CN101172595A - Process for producing iron phosphate - Google Patents
Process for producing iron phosphate Download PDFInfo
- Publication number
- CN101172595A CN101172595A CNA2007101560640A CN200710156064A CN101172595A CN 101172595 A CN101172595 A CN 101172595A CN A2007101560640 A CNA2007101560640 A CN A2007101560640A CN 200710156064 A CN200710156064 A CN 200710156064A CN 101172595 A CN101172595 A CN 101172595A
- Authority
- CN
- China
- Prior art keywords
- iron
- raw material
- phosphoric acid
- source compound
- phosphate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Catalysts (AREA)
Abstract
The invention relates to a preparation method of iron phosphate. The prior preparation method of iron phosphate has the disadvantages that the art is complex, the production cost is high, and the composition control is difficult. The invention takes iron source compound and phosphoric acid as raw material, takes simple organics as catalytic agent, the raw material and the catalytic agent are mixed and reacted for 20 minutes to 2 hours under 80 to 160 DEG C, therefore, the iron phosphate with the chemical formula of FexPO4 can be composed, wherein, the x is larger than or equal to 0.90 and smaller than or equal to 1.10. The raw material and the catalytic agent used by the method of the invention are common chemically raw material, the reaction is performed under a lower temperature and in ordinary pressure, therefore, the required equipment is simple, the energy consumption is low, and the cost of the products is lower. Because the reaction is performed under the lower temperature, the volatilization of elements is avoided, and the composition of the products can be easily controlled.
Description
Technical field
The invention belongs to chemical technology field, particularly relate to a kind of preparation method of ferric phosphate.
Technical background
Tertiary iron phosphate is a kind of broad-spectrum industrial chemicals, can be used as the thickening material of food and mends chalybeate, can also be used for pigment, ceramic metal glaze colour glaze.In recent years, tertiary iron phosphate as the raw material of producing lithium ion battery anode material lithium iron phosphate, has important utility value again.
Ferric oxide is the compound of stable performance, and its active and ageing put that degree is relevant, and ageing is of a specified duration more, and its chemical property is stable more.Industrialized ferric oxide all is a long time aging, so its stable performance, and under common performance condition, it is difficult to and phosphatase reaction.Newly-generated ferric oxide under acidic conditions, can and phosphatase reaction.Phosphoric acid contains three hydrogen, but only in the very strong situation of alkalescence, ionization just takes place the 3rd hydrogen, and tertiary iron phosphate is unstable in highly basic.Therefore, under normal conditions, newly-generated ferric oxide and phosphatase reaction can only generate the acid tertiary iron phosphate, and can not generate tertiary iron phosphate.
Industrialized tertiary iron phosphate production method is at high temperature to be reacted by wustite and phosphoric acid salt to form, and has the production cost height, complex process, shortcomings such as Composition Control difficulty.
Summary of the invention
The purpose of this invention is to provide the method for preparing tertiary iron phosphate that a kind of production cost is low, composition is easy to control.
The present invention is a raw material with source of iron joint compound and phosphoric acid, is catalyzer with the simple organic, with raw material and catalyst mix, reacts 20 minutes to 2 hours down at 80 ℃-160 ℃ then, just can synthesize tertiary iron phosphate.
Concrete grammar is: with phosphoric acid and Fe source compound is raw material, is catalyzer with the simple organic; With raw material and catalyst mix, under normal pressure and low temperature, to react, temperature of reaction is T, the reaction times is t, 80 ℃≤T≤160 ℃, 20min≤t≤120min, obtaining chemical formula is Fe
xPO
4Tertiary iron phosphate, 0.90≤x≤1.10 wherein.
Described Fe source compound is any one or the wherein multiple mixture in ferric oxide, iron protoxide and the Z 250.
Described simple organic is any one or the wherein multiple mixture in glucose, sucrose, dextrin and the starch.
In the described Fe source compound in iron ion and the phosphoric acid mol ratio of phosphate anion be 0.9~1.1: 1.
The mass ratio of the iron level in described catalyzer and the Fe source compound is 0.01~1: 1.
The method for preparing tertiary iron phosphate of the present invention has been utilized the katalysis of phosphoric acid increased activity and catalyzer under described temperature of reaction, generates tertiary iron phosphate.
If the inventive method raw materials used employing iron protoxide and Z 250 wherein contain+iron ion of divalent, in reaction process, the iron of+divalent can be generated the iron of+3 valencys by airborne dioxygen oxidation.
Raw material that the inventive method is used and catalyzer all are cheap industrial chemicals commonly used, are reflected under lower temperature and the normal pressure and carry out, and required equipment is simple, and energy consumption is little, so the cost of product is lower.Carry out at low temperatures because of reaction, avoided the volatilization of element, be easy to control the composition of product.
Embodiment
Embodiment one:
With ferric oxide and phosphoric acid is raw material, the mol ratio of the phosphate radical in the ferric oxide in iron ion and the phosphoric acid is 0.90: 1, is catalyzer with glucose, its quality be in the ferric oxide weight of iron 1%, ferric oxide, phosphoric acid and glucose are mixed, react 120min down at 80 ℃.Making chemical formula is Fe
0.90PO
4Tertiary iron phosphate.
Embodiment two:
With iron protoxide and phosphoric acid is raw material, the mol ratio of the phosphate radical in the iron protoxide in iron ion and the phosphoric acid is 0.95: 1, with sucrose is catalyzer, its quality be in the iron protoxide weight of iron 5%, iron protoxide, phosphoric acid and sucrose are blended in 100 ℃ of down reaction 80min.Making chemical formula is Fe
0.95PO
4Tertiary iron phosphate.
Embodiment three:
With Z 250 and phosphoric acid is raw material, the mol ratio of the phosphate radical in the Z 250 in iron ion and the phosphoric acid is 1: 1, is catalyzer with starch, its quality be in the Z 250 weight of iron 10%, Z 250, phosphoric acid and starch are mixed, react 40min down at 140 ℃.Making chemical formula is FePO
4Tertiary iron phosphate.
Embodiment four:
With Fe source compound and phosphoric acid is raw material, Fe source compound is the mixture of Z 250 and iron protoxide, the mol ratio of Z 250 and iron protoxide is 1: 1, the mol ratio of the phosphate radical in the Fe source compound in iron ion and the phosphoric acid is 1.05: 1, with the dextrin is catalyzer, its quality be in the Fe source compound weight of iron 30%, Fe source compound, phosphoric acid and dextrin are mixed, at 160 ℃ of reaction 20min down.Making chemical formula is Fe
1.05PO
4Tertiary iron phosphate.
Embodiment five:
With Fe source compound and phosphoric acid is raw material, Fe source compound is the mixture of iron protoxide and ferric oxide, the mol ratio of iron protoxide and ferric oxide is 1: 1, the mol ratio of the phosphate radical in the Fe source compound in iron ion and the phosphoric acid is 1.10: 1, catalyzer is the mixture of dextrose plus saccharose, the mass ratio of dextrose plus saccharose is 1: 1, the catalyzer total mass be in the Fe source compound weight of iron 50%, with Fe source compound, phosphoric acid and catalyst mix at 160 ℃ of following reaction 40 min.Making chemical formula is Fe
1.10PO
4Tertiary iron phosphate.
Embodiment six:
With Fe source compound and phosphoric acid is raw material, Fe source compound is the mixture of ferric oxide, iron protoxide and Z 250, the mol ratio of ferric oxide, iron protoxide and Z 250 is 1: 1: 1, the iron ion in the Fe source compound and the mol ratio of the phosphate radical in the phosphoric acid are 1.10: 1, catalyzer is the mixture of glucose and dextrin, the mass ratio of glucose and dextrin is 1: 1, the catalyzer total mass be in the Fe source compound weight of iron 70%, with Fe source compound, phosphoric acid and catalyst mix at 140 ℃ of following reaction 80min.Making chemical formula is Fe
1.10PO
4Tertiary iron phosphate.
Embodiment seven:
With ferric oxide and phosphoric acid is raw material, the iron ion in the ferric oxide and the mol ratio of the phosphate radical in the phosphoric acid are 1: 1, catalyzer is the mixture of grape sugar and starch, the mass ratio of grape sugar and starch is 1: 1, the catalyzer total mass is identical with weight of iron in the Fe source compound, and Fe source compound, phosphoric acid and catalyst mix are reacted 30 min down at 120 ℃.Making chemical formula is FePO
4Tertiary iron phosphate.
Embodiment eight:
With ferric oxide and phosphoric acid is raw material, the iron ion in the ferric oxide and the mol ratio of the phosphate radical in the phosphoric acid are 1: 1, catalyzer is the mixture of glucose, starch, sucrose and dextrin, the mass ratio of glucose, starch, sucrose and dextrin is 1: 1: 1: 1, the catalyzer total mass be in the Fe source compound weight of iron 25%, with Fe source compound, phosphoric acid and catalyst mix at 140 ℃ of following reaction 80 min.Making chemical formula is FePO
4Tertiary iron phosphate.
Claims (1)
1. preparation method of ferric phosphate is characterized in that this method is is raw material with phosphoric acid and Fe source compound, is catalyzer with the simple organic; With raw material and catalyst mix, under normal pressure and low temperature, to react, temperature of reaction is T, the reaction times is t, 80 ℃≤T≤160 ℃, 20min≤t≤120 min, obtaining chemical formula is Fe
xPO
4Tertiary iron phosphate, 0.90≤x≤1.10 wherein;
Described Fe source compound is any one or the wherein multiple mixture in ferric oxide, iron protoxide and the Z 250;
Described simple organic is any one or the wherein multiple mixture in glucose, sucrose, dextrin and the starch;
In the described Fe source compound in iron ion and the phosphoric acid mol ratio of phosphate anion be 0.9~1.1: 1;
The mass ratio of the iron level in described catalyzer and the Fe source compound is 0.01~1: 1.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2007101560640A CN100540464C (en) | 2007-10-12 | 2007-10-12 | A kind of preparation method of ferric phosphate |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2007101560640A CN100540464C (en) | 2007-10-12 | 2007-10-12 | A kind of preparation method of ferric phosphate |
Publications (2)
Publication Number | Publication Date |
---|---|
CN101172595A true CN101172595A (en) | 2008-05-07 |
CN100540464C CN100540464C (en) | 2009-09-16 |
Family
ID=39421383
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB2007101560640A Expired - Fee Related CN100540464C (en) | 2007-10-12 | 2007-10-12 | A kind of preparation method of ferric phosphate |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN100540464C (en) |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102306791A (en) * | 2011-08-18 | 2012-01-04 | 合肥国轩高科动力能源有限公司 | Preparation method of carbon-coated non-stoichiometric lithium iron phosphorus oxide material |
CN102745662A (en) * | 2012-06-15 | 2012-10-24 | 兰州理工大学 | Preparation method of amorphous iron phosphate |
CN103058160A (en) * | 2012-11-06 | 2013-04-24 | 浙江南都电源动力股份有限公司 | Preparation method of low cost battery level iron phosphate based on ferrous powder corrosion |
US8541136B2 (en) | 2008-01-17 | 2013-09-24 | A123 Systems Llc | Mixed metal olivine electrode materials for lithium ion batteries |
US9174846B2 (en) | 2009-09-18 | 2015-11-03 | A123 Systems Llc | Ferric phosphate and methods of preparation thereof |
US9178215B2 (en) | 2009-08-25 | 2015-11-03 | A123 Systems Llc | Mixed metal olivine electrode materials for lithium ion batteries having improved specific capacity and energy density |
US9660267B2 (en) | 2009-09-18 | 2017-05-23 | A123 Systems, LLC | High power electrode materials |
CN108313997A (en) * | 2018-05-14 | 2018-07-24 | 中钢集团安徽天源科技股份有限公司 | A kind of preparation method of the ball shape ferric phosphate of size fractionated distribution |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3070423A (en) * | 1960-10-17 | 1962-12-25 | Chemetron Corp | Preparation of white iron phosphate |
US3407034A (en) * | 1965-06-16 | 1968-10-22 | Pfizer & Co C | White iron phosphate |
US4374109A (en) * | 1981-12-17 | 1983-02-15 | Ashland Oil, Inc. | Manufacture of phosphosiderite iron phosphate |
US4414187A (en) * | 1982-05-19 | 1983-11-08 | The United States Of America As Represented By The United States Department Of Energy | Preparation of metal phosphates by a reaction using boron phosphate |
CN1041077C (en) * | 1993-11-18 | 1998-12-09 | 董国兴 | High ferric phosphate powder and its making method |
-
2007
- 2007-10-12 CN CNB2007101560640A patent/CN100540464C/en not_active Expired - Fee Related
Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8541136B2 (en) | 2008-01-17 | 2013-09-24 | A123 Systems Llc | Mixed metal olivine electrode materials for lithium ion batteries |
US9178215B2 (en) | 2009-08-25 | 2015-11-03 | A123 Systems Llc | Mixed metal olivine electrode materials for lithium ion batteries having improved specific capacity and energy density |
US9174846B2 (en) | 2009-09-18 | 2015-11-03 | A123 Systems Llc | Ferric phosphate and methods of preparation thereof |
US9660267B2 (en) | 2009-09-18 | 2017-05-23 | A123 Systems, LLC | High power electrode materials |
US9954228B2 (en) | 2009-09-18 | 2018-04-24 | A123 Systems, LLC | High power electrode materials |
US10522833B2 (en) | 2009-09-18 | 2019-12-31 | A123 Systems, LLC | High power electrode materials |
US11652207B2 (en) | 2009-09-18 | 2023-05-16 | A123 Systems Llc | High power electrode materials |
CN102306791A (en) * | 2011-08-18 | 2012-01-04 | 合肥国轩高科动力能源有限公司 | Preparation method of carbon-coated non-stoichiometric lithium iron phosphorus oxide material |
CN102306791B (en) * | 2011-08-18 | 2014-08-06 | 合肥国轩高科动力能源股份公司 | Method for preparing carbon-cladding non-stoichiometric lithium iron phosphorous oxide material |
CN102745662A (en) * | 2012-06-15 | 2012-10-24 | 兰州理工大学 | Preparation method of amorphous iron phosphate |
CN103058160A (en) * | 2012-11-06 | 2013-04-24 | 浙江南都电源动力股份有限公司 | Preparation method of low cost battery level iron phosphate based on ferrous powder corrosion |
CN108313997A (en) * | 2018-05-14 | 2018-07-24 | 中钢集团安徽天源科技股份有限公司 | A kind of preparation method of the ball shape ferric phosphate of size fractionated distribution |
Also Published As
Publication number | Publication date |
---|---|
CN100540464C (en) | 2009-09-16 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN100540464C (en) | A kind of preparation method of ferric phosphate | |
CN101597086A (en) | Method for preparing nano manganese dioxide with different crystal forms in low-temperature acid solution | |
CN101531355A (en) | Method for preparing high purity ferric phosphate using ferrous sulfate as by-product of white titanium pigment | |
CN105985776B (en) | Preparation method of soil conditioner rich in citric acid soluble silicon | |
CN102616857A (en) | Preparation method of manganese molybdate microcrystal | |
CN112142027A (en) | Preparation method of nano layered zirconium phosphate and silver-loaded zirconium phosphate thereof | |
CA2493224A1 (en) | Alkali metal hydrogen phosphates as precursors for phosphate-containing electrochemical active materials | |
CN101633516A (en) | Preparation method of high-purity cerium hydroxide | |
CN108862226A (en) | Preparation method of high-purity battery-grade iron phosphate | |
CN103456954A (en) | Preparation method of active electrode material | |
Abe et al. | Photocatalytic water splitting into H2 and O2 over R2Ti2O7 (R= Y, rare earth) with pyrochlore structure | |
CN101143324A (en) | Catalyst for preparing 2-methylfuran by gas-phase hydrogenation of furaldehyde and its preparation method | |
CN101376507A (en) | Method for producing sodium fluoride | |
CN102320644A (en) | Method for preparing copper-oxide powder | |
CN106000390A (en) | Method for preparation of Bi2O3/BiTaO4 composite photocatalyst by molten salt technique | |
CN101428860B (en) | Method for producing high purity MnOOH | |
CN1935673A (en) | Method for preparing trimanganese tetraoxide by direct oxidation of free bivalent manganese ion | |
CN103801297B (en) | A kind of Preparation method and use of copper nickel compoilite oxide catalyst | |
CN100575250C (en) | A kind of alkali formula method preparing phosphate iron lithium | |
CN101920994A (en) | Method for preparing vanadyl sulfate | |
CN108069668A (en) | Features backwater presses impervious marine glue paste paint | |
CN115227719B (en) | Calcium-phosphorus nanoenzyme with excellent peroxidase activity | |
CN110776477B (en) | Method for preparing DM by oxidizing M with hydrogen peroxide | |
CN101804992A (en) | Method for preparing superfine aluminium silicate by bentonite | |
CN107697896A (en) | A kind of method that high-purity phosphoric acid iron is prepared using ferric manganese ore as raw material |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
C17 | Cessation of patent right | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20090916 Termination date: 20121012 |