysite major parts are made by ore, from the natural crystal to the chemical pure or analytically pure molysite, need through a series of removal of impurities operation, and need add some doped elements useful when preparing high-performance iron phosphate lithium to its chemical property with chemical pure or analytical pure molysite, these doped elements just exist in natural mineral mostly, thereby cause flow process to repeat, cost increases greatly.Therefore, the presoma that directly utilizes mineral to prepare lithium ion battery anode material lithium iron phosphate is the effective ways that reduce its production cost.
On the other hand, the China's titanium iron ore deposit is abundant, about 3,000 ten thousand tons of total reserves, at present mainly be to utilize titanium elements wherein to produce titanium white, titanium sponge and artificial rutile etc., and other element such as iron, magnesium, aluminium, manganese, nickel, cobalt etc. are not all well utilized, this has not only wasted resource, and also can cause severe contamination to environment.
Along with lacking day by day of resource and becoming increasingly conspicuous of environmental problem, new technology, the novel process of accelerating various elements in the research and development comprehensive utilization mineral have become the inexorable trend that mineral utilize.The present invention is with a kind of brand-new thinking, be the ferric oxide of the presoma-doping type metallic element of raw material synthesizing lithium ionic cell positive pole material lithium iron phosphate directly with natural ilmenite, because metal-doped element (titanium, aluminium, magnesium, manganese, nickel, cobalt etc.) is evenly distributed in the granular precursor, therefore need not to mix again during synthesizing iron lithium phosphate, these doped elements can improve the electroconductibility of iron lithium phosphate greatly, thereby greatly improve its chemical property.Therefore, the present invention is particularly suitable for providing the fine source of iron for the production of lithium ion battery anode material lithium iron phosphate, if form large-scale production, will bring huge economic benefit and ecological benefits to society.So far for this reason, do not see the report for preparing the lithium ion battery anode material lithium iron phosphate presoma about the comprehensive utilization ilmenite.
Summary of the invention
The method that technical problem to be solved by this invention provides that a kind of raw material sources are wide, technical process is simple, good product quality and the comprehensive utilization ilmenite stable, that cost is low prepare ferric lithium phosphate precursor.
In order to solve the problems of the technologies described above, comprehensive utilization ilmenite provided by the invention prepares the method for ferric lithium phosphate precursor, the steps include:
(1), ilmenite is gone out with acidleach, filter, filtrate, in a certain amount of other source of iron of dissolved in filtrate, make that the concentration of Fe is 0.01-3mol/L in the mixing solutions, the mol ratio of Ti and Fe is 0.0005-0.5;
(2), to add an amount of concentration in mixing solutions be the oxygenant of 0.01-6mol/L, is the pH=1.5-6.0 of aqueous solution regulation system of the alkali of 0.01-6mol/L with concentration, makes part iron and some foreign ion co-precipitation, filters, must filtrate;
(3), adding concentration in filtrate is the precipitation agent of 0.01-6mol/L, with concentration the pH=4.0-14.0 of aqueous solution regulation system of the alkali of 0.01-6mol/L, in 10-90 ℃ stirred reactor, react 10min-24h, filter, washing, will be deposited in 50-150 ℃ down the oven dry back in air 300-800 ℃ down calcining 1-24h promptly get the ferric oxide of the presoma-doping type metallic element of lithium ion battery anode material lithium iron phosphate.
Acid described in the above-mentioned steps (1) is a kind of in sulfuric acid and the hydrochloric acid.
Other source of iron described in the above-mentioned steps (1) is one or more in magnetite, rhombohedral iron ore, maghemite, limonite, spathic iron ore, metallic iron, ferric sulfate, ferrous sulfate, iron(ic) chloride, iron protochloride, iron nitrate, the Iron nitrate.
Alkali described in above-mentioned steps (1) and the step (3) is one or more in lithium hydroxide, sodium hydroxide, potassium hydroxide, the ammoniacal liquor.
Oxygenant described in the above-mentioned steps (2) is a kind of in sodium peroxide, hydrogen peroxide, potassium permanganate, chloric acid steel, clorox, Potcrate, the potassium hypochlorite.
Precipitation agent described in the above-mentioned steps (3) is one or more in Quilonum Retard, lithium bicarbonate, volatile salt, bicarbonate of ammonia, yellow soda ash, sodium bicarbonate, salt of wormwood, the saleratus.
The present invention is in order to overcome the lithium ion battery anode material lithium iron phosphate poorly conductive, raw material (source of iron) cost height, shortcomings such as unstable product quality, the comprehensive utilization ilmenite that provides prepares the method for lithium ion battery anode material lithium iron phosphate presoma, this method is a raw material with cheap natural ilmenite, earlier with its leaching, and a certain amount of other source of iron of adding forms mixing solutions in leach liquor, can make element (titanium useful in the mixing solutions by the control synthesis condition to electrochemical performances of lithium iron phosphate, aluminium, magnesium, manganese, nickel, cobalt etc.) optionally enter precipitation, in air, calcine the ferric oxide of the presoma-doping type metallic element that promptly gets iron lithium phosphate after the drying precipitate.Raw material sources of the present invention are wide, technical process is simple, good product quality and stable, cost is low, is particularly suitable for providing the fine source of iron for the scale operation of iron lithium phosphate, also makes the ilmenite resource obtain comprehensive utilization simultaneously.
The present invention compares with the method that other prepares ferric lithium phosphate precursor, and its advantage fully shows in the following areas:
1) be raw material with natural ilmenite, cost is far below general chemical pure, analytical pure raw material.
2) can make in the ilmenite the useful element of electrochemical performances of lithium iron phosphate is optionally entered precipitation by the control synthesis condition, and the deleterious element of electrochemical performances of lithium iron phosphate is not entered precipitation, technical process is simple.
3) product (ferric lithium phosphate precursor) is the ferric oxide of doping type metallic element, and metal-doped element is evenly distributed in the granular precursor, has solved the problem that doped element is difficult to mix, and has improved the electric conductivity of material greatly.
4) the short and control easily of generated time is the size of may command product (ferric lithium phosphate precursor) particle diameter by generated time.
In sum, the method that the present invention is that a kind of raw material sources are wide, technical process is simple, good product quality and the comprehensive utilization ilmenite stable, that cost is low prepare ferric lithium phosphate precursor.
Description of drawings
Fig. 1 is the presoma sem photograph of embodiment 1;
Fig. 2 is the presoma sem photograph of embodiment 2.
Embodiment
The invention will be further described below in conjunction with the drawings and specific embodiments.
Embodiment 1:
The 1kg ilmenite is leached with sulfuric acid, filters, filtrate, at a certain amount of rhombohedral iron ore of dissolved in filtrate and ferric sulfate, make that the concentration of Fe is 0.1mol/L in the mixing solutions, the mol ratio of Ti and Fe is 0.5; The sodium peroxide solution that in mixing solutions, adds an amount of 0.01mol/L, the pH with system transfers to about 1.5 with the sodium hydroxide solution of 0.5mol/L, and stirred for several minute after-filtration must filtrate; The sal volatile that in filtrate, adds an amount of 1mol/L, pH with system transfers to about 6.0 with the ammoniacal liquor of 2mol/L, in 50 ℃ stirred reactor, react 10min, filter, washing, will be deposited in 100 ℃ down the oven dry back in air 600 ℃ down calcining 2h promptly get the ferric oxide of the presoma-doping type metallic element of lithium ion battery anode material lithium iron phosphate.
Embodiment 2:
The 1kg ilmenite is leached with hydrochloric acid, filters, filtrate, at a certain amount of iron(ic) chloride of dissolved in filtrate, make that the concentration of Fe is 1mol/L in the mixing solutions, the mol ratio of Ti and Fe is 0.3; The chlorine bleach liquor who in mixing solutions, adds an amount of 3mol/L, the pH with system transfers to about 3.0 with the lithium hydroxide solution of 2mol/L, and stirred for several minute after-filtration must filtrate; The sodium carbonate solution that in filtrate, adds an amount of 2mol/L, pH with system transfers to about 4.0 with the sodium hydroxide solution of 0.1mol/L, in 10 ℃ stirred reactor, react 4h, filter, washing, will be deposited in 50 ℃ down the oven dry back in air 800 ℃ down calcining 1h promptly get the ferric oxide of the presoma-doping type metallic element of lithium ion battery anode material lithium iron phosphate.
Embodiment 3:
The 1kg ilmenite is leached with sulfuric acid, filters, filtrate, at a certain amount of ferrous sulfate of dissolved in filtrate and iron protochloride, make that the concentration of Fe is 2mol/L in the mixing solutions, the mol ratio of Ti and Fe is 0.1; The potassium chlorate solution who in mixing solutions, adds an amount of 1mol/L, the pH with system transfers to about 6.0 with the ammoniacal liquor of 3mol/L, and stirred for several minute after-filtration must filtrate; The potassium bicarbonate solution that in filtrate, adds an amount of 3mol/L, pH with system transfers to about 14.0 with the 6mol/L potassium hydroxide solution, in 70 ℃ stirred reactor, react 2h, filter, washing, will be deposited in 150 ℃ down the oven dry back in air 300 ℃ down calcining 24h promptly get the ferric oxide of the presoma-doping type metallic element of lithium ion battery anode material lithium iron phosphate.
Embodiment 4:
The 1kg ilmenite is leached with hydrochloric acid, filters, filtrate, at a certain amount of spathic iron ore of dissolved in filtrate and iron(ic) chloride, make that the concentration of Fe is 0.01mol/L in the mixing solutions, the mol ratio of Ti and Fe is 0.05; The hydrogen peroxide that in mixing solutions, adds an amount of 1mol/L, the pH with system transfers to about 4.0 with the sodium hydroxide solution of 3mol/L, and stirred for several minute after-filtration must filtrate; The ammonium bicarbonate soln that in filtrate, adds an amount of 0.01mol/L, pH with system transfers to about 8.0 with the ammoniacal liquor of 3mol/L, in 90 ℃ stirred reactor, react 1h, filter, washing, will be deposited in 120 ℃ down the oven dry back in air 500 ℃ down calcining 5h promptly get the ferric oxide of the presoma-doping type metallic element of lithium ion battery anode material lithium iron phosphate.
Embodiment 5:
The 1kg ilmenite is leached with hydrochloric acid, filters, filtrate, at a certain amount of limonite of dissolved in filtrate and metal iron powder, make that the concentration of Fe is 3mol/L in the mixing solutions, the mol ratio of Ti and Fe is 0.0005; The potassium permanganate solution that in mixing solutions, adds an amount of 6mol/L, the pH with system transfers to about 5.0 with the sodium hydroxide solution of 6mol/L, and stirred for several minute after-filtration must filtrate; The sodium hydrogen carbonate solution that in filtrate, adds an amount of 6mol/L, pH with system transfers to about 6.0 with the sodium hydroxide solution of 0.01mol/L, in 30 ℃ stirred reactor, react 24h, filter, washing, will be deposited in 80 ℃ down the oven dry back in air 500 ℃ down calcining 10h promptly get the ferric oxide of the presoma-doping type metallic element of lithium ion battery anode material lithium iron phosphate.
Although the present invention is described in each preferred embodiment, but the easy cleavage the present invention of those skilled in the art is not limited to foregoing description, it can be changed by multiple alternate manner or improve, and does not break away from the spirit and scope of illustrating in the claim of the present invention.Can also be in magnetite, maghemite, iron nitrate, the Iron nitrate one or more as other source of iron.Oxygenant can also be sodium chlorate or potassium hypochlorite.Precipitation agent can also be in Quilonum Retard, lithium bicarbonate, the salt of wormwood one or more.
Claims (6)
1. one kind fully utilizes the method that ilmenite prepares ferric lithium phosphate precursor, it is characterized in that: the steps include:
(1), ilmenite is gone out with acidleach, filter, filtrate, in a certain amount of other source of iron of dissolved in filtrate, make that the concentration of Fe is 0.01-3mol/L in the mixing solutions, the mol ratio of Ti and Fe is 0.0005-0.5;
(2), to add an amount of concentration in mixing solutions be the oxygenant of 0.01-6mol/L, is the pH=1.5-6.0 of aqueous solution regulation system of the alkali of 0.01-6mol/L with concentration, makes part iron and some foreign ion co-precipitation, filters, must filtrate;
(3), adding concentration in filtrate is the precipitation agent of 0.01-6mol/L, with concentration the pH=4.0-14.0 of aqueous solution regulation system of the alkali of 0.01-6mol/L, in 10-90 ℃ stirred reactor, react 10min-24h, filter, washing, will be deposited in 50-150 ℃ down the oven dry back in air 300-800 ℃ down calcining 1-24h promptly get the presoma of lithium ion battery anode material lithium iron phosphate.
2. comprehensive utilization ilmenite according to claim 1 prepares the method for ferric lithium phosphate precursor, it is characterized in that: the acid described in the above-mentioned steps (1) is a kind of in sulfuric acid and the hydrochloric acid.
3. comprehensive utilization ilmenite according to claim 1 prepares the method for ferric lithium phosphate precursor, it is characterized in that: other source of iron described in the above-mentioned steps (1) is one or more in magnetite, rhombohedral iron ore, maghemite, limonite, spathic iron ore, metallic iron, ferric sulfate, ferrous sulfate, iron(ic) chloride, iron protochloride, iron nitrate, the Iron nitrate.
4. comprehensive utilization ilmenite according to claim 1 prepares the method for ferric lithium phosphate precursor, it is characterized in that: alkali described in above-mentioned steps (1) and the step (3) is one or more in lithium hydroxide, sodium hydroxide, potassium hydroxide, the ammoniacal liquor.
5. comprehensive utilization ilmenite according to claim 1 prepares the method for ferric lithium phosphate precursor, it is characterized in that: oxygenant described in the above-mentioned steps (2) is a kind of in sodium peroxide, hydrogen peroxide, potassium permanganate, sodium chlorate, clorox, Potcrate, the potassium hypochlorite.
6. comprehensive utilization ilmenite according to claim 1 prepares the method for ferric lithium phosphate precursor, it is characterized in that: precipitation agent described in the above-mentioned steps (3) is one or more in Quilonum Retard, lithium bicarbonate, volatile salt, bicarbonate of ammonia, yellow soda ash, sodium bicarbonate, salt of wormwood, the saleratus.
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102856545B (en) * | 2012-09-11 | 2014-07-23 | 清华大学 | Preparation method of micro-nano-grade metal-ion-doped lithium iron phosphate anode material |
| CN103022491A (en) * | 2012-12-31 | 2013-04-03 | 广西地博矿业集团股份有限公司 | Method for preparing lithium iron phosphate precursor for positive pole material of lithium-ion battery |
| CN103268938A (en) * | 2013-01-22 | 2013-08-28 | 合肥国轩高科动力能源股份公司 | Method for preparing lithium manganese iron phosphate solid solution lithium-ion cathode material |
| CN104805299B (en) * | 2015-04-14 | 2017-02-22 | 东北大学 | Method for preparing lithium battery electrode materials LiFePO4 and Li4Ti5O12 from vanadium extraction slag |
| CN105140504B (en) * | 2015-08-11 | 2018-02-02 | 东北大学 | A kind of method that electrode material of lithium battery is prepared using vanadium extraction waste |
| CN107572596B (en) * | 2017-09-14 | 2020-02-18 | 武汉科技大学 | Method for preparing high-purity iron oxide red from high-phosphorus oolitic hematite |
| CN107863531B (en) * | 2017-11-03 | 2020-04-28 | 山东科技大学 | Method for preparing lithium ion battery anode material by using siderite |
| CN109573974A (en) * | 2018-10-22 | 2019-04-05 | 天齐锂业（江苏）有限公司 | Aluminum removing method based on acid leaching solution in waste lithium iron phosphate battery recycling |
| CN110550615B (en) * | 2019-10-14 | 2020-12-15 | 王敏 | Preparation method of high-energy-density lithium iron phosphate |
| CN113753872A (en) * | 2021-09-15 | 2021-12-07 | 广东邦普循环科技有限公司 | Comprehensive utilization method of iron-containing minerals |
| CN115367725B (en) * | 2022-08-29 | 2024-05-10 | 广东邦普循环科技有限公司 | Doped lithium iron phosphate and preparation method and application thereof |
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