CN103482606A - Production method for intermediate phase carbon anode material - Google Patents
Production method for intermediate phase carbon anode material Download PDFInfo
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- CN103482606A CN103482606A CN201310434835.3A CN201310434835A CN103482606A CN 103482606 A CN103482606 A CN 103482606A CN 201310434835 A CN201310434835 A CN 201310434835A CN 103482606 A CN103482606 A CN 103482606A
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Abstract
The invention provides a production method for an intermediate phase carbon anode material. Mesocarbon microbeads with the median particle diameters of 5-18 microns are used as a raw material A, boron nitride micro powder with the median particle diameter not greater than 5 microns is used as a raw material B, and epoxy resin with the median particle diameter not greater than 5 microns or phenolic resin is used as a raw material C. The production method comprises the following steps: taking the raw material A firstly, and performing graphitization treatment at the temperature of 2800-3200 DEG C; then putting the obtained raw material A subjected to super-high temperature graphitization treatment and cooling treatment into an H2SO4 solution with the concentration of 0.5-1 mol/L, heating to 60-80 DEG C, and soaking for 5-8 hours; thereafter, taking out the raw material A soaked in the H2SO4 solution, and washing and filtering by adopting water to obtain the neutral substance, and then drying at the temperature of 120 DEG C; finally, performing cover treatment. The intermediate phase carbon anode material produced through the method has the advantages of high capacity, high discharging efficiency, good cycle performance and good compatibility with an electrolyte.
Description
Technical field
The present invention relates to a kind of production method of intermediate-phase carbon negative material, belong to the lithium ion battery negative material technical field.
Background technology
Lithium ion battery adopts the Carbon Materials of reversible embedding, de-lithium to replace traditional lithium cell, and the embedding with lithium ion in the charcoal negative pole and deviate from the deposition and resolution reaction of substituted in reaction on pure lithium electrode can make the cycle life of battery and security greatly improve.Carbon Materials is made the negative pole of lithium ion battery, can also meet a series of requirements such as the large capacity of lithium ion battery, high-voltage and long circulation life, therefore is subject to people and pays close attention to greatly simultaneously.
MCMB (MCMB) is a kind of lithium-ion-power cell carbon cathode material with very big potentiality to be exploited and application prospect, and except the general characteristic with graphite carbon negative material, it also has unique advantage aspect Structure and form.MCMB is that to take petroleum asphalt based or coal-tar pitch base be raw material, mesophasespherule through thermolysis and thermal polycondensation reaction generation, the one-tenth of MCMB is endorsed and is divided into homogeneous nucleation and free charcoal nucleation, wherein, the MCMB of homogeneous nucleation has the layer molecule homogeneous texture, be conducive to the Infix and desfix of lithium ion, can be applicable to lithium ion battery negative material.And MCMB is ball-like structure, tap density is large, can realize tight filling, can make the battery that volume and capacity ratio is higher; Specific surface area is little, and the irreversible capacity loss that while having reduced charging, electrolytic solution causes in side reactions such as Surface Creation SEI films, can also improve safety performance; Due to its distinctive spherical and stable internal structure, can also meet the requirement of high current charge-discharge.So, through the MCMB of high temperature graphitization, be to use more a kind of carbon cathode material in current lithium ion battery industry.Yet, MCMB also comes with some shortcomings as negative material, because surperficial degree of graphitization is higher, causes the consistency of itself and electrolyte solution poor, hindered lithium ion and entered carbon microspheres inside from surface diffusion, made most of crystal can't carry out fast the reaction of doff lithium.
Summary of the invention
The production method that the purpose of this invention is to provide a kind of intermediate-phase carbon negative material, to overcome, the capacity that MCMB exists is low, poorly conductive and with the natural flaw such as compatibility of electrolyte is bad.
Technical scheme of the present invention: a kind of production method of intermediate-phase carbon negative material, concrete production technique is:
(a) take the MCMB that the meta particle diameter is 5 ~ 18 μ m is raw material A, and described MCMB is petroleum asphalt based or the coal-tar pitch base obtains the mesophase globule of homogeneous nucleation through thermolysis and thermal polycondensation reaction;
(b) take the boron nitride micro mist that the meta particle diameter is≤5 μ m is raw material B, and described boron nitride is hexagonal boron nitride;
(c) take the resin that the meta particle diameter is≤5 μ m is raw material C, and described resin is resol or epoxy resin;
(d) ultrahigh-temperature graphitization processing: get above-mentioned raw materials A, at 2800 ~ 3200 ℃, carry out graphitization processing;
(e) oxide treatment: will complete the ultrahigh-temperature graphitization processing and cooling after the raw material A that obtains put into the H that concentration is 0.5 ~ 1mol/L
2sO
4in solution, be warming up to 60 ~ 80 ℃, soak 5 ~ 8h.
(f) neutralization and drying treatment: take out above-mentioned at H
2sO
4the raw material A of soaking in solution, first wash with water and be filtered into neutrality, then dry at 120 ℃ of temperature;
(h) coat and process: first raw material B and raw material C are carried out to the air-flow mixing in the ratio of (20-30)/(80 ~ 70) under the normal temperature state, then in (B+C)/A=(3 ~ 15)/ratio of (97 ~ 85) is uniformly mixed 300 ~ 600 ℃ of temperature, described being uniformly mixed adopts twin screw or two ribbon alr mode, finally at 1300 ℃ ~ 1800 ℃, carries out the charing processing; Perhaps first by raw material in C/A=(3 ~ 15)/ratio of (97 ~ 85) is uniformly mixed 300 ~ 600 ℃ of temperature, finally at 1000 ℃ ~ 1300 ℃, carries out the charing processing.
Beneficial effect of the present invention:
1, because the present invention carries out the ultrahigh-temperature graphitization processing more than 3000 ℃ to MCMB, therefore more can improve its embedding lithium ability, improve charge/discharge capacity;
2, by adopting the H that concentration is 0.5 ~ 1mol/L
2sO
4solution carries out the suitable oxidizing processing to the raw material A surface, the active group that interface is generated is conducive to increase the wettability between electrode/electrolyte, oxygenizement can form micropore in addition, hold more lithium ion, even in the situation that surface coats is inhomogeneous, also can form rapidly the SEI film with electrolytic solution, improve circulation, and guarantee security;
3, adopt surperficial coating can make the condition of surface of carbonaceous mesophase spherules be improved, the consistency of material and electrolytic solution is improved, in addition, but add the conductivity of a small amount of boron nitride strongthener.
In sum, the present invention can improve the performance of electrode effectively by the MCMB material being carried out to top layer oxidation modification and doping coating decoration, and production technique is simple, and production efficiency is high, and cost is low, and course of processing safety, can be used for suitability for industrialized production.
Embodiment
embodiment 1:
Take MCMB raw material A 8000g, at 2800 ℃ of temperature, carry out greying, be immersed in 0.8mol/L H after cooling
2sO
4in solution, be warming up to 80 ℃, after soaking 5h, wash with water and be filtered into neutrality, dry at 120 ℃ of temperature.
Take boron nitride raw B 80g, resol raw material C 320g, carry out at normal temperatures air-flow and mix 30 minutes.
Take dried MCMB 5640g, add the mixture 360g of above-mentioned raw materials B and C, at 300 ℃ of temperature, be uniformly mixed 90 minutes; Temperature is raised to 450 ℃ again, strong mixing maintains 240 minutes; Continue slowly to be warming up to 600 ℃, stir and maintain 240 minutes; Finally at 1600 ℃ of temperature, carry out charing.
With LIR2430 type button cell, do experiment, gained negative material loading capacity is 326.5mAh/g, and discharging efficiency is 93.9%, as shown in table 1.
embodiment 2:
Take MCMB raw material A 8000g, at 3000 ℃ of temperature, carry out greying, be immersed in 0.6mol/L H after cooling
2sO
4in solution, be warming up to 60 ℃, after soaking 5h, wash with water and be filtered into neutrality, dry at 120 ℃ of temperature.
Take dried MCMB 5520g, add epoxy resin raw material C 480g, at 300 ℃ of temperature, be uniformly mixed 120 minutes; Temperature is raised to 450 ℃ again, strong mixing maintains 300 minutes; Continue slowly to be warming up to 600 ℃, stir and maintain 180 minutes; Finally at 1300 ℃ of temperature, carry out charing.
With LIR2430 type button cell, do experiment, gained negative material loading capacity is 331.6mAh/g, and discharging efficiency is 94.0%, as shown in table 1.
embodiment 3:
Take MCMB raw material A 8000g, at 3000 ℃ of temperature, carry out greying, be immersed in 1mol/L H after cooling
2sO
4in solution, be warming up to 80 ℃, after soaking 6h, wash with water and be filtered into neutrality, dry at 120 ℃ of temperature.
Take boron nitride raw B 100g, epoxy resin raw material C 300g, carry out at normal temperatures air-flow and mix 30 minutes.
Take dried MCMB 5700g, add the mixture 300g of above-mentioned raw materials B and C, at 300 ℃ of temperature, be uniformly mixed 90 minutes; Temperature is raised to 450 ℃ again, strong mixing maintains 240 minutes; Continue slowly to be warming up to 600 ℃, stir and maintain 240 minutes; Finally at 1500 ℃ of temperature, carry out charing.
With LIR2430 type button cell, do experiment, gained negative material loading capacity is 329.3mAh/g, and discharging efficiency is 94.6%, as shown in table 1.
embodiment 4:
Take MCMB raw material A 8000g, at 3200 ℃ of temperature, carry out greying, be immersed in 0.8mol/L H after cooling
2sO
4in solution, be warming up to 60 ℃, after soaking 8h, wash with water and be filtered into neutrality, dry at 120 ℃ of temperature.
Take dried MCMB 5520g, add resol raw material C 480g, at 300 ℃ of temperature, be uniformly mixed 120 minutes; Temperature is raised to 450 ℃ again, strong mixing maintains 300 minutes; Continue slowly to be warming up to 600 ℃, stir and maintain 180 minutes; Finally at 1200 ℃ of temperature, carry out charing.
With LIR2430 type button cell, do experiment, gained negative material loading capacity first is 334.8mAh/g, and discharging efficiency is 94.2%, as shown in table 1.
embodiment 5:
Take MCMB raw material A 8000g, at 3200 ℃ of temperature, carry out greying, be immersed in 1mol/L H after cooling
2sO
4in solution, be warming up to 60 ℃, after soaking 7h, wash with water and be filtered into neutrality, dry at 120 ℃ of temperature.
Take boron nitride raw B 120g, resol raw material C 280g, carry out at normal temperatures air-flow and mix 30 minutes.
Take dried MCMB 5520g, add the mixture 480g of above-mentioned raw materials B and C, at 300 ℃ of temperature, be uniformly mixed 90 minutes; Temperature is raised to 450 ℃ again, strong mixing maintains 240 minutes; Continue slowly to be warming up to 600 ℃, stir and maintain 240 minutes; Finally at 1800 ℃ of temperature, carry out charing.
With LIR2430 type button cell, do experiment, gained negative material loading capacity is 346.3mAh/g, and discharging efficiency is 95.1%, as shown in table 1.
embodiment 6:
Take MCMB raw material A 8000g, at 3200 ℃ of temperature, carry out greying, be immersed in 0.6mol/L H after cooling
2sO
4in solution, be warming up to 80 ℃, after soaking 6h, wash with water and be filtered into neutrality, dry at 120 ℃ of temperature.
Take dried MCMB 5400g, add epoxy resin raw material C 600g, at 300 ℃ of temperature, be uniformly mixed 90 minutes; Temperature is raised to 450 ℃ again, strong mixing maintains 240 minutes; Continue slowly to be warming up to 600 ℃, stir and maintain 240 minutes; Finally at 1300 ℃ of temperature, carry out charing.
With LIR2430 type button cell, do experiment, gained negative material loading capacity is 342.2mAh/g, and discharging efficiency is 94.5%, as shown in table 1.
embodiment 7:
Take MCMB raw material A 8000g, at 3000 ℃ of temperature, carry out greying, be immersed in 0.6mol/L H after cooling
2sO
4in solution, be warming up to 60 ℃, after soaking 6h, wash with water and be filtered into neutrality, dry at 120 ℃ of temperature.
Take boron nitride raw B 120g, resol raw material C 280g, carry out at normal temperatures air-flow and mix 30 minutes.
Take dried MCMB 5520g, add the mixture 480g of above-mentioned raw materials B and C, at 300 ℃ of temperature, be uniformly mixed 90 minutes; Temperature is raised to 450 ℃ again, strong mixing maintains 240 minutes; Continue slowly to be warming up to 600 ℃, stir and maintain 240 minutes; Finally at 1600 ℃ of temperature, carry out charing.
With LIR2430 type button cell, do experiment, gained negative material loading capacity is 334.2mAh/g, and discharging efficiency is 94.8%, as shown in table 1.
embodiment 8:
Take MCMB raw material A 8000g, at 2800 ℃ of temperature, carry out greying, be immersed in 0.6mol/L H after cooling
2sO
4in solution, be warming up to 80 ℃, after soaking 8h, wash with water and be filtered into neutrality, dry at 120 ℃ of temperature.
Take boron nitride raw B 80g, epoxy resin raw material C 320g, carry out at normal temperatures air-flow and mix 30 minutes.
Take dried MCMB 5760g, add the mixture 240g of above-mentioned raw materials B and C, at 300 ℃ of temperature, be uniformly mixed 90 minutes; Temperature is raised to 450 ℃ again, strong mixing maintains 240 minutes; Continue slowly to be warming up to 600 ℃, stir and maintain 240 minutes; Finally at 1800 ℃ of temperature, carry out charing.
With LIR2430 type button cell, do experiment, gained negative material loading capacity is 328.4mAh/g, and discharging efficiency is 94.6%, as shown in table 1.
embodiment 9:
Take MCMB raw material A 8000g, at 2800 ℃ of temperature, carry out greying, be immersed in 0.8mol/L H after cooling
2sO
4in solution, be warming up to 80 ℃, after soaking 6h, wash with water and be filtered into neutrality, dry at 120 ℃ of temperature.
Take dried MCMB 5760g, add resol raw material C 240g, at 300 ℃ of temperature, be uniformly mixed 90 minutes; Temperature is raised to 450 ℃ again, strong mixing maintains 240 minutes; Continue slowly to be warming up to 600 ℃, stir and maintain 240 minutes; Finally at 1100 ℃ of temperature, carry out charing.
With LIR2430 type button cell, do experiment, gained negative material loading capacity is 324.0mAh/g, and discharging efficiency is 93.6%, as shown in table 1.
subordinate list 1
button cell test data summary sheet
Claims (5)
1. the production method of an intermediate-phase carbon negative material, concrete production technique is:
(a) take the MCMB that the meta particle diameter is 5 ~ 18 μ m is raw material A;
(b) take the boron nitride micro mist that the meta particle diameter is≤5 μ m is raw material B;
(c) take the resin that the meta particle diameter is≤5 μ m is raw material C;
(d) ultrahigh-temperature graphitization processing: get above-mentioned raw materials A, at 2800 ~ 3200 ℃, carry out graphitization processing;
(e) oxide treatment: will complete the ultrahigh-temperature graphitization processing and cooling after the raw material A that obtains put into the H that concentration is 0.5 ~ 1mol/L
2sO
4in solution, be warming up to 60 ~ 80 ℃, soak 5 ~ 8h;
(f) neutralization and drying treatment: take out above-mentioned at H
2sO
4the raw material A of soaking in solution, first wash with water and be filtered into neutrality, then dry at 120 ℃ of temperature;
(h) coat and process: first raw material B and raw material C are carried out to the air-flow mixing in the ratio of (20-30)/(80 ~ 70) under the normal temperature state, then in (B+C)/A=(3 ~ 15)/ratio of (97 ~ 85) is uniformly mixed 300 ~ 600 ℃ of temperature, finally at 1300 ℃ ~ 1800 ℃, carries out the charing processing; Perhaps first by raw material in C/A=(3 ~ 15)/ratio of (97 ~ 85) is uniformly mixed 300 ~ 600 ℃ of temperature, finally at 1000 ℃ ~ 1300 ℃, carries out the charing processing.
2. the production method of a kind of intermediate-phase carbon negative material as claimed in claim 1 is characterized in that: described MCMB is petroleum asphalt based or the coal-tar pitch base obtains the mesophase globule of homogeneous nucleation through thermolysis and thermal polycondensation reaction.
3. the production method of a kind of intermediate-phase carbon negative material as claimed in claim 1, it is characterized in that: described resin is resol or epoxy resin.
4. the production method of a kind of intermediate-phase carbon negative material as claimed in claim 1, it is characterized in that: described boron nitride is hexagonal boron nitride.
5. the production method of a kind of intermediate-phase carbon negative material as claimed in claim 1, is characterized in that: described employing twin screw or the two ribbon alr mode of being uniformly mixed.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103996855A (en) * | 2014-05-27 | 2014-08-20 | 大连宏光锂业股份有限公司 | Production method of interphase carbon-coated graphite negative electrode material |
| CN104779396A (en) * | 2015-04-22 | 2015-07-15 | 大连宏光锂业股份有限公司 | Production method of lithium ion composite graphite cathode material |
| CN105236395A (en) * | 2015-09-01 | 2016-01-13 | 大连宏光锂业股份有限公司 | Production method of composite artificial graphite anode material |
| CN105923619A (en) * | 2016-04-25 | 2016-09-07 | 秦皇岛华瑞煤焦化工有限公司 | Production method for carbon microspheres and used device thereof |
| CN112028064A (en) * | 2020-08-18 | 2020-12-04 | 赣州市瑞富特科技有限公司 | Preparation method of micro hollow sphere graphite negative electrode material |
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| CN112028064A (en) * | 2020-08-18 | 2020-12-04 | 赣州市瑞富特科技有限公司 | Preparation method of micro hollow sphere graphite negative electrode material |
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