CN108408709B - Preparation process of pollution-free low-cost lithium manganese iron phosphate crystal material - Google Patents
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Abstract
The invention discloses a preparation process of a pollution-free low-cost lithium iron manganese phosphate crystal material, which is completed by the following steps: selecting iron powder and manganese powder with high purity, wherein the granularity is selected to be between 20 meshes and 20000 meshes; selecting manganese powder, iron powder, phosphoric acid and a lithium source solution according to a certain mass ratio, diluting the manganese powder, the iron powder, the phosphoric acid and the lithium source solution, and then placing the diluted manganese powder, the diluted iron powder, the diluted phosphoric acid and the lithium source solution into an acid-resistant reactor to be stirred so as to enable the iron powder, the manganese powder and the phosphoric acid to fully react; adding a lithium source solution into the obtained reaction precursor slurry, and fully and uniformly stirring, wherein the selected lithium source solution is soluble lithium source lithium hydroxide or lithium acetate; transferring the obtained slurry into a reaction kettle, and starting a hydrothermal reaction; and (3) carrying out solid-liquid separation on the slurry obtained after the reaction, and carrying out inclusion carbonization annealing treatment on the separated solid lithium manganese iron phosphate to obtain the lithium manganese iron phosphate crystal material. Compared with the prior art, the invention has the advantages of lower cost and convenient process operation, and the prepared lithium iron manganese phosphate crystal material has higher commercial value and no pollution in the manufacturing process, thereby meeting the current requirement on environmental protection.
Description
Technical Field
The invention relates to the technical field of chemical material synthesis, in particular to a preparation process of a pollution-free low-cost lithium iron manganese phosphate crystal material.
Background
With the rapid development of electric automobiles, the 3C and energy storage market demands are gradually expanded, and higher requirements are also put on the energy density of materials. Although the ternary material has higher energy density, the safety problem cannot be well solved so far, and a large amount of rare element cobalt is required for the preparation of the ternary material. Although the traditional lithium iron phosphate has a series of advantages of environmental friendliness, safety, low price, long service life and the like, the exertion of energy density is limited by the voltage of 3.2V. Although lithium manganese phosphate has an olivine stable structure similar to that of lithium iron phosphate and a voltage plateau of 4.1V, lithium manganese phosphate has a particularly poor conductivity, belongs to an insulator, and is difficult to be charged and discharged effectively, thereby limiting its commercial use. Under the background, people find that iron is doped in the lithium manganese phosphate, the iron and the manganese are mutually dissolved in any ratio, a solid solution can be formed, and the conductivity of the lithium manganese phosphate can be changed.
Disclosure of Invention
In order to solve the defects, the invention aims to provide a preparation process of a pollution-free low-cost lithium manganese iron phosphate crystal material, which has the advantages of low manufacturing cost and convenient operation, and not only the prepared lithium manganese iron phosphate crystal material has high commercial value, but also the manufacturing process is pollution-free, thereby meeting the current requirements on environmental protection.
In order to achieve the purpose, the invention adopts the technical scheme that: a process for preparing the pollution-free low-cost lithium iron manganese phosphate crystal material with chemical formula
LiFe (1-x) MnxPO4 (wherein x is more than or equal to 0.05 and less than or equal to 0.8), wherein x represents an atomic ratio or a molar ratio, when x is less than 0.05, the main term is lithium iron phosphate, a high-voltage platform is hardly exerted, when x is more than 0.8, the electrochemical performance of the preparation process is rapidly deteriorated through repeated tests, and the reaction equation of the preparation process is that
Fe+Mn+ H3PO4+LiOH→LiFe(1-X)MnXPO4+H2 +H2O，
Wherein Fe represents iron powder, Mn represents manganese powder, H3PO4 represents phosphoric acid, LiOH represents a lithium hydroxide solution,
the preparation process comprises the following steps:
1) selecting high-purity iron powder and manganese powder, selecting the granularity of 20-20000 meshes, wherein the selected granularity range can ensure that the reaction speed is moderate, the control is easy, and the reaction is too violent and difficult to control when the granularity is too fine;
2) according to the proportion of Fe: mn: h3PO 4: LiOH = (1-x): x: 1: (1.01-1.1) weighing iron powder, manganese powder, phosphoric acid and lithium source solution according to the mass ratio, diluting the iron powder, the manganese powder and the phosphoric acid, and then placing the diluted iron powder, the diluted manganese powder and the diluted phosphoric acid into an acid-resistant reactor to be stirred so as to enable the iron powder, the manganese powder and the phosphoric acid to fully react for 5-24 hours;
3) adding a lithium source solution into the reaction precursor slurry obtained in the step 2), and fully and uniformly stirring, wherein the selected lithium source solution is soluble lithium source lithium hydroxide or lithium acetate;
4) transferring the slurry obtained in the step 3) into a reaction kettle, and starting hydrothermal reaction at the temperature of 160-;
5) and (3) carrying out solid-liquid separation on the slurry obtained after the hydrothermal reaction in the step 4), carrying out inclusion carbonization annealing treatment on the separated solid lithium manganese iron phosphate, introducing inert gas for protection or selecting vacuum during annealing, wherein the annealing temperature is 550-850 ℃, and the annealing time is 3-24 hours, so as to obtain the lithium manganese iron phosphate crystal material.
Preferably, the iron powder and the manganese powder selected in the step 1) are treated by electrolysis, reduction or atomization before reaction.
In the step 1), the granularity of the selected iron powder and manganese powder is between 200 meshes and 8000 meshes.
And 2) in the full reaction process, introducing oxidizing gas with the effect of improving the reaction rate, wherein the oxidizing gas is air, oxygen or ozone.
Step 2) in the full reaction process, adding organic acid with the effect of accelerating reaction balance, wherein the adding proportion is 0.1-1, and the organic acid is citric acid, or acetic acid, or carboxylic acid, or sulfonic acid.
And 2) heating the acid-proof reactor in the full reaction process to ensure that the manganese powder and the phosphoric acid are completely reacted, wherein the heating temperature is 25-80 ℃.
And 3) adding the lithium source solution in a stirring, atomizing and adding manner.
The heating temperature of the acid-proof reactor is 35-60 ℃.
The heating mode of the acid-proof reactor is oil bath, or water bath, or steam, or far infrared, or electric heating.
The invention has the beneficial effects that: 1) compared with the prior art, the pollution-free low-cost lithium manganese iron phosphate crystal material obtained by the technical scheme has the advantages that the overall level of the material at the present stage is effectively improved, the synthesis cost is very low, and the raw materials are wide in source, non-toxic and cheap in price;
2) the product quality of the existing process is not good integrally, the environment is polluted, a large amount of waste water and waste gas are discharged, the energy consumption is high (350 cubic carbon dioxide, ammonia, oxycarbide and nitric oxide are discharged when 1 ton of products are produced by a solid phase method, the energy consumption of high-energy ball milling is also very high, the power is more than 200 KW/hour), and the cost is high, the process adopted by the invention can change the condition, and the process is environment-friendly and pollution-free;
3) the solid-phase method is difficult to produce qualified lithium manganese iron phosphate, 3 times of lithium hydroxide and ferric manganese salt are required to be added in the traditional hydrothermal method, the recovery is difficult, the pollution is caused, the price of the lithium source is increased for a long time, and the synthesis cost is increased;
4) the lithium iron manganese phosphate prepared by the method has good electrochemical performance, and the particle size is in nano normal distribution;
5) the manganese lithium iron phosphate prepared by the invention has the charge of 162mah/g, the discharge of 151mah/g and the 1C discharge of 148 mah/g, and the true density of the material is as high as 4.0g/cm3，The method has the advantages of stable and consistent batch, good rate discharge performance and good processing performance, can meet the higher requirements of power batteries on the anode material, and effectively improves the energy density of the anode material.
Drawings
The technical features of the present invention will be further described with reference to the accompanying drawings and examples.
Fig. 1 is a morphology diagram of lithium iron manganese phosphate in the invention under an electron microscope.
Fig. 2 is a particle size distribution diagram of lithium manganese iron phosphate in the present invention.
Fig. 3 is an XRD pattern of lithium manganese iron phosphate in the present invention.
Detailed Description
Example one
A preparation process of a pollution-free low-cost lithium iron manganese phosphate crystal material comprises the following steps:
1) mixing iron powder, manganese powder and phosphoric acid according to a molar ratio of 0.3: 0.7: 1, weighing, wherein the diluted concentration of phosphoric acid is 40%;
2) adding the substances weighed in the step 1) into an acid-resistant reactor, controlling the temperature of a reaction system to be 30 ℃, introducing oxygen, starting pre-reaction, and reacting for 24 hours;
3) and 2) adding a lithium hydroxide solution after the reaction is finished, wherein the lithium hydroxide and the phosphoric acid are added according to the proportion of 1: 1, mixing, transferring the precursor into an autoclave after uniform mixing, and carrying out closed reaction, wherein the temperature in the synthesis process is 120-260 ℃, the pressure of the autoclave is 0.2-4.7MPa, the whole reaction process is continuously dispersed and stirred, the reaction time is controlled to be 3-24 hours, the temperature rise rate is controlled to be 1-10 ℃/min, and the temperature reduction rate is controlled to be 1-20 ℃/min;
4) after the hydrothermal reaction in the step 3) is finished, allowing the lithium iron manganese phosphate crystals to nucleate and crystallize and grow, then cooling, taking out of the kettle, carrying out solid-liquid separation, and drying at low temperature or in vacuum;
5) subjecting the precursor obtained in step 4) to inclusion carbonization annealing treatment (refer to patent: ZL 201410141267.2), the annealing temperature is about 800 ℃, the heat preservation time is 24 hours, and inert protective gas is introduced to prepare the lithium iron manganese phosphate crystal material.
Example two
A preparation process of a pollution-free low-cost lithium iron manganese phosphate crystal material comprises the following steps:
1) mixing iron powder, manganese powder and phosphoric acid according to a molar ratio of 0.5: 0.5: 1-1.2, and the diluted concentration of phosphoric acid is 35 percent;
2) adding the materials weighed in the step 1) into an acid-resistant reactor, controlling the temperature of a reaction system to be 25-80 ℃, introducing oxygen, and starting pre-reaction for 18 hours;
3) and 2) adding a lithium hydroxide solution after the reaction is finished, wherein the lithium hydroxide and the phosphoric acid are mixed according to the weight ratio of 1-1.2: 1, mixing, transferring the precursor into an autoclave after uniform mixing, and carrying out closed reaction, wherein the temperature in the synthesis process is 120-260 ℃, the pressure of the autoclave is 0.2-4.7MPa, the whole reaction process is continuously dispersed and stirred, the reaction time is controlled to be 3-24 hours, the temperature rise rate is controlled to be 1-10 ℃/min, and the temperature reduction rate is controlled to be 1-20 ℃/min;
4) after the hydrothermal reaction in the step 3) is finished, allowing the lithium iron manganese phosphate crystals to nucleate and crystallize and grow, then cooling, taking out of the kettle, carrying out solid-liquid separation, and drying at low temperature or in vacuum;
5) subjecting the precursor obtained in step 4) to inclusion carbonization annealing treatment (refer to patent No.: ZL 201410141267.2), the annealing temperature is about 800 ℃, the heat preservation time is 24 hours, and inert protective gas is introduced to prepare the lithium iron manganese phosphate crystal material.
EXAMPLE III
A preparation process of a pollution-free low-cost lithium iron manganese phosphate crystal material comprises the following steps:
1) mixing iron powder, manganese powder and phosphoric acid according to a molar ratio of 0.4: 0.6: 1-1.2, and the diluted concentration of phosphoric acid is 30 percent;
2) adding the materials weighed in the step 1) into an acid-resistant reactor, controlling the temperature of a reaction system to be 25-80 ℃, introducing oxygen, and starting pre-reaction for 18 hours;
3) and 2) adding a lithium hydroxide solution after the reaction is finished, wherein the lithium hydroxide and the phosphoric acid are mixed according to the weight ratio of 1-1.2: 1, mixing, transferring the precursor into an autoclave after uniform mixing, and carrying out closed reaction, wherein the temperature in the synthesis process is 120-260 ℃, the pressure of the autoclave is 0.2-4.7MPa, the whole reaction process is continuously dispersed and stirred, the reaction time is controlled to be 3-24 hours, the temperature rise rate is controlled to be 1-10 ℃/min, and the temperature reduction rate is controlled to be 1-20 ℃/min;
4) after the hydrothermal reaction in the step 3) is finished, allowing the lithium iron manganese phosphate crystals to nucleate and crystallize and grow, then cooling, taking out of the kettle, carrying out solid-liquid separation, and drying at low temperature or in vacuum;
5) subjecting the precursor obtained in step 4) to inclusion carbonization annealing treatment (refer to patent No.: ZL 201410141267.2), the annealing temperature is about 800 ℃, the heat preservation time is 24 hours, and inert protective gas is introduced to prepare the lithium iron manganese phosphate crystal material.
Example four
A preparation process of a pollution-free low-cost lithium iron manganese phosphate crystal material comprises the following steps:
1) mixing iron powder, manganese powder and phosphoric acid according to a molar ratio of 0.2: 0.8: 1-1.2, and the diluted concentration of phosphoric acid is 25 percent;
2) adding the materials weighed in the step 1) into an acid-resistant reactor, controlling the temperature of a reaction system to be 25-80 ℃, introducing oxygen, starting pre-reaction, and reacting for 20 hours;
3) and 2) adding a lithium hydroxide solution after the reaction is finished, wherein the lithium hydroxide and the phosphoric acid are mixed according to the weight ratio of 1-1.2: 1, mixing, transferring the precursor into an autoclave after uniform mixing, and carrying out closed reaction, wherein the temperature in the synthesis process is 120-260 ℃, the pressure of the autoclave is 0.2-4.7MPa, the whole reaction process is continuously dispersed and stirred, the reaction time is controlled to be 3-24 hours, the temperature rise rate is controlled to be 1-10 ℃/min, and the temperature reduction rate is controlled to be 1-20 ℃/min;
4) after the hydrothermal reaction in the step 3) is finished, allowing the lithium iron manganese phosphate crystals to nucleate and crystallize and grow, then cooling, taking out of the kettle, carrying out solid-liquid separation, and drying at low temperature or in vacuum;
5) subjecting the precursor obtained in step 4) to inclusion carbonization annealing treatment (refer to patent No.: ZL 201410141267.2), the annealing temperature is about 800 ℃, the heat preservation time is 24 hours, and inert protective gas is introduced to prepare the lithium iron manganese phosphate crystal material.
The manganese lithium iron phosphate prepared by the invention has good electrochemical performance, the particle size is in nano normal distribution, and the method can be obtained by referring to the attached figure 2.
Referring to fig. 3, the XRD chart of lithium manganese iron phosphate in the present invention is a qualitative x-ray spectrum analysis chart, which can prove that this material is lithium manganese iron phosphate.
The above description is only a preferred embodiment of the present invention, and the above specific embodiments are not intended to limit the present invention, and modifications, modifications or equivalents thereof, which may occur to those skilled in the art, are included within the scope of the present invention.
Claims (2)
1. A process for preparing the pollution-free low-cost lithium iron manganese phosphate crystal material with the chemical formula of LiFe(1-x)MnxPO4，Wherein x is more than or equal to 0.05 and less than or equal to 0.8, x represents an atomic ratio or a molar ratio, when x is less than 0.05, the main phase is lithium iron phosphate, a high-voltage platform is hardly exerted, and when x is more than 0.8, the electrochemical performance of the lithium iron phosphate is rapidly deteriorated through repeated tests, and the lithium iron phosphate electrochemical device is characterized in that: the reaction equation of the preparation process is
Fe+Mn+H3PO4+LiOH→LiFe(1-X)MnXPO4+H2 +H2O，
Wherein Fe represents iron powder, Mn represents manganese powder, H3PO4Representing phosphoric acid, LiOH representing a lithium hydroxide solution,
the preparation process comprises the following steps:
1) selecting high-purity iron powder and manganese powder, selecting the granularity of 20-20000 meshes, wherein the selected granularity range can ensure that the reaction speed is moderate, the control is easy, and the reaction is too violent and difficult to control when the granularity is too fine; the selected iron powder and manganese powder are treated by electrolysis, reduction or atomization process before reaction;
2) according to the proportion of Fe: mn: h3PO4: LiOH = (1-x): x: 1: (1.01-1.1) weighing iron powder, manganese powder, phosphoric acid and lithium source solution according to the mass ratio, diluting the iron powder, the manganese powder and the phosphoric acid, then placing the diluted iron powder, the diluted manganese powder and the diluted phosphoric acid into an acid-resistant reactor, stirring the diluted iron powder, the diluted manganese powder and the diluted phosphoric acid to fully react, heating the acid-resistant reactor to fully react the manganese powder and the phosphoric acid, wherein the heating temperature is 25-80 ℃, and the reaction time is 5-24 hours; in the full reaction process, introducing oxidizing gas with the effect of improving the reaction rate, wherein the oxidizing gas is air, oxygen or ozone; adding organic acid with the effect of accelerating reaction balance, wherein the adding proportion is 0.1-1, and the organic acid is citric acid, or acetic acid, or sulfonic acid;
3) adding a lithium source solution into the reaction precursor slurry obtained in the step 2), and fully and uniformly stirring, wherein the selected lithium source solution is soluble lithium source lithium hydroxide; adding a lithium source solution in a stirring and atomizing manner;
4) transferring the slurry obtained in the step 3) into a reaction kettle, and starting hydrothermal reaction at the temperature of 160-;
5) and (3) carrying out solid-liquid separation on the slurry obtained after the hydrothermal reaction in the step 4), carrying out inclusion carbonization annealing treatment on the separated solid lithium manganese iron phosphate, introducing inert gas for protection or selecting vacuum during annealing, wherein the annealing temperature is 550-850 ℃, and the annealing time is 3-24 hours, so as to obtain the lithium manganese iron phosphate crystal material.
2. The preparation process of the pollution-free low-cost lithium iron manganese phosphate crystal material according to claim 1, characterized by comprising the following steps: the heating temperature of the acid-proof reactor is 35-60 ℃; the heating mode of the acid-proof reactor is oil bath, or water bath, or steam, or far infrared, or electric heating.
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