CN102361097A - Preparation method of low-temperature electrolyte for lithium iron phosphate power battery - Google Patents

Preparation method of low-temperature electrolyte for lithium iron phosphate power battery Download PDF

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Publication number
CN102361097A
CN102361097A CN2011103585899A CN201110358589A CN102361097A CN 102361097 A CN102361097 A CN 102361097A CN 2011103585899 A CN2011103585899 A CN 2011103585899A CN 201110358589 A CN201110358589 A CN 201110358589A CN 102361097 A CN102361097 A CN 102361097A
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accounts
electrolyte
temperature
low
carbonate
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郭西凤
刘红光
刘大凡
赵洪
袁莉
安峰
张玥
王坤
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China National Offshore Oil Corp CNOOC
CNOOC Tianjin Chemical Research and Design Institute Co Ltd
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China National Offshore Oil Corp CNOOC
CNOOC Tianjin Chemical Research and Design Institute Co Ltd
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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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Abstract

The invention is a preparation method of a low-temperature electrolyte for a lithium iron phosphate power battery; the invention is characterized in that the method comprises the following steps: under the protection of dry inert gas, proportionally adding a plurality of dehydrated organic solvents with a water content of less than 5 ppm into a stainless steel preparation vessel with a jacket, stirring, well mixing, gradually adding certain amounts of electrolyte salts and additives in order, controlling the preparation temperature to be less than 20 DEG C, stirring and mixing for 30-60 min, and filtering the solution by a 0.45 and 0.1-micron two-step precision filter to obtain the low-temperature electrolyte product.

Description

A kind of lithium iron phosphate dynamic battery is with the preparation method of low-temperature electrolyte
Technical field
The present invention relates to the lithium ion power battery electrolyte technical field, disclose the preparation method of a kind of lithium iron phosphate dynamic battery with low-temperature electrolyte.
Background technology
Along with global petroleum resources are nervous, air environmental pollution increases the weight of, the electric automobile of energy-conserving and environment-protective has been acknowledged as the main direction of 21 century automobile industry development.Chinese Government payes attention to for exploitation of new-energy automobile correlation technique and industrialization working depth, has all set up the great special project of country's 863 " energy-conservation and new-energy automobiles " at " 15 ", Eleventh Five-Year Plan.Since 2009, country further strengthens the support dynamics of new energy field, has put into effect " thousand in ten cities " electric automobile plan.
LiFePO 4 material is to use more positive electrode in China's used for electric vehicle lithium-ion-power cell, its have cheapness, safely, unique advantage such as have extended cycle life.But the conductivity of LiFePO 4 material own is lower; Though can improve the electrical conductivity at room temperature of LiFePO 4 material to a certain extent through carbon coating and material nanoization; But under cryogenic conditions; Especially its discharge performance can sharply drop to below 20% of normal temperature capacity owing to the defective of conductivity in the environment for use below the degree of northern area winter-20, has greatly limited the use zone of lithium iron phosphate dynamic battery.
Except that improving the performance of LiFePO 4 material own, through also can improve the cryogenic property of electrokinetic cell to a certain extent to the improvement of electrolyte for lithium-ion power battery.Main being started with by the solvent in the electrolyte, lithium salts and additive three aspects improved.Like variation through solvent complex kind, ratio, widen double solvents the serviceability temperature scope, reduce the viscosity of double solvents under the low temperature; Reduce lithium salts---the consumption of lithium hexafluoro phosphate commonly used, add part low-temperature ion conductivity preferably lithium salts increase the low-temperature conductive property of electrolyte; In addition, also need select suitable additive,, improve electrolyte/electrode interface stability to guarantee the combination property of electrolyte with further raising electrolyte low-temperature conductivity according to the variation of solvent and lithium salts.
(battery, 2004,34 (1): 10-12 such as Xiao Lifen; Electrochimica Acta, 2004,49:4857-4863) improve the electrolyte cryogenic property through optimizing solvent burden ratio content, obtained the LiPF of best electrolyte 1M 6EC/DMC/EMC (volume ratio 8.3: 25: 66.7) is used for lithium ion battery, under can the temperature remains within the normal range to the 2.0V capacity under-40 ℃ with the 0.1C multiplying power discharging 90.3%.
Wang etc. (Solid State lonics, 2006,177:1477-1481) studied 1M LiPF 6The electrolyte of EC/MPC, and use it for LiMn 2O 4/ Li battery.When EC and MPC ratio are 1: 3, can reach 111.6mA/g in the discharge capacity of-20 ℃ of following batteries.
Zhang Shengshui etc. (Electrochemistry Communications, 2002,4:928-932) find LiBF 4Though conductivity does not have the LiPF in the same solvent 6Conductivity is high, but LiBF 4Base electrolyte has good cryogenic property.Under-30 ℃, electrolyte for lithium ion battery 1M LiBF 4The capacity of PC/EC/EMC (mass ratio 1: 1: 3) is 86% under 20 ℃, and uses LiPF 6Base electrolyte can only keep 72%.But also find LiBF 4Base electrolyte also has less degree of polarization under-30 ℃.
Though it is more that the research of low-temperature electrolyte is carried out, for this new type power positive electrode for battery material of LiFePO4, the technology of preparing of the low-temperature electrolyte that matches with it is not perfect.
Summary of the invention
The invention provides a kind of preparation method who is applicable to lithium iron phosphate dynamic battery with low-temperature electrolyte.Purpose is to improve the lithium iron phosphate dynamic battery cryogenic property.
The present invention is the preparation method of a kind of lithium iron phosphate dynamic battery with low-temperature electrolyte; It is characterized in that:
Under dry inert gas protection, will pass through the multiple organic solvent that moisture after the processed is lower than 5ppm; Add according to a certain percentage in the stainless steel preparation still of jacketed; Add a certain amount of electrolytic salt and additive after mixing in order gradually; Control preparation temperature is no more than 20 ℃; Mixed 30～60 minutes, this solution obtains the low-temperature electrolytic liquid product again after 0.45,0.1 micron two steps accurate filters filtration.
Be selected from the following solvent one or more as organic solvent used in the nonaqueous electrolytic solution of the present invention: dimethyl carbonate (DMC); Methyl ethyl carbonate (EMC); Diethyl carbonate (DEC); Ethylene carbonate (EC); Propene carbonate (PC); Fluorinated ethylene carbonate (FEC); Gamma-butyrolacton (GBL); Methyl nine fluorine butyl ether; Trifluoromethyl propene carbonate (TFPC); Methyl acetate (MA); Ethyl acetate (EA); Methyl formate (MF); Methyl propionate (MP); Ethyl propionate (EP); Methyl butyrate (MB); Ethyl butyrate (EB); Acetate trifluoromethyl ethyl ester (TFEA).
Be selected from the following electrolytic salt one or more: LiPF as electrolytic salt used in the low-temperature electrolyte of the present invention 6, LiBF 4, LiBOB, LiODFB, LiTFSI.
Be selected from the following compounds one or more as additive used in the low-temperature electrolyte of the present invention: vinylene carbonate (VC), 1; 3-propane sultone (PS), vinylethylene carbonate (VEC), fluorinated ethylene carbonate (FEC), biphenyl (BP), cyclohexyl benzene (CHB), sulfurous acid ethyl ester (ES), dimethyl sulfite (DMS), N; N-dimethyl trifluoroacetamide (DTA), 2-methyltetrahydrofuran (MTHF).
Above-mentioned organic solvent accounts for 80～85% of electrolyte total weight.Be selected from the mixed solvent system for EC/DMC/EMC/TFPC, wherein each solvent weight percent is: EC accounts for 10～25%, and DMC accounts for 30～45%, and EMC accounts for 20～30%, and TFPC accounts for 20～30%.
Above-mentioned electrolytic salt accounts for 10～13% of nonaqueous electrolytic solution total weight.Be selected from and be LiPF 6/ LiBF 4/ LiTFSI mixed electrolyte salt system, wherein each electrolytic salt percentage by weight is: LiPF 6Account for 75～90%, LiBF 4Account for 10～25%, LiTFSI accounts for 3～8%.
Above-mentioned additive accounts for 2～10% of nonaqueous electrolytic solution total weight.Be selected from and be VC/PS/DTA/FEC compound additive system.The percentage that each additive accounts for the electrolyte total weight is: VC accounts for 1～5%, and PS accounts for 0.2～2%, and DTA accounts for 3～5%, and FEC accounts for 1～2.5%.
The present invention is through reducing electrolyte medium-high viscosity, dystectic EC consumption; Increase linear carbonate DMC, EMC consumption, and add the higher TFPC of dielectric constant and make the electrolyte mixed solvent system have lower viscosity and lithium salts dissolubility preferably at low temperatures.Select the LiBF that has high conductance at low temperatures simultaneously for use 4Substitute partial L iPF 6, the low-temperature conductive property of enhancing electrolyte.All have charge-discharge performance preferably under low temperature and the normal temperature for making electrolyte tie up to, VC, PS through adding the auxiliary electrolyte fusing point that reduces of DTA, add the performance that FEC improves the electrode/electrolyte interfacial film as the additive preferably except that selecting filming performance for use.The integrated use of above-mentioned means can improve the low temperature discharge capacity of lithium iron phosphate dynamic battery more than 10～20%, can reach more than 70% of normal temperature discharge capacity.
Embodiment
Embodiment 1
Under drying nitrogen (moisture is lower than 10ppm) protection; (moisture is lower than 5ppm will to pass through DMC, EMC, TFPC, EC after the processed; Weight ratio 3: 3: 2: 2) add in order in the stainless steel preparation still of jacketed, the control mixing temperature is not higher than 20 ℃, mixes 30 minutes; Add LiPF subsequently in order gradually 6, LiBF 4(weight ratio 4: 1, electrolytic salt total weight account for electrolyte total weight 10%), the control mixing temperature is not higher than 20 ℃, mixes 30 minutes; Add the VC account for electrolyte total weight 2%, 0.4% PS, 5% DTA and 3% FEC at last, continue to stir 30 minutes.This solution obtains the electrolyte product A again after 0.45,0.1 micron accurate filter filtration.
Embodiment 2
Under drying nitrogen (moisture is lower than 10ppm) protection; (moisture is lower than 5ppm will to pass through DMC, EMC, EC after the processed; Weight ratio 3: 5: 2) add in order in the stainless steel preparation still of jacketed, the control mixing temperature is not higher than 20 ℃, mixes 30 minutes; Add LiPF subsequently in order gradually 6(weight ratio 4: 1, weight account for electrolyte total weight 10%), the control mixing temperature is not higher than 20 ℃, mixes 30 minutes; Add at last and account for the VC of electrolyte total weight 3%, 0.3% PS, 5% FEC, continuation stirring 30 minutes.This solution obtains the electrolyte product B again after 0.45,0.1 micron accurate filter filtration.
Embodiment 3
Under drying nitrogen (moisture is lower than 10ppm) protection; (moisture is lower than 5ppm will to pass through EMC, TFPC, EC after the processed; Weight ratio 5: 2: 3) add in order in the stainless steel preparation still of jacketed, the control mixing temperature is not higher than 20 ℃, mixes 30 minutes; Add LiPF subsequently in order gradually 6, LiBF 4(weight ratio 4: 1, electrolytic salt total weight account for electrolyte total weight 12%), the control mixing temperature is not higher than 20 ℃, mixes 30 minutes; Adding the VC account for electrolyte total weight 5%, 0.2% PS and 5% DTA at last continues to stir 30 minutes.This solution obtains the nonaqueous electrolytic solution products C again after 0.45,0.1 micron accurate filter filtration.
The properties of product test
The electrolyte A that the foregoing description is prepared, B, C are made into the flexible packaging power battery by power battery standard producton order; Wherein positive electrode is a LiFePO4; Negative material is a Delanium, sees table 1 through the correction data that changes into, obtain after partial volume, normal temperature discharge performance and the low temperature performance test.
Table 1. low-temperature electrolyte The performance test results (1C discharges and recharges)
Numbering Capacity (Ah, 25 ℃) Capacity (Ah ,-20 ℃) Capability retention (%)
A 15.87 11.14 70.2
B 15.13 8.11 53.6
C 15.49 9.87 63.7

Claims (7)

1. a lithium iron phosphate dynamic battery is with the preparation method of low-temperature electrolyte; It is characterized in that:
Under dry inert gas protection, will pass through the multiple organic solvent that moisture after the processed is lower than 5ppm; Add according to a certain percentage in the stainless steel preparation still of jacketed; Add a certain amount of electrolytic salt and additive after mixing in order gradually; Control preparation temperature is no more than 20 ℃; Mixed 30～60 minutes, this solution obtains the low-temperature electrolytic liquid product again after 0.45,0.1 micron two steps accurate filters filtration.
2. according to the described method of claim 1; It is characterized in that: be selected from the following solvent one or more as organic solvent used in the nonaqueous electrolytic solution of the present invention: dimethyl carbonate DMC; Methyl ethyl carbonate EMC; Diethyl carbonate DEC; Ethylene carbonate EC; Propene carbonate PC; Fluorinated ethylene carbonate FEC; Gamma-butyrolacton GBL; Methyl nine fluorine butyl ether; Trifluoromethyl propene carbonate TFPC; Methyl acetate MA; Ethyl acetate EA; Methyl formate MF; Methyl propionate MP; Ethyl propionate EP; Methyl butyrate MB; Ethyl butyrate EB; Acetate trifluoromethyl ethyl ester TFEA.
3. according to the described method of claim 1; It is characterized in that: be selected from the following electrolytic salt one or more: LiPF as electrolytic salt used in the low-temperature electrolyte of the present invention 6, LiBF 4, LiBOB, LiODFB, LiTFSI.
4. according to the described method of claim 1; It is characterized in that: be selected from the following compounds one or more: vinylene carbonate VC, 1 as additive used in the low-temperature electrolyte of the present invention; 3-propane sultone PS, vinylethylene carbonate VEC, fluorinated ethylene carbonate FEC, biphenyl BP, cyclohexyl benzene CHB, sulfurous acid ethyl ester ES, dimethyl sulfite DMS, N; N-dimethyl trifluoroacetamide DTA, 2-methyltetrahydrofuran MTHF.
5. according to the described method of claim 1; It is characterized in that: said organic solvent accounts for 80～85% of electrolyte total weight; Be selected from the mixed solvent system for EC/DMC/EMC/TFPC, wherein each solvent weight percent is: EC accounts for 10～25%, and DMC accounts for 30～45%, and EMC accounts for 20～30%, and TFPC accounts for 20～30%.
6. according to the described method of claim 1; It is characterized in that: said electrolytic salt accounts for 10～13% of nonaqueous electrolytic solution total weight; Be selected from and be LiPF 6/ LiBF 4/ LiTFSI mixed electrolyte salt system, wherein each electrolytic salt percentage by weight is: LiPF 6Account for 75～90%, LiBF 4Account for 10～25%, LiTFSI accounts for 3～8%.
7. according to the described method of claim 1; It is characterized in that: said additive accounts for 2～10% of nonaqueous electrolytic solution total weight.Be selected from and be VC/PS/DTA/FEC compound additive system; The percentage that each additive accounts for the electrolyte total weight is: VC accounts for 1～5%, and PS accounts for 0.2～2%, and DTA accounts for 3～5%, and FEC accounts for 1～2.5%.
CN2011103585899A 2011-11-14 2011-11-14 Preparation method of low-temperature electrolyte for lithium iron phosphate power battery Pending CN102361097A (en)

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CN102544581A (en) * 2012-02-26 2012-07-04 河北工业大学 Flame-retardant electrolyte for lithium iron phosphate power cell
CN102593515A (en) * 2012-03-20 2012-07-18 惠州市赛能电池有限公司 Electrolyte of lithium ion battery
CN102683745A (en) * 2012-03-01 2012-09-19 华瑞(新乡)化工有限公司 Method for preparing electrolyte of novel 5V lithium ion battery
CN102832409A (en) * 2012-08-13 2012-12-19 中航锂电（洛阳）有限公司 Low temperature lithium ion battery electrolyte and its preparation method
CN102983362A (en) * 2012-12-20 2013-03-20 中国东方电气集团有限公司 Low-temperature electrolyte for LiFePO4 (lithium iron phosphate) lithium-ion batteries
CN103219544A (en) * 2013-04-10 2013-07-24 山东威高东生新能源科技有限公司 Low-temperature electrolyte for ternary power lithium ion battery and preparation method
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CN103682435A (en) * 2013-11-22 2014-03-26 深圳市迪凯特电池科技有限公司 Electrolyte for high-rate pulse discharge lithium ion battery
CN103762383A (en) * 2014-01-14 2014-04-30 南昌大学 Lithium ion battery low-temperature electrolyte and preparation method thereof
CN103779605A (en) * 2013-12-20 2014-05-07 宁波维科电池股份有限公司 Low-temperature lithium iron phosphate ion battery electrolyte and preparation method thereof
CN104969402A (en) * 2012-12-28 2015-10-07 约翰逊控制技术公司 Electrolyte solutions for lithium-ion battery cells operating over a wide temperature range
CN105390748A (en) * 2015-12-14 2016-03-09 苏州华一新能源科技有限公司 Lithium ion battery electrolyte and lithium ion battery
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CN106025362A (en) * 2016-06-28 2016-10-12 华蓥市高科龙电子科技有限公司 Low-temperature type lithium-ion battery electrolyte
CN106025362B (en) * 2016-06-28 2018-12-21 华蓥市高科龙电子科技有限公司 A kind of electrolyte of low temp lithium ion battery
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Application publication date: 20120222