CN111908441B - Method for preparing titanium-doped ferric phosphate by wet process - Google Patents
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Abstract
The invention relates to the technical field of electrochemical power source material preparation, and discloses a method for preparing titanium-doped ferric phosphate by a wet method. The method comprises the following steps: (1) Dissolving ferrous salt in water, adding phosphoric acid, mixing uniformly, adding scrap iron, reacting, and filtering to obtain a clear solution; (2) Adding the saturated titanium salt solution into the clear solution obtained in the step (1) and stirring and uniformly mixing; (3) Adding an oxidant into the solution obtained in the step (2) for oxidation to obtain a slurry containing pale yellow precipitate; (4) Adding an alkaline solution into the slurry obtained in the step (3), adjusting the pH value of the solution, and then heating to obtain milky slurry; (5) Filtering the slurry obtained in the step (4) to obtain a filter cake, and then washing, drying and sintering the filter cake. The method adopts a coated coprecipitation method, and is doped with titanium in the process of synthesizing ferric phosphate, and has simple process flow, low production cost and good doping uniformity.
Description
Technical Field
The invention relates to the technical field of electrochemical power source material preparation, in particular to a method for preparing titanium-doped ferric phosphate by a wet method.
Background
The lithium iron phosphate is one of the anode materials with the largest application amount in the current lithium ion battery industry, has the advantages of high capacity, good cycle performance, good safety, low cost and the like, and is widely applied to the fields of power and energy storage. At present, the lithium iron phosphate is generally doped and modified in the industry so as to achieve the purpose of improving the material performance. The main doping method at present is to add an additive during wet mixing in the lithium iron phosphate synthesis process, and achieve the doping effect by means of the subsequent high-temperature sintering process.
The doping process in the lithium iron phosphate synthesis process is difficult to dope due to the fact that the titanium dioxide is too high in melting point in the sintering process, the existence of doped particles can influence the growth of primary particles of the lithium iron phosphate, and finally, the doping effect is poor and the compaction density of the material is difficult to promote.
The iron phosphate doping is also one of the routes of the lithium iron phosphate doping, and the existing iron phosphate doping is to mix a titanium source and an iron source under an acidic condition and then coprecipitate, and then achieve the doping effect in the high-temperature sintering process. After the ferric phosphate is doped, the material has certain performance advantages when the lithium iron phosphate material is synthesized.
The doping is carried out in the iron phosphate synthesis process, and the doping method of coprecipitation is carried out by using the iron and titanium solution, so that titanium and iron can be uniformly distributed, titanium doped iron phosphate is directly formed in the iron phosphate sintering process, and the problems of difficult doping and difficult compaction improvement caused by doping in the lithium iron phosphate synthesis process are avoided. However, the solution of titanium and iron has strong acidity, and when the pH value is regulated in the process of synthesizing ferric phosphate, the required pH value regulator is greatly increased, the production cost of ferric phosphate is increased to a certain extent, and byproducts in the synthesis process are increased, so that the impurity removal process is more complicated, and the cost of a final finished product is increased.
Disclosure of Invention
The invention aims to solve the problem of high cost for producing titanium-doped ferric phosphate in the prior art, and provides a synthetic method for preparing titanium-doped ferric phosphate by a wet method.
In order to achieve the above object, the present invention provides a method for preparing titanium-doped ferric phosphate by wet process, comprising the steps of:
(1) Dissolving ferrous salt in water, adding phosphoric acid, mixing uniformly, adding scrap iron, reacting, and filtering to obtain a clear solution;
(2) Adding the saturated titanium salt solution into the clear solution obtained in the step (1) and stirring and uniformly mixing;
(3) Adding an oxidant into the solution obtained in the step (2) for oxidation to obtain a slurry containing pale yellow precipitate;
(4) Adding an alkaline solution into the slurry obtained in the step (3), adjusting the pH value of the solution, and then heating to obtain milky slurry;
(5) Filtering the slurry obtained in the step (4) to obtain a filter cake, and then washing, drying and sintering the filter cake.
Preferably, in step (1), the temperature of the reaction is 40-60 ℃; the reaction time is 3-5h.
Preferably, the specific operation of step (2) is: and (3) dropwise adding the saturated titanium salt solution into the clear solution obtained in the step (1) and stirring and uniformly mixing at the rotating speed of 100-200 rpm.
Preferably, in step (2), the stirring time is 8-12min.
Preferably, in step (3), the oxidizing agent is hydrogen peroxide.
Preferably, in step (3), the time of the oxidation is 0.75-1.25h.
Preferably, in step (4), the alkaline solution is sodium hydroxide and/or ammonia water.
Preferably, in step (4), the pH of the adjustment solution is between 1.2 and 1.8.
Preferably, in step (4), the temperature of the heating is 60-100 ℃; the heating time is 1-4h.
Preferably, in step (5), the sintering temperature is 700-800 ℃; the sintering time is 2-8h.
The method is a coating coprecipitation method, a nanoscale titanium source is preferentially precipitated under the weak acid condition, then a small amount of pH regulator is added, and ferric phosphate is subjected to coating precipitation on the surface of the titanium source, so that the uniform doping effect same as that of the coprecipitation is achieved, and a titanium doped ferric phosphate dihydrate is obtained, and a titanium doped ferric phosphate finished product is obtained after sintering. Compared with the prior art, the method adopted by the invention greatly reduces the addition amount of the pH regulator, has the advantages of less raw material consumption, simple process flow, reduced iron phosphate doping cost and good doping uniformity, and can be used for doping other metal elements (such as vanadium, magnesium, manganese and the like) and achieve equivalent effects.
Drawings
FIG. 1 is a process flow diagram of a method for preparing titanium doped ferric phosphate by wet process according to the present invention.
Detailed Description
The following describes specific embodiments of the present invention in detail with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The invention provides a method for preparing titanium-doped ferric phosphate by a wet method, wherein a process flow chart of the method is shown in figure 1, and the method comprises the following steps of:
(1) Dissolving ferrous salt in water, adding phosphoric acid, mixing uniformly, adding scrap iron, reacting, and filtering to obtain a clear solution;
(2) Adding the saturated titanium salt solution into the clear solution obtained in the step (1) and stirring and uniformly mixing;
(3) Adding an oxidant into the solution obtained in the step (2) for oxidation to obtain a slurry containing pale yellow precipitate;
(4) Adding an alkaline solution into the slurry obtained in the step (3), adjusting the pH value of the solution, and then heating to obtain milky slurry;
(5) Filtering the slurry obtained in the step (4) to obtain a filter cake, and then washing, drying and sintering the filter cake.
In the method of the present invention, in step (1), the ferrous salt may be a conventional choice in the art. Preferably, the ferrous salt is ferrous sulfate.
In the method of the present invention, in step (1), the concentration of phosphoric acid is not particularly required. Preferably, the concentration of phosphoric acid is 85 wt%.
In the process according to the invention, in step (1), the temperature of the reaction is 40-60 ℃. In particular embodiments, the temperature of the reaction may be 40 ℃, 45 ℃, 50 ℃, 55 ℃, or 60 ℃.
In the method of the present invention, in step (1), the reaction time is 3 to 5 hours. In specific embodiments, the reaction time may be 3 hours, 3.5 hours, 4 hours, 4.5 hours, or 5 hours.
In the process according to the invention, in step (2), the titanium salt may be a conventional choice in the art. Preferably, the titanium salt is titanium sulfate.
In the method of the present invention, the specific operation of step (2) is: and (3) dropwise adding the saturated titanium salt solution into the clear solution obtained in the step (1) and stirring and uniformly mixing at the rotating speed of 100-200 rpm.
In the method of the present invention, in the step (2), the stirring time is 8 to 12 minutes. In specific embodiments, the stirring time may be 8min, 9min, 10min, 11min, or 12min.
In the process according to the invention, in step (3), the oxidizing agent may be a conventional choice in the art. Preferably, the oxidant is hydrogen peroxide.
In the method of the present invention, in step (3), the time of the oxidation is 0.75 to 1.25 hours. In specific embodiments, the time of oxidation may be 0.75h, 0.8h, 0.9h, 1h, 1.1h, 1.2h, or 1.25h.
In the method of the present invention, in step (4), the alkaline solution may be a conventional choice in the art. Preferably, the alkaline solution is sodium hydroxide and/or ammonia water.
In the method of the present invention, in step (4), the pH of the solution is adjusted to 1.2 to 1.8.
In the method according to the invention, in step (4), the heating temperature is 60-100 ℃. In particular embodiments, the temperature of the heating may be 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃, or 100 ℃.
In the method of the present invention, in step (4), the heating time is 1 to 4 hours. In specific embodiments, the heating time may be 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, or 4h.
In the method of the present invention, in step (5), the sintering temperature is 700 to 800 ℃. In particular embodiments, the sintering temperature may be 700 ℃, 710 ℃, 720 ℃, 730 ℃, 740 ℃, 750 ℃, 760 ℃, 770 ℃, 780 ℃, 790 ℃, or 800 ℃.
In the method of the present invention, in step (5), the sintering time is 2 to 8 hours. In specific embodiments, the sintering time may be 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h, 5.5h, 6h, 6.5h, 7h, 7.5h, or 8h.
Compared with the prior art, the method provided by the invention has the following advantages:
(1) And (3) adopting a coating coprecipitation method to preferentially precipitate a nanoscale titanium source under a weak acid condition, then adding a small amount of pH regulator, and carrying out coating precipitation on the surface of the titanium source to achieve the same uniform doping effect as the coprecipitation, thereby obtaining titanium doped ferric phosphate dihydrate, and obtaining a titanium doped ferric phosphate finished product after sintering. The method adopted by the invention greatly reduces the addition amount of the pH regulator and reduces the cost.
(2) Because of adopting the cladding coprecipitation method, the titanium doping amount is adjusted according to the earlier-stage titanium source adding amount, and in theory, the titanium doping amount can be adjusted once between 100 and 10000ppm, the application range is wide, and the doping amount is high.
(3) The coating type coprecipitation method is adopted for doping, a titanium source can be uniformly dispersed in the ferric phosphate dihydrate particles, titanium doped ferric phosphate with good doping uniformity is obtained after full sintering, the performance improvement on the ferric phosphate is obvious, and the doping uniformity is good.
(4) Can be used for doping other metal elements (such as vanadium, magnesium, manganese and the like) and can achieve equivalent effects.
(5) The prepared titanium doped ferric phosphate finished product can be used for preparing high-performance lithium iron phosphate anode materials.
The present invention will be described in detail by way of examples, but the scope of the present invention is not limited thereto.
Example 1
(1) 68g of ferrous sulfate is dissolved in 300g of pure water, 59.2g of phosphoric acid with the concentration of 85 wt% is added, 12.5g of scrap iron is added after stirring and dispersing, the reaction temperature is controlled to be 50 ℃, the reaction is completed after 4 hours, and then a clear blue-green solution is obtained after filtration.
(2) 0.4g of titanium sulfate was prepared as a saturated solution, slowly dropped into the clear solution obtained in the step (1), and stirred at a rotation speed of 200rpm for 10 minutes.
(3) And (3) adding 45g of hydrogen peroxide into the solution obtained in the step (2) at a constant speed for oxidization for 1h to obtain the slurry containing light yellow precipitate.
(4) 6.7g of sodium hydroxide is dissolved in 200g of water to prepare an alkaline solution, the alkaline solution is added into the slurry obtained in the step (3) to adjust the pH value to 1.5, and then the slurry is heated to 85 ℃ and is kept for 4 hours to obtain milky slurry.
(5) And (3) filtering the slurry obtained in the step (4) to obtain a white filter cake, washing and drying the filter cake, and sintering the filter cake at 750 ℃ for 4 hours to obtain 63.9g of titanium-doped anhydrous ferric phosphate finished product A1.
Example 2
The procedure described in example 1 was followed, except that in step (2), the mass of titanium sulfate used was 0.8g, to obtain 63.3g of a titanium-doped anhydrous iron phosphate finished product A2.
Example 3
The procedure described in example 1 was followed, except that in step (2), the mass of titanium sulfate used was 1.2g, to obtain 63.5g of a titanium-doped iron phosphate finished product A3.
Example 4
The procedure of example 1 was followed, except that in step (1), the reaction temperature was 40℃to obtain 61.2g of a titanium-doped anhydrous iron phosphate finished product A4.
Example 5
The procedure of example 1 was followed, except that in step (3), the oxidation time was 0.75h, yielding 62.9g of titanium-doped anhydrous iron phosphate finished product A5.
Example 6
The procedure of example 2 was followed, except that in step (4), the heating temperature was 60℃to obtain 63.5g of a titanium-doped anhydrous iron phosphate finished product A6.
Example 7
The procedure of example 2 was followed, except that in step (4), the heating time was 1h, to obtain 63.7g of a titanium-doped anhydrous iron phosphate finished product A7.
Example 8
The procedure described in example 3 was followed, except that in step (5), the sintering time was 6 hours, to obtain 63.9g of a titanium-doped anhydrous iron phosphate finished product A8.
Example 9
(1) 3.4kg of ferrous sulfate was dissolved in 15kg of pure water, 2.96kg of phosphoric acid with a concentration of 85 wt% was added, 625g of iron filings were added after stirring and dispersion, the reaction temperature was controlled at 50℃and the reaction was completed after 4 hours, followed by filtration to obtain a clear blue-green solution.
(2) 40g of titanium sulfate was prepared as a saturated solution, slowly dropped into the clear solution obtained in the step (1), and stirred at a rotation speed of 100rpm for 10 minutes.
(3) And (3) adding 2.25kg of hydrogen peroxide into the solution obtained in the step (2) at a constant speed for oxidation for 1h to obtain slurry containing pale yellow precipitate.
(4) 335g of sodium hydroxide was dissolved in 10kg of water to prepare an alkaline solution, which was added to the slurry obtained in step (3) to adjust the pH to 1.6, and then heated to 85℃and kept at that temperature for 4 hours to obtain a milky slurry.
(5) And (3) filtering the slurry obtained in the step (4) to obtain a white filter cake, washing and drying the filter cake, and sintering the filter cake at 750 ℃ for 4 hours to obtain 3.1kg of titanium-doped anhydrous ferric phosphate finished product A9.
Comparative example 1
The method is implemented by adopting the existing titanium doped ferric phosphate production technology process, and comprises the following specific steps:
(1) 124.8g of ferrous sulfate was dissolved in 300g of pure water, 57g of phosphoric acid was added and stirred uniformly, and then 10g of concentrated sulfuric acid was added to adjust the pH to about 0.1.
(2) Adding 0.4g of titanium sulfate into the solution in the step (1), and fully stirring and dissolving to obtain a ferrous and titanium coexisting solution system.
(3) And (3) adding 45g of hydrogen peroxide into the solution obtained in the step (3) at a constant speed for oxidization for 1h to obtain a wine red ferric iron solution.
(4) 46.9g of sodium hydroxide is dissolved in 200g of water to prepare an alkaline solution, the alkaline solution is added into the solution obtained in the step (3) to adjust the pH value to 1.5, and then the temperature is raised and heated to 90 ℃ and the temperature is kept for 4 hours, so that the milky white slurry is obtained.
(5) And (3) filtering the slurry obtained in the step (4) to obtain a white filter cake, washing and drying the filter cake, and sintering the filter cake at 700 ℃ for 4 hours to obtain 63.8g of titanium-doped anhydrous ferric phosphate finished product D1.
Comparative example 2
The process according to example 3 was carried out, except that in step (5), the sintering temperature was 600℃to give 63.8g of finished titanium-doped anhydrous iron phosphate D2, which was incompletely doped with Ti and partly as free TiO 2 In the form of a gel.
Test example 1
The specific surface area, fe content, P content and Fe/P molar ratio of the titanium-doped ferric phosphate finished products prepared in examples 1-9 and comparative examples 1-2 were measured according to the national standard of GBT 30835-2014 carbon composite lithium iron phosphate cathode material for lithium ion batteries, and the results are shown in Table 1.
Test example 2
The titanium content of the titanium-doped iron phosphate finished products prepared in examples 1 to 9 and comparative examples 1 to 2 was measured using an inductively coupled plasma spectrometer, and the results are shown in Table 1.
TABLE 1
As can be seen from the results in Table 1, the titanium-doped ferric phosphate prepared by the method has relatively stable physical and chemical properties and balanced titanium doping amount, the titanium doping amount is adjustable, the process applicability is strong, only a small amount of pH regulator is needed to be added in the preparation process, and the cost is relatively low. The titanium doped ferric phosphate prepared by the invention can be used as a raw material for preparing a lithium iron phosphate material, so that the lithium iron phosphate material has good electrochemical performance and higher compaction density, and meets the application requirements of the current lithium iron phosphate power battery field.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (5)
1. A method for preparing titanium-doped ferric phosphate by a wet method, which is characterized in that ferric phosphate is coated and precipitated on the surface of a titanium source, and comprises the following steps:
(1) Dissolving ferrous salt in water, adding phosphoric acid, mixing uniformly, adding scrap iron, reacting, and filtering to obtain a clear solution;
(2) Adding the saturated titanium salt solution into the clear solution obtained in the step (1) and stirring and uniformly mixing;
(3) Adding an oxidant into the solution obtained in the step (2) for oxidation to obtain a slurry containing pale yellow precipitate;
(4) Adding an alkaline solution into the slurry obtained in the step (3), adjusting the pH value of the solution, and then heating to obtain milky slurry;
(5) Filtering the slurry obtained in the step (4) to obtain a filter cake, and then washing, drying and sintering the filter cake;
the specific operation of the step (2) is as follows: dropwise adding the saturated titanium salt solution into the clear solution obtained in the step (1) and stirring and uniformly mixing at the rotating speed of 100-200 rpm;
in the step (2), the stirring time is 8-12min;
in step (4), the heating temperature is 60-100 ℃; the heating time is 1-4h;
in the step (4), the pH value of the solution is adjusted to be 1.2-1.8;
in the step (5), the sintering temperature is 700-800 ℃; the sintering time is 2-8h.
2. The method for preparing titanium-doped ferric phosphate by wet process according to claim 1, wherein in step (1), the temperature of the reaction is 40-60 ℃; the reaction time is 3-5h.
3. The method for preparing titanium-doped ferric phosphate according to claim 1, wherein in the step (3), the oxidizing agent is hydrogen peroxide.
4. The method for preparing titanium-doped ferric phosphate according to claim 1, wherein in the step (3), the time of the oxidation is 0.75-1.25h.
5. The method for producing titanium-doped ferric phosphate according to claim 1, wherein in the step (4), the alkaline solution is sodium hydroxide and/or ammonia water.
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| CN101264875A (en) * | 2008-04-15 | 2008-09-17 | 中南大学 | Method for preparing ferric lithium phosphate precursor by comprehensive utilization of ilmenite |
| CN106185857A (en) * | 2016-07-18 | 2016-12-07 | 铜陵纳源材料科技有限公司 | A kind of battery-grade iron phosphate and preparation method thereof |
| CN108862226A (en) * | 2018-08-15 | 2018-11-23 | 南通百川新材料有限公司 | Preparation method of high-purity battery-grade iron phosphate |
| CN109761209A (en) * | 2019-03-06 | 2019-05-17 | 深圳海纳百川科技有限公司 | A kind of production technology and its production equipment of ferric phosphate |
| CN111115604A (en) * | 2020-01-03 | 2020-05-08 | 博创宏远新材料有限公司 | Preparation method of carbon-doped iron phosphate |
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| CN101264875A (en) * | 2008-04-15 | 2008-09-17 | 中南大学 | Method for preparing ferric lithium phosphate precursor by comprehensive utilization of ilmenite |
| CN106185857A (en) * | 2016-07-18 | 2016-12-07 | 铜陵纳源材料科技有限公司 | A kind of battery-grade iron phosphate and preparation method thereof |
| CN108862226A (en) * | 2018-08-15 | 2018-11-23 | 南通百川新材料有限公司 | Preparation method of high-purity battery-grade iron phosphate |
| CN109761209A (en) * | 2019-03-06 | 2019-05-17 | 深圳海纳百川科技有限公司 | A kind of production technology and its production equipment of ferric phosphate |
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Address after: 435100 No. 66 Changle Avenue, Luojiaqiao Street, Daye City, Huangshi City, Hubei Province Applicant after: Hubei Rongtong High tech Advanced Materials Group Co.,Ltd. Address before: 435100 No. 66 Changle Avenue, Luojiaqiao Street, Daye City, Huangshi City, Hubei Province Applicant before: HUBEI RT ADVANCED MATERIALS Co.,Ltd. |
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