CN110316711A - A kind of method that liquid phase method prepares lithium iron phosphate positive material presoma - Google Patents
A kind of method that liquid phase method prepares lithium iron phosphate positive material presoma Download PDFInfo
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- CN110316711A CN110316711A CN201910454079.8A CN201910454079A CN110316711A CN 110316711 A CN110316711 A CN 110316711A CN 201910454079 A CN201910454079 A CN 201910454079A CN 110316711 A CN110316711 A CN 110316711A
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- Prior art keywords
- iron phosphate
- positive material
- phosphate positive
- lithium iron
- material presoma
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of methods that liquid phase method prepares lithium iron phosphate positive material presoma, are related to technical field of powdered material preparation, comprising the following steps: lithium carbonate is carried out carbonic acid hydrogenation, obtains lithia water；Carbon source, hypophosphite monohydrate iron are added in lithium hydrogen phosphate solution, stirring obtains mixed liquor；Mixed liquor is evaporated to get lithium iron phosphate positive material presoma.The present invention can be achieved hypophosphite monohydrate iron and overcome the disadvantages of process flow in traditional preparation process is long, raw material mixing is not uniform enough, energy consumption is high without carrying out drying calcining to hypophosphite monohydrate iron material to the continuous production of LiFePO4, reduce production cost.This method simple process can be continuously produced and easy to operate, can prepare uniformly mixed lithium iron phosphate positive material presoma, and can farthest retain the granule-morphology of raw material, reduces and reunites.
Description
Technical field
The present invention relates to technical field of powdered material preparation more particularly to a kind of liquid phase method to prepare lithium iron phosphate positive material
The method of presoma.
Background technique
With the rapid development of society, the development of high energy consumption industry rapidly depletes traditional resource, problem of environmental pollution
At social concern urgently to be resolved, the new energy for finding environmental protection and low energy consumption becomes particularly important.Lithium ion battery is as one
The high performance secondary green battery of kind, more other conventional batteries, prominent feature mainly have: height storage energy density, long use
Cycle life, high voltage-rated, high power endurance, low self-discharge rate, high/low temperature are adaptable, fill from heavy and light and high current
Electric discharge etc..
On July 31st, 2017, national Ministry of Industry and Information have issued the 7th of " new-energy automobile, which promotes and applies, recommends vehicle catalogue "
Criticize content augmentation.According to statistics, 1-7 batch lithium ion batteries have voltage high, and energy density is big, recommend to share in catalogue 1939 sections it is pure
Electric vehicle is selected.According to mating battery statistics, LiFePO4 shares 1066 sections and is sure to occupy first, and accounting 55%, ternary lithium battery is total to
Have followed by 631 sections, accounting 32%, 157 sections of accountings 8% of LiMn2O4, lithium titanate and unknown lithium battery distinguish 3% He of accounting
2%.It is increasingly weighed there is some evidence that ferric phosphate lithium cell plays in China's energy-saving and emission-reduction, innovation energy reform
The effect wanted.
Traditional high temperature solid phase synthesis generally presses LiFePO4The atomic ratio of molecular formula carries out ingredient, obtains phosphorus after ball milling
The presoma of sour iron lithium anode material, by presoma, the heating in protective atmosphere (nitrogen or argon gas), can obtain LiFePO after cooling4
Powder body material.Solid-phase ball milling method prepares lithium iron phosphate positive material presoma and needs that hypophosphite monohydrate iron sample is first dried calcining,
Process flow is long, and energy consumption is high.And liquid phase method prepares lithium iron phosphate positive material presoma and allows continuous production, without to phosphorus
Sour iron is handled, and stock dispersion is more preferable in the liquid phase, and mixing is more uniform, and the presoma obtained in this way is made after sintering
Standby LiFePO4 consistency out more, while also saving cost.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of liquid phase methods to prepare lithium iron phosphate positive material
The method of presoma, it can be achieved that hypophosphite monohydrate iron to lithium iron phosphate positive material presoma continuous production, and simple process, at
This is lower.
The invention proposes a kind of methods that liquid phase method prepares lithium iron phosphate positive material presoma, comprising the following steps:
S1, lithium carbonate is subjected to carbonic acid hydrogenation, obtains lithia water；
S2, carbon source, hypophosphite monohydrate iron are added in lithium hydrogen phosphate solution, stirring obtains mixed liquor；
S3, mixed liquor is evaporated to get lithium iron phosphate positive material presoma.
Preferably, in S1, lithium carbonate carries out carbonic acid hydrogenation, and specific step is as follows: lithium carbonate is added to deionization
In water, it is passed through CO thereto2Gas, stirring make it carry out hydrogenation, and lithia water is made.
Preferably, in S1, in carbonic acid hydrogenation, the solid-liquid mass ratio of lithium carbonate and deionized water is 1:20~30, excellent
It is selected as 1:25.
Preferably, in S1, in carbonic acid hydrogenation, CO2The flow velocity of gas is 1~5L/min；Preferably 3L/min.
Preferably, in S1, in carbonic acid hydrogenation, reaction temperature is 15~25 DEG C, and the reaction time is 1~3h.
Preferably, in S2, the molar ratio of hypophosphite monohydrate iron, lithium carbonate and carbon source is 1:1.03~1.05:0.15~0.2.
Preferably, in S2, carbon source is glucose, sucrose, citric acid, any one in urea.
Preferably, it in S3, carries out being evaporated processing using rotary evaporator, rotating evaporation temperature is 60~80 DEG C.
Lithium iron phosphate positive material is prepared using the above-mentioned lithium iron phosphate positive material presoma being prepared, step is such as
Under: above-mentioned lithium iron phosphate positive material presoma is transferred in quartz boat and is placed in tube furnace, in high-purity N2Under protection, with
The heating rate of 4 DEG C/min is warming up to 350 DEG C, keeps the temperature 4h, is then warming up to 700 DEG C with 2 DEG C/min, keeps the temperature 10h, natural cooling
To room temperature, lithium iron phosphate positive material LiFePO is obtained4/ C sample.
The utility model has the advantages that the invention proposes a kind of method that liquid phase method prepares lithium iron phosphate positive material presoma, it can be real
The continuous production of existing hypophosphite monohydrate iron to LiFePO4 overcomes tradition without carrying out drying calcining to hypophosphite monohydrate iron material
The disadvantages of process flow is long in preparation process, raw material mixing is not uniform enough, energy consumption is high, reduces production cost.This method technique
Simply, it can be continuously produced and easy to operate, uniformly mixed lithium iron phosphate positive material presoma can be prepared, and can be maximum
Retain to degree the granule-morphology of raw material, reduces and reunite.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of the lithium iron phosphate positive material presoma prepared in the embodiment of the present invention 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of the lithium iron phosphate positive material presoma prepared in the embodiment of the present invention 2；
Fig. 3 is the x-ray diffraction pattern of the lithium iron phosphate positive material prepared in the embodiment of the present invention 1；
Fig. 4 is the x-ray diffraction pattern of the lithium iron phosphate positive material prepared in the embodiment of the present invention 2；
Fig. 5 is that the lithium iron phosphate positive material prepared in Example 1 and Example 2 of the present invention fills performance map again；
Fig. 6 is that the lithium iron phosphate positive material prepared in Example 1 and Example 2 of the present invention puts performance map again；
Fig. 7 is the normal-temperature circulating performance figure of the lithium iron phosphate positive material prepared in Example 1 and Example 2 of the present invention.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
S1,100g lithium carbonate is weighed, deionized water is added by solid-liquid mass ratio 1:25, is passed through CO2Gas (flow velocity 3L/
Min), controlled at 25 DEG C, being stirred to react 2h hydrogenates lithium carbonate, obtains lithia water；
S2, according to Iron phosphate (FePO4) dihydrate, lithium carbonate, glucose molar ratio be 1:1.03:0.2, weigh two hypophosphite monohydrates
Iron 245.47g, glucose 47.3g；First glucose is added in lithia water and stirs 30min, adds two hypophosphite monohydrates
Iron stirs 60min, obtains mixed liquor；
S3, it mixed liquor is transferred in rotary evaporator is evaporated to obtain lithium iron phosphate positive material presoma at 70 DEG C；
S4, it lithium iron phosphate positive material presoma is transferred in quartz boat is placed in tube furnace, in high-purity N2Protection
Under, 350 DEG C are warming up to the heating rate of 4 DEG C/min, keeps the temperature 4h, is then warming up to 700 DEG C with 2 DEG C/min, keeps the temperature 10h, from
It is so cooled to room temperature, obtains LiFePO4/C sample, be denoted as LFP-1.
Embodiment 2
S1,100g lithium carbonate is weighed, deionized water is added by solid-liquid mass ratio 1:25, is passed through CO2Gas (flow velocity 3L/
Min), controlled at 25 DEG C, being stirred to react 2h hydrogenates lithium carbonate, obtains lithia water；
S2, according to Iron phosphate (FePO4) dihydrate, lithium carbonate, sucrose molar ratio be 1:1.03:0.1, weigh Iron phosphate (FePO4) dihydrate
245.47g, sucrose 45.0g；First sucrose is added in lithia water and stirs 30min, adds Iron phosphate (FePO4) dihydrate, is stirred
60min obtains mixed liquor；
S3, it mixed liquor is transferred in rotary evaporator is evaporated to obtain lithium iron phosphate positive material presoma at 70 DEG C；
S4, it lithium iron phosphate positive material presoma is transferred in quartz boat is placed in tube furnace, in high-purity N2Protection
Under, 350 DEG C are warming up to the heating rate of 4 DEG C/min, keeps the temperature 4h, is then warming up to 700 DEG C with 2 DEG C/min, keeps the temperature 10h, from
It is so cooled to room temperature, obtains LiFePO4/ C sample, is denoted as LFP-2.
Embodiment 3
S1,100g lithium carbonate is weighed, deionized water is added by solid-liquid mass ratio 1:20, is passed through CO2Gas (flow velocity 1L/
Min), controlled at 15 DEG C, being stirred to react 1h hydrogenates lithium carbonate, obtains lithia water；
S2, according to Iron phosphate (FePO4) dihydrate, lithium carbonate, citric acid molar ratio be 1:1.03:0.15, weigh two hypophosphite monohydrates
Iron 245.47g, citric acid 37.87g；First citric acid is added in lithia water and stirs 30min, adds two hypophosphite monohydrates
Iron stirs 60min, obtains mixed liquor；
S3, it mixed liquor is transferred in rotary evaporator is evaporated to obtain lithium iron phosphate positive material presoma at 60 DEG C；
S4, it lithium iron phosphate positive material presoma is transferred in quartz boat is placed in tube furnace, in high-purity N2Protection
Under, 350 DEG C are warming up to the heating rate of 4 DEG C/min, keeps the temperature 4h, is then warming up to 700 DEG C with 2 DEG C/min, keeps the temperature 10h, from
It is so cooled to room temperature, obtains LiFePO4/ C sample.
Embodiment 4
S1,100g lithium carbonate is weighed, deionized water is added by solid-liquid mass ratio 1:30, is passed through CO2Gas (flow velocity 5L/
Min), controlled at 25 DEG C, being stirred to react 3h hydrogenates lithium carbonate, obtains lithia water；
S2, according to Iron phosphate (FePO4) dihydrate, lithium carbonate, urea molar ratio be 1:1.05:0.2, weigh Iron phosphate (FePO4) dihydrate
240.80g, urea 15.48g；First urea is added in lithia water and stirs 30min, Iron phosphate (FePO4) dihydrate is added, stirs
60min is mixed, mixed liquor is obtained；
S3, it mixed liquor is transferred in rotary evaporator is evaporated to obtain lithium iron phosphate positive material presoma at 80 DEG C；
S4, it lithium iron phosphate positive material presoma is transferred in quartz boat is placed in tube furnace, in high-purity N2Protection
Under, 350 DEG C are warming up to the heating rate of 4 DEG C/min, keeps the temperature 4h, is then warming up to 700 DEG C with 2 DEG C/min, keeps the temperature 10h, from
It is so cooled to room temperature, obtains LiFePO4/ C sample.
To lithium iron phosphate positive material presoma and lithium iron phosphate positive material the carry out table prepared in the embodiment of the present invention
Sign is as a result as follows.
Fig. 1 and Fig. 2 is respectively the scanning electron microscope (SEM) photograph of the lithium iron phosphate positive material presoma prepared in Examples 1 and 2.From
It is equal that lithium compound is generated as can be seen that lithium carbonate uniformly mixes after being hydrogenated to lithium bicarbonate with hypophosphite monohydrate iron in figure, after being evaporated
It is even to be dispersed in around hypophosphite monohydrate iron.
Fig. 3 and Fig. 4 is respectively the x-ray diffraction pattern of the lithium iron phosphate positive material prepared in Examples 1 and 2.From figure
It can be seen that the LiFePO4/C sample that the presoma that liquid phase method is prepared is prepared after sintering is pure phase LiFePO4.
Fig. 5 is that the lithium iron phosphate positive material prepared in Example 1 and Example 2 of the present invention fills performance map again.From figure
In it can be seen that under 5C multiplying power constant current pour than being still greater than 92%, fill have excellent performance again.
Fig. 6 is that the lithium iron phosphate positive material prepared in Example 1 and Example 2 of the present invention puts performance map again.From figure
In it can be seen that in 5C multiplying power discharge capacity conservation rate be still greater than 95%, put have excellent performance again.
Fig. 7 is the normal-temperature circulating performance figure of the lithium iron phosphate positive material prepared in Example 1 and Example 2 of the present invention.
As can be seen from the figure 800 weeks LFP-1 capacity retention ratios are recycled under 1C multiplying power is remained above 90% greater than 94%, LFP-2 capacity；
The two comparison LFP-1 cycle performance is better than LFP-2.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of method that liquid phase method prepares lithium iron phosphate positive material presoma, which comprises the following steps:
S1, lithium carbonate is subjected to carbonic acid hydrogenation, obtains lithia water；
S2, carbon source, hypophosphite monohydrate iron are added in lithium hydrogen phosphate solution, stirring obtains mixed liquor；
S3, mixed liquor is evaporated to get lithium iron phosphate positive material presoma.
2. the method that liquid phase method according to claim 1 prepares lithium iron phosphate positive material presoma, which is characterized in that S1
In, lithium carbonate carries out carbonic acid hydrogenation, and specific step is as follows: lithium carbonate being add to deionized water, is passed through thereto
CO2Gas, stirring make it carry out hydrogenation, and lithia water is made.
3. the method that liquid phase method according to claim 1 or 2 prepares lithium iron phosphate positive material presoma, feature exist
In in S1, in carbonic acid hydrogenation, the solid-liquid mass ratio of lithium carbonate and deionized water is 1:20~30, preferably 1:25.
4. the method that liquid phase method according to claim 1 or 2 prepares lithium iron phosphate positive material presoma, feature exist
In, in S1, in carbonic acid hydrogenation, CO2The flow velocity of gas is 1~5L/min；Preferably 3L/min.
5. the method that liquid phase method according to claim 1 or 2 prepares lithium iron phosphate positive material presoma, feature exist
In in S1, in carbonic acid hydrogenation, reaction temperature is 15~25 DEG C, and the reaction time is 1~3h.
6. the method that liquid phase method according to claim 1 prepares lithium iron phosphate positive material presoma, which is characterized in that S2
In, the molar ratio of hypophosphite monohydrate iron, lithium carbonate and carbon source is 1:1.03~1.05:0.15~0.2.
7. the method that liquid phase method according to claim 1 or 6 prepares lithium iron phosphate positive material presoma, feature exist
In in S2, carbon source is glucose, sucrose, citric acid, any one in urea.
8. the method that liquid phase method according to claim 1 prepares lithium iron phosphate positive material presoma, which is characterized in that S3
In, it carries out being evaporated processing using rotary evaporator, rotating evaporation temperature is 60~80 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111403725A (en) * | 2020-04-24 | 2020-07-10 | 山东精工电子科技有限公司 | Aluminum oxide coated hafnium/nitrogen co-doped lithium iron phosphate cathode material and preparation method thereof |
| CN114180547A (en) * | 2021-12-31 | 2022-03-15 | 常州锂源新能源科技有限公司 | Preparation method of low-cost high-power lithium iron phosphate |
| CN115583642A (en) * | 2022-10-25 | 2023-01-10 | 西安合升汇力新材料有限公司 | LiFe x Mn y D z PO 4 @ C and preparation and application of precursor thereof |
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| CN111403725A (en) * | 2020-04-24 | 2020-07-10 | 山东精工电子科技有限公司 | Aluminum oxide coated hafnium/nitrogen co-doped lithium iron phosphate cathode material and preparation method thereof |
| CN114180547A (en) * | 2021-12-31 | 2022-03-15 | 常州锂源新能源科技有限公司 | Preparation method of low-cost high-power lithium iron phosphate |
| CN115583642A (en) * | 2022-10-25 | 2023-01-10 | 西安合升汇力新材料有限公司 | LiFe x Mn y D z PO 4 @ C and preparation and application of precursor thereof |
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