CN106064810A - A kind of method preparing iron phosphate - Google Patents
A kind of method preparing iron phosphate Download PDFInfo
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- CN106064810A CN106064810A CN201610373365.8A CN201610373365A CN106064810A CN 106064810 A CN106064810 A CN 106064810A CN 201610373365 A CN201610373365 A CN 201610373365A CN 106064810 A CN106064810 A CN 106064810A
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- iron
- iron phosphate
- phosphate
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- phosphoric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- 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
- C01P2006/11—Powder tap density
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of method preparing iron phosphate, first use the oxide of iron powder or ferrum as source of iron, ferrous phosphate mother solution is prepared as phosphorus source using phosphoric acid, it is subsequently adding hydrogen peroxide and prepares iron phosphate crude product, finally use distilled water wash iron phosphate crude product, product drying iron phosphate product after washing, phosphoric acid filter liquor is recyclable to be reused.The method preparing iron phosphate of the present invention, directly uses the oxide of iron powder or ferrum as raw material, produces iron phosphate than phosphate with iron salt, and its trace meter content is more easy to control, and tap density index is more stable；Use phosphoric acid to can be recycled as phosphorus source, phosphoric acid, be recycled to prepare the ferrous phosphate stage as phosphorus source using the filtrate of iron phosphate, effectively reduce the content of phosphor in sewage, improve the utilization rate of phosphorus source simultaneously.
Description
Technical field
The present invention relates to a kind of method preparing energy and material, particularly relate to a kind of method preparing iron phosphate.
Background technology
Lithium ion battery is the green high-capacity battery of a new generation, have that voltage is high, energy density big, good cycle, from
Discharge the many merits such as little, memory-less effect, operating temperature range width, is widely used in mobile phone, notebook computer, number
Camera, video camera, electronic instrument etc., also have in fields such as UPS, electric tool, electric bicycle, electric automobile, energy-storage batteries
There is the application prospect of light.In recent years, the yield of lithium ion battery is skyrocketed through, and application constantly expands, it has also become two
The new high-tech product that eleventh century is significant to national economy and people's lives.
At present, lithium ion battery reaches its maturity in the compact battery field of portable type electronic product, and range of application is just
Progressively to middle Large Copacity, in high-power power type and accumulation energy type field of batteries expand.Positive electrode is the weight of lithium ion battery
Wanting ingredient, its performance determines the combination property of battery to a great extent.Positive electrode research and performance improvement are lithiums
One of core of ion battery development.
Iron phosphate is also known as high ferric phosphate, and English name is iron (iii) phosphate tetrahydrate, and No. CAS is
10045-86-0.Iron phosphate is commonly used for making the raw material of the LiFePO4 of lithium battery, along with the utilization of new forms of energy, to iron phosphate
Demand is increasing, and the production technology of current iron phosphate mostly is phosphate and produces iron phosphate with iron salt, and rarer phosphoric acid is straight with ferrum
Deliver a child produce iron phosphate technique；The production time of phosphate and iron salt production iron phosphate is above phosphoric acid with energy consumption and directly gives birth to ferrum
Producing iron phosphate, and generate other by-product salt, subsequent treatment is the most difficult.Additionally, due to the impurity content of iron salt is high, right
The production of iron phosphate purifies large effect, uses in the production process of iron salt, higher to the technological requirement purified；And iron powder
And oxide purity is the highest, during producing iron phosphate, greatly reduce the impurity content of product.As used sulfur
Acid ferrous iron be raw material, and needs consider the content of the metal ions such as wherein titanium, in addition it is also necessary to the problem of consideration process sulfate radical.
In summary, sad filter after making ferrous phosphate in iron phosphate production technology of the prior art, the product of preparation
Purity is relatively low, by-product is many, it is necessary to provide the new preparation method of a kind of iron phosphate to solve the problems referred to above.
Summary of the invention
It is an object of the invention to for the deficiencies in the prior art, it is provided that a kind of impurity content is low, technique simply prepares phosphorus
The method of acid ferrum.
The present invention is achieved by the following technical solutions:
A kind of method preparing iron phosphate, comprises the steps:
S1, successively adding source of iron and the phosphorus source that mol ratio is 1:2-3 in reaction vessel, described source of iron is iron powder or ferrum
Oxide, is subsequently adding appropriate water and makes the mass percentage content of ferrum in system be 2%-5%, be stirred continuously lower intensification,
At 70-98 DEG C, react 0.5-2h, be filtrated to get ferrous phosphate mother solution；
S2, in the product of step S1 add hydrogenperoxide steam generator, continuously add ethanol solution, be stirred continuously lower intensification,
At 50-98 DEG C, react 1-4h, be filtrated to get iron phosphate crude product；
S3, the product phosphoric acid ferrum crude product 15-30min of employing distilled water agitator treating step S2, repeated washing 2-4 time, mistake
Filter obtains filtrate and iron phosphate crude product A, and described filtrate is recycled in step S1 be continuing with as phosphorus source；
S4, the product phosphoric acid ferrum crude product A of step S3 is positioned over dried 4.5-6h in the baking oven of 65-75 DEG C, to obtain final product
Iron phosphate product.
Preferably, phosphorus source is phosphoric acid solution.
Preferably, described ferrous phosphate is 1:0.5-1.5 with the mol ratio of hydrogen peroxide.
Preferably, described hydrogenperoxide steam generator is 1:0-1 with the mass ratio of ethanol.
Preferably, in described step S3, the mass ratio of iron phosphate crude product A and distilled water is 1:2-4.
Preferably, in described step S3, the temperature of distilled water is 50-80 DEG C.
Preferably, the oxide of described ferrum is ferroso-ferric oxide.
The invention has the beneficial effects as follows:
(1) directly use the oxide of iron powder or ferrum to prepare ferrous phosphate as raw material, efficiently solve phosphate and ferrum
Salt carries out displacement reaction and makes the problem such as sad filter after ferrous phosphate, improves response speed and production efficiency, reduces energy consumption,
Decrease water distribution quantity simultaneously；
(2) directly use the oxide of iron powder or ferrum as raw material, produce iron phosphate than phosphate with iron salt, it is to avoid
The generation of a large amount of by-product salt, improves product yield simultaneously；
(3) directly use the oxide of iron powder or ferrum as raw material, produce iron phosphate, its trace than phosphate with iron salt
Tenor is more easy to control, and tap density index is more stable；
(4) use phosphoric acid to can be recycled as phosphorus source, phosphoric acid, be recycled to prepare phosphorus as phosphorus source using the filtrate of iron phosphate
In the acid ferrous stage, effectively reduce the content of phosphor in sewage, improve the utilization rate of phosphorus source simultaneously.
Detailed description of the invention
Technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described enforcement
Example is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained on the premise of not making creative work, broadly falls into present invention protection
Scope.
Embodiment 1:
A kind of method preparing iron phosphate, comprises the steps:
S1, weigh 27g iron powder in reactor, add 1230mL distilled water after adding 94g phosphoric acid, be stirred continuously lower intensification
To 70 DEG C, react 2h, be filtrated to get ferrous phosphate mother solution；
S2, in the product phosphoric acid ferrous iron mother solution of step S1 add 9.0g mass fraction be the hydrogenperoxide steam generator of 30%,
Continuously add 9.0g ethanol solution, be stirred continuously down and be warming up to 50 DEG C, react 4h, be filtrated to get iron phosphate crude product；
S3, use the product phosphoric acid ferrum crude product 15min of distilled water 180g agitator treating step S2 of 50 DEG C, repeated washing 2
Secondary, it is filtrated to get filtrate and iron phosphate crude product A, described filtrate is recycled in step S1 be continuing with as phosphorus source；
S4, the product phosphoric acid ferrum crude product A of step S3 is positioned over dried 6h in the baking oven of 65 DEG C, obtains iron phosphate and produce
Product.
Calculating product yield with source of iron and reach 99.1%, granularity reaches 3um and meets HG/T4701-2014 " battery phosphoric acid
Ferrum " Industry code requirements, tap density reaches 0.75g/cm3, meets HG/T4701-2014 " battery iron phosphate " industry standard
Requirement.
Embodiment 2:
A kind of method preparing iron phosphate, comprises the steps:
S1, weigh 116g ferroso-ferric oxide in reactor, add 283mL distilled water after adding 141g phosphoric acid, constantly stir
Mix down and be warming up to 98 DEG C, react 0.5h, be filtrated to get ferrous phosphate mother solution；
S2, in the product phosphoric acid ferrous iron mother solution of step S1 add 27g mass fraction be the hydrogenperoxide steam generator of 30%, continue
Continuous addition 20g ethanol solution, is stirred continuously down and is warming up to 98 DEG C, react 1h, be filtrated to get iron phosphate crude product；
S3, use the product phosphoric acid ferrum crude product 30min of distilled water 360g agitator treating step S2 of 80 DEG C, repeated washing 4
Secondary, it is filtrated to get filtrate and iron phosphate crude product A, described filtrate is recycled in step S1 be continuing with as phosphorus source；
S4, the product phosphoric acid ferrum crude product A of step S3 is positioned over dried 4.5h in the baking oven of 75 DEG C, obtains iron phosphate
Product.
Calculating product yield with source of iron and reach 99.3%, granularity reaches 4um and meets HG/T4701-2014 " battery phosphoric acid
Ferrum " Industry code requirements, tap density reaches 0.85g/cm3, meets HG/T4701-2014 " battery iron phosphate " industry standard
Requirement.
Embodiment 3:
A kind of method preparing iron phosphate, comprises the steps:
S1, weigh 27g iron powder in reactor, add 600mL distilled water after adding 138g phosphoric acid, be stirred continuously lower intensification
To 80 DEG C, react 2h, be filtrated to get ferrous phosphate mother solution；
S2, in the product phosphoric acid ferrous iron mother solution of step S1 add 65g mass fraction be the hydrogenperoxide steam generator of 30%, no
It is warming up to 60 DEG C under disconnected stirring, reacts 4h, be filtrated to get iron phosphate crude product；
S3, use the product phosphoric acid ferrum crude product 20min of distilled water 400g agitator treating step S2 of 70 DEG C, repeated washing 3
Secondary, it is filtrated to get filtrate and iron phosphate crude product A, described filtrate is recycled in step S1 be continuing with as phosphorus source；
S4, the product phosphoric acid ferrum crude product A of step S3 is positioned over dried 5h in the baking oven of 70 DEG C, obtains iron phosphate and produce
Product.
Calculating product yield with source of iron and reach 99.0%, granularity reaches 3.6um and meets HG/T4701-2014 " battery phosphorus
Acid ferrum " Industry code requirements, tap density reaches 0.82g/cm3, meets HG/T4701-2014 " battery iron phosphate " industry mark
Alignment request.
The invention has the beneficial effects as follows:
(1) directly use the oxide of iron powder or ferrum to prepare ferrous phosphate as raw material, efficiently solve phosphate and ferrum
Salt carries out displacement reaction and makes the problem such as sad filter after ferrous phosphate, improves response speed and production efficiency, reduces energy consumption,
Decrease water distribution quantity simultaneously；
(2) directly use the oxide of iron powder or ferrum as raw material, produce iron phosphate than phosphate with iron salt, it is to avoid
The generation of a large amount of by-product salt, improves product yield simultaneously；
(3) directly use the oxide of iron powder or ferrum as raw material, produce iron phosphate, its trace than phosphate with iron salt
Tenor is more easy to control, and tap density index is more stable；
(4) use phosphoric acid to can be recycled as phosphorus source, phosphoric acid, be recycled to prepare phosphorus as phosphorus source using the filtrate of iron phosphate
In the acid ferrous stage, effectively reduce the content of phosphor in sewage, improve the utilization rate of phosphorus source simultaneously.
The above is the preferred embodiment of the present invention, it should be noted that for those skilled in the art
For, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications are also considered as
Protection scope of the present invention.
Claims (7)
1. the method preparing iron phosphate, it is characterised in that comprise the steps:
S1, successively adding source of iron and the phosphorus source that mol ratio is 1:2-3 in reaction vessel, described source of iron is the oxidation of iron powder or ferrum
Thing, is subsequently adding appropriate water and makes the mass percentage content of ferrum in system be 2%-5%, be stirred continuously lower intensification, at 70-
React 0.5-2h at 98 DEG C, be filtrated to get ferrous phosphate mother solution；
S2, in the product of step S1 add hydrogenperoxide steam generator, continuously add ethanol solution, be stirred continuously lower intensification, at 50-
React 1-4h at 98 DEG C, be filtrated to get iron phosphate crude product；
S3, the product phosphoric acid ferrum crude product 15-30min of employing distilled water agitator treating step S2, repeated washing 2-4 time, filters
To filtrate and iron phosphate crude product A, described filtrate is recycled in step S1 be continuing with as phosphorus source；
S4, the product phosphoric acid ferrum crude product A of step S3 is positioned over dried 4.5-6h in the baking oven of 65-75 DEG C, obtains phosphoric acid
Iron product.
A kind of method preparing iron phosphate the most according to claim 1, it is characterised in that phosphorus source is phosphoric acid solution.
A kind of method preparing iron phosphate the most according to claim 1 and 2, it is characterised in that described ferrous phosphate and mistake
The mol ratio of hydrogen oxide is 1:0.5-1.5.
A kind of method preparing iron phosphate the most according to claim 3, it is characterised in that described hydrogenperoxide steam generator and second
The mass ratio of alcohol is 1:0-1.
A kind of method preparing iron phosphate the most according to claim 4, it is characterised in that in described step S3, iron phosphate is thick
Product A is 1:2-4 with the mass ratio of distilled water.
A kind of method preparing iron phosphate, it is characterised in that distill in described step S3
The temperature of water is 50-80 DEG C.
A kind of method preparing iron phosphate the most according to claim 6, it is characterised in that the oxide of described ferrum is four oxygen
Change three-iron.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610373365.8A CN106064810A (en) | 2016-05-31 | 2016-05-31 | A kind of method preparing iron phosphate |
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| CN201610373365.8A CN106064810A (en) | 2016-05-31 | 2016-05-31 | A kind of method preparing iron phosphate |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107032316A (en) * | 2017-06-12 | 2017-08-11 | 百川化工(如皋)有限公司 | A kind of preparation method of ferric phosphate |
| CN108529582A (en) * | 2018-03-28 | 2018-09-14 | 纽迈（常州）新材料有限公司 | A kind of clean preparation method of ferric orthophosphate |
| CN108609595A (en) * | 2018-05-10 | 2018-10-02 | 湖南雅城新材料有限公司 | Ferric phosphate and its preparation method and application |
| CN110294466A (en) * | 2019-08-19 | 2019-10-01 | 四川轻化工大学 | A kind of preparation method of nano-sheet ferric phosphate |
| WO2019200557A1 (en) * | 2018-04-18 | 2019-10-24 | 南通百川新材料有限公司 | Preparation method for iron phosphate |
| CN110482512A (en) * | 2019-07-12 | 2019-11-22 | 乳源东阳光磁性材料有限公司 | A kind of preparation method of battery-grade iron phosphate |
| CN110615419A (en) * | 2019-07-01 | 2019-12-27 | 湖北虹润高科新材料有限公司 | Iron phosphate production facility |
-
2016
- 2016-05-31 CN CN201610373365.8A patent/CN106064810A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107032316A (en) * | 2017-06-12 | 2017-08-11 | 百川化工(如皋)有限公司 | A kind of preparation method of ferric phosphate |
| CN108529582A (en) * | 2018-03-28 | 2018-09-14 | 纽迈（常州）新材料有限公司 | A kind of clean preparation method of ferric orthophosphate |
| WO2019200557A1 (en) * | 2018-04-18 | 2019-10-24 | 南通百川新材料有限公司 | Preparation method for iron phosphate |
| CN108609595A (en) * | 2018-05-10 | 2018-10-02 | 湖南雅城新材料有限公司 | Ferric phosphate and its preparation method and application |
| CN108609595B (en) * | 2018-05-10 | 2020-08-21 | 湖南雅城新材料有限公司 | Iron phosphate and preparation method and application thereof |
| CN110615419A (en) * | 2019-07-01 | 2019-12-27 | 湖北虹润高科新材料有限公司 | Iron phosphate production facility |
| CN110482512A (en) * | 2019-07-12 | 2019-11-22 | 乳源东阳光磁性材料有限公司 | A kind of preparation method of battery-grade iron phosphate |
| CN110294466A (en) * | 2019-08-19 | 2019-10-01 | 四川轻化工大学 | A kind of preparation method of nano-sheet ferric phosphate |
| CN110294466B (en) * | 2019-08-19 | 2020-11-17 | 四川轻化工大学 | Preparation method of nano flaky iron phosphate |
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Application publication date: 20161102 |