CN103117386A - Method for determining manganese content of raw material manganese peroxide for synthesizing lithium manganese oxide spinel and raw material lithium carbonate/manganese peroxide ratio - Google Patents
Method for determining manganese content of raw material manganese peroxide for synthesizing lithium manganese oxide spinel and raw material lithium carbonate/manganese peroxide ratio Download PDFInfo
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- CN103117386A CN103117386A CN2013100468055A CN201310046805A CN103117386A CN 103117386 A CN103117386 A CN 103117386A CN 2013100468055 A CN2013100468055 A CN 2013100468055A CN 201310046805 A CN201310046805 A CN 201310046805A CN 103117386 A CN103117386 A CN 103117386A
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- manganese
- lithium
- manganese dioxide
- raw material
- lithium carbonate
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- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 title claims abstract description 331
- 239000011572 manganese Substances 0.000 title claims abstract description 157
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 title claims abstract description 138
- 229910052808 lithium carbonate Inorganic materials 0.000 title claims abstract description 138
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 115
- 238000000034 method Methods 0.000 title claims abstract description 108
- 239000002994 raw material Substances 0.000 title claims abstract description 93
- 239000011029 spinel Substances 0.000 title claims abstract description 82
- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 82
- 229910002102 lithium manganese oxide Inorganic materials 0.000 title abstract 4
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 title abstract 4
- 230000002194 synthesizing effect Effects 0.000 title abstract 4
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 claims abstract description 88
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 68
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 68
- 239000000126 substance Substances 0.000 claims abstract description 35
- 230000008569 process Effects 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 claims description 77
- 239000011010 synthetic spinel Substances 0.000 claims description 62
- OZOAXHQNOFIFGD-UHFFFAOYSA-N manganese(2+) oxygen(2-) Chemical compound [O-2].[O-2].[Mn+2].[Mn+2] OZOAXHQNOFIFGD-UHFFFAOYSA-N 0.000 claims description 34
- 238000006467 substitution reaction Methods 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 10
- 238000005259 measurement Methods 0.000 claims description 7
- 238000004088 simulation Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 description 20
- 238000001816 cooling Methods 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 230000009897 systematic effect Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229940072033 potash Drugs 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 229910000319 transition metal phosphate Inorganic materials 0.000 description 1
Classifications
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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
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a method for determining manganese content of raw material manganese peroxide for synthesizing lithium manganese oxide spinel and raw material lithium carbonate/manganese peroxide ratio, which comprises the following steps: deducing the relational expression of product lithium/manganese mol ratio and manganese content of raw material manganese peroxide according to the chemical reaction equation; setting reference manganese content of manganese peroxide and lithium/manganese reference mol ratio of the synthetic product, and deducing the theoretically required reference amounts of lithium carbonate and manganese peroxide; synthesizing the lithium manganese oxide spinel according to the reference amounts of lithium carbonate and manganese peroxide under fitted technological conditions, measuring the lithium manganate lithium/manganese actual mol ratio by an ICP method, and acquiring the actual manganese content of the manganese peroxide; and by using the lithium carbonate as the reference amount, the manganese content of the manganese peroxide as the actual manganese content and the lithium/manganese ratio of the lithium manganate as the reference mol ratio, synthesizing the lithium manganese oxide spinel, and calculating the actually required amount of manganese peroxide. The method can avoid the process system errors caused by the technical process and the measuring system errors caused by the conventional chemical method, is simple and convenient, has the advantages of high accuracy and high practicality, and can implement continuous operation.
Description
Technical field
The invention belongs to technical field of lithium ion, be specifically related to a kind of definite method of synthetic spinel LiMn2O4 raw material manganese dioxide manganese content and raw material lithium carbonate and manganese dioxide proportioning.
Background technology
Lithium ion battery have energy density high, have extended cycle life, the characteristics such as volume is little, lightweight, fail safe is good, be widely used in the power energy field such as the consumer goods electronic applications such as walkie electronic apparatus, digital camera, notebook computer and mobile communication and electric tool, electric bicycle, electric automobile.At present, the anode material for lithium-ion batteries of primary commercial use has: the lithium transition metal phosphate of lithium manganate having spinel structure, layer structure lithium transition-metal oxide and olivine structural etc.Wherein spinel lithium manganate due to thermal stability, rich in natural resources characteristic and the good fail safe of excellence, especially gets most of the attention.
The primary raw material of solid phase method industrialization synthetic spinel LiMn2O4 comprises as the lithium carbonate in lithium source with as the manganese dioxide (electrolytic manganese dioxide and chemical manganese bioxide) in manganese source, because there is multiple price in the oxide of manganese, as Mn
2+, Mn
3+, Mn
4+Deng, and the each side reason such as impurity content difference, in raw material, there is wave phenomenon in the manganese content of manganese oxide, directly has influence on the accuracy of raw material proportioning and product constituent content.Therefore, before synthetic LiMn2O4 and batching, need to accurately determine manganese content and the raw material proportioning of raw material manganese dioxide.
Traditional manganese dioxide manganese content test method, though be chemical analysis (as complexometry, titration etc.) or instrument test method (as ultraviolet spectrometer etc.), due to the reasons such as purity, consumption or instrument and equipment operating accuracy of analytical reagent, all there is larger systematic error.
In the process of solid phase method industrialization synthetic spinel LiMn2O4, the Li/Mn mol ratio of synthetic product is the important parameter that characterizes raw material distributing precision and product constituent content precision, is directly connected to the quality of LiMn2O4 product and the performance of lithium ion battery.The principal element that affects the Li/Mn mol ratio precision of synthetic product has:
(1) raw material ratio precision: exist larger systematic error, the systematic error of raw material lithium carbonate master assay all to have influence on the raw material distributing precision as raw material manganese dioxide manganese content test;
(2) building-up process process conditions: the systematic error that causes as the technical processs such as volatilization of the volatilization of impurity in building-up process, synthesis temperature, time, atmosphere, elemental lithium, also can considerable influence to the precision of Li/Mn mol ratio.
In the prior art, owing to having ignored the procedures system error that synthesis process brings, there is simultaneously larger measuring system mistake error, makes precision and the raw material distributing precision of the Li/Mn mol ratio of synthetic product be difficult to accurately determine and control.
Summary of the invention
The object of the present invention is to provide a kind of definite method of synthetic spinel LiMn2O4 raw material manganese dioxide manganese content and raw material lithium carbonate and manganese dioxide proportioning, by match synthetic spinel LiMn2O4, recently realize for the Li/Mn of Accurate Measurement synthetic product mole the accurate of raw material manganese dioxide manganese content and raw material proportioning determined, thereby realization is to the accurate control of synthetic product Li/Mn mol ratio.The procedures system error that the method has avoided technical process to bring, the measuring system error that also can avoid the measurement of conventional chemical method to bring simultaneously realizes accurately determining raw material manganese dioxide manganese content and raw material proportioning under the fit technique condition.
Above-mentioned purpose of the present invention is achieved by the following technical solution: a kind of definite method of synthetic spinel LiMn2O4 raw material manganese dioxide manganese content and raw material lithium carbonate and manganese dioxide proportioning contains following steps:
(1) take lithium carbonate as the lithium source, take manganese dioxide as the manganese source, the synthetic spinel LiMn2O4, the quality of setting lithium carbonate is x, the quality of manganese dioxide is y, manganese dioxide manganese content is a (w.t.%), in synthetic spinel lithium manganate, the mol ratio of lithium/manganese is b, lithium carbonate and manganese dioxide carry out chemical reaction according to following chemical formula, according to the mol ratio of lithium carbonate and manganese dioxide, the relation formula that draws between the mol ratio b of lithium/manganese in manganese dioxide manganese content a and spinel lithium manganate is: a * b=1.487 (xu%/y)
Wherein: u% is the quality percentage composition of raw material lithium carbonate, wherein u% 〉=99.5%; As a rule, u% can reach 99.5% can satisfy raw materials requirement, if but the content of u% is higher better, usually be set as constant;
M
1Be Li
2CO
3Molecular weight is 73.89;
M
2Being the atomic weight of Mn, is 54.938;
M
3Be Li
2bMn
2O
4Molecular weight calculates and gets depending on the b value;
X is the lithium carbonate quality;
Y is the manganese dioxide quality;
Z generates product quality for reaction, for setting constant;
(2) the benchmark manganese content of setting manganese dioxide is a
0(w.t.%), in spinel lithium manganate, the benchmark mol ratio of lithium/manganese is b
0, according to the chemical formula synthetic spinel LiMn2O4 in step (1), derive the benchmark consumption x of required in theory lithium carbonate
0, the benchmark consumption y of manganese dioxide
0, x wherein
0=(zb
0M
1)/(u%M
3), y
0=(2zM
2)/(a
0M
3);
(3) be x according to the lithium carbonate quality
0, the manganese dioxide quality is y
0, according to the chemical formula synthetic spinel LiMn2O4 in step (1), adopt the ICP method n the measurement of precision such as to carry out to the actual mol ratio of lithium/manganese in spinel lithium manganate, and get its statistics average data
Will
x
0And y
0, substitution relational expression a * b=1.487 (xu%/y) draws the actual manganese content of manganese dioxide
(4) keeping the lithium carbonate quality is x
0, the actual manganese content of manganese dioxide is a ', in spinel lithium manganate, the mol ratio of lithium/manganese is b
0, lithium carbonate and manganese dioxide are carried out chemical reaction according to the chemical formula in step (1), when generating spinel lithium manganate, according to relational expression a * b=1.487 (xu%/y), calculate the consumption y ' of the manganese dioxide of actual needs, y '=(1.487x
0U%)/(a ' * b
0); The actual amount proportioning of lithium carbonate and manganese dioxide is x
0: y '.
In step of the present invention (1)-(3), the synthetic spinel LiMn2O4 carries out under the fit technique condition.Be that all fit technique conditions of the present invention are the actual building-up process of simulation spinel lithium manganate, when comprising the laboratory lab scale, actual building-up process during the simulation industrial production, industrial condition when also comprising direct modeling spinel lithium manganate actual industrial production, the process conditions that adopt when adopting the actual building-up process of simulating spinel lithium manganate can be avoided the impact of the factors such as procedures system error.
Fit technique condition of the present invention is preferably the simulation process condition that does not have the procedures system error with the actual building-up process of spinel lithium manganate.
Fit technique condition of the present invention is preferably the actual production synthetic technological condition of simulation spinel lithium manganate.
In step of the present invention (1) in manganese dioxide in manganese content a and spinel lithium manganate the relation formula between the mol ratio b of lithium/manganese obtain in the following way: according to the mol ratio of lithium carbonate and manganese dioxide: b:2=xu%/M
1: ya/M
2, draw a * b=(2u%M
2/ M
1) * (x/y) is with u, M
1And M
2The numerical value substitution, obtain relational expression a * b=1.487 (xu%/y).
In step of the present invention (1), u% is the quality percentage composition of raw material lithium carbonate, wherein u% 〉=99.5%; As a rule, u% can reach 99.5% can satisfy raw materials requirement, if but the content of u% is higher better, and usually be set as constant and can not affect accurately determining raw material manganese dioxide manganese content and raw material proportioning under fit technique condition of the present invention.
The benchmark consumption x of required lithium carbonate in theory in step of the present invention (2)
0By the determining with magnitude relation of lithium carbonate and LiMn2O4, the benchmark consumption y of required manganese dioxide in theory in step (2)
0Determining with magnitude relation by manganese dioxide and LiMn2O4.
In step of the present invention (2), the consumption of lithium carbonate, manganese dioxide is respectively benchmark consumption x
0, y
0The time, the use magnitude relation of the chemical equation of synthetic LiMn2O4 and each raw material is as follows:
Wherein: u% is the quality percentage composition of lithium carbonate, wherein u% 〉=99.5%; As a rule, u% can reach 99.5% can satisfy raw materials requirement, if but the content of u% is higher better, usually be set as constant;
M
1Be Li
2CO
3Molecular weight is 73.89;
M
2Being the atomic weight of Mn, is 54.938;
M
3Be Li
2b
0Mn
2O
4Molecular weight, depending on b
0Value is calculated and is got;
x
0For generating the spinel lithium manganate required benchmark lithium carbonate quality in theory that quality is z;
y
0For generating the spinel lithium manganate required benchmark manganese dioxide quality in theory that quality is z;
Z generates the spinel lithium manganate quality for reaction, for setting constant.
The benchmark consumption x of lithium carbonate in the present invention
0Refer under initial fit technique condition, when the benchmark manganese content that adopts manganese dioxide is a
0(w.t.%), in spinel lithium manganate, the benchmark mol ratio of lithium/manganese is b
0, be the spinel lithium manganate of z as the need preparation quality, the plan that needs to set lithium carbonate and manganese dioxide feeds intake, wherein the plan of the lithium carbonate benchmark consumption x that feeds intake and be the lithium carbonate described in the application
0, the benchmark consumption y that the plan of manganese dioxide feeds intake and is the manganese dioxide described in the application
0
57.4%≤a in step of the present invention (2)
0＜=62%, 0.50≤b
0＜=0.615.
Adopt in step of the present invention (3) the ICP method precision such as to carry out to the actual mol ratio of lithium/manganese in spinel lithium manganate and measure for n time, obtain n measurement calculated value b
1', b
2', b
3' ..., b '
n, the arithmetic mean of n measured value
N＞5 wherein.
Compared with prior art, the present invention has following advantage: the inventive method match spinel lithium manganate technique building-up process, the procedures system error of having avoided technical process to bring, the measuring system error that simultaneously also can avoid the measurement of conventional chemical method to bring, realize accurately determining raw material manganese dioxide manganese content and raw material proportioning under the fit technique condition, have advantages of simple, convenient, but precision is high, practical and continued operation, is particularly useful for Industrialized Production Practice.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment, but the present invention is not limited in following examples, and following reagent is commercially available if no special instructions.
Embodiment 1
The synthetic spinel LiMn2O4 raw material manganese dioxide manganese content that the present embodiment provides and definite method of raw material lithium carbonate and manganese dioxide proportioning contain following steps:
(1) the manganese content a (w.t.%) of raw material manganese dioxide derives with the relation formula of product LiMn2O4 lithium/manganese mol ratio b: take lithium carbonate as the lithium source, take manganese dioxide as the manganese source, the synthetic spinel LiMn2O4, wherein the synthetic spinel LiMn2O4 carries out under the fit technique condition, this fit technique condition is not have the process conditions of procedures system error with the actual building-up process of spinel lithium manganate, set the quality x of lithium carbonate, the quality of manganese dioxide is y, manganese dioxide manganese content is a, in synthetic spinel lithium manganate, the mol ratio of lithium/manganese is b, lithium carbonate and manganese dioxide carry out chemical reaction according to following chemical formula, mol ratio by lithium carbonate and manganese dioxide, draw in manganese dioxide that in manganese content a and spinel lithium manganate, the relation formula between the mol ratio b of lithium/manganese is: a * b=1.487 (xu%/y)
Wherein: u% is the quality percentage composition of raw material lithium carbonate, and wherein u% 〉=99.5%, set u%=99.5%;
M
1Be Li
2CO
3Molecular weight is 73.89;
M
2Being the atomic weight of Mn, is 54.938;
M
3Be Li
2bMn
2O
4Molecular weight calculates and gets depending on the b value;
X is the lithium carbonate quality;
Y is the manganese dioxide quality;
Z generates product quality for reaction, for setting constant; Z for ease of calculating, all adopts 1000kg in following examples, in fact, can be the quality of the synthetic spinel lithium manganate of any needs.
Wherein in manganese dioxide in manganese content a and spinel lithium manganate the relation formula between the mol ratio b of lithium/manganese obtain in the following way: according to the mol ratio of lithium carbonate and manganese dioxide: b:2=xu%/M
1: ya/M
2, draw a * b=(2u%M
2/ M
1) * (x/y) is with u%, M
1And M
2The numerical value substitution, obtain relational expression a * b=1.48 (x/y).
(2) setting manganese dioxide benchmark manganese content is a
0(w.t.%), a wherein
0=0.59(59w.t.%), the benchmark mol ratio of setting lithium/manganese in spinel lithium manganate is b
0, b wherein
0=0.54, according to the chemical formula synthetic spinel LiMn2O4 in step (1), setting needs synthetic 1 ton of (z=1000kg) spinel lithium manganate, and its structural formula is Li
1.08Mn
2O
4, derive the benchmark consumption x of required in theory lithium carbonate
0, the benchmark consumption y of manganese dioxide
0, the benchmark consumption x of required lithium carbonate in theory
0By the determining with magnitude relation of lithium carbonate and LiMn2O4, the benchmark consumption y of required manganese dioxide in theory
0Be by the determining with magnitude relation of manganese dioxide and LiMn2O4, draw x through deriving
0=(zb
0M
1)/(u%M
3), with b
0=0.54, M
1=73.89, M
3=181.368, u%=99.5% substitution x
0Relational expression in, calculate x
0=221.10kg, y
0=(2zM
2)/(a
0M
3)=1026.81kg, with z=1000kg, M
2=54.938, a
0=0.59, M
3=181.368 substitution y
0Relational expression in, calculate y
0=1026.81kg;
(3) be x according to the lithium carbonate quality
0=221.10kg, manganese dioxide quality are y
0=1026.81kg according to the chemical formula synthetic spinel LiMn2O4 in step (1), adopts the ICP method precision such as to carry out to the actual mol ratio of lithium/manganese in spinel lithium manganate and measures for 10 times, and get its statistics average data
Will
x
0And y
0, substitution relational expression a * b=1.48 (x/y) draws the actual manganese content of manganese dioxide
Wherein the synthetic spinel LiMn2O4 carries out under the actual process condition, and specific embodiment is:
(a) take the weight that takes respectively raw material lithium carbonate and manganese dioxide as the raw material proportioning according to the benchmark proportioning, raw material granularity is respectively 4～6 μ m, 18～20 μ m;
(b) material that takes is put into oblique type batch mixer, ratio of grinding media to material is 2:1(weight), carried out ball mill mixing 6 hours;
(c) material that mixes is incubated 20 hours at 800 ℃, carries out chemical reaction;
The material that (d) will react completely pulverizes and sieves and obtains the Li that granularity is 20 μ m after cooling
1.08Mn
2O
4Powder.
Adopt ICP method measuring and calculating Li/Mn mol ratio:
Randomly draw 10 parts, synthetic product sample, the ICP results of measuring is as shown in table (1):
The lithium of each sample/manganese ratio in table 110 part spinel lithium manganate sample
(4) keeping the lithium carbonate quality is x
0, the actual manganese content of manganese dioxide is a ', in spinel lithium manganate, the mol ratio of lithium/manganese is b
0, lithium carbonate and manganese dioxide are carried out chemical reaction according to the chemical formula in step (1), when generating spinel lithium manganate, according to relational expression a * b=1.48 (x/y), with x
0=221.10, a '=0.5970, b
0=0.54, calculate the consumption y ' of the manganese dioxide of actual needs, y '=(1.48x
0)/(a ' * b
0)=1015.03kg; The actual amount proportioning of lithium carbonate and manganese dioxide is x
0: y '=221.10:1015.03.
Embodiment 2
The synthetic spinel LiMn2O4 raw material manganese dioxide manganese content that the present embodiment provides and definite method of raw material lithium carbonate and manganese dioxide proportioning contain following steps:
(1) the manganese content a (w.t.%) of raw material manganese dioxide derives with the relation formula of product LiMn2O4 lithium/manganese mol ratio b: take lithium carbonate as the lithium source, take manganese dioxide as the manganese source, the synthetic spinel LiMn2O4, wherein the synthetic spinel LiMn2O4 carries out under the fit technique condition, this fit technique condition is not carried out under the process conditions of procedures system error for not existing with the actual building-up process of spinel lithium manganate, set the quality x of lithium carbonate, the quality of manganese dioxide is y, manganese dioxide manganese content is a, in synthetic spinel lithium manganate, the mol ratio of lithium/manganese is b, lithium carbonate and manganese dioxide carry out chemical reaction according to following chemical formula, mol ratio according to lithium carbonate and manganese dioxide, draw in manganese dioxide that in manganese content a and spinel lithium manganate, the relation formula between the mol ratio b of lithium/manganese is: a * b=1.487 (xu%/y)
Wherein: u% is the quality percentage composition of raw material lithium carbonate, and wherein u% 〉=99.5%, set u%=99.5%;
M
1Be Li
2CO
3Molecular weight is 73.89;
M
2Being the atomic weight of Mn, is 54.938;
M
3Be Li
2bMn
2O
4Molecular weight calculates and gets depending on the b value;
X is the lithium carbonate quality;
Y is the manganese dioxide quality;
Z generates product quality for reaction, for setting constant;
Wherein in manganese dioxide in manganese content a and spinel lithium manganate the relation formula between the mol ratio b of lithium/manganese obtain in the following way: according to the mol ratio of lithium carbonate and manganese dioxide: b:2=xu%/M
1: ya/M
2, draw a * b=(2u%M
2/ M
1) * (x/y) is with u%, M
1And M
2The numerical value substitution, obtain relational expression a * b=1.48 (x/y).
(2) setting benchmark manganese content is a
0(w.t.%), a wherein
0=0.574(57.4w.t.%), the benchmark mol ratio of setting lithium/manganese in spinel lithium manganate is b
0, b wherein
0=0.615, according to the chemical formula synthetic spinel LiMn2O4 in step (1), setting needs synthetic 1 ton of (z=1000kg) spinel lithium manganate, and its structural formula is Li
1.23Mn
2O
4, derive the benchmark consumption x of required in theory lithium carbonate
0, the benchmark consumption y of manganese dioxide
0, the benchmark consumption x of required lithium carbonate in theory
0By the determining with magnitude relation of lithium carbonate and LiMn2O4, the benchmark consumption y of required manganese dioxide in theory
0Be by the determining with magnitude relation of manganese dioxide and LiMn2O4, draw x through deriving
0=(zb
0M
1)/(u%M
3), with b
0=0.615, M
1=73.89, M
3=182.409, u%=99.5% substitution x
0Relational expression in, calculate x
0=250.38kg, y
0=(2zM
2)/(a
0M
3)=1049.41kg, with z=1000kg, M
2=54.938, a
0=0.574, M
3=182.409 substitution y
0Relational expression in, calculate y
0=1049.41kg;
(3) be x according to the lithium carbonate quality
0=250.38kg, manganese dioxide quality are y
0=1049.41kg according to the chemical formula synthetic spinel LiMn2O4 in step (1), adopts the ICP method precision such as to carry out to the actual mol ratio of lithium/manganese in spinel lithium manganate and measures for 10 times, and get its statistics average data
Will
x
0And y
0, substitution relational expression a * b=1.48 (x/y) draws the actual manganese content of manganese dioxide
Wherein the synthetic spinel LiMn2O4 carries out under the actual process condition, and only for enumerating, the concrete technology condition can be with reference to the preparation process of each spinel lithium manganate herein, and specific embodiment is:
(a) take the weight of raw material lithium carbonate and manganese dioxide as the raw material proportioning according to the benchmark proportioning, raw material granularity is respectively 4～6 μ m, 18～20 μ m;
(b) material that takes is put into oblique type batch mixer, ratio of grinding media to material is 2:1(weight), carried out ball mill mixing 6 hours;
(c) material that mixes is incubated 20 hours at 800 ℃, carries out chemical reaction;
The material that (d) will react completely pulverizes and sieves and obtains the Li that granularity is 20 μ m after cooling
1.23Mn
2O
4Powder.
Adopt ICP method measuring and calculating Li/Mn mol ratio:
Randomly draw 10 parts, synthetic product sample, the ICP results of measuring is as shown in table (1):
The lithium of each sample/manganese ratio in table 210 part spinel lithium manganate sample
(4) keeping the lithium carbonate quality is x
0, the actual manganese content of manganese dioxide is a ', in spinel lithium manganate, the mol ratio of lithium/manganese is b
0, lithium carbonate and manganese dioxide are carried out chemical reaction according to the chemical formula in step (1), when generating spinel lithium manganate, according to relational expression a * b=1.48 (x/y), with x
0=250.38, a '=0.5884, b
0=0.615, calculate the consumption y ' of the manganese dioxide of actual needs, y '=(1.487x
0U%)/(a ' * b
0)=1024.03kg; The actual amount proportioning of lithium carbonate and manganese dioxide is x
0: y '=250.38:1024.03.
Embodiment 3
The synthetic spinel LiMn2O4 raw material manganese dioxide manganese content that the present embodiment provides and definite method of raw material lithium carbonate and manganese dioxide proportioning contain following steps:
(1) the manganese content a (w.t.%) of raw material manganese dioxide derives with the relation formula of product LiMn2O4 lithium/manganese mol ratio b: take lithium carbonate as the lithium source, take manganese dioxide as the manganese source, the synthetic spinel LiMn2O4, wherein the synthetic spinel LiMn2O4 carries out under the fit technique condition, this fit technique condition is not carried out under the process conditions of procedures system error for not existing with the actual building-up process of spinel lithium manganate, set the quality x of lithium carbonate, the quality of manganese dioxide is y, manganese dioxide manganese content is a, in synthetic spinel lithium manganate, the mol ratio of lithium/manganese is b, lithium carbonate and manganese dioxide carry out chemical reaction according to following chemical formula, mol ratio according to lithium carbonate and manganese dioxide, draw in manganese dioxide that in manganese content a and spinel lithium manganate, the relation formula between the mol ratio b of lithium/manganese is: a * b=1.487 (x u%/y)
Wherein: u% is the quality percentage composition of raw material lithium carbonate, and wherein u% 〉=99.5%, set u%=99.5%;
M
1Be Li
2CO
3Molecular weight is 73.89;
M
2Being the atomic weight of Mn, is 54.938;
M
3Be Li
2bMn
2O
4Molecular weight calculates and gets depending on the b value;
X is the lithium carbonate quality;
Y is the manganese dioxide quality;
Z generates product quality for reaction, for setting constant;
Wherein in manganese dioxide in manganese content and spinel lithium manganate the relation formula between the mol ratio b of lithium/manganese obtain in the following way: according to the mol ratio of lithium carbonate and manganese dioxide: b:2=xu%/M
1: ya/M
2, draw a * b=(2u%M
2/ M
1) * (x/y) is with u%, M
1And M
2The numerical value substitution, obtain relational expression a * b=1.48 (x/y).
(2) setting benchmark manganese content is a
0(w.t.%), a wherein
0=0.62(62w.t.%), the benchmark mol ratio of setting lithium/manganese in spinel lithium manganate is b
0, b wherein
0=0.50, according to the chemical formula synthetic spinel LiMn2O4 in step (1), setting needs synthetic 1 ton of (z=1000kg) spinel lithium manganate, and its structural formula is Li
1.00Mn
2O
4, derive the benchmark consumption x of required in theory lithium carbonate
0, the benchmark consumption y of manganese dioxide
0, the benchmark consumption x of required lithium carbonate in theory
0By the determining with magnitude relation of potash and LiMn2O4, the benchmark consumption y of required manganese dioxide in theory
0Be by the determining with magnitude relation of manganese dioxide and LiMn2O4, draw x through deriving
0=(zb
0M
1)/(u%M
3), with b
0=0.50, M
1=73.89, M
3=180.813, u%=99.5% substitution x
0Relational expression in, calculate x
0=205.35kg, y
0=(2zM
2)/(a
0M
3)=980.13kg, with z=1000kg, M
2=54.938, a
0=0.50, M
3=180.813 substitution y
0Relational expression in, calculate y
0=980.13kg;
(3) be x according to the lithium carbonate quality
0=205.35kg, manganese dioxide quality are y
0=980.13kg according to the chemical formula synthetic spinel LiMn2O4 in step (1), adopts the ICP method precision such as to carry out to the actual mol ratio of lithium/manganese in spinel lithium manganate and measures for 10 times, and get its statistics average data
Will
x
0And y
0, substitution relational expression a * b=1.48 (x/y) draws the actual manganese content of manganese dioxide
Wherein the synthetic spinel LiMn2O4 carries out under the actual process condition, and specific embodiment is:
(a) take the weight of raw material lithium carbonate and manganese dioxide as the raw material proportioning according to the benchmark proportioning, raw material granularity is respectively 4～6 μ m, 18～20 μ m;
(b) material that takes is put into oblique type batch mixer, ratio of grinding media to material is 2:1(weight), carried out ball mill mixing 6 hours;
(c) material that mixes is incubated 16 hours at 780 ℃, carries out chemical reaction;
The material that (d) will react completely pulverizes and sieves and obtains the Li that granularity is 20 μ m after cooling
1.00Mn
2O
4Powder.
Adopt ICP method measuring and calculating Li/Mn mol ratio:
Randomly draw 10 parts, synthetic product sample, the ICP results of measuring is as shown in table (1):
The lithium of each sample/manganese ratio in table 310 part spinel lithium manganate sample
(4) keeping the lithium carbonate quality is x
0, the actual manganese content of manganese dioxide is a ', in spinel lithium manganate, the mol ratio of lithium/manganese is b
0, lithium carbonate and manganese dioxide are carried out chemical reaction according to the chemical formula in step (1), when generating spinel lithium manganate, according to relational expression a * b=1.48 (x/y), with x
0=205.35, a '=0.5992, b
0=0.50, calculate the consumption y ' of the manganese dioxide of actual needs, y '=(1.48x
0)/(a ' * b
0)=1014.41kg; The actual amount proportioning of lithium carbonate and manganese dioxide is x
0: y '=205.35:1014.41.
Embodiment 4
The synthetic spinel LiMn2O4 raw material manganese dioxide manganese content that the present embodiment provides and definite method of raw material lithium carbonate and manganese dioxide proportioning contain following steps:
(1) the manganese content a (w.t.%) of raw material manganese dioxide derives with the relation formula of product LiMn2O4 lithium/manganese mol ratio b: take lithium carbonate as the lithium source, take manganese dioxide as the manganese source, the synthetic spinel LiMn2O4, wherein the synthetic spinel LiMn2O4 carries out under the fit technique condition, this fit technique condition is not have the process conditions of procedures system error with the actual building-up process of spinel lithium manganate, set the quality x of lithium carbonate, the quality of manganese dioxide is y, manganese dioxide manganese content is a, in synthetic spinel lithium manganate, the mol ratio of lithium/manganese is b, lithium carbonate and manganese dioxide carry out chemical reaction according to following chemical formula, mol ratio by lithium carbonate and manganese dioxide, the relation formula that draws between the mol ratio b of lithium/manganese in manganese dioxide manganese content a and spinel lithium manganate is: a * b=1.487 (xu%/y)
Wherein: u% is the quality percentage composition of raw material lithium carbonate, and wherein u% 〉=99.5%, set u%=99.5%;
M
1Be Li
2CO
3Molecular weight is 73.89;
M
2Being the atomic weight of Mn, is 54.938;
M
3Be Li
2bMn
2O
4Molecular weight calculates and gets depending on the b value;
X is the lithium carbonate quality;
Y is the manganese dioxide quality;
Z generates product quality for reaction, for setting constant;
Wherein in manganese dioxide in manganese content a and spinel lithium manganate the relation formula between the mol ratio b of lithium/manganese obtain in the following way: according to the mol ratio of lithium carbonate and manganese dioxide: b:2=xu%/M
1: ya/M
2, draw a * b=(2u%M
2/ M
1) * (x/y) is with u%, M
1And M
2The numerical value substitution, obtain relational expression a * b=1.48 (x/y).
(2) setting manganese dioxide benchmark manganese content is a
0(w.t.%), a wherein
0=0.60(60w.t.%), the benchmark mol ratio of setting lithium/manganese in spinel lithium manganate is b
0, b wherein
0=0.56, according to the chemical formula synthetic spinel LiMn2O4 in step (1), setting needs synthetic 1 ton of (z=1000kg) spinel lithium manganate, and its structural formula is Li
1.12Mn
2O
4, derive the benchmark consumption x of required in theory lithium carbonate
0, the benchmark consumption y of manganese dioxide
0, the benchmark consumption x of required lithium carbonate in theory
0By the determining with magnitude relation of lithium carbonate and LiMn2O4, the benchmark consumption y of required manganese dioxide in theory
0Be by the determining with magnitude relation of manganese dioxide and LiMn2O4, draw x through deriving
0=(zb
0M
1)/(u%M
3), with b
0=0.54, M
1=73.89, M
3=181.646, u%=99.5% substitution x
0Relational expression in, calculate x
0=228.94kg, y
0=(2zM
2)/(a
0M
3)=1008.15kg, with z=1000kg, M
2=54.938, a
0=0.59, M
3=181.646 substitution y
0Relational expression in, calculate y
0=1008.15kg;
(3) be x according to the lithium carbonate quality
0=228.94kg, manganese dioxide quality are y
0=1008.15kg according to the chemical formula synthetic spinel LiMn2O4 in step (1), adopts the ICP method precision such as to carry out to the actual mol ratio of lithium/manganese in spinel lithium manganate and measures for 8 times, and get its statistics average data
Will
x
0And y
0, substitution relational expression a * b=1.48 (x/y) draws the actual manganese content of manganese dioxide
Wherein the synthetic spinel LiMn2O4 carries out under the actual process condition, and specific embodiment is:
(a) take the weight that takes respectively raw material lithium carbonate and manganese dioxide as the raw material proportioning according to the benchmark proportioning, raw material granularity is respectively 4～6 μ m, 18～20 μ m;
(b) material that takes is put into oblique type batch mixer, ratio of grinding media to material is 2:1(weight), carried out ball mill mixing 6 hours;
(c) material that mixes is incubated 20 hours at 800 ℃, carries out chemical reaction;
The material that (d) will react completely pulverizes and sieves and obtains the Li that granularity is 20 μ m after cooling
1.12Mn
2O
4Powder.
Adopt ICP method measuring and calculating Li/Mn mol ratio:
Randomly draw 8 parts, synthetic product sample, the ICP results of measuring is as shown in table (1):
The lithium of each sample/manganese ratio in table 48 part spinel lithium manganate sample
(4) keeping the lithium carbonate quality is x
0, the actual manganese content of manganese dioxide is a ', in spinel lithium manganate, the mol ratio of lithium/manganese is b
0, lithium carbonate and manganese dioxide are carried out chemical reaction according to the chemical formula in step (1), when generating spinel lithium manganate, according to relational expression a * b=1.48 (x/y), with x
0=228.94, a '=0.5958, b
0=0.56, calculate the consumption y ' of the manganese dioxide of actual needs, y '=(1.48x
0)/(a ' * b
0)=1015.53kg; The actual amount proportioning of lithium carbonate and manganese dioxide is x
0: y '=228.94:1015.53.
Embodiment 5
The synthetic spinel LiMn2O4 raw material manganese dioxide manganese content that the present embodiment provides and definite method of raw material lithium carbonate and manganese dioxide proportioning contain following steps:
(1) the manganese content a (w.t.%) of raw material manganese dioxide derives with the relation formula of product LiMn2O4 lithium/manganese mol ratio b: take lithium carbonate as the lithium source, take manganese dioxide as the manganese source, the synthetic spinel LiMn2O4, wherein the synthetic spinel LiMn2O4 carries out under the fit technique condition, this fit technique condition is not have the process conditions of procedures system error with the actual building-up process of spinel lithium manganate, set the quality x of lithium carbonate, the quality of manganese dioxide is y, in manganese dioxide, manganese content is a, in synthetic spinel lithium manganate, the mol ratio of lithium/manganese is b, lithium carbonate and manganese dioxide carry out chemical reaction according to following chemical formula, mol ratio by lithium carbonate and manganese dioxide, the relation formula that draws between the mol ratio b of lithium/manganese in manganese dioxide manganese content a and spinel lithium manganate is: a * b=1.487 (xu%/y)
Wherein: u% is the quality percentage composition of raw material lithium carbonate, and wherein u% 〉=99.5%, set u%=99.98%;
M
1Be Li
2CO
3Molecular weight is 73.89;
M
2Being the atomic weight of Mn, is 54.938;
M
3Be Li
2bMn
2O
4Molecular weight calculates and gets depending on the b value;
X is the lithium carbonate quality;
Y is the manganese dioxide quality;
Z generates product quality for reaction, for setting constant;
Wherein in manganese dioxide in manganese content a and spinel lithium manganate the relation formula between the mol ratio b of lithium/manganese obtain in the following way: according to the mol ratio of lithium carbonate and manganese dioxide: b:2=xu%/M
1: ya/M
2, draw a * b=(2u%M
2/ M
1) * (x/y) is with u%, M
1And M
2The numerical value substitution, obtain relational expression a * b=1.487 (x/y).
(2) setting manganese dioxide benchmark manganese content is a
0(w.t.%), a wherein
0=0.595(59.5w.t.%), the benchmark mol ratio of setting lithium/manganese in spinel lithium manganate is b
0, b wherein
0=0.58, according to the chemical formula synthetic spinel LiMn2O4 in step (1), setting needs synthetic 1 ton of (z=1000kg) spinel lithium manganate, and its structural formula is Li
1.16Mn
2O
4, derive the benchmark consumption x of required in theory lithium carbonate
0, the benchmark consumption y of manganese dioxide
0, the benchmark consumption x of required lithium carbonate in theory
0By the determining with magnitude relation of lithium carbonate and LiMn2O4, the benchmark consumption y of required manganese dioxide in theory
0Be by the determining with magnitude relation of manganese dioxide and LiMn2O4, draw x through deriving
0=(zb
0M
1)/(u%M
3), with b
0=0.58, M
1=73.89, M
3=181.924, u%=99.98% substitution x
0Relational expression in, calculate x
0=235.62kg, y
0=(2zM
2)/(a
0M
3)=1015.07kg, with z=1000kg, M
2=54.938, a
0=0.59, M
3=181.924 substitution y
0Relational expression in, calculate y
0=1015.07kg;
(3) be x according to the lithium carbonate quality
0=235.62kg, manganese dioxide quality are y
0=1015.07kg according to the chemical formula synthetic spinel LiMn2O4 in step (1), adopts the ICP method precision such as to carry out to the actual mol ratio of lithium/manganese in spinel lithium manganate and measures for 10 times, and get its statistics average data
Will
x
0And y
0, substitution relational expression a * b=1.487 (x/y) draws the actual manganese content of manganese dioxide
Wherein the synthetic spinel LiMn2O4 carries out under the actual process condition, and specific embodiment is:
(a) take the weight that takes respectively raw material lithium carbonate and manganese dioxide as the raw material proportioning according to the benchmark proportioning, raw material granularity is respectively 4～6 μ m, 18～20 μ m;
(b) material that takes is put into oblique type batch mixer, ratio of grinding media to material is 2:1(weight), carried out ball mill mixing 6 hours;
(c) material that mixes is incubated 20 hours at 800 ℃, carries out chemical reaction;
The material that (d) will react completely pulverizes and sieves and obtains the Li that granularity is 20 μ m after cooling
1.16Mn
2O
4Powder.
Adopt ICP method measuring and calculating Li/Mn mol ratio:
Randomly draw 10 parts, synthetic product sample, the ICP results of measuring is as shown in table (1):
The lithium of each sample/manganese ratio in table 510 part spinel lithium manganate sample
(4) keeping the lithium carbonate quality is x
0, the actual manganese content of manganese dioxide is a ', in spinel lithium manganate, the mol ratio of lithium/manganese is b
0, lithium carbonate and manganese dioxide are carried out chemical reaction according to the chemical formula in step (1), when generating spinel lithium manganate, according to relational expression a * b=1.48 (x/y), with x
0=235.62, a '=0.5964, b
0=0.58, calculate the consumption y ' of the manganese dioxide of actual needs, y '=(1.487x
0)/(a ' * b
0)=1012.87kg; The actual amount proportioning of lithium carbonate and manganese dioxide is x
0: y '=235.62:1012.87.
The specific embodiment of more than enumerating is the explanation that the present invention is carried out.It is pointed out that above embodiment only for the invention will be further described, does not consist of limiting the scope of the invention, nonessential modification and adjustment that other people prompting according to the present invention is made still belong to protection scope of the present invention.
Claims (9)
1. definite method of a synthetic spinel LiMn2O4 raw material manganese dioxide manganese content and raw material lithium carbonate and manganese dioxide proportioning is characterized in that comprising following steps:
(1) take lithium carbonate as the lithium source, take manganese dioxide as the manganese source, the synthetic spinel LiMn2O4, the quality of setting lithium carbonate is x, the quality of manganese dioxide is y, manganese dioxide manganese content is a (w.t.%), in synthetic spinel lithium manganate, the mol ratio of lithium/manganese is b, lithium carbonate and manganese dioxide carry out chemical reaction according to following chemical formula, according to the mol ratio of lithium carbonate and manganese dioxide, the relation formula that draws between the mol ratio b of lithium/manganese in manganese dioxide manganese content a and spinel lithium manganate is: a * b=1.487 (xu%/y)
Wherein: u% is the quality percentage composition of raw material lithium carbonate, wherein u% 〉=99.5%;
M
1Be Li
2CO
3Molecular weight is 73.89;
M
2Being the atomic weight of Mn, is 54.938;
M
3Be Li
2bMn
2O
4Molecular weight calculates and gets depending on the b value;
X is the lithium carbonate quality;
Y is the manganese dioxide quality;
Z generates product quality for reaction, for setting constant;
(2) the benchmark manganese content of setting manganese dioxide is a
0(w.t.%), in spinel lithium manganate, the benchmark mol ratio of lithium/manganese is b
0, according to the chemical formula synthetic spinel LiMn2O4 in step (1), derive the benchmark consumption x of required in theory lithium carbonate
0, the benchmark consumption y of manganese dioxide
0, x wherein
0=(zb
0M
1)/(u%M
3), y
0=(2zM
2)/(a
0M
3);
(3) be x according to the lithium carbonate quality
0, the manganese dioxide quality is y
0, according to the chemical formula synthetic spinel LiMn2O4 in step (1), adopt the ICP method n the measurement of precision such as to carry out to the actual mol ratio of lithium/manganese in spinel lithium manganate, and get its statistics average data
Will
x
0And y
0, substitution relational expression a * b=1.487 (xu%/y) draws the actual manganese content of manganese dioxide
(4) keeping the lithium carbonate quality is x
0, the actual manganese content of manganese dioxide is a ', in spinel lithium manganate, the mol ratio of lithium/manganese is b
0, lithium carbonate and manganese dioxide are carried out chemical reaction according to the chemical formula in step (1), when generating spinel lithium manganate, according to relational expression a * b=1.487 (xu%/y), calculate the consumption y ' of the manganese dioxide of actual needs, y '=(1.487x
0U%)/(a ' * b
0); The actual amount proportioning of lithium carbonate and manganese dioxide is x
0: y '.
2. definite method of synthetic spinel LiMn2O4 raw material manganese dioxide manganese content according to claim 1 and raw material lithium carbonate and manganese dioxide proportioning is characterized in that: in step (1)-(3), the synthetic spinel LiMn2O4 carries out under the fit technique condition.
3. definite method of synthetic spinel LiMn2O4 raw material manganese dioxide manganese content according to claim 2 and raw material lithium carbonate and manganese dioxide proportioning is characterized in that: described fit technique condition is not for existing the simulation process condition of procedures system error with the actual building-up process of spinel lithium manganate.
4. definite method of synthetic spinel LiMn2O4 raw material manganese dioxide manganese content according to claim 2 and raw material lithium carbonate and manganese dioxide proportioning is characterized in that: described fit technique condition is the actual production synthetic technological condition of simulation spinel lithium manganate.
5. definite method of synthetic spinel LiMn2O4 raw material manganese dioxide manganese content according to claim 1 and raw material lithium carbonate and manganese dioxide proportioning is characterized in that: in step (1) in manganese dioxide in manganese content a and spinel lithium manganate the relation formula between the mol ratio b of lithium/manganese obtain in the following way: according to the mol ratio of lithium carbonate and manganese dioxide: b:2=xu%/M
1: ya/M
2, draw a * b=(2u%M
2/ M
1) * (x/y) is with u, M
1And M
2The numerical value substitution, obtain relational expression a * b=1.487 (xu%/y).
6. definite method of synthetic spinel LiMn2O4 raw material manganese dioxide manganese content according to claim 1 and raw material lithium carbonate and manganese dioxide proportioning is characterized in that: the benchmark consumption x of required lithium carbonate in theory in step (2)
0By the determining with magnitude relation of lithium carbonate and LiMn2O4, the benchmark consumption y of required manganese dioxide in theory in step (2)
0Determining with magnitude relation by manganese dioxide and LiMn2O4.
7. definite method of synthetic spinel LiMn2O4 raw material manganese dioxide manganese content according to claim 1 and raw material lithium carbonate and manganese dioxide proportioning is characterized in that: in step (2), the consumption of lithium carbonate, manganese dioxide is respectively benchmark consumption x
0, y
0The time, the use magnitude relation of the chemical equation of synthetic LiMn2O4 and each raw material is as follows:
Wherein: u% is the quality percentage composition of lithium carbonate, wherein u% 〉=99.5%;
M
1Be Li
2CO
3Molecular weight is 73.89;
M
2Being the atomic weight of Mn, is 54.938;
M
3Be Li
2b
0Mn
2O
4Molecular weight, depending on b
0Value is calculated and is got;
x
0For generating the spinel lithium manganate required benchmark lithium carbonate quality in theory that quality is z;
y
0For generating the spinel lithium manganate required benchmark manganese dioxide quality in theory that quality is z;
Z generates the spinel lithium manganate quality for reaction, for setting constant.
8. definite method of synthetic spinel LiMn2O4 raw material manganese dioxide manganese content according to claim 1 and raw material lithium carbonate and manganese dioxide proportioning, is characterized in that: 57.4%≤a in step (2)
0＜=62%, 0.50≤b
0＜=0.615.
9. definite method of synthetic spinel LiMn2O4 raw material manganese dioxide manganese content according to claim 1 and raw material lithium carbonate and manganese dioxide proportioning, it is characterized in that: adopt in step (3) the ICP method precision such as to carry out to the actual mol ratio of lithium/manganese in spinel lithium manganate and measure for n time, obtain n measurement calculated value b
1', b
2', b
3' ..., b '
n, the arithmetic mean of n measured value
N＞5 wherein.
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| CN104600281A (en) * | 2014-12-30 | 2015-05-06 | 山东神工海特电子科技有限公司 | Preparation method of lithium manganate material and method for preparing battery from lithium manganate material |
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