CN110518243A - Lignin is preparing the application in lithium battery graphite cathode material - Google Patents
Lignin is preparing the application in lithium battery graphite cathode material Download PDFInfo
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- CN110518243A CN110518243A CN201910769546.6A CN201910769546A CN110518243A CN 110518243 A CN110518243 A CN 110518243A CN 201910769546 A CN201910769546 A CN 201910769546A CN 110518243 A CN110518243 A CN 110518243A
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- lignin
- lithium battery
- cathode material
- biomass
- graphite cathode
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
- H01M4/602—Polymers
- H01M4/606—Polymers containing aromatic main chain polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses lignin to prepare the application in lithium battery graphite cathode material, the preparation process of the lignin are as follows: it is feed liquid after hydrolyzing that the reaction solution after reaction, which is hydrolyzed, in biomass in an acidic solution, the water of 2-10 volume times is added in feed liquid after gained hydrolysis, stirring, there is solid precipitation, filtering, filter residue are dried after clear water washs to get the lignin.By means of the present invention can liquefy completely biomass hydrolysis, then the lignin that biomass liquefying hydrolysis generates is extracted, the aromaticity of the lignin is high, sulfur content is low, when being applied to prepare lithium battery graphite cathode material, there are preferable first discharge specific capacity, for the first time performance parameters such as coulombic efficiency, powder compacted density, degree of graphitization and fixed carbon content.
Description
Technical field
The present invention relates to lignin to prepare the application in lithium battery graphite cathode material.
Background technique
Mainly mass storage is in the life with us in the form of agricultural and forest trimmings for biomass, domestic biomass
Waste material derives from the stalk of the crops such as soya corn, while Furniture Factory also generates raw a large amount of sawdust during manufacturing furniture
And wood shavings, it deals with improperly and will also result in environmental pollution.Chinese stalk theoretical yield collects stock number up to 8.84 hundred million tons within 2017
700,000,000 tons big, wherein arriving rice straw 25%, wheat straw 18.3%, corn stalk accounts for about 33%, and cotton straw 3%, rape flower and peanut about turn 4.4%.
It is mainly distributed on Liaoning, Jilin, 13, Heilungkiang etc. major grain producing area, stalk resource amount accounted for 70% of total amount or more.
Usual agricultural biomass waste material has several processing methods: 1) by on-site incineration returning to the field, but causing serious
Air pollution, so country is special to put into effect " stalk prohibit burn and comprehensive utilization management method ", to forbid open incineration stalk.2)
Biomass power generation, agricultural biomass waste material direct plunge into electricity generation boiler.Although this method solves pollution caused by on-site incineration
Problem, but biomass economy rate is low.3) biomass through pyrolysis method (such as Chinese patent 201210048116.3, by biomass thermal
Cracking process generate biomass coke tar): under anoxic condition by (400-600 degrees Celsius) of high temperature processing, make biomass decomposition at
Biomass charcoal, biomass coke tar or pyrolysis gas, this method effectively make biomass fast decoupled, generate it is different can
Use fuel.Can do that fuel uses mainly: the pyrolysis gas of biomass and biomass coke tar of low heat value.Although this method realizes
Biomass is to the conversion of bio-fuel, but the added value of biofuel products is lower.
But in the prior art, there are no about " using biomass as starting material, preparing the lithium battery graphite of high added value
The document report of negative electrode material ".And in the prior art, generally use petroleum coke as the raw material for preparing artificial graphite, still
Petroleum coke has the following deficiencies: 1, content of beary metal height, 2, sulfur content height.Secondly, natural graphite is also as cathode of lithium battery
The common used material of material, but the impurity in natural material is more, separation and Extraction impurity needs to keep away using toxic chlorine
That exempts from increases the complexity of technique.Furthermore petroleum and natural graphite are all non-renewable resources, petroleum coke is largely used
Global warming can be brought, the problems such as environmental pollution.
Therefore, the novel new method for preparing lithium battery graphite cathode material of one kind is developed to be of great significance.
Summary of the invention
For above-mentioned technical problem of the existing technology, the purpose of the present invention is to provide lignin to prepare lithium battery
Application in graphite cathode material, by means of the present invention can liquefy completely biomass hydrolysis, then extract biomass liquid
Change the lignin that hydrolysis generates, the aromaticity of the lignin is high, sulfur content is low, is being applied to prepare lithium battery graphite cathode material
When, there is preferable performance parameter.
The lignin is preparing the application in lithium battery graphite cathode material, it is characterised in that the system of the lignin
Standby process are as follows: it is feed liquid after hydrolyzing that the reaction solution after reaction, which is hydrolyzed, in biomass in an acidic solution, after gained hydrolysis
The water of 2-10 volume times is added in feed liquid, stirring has solid precipitation, filters, and filter residue is dried after clear water washs to get the wood
Quality.
The lignin is preparing the application in lithium battery graphite cathode material, it is characterised in that with lignin be original
The step of expecting, preparing lithium battery graphite cathode material are as follows:
1) lignin is mixed with stabiliser solution by 1: 2 ~ 12 mass ratio, stands and stablizes 3 ~ 6 hours at 40 ~ 70 DEG C
Afterwards, it filters, filter residue and drying obtains stablizing lignin；
2) lignin will be stablized obtained by step 1) to be placed in rotary kiln, under nitrogen protection atmosphere, and in 1200 ~ 1500 DEG C of temperature
Lower calcining 2 ~ 4 hours, obtains calcined lignin；
3) calcined lignin obtained by step 2 is placed in graphitizing furnace, under argon atmosphere, and in 2500 ~ 2800
DEG C temperature lower calcination 3 ~ 15 hours, subsequent cooled to room temperature was to get the lithium battery graphite cathode material.
The lignin is preparing the application in lithium battery graphite cathode material, it is characterised in that the stabiliser solution
For the ammonium dibasic phosphate aqueous solution of mass concentration 10% ~ 20%.
The lignin is preparing the application in lithium battery graphite cathode material, it is characterised in that the biomass is in acid
Property solution in be hydrolyzed reaction after reaction solution, be to be prepared according to following procedure:
S1: biological particles be added reaction kettle in, under anaerobic state be added water cosolvent, heated under stirring 150 DEG C-
220 DEG C, lewis acid is added, reaction 20-40 minutes, the biomass mixed liquor after must hydrolyzing is hydrolyzed；
S2: into the biomass mixed liquor of step S1 plus alkali neutralization adjusts pH to 4.5-8, and cooled and filtered removes what neutralization obtained
Ash content in sediment and biomass is to get the reaction solution.
The lignin is preparing the application in lithium battery graphite cathode material, it is characterised in that biomass in step S1
For particle water content less than 8%, grain diameter is less than 25mm, and biomass is timber, stalk, paper product, pine, careless class, rice husk, sweet
Bagasse, cotton, jute, flax, bamboo, sisal hemp, abaca, straw, any one or a few mixture in corncob.
The lignin is preparing the application in lithium battery graphite cathode material, it is characterised in that in step S1, water is total
The water and tetrahydrofuran mixed liquor that solvent is mass ratio 1:1-1:5.
The lignin is preparing the application in lithium battery graphite cathode material, it is characterised in that in step S1, biology
The mass ratio of matter and water cosolvent is 1: 2-7；The lewis acid is at least one of sulfuric acid, hydrochloric acid, nitric acid, the road
The quality of Lewis acid is the 0.3%-3% of water cosolvent quality.
Compared with the existing technology, the beneficial effect that the present invention obtains is:
1) reaction solution after reaction is hydrolyzed in an acidic solution and is denoted as feed liquid after hydrolysis for biomass, after the hydrolysis in feed liquid
Such as containing biomass hydrolysate: the lignin after the sugar of C5-C6, furfural, levulic acid and hydrolysis, the wood after the hydrolysis
Quality is adsorption.A certain amount of water mixing is added after to hydrolysis in feed liquid, lignin can be reduced in the water
Solubility after solution in feed liquid, and then (biomass hydrolysates such as sugar, furfural, levulic acid of C5-C6 are basic for precipitation lignin
Dissolution in feed liquid, can be used as the use of the purposes such as liquid fuel, plant nutrition liquid after hydrolyzing.Wherein the precipitation purity of lignin and
Quality is higher, is conducive to prepare downstream high value-added product).The lignin of precipitation is after clear water is cleaned and dried, institute
Lignin product aromaticity it is higher and the sulfur content of gained lignin, ash content are lower, it is high to be particularly suitable for preparation downstream
The graphite material of added value.
2) when the lignin that the present invention extracts is used to prepare lithium battery graphite cathode material, there is the ratio that preferably discharges for the first time
Capacity, for the first time coulombic efficiency, powder compacted density, the performance parameter of degree of graphitization and fixed carbon content, meet cathode of lithium battery
The use standard of material.Secondly, method of the invention can reduce lithium battery efficiently using renewable resources such as biomass straws
Consumption of the negative electrode material to natural resources improves economic benefit while rate reduces environmental pollution.
Specific embodiment
The present invention is further explained in the light of specific embodiments, but the scope of protection of the present invention is not limited thereto.
Embodiment 1:
The method for preparing lithium battery graphite cathode material using lignin, comprising the following steps:
1) 20 kilograms of particles of pine (particles of pine water content is less than 25mm less than 8%, grain diameter), 20 are added in a kettle
Kg of water, 60 kilograms of tetrahydrofurans and the 600g concentrated sulfuric acid are uniformly mixed (concentrated sulfuric acid mass concentration is 98%).In a nitrogen atmosphere,
Reaction kettle is stirred and heated to 180 DEG C and reacts 20 minutes, and the cellulose, hemicellulose, lignin in confirmation particles of pine are by liquid
After changing hydrolysis, the sulfuric acid in the calcium hydroxide slurry of 1 kilogram of 50%w/w concentration and in solution is added, and be obtained by filtration 100 kilograms
Reaction solution；
2) 100 kilograms of reaction solutions obtained by step 1) and 250 kg of water are mixed and stirred for uniformly, there is solid precipitation, filtered, filter residue
It is dry after being rinsed with 500 kg of water, obtain 10 kilograms of lignin；
3) 10 kilograms of lignin obtained by step 2 are mixed with 100 kilograms of mass concentration for 10% ammonium dibasic phosphate aqueous solution, and
It stands and stablizes 4 hours at a temperature of 60 DEG C, then filter, filter residue drying obtains 10 kilograms of stable lignin；
4) 10 kilograms of stable lignin obtained by step 3) are placed in rotary furnace, under nitrogen protection atmosphere, calcine 4 in 1400 DEG C
Hour, obtain 5 kilograms of calcined lignin；
5) 5 kilograms of calcined lignin obtained by step 4) are placed in graphitizing furnace, under argon atmosphere, in 2700 DEG C
Calcining 12 hours, subsequent cooled to room temperature is to get 3 kilograms of lithium battery graphite cathode materials.
Be tested for the property to lignin obtained by 1 step 2 of embodiment: testing its aromaticity by 21461 method of ISO is
85%, testing its sulfur content according to GB/T2286 method is 0.01%, and testing its ash content by 2001 method of GB/T is 0.1%.
In the prior art, whether evaluation lithium battery graphite cathode material complies with standard, and need to usually meet following 5 aspects
Performance detection standard:
1 first discharge specific capacity: the first discharge specific capacity of GB/T 24533-2019 standard testing theory, the party are generallyd use
What method obtained is the storage performance of material, and the first discharge specific capacity of high performance natural graphite material is about on the left side 360mAh/g
The right side, and the petroleum coke in artificial graphite is discharged for the first time than molten amount generally between 300-350mAh/g, lithium battery graphite is negative
The first discharge specific capacity of pole material cannot be too small.
2 coulombic efficiencies for the first time: the head of GB/T 24533-2019 standard testing lithium battery graphite cathode material is generallyd use
Secondary coulombic efficiency.In secondary charging process, lithium ion is embedded into negative electrode material, when the cell is discharged, is embedded into negative electrode material
Lithium ion return in positive electrode, since the hole in material is intricate, not every lithium ion can complete deintercalation,
Therefore this method test obtain is actually available capacity after initial charge, the available space of the higher negative electrode material of numerical value
Higher, the coulombic efficiency for the first time of general petroleum coke is between 90-95%.
3 powder compacted densities: the powder of GB/T 24533-2019 standard testing lithium battery graphite cathode material is generallyd use
Last compacted density.Compacted density is higher, and the lithium battery energy density of same volume is higher, the petroleum coke lithium battery of general artificial graphite
The compacted density of negative electrode material is in 1.0-1.4g/cm3。
4 degree of graphitization: the graphitization of GB/T 24533-2019 standard testing lithium battery graphite cathode material is generallyd use
Degree.The higher lithium cell cathode material of degree of graphitization, performance are better.The petroleum coke of general artificial graphite is after graphitization
Degree of graphitization between 85%-95%.
5 fixed carbon contents: the fixation carbon content of 3521 standard testing lithium battery graphite cathode material of GB/T is generallyd use.
Fixed carbon content represents in negative electrode material, the content of carbon, and fixed carbon content is higher, represents the ash content in material and can
The content of volatile matter is lower, and properties of product are better.The fixation carbon content of high-performance petroleum coke is generally between 99.7%-99.97%.
Embodiment 1 is as shown in table 1 using the performance test data of the lithium battery graphite cathode material of lignin preparation, table 1
In also column taken the performance standard of the general coke of petroleum under standard GB/T/T 24533-2019 in artificial graphite.
Table 1
As it can be seen from table 1 lithium battery graphite cathode material prepared by the embodiment of the present invention 1, capability and performance and artificial graphite
In the general coke of petroleum quality performance parameter it is suitable.As can be seen that utilization lignin through the invention prepares lithium battery graphite
Negative electrode material meets the use standard of lithium cell cathode material.It is by means of the present invention raw material, exploitation using biomass
Produce the graphite material product of downstream high added value.
Content described in this specification is only to enumerate to inventive concept way of realization, and protection scope of the present invention is not answered
When the concrete form for being seen as limited by embodiment and being stated.
Claims (7)
1. lignin is preparing the application in lithium battery graphite cathode material, it is characterised in that the preparation process of the lignin
Are as follows: it is feed liquid after hydrolyzing that the reaction solution after reaction, which is hydrolyzed, in biomass in an acidic solution, after gained hydrolysis in feed liquid
The water of 2-10 volume times is added, stirring has solid precipitation, filters, and filter residue is dried after clear water washs to get the lignin.
2. lignin as described in claim 1 is preparing the application in lithium battery graphite cathode material, it is characterised in that with wood
The step of quality is raw material, prepares lithium battery graphite cathode material are as follows:
1) lignin is mixed with stabiliser solution by 1: 2 ~ 12 mass ratio, stands and stablizes 3 ~ 6 hours at 40 ~ 70 DEG C
Afterwards, it filters, filter residue and drying obtains stablizing lignin；
2) lignin will be stablized obtained by step 1) to be placed in rotary kiln, under nitrogen protection atmosphere, and in 1200 ~ 1500 DEG C of temperature
Lower calcining 2 ~ 4 hours, obtains calcined lignin；
3) calcined lignin obtained by step 2 is placed in graphitizing furnace, under argon atmosphere, and in 2500 ~ 2800
DEG C temperature lower calcination 3 ~ 15 hours, subsequent cooled to room temperature was to get the lithium battery graphite cathode material.
3. lignin as claimed in claim 2 is preparing the application in lithium battery graphite cathode material, it is characterised in that described
Stabiliser solution is the ammonium dibasic phosphate aqueous solution of mass concentration 10% ~ 20%.
4. lignin as described in claim 1 is preparing the application in lithium battery graphite cathode material, it is characterised in that described
The reaction solution after reaction is hydrolyzed in biomass in an acidic solution, is prepared according to following procedure:
S1: biological particles be added reaction kettle in, under anaerobic state be added water cosolvent, heated under stirring 150 DEG C-
220 DEG C, lewis acid is added, reaction 20-40 minutes, the biomass mixed liquor after must hydrolyzing is hydrolyzed；
S2: into the biomass mixed liquor of step S1 plus alkali neutralization adjusts pH to 4.5-8, and cooled and filtered removes what neutralization obtained
Ash content in sediment and biomass is to get the reaction solution.
5. lignin as claimed in claim 4 is preparing the application in lithium battery graphite cathode material, it is characterised in that step
For biological particles water content less than 8%, grain diameter is less than 25mm in S1, and biomass is timber, stalk, paper product, pine, grass
Class, rice husk, bagasse, cotton, jute, flax, bamboo, sisal hemp, abaca, straw, any one or a few mixing in corncob
Object.
6. lignin as claimed in claim 4 is preparing the application in lithium battery graphite cathode material, it is characterised in that step
In S1, water and tetrahydrofuran mixed liquor that water cosolvent is mass ratio 1:1-1:5.
7. lignin as claimed in claim 4 is preparing the application in lithium battery graphite cathode material, it is characterised in that step
In S1, the mass ratio of biomass and water cosolvent is 1: 2-7；The lewis acid is sulfuric acid, hydrochloric acid, at least one in nitric acid
Kind, the lewis acidic quality is the 0.3%-3% of water cosolvent quality.
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Cited By (2)
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| CN112812796A (en) * | 2021-01-13 | 2021-05-18 | 中国石油大学(华东) | Bio-based needle coke and preparation method thereof |
| CN113903891A (en) * | 2021-09-03 | 2022-01-07 | 北京化工大学 | Preparation method and application of amorphous carbon-based composite anode material containing metalloid lithium |
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