CN101172594A - Process for producing iron phosphate for producing iron lithium phosphate material - Google Patents
Process for producing iron phosphate for producing iron lithium phosphate material Download PDFInfo
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- CN101172594A CN101172594A CNA2007100598053A CN200710059805A CN101172594A CN 101172594 A CN101172594 A CN 101172594A CN A2007100598053 A CNA2007100598053 A CN A2007100598053A CN 200710059805 A CN200710059805 A CN 200710059805A CN 101172594 A CN101172594 A CN 101172594A
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Abstract
The invention discloses a preparation method of iron phosphate for preparing lithium iron phosphate material, and relates to heavy metal phosphate. The steps of the method are as follows: analytically pure soluble molysite is dissolved in distilled water, thereby being prepared into 0.05 to 5 M water solution, and being added with anionic surface-active agent with the mass being 0.01 to 3 percent of the mass of the molysite, then analytically pure phosphoric acid is added according to the mol ratio of Fe<3+>:PO4<3-> equal to 1:0.8 to 1.2 and stirred, alkaline solution with the concentration of 1 to 9 M is slowly added in stirring state, the adding time is more than 1 hour until the Ph value of the solution reaches 6 to 7, the deposited matter of iron phosphate is filtered, the filtered iron phosphate is cleaned for 3 to 5 times with distilled water with the 2 to 5 times weight of the iron phosphate, the iron phosphate is dried in the range of 60 to 90 DEG C under a vacuum condition, and the finished FePO4.2H2O powder is gotten. The iron phosphate product with two crystal water prepared by the invention has high reaction activity, and the performance of the lithium iron phosphate material prepared with the iron phosphate product is superior to the lithium iron phosphate material prepared with the commercial iron phosphate product.
Description
Technical field
Technical scheme of the present invention relates to heavy metal phosphoric acid salt, specifically is used to prepare the preparation method of ferric phosphate of LiFePO 4 material.
Background technology
Iron lithium phosphate is owing to have high theoretical capacity (170mAh/g), high working voltage (voltage platform about 3.5V), suitable mass density (3.64g/cm
3), self-discharge is little, LiFePO under low current density
4In Li
+Almost can 100% embed/take off embedding, have extended cycle life, good cycle, memory-less effect, cheap, Heat stability is good, advantage such as environmentally friendly, be expected to replace the higher LiCoO of cost
2Become anode material for lithium-ion batteries of new generation.
At present, solid reaction process is a LiFePO 4 material synthetic main method.In CN 1581537, CN 1753216, CN 1958440, CN 1958441 and CN 1884053 disclosed method for preparing lithium iron phosphate material, all mention with tertiary iron phosphate as main synthesis material.Yet the preparation method of highly active tertiary iron phosphate raw material is not proposed all in these documents.
Performance difference according to the tertiary iron phosphate material that experiment showed, different methods preparation is very big, and is also very big with the performance inconsistency of the LiFePO 4 material of its manufacturing.Traditional industry is produced the method for tertiary iron phosphate and was made in 2-3 hour in 180-190 ℃ of reaction in sealed vessel with phosphoric acid and iron trichloride; Another kind method is to add phosphoric acid with ferrous salt in the presence of oxygenant to make.The tertiary iron phosphate that aforesaid method makes after filtration, become commercially available tertiary iron phosphate finished product after the washing, drying.With the iron lithium phosphate that commercially available tertiary iron phosphate finished product is made, not only tap density is lower, and electrochemistry capacitance is relatively poor (is no more than 130mAh/g, 0.2C).Find by analysis, commercially available tertiary iron phosphate product all has complete crystalline-granular texture, reactive behavior is not high, lithium ion spreads very difficult therein, be difficult in the sintering process subsequently and insert lithium ion and to form the iron lithium phosphate crystal that is applicable to anode material for lithium-ion batteries, therefore with the poor-performing of the LiFePO 4 material of commercially available tertiary iron phosphate finished product manufacturing.
Summary of the invention
Technical problem to be solved by this invention is: the preparation method of ferric phosphate that is provided for preparing LiFePO 4 material.The tertiary iron phosphate material that has two crystal water that obtains with the inventive method manufacturing, have the crystalline structure similar to iron lithium phosphate, overcome commercially available tertiary iron phosphate product complete crystalline-granular texture has been arranged, reactive behavior is not high, lithium ion spreads very difficult therein, be difficult in insertion lithium ion in the sintering process subsequently and form the iron lithium phosphate crystalline shortcoming that is applicable to anode material for lithium-ion batteries, thereby improved the performance of LiFePO 4 material.
The present invention solves this technical problem the technical scheme that is adopted: the preparation method of ferric phosphate that is used to prepare LiFePO 4 material, the steps include: at first the analytical pure soluble ferric iron salt to be dissolved in distilled water, be mixed with the aqueous solution of 0.05～5M, adding quality is the anion surfactant of molysite quality 0.01～3%, making iron ion form the micella of tensio-active agent parcel, is Fe according to mol ratio then
3+: PO
4 3-=1: 0.8～1.2 ratio adds analytical pure phosphoric acid and stirs, slowly adding concentration under whipped state is the basic solution of 1～9 M, the reinforced time was greater than 1 hour, reach 6～7 up to the pH value of solution value, the tertiary iron phosphate sedimentable matter is filtered, and the tertiary iron phosphate that filters out is with the distilled water wash of 2～5 times of its weight 3～5 times, under vacuum condition, in 60～90 ℃ of scopes, dry, obtain product F ePO
42H
2The O powder.
Above-mentioned soluble ferric iron salt is iron trichloride, iron nitrate or ferric sulfate.
Above-mentioned anion surfactant is Sodium dodecylbenzene sulfonate, sodium olefin sulfonate or sodium lauryl sulphate.
Above-mentioned basic solution is NaOH, the KOH aqueous solution or ammoniacal liquor.
The above-mentioned soluble ferric iron salt and the purity of phosphoric acid are not limited to the analytical pure level.
The invention has the beneficial effects as follows:
The tertiary iron phosphate product that has two crystal water that the inventive method makes, has very high reactive behavior, also have the crystalline structure similar to iron lithium phosphate, in sintering process subsequently, lose crystal water, the effusion of crystal water can make crystalline structure the hole of flourishing molecular level occur, has destroyed complete crystalline-granular texture, form subsurface defect thus, reactive behavior is significantly increased.This tertiary iron phosphate product increases through dehydration back sedimentation, thereby has high-ratio surface and high reactivity, has a large amount of submicrometer structures simultaneously.Such structure helps lithium ion and enters in the tertiary iron phosphate, generates iron lithium phosphate rapidly.With the LiFePO 4 material uniform particle diameter that this product is made, crystalline phase is pure, and chemical property is very stable, and its performance is better than the LiFePO 4 material (seeing Table 1) made with commercially available tertiary iron phosphate product.
The performance of the LiFePO 4 material that the different phosphoric acid iron products of table 1 are made relatively
| The commercially available marine products tertiary iron phosphate product of going up | The tertiary iron phosphate product is produced in commercially available Henan | The inventive method is produced the tertiary iron phosphate product | |
| 10 batches of sample average particle diameter/μ m | 15±9 | 12±7 | 10±2 |
| XRD diffraction crystalline phase is analyzed | No dephasign | No dephasign | No dephasign |
| Loading capacity/mAhg -1，0.2C | 125±7 | 130±5 | 150±3 |
In addition, the tertiary iron phosphate product that makes with the inventive method prepares LiFePO 4 material, and compares with commercially available tertiary iron phosphate product, and needed temperature of reaction is low, the time short (seeing Table 2).
Table 2 prepares the contrast of LiFePO 4 material reaction conditions with different phosphoric acid iron products
| The commercially available marine products tertiary iron phosphate product of going up | The tertiary iron phosphate product is produced in commercially available Henan | The inventive method is produced the tertiary iron phosphate product | |
| Need temperature of reaction/℃ | 800 | 800 | 700 |
| Need reaction times/h | 12 | 15 | 6 |
Embodiment
Embodiment 1
Analytically pure iron trichloride is dissolved in distilled water, is mixed with the aqueous solution of 0.05 M, adding quality is the Sodium dodecylbenzene sulfonate of iron trichloride quality 0.01%, makes iron ion form the micella of tensio-active agent parcel, is Fe according to mol ratio then
3+: PO
4 3-=1: 0.8 ratio adds analytical pure phosphoric acid and stirs, the NaOH aqueous solution that under whipped state, slowly adds 1M concentration, the reinforced time was greater than 1 hour, reach 6 up to the pH value of solution value, the tertiary iron phosphate sedimentable matter that generates is filtered, and the tertiary iron phosphate that filters out is with the distilled water wash of 2 times of its weight 3 times, under vacuum condition, in 60 ℃ of oven dry, obtain product F ePO
42H
2The O powder.
Embodiment 2
The analytical pure iron nitrate is dissolved in distilled water, is mixed with the aqueous solution of 5 M, adding quality is the sodium olefin sulfonate of iron nitrate quality 3%, makes iron ion form the micella of tensio-active agent parcel, is Fe according to mol ratio then
3+: PO
4 3-=1: 1.2 ratio adds analytical pure phosphoric acid and stirs, the KOH aqueous solution that under whipped state, slowly adds 9M, the reinforced time was greater than 1 hour, reach 7 up to the pH value of solution value, the tertiary iron phosphate sedimentable matter that generates is filtered, the tertiary iron phosphate that filters out is with the distilled water wash of 5 times of its weight, wash altogether 5 times, under vacuum condition,, obtain product F ePO in 90 ℃ of oven dry
42H
2The O powder.
Embodiment 3
Analytical pure sulfuric acid iron is dissolved in distilled water, is mixed with the aqueous solution of 0.5M, adding quality is the sodium lauryl sulphate of ferric sulfate quality 0.1%, makes iron ion form the micella of tensio-active agent parcel, is Fe according to mol ratio then
3+: PO
4 3-=1: 1.0 ratio adds analytical pure phosphoric acid and stirs, the ammonia soln that under whipped state, slowly adds 3M, the reinforced time was greater than 1 hour, reach 6 up to the pH value of solution value, the tertiary iron phosphate sedimentable matter that generates is filtered, and the tertiary iron phosphate that filters out is with the distilled water wash of 3 times of its weight 4 times, under vacuum condition, in 80 ℃ of oven dry, obtain product F ePO
42H
2The O powder.
Embodiment 4
The analytical pure iron trichloride is dissolved in distilled water, is mixed with the aqueous solution of 0.3M, adding quality is the Sodium dodecylbenzene sulfonate of iron trichloride quality 1%, makes iron ion form the micella of tensio-active agent parcel, is Fe according to mol ratio then
3+: PO
43-=1: 1.1 ratio adds analytical pure phosphoric acid and stirs, the NaOH aqueous solution that under whipped state, slowly adds 2M, the reinforced time was greater than 1 hour, reach 7 up to the pH value of solution value, the tertiary iron phosphate sedimentable matter that generates is filtered, and the tertiary iron phosphate that filters out is with the distilled water wash of 2 times of its weight 5 times, under vacuum condition, in 60 ℃ of oven dry, obtain product F ePO
42H
2The O powder.
Claims (4)
1. be used to prepare the preparation method of ferric phosphate of LiFePO 4 material, it is characterized in that the steps include: at first the analytical pure soluble ferric iron salt being dissolved in distilled water, be mixed with the aqueous solution of 0.05～5M, adding quality is the anion surfactant of molysite quality 0.01～3%, making iron ion form the micella of tensio-active agent parcel, is Fe according to mol ratio then
3+: PO
4 3-=1: 0.8～1.2 ratio adds analytical pure phosphoric acid and stirs, slowly adding concentration under whipped state is the basic solution of 1～9 M, the reinforced time was greater than 1 hour, reach 6～7 up to the pH value of solution value, the tertiary iron phosphate sedimentable matter is filtered, and the tertiary iron phosphate that filters out is with the distilled water wash of 2～5 times of its weight 3～5 times, under vacuum condition, in 60～90 ℃ of scopes, dry, obtain product F ePO
42H
2The O powder.
2. prepare the preparation method of ferric phosphate of LiFePO 4 material according to being used to described in the claim 1, it is characterized in that: described soluble ferric iron salt is iron trichloride, iron nitrate or ferric sulfate.
3. prepare the preparation method of ferric phosphate of LiFePO 4 material according to being used to described in the claim 1, it is characterized in that: described anion surfactant is Sodium dodecylbenzene sulfonate, sodium olefin sulfonate or sodium lauryl sulphate.
4. prepare the preparation method of ferric phosphate of LiFePO 4 material according to being used to described in the claim 1, it is characterized in that: described basic solution is NaOH, the KOH aqueous solution or ammoniacal liquor.
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|---|---|---|---|
| CN200710059805A CN100588611C (en) | 2007-10-11 | 2007-10-11 | Process for producing iron phosphate for producing iron lithium phosphate material |
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Cited By (26)
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|---|---|---|---|---|
| CN101913585A (en) * | 2010-08-05 | 2010-12-15 | 武汉大学 | Synthesizing method of battery-level ultra-thin iron phosphate |
| CN102009967A (en) * | 2010-12-23 | 2011-04-13 | 武汉大学 | Method for preparing iron phosphate with micro/nano structure |
| CN102009968A (en) * | 2011-01-14 | 2011-04-13 | 武汉大学 | Preparation method of nano-flaky FePO4.2H2O |
| CN102040208A (en) * | 2011-01-12 | 2011-05-04 | 山西泰众新能源有限公司 | Method for preparing iron phosphate |
| CN102079516A (en) * | 2010-12-27 | 2011-06-01 | 东莞市安灿新能源科技有限公司 | Preparation method of sheet-form iron phosphate crystal |
| CN101708834B (en) * | 2009-12-11 | 2011-06-22 | 广西壮族自治区化工研究院 | Wafer-like ferric phosphate, preparation method and application thereof |
| CN102153061A (en) * | 2011-03-25 | 2011-08-17 | 天津恒普科技发展有限公司 | Method for synthesizing ferric phosphate material |
| CN102299320A (en) * | 2011-07-20 | 2011-12-28 | 彩虹集团公司 | Preparation method for lithium iron phosphate material applicable to power batteries |
| CN102303858A (en) * | 2011-07-20 | 2012-01-04 | 彩虹集团公司 | Preparation method of nanoscale ferric phosphate for lithium iron phosphate |
| CN102431988A (en) * | 2011-10-12 | 2012-05-02 | 浙江南都电源动力股份有限公司 | New process for preparing low-cost cell-grade iron phosphate material from basic iron acetate |
| CN102616763A (en) * | 2012-04-01 | 2012-08-01 | 清华大学深圳研究生院 | Preparation method of iron phosphate for preparing lithium iron phosphate and iron phosphate |
| CN102623695A (en) * | 2012-03-29 | 2012-08-01 | 天津巴莫科技股份有限公司 | Phosphate lithium ion battery cathode material and preparation method thereof |
| CN102745662A (en) * | 2012-06-15 | 2012-10-24 | 兰州理工大学 | Preparation method of amorphous iron phosphate |
| CN103435023A (en) * | 2013-05-17 | 2013-12-11 | 武汉工程大学 | Preparation method for ultrafine lithium phosphate powder |
| CN103606676A (en) * | 2013-11-12 | 2014-02-26 | 深圳市贝特瑞新能源材料股份有限公司 | Lithium iron phosphate/carbon nanocomposite and preparation method thereof |
| CN103633323A (en) * | 2012-08-28 | 2014-03-12 | 比亚迪股份有限公司 | Lithium iron phosphate anode active material preparation method and lithium iron phosphate anode active material prepared therethrough |
| CN104944400A (en) * | 2015-07-20 | 2015-09-30 | 河北工业大学 | Technology for preparing iron phosphate through hydrolytic method |
| CN105406068A (en) * | 2015-12-08 | 2016-03-16 | 山东精工电子科技有限公司 | Preparation method for low-temperature improved type lithium iron phosphate nanomaterial |
| CN106517128A (en) * | 2016-11-08 | 2017-03-22 | 河南省净寰新能源科技有限公司 | Low-cost cell-grade ferric phosphate micro powder preparation method |
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| CN114314545A (en) * | 2021-12-17 | 2022-04-12 | 江苏双登富朗特新能源有限公司 | Preparation method of superfine lithium iron phosphate cathode material |
| CN115072905A (en) * | 2022-07-14 | 2022-09-20 | 国环电池科技(苏州)有限公司 | Treatment method of battery wastewater and method for recycling high-purity iron phosphate from battery wastewater |
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Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4374109A (en) * | 1981-12-17 | 1983-02-15 | Ashland Oil, Inc. | Manufacture of phosphosiderite iron phosphate |
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| CN101913585A (en) * | 2010-08-05 | 2010-12-15 | 武汉大学 | Synthesizing method of battery-level ultra-thin iron phosphate |
| CN102009967B (en) * | 2010-12-23 | 2012-06-20 | 武汉大学 | Method for preparing iron phosphate with micro/nano structure |
| CN102009967A (en) * | 2010-12-23 | 2011-04-13 | 武汉大学 | Method for preparing iron phosphate with micro/nano structure |
| CN102079516A (en) * | 2010-12-27 | 2011-06-01 | 东莞市安灿新能源科技有限公司 | Preparation method of sheet-form iron phosphate crystal |
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| CN102153061A (en) * | 2011-03-25 | 2011-08-17 | 天津恒普科技发展有限公司 | Method for synthesizing ferric phosphate material |
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| CN102303858A (en) * | 2011-07-20 | 2012-01-04 | 彩虹集团公司 | Preparation method of nanoscale ferric phosphate for lithium iron phosphate |
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| CN102616763A (en) * | 2012-04-01 | 2012-08-01 | 清华大学深圳研究生院 | Preparation method of iron phosphate for preparing lithium iron phosphate and iron phosphate |
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| CN103633323A (en) * | 2012-08-28 | 2014-03-12 | 比亚迪股份有限公司 | Lithium iron phosphate anode active material preparation method and lithium iron phosphate anode active material prepared therethrough |
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| CN105406068A (en) * | 2015-12-08 | 2016-03-16 | 山东精工电子科技有限公司 | Preparation method for low-temperature improved type lithium iron phosphate nanomaterial |
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| US20240025745A1 (en) * | 2021-07-01 | 2024-01-25 | Guangdong Brunp Recycling Technology Co., Ltd. | Preparation method for nano ferric phosphate with low sulphur content |
| CN113353908A (en) * | 2021-07-07 | 2021-09-07 | 天台布瑞电源技术有限公司 | Preparation method of rod-shaped nano iron phosphate material |
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| CN114314545B (en) * | 2021-12-17 | 2022-11-18 | 江苏双登富朗特新能源有限公司 | Preparation method of superfine lithium iron phosphate cathode material |
| CN115072905A (en) * | 2022-07-14 | 2022-09-20 | 国环电池科技(苏州)有限公司 | Treatment method of battery wastewater and method for recycling high-purity iron phosphate from battery wastewater |
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