CN109796000B - Preparation method of mixed precursor pyrolytic carbon negative electrode material for low-temperature power battery - Google Patents
Preparation method of mixed precursor pyrolytic carbon negative electrode material for low-temperature power battery Download PDFInfo
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Abstract
The invention discloses a preparation method of a mixed precursor pyrolytic carbon cathode material for a low-temperature power battery, which comprises the following steps of: dissolving resin in a solvent to prepare a resin solution, adding an additive, uniformly stirring to obtain a stirring product, drying, pretreating, pyrolyzing, cooling, grinding and sieving the pyrolysis product to obtain the mixed precursor pyrolytic carbon negative electrode material for the low-temperature power battery. The method is simple to operate, the raw materials are common low-cost materials such as resin and the like, and the compaction density is improved to 1.5-2.0 g/cm3Is beneficial to improving the volume energy density, and the specific surface area of the prepared material is controlled to be 1-10m2The first coulombic efficiency is over 79 percent, the interlayer spacing is more than 0.37nm, the safety performance is good, and the method is suitable for full battery industrialization; and the compacted density is high.
Description
The technical field is as follows:
the invention belongs to the technical field of new energy, and particularly relates to a preparation method of a mixed precursor pyrolytic carbon negative electrode material for a low-temperature power battery.
Background art:
with the increasing interest in the exhaustion of non-renewable petrochemical fuels such as petroleum, natural gas, etc., air pollution and room temperature effects become global issues. The solution of energy problems and the realization of sustainable development of low-carbon economic roads have become common consensus of countries in the world. New energy automobile mainly relies on secondary battery energy storage, and secondary battery can charge and discharge repeatedly, and efficient, environmental suitability is strong, has better economic practicality, becomes the main direction of energy storage research.
While low temperatures are the largest bottleneck encountered by power batteries, boston batteries find that low temperatures have a fatal effect on battery life: the battery with the capacity of 3.5Ah rapidly attenuates the electric quantity to 0.5Ah at the temperature of minus 10 ℃ and is basically discarded. Similar problems are encountered in northern europe with the best electric cars tesla. The low temperature is a big enemy of the electric automobile, and the electric automobile is difficult to popularize in alpine regions without solving the problem.
The charge and discharge of the battery belong to electrochemical reactions, since the charge and discharge are chemically related and have a great relationship with temperature, the reaction is obviously slowed down along with the temperature reduction, so that the discharge power is reduced, and even the cycle performance is obviously reduced. Compared with the influence of low temperature on the battery electrode material, the negative electrode is subjected to lithium ionThe decrease in the sub-diffusion coefficient is more pronounced, which has an effect that exceeds the positive electrode, the increase in the interface resistance and the decrease in the conductivity of the electrolyte. Therefore, the development of the lithium ion battery cathode material with high diffusion coefficient becomes one of the most critical factors for solving the low temperature performance. Recent studies indicate that small interlayer spacing is a key factor for limiting low-temperature performance, and large interlayer spacing is beneficial to lithium ion diffusion. The common graphite product has small interlayer spacing (0.335nm) and is not suitable for low-temperature environment. The pyrolytic carbon product has larger interlayer spacing, but the pyrolytic carbon is usually used as active carbon and has large specific surface area (more than 10 m)2/g), which is difficult to control, resulting in low coulombic efficiency for the first time, and too high cost of the pyrolytic carbon material on the market, which are not suitable for full battery industrialization.
The invention content is as follows:
the invention aims to provide a preparation method of a mixed precursor pyrolytic carbon negative electrode material for a low-temperature power battery, aiming at the defects of the prior art, and the preparation method is simple, low in cost, good in low-temperature performance, small in specific surface area, large in interlayer spacing and high in first charge-discharge efficiency.
In order to realize the purpose, the invention adopts the following technical scheme:
a preparation method of a mixed precursor pyrolytic carbon negative electrode material for a low-temperature power battery comprises the following steps:
(1) dissolving resin in a solvent to prepare a resin solution, wherein the mass ratio of the resin to the solvent in the resin solution is 1 (0.1-20);
(2) dissolving an additive in a resin solution, and uniformly stirring to obtain a stirred product, wherein the mass ratio of the additive to the resin in the resin solution is 1: (1-50);
(3) drying the stirred product, and then pretreating in an inert atmosphere to obtain a pretreated product;
(4) and pyrolyzing the pretreated product to obtain a pyrolysis product, cooling the pyrolysis product, grinding the cooled pyrolysis product, and sieving the cooled pyrolysis product with a 325-mesh sieve to obtain the mixed precursor pyrolytic carbon negative electrode material for the low-temperature power battery, wherein the pyrolysis operation is carried out under the protection of inert gas, the pyrolysis temperature is 800-2000 ℃, and the high-temperature pyrolysis time is 2-10 hours.
In the step (1), the resin includes, but is not limited to, one or a mixture of acrylic resin, epoxy resin, polyurethane, alkyd resin, asphalt, phenolic resin, polyvinyl alcohol, vitamin, urea resin, melamine formaldehyde resin, poly-N-vinyl pyrrolidone, polyethylene oxide and silicone resin.
In the step (1), the solvent includes, but is not limited to, one or more of deionized water, ethanol, acetone, benzene, toluene, tetrahydrofuran, carbon tetrachloride, diethyl ether, isopropyl ether, n-butyl ether, trichloroethylene, diphenyl ether, dichloromethane, dichloroethane, carbon disulfide, cyclohexane, hexane, kerosene, and petroleum ether.
In the step (2), the additive is one or more of glucose, fructose, sucrose, starch, lactose, polyethylene glycol, glycerol, lignin, amino acid, nucleotide, protein, dimethyl phthalate, dihexyl phthalate, dibutyl phthalate, dioctyl adipate or didecyl adipate, ethylene glycol, propylene glycol, polyethylene glycol, polypropylene glycol, pentaerythritol, diethylene glycol, propylene glycol, 1, 4-butanediol and citric acid.
And (3) distilling the stirred product to dry, wherein the distillation temperature is 50-300 ℃, the pretreatment is carried out in an inert atmosphere of argon or nitrogen, the temperature is 120-350 ℃, and the time is 1-20 hours.
In the step (4), the specific surface area of the prepared mixed precursor pyrolytic carbon negative electrode material for the low-temperature power battery is 1-10m2A layer spacing of 0.37 to 0.50nm, a high compaction density of 1.5 to 2.0g/cm3The initial coulombic efficiency is 79-99%, the reversible capacity of 0.1C multiplying power in normal temperature test is 250-500 mAh/g, the reversible capacity of 200-400 mAh/g in 20 ℃ test, and the reversible capacity of 30-60% of the charge-discharge capacity in normal temperature test at 70 ℃.
The mixed precursor pyrolytic carbon negative electrode material for the low-temperature power battery prepared by any method.
The invention has the beneficial effects that:
(1) the preparation method adopted by the mixed precursor pyrolytic carbon negative electrode material for the low-temperature power battery has the advantages of common equipment, low manufacturing cost and simple operation, is beneficial to large-scale production and is extremely easy to popularize.
(2) The main raw materials of the mixed precursor pyrolytic carbon negative electrode material for the low-temperature power battery are common low-cost materials such as resin and the like, and the obtained product has relatively low cost and is suitable for large-scale application; the adopted additive increases the compaction density to 1.5-2.0 g/cm3While controlling the specific surface area of the material to be 1-10m2(iv)/g, such that the first coulombic efficiency of the material exceeds 79%.
(3) The mixed precursor pyrolytic carbon negative electrode material for the low-temperature power battery has larger interlayer spacing larger than 0.37nm, is in an amorphous state, has short ion diffusion path, and is beneficial to low-temperature lithium ion diffusion; meanwhile, lithium is not separated out under the condition of low temperature, the safety performance is good, and the method is suitable for full battery industrialization; and the compaction density is high, which is beneficial to improving the volume energy density.
The specific implementation mode is as follows:
the following describes a specific embodiment of the present invention with reference to examples to further illustrate the technical effects of the technical solutions of the present invention, and the embodiments of the present invention are not limited to the contents described in the examples.
Example 1
A preparation method of a mixed precursor pyrolytic carbon negative electrode material for a low-temperature power battery comprises the following steps:
(1) dissolving 5g of asphalt into 10g of tetrahydrofuran, and stirring for 200r/min by an electric stirrer to prepare a resin solution;
(2) dissolving 0.5g of glycerol in the resin solution obtained in the step (1), and stirring uniformly by electrically stirring for 200 r/min;
(3) removing the solvent from the product obtained in the step (2) at 66 ℃ by adopting a thermal distillation method, then transferring the sample into a tubular atmosphere furnace, and pretreating under the protection of nitrogen with the purity of 99.97 percent at the temperature of 120 ℃ for 1 h;
(4) and (4) introducing nitrogen with the purity of 99.97% into the tube furnace in the step (3), heating to 800 ℃, preserving heat for 2 hours, cooling, grinding, and sieving with a 325-mesh sieve to obtain the mixed precursor pyrolytic carbon negative electrode material for the low-temperature power battery.
And uniformly mixing the obtained mixed precursor pyrolytic carbon negative electrode material, conductive agent acetylene black and binder PVDF according to the mass ratio of 9:0.5:0.5, preparing an electrode plate by using copper foil as a current collector, preparing a metal lithium plate as a counter electrode, and assembling the electrolyte as a commercially available low-temperature electrolyte to form a half battery, and performing constant-current charge and discharge tests on the half battery by adopting a Shenzhen New Weier battery test system, wherein the charge and discharge voltage interval is 0.01-2.0V. The specific surface area of the detected material was 10m2A layer spacing of 0.50nm, a compacted density of 1.5g/cm3The first coulombic efficiency is 79 percent, the reversible capacity of 0.1C multiplying power in normal temperature test is 500mAh/g, the reversible capacity of minus 20 ℃ test is 300mAh/g, and the reversible capacity of minus 70 ℃ test is 50 percent of the charge-discharge capacity in normal temperature test.
Example 2
A preparation method of a mixed precursor pyrolytic carbon negative electrode material for a low-temperature power battery comprises the following steps:
(1) dissolving 5g of phenolic resin into 100g of ethanol, and stirring for 200r/min under an electric condition to obtain a resin solution;
(2) dissolving 0.1g of glucose in the resin solution obtained in the step (1), and stirring uniformly at 200r/min by electric stirring;
(3) removing the solvent from the product obtained in the step (2) by adopting a thermal distillation method at 80 ℃, then transferring the dried sample into a tubular atmosphere furnace, and pretreating under the protection of nitrogen at 200 ℃ for 10 hours;
(4) and (4) introducing argon with the purity of 99.97% into the tube furnace in the step (3), heating to 800 ℃, preserving heat for 2 hours, cooling, grinding, and sieving with a 325-mesh sieve to obtain the mixed precursor pyrolytic carbon negative electrode material for the low-temperature power battery.
Uniformly mixing the obtained mixed precursor pyrolytic carbon negative electrode material, conductive agent acetylene black and binder PVDF according to the mass ratio of 9:0.5:0.5, preparing an electrode plate by taking copper foil as a current collector, taking a metal lithium plate as a counter electrode and taking electrolyte as low-temperature electrolyte sold in the market, assembling into a half-cell, and adopting Shenzhen New Willer electricityThe cell test system performs constant-current charge and discharge test on the half-cell, and the charge and discharge voltage interval is 0.01-2.0V. The specific surface area of the detected material was 5m2(g), interlayer spacing of 0.50nm, and compacted density of 1.5g/cm3The first coulombic efficiency is 80%, the reversible capacity of 0.1C multiplying power in normal temperature test is 500mAh/g, the reversible capacity of 20 ℃ is 400mAh/g, and the reversible capacity of 70 ℃ is 50% of the charge-discharge capacity in normal temperature test.
Example 3
A preparation method of a mixed precursor pyrolytic carbon negative electrode material for a low-temperature power battery comprises the following steps:
(1) dissolving 5g of epoxy resin into 50g of deionized water, and electrically stirring for 200r/min to prepare a resin solution;
(2) dissolving 5g of sucrose in the resin solution obtained in the step (1), and stirring uniformly at 200r/min under electric stirring;
(3) removing the solvent from the product obtained in the step (2) by adopting a thermal distillation method at 100 ℃, then transferring the dried sample into a tubular atmosphere furnace, and pretreating under the protection of nitrogen at 300 ℃ for 5 hours;
(4) and (4) introducing nitrogen with the purity of 99.97% into the tube furnace in the step (3), heating to 2000 ℃, preserving heat for 2 hours, cooling, grinding, and sieving with a 325-mesh sieve to obtain the mixed precursor pyrolytic carbon negative electrode material for the low-temperature power battery.
Uniformly mixing the obtained mixed precursor pyrolytic carbon negative electrode material, conductive agent acetylene black and binder PVDF according to the mass ratio of 9:0.5:0.5, preparing an electrode plate by using copper foil as a current collector, using a metal lithium plate as a counter electrode and using electrolyte as commercially available low-temperature electrolyte to assemble a half-cell, and performing constant-current charge and discharge test on the half-cell by adopting a Shenzhen New Will cell test system, wherein the charge and discharge voltage interval is 0.01-2.0V. The specific surface area of the material to be tested was 1.5m2(g), interlayer spacing of 0.38nm, and compacted density of 1.8g/cm3The first coulombic efficiency is 95%, the reversible capacity tested at 0.1C multiplying power at normal temperature is 350mAh/g, the reversible capacity tested at-20 ℃ is 200mAh/g, and the reversible capacity tested at-70 ℃ is 30% of the charge-discharge capacity at normal temperature.
Example 4
A preparation method of a mixed precursor pyrolytic carbon negative electrode material for a low-temperature power battery comprises the following steps:
(1) dissolving 5g of urea-formaldehyde resin into 1g of acetone, and stirring uniformly by stirring for 200 r/min;
(2) dissolving 2.5g of polyethylene glycol in the resin solution obtained in the step (1), and stirring uniformly at 200r/min under electric stirring;
(3) removing the solvent from the product obtained in the step (2) by adopting a thermal distillation method at 100 ℃, then transferring the dried sample into a tubular atmosphere furnace, and pretreating under the protection of argon at 350 ℃ for 5 hours;
(4) and (4) introducing argon with the purity of 99.97% into the tube furnace in the step (3), heating to 900 ℃, preserving heat for 8 hours, cooling, grinding, and sieving with a 325-mesh sieve to obtain the mixed precursor pyrolytic carbon negative electrode material for the low-temperature power battery.
Uniformly mixing the obtained mixed precursor pyrolytic carbon negative electrode material, conductive agent acetylene black and binder PVDF according to the mass ratio of 9:0.5:0.5, preparing an electrode plate by using copper foil as a current collector, using a metal lithium plate as a counter electrode and using electrolyte as commercially available low-temperature electrolyte to assemble a half-cell, and performing constant-current charge and discharge test on the half-cell by adopting a Shenzhen New Will cell test system, wherein the charge and discharge voltage interval is 0.01-2.0V. The specific surface area of the detected material was 8m2(g), interlayer spacing of 0.41nm, and compacted density of 1.6g/cm3The first coulombic efficiency is 85%, the reversible capacity of 0.1C multiplying power in normal temperature test is 460mAh/g, the reversible capacity of minus 20 ℃ test is 280mAh/g, and the reversible capacity of minus 70 ℃ test is 40% of the normal temperature charge-discharge capacity.
Example 5
A preparation method of a mixed precursor pyrolytic carbon negative electrode material for a low-temperature power battery comprises the following steps:
(1) dissolving 5g of polyvinyl alcohol into 50g of toluene, and stirring uniformly by electric stirring for 200 r/min;
(2) dissolving 2g of diethylene glycol in the resin solution obtained in the step (1), and stirring uniformly by electrically stirring for 200 r/min;
(3) removing the solvent from the product obtained in the step (2) by adopting a thermal distillation method at 150 ℃, then transferring the dried sample into a tubular atmosphere furnace, and pretreating under the protection of nitrogen at 120 ℃ for 10 hours;
(4) and (4) introducing nitrogen with the purity of 99.97% into the tube furnace in the step (3), heating to 1500 ℃, preserving heat for 5 hours, cooling, grinding, and sieving with a 325-mesh sieve to obtain the mixed precursor pyrolytic carbon negative electrode material for the low-temperature power battery.
Uniformly mixing the obtained mixed precursor pyrolytic carbon negative electrode material, conductive agent acetylene black and binder PVDF according to the mass ratio of 9:0.5:0.5, preparing an electrode plate by using copper foil as a current collector, using a metal lithium plate as a counter electrode and using electrolyte as commercially available low-temperature electrolyte to assemble a half-cell, and performing constant-current charge and discharge test on the half-cell by adopting a Shenzhen New Will cell test system, wherein the charge and discharge voltage interval is 0.01-2.0V. The specific surface area of the detected material was 8.2m2(g), interlayer spacing of 0.39nm, and compacted density of 1.7g/cm3The first coulombic efficiency is 80%, the reversible capacity of a 0.1C multiplying power normal temperature test is 380mAh/g, the reversible capacity of a-20 ℃ test is 200mAh/g, and the reversible capacity of a-70 ℃ test is 35% of the normal temperature charge-discharge capacity.
Example 6
A preparation method of a mixed precursor pyrolytic carbon negative electrode material for a low-temperature power battery comprises the following steps:
(1) dissolving 5g of silicon resin into 80g of dichloroethane, and stirring uniformly by stirring for 200r/min electrically;
(2) dissolving 3.5g of dihexyl phthalate in the resin solution obtained in the step (1), and stirring uniformly at 200r/min under electric stirring;
(3) removing the solvent from the product obtained in the step (2) by adopting a thermal distillation method at 300 ℃, then transferring the dried sample into a tubular atmosphere furnace, and pretreating under the protection of nitrogen at 350 ℃ for 3 hours;
(4) and (4) introducing argon with the purity of 99.97% into the tube furnace in the step (3), heating to 1000 ℃, preserving heat for 8 hours, cooling, grinding, and sieving with a 325-mesh sieve to obtain the mixed precursor pyrolytic carbon negative electrode material for the low-temperature power battery.
Mixing the obtained mixed precursor pyrolytic carbon cathode material with conductive agent acetylene black and adhesiveAnd uniformly mixing the caking agents PVDF according to the mass ratio of 9:0.5:0.5, using copper foil as a current collector to prepare an electrode plate, using a metal lithium plate as a counter electrode, using electrolyte as low-temperature electrolyte sold in the market, assembling the electrode plate and the lithium plate into a half battery, and performing constant-current charge and discharge test on the half battery by adopting a Shenzhen New Will battery test system, wherein the charge and discharge voltage interval is 0.01-2.0V. The specific surface area of the material to be tested was 5.5m2(g), interlayer spacing of 0.43nm, and compacted density of 1.55g/cm3The first coulombic efficiency is 91%, the reversible capacity tested at 0.1C multiplying power at normal temperature is 420mAh/g, the reversible capacity tested at-20 ℃ is 200mAh/g, and the reversible capacity tested at-70 ℃ is 38% of the charge-discharge capacity at normal temperature.
Claims (2)
1. A preparation method of a mixed precursor pyrolytic carbon negative electrode material for a low-temperature power battery is characterized by comprising the following steps of:
(1) dissolving resin in a solvent to prepare a resin solution, wherein the resin and the solvent in the resin solution are in a mass ratio of 1 (0.1-20), the resin is one of epoxy resin, asphalt, polyvinyl alcohol, urea-formaldehyde resin or silicon resin, and the solvent is one of deionized water, acetone, toluene, tetrahydrofuran or dichloroethane;
(2) dissolving an additive in a resin solution, and uniformly stirring to obtain a stirred product, wherein the mass ratio of the additive to the resin in the resin solution is 1: (1-50), wherein the additive is one of polyethylene glycol, glycerol, dihexyl phthalate or diethylene glycol;
(3) drying the stirred product, and then pretreating in an inert atmosphere at the temperature of 120-350 ℃ for 1-20 h to obtain a pretreated product;
(4) pyrolyzing the pretreated product to obtain a pyrolysis product, cooling the pyrolysis product, grinding the cooled pyrolysis product to be fine, and sieving the cooled pyrolysis product with a 325-mesh sieve to obtain the mixed precursor pyrolytic carbon negative electrode material for the low-temperature power battery, wherein the pyrolysis operation is carried out under the protection of inert gas, the pyrolysis temperature is 800-2000 ℃, the high-temperature pyrolysis time is 2-10 h, and the specific surface area of the prepared mixed precursor pyrolytic carbon negative electrode material for the low-temperature power battery is 1.5-10 m2G, interlayer spacing of0.37 to 0.50nm, and a compacted density of 1.5 to 2.0g/cm3The initial coulombic efficiency is 79-99%, the reversible capacity of 0.1C multiplying power in normal temperature test is 250-500 mAh/g, the reversible capacity of 200-400 mAh/g in 20 ℃ test, and the reversible capacity of 30-60% of the charge-discharge capacity in normal temperature test at 70 ℃.
2. The preparation method of the mixed precursor pyrolytic carbon negative electrode material for the low-temperature power battery according to claim 1, wherein in the step (3), the stirring product is dried by distillation at the distillation temperature of 50-300 ℃, and the pretreatment is performed in an inert atmosphere of argon or nitrogen.
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| CN102723492A (en) * | 2012-06-28 | 2012-10-10 | 深圳市贝特瑞新能源材料股份有限公司 | Method for preparing hard carbon material and lithium ion battery |
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