CN107069082A - One kind is saccharide-modified to lead lighium polymer/inorganic hybridization electrolyte and its application - Google Patents
One kind is saccharide-modified to lead lighium polymer/inorganic hybridization electrolyte and its application Download PDFInfo
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- H—ELECTRICITY
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- 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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- 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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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract
Saccharide-modified lighium polymer/inorganic hybridization electrolyte and its application are led the invention discloses one kind.The electrolyte leads lighium polymer and lithium salts including saccharide-modified；The saccharide-modified lighium polymer of leading is mixed to get by saccharide compound with leading lighium polymer and/or leading lithium micromolecular compound by cross-linking reaction or directly；The electrolyte has the high conductivity of inorganic material and the flexible nature of polymeric material concurrently, with very high lithium ion conductivity and good processing characteristics, there is capacity big, the lithium ion battery of good cycle, lithium sulphur or the empty battery of lithium etc. suitable for preparing, and electrolyte cost is low, the simple range of choice and application field for expanding lithium battery material is prepared.
Description
Technical field
The present invention relates to a kind of electrolyte, more particularly to a kind of saccharide-modified lighium polymer/inorganic hybridization of leading is electrolysed
Matter and its application in the empty battery of lithium ion battery, lithium-sulfur cell or lithium, belong to technical field of lithium batteries.
Background technology
Since lithium ion battery puts goods on the market since 1991, machine, notebook computer, electric tool, electricity have been widely used to
The middle-size and small-size field of batteries such as dynamic bicycle.With the development of the large-sized battery application fields such as electric automobile and energy storage, to battery
Energy density, security performance propose requirements at the higher level.Traditional electrolyte mainly has carbonates solution composition, with flowable
Property, combustibility, toxicity, explosivity, be an important cause of the electric safety problem of lithium, while the structure for also constraining battery is set
Meter, reduces energy density.Exploitation with high-energy-density, safe and reliable, cheap, environment-friendly lithium battery material and
Battery system, it has also become the developing direction of lithium battery industry.
Materials are to realize one of approach of the cheap preparation of material and environment-friendlyization from natural products.Chinese patent is (public
The number of opening CN104051790A) a kind of method that lithium battery is prepared by garlic or onion is disclosed, the plant that garlic, onion etc. are enriched
Goods and materials source makes full use of field of lithium.To expand battery material selection range, reduction material cost, the peace for lifting lithium battery
Full property and structure diversity open up a new way.
The content of the invention
The problem of existing for prior art, the purpose of the present invention is to be to provide that a kind of cost is low, high conduction performance, can
Lighium polymer/inorganic hybridization electrolyte is led for preparing high power capacity, the saccharide-modified of high circulation performance lithium battery.
Another object of the present invention is to be to provide a kind of saccharide-modified lighium polymer/inorganic hybridization electrolyte of leading in system
Application in standby high power capacity, high circulation performance, the lithium battery of low cost.
In order to realize above-mentioned technical purpose, it is electrolysed the invention provides the saccharide-modified lighium polymer/inorganic hybridization of leading of one kind
Matter, including saccharide-modified lead lighium polymer and lithium salts；The saccharide-modified lighium polymer of leading is polymerize by saccharide compound with leading lithium
Thing and/or lead lithium micromolecular compound and be mixed to get by cross-linking reaction or directly；It is described to lead lighium polymer or lead lithium small molecule
Compound includes the active group that can pass through chemical bonding with saccharide compound.
Technical scheme is crosslinked by saccharide compound to leading lighium polymer or leading lithium micromolecular compound
Modified, saccharide compound abundance is substantially reduced in electrolyte cost, the particularly saccharide compound molecular structure of itself
Containing sufficient oxygen element, such as hydroxyl, ehter bond, carbonyl are acted on lithium is led well.Gathered by saccharide compound with leading lithium
On the one hand compound or the cross-linking reaction for leading lithium micromolecular compound, the lighium polymer of leading of formation have three-dimensional structure, its stability
Good, as solid electrolyte material, its good processability, capacity is high；On the other hand, by combine sugar and lead lighium polymer or
Compound leads lithium performance, and synergy is remarkably reinforced, polymer is led lithium ability and increase substantially.
Technical scheme carries out physics by saccharide compound with leading lighium polymer or leading lithium micromolecular compound
Mixing, leads the physical mixed between lighium polymer by difference and prepares electrolyte, to improve the electrical conductivity of electrolyte, and have height concurrently
Electrical conductivity and preferably mechanical property.Particularly leading under conditions of lighium polymer is difficult to dissolve with solvent, available physical mixing
Improve the performance of electrolyte.
It is preferred that scheme, the saccharide compound and the crosslinking led lighium polymer and/or lead lithium micromolecular compound
It is 1 to react molar ratio：99~99：1.
It is preferred that scheme, the saccharide compound leads lighium polymer and/or leads the direct of lithium micromolecular compound with described
It is 1 to mix molar ratio：99~99：1.
More preferably scheme, the condition of the cross-linking reaction is：Temperature is 25~90 DEG C, and the time is 4~24h.
More preferably scheme, the saccharide compound is natural saccharide compound and/or modified saccharide compound.Natural sugar
Class compound includes at least one of monose, oligosaccharide and polysaccharide, such as starch, cellulose, sucrose, glucose and fructose
Deng.For example natural saccharide compound of described modification saccharide compound passes through coupling agent modified, coupling agent such as BH3, silane coupler
Deng.
More preferably scheme, it is described lead lighium polymer or lead lithium small molecule contain alkoxy, borine radical, boron oxygen key, silicon hydrogen
At least one of base, carboxyl, amino, sulfydryl, sulfonic group, phosphate and epoxy radicals active functional group group.These active groups master
It can be chemically bonded with the functional group included in saccharide compound.
Further preferred scheme, the lighium polymer of leading contains at least one in oxy radical, nitrogen-containing group, sulfur-containing group
The group of lithium ion can be complexed by planting.Such as linear carbonate unit, cyclic carbonate ester units, nitrogen heterocyclic ring, ether-oxygen bond, thioether
Key, sulfur heterocyclic ring etc..
It is preferred that scheme, it is described it is saccharide-modified lead lighium polymer/inorganic hybridization electrolyte also include micro-nano structure material；
The saccharide-modified mass percent for leading lighium polymer/inorganic hybridization electrolyte, which is constituted, is：
It is saccharide-modified to lead lighium polymer 20~80%；Lithium salts 10~70%；Micro-nano structure material 0.5~10%.
More preferably scheme, the lithium salts includes organic lithium salt and inorganic lithium salt；The mass percent of the organic lithium salt
Content is 10%~90%.Preferred scheme, the organic lithium salt is LiFP6、LiBF4, in LiTFSI, LiFSI, LiBOB
It is at least one；The inorganic lithium salt is LiClO4、Li2S、Li3.25Ge0.25P0.75S4、Li3PS4、Li4GeS4、Li7P3S11、
Li6PS5Cl、Li7P2S8I、LiPON、LLZO、LLTO、LATP、LAGP、LISICON、LiBH4, at least one of LiI.
More preferably scheme, the micro-nano structure material is Al2O3、SiO2、V2O5、Fe2O3And metal organic frame knot
At least one of structure material.
Present invention also offers the saccharide-modified application for leading lighium polymer/inorganic hybridization electrolyte, it is applied to
The empty battery of lithium ion battery, lithium-sulfur cell or lithium.
Compared with the prior art, the advantageous effects that technical scheme is brought：
1. saccharide-modified lighium polymer/inorganic hybridization electrolyte primary raw material of leading of the present invention is using natural carbohydrate chemical combination
Thing, with it is cheap, originate wide the characteristics of, reduce the cost of battery material, widen the selection range of lithium battery material；
2. the present invention it is saccharide-modified lead lighium polymer/inorganic hybridization electrolyte by saccharide compound and lead lighium polymer or
Lead lithium micromolecular compound to obtain by physical mixed or cross-linking reaction, have the high conductivity and polymeric material of inorganic material concurrently
Flexible nature, with high conductivity and excellent processing characteristics.Saccharide compound is with leading lighium polymer or micromolecular compound
Between synergy be remarkably reinforced, substantially increase and the electric conductivity of electrolyte, particularly saccharide compound and lead lighium polymer
Or lead lithium micromolecular compound by chemical combination crosslinking build the good three-dimensional net structure of stability, greatly promote the biography of lithium ion
Lead, while electrical conductivity is lifted, strengthen the processing characteristics of electrolyte.
3. saccharide-modified lighium polymer/inorganic hybridization electrolyte of leading of the present invention has a wide range of application, existing skill can be replaced
Lithium air, lithium sulphur, the electrolyte of lithium ion battery are used in art, can obtain high power capacity, the lithium battery of good cycle, and
With it is environment-friendly the characteristics of, improve lithium battery green, improve battery recycling.
Brief description of the drawings
【Fig. 1】The ferric phosphate lithium cell charging and discharging curve figure made from the embodiment of the present invention 1.
Embodiment
Implement row below and be intended to further illustrate present invention, rather than limitation the claims in the present invention protection domain.
Implement row 1
0.5g starch, 10g dimethyl sulfoxides is taken to be placed in flask, 80 DEG C of control is stirred 1 hour under argon gas protection, Ran Houjia
It is 2 to enter with starch glucose unit mol ratio:3 carboxy polyethylene glycol, reacts 12 hours, and revolving removes solvent, obtains product.
The 0.01g products and 0.1g PEO and 0.033gLiTFSI are dissolved in acetonitrile, drips in plastic sheeting matrix surface, is placed in hand
60 DEG C of dry 12h, obtain solid electrolyte film in casing, the film are used in ferric phosphate lithium cell, obtained room temperature
0.2C charging and discharging curves are as shown in Figure 1.
Embodiment 2
0.5g starch, 10g dimethyl sulfoxides is taken to be placed in flask, 80 DEG C of control is stirred 1 hour under argon gas protection, Ran Houjia
It is 2 to enter with starch glucose unit mol ratio:3 carboxy polyethylene glycol, reacts 12 hours, and product is directly used in configuration electrolysis
Matter.2g reactions resulting solution is well mixed with 0.04g LiTFSI, resulting solution is dripped in plastic sheeting matrix surface, is placed in hand
60 DEG C of dry 12h, obtain solid electrolyte film in casing, and the film conductivity is 4.2 × 10-5S/cm。
Embodiment 3
0.5g sucrose, 10g pyridines is taken to be placed in flask, 45 DEG C of control is stirred 1 hour under argon gas protection, is then added dropwise
It is 8 to enter with sucrose mol ratio:3 BH3.THF solution, reacts 12h, and reaction mixture is directly used in preparation electrolyte.2g is reacted
Resulting solution is mixed evenly with 0.1g molecular weight for 4,000,000 PEO and 0.04gLiTFSI, forms gel.By the gel
It is coated on sulphur positive pole, 5min is stood in argon gas glove box, using metal Li as negative pole, is assembled into button cell, battery can be obtained
Obtain 1452mAh/g initial discharge capacity.
Embodiment 4
0.5g agar is taken, 95 DEG C of control is stirred 1 hour under argon gas protection, melts it, is then added and is rubbed with its hydroxyl
You are than being 1:3 BH3.THF solution, reacts 12h.Obtained product is pulverized.By the 0.02g products, 0.2g PEO and
0.26g LiTFSI are dissolved in acetonitrile, after stirring, and solvent evaporates into solid electrolyte film, and electrical conductivity is 3.8 × 10-5S/
cm。
Embodiment 5
0.5g sucrose, 10g pyridines is taken to be placed in flask, 45 DEG C of control is stirred 13 hours under argon gas protection, by obtained by 2g
Solution adds 0.04gLiTFSI, and drying and volatilizing obtains pure sugared electrolyte, and the electrolyte is cracked into powder, it is impossible to film forming.
0.5g sucrose, 10g pyridines is taken to be placed in flask, 45 DEG C of control is stirred 1 hour under argon gas protection, is then added dropwise
It is 8 to enter with sucrose mol ratio:3 BH3.THF solution, reacts 12h, and it is 4,000,000 that 2g is reacted into resulting solution with 0.1g molecular weight
PEO, 0.04gLiTFSI be mixed evenly, solvent flashing can obtain solid polymer electrolyte.The electrolyte is coated on and contained
On carbon electrode, as on the C2025 anode covers in tool hole, negative pole and negative electrode casing are covered, the empty battery of lithium is assembled into.The battery is 60
DEG C, first circle discharge platform is 2.60V under the conditions of 0.005mAh.
Embodiment 6
0.5g starch, 10gDMSO is taken to be placed in flask, 45 DEG C of control is stirred 1 hour under argon gas protection, is then added dropwise
It is 5 to enter with starch glucose unit mol ratio:3 BH3.THF solution, reacts 12h, and reaction mixture is directly used in preparation electrolysis
Matter.2g reactions resulting solution is mixed evenly with 0.01gMOF and 0.04gLiTFSI, lithium gel, electrical conductivity are led in formation
For 1.2 × 10-3S/cm。
Embodiment 7
0.5g sucrose, 10g pyridines is taken to be placed in flask, 45 DEG C of control is stirred 1 hour under argon gas protection, is then added dropwise
It is 5 to enter with sucrose glucose unit mol ratio:3 BH3.THF solution, reacts 12h.2g is reacted into resulting solution and 0.04g
LiTFSI and 0.1g PEO are mixed evenly, and evaporate into uniform film, and electrical conductivity is up to 7.8 × 10-5S/cm.Take 0.1g sugarcanes
In sugar, 0.04g LiTFSI and 0.1g PEO, solvent is volatilized, obtained film surface has obvious particle.
Embodiment 8
0.5g starch, 10g dimethyl sulfoxides is taken to be placed in flask, 80 DEG C of control is stirred 1 hour under argon gas protection, Ran Houjia
It is 2 to enter with starch glucose unit mol ratio:3 carboxy polyethylene glycol, reacts 12 hours, and revolving removes solvent, obtains product.
By the 0.1g products, 0.7g PEO, 0.3g TFSI and 0.05g MIL-53 (Al) are dissolved in acetonitrile, after stirring, solvent
Volatilization film forming, obtained electrolytic conductivity is 1.2 × 10-5S/cm。
Embodiment 9
0.5g starch, 10g dimethyl sulfoxides is taken to be placed in flask, 80 DEG C of control is stirred 1 hour under argon gas protection, Ran Houjia
It is 2 to enter with starch glucose unit mol ratio:3 carboxy polyethylene glycol, reacts 12 hours, and revolving removes solvent, obtains product.
By the 0.1g products, 0.7g PEO and 0.3g TFSI are dissolved in acetonitrile, after stirring, solvent volatilization film forming, obtained electrolysis
Matter electrical conductivity is 8.9 × 10-6S/cm。
Embodiment 10
0.5g starch, 10g dimethyl sulfoxides is taken to be placed in flask, 80 DEG C of control is stirred 1 hour under argon gas protection, Ran Houjia
It is 2 to enter with starch glucose unit mol ratio:3 carboxy polyethylene glycol, reacts 12 hours, and product is directly used in configuration electrolysis
Matter.By 2g reaction resulting solutions and 0.04g LiTFSI, 0.01g Li3.25Ge0.25P0.75S4It is well mixed, resulting solution drip in
Plastic sheeting matrix surface, is placed in 60 DEG C of dry 12h in glove box, obtains solid electrolyte film, and the film conductivity is 6.8
×10-5S/cm。
Claims (10)
1. one kind is saccharide-modified to lead lighium polymer/inorganic hybridization electrolyte, it is characterised in that：Lighium polymer is led including saccharide-modified
And lithium salts；The saccharide-modified lighium polymer of leading is led to by saccharide compound with leading lighium polymer and/or leading lithium micromolecular compound
Cross cross-linking reaction or be directly mixed to get；It is described to lead lighium polymer or lead lithium micromolecular compound comprising be logical with saccharide compound
Cross the active group of chemical bonding.
2. saccharide-modified lighium polymer/inorganic hybridization electrolyte is led according to claim 1, it is characterised in that：The sugar
Class compound is 1 with the cross-linking reaction molar ratio led lighium polymer and/or lead lithium micromolecular compound：99~99：1；
The saccharide compound is 1 with the direct molar ratio that mixes led lighium polymer and/or lead lithium micromolecular compound：
99~99：1.
3. saccharide-modified lighium polymer/inorganic hybridization electrolyte is led according to claim 1 or 2, it is characterised in that：It is described
The condition of cross-linking reaction is：Temperature is 25~90 DEG C, and the time is 4~24h.
4. saccharide-modified lighium polymer/inorganic hybridization electrolyte is led according to claim 1 or 2, it is characterised in that：It is described
Saccharide compound is natural saccharide compound and/or modified saccharide compound.
5. saccharide-modified lighium polymer/inorganic hybridization electrolyte is led according to claim 1 or 2, it is characterised in that：It is described
Lead lighium polymer or lead lithium small molecule contain alkoxy, borine radical, boron oxygen key, silicon hydrogen-based, carboxyl, amino, sulfydryl, sulfonic group,
At least one of phosphate and epoxy radicals active functional group group.
6. saccharide-modified lighium polymer/inorganic hybridization electrolyte is led according to claim 5, it is characterised in that：It is described to lead
Lighium polymer, which contains at least one of oxy radical, nitrogen-containing group, sulfur-containing group, can be complexed the group of lithium ion.
7. saccharide-modified lighium polymer/inorganic hybridization electrolyte is led according to claim 1 or 2, it is characterised in that：
Saccharide-modified lighium polymer/inorganic hybridization the electrolyte of leading also includes micro-nano structure material；
The saccharide-modified mass percent for leading lighium polymer/inorganic hybridization electrolyte, which is constituted, is：
It is saccharide-modified to lead lighium polymer 20~80%；
Lithium salts 10~70%；
Micro-nano structure material 0.5~10%.
8. saccharide-modified lighium polymer/inorganic hybridization electrolyte is led according to claim 7, it is characterised in that：The lithium
Salt includes organic lithium salt and inorganic lithium salt；
The mass percentage content of the organic lithium salt is 10%~90%；
The micro-nano structure material is Al2O3、SiO2、TiO2、V2O5、Fe2O3And at least one in metal-organic framework material
Kind.
9. saccharide-modified lighium polymer/inorganic hybridization electrolyte is led according to claim 8, it is characterised in that：
The organic lithium salt is LiFP6、LiBF4, at least one of LiTFSI, LiFSI, LiBOB；
The inorganic lithium salt is LiClO4、Li2S、Li3.25Ge0.25P0.75S4、Li3PS4、Li4GeS4、Li7P3S11、Li6PS5Cl、
Li7P2S8I、LiPON、LLZO、LLTO、LATP、LAGP、LISICON、LiBH4, at least one of LiI.
10. any one of the claim 1~9 saccharide-modified application for leading lighium polymer/inorganic hybridization electrolyte, its feature exists
In：Applied to the empty battery of lithium ion battery, lithium-sulfur cell or lithium.
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| CN109980275A (en) * | 2019-03-21 | 2019-07-05 | 中南大学 | A kind of wide warm solid polyelectrolyte and its preparation and the application in all solid state alkali metal/alkaline earth metal batteries |
| CN110400964A (en) * | 2019-07-31 | 2019-11-01 | 苏州顺创新能源科技有限公司 | A kind of lithium ion battery solid electrolyte membrane |
| CN112786961A (en) * | 2021-03-23 | 2021-05-11 | 上海电气集团股份有限公司 | Biomass-based gel electrolyte, lithium ion battery, preparation method and application |
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Application publication date: 20170818 |