CN102903897A - Method for preparing nickel lithium manganate having spinel structure by static mixer type reactor - Google Patents
Method for preparing nickel lithium manganate having spinel structure by static mixer type reactor Download PDFInfo
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- CN102903897A CN102903897A CN2012102538289A CN201210253828A CN102903897A CN 102903897 A CN102903897 A CN 102903897A CN 2012102538289 A CN2012102538289 A CN 2012102538289A CN 201210253828 A CN201210253828 A CN 201210253828A CN 102903897 A CN102903897 A CN 102903897A
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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a method for preparing nickel lithium manganate (LiN0.5Mn1.5O4) having a spinel structure by a static mixer type reactor, which comprises the following steps: a mixing solution of a nickel source and a manganese source as well as a carbonate solution is placed according to equal volume flow from one end of the static mixer type reactor, a liquid phase mixing reaction is carried out in the static mixer type reactor to generate an emulsion, the emulsion is aged and a membrane is washed to remove the impurity ion, and a nickel manganese composite carbonate precursor powder is obtained through spray drying, the precursor powder is coasted at the temperature of 400-500 DEG C for 5-10 hours to obtain a nickel manganese composite oxide, the lithium source is added in the nickel manganese composite oxide according to mol ratio of Li<+> to Ni<2+> to Mn<4+> being 1.05: 0.5: 1.5, and performing ball milling and uniformly mixing, and sintering at the temperature of 800-950 DEG C for 8-15 hours to obtain the finished product. The obtained material has the advantages of pure phase, good crystallization, small particle size, narrow particle size distribution and low raw material price, the technology is simple and a continuous industrial production is easy to be carried out, 0.2C initial discharge specific capacity can reach 130mAh/g, and 0.5C multiplying power 50 times circulation capacity maintenance rate is more than 98%.
Description
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries, relate in particular to a kind of method of utilizing static mixing tubular type reactor to prepare the nickel lithium manganate material, belong to the battery material preparing technical field.
Background technology
Spinel lithium manganate has the plurality of advantages such as toxicity is little, cost is low, the raw material wide material sources, and application prospect is good as the positive electrode of lithium ion battery.But pure LiMn
2O
4Chemical property is unsatisfactory, and the first charge-discharge capacity is low, the defective such as non-refractory, capacity attenuation are fast.Nickel doped spinel LiNi wherein
0.5Mn
1.5O
4Show excellent chemical property, relatively pure LiMn
2O
4, spinelle LiNi
0.5Mn
1.5O
4Have current potential platform high (4.7V), specific power is large, and crystal structure is stable, the advantages such as good cycle.
Present nickel LiMn2O4 (LiNi
0.5Mn
1.5O
4) the many people in synthetic aspect done a large amount of work.For example solid phase is synthetic is common method, and this method advantage is that technique is simple, easily realizes industrialization, but owing to reactant is difficult for mixing, the large and skewness of the particle diameter of product, pattern is irregular, therefore has batch problem of stability deficiency.Sol-gel process precursor solution chemical uniformity good (can reach the molecular level level), the Gel heat-treatment temperature is low, powder granularity is little and narrowly distributing, the powder sintering performance is good, and course of reaction is easy to control, but dry the contraction greatly, the industrialization difficulty is high, and the production cycle is long.Ultrasonic spray pyrolysis can obtain preferably electrical property material, but needs reative cell to have high temperature more than 500 ℃, and equipment requirement is high, is difficult to suitability for industrialized production.Traditional liquid-phase coprecipitation adopts tank reactor to be operating as the master with batch process usually; because the reaction mass amount is restricted; course of reaction is lasting; be unfavorable for large-scale production; and be accompanied by the carrying out of course of reaction; reaction condition (such as concentration, pH value) constantly changes, and has affected micro mist grain size size and has distributed.
Summary of the invention
The objective of the invention is to be to overcome the deficiencies in the prior art, provide a kind of the utilization can reach that microcosmic mixes and the static mixing tubular type reactor of boosting productivity carries out the liquid phase pipe reaction to the mixed solution of nickel source, manganese source compound with carbonate solution and synthesizes nickel manganese compound carbonate, will obtain nickel LiMn2O4 (LiNi with Li source compound mixing sintering again after its high-temperature calcination
0.5Mn
1.5O
4) method,
The present invention to achieve these goals adopts following technical scheme:
Static mixing tubular type reactor prepares spinel structure nickel LiMn2O4 (LiNi
0.5Mn
1.5O
4) method, may further comprise the steps:
(1) configuration concentration is 0.1～2mol/L nickel source solution and manganese source solution respectively, then with its mixing, is made into the question response solution A, and the mol ratio that requires nickel ion, manganese ion is 1:3; Configuration concentration is 0.2～4mol/L carbonate solution and ammonia spirit respectively, with its mixing, is made into the question response solution B;
(2) use respectively two charge pumps that the solution A in the step (1) and B are squeezed into from static mixing tubular type reactor one end by the equal-volume flow, carry out hybrid reaction and generate emulsion, by adjusting the amount of ammoniacal liquor in the B solution, the pH value of emulsion in the reactor is controlled between 8～11.
(3) behind the emulsion ageing 1～4h with step (2), carry out the slurry liquid that the film washing obtains dispelling foreign ion.
(4) obtain nickel manganese compound carbonate precursor powder after step (3) being dispelled the slurry liquid spray drying of foreign ion.
(5) with 400-500 ℃ of calcining of the precursor powder in the step (4) 5-10h, obtain the nickel manganese composite oxide.
(6) Li is pressed in the lithium source
+: Ni
2+: Mn
4+For the 1.05:0.5:1.5 mol ratio adds in the nickel manganese composite oxide, wherein the lithium source is excessive 5%, the ball milling mixing, and at 800-950 ℃ of sintering 8-15h, LiNi gets product
0.5Mn
1.5O
4
The nickel source compound is in the described step (1): a kind of or its mixture of nickelous sulfate, nickel nitrate, nickel chloride, nickel acetate.
The manganese source compound is in the described step (1): a kind of or its mixture of manganese sulfate, manganese nitrate, manganese chloride, manganese acetate.
Carbonate compound is in the described step (1): a kind of or its mixture of sodium carbonate, sodium acid carbonate, ammonium carbonate.
Volume flow is 0.1～5L/min in the described step (2).
Li source compound is in the described step (6): a kind of or its mixture of lithium carbonate, lithium acetate, lithium nitrate, lithium hydroxide.
The explanation of static mixing tubular type reactor:
The present invention utilizes static mixing tubular type reactor to prepare spinel structure nickel LiMn2O4 (LiNi
0.5Mn
1.5O
4) method.Static mixing tubular type reactor is that the material flow that wish is mixed is entered reactor along pipeline, material flow is under the kinetic energy effect of himself, pass through successively the specific channel of one group of left-and-right spiral element formation of alternative arrangement, the material that this moment, wish was mixed is forced to generation cutting and distortion, displacement and distortion, separates and merge, thereby realize mixing, carry out simultaneously in shunting action mode and footpath mutually immixture mode, and show as a kind of flow performance of approximate average piston flow pattern.
The invention has the beneficial effects as follows:
Resulting materials phase of the present invention is pure, the well-crystallized, and particle diameter is little, narrow particle size distribution, the prices of raw and semifnished materials are cheap, and technique is simple, be easy to the serialization industrial production, and the 0.2C first discharge specific capacity reaches 130mAh/g, 50 circulation volume conservation rates of 0.5C multiplying power are 98% with first-class advantage.
Description of drawings
Fig. 1 is static mixer screw element standard package figure;
A right-hand screw element among the figure, b left-hand screw element, c static mixer standard package;
Fig. 2 is shunting action figure in the static mixer;
Fig. 3 is embodiment 1 product X ray diffracting spectrum;
Fig. 4 is embodiment 1 product battery 0.2C charging, and 0.2C, 0.8C, 2C head are put capacity and voltage curve;
Fig. 5 is embodiment 1 product battery 0.5C cycle performance figure.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
(1) configuration concentration is the 0.1mol/L nickel sulfate solution, and concentration is the 0.1mol/L manganese sulfate solution, then with its mixing, is made into the question response solution A, and the mol ratio that requires nickel ion, manganese ion is 1:3; Carbonate 0.2mol/L solution and ammonia spirit with its mixing, are made into the question response solution B;
(2) use respectively two charge pumps that the solution A in the step (1) and B are squeezed into from static mixing tubular type reactor one end by 1L/min equal-volume flow, carry out hybrid reaction and generate emulsion, by adjusting the amount of ammoniacal liquor in the B solution, the pH value in the reactor is controlled between 8.5～9.5;
(3) behind the emulsion ageing 2h with step (2), carry out the slurry liquid that the film washing obtains dispelling foreign ion;
(4) obtain nickel manganese compound carbonate precursor powder after step (3) being dispelled the slurry liquid spray drying of foreign ion;
(5) with 450 ℃ of calcinings of the precursor powder in the step (4) 5h, obtain the nickel manganese composite oxide;
(6) lithium carbonate is pressed Li
+: Ni
2+: Mn
4+For the 1.05:0.5:1.5 mol ratio adds in the nickel manganese composite oxide, wherein the lithium source is excessive 5%, and the ball milling mixing at 900 ℃ of sintering 10h, gets product.
Fig. 3 is present embodiment product X-x ray diffraction collection of illustrative plates, and as can be seen from the figure, diffraction maximum is sharp-pointed, illustrates that the present embodiment product is single LiNi
0.5Mn
1.5O
4Phase, and the well-crystallized of product; Fig. 4 is that present embodiment product 0.2C first discharge specific capacity is 130.4mAh/g, and Fig. 5 is that 50 circulation volume conservation rates of present embodiment product 0.5C multiplying power are 98.7%.
Embodiment 2:
(1) configuration concentration is the 0.5mol/L nickel nitrate solution, and concentration is the 0.5mol/L manganese nitrate solution, then with its mixing, is made into the question response solution A, and the mol ratio that requires nickel ion, manganese ion is 1:3; Ammonium carbonate 1mol/L solution and ammonia spirit with its mixing, are made into the question response solution B;
(2) use respectively two charge pumps that the solution A in the step (1) and B are squeezed into from static mixing tubular type reactor one end by 2.5L/min equal-volume flow, carry out hybrid reaction and generate emulsion, by adjusting the amount of ammoniacal liquor in the B solution, the pH value in the reactor is controlled between 9.0～10.0;
(3) behind the emulsion ageing 2h with step (2), carry out the slurry liquid that the film washing obtains dispelling foreign ion;
(4) obtain nickel manganese compound carbonate precursor powder after step (3) being dispelled the slurry liquid spray drying of foreign ion;
(5) with 450 ℃ of calcinings of the precursor powder in the step (4) 7h, obtain the nickel manganese composite oxide;
(6) lithium nitrate is pressed Li
+: Ni
2+: Mn
4+For the 1.05:0.5:1.5 mol ratio adds in the nickel manganese composite oxide, wherein the lithium source is excessive 5%, and the ball milling mixing at 950 ℃ of sintering 8h, gets product.
Present embodiment product 0.2C first discharge specific capacity is 129.5mAh/g, and 50 circulation volume conservation rates of 0.5C multiplying power are 98.3%.
Embodiment 3:
(1) configuration concentration is the 1mol/L nickel chloride solution, and concentration is the 1mol/L manganese chloride solution, then with its mixing, is made into the question response solution A, and the mol ratio that requires nickel ion, manganese ion is 1:3; Sodium acid carbonate 4mol/L solution and ammonia spirit with its mixing, are made into the question response solution B;
(2) use respectively two charge pumps that the solution A in the step (1) and B are squeezed into from static mixing tubular type reactor one end by 5L/min equal-volume flow, carry out hybrid reaction and generate emulsion, by adjusting the amount of ammoniacal liquor in the B solution, the pH value in the reactor is controlled between 9.5～10.5;
(3) behind the emulsion ageing 2h with step (2), carry out the slurry liquid that the film washing obtains dispelling foreign ion;
(4) obtain nickel manganese compound carbonate precursor powder after step (3) being dispelled the slurry liquid spray drying of foreign ion;
(5) with 500 ℃ of calcinings of the precursor powder in the step (4) 10h, obtain the nickel manganese composite oxide;
(6) lithium hydroxide is pressed Li
+: Ni
2+: Mn
4+For the 1.05:0.5:1.5 mol ratio adds in the nickel manganese composite oxide, wherein the lithium source is excessive 5%, and the ball milling mixing at 850 ℃ of sintering 15h, gets product.
Present embodiment product 0.2C first discharge specific capacity is 130.2mAh/g, and 50 circulation volume conservation rates of 0.5C multiplying power are 98.8%.
Embodiment 4:
(1) configuration concentration is the 2mol/L nickel acetate solution, and concentration is 2mol/L manganese acetate solution, then with its mixing, is made into the question response solution A, and the mol ratio that requires nickel ion, manganese ion is 1:3; Sodium carbonate 4mol/L solution and ammonia spirit with its mixing, are made into the question response solution B;
(2) use respectively two charge pumps that the solution A in the step (1) and B are squeezed into from static mixing tubular type reactor one end by 5L/min equal-volume flow, carry out hybrid reaction and generate emulsion, by adjusting the amount of ammoniacal liquor in the B solution, the pH value in the reactor is controlled between 10.0～11.0;
(3) behind the emulsion ageing 2h with step (2), carry out the slurry liquid that the film washing obtains dispelling foreign ion;
(4) obtain nickel manganese compound carbonate precursor powder after step (3) being dispelled the slurry liquid spray drying of foreign ion.
(5) with 500 ℃ of calcinings of the precursor powder in the step (4) 10h, obtain the nickel manganese composite oxide;
(6) lithium acetate is pressed Li
+: Ni
2+: Mn
4+For the 1.05:0.5:1.5 mol ratio adds in the nickel manganese composite oxide, wherein the lithium source is excessive 5%, and the ball milling mixing at 900 ℃ of sintering 10h, gets product.
Present embodiment product 0.2C first discharge specific capacity is 129.4mAh/g, and 50 circulation volume conservation rates of 0.5C multiplying power are 98.5%.
Embodiment 5:
(1) configuration concentration is 0.8mol/L nickel sulfate solution, 0.8mol/L nickel nitrate solution, concentration is 0.8mol/L manganese sulfate solution, 0.8mol/L manganese nitrate solution, then with its mixing, be made into the question response solution A, the mol ratio that requires nickel ion, manganese ion is 1:3; Sodium carbonate 1.6mol/L solution and ammonia spirit with its mixing, are made into the question response solution B;
(2) use respectively two charge pumps that the solution A in the step (1) and B are squeezed into from static mixing tubular type reactor one end by 2.5L/min equal-volume flow, carry out hybrid reaction and generate emulsion, by adjusting the amount of ammoniacal liquor in the B solution, the pH value in the reactor is controlled between 9.5～10.5;
(3) behind the emulsion ageing 2h with step (2), carry out the slurry liquid that the film washing obtains dispelling foreign ion;
(4) obtain nickel manganese compound carbonate precursor powder after step (3) being dispelled the slurry liquid spray drying of foreign ion.
(5) with 500 ℃ of calcinings of the precursor powder in the step (4) 10h, obtain the nickel manganese composite oxide;
(6) lithium carbonate is pressed Li
+: Ni
2+: Mn
4+For the 1.05:0.5:1.5 mol ratio adds in the nickel manganese composite oxide, wherein the lithium source is excessive 5%, and the ball milling mixing at 900 ℃ of sintering 10h, gets product.
Present embodiment product 0.2C first discharge specific capacity is 130.47mAh/g, and 100 circulation volume conservation rates of 0.5C multiplying power are 98.2%.
Claims (6)
1. a static mixing tubular type reactor prepares spinel structure nickel LiMn2O4 (LiNi
0.5Mn
1.5O
4) method, it is characterized in that comprising following preparation process:
(1) configuration concentration is 0.1～2mol/L nickel source solution and manganese source solution respectively, then with its mixing, is made into the question response solution A, and the mol ratio that requires nickel ion, manganese ion is 1:3; Configuration concentration is 0.2～4mol/L carbonate solution and ammonia spirit respectively, with its mixing, is made into the question response solution B;
(2) use respectively two charge pumps that the solution A in the step (1) and B are squeezed into from static mixing tubular type reactor one end by the equal-volume flow, carry out hybrid reaction and generate emulsion, by adjusting the amount of ammoniacal liquor in the B solution, the pH value of emulsion in the reactor is controlled between 8～11;
(3) behind the emulsion ageing 1～4h with step (2), carry out the slurry liquid that the film washing obtains dispelling foreign ion;
(4) obtain nickel manganese compound carbonate precursor powder after the slurry liquid spray drying of dispelling foreign ion with step (3);
(5) with behind 400-500 ℃ of calcining of the precursor powder in the step (4) 5-10h, obtain the nickel manganese composite oxide;
(6) Li is pressed in the lithium source
+: Ni
2+: Mn
4+For the 1.05:0.5:1.5 mol ratio adds in the nickel manganese composite oxide, wherein the lithium source is excessive 5%, the ball milling mixing, and behind 800-950 ℃ of sintering 8-15h, LiNi gets product
0.5Mn
1.5O
4
2. static mixing tubular type reactor according to claim 1 prepares spinel structure nickel LiMn2O4 (LiNi
0.5Mn
1.5O
4) method, it is characterized in that nickel source compound is in (1): a kind of or its mixture of nickelous sulfate, nickel nitrate, nickel chloride, nickel acetate.
3. static mixing tubular type reactor according to claim 1 prepares spinel structure nickel LiMn2O4 (LiNi
0.5Mn
1.5O
4) method, it is characterized in that manganese source compound is in (1): a kind of or its mixture of manganese sulfate, manganese nitrate, manganese chloride, manganese acetate.
4. static mixing tubular type reactor according to claim 1 prepares spinel structure nickel LiMn2O4 (LiNi
0.5Mn
1.5O
4) method, it is characterized in that carbonate compound is in (1): a kind of or its mixture of sodium carbonate, sodium acid carbonate, ammonium carbonate.
5. static mixing tubular type reactor according to claim 1 prepares spinel structure nickel LiMn2O4 (LiNi
0.5Mn
1.5O
4) method, it is characterized in that volume flow is 0.1～5L/min in (2).
6. static mixing tubular type reactor according to claim 1 prepares spinel structure nickel LiMn2O4 (LiNi
0.5Mn
1.5O
4) method, it is characterized in that Li source compound is in (6): a kind of or its mixture of lithium carbonate, lithium acetate, lithium nitrate, lithium hydroxide.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103682323A (en) * | 2013-12-31 | 2014-03-26 | 湖南汇通科技有限责任公司 | Lithium nickel manganese oxide cathode material, precursor thereof and preparation method thereof |
| CN110316769A (en) * | 2019-07-23 | 2019-10-11 | 铜陵金泰电池材料有限公司 | A method of anode material for lithium-ion batteries is prepared based on static mixer device |
| EP3555941A4 (en) * | 2016-12-19 | 2020-08-19 | GRST International Limited | Method of preparing cathode material for secondary battery |
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| CN102163713A (en) * | 2011-03-17 | 2011-08-24 | 广州市香港科大***研究院 | Method for preparing high-voltage spinel anode material of lithium-ion secondary battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103682323A (en) * | 2013-12-31 | 2014-03-26 | 湖南汇通科技有限责任公司 | Lithium nickel manganese oxide cathode material, precursor thereof and preparation method thereof |
| EP3555941A4 (en) * | 2016-12-19 | 2020-08-19 | GRST International Limited | Method of preparing cathode material for secondary battery |
| US10903516B2 (en) | 2016-12-19 | 2021-01-26 | Grst International Limited | Method of preparing cathode material for secondary battery |
| CN110316769A (en) * | 2019-07-23 | 2019-10-11 | 铜陵金泰电池材料有限公司 | A method of anode material for lithium-ion batteries is prepared based on static mixer device |
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