CN113460987A - Doped iron phosphate and preparation method and application thereof - Google Patents

Doped iron phosphate and preparation method and application thereof Download PDF

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CN113460987A
CN113460987A CN202110536635.3A CN202110536635A CN113460987A CN 113460987 A CN113460987 A CN 113460987A CN 202110536635 A CN202110536635 A CN 202110536635A CN 113460987 A CN113460987 A CN 113460987A
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iron phosphate
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段金亮
李长东
夏阳
阮丁山
陈若葵
乔延超
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Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
Hunan Bangpu Automobile Circulation Co Ltd
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Guangdong Brunp Recycling Technology Co Ltd
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Publication of CN113460987A publication Critical patent/CN113460987A/en
Priority to PCT/CN2021/142927 priority patent/WO2022242184A1/en
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Abstract

The invention belongs to the technical field of battery materials, and discloses doped iron phosphate and a preparation method and application thereof. The grain diameter of the doped ferric phosphate is 2.5-3.5 mu m, and the tap density is 0.71-0.8g/cm3The specific surface area is 8.56-9.3m2(ii) in terms of/g. The invention can prepare the battery-grade iron phosphate with uniformly distributed doping elements, the condition and the components are easy to control, the industrial production is easy, the grain diameter of the doping iron phosphate is 2.5-3.5 mu m, and the tap density is 0.71-0.8g/cm3The problems of difficult doping and difficult compaction improvement caused by doping in the lithium iron phosphate synthesis process are solved.

Description

Doped iron phosphate and preparation method and application thereof
Technical Field
The invention belongs to the technical field of battery materials, and particularly relates to doped iron phosphate and a preparation method and application thereof.
Background
The olivine-type lithium iron phosphate has the advantages of high energy density, stable voltage platform, long service life, low cost, good safety performance and the like, is considered to be a promising anode material, and is widely applied to industries such as power automobiles, energy storage and the like. However, due to the structure of the lithium iron phosphate material, the electronic conductivity is low, and the diffusion coefficient of lithium ions is small, so that the development of lithium iron phosphate is greatly restricted.
However, most of the existing doping methods for lithium iron phosphate are to add doping elements during the process of mixing lithium iron phosphate, and then obtain a doped modified lithium iron phosphate material through the subsequent processes of roasting, etc., but the components and conditions of the above modification methods are difficult to control, and the doping elements are not uniform, so that the industrial production is not easy to realize.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides doped iron phosphate and a preparation method and application thereof, the preparation condition and the components of the doped iron phosphate are easy to control, the industrial production is easy, the particle size of the doped iron phosphate is 2.5-3.5 mu m, and the tap density is 0.71-0.8g/cm3The specific surface area is 8.56-9.3m2The difficulty of doping caused by doping in the synthesis process of the lithium iron phosphate is avoidedAnd difficulty in improving compaction.
In order to achieve the purpose, the invention adopts the following technical scheme:
doped ferric phosphate, wherein the grain diameter of the doped ferric phosphate is 2.5-3.5 mu m, and the tap density is 0.71-0.8g/cm3The specific surface area is 8.56-9.3m2/g。
A preparation method of doped ferric phosphate comprises the following steps:
(1) dissolving a phosphorus source and an iron source in an acidic solution, filtering and collecting filtrate to obtain acidic ferrophosphorus solution;
(2) and adding a substance containing a doping element into the acidic ferrophosphorus solution, adjusting the pH value, heating and stirring, reacting, and carrying out liquid-solid separation to obtain the doped ferric phosphate.
Preferably, in step (1), the phosphorus source is a phosphate-containing substance; the phosphate-containing substance includes organic phosphate and inorganic phosphate.
Further preferably, the phosphate-containing substance is at least one of phosphoric acid, dihydrogen phosphate, hydrogen phosphate, hydroxyethylidene diphosphonate, or aminotrimethylene phosphate.
More preferably, the phosphate-containing substance is phosphoric acid.
Preferably, in the step (1), the iron source is a substance containing iron element; the iron source is ferrophosphorus waste, ferrophosphorus leaching slag, iron powder and magnetite (Fe)3O4) Hematite (Fe)2O3) At least one of iron phosphate, lithium iron phosphate, ferric sulfate, ferrous sulfate, ferric chloride, ferrous chloride, ferric nitrate or ferrous nitrate.
Preferably, in the step (1), the acidic solution is at least one of sulfuric acid, hydrochloric acid, nitric acid and phosphoric acid.
Preferably, in the step (1), the concentration of the acidic solution is 1-16 mol/L. Further preferably, the concentration of the acidic solution is 2-10 mol/L.
Preferably, in the step (1), the iron-phosphorus ratio in the ferrophosphorus solution is 1: (1-1.20).
Preferably, in the step (2), the doping element is at least one of Ti, Al, V, Ni, Co, Mn, Mg, Cr, and Mo.
Preferably, in the step (2), the doping element substance is a solution of a soluble salt or oxide of the doping element.
More preferably, the doping element-containing substance is at least one of titanium trichloride, titanium oxide, aluminum sulfate, aluminum chloride, nickel sulfate, magnesium chloride, chromium sesquioxide, or molybdenum trioxide.
Preferably, in the step (2), the doping amount of the doping element in the doping element-containing substance is 0.1-10%.
Preferably, in the step (2), when the iron source is ferrous iron, aeration oxidation is further included before the pH adjustment; the gas used for the aeration oxidation is oxygen. The aeration oxidation is to remove Fe in the solution2+Is oxidized into Fe3+The subsequent iron precipitation rate is improved.
Preferably, in the step (2), the substance used for adjusting the pH is at least one of sodium hydroxide, ammonia water or sodium carbonate.
Preferably, in the step (2), the stirring speed is 100-1300 r/min, and more preferably 350-800 r/min.
The invention also provides a preparation method of the doped coated carbon type lithium iron phosphate, which comprises the following steps:
and mixing the doped iron phosphate and a lithium source, adding a carbon source, adding water for sanding, spray-drying, and roasting to obtain the doped lithium iron phosphate.
Preferably, the molar ratio of ferric phosphate in the doped ferric phosphate to lithium in the lithium source is 1: (0.98-1.05).
Preferably, the roasting temperature is 750-800 ℃, and the roasting atmosphere is nitrogen or argon.
Preferably, the lithium source is selected from at least one of lithium carbonate, lithium hydroxide, lithium nitrate or lithium acetate.
Preferably, the carbon source is glucose.
Further preferably, the mass fraction of glucose is 5-10%.
Compared with the prior art, the invention has the following beneficial effects:
1. the battery-grade iron phosphate prepared by the invention has the advantages that the doping elements are uniformly distributed, the condition and the components are easy to control, the industrial production is easy, the grain diameter of the doped iron phosphate is 2.5-3.5 mu m, and the tap density is 0.71-0.8g/cm3The specific surface area is 8.56-9.3m2And the problems of difficult doping and difficult improvement of compaction caused by doping in the lithium iron phosphate synthesis process are solved.
2. The preparation method of the doped iron phosphate is simple to operate, and the substance containing the doping elements is added into the ferrophosphorus solution to synthesize the iron phosphate, so that the doping process and the precipitation process are performed simultaneously, the problems of difficult doping and difficult improvement of compaction caused by doping in the synthesis process of the lithium iron phosphate are solved, the condition and the components are easy to control, and the battery-grade iron phosphate with uniformly distributed doping elements can be obtained; the precursor with uniformly distributed doping elements has a large influence on the performance of the lithium iron phosphate, and the electrochemical performance of the lithium iron phosphate can be further improved by uniformly doping.
3. Compared with the lithium iron phosphate prepared by doping in the synthesis section, the lithium iron phosphate material prepared by doping the iron phosphate has obviously improved electrochemical performance because the electrochemical performance of the lithium iron phosphate material can be improved by improving the uniformity of the doping elements.
Drawings
Fig. 1 is an SEM image of titanium-doped iron phosphate of example 1 of the present invention.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
Example 1
The preparation method of doped iron phosphate, specifically the preparation method of titanium doped iron phosphate, includes the following steps:
(1) taking a phosphorus source as phosphoric acid and an iron source as reduced iron powder, dissolving the reduced iron powder in 2mol/L sulfuric acid to obtain an acidic iron solution, and supplementing the phosphoric acid into the acidic iron solution according to the iron-phosphorus ratio of 1: 1.03 to obtain an acidic iron-phosphorus solution;
(2) adding 0.2g/L titanium trichloride solution into the acidic ferrophosphorus solution, and introducing oxygen to oxidize for 1h until Fe in the solution2+Oxidation to Fe3+Adding sodium hydroxide to adjust the pH value to 3, reacting for 3 hours at 90 ℃, and performing liquid-solid separation to obtain titanium doped iron phosphate;
(3) and washing, filtering, drying and dehydrating the obtained titanium doped iron phosphate to obtain a finished product of the titanium doped iron phosphate.
Fig. 1 is an SEM image of titanium-doped iron phosphate according to example 1 of the present invention; the multiplying factor in a of fig. 1 is 50000, the multiplying factor in b of fig. 1 is 10000, and it can be seen from a and b of fig. 1 that the doped iron phosphate with good sphericity is prepared and is uniformly doped.
Example 2
The preparation method of doped iron phosphate, specifically the preparation method of titanium doped iron phosphate, includes the following steps:
(1) dissolving ferrophosphorus leaching slag obtained after lithium extraction in 2mol/L sulfuric acid to obtain an acidic ferrophosphorus solution;
(2) adding 0.3g/L of vitriol into the acidic ferrophosphorus solution, stirring and dissolving, adding sodium hydroxide to adjust the pH value to 3 after complete dissolution, reacting for 4 hours at 85 ℃, and performing liquid-solid separation to obtain vanadium doped iron phosphate;
(3) and washing, filtering, drying and dehydrating the obtained vanadium doped iron phosphate to obtain a finished product of the titanium doped iron phosphate.
Example 3
The preparation method of doped iron phosphate, specifically the preparation method of nickel-doped iron phosphate, includes the following steps:
(1) respectively dissolving sodium dihydrogen phosphate and ferric sulfate in 2mol/L sulfuric acid to obtain an acidic iron solution and an acidic phosphorus solution, and preparing the acidic iron-phosphorus solution according to the iron-phosphorus ratio of 1: 1.05;
(2) adding 0.2g/L nickel sulfate into the ferrophosphorus solution, stirring and dissolving, adding sodium carbonate to adjust the pH value to 3 after complete dissolution, reacting for 3 hours at 90 ℃, and performing liquid-solid separation to obtain nickel-doped iron phosphate;
(3) and washing, filtering, drying and dehydrating the obtained nickel-doped iron phosphate to obtain the nickel-doped iron phosphate.
Example 4
The preparation method of doped iron phosphate, specifically the preparation method of titanium doped iron phosphate, includes the following steps:
(1) respectively dissolving sodium hydrogen phosphate and ferrous nitrate in 4mol/L nitric acid to obtain an acidic iron solution and an acidic phosphorus solution, and preparing the acidic phosphorus-iron solution according to the iron-phosphorus ratio of 1: 1.03;
(2) adding 0.2g/L titanium trichloride solution into the acidic ferrophosphorus solution, and introducing oxygen to oxidize for 2h until Fe in the solution2+Oxidation to Fe3+Adding sodium hydroxide to adjust the pH value to 3, reacting for 3 hours at 90 ℃, and performing liquid-solid separation to obtain titanium doped iron phosphate;
(3) and washing, filtering, drying and dehydrating the obtained titanium doped iron phosphate to obtain a finished product of the titanium doped iron phosphate.
Comparative example 1
The method for preparing iron phosphate of this comparative example comprises the following steps:
(1) respectively dissolving phosphoric acid and magnetite in 2mol/L sulfuric acid to obtain an acidic iron solution and an acidic phosphorus solution, and preparing an acidic phosphorus iron solution according to the iron-phosphorus ratio of 1: 1.03;
(2) introducing air into the ferrophosphorus solution to oxidize for 1h to obtain Fe in the solution2+Oxidation to Fe3+Adding ammonia water to adjust the pH value to 3, reacting for 4 hours at 90 ℃, and carrying out liquid-solid separation to obtain iron phosphate;
(3) and washing, filtering, drying and dehydrating the iron phosphate to obtain the finished iron phosphate.
Comparative example 2
The preparation method of the zinc-doped lithium iron phosphate/carbon composite material comprises the following steps:
(1) taking iron phosphate, lithium carbonate, glucose and zinc acetate as raw materials, taking deionized water as a dispersing agent to form slurry, and carrying out ultrasonic dispersion after stirring the slurry;
(2) placing the uniformly dispersed slurry in an agate tank, carrying out wet ball milling treatment on the slurry in a planetary ball mill, and carrying out microwave treatment on the ball-milled slurry;
(3) drying the slurry subjected to microwave treatment by a spray dryer to obtain semi-finished powder, and performing dry grinding treatment on the semi-finished powder in a ball milling tank for primary crushing;
(4) and carrying out high-temperature calcination treatment on the primary crushed particles in a protective atmosphere, and then carrying out secondary crushing to obtain the lithium iron phosphate.
And (4) comparing the results:
table 1 main element analysis table of iron phosphate prepared in example 1
Figure BDA0003069875750000051
Figure BDA0003069875750000061
Table 2 specific test data for doped iron phosphates of examples 1-3 and iron phosphate of comparative example 1
Serial number Particle size D50(μm) Tap density (g/cm)3) Scale (m)2/g)
Example 1 2.71 0.71 8.83
Example 2 3.23 0.75 9.27
Example 3 2.96 0.73 8.56
Comparative example 1 2.85 0.72 8.55
As can be seen from table 2, the particle size, tap density, specific surface area of the doped iron phosphate prepared in examples 1 to 3 and the data of the iron phosphate prepared in comparative example 1 are not very different, which indicates that the physical index of the iron phosphate is not greatly affected by the doping element, and further indicates that the doping element of the present invention is uniformly distributed on the iron phosphate.
Table 3 comparison table of compacted density and electric property test results of synthetic lithium iron phosphate powder
Figure BDA0003069875750000062
Table 3 is a comparison table of the detection results of the compaction density and the electrical property of the doped iron phosphate of examples 1 to 3 and the lithium iron phosphate powder synthesized by the comparative example, and it can be seen from the data in the table that the electrochemical properties of the lithium iron phosphate material prepared from the element-doped iron phosphate are significantly improved compared with those of the lithium iron phosphate prepared from the undoped iron phosphate because the conductive performance of the lithium iron phosphate material is improved by the introduction of the doping element, thereby improving the electrochemical properties of the lithium iron phosphate material; the comparison of the performance of the lithium iron phosphate prepared in the comparative example 2 (solid phase doping) shows that the performance of the lithium iron phosphate prepared by doping the iron phosphate in the examples 1 to 3 is better, which indicates that the electrochemical performance of the lithium iron phosphate material can be improved by improving the uniformity of the doping elements through the liquid phase doping.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present invention. Furthermore, the embodiments of the present invention and the features of the embodiments may be combined with each other without conflict.

Claims (10)

1. The doped ferric phosphate is characterized in that the particle size of the doped ferric phosphate is 2.5-3.5 mu m, and the tap density is 0.71-0.8g/cm3The specific surface area is 8.56-9.3m2/g。
2. The method for the preparation of doped iron phosphate according to claim 1, characterized in that it comprises the following steps:
(1) dissolving a phosphorus source and an iron source in an acidic solution, filtering and collecting filtrate to obtain acidic ferrophosphorus solution;
(2) adding a substance containing a doping element into the acidic ferrophosphorus solution, adjusting the pH value, heating and stirring, reacting, and carrying out liquid-solid separation to obtain the doped ferric phosphate.
3. The production method according to claim 2, wherein in the step (1), the phosphorus source is a phosphate-containing substance; the phosphate-containing substance is at least one of phosphoric acid, dihydrogen phosphate, hydrogen phosphate, hydroxyethylidene diphosphonate or aminotrimethylene phosphate.
4. The preparation method according to claim 2, wherein in the step (1), the iron source is at least one of ferrophosphorus waste, ferrophosphorus leaching residue, iron powder, magnetite, hematite, iron phosphate, lithium iron phosphate, ferric sulfate, ferrous sulfate, ferric chloride, ferrous chloride, ferric nitrate or ferrous nitrate.
5. The method according to claim 2, wherein in the step (2), the doping element is at least one of Ti, Al, V, Ni, Co, Mn, Mg, Cr, or Mo.
6. The method according to claim 2, wherein in the step (2), the doping element substance is a solution of a soluble salt or oxide of the doping element; the substance containing the doping elements is at least one of titanium trichloride, titanium oxide, aluminum sulfate, aluminum chloride, nickel sulfate, magnesium chloride, chromium sesquioxide or molybdenum trioxide.
7. The method according to claim 2, wherein in the step (2), when the iron source is ferrous iron, the adjusting the pH further comprises aeration oxidation; the gas used for the aeration oxidation is oxygen.
8. The method according to claim 2, wherein in the step (2), the substance used for adjusting the pH is at least one of sodium hydroxide, aqueous ammonia, or sodium carbonate.
9. A preparation method of doped coated carbon type lithium iron phosphate is characterized by comprising the following steps:
mixing the doped iron phosphate and a lithium source according to claim 1, adding a carbon source, adding water, performing sanding treatment, spray drying, and roasting to obtain the doped coated carbon type lithium iron phosphate.
10. The method according to claim 9, wherein the carbon source is glucose.
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Publication number Priority date Publication date Assignee Title
WO2022242184A1 (en) * 2021-05-17 2022-11-24 广东邦普循环科技有限公司 Doped iron phosphate, and preparation method therefor and application thereof
CN114572951A (en) * 2022-01-28 2022-06-03 宜昌邦普循环科技有限公司 Doped iron phosphate and preparation method and application thereof
CN114572951B (en) * 2022-01-28 2023-09-12 宜昌邦普循环科技有限公司 Doped ferric phosphate and preparation method and application thereof
CN114702021A (en) * 2022-05-09 2022-07-05 兰州兰石中科纳米科技有限公司 Method for preparing lithium iron phosphate by in-situ doping of metal elements

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