CN108832177A - A kind of POSS compound cellulose/polycarbonate solid polymer dielectric and preparation method - Google Patents
A kind of POSS compound cellulose/polycarbonate solid polymer dielectric and preparation method Download PDFInfo
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- CN108832177A CN108832177A CN201810555201.6A CN201810555201A CN108832177A CN 108832177 A CN108832177 A CN 108832177A CN 201810555201 A CN201810555201 A CN 201810555201A CN 108832177 A CN108832177 A CN 108832177A
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- 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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Abstract
The present invention relates to a kind of POSS compound cellulose/polycarbonate solid polymer dielectrics and preparation method, the quality proportioning of component to be：POSS accounts for the 1%-15% of polymeric matrix, cellulose accounts for the 10%-90% of polymeric matrix, polycarbonate accounts for the 10%-90% of polymeric matrix, lithium salts accounts for the 5%-15% of polymeric matrix, and above-mentioned four groups of assignment systems solution after-pouring is blended and obtains POSS compound cellulose/polycarbonate solid polymer dielectric；The cellulose is methylcellulose.Casting method proposed by the present invention, which prepares POSS compound cellulose/polycarbonate solid polymer dielectric, has the characteristics that good mechanical property, high-temperature conductivity are high, POSS facilitates the raising of polymer dielectric heat resistance and mechanical performance, cellulose helps to provide good mechanical performance, and polycarbonate helps to improve ionic conductivity.POSS compound cellulose/polycarbonate solid polymer dielectric of the invention can satisfy the requirement as lithium ion battery electrolyte to ionic conductivity.
Description
Technical field
The invention belongs to solid polymer electrolyte preparation technical fields, are related to a kind of POSS compound cellulose/poly- carbonic acid
Ester solid polymer electrolyte and preparation method.
Background technique
With environmental pollution get worse and fossil fuel it is increasingly deficient, people are sought for novel energy wood
Material.Lithium ion battery has the characteristics that high-energy density, long life and environmentally friendly, is widely used in mobile phone, pen
Remember this computer, digital camera and electric car etc..Current lithium ion battery is mainly liquid electrolyte, it makes in long-term circulation
With will appear the phenomenon of leakage in the process, the burning even danger of explosion can occur under extreme case.Develop novel electrolysis plastid
It is extremely urgent.Solid polymer electrolyte has higher energy density relative to liquid electrolyte, and high operating voltage is good
Flexibility and design.It is in use not in leakage problem with the battery of its assembling due to being all solid state, peace
Full property is higher.Solid state electrolysis Quality Research is based primarily upon polyethers at present, but there is also electricity at present for solid polymer electrolyte
The problem of conductance is low and bad mechanical property, is unable to satisfy the normal use of battery.Design prepares novel solid polymer electrolytic
Matter makes it in the case where meeting the assembling and safety issue of battery, and ion transmission performance and the electrochemistry for improving battery are steady
It is qualitative, it is the hot and difficult issue studied at present.
Silsesquioxane (POSS) is a kind of hybrid inorganic-organic materials, and inorganic silicon oxygen cage modle nuclear energy enough effectively improves material
Its compatibility with polymer can be improved in the heat resistance and mechanical performance of material, organic moiety.
Cellulose due to its rich reserves, it is biodegradable, renewable, it is easy obtain, it is at low cost, be substitution petroleum base
The good selection of material.Cellulose is mainly derived from timber, is a kind of linear homopolymer, have porosity is high, mechanical property is good,
The features such as nontoxic, light-weight, and with its preparation electrolyte have good wetability and thermal stability, it has also become battery every
A kind of alternative materials of film.But cellulose crystallite is high, the electrolytic conductivity prepared with it is low, is unable to satisfy battery
Demand.
Polycarbonate has the performances such as excellent impact strength, the transparency, resistance to ag(e)ing and fatigue durability, is widely used in
Industrial production.Due to its unique property, it is used for the research of electronics industry.Contain polar group, phase in polycarbonate structure
There is higher dielectric constant for polyethers, be more advantageous to the dissociation of lithium salts.However, carbonate polymer solid electrolyte
Film forming it is poor, bad mechanical property.
, will be good with polymer compatibility based on the above analysis, but be conducive to mechanical performance raising POSS and film forming it is poor,
The high polycarbonate of the conductivity cellulose low with good film-forming property, conductivity mixes in varing proportions, the side poured using solution
Solid polymer electrolyte of good performance is prepared in method.
Summary of the invention
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes a kind of POSS compound cellulose/polycarbonate solid
Polymer dielectric and preparation method select mechanical performance to improve the mechanical performance and ionic conductivity of solid electrolyte
Good cellulose, the high polycarbonate of dielectric constant are raw material, and cellulose/polycarbonate solid polymer dielectric is made, full
Requirement of the foot as lithium ion battery electrolyte to ionic conductivity.
Technical solution
A kind of POSS compound cellulose/polycarbonate solid polymer dielectric, it is characterised in that the quality proportioning of component
Wei ︰ POSS accounts for the 1%-15% of polymeric matrix, and cellulose accounts for the 10%-90% of polymeric matrix, and polycarbonate accounts for polymer
The 10%-90% of matrix, lithium salts account for the 5%-15% of polymeric matrix, and above-mentioned four groups of assignment systems solution after-pouring is blended and obtains
POSS compound cellulose/polycarbonate solid polymer dielectric；The cellulose is methylcellulose.
The POSS is POSS- (C3H6Cl)8Or POSS-PMMA.
The methylcellulose dosage is the 20%-80% of total polymer mass.
The polycarbonate accounts for the 20%-80% of the gross mass of polymeric matrix.
The polycarbonate is poly- ethylene carbonate PEC, polypropylene carbonate PPC or polymerized thylene carbonate vinyl acetate PVCA.
The lithium salts is lithium perchlorate LiClO4, hexafluoro phosphorus lithium LiFP6Or trifluoromethyl sulfonic acid lithium LiCF3SO3。
A method of preparing the POSS compound cellulose/polycarbonate solid polymer dielectric, it is characterised in that
Step for example Xias ︰
Step 1 ︰ mixes POSS, methylcellulose, polycarbonate and lithium salts and solvent, is heated to 30 DEG C -50 DEG C simultaneously
Stirring to cellulose, polymer and lithium salts dissolution becomes solution；
Solution down in polytetrafluoro culture dish, in 25 DEG C of -40 DEG C of vacuum drying 10h-12h, then is warming up to 60 by step 2 ︰
DEG C -80 DEG C, it is dried in vacuo 20h-24h, obtains POSS compound cellulose/polycarbonate solid polymer dielectric.
The solvent is n,N-Dimethylformamide DMF, toluene, methylene chloride or its blend.
Beneficial effect
A kind of POSS compound cellulose/polycarbonate solid polymer dielectric proposed by the present invention and preparation method, add
The POSS entered facilitates the raising of polymer dielectric heat resistance and mechanical performance, and the cellulose of addition facilitates electrostrictive polymer
The raising of the mechanical performance of matter is solved, polycarbonate has high dielectric constant, facilitates the raising of polymer dielectric conductivity.
And common solid polymer electrolyte matrix PEO, dielectric constant are lower, cannot dissociate lithium salts well, be easy to cause ion
A large amount of aggregations, inhibit Li+Migration.Although polycarbonate has high dielectric constant, its film forming is poor.So by its with both
With excellent filming performance, and environmental-friendly and cheap cellulose combines, and adds hybrid inorganic-organic materials
POSS obtains the compound cellulose of POSS/polycarbonate solid polymer dielectric.
Casting method preparation POSS compound cellulose/polycarbonate solid polymer dielectric proposed by the present invention has machinery
The feature that performance is good, high-temperature conductivity is high, POSS facilitate the raising of polymer dielectric heat resistance and mechanical performance, fiber
It is known as and helps provide good mechanical performance, polycarbonate helps to improve ionic conductivity.
POSS compound cellulose/polycarbonate solid polymer dielectric of the invention can satisfy as lithium ion battery
Requirement of the electrolyte to ionic conductivity.
Detailed description of the invention
POSS compound cellulose/polycarbonate solid polymer dielectric preparation process flow 1 ︰ of figure of the invention；
(A-D respectively corresponds case study on implementation to 2 ︰ POSS compound cellulose of figure/polycarbonate solid polymer dielectric photo
1-4 obtained solid electrolyte)；
3 ︰ (a) different proportion POSS compound cellulose of figure/conductance of the polycarbonate solid polymer dielectric at 50 DEG C
Rate figure；(b) conductivity map of the compound 80%PPC/20% methylcellulose of POSS at different temperatures.
Specific embodiment
Now in conjunction with embodiment, attached drawing to mono- step Miao Shu ︰ of Zuo Jin of the present invention
1 ︰ reacting flow chart of embodiment is as shown in Figure 1.
Step 1 ︰ weighs methylcellulose and polypropylene carbonate according to 20 ︰, 80 mass ratio and mixes in beaker, and presses
LiClO is weighed according to polymeric matrix 10%4In beaker, POSS- (C is weighed according to polymeric matrix 10%3H6Cl)8In beaker
In, the DMF of 3mL is added, completely in 30 DEG C of -50 DEG C of water-bath heating stirrings to its dissolution, obtains pouring solution.
Step 2 ︰ pours into acquired solution in polytetrafluoro culture dish, 25 DEG C of -40 DEG C of vacuum drying 10h-12h, then is warming up to
60 DEG C -80 DEG C, it is dried in vacuo 20h-24h, obtains POSS compound cellulose/polycarbonate solid polymer dielectric A.
2 ︰ of embodiment
Step 1 ︰ weighs methylcellulose and polypropylene carbonate according to 40 ︰, 60 mass ratio and mixes in beaker, and presses
LiClO is weighed according to polymeric matrix 10%4In beaker, POSS- (C is weighed according to polymeric matrix 10%3H6Cl)8In beaker
In, the DMF of 3mL is added, completely in 30 DEG C of -50 DEG C of water-bath heating stirrings to its dissolution, obtains pouring solution.
Step 2 ︰ pours into acquired solution in polytetrafluoro culture dish, 25 DEG C of -40 DEG C of vacuum drying 10h-12h, then is warming up to
60 DEG C -80 DEG C, it is dried in vacuo 20h-24h, obtains POSS compound cellulose/polycarbonate solid polymer dielectric B.
3 ︰ of embodiment
Step 1 ︰ weighs methylcellulose according to 60 ︰, 40 mass ratio and poly- ethylene carbonate mixes in beaker, and presses
LiClO is weighed according to polymeric matrix 10%4In beaker, POSS- (C is weighed according to polymeric matrix 10%3H6Cl)8In beaker
In, the DMF of 3mL is added, completely in 30 DEG C of -50 DEG C of water-bath heating stirrings to its dissolution, obtains pouring solution.
Step 2 ︰ pours into acquired solution in polytetrafluoro culture dish, 25 DEG C of -40 DEG C of vacuum drying 10h-12h, then is warming up to
60 DEG C -80 DEG C, it is dried in vacuo 20h-24h, obtains POSS compound cellulose/polycarbonate solid polymer dielectric C.
4 ︰ of embodiment
Step 1 ︰ weighs methylcellulose according to 80 ︰, 20 mass ratio and poly- ethylene carbonate mixes in beaker, and presses
LiClO is weighed according to polymeric matrix 10%4In beaker, POSS- (C is weighed according to polymeric matrix 10%3H6Cl)8In beaker
In, the DMF of 3mL is added, completely in 30 DEG C of -50 DEG C of water-bath heating stirrings to its dissolution, obtains pouring solution.
Step 2 ︰ pours into acquired solution in polytetrafluoro culture dish, 25 DEG C of -40 DEG C of vacuum drying 10h-12h, then is warming up to
60 DEG C -80 DEG C, it is dried in vacuo 20h-24h, obtains POSS compound cellulose/polycarbonate solid polymer dielectric D.
Claims (8)
1. a kind of POSS compound cellulose/polycarbonate solid polymer dielectric, it is characterised in that the quality proportioning of component is：
POSS accounts for the 1%-15% of polymeric matrix, and cellulose accounts for the 10%-90% of polymeric matrix, and polycarbonate accounts for polymeric matrix
10%-90%, lithium salts accounts for the 5%-15% of polymeric matrix, and above-mentioned four groups of assignment systems solution after-pouring is blended, and to obtain POSS multiple
Condensating fiber element/polycarbonate solid polymer dielectric；The cellulose is methylcellulose.
2. POSS compound cellulose/polycarbonate solid polymer dielectric according to claim 1, it is characterised in that：Institute
Stating POSS is POSS- (C3H6Cl)8Or POSS-PMMA.
3. POSS compound cellulose/polycarbonate solid polymer dielectric according to claim 1, it is characterised in that：Institute
State the 20%-80% that methylcellulose dosage is total polymer mass.
4. POSS compound cellulose/polycarbonate solid polymer dielectric according to claim 1, it is characterised in that：Institute
The polycarbonate stated accounts for the 20%-80% of the gross mass of polymeric matrix.
5. according to claim 1 or the 4 POSS compound cellulose/polycarbonate solid polymer dielectrics, it is characterised in that：
The polycarbonate is poly- ethylene carbonate PEC, polypropylene carbonate PPC or polymerized thylene carbonate vinyl acetate PVCA.
6. POSS compound cellulose/polycarbonate solid polymer dielectric according to claim 1, it is characterised in that：Institute
Stating lithium salts is lithium perchlorate LiClO4, hexafluoro phosphorus lithium LiFP6Or trifluoromethyl sulfonic acid lithium LiCF3SO3。
7. a kind of claim 1~7 any one of described POSS compound cellulose/polycarbonate solid polymer dielectric of preparing
Method, it is characterised in that steps are as follows：
Step 1：POSS, methylcellulose, polycarbonate and lithium salts and solvent are mixed, 30 DEG C -50 DEG C is heated to and stirs
Become solution to the dissolution of cellulose, polymer and lithium salts；
Step 2：By solution down in polytetrafluoro culture dish, in 25 DEG C of -40 DEG C of vacuum drying 10h-12h, then it is warming up to 60 DEG C -80
DEG C, it is dried in vacuo 20h-24h, obtains POSS compound cellulose/polycarbonate solid polymer dielectric.
8. according to the method described in claim 7, it is characterized in that：The solvent be n,N-Dimethylformamide DMF, toluene,
Methylene chloride or its blend.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109786823A (en) * | 2019-01-22 | 2019-05-21 | 广东天劲新能源科技股份有限公司 | A kind of PMMA base method for preparing gel polymer electrolyte |
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| CN105591154A (en) * | 2015-02-13 | 2016-05-18 | 中国科学院青岛生物能源与过程研究所 | Polycarbonate all-solid-state polymer electrolyte, all-solid-state secondary lithium battery made of same and preparation and application thereof |
| CN105762409A (en) * | 2016-03-02 | 2016-07-13 | 西北工业大学 | POSS composite porous gel polymer electrolyte and electrostatic spinning preparation method |
| CN107195963A (en) * | 2017-04-17 | 2017-09-22 | 哈尔滨工业大学无锡新材料研究院 | A kind of polymer dielectric of high conductivity and preparation method thereof |
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- 2018-06-01 CN CN201810555201.6A patent/CN108832177A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105591154A (en) * | 2015-02-13 | 2016-05-18 | 中国科学院青岛生物能源与过程研究所 | Polycarbonate all-solid-state polymer electrolyte, all-solid-state secondary lithium battery made of same and preparation and application thereof |
| CN105762409A (en) * | 2016-03-02 | 2016-07-13 | 西北工业大学 | POSS composite porous gel polymer electrolyte and electrostatic spinning preparation method |
| CN107195963A (en) * | 2017-04-17 | 2017-09-22 | 哈尔滨工业大学无锡新材料研究院 | A kind of polymer dielectric of high conductivity and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109786823A (en) * | 2019-01-22 | 2019-05-21 | 广东天劲新能源科技股份有限公司 | A kind of PMMA base method for preparing gel polymer electrolyte |
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