CN110128653A - A kind of high-performance polyimide preparation method and its application in electrode of lithium cell - Google Patents
A kind of high-performance polyimide preparation method and its application in electrode of lithium cell Download PDFInfo
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- CN110128653A CN110128653A CN201910453834.0A CN201910453834A CN110128653A CN 110128653 A CN110128653 A CN 110128653A CN 201910453834 A CN201910453834 A CN 201910453834A CN 110128653 A CN110128653 A CN 110128653A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1075—Partially aromatic polyimides
- C08G73/1082—Partially aromatic polyimides wholly aromatic in the tetracarboxylic moiety
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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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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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 present invention provides a kind of high-performance polyimide preparation method and its application in electrode of lithium cell, the high-performance polyimide preparation method is the following steps are included: S1, weigh aromatic dianhydride, it is placed in a reaction flask, nitrogen is passed through into reaction flask, continue 20~40min, non-protonic solvent is added, is stirred with the speed of 100~200r/min to aromatic dianhydride and is completely dissolved, obtains reaction solution I；S2, the temperature for adjusting reaction solution I are 38~45 DEG C, and diamines is added into reaction solution I with the speed of 2~4g/min, after being added to diamines, are kept for 35~45 DEG C and continue stirring 5~8 days to get high-performance polyimide.Preparation method proposed by the present invention, it is easy to operate, it is easy to use, raw material sources are abundant, and the high-performance polyimide operability being prepared is good, and chemical property and mechanical performance are excellent, and corrosion-resistant, electrolyte resistance and bending resistance are good.
Description
Technical field
The present invention relates to technical field of organic synthesis more particularly to a kind of high-performance polyimide preparation method and its in lithium
Application in battery electrode.
Background technique
Lithium ion battery because of its specific energy height, operating voltage height, light weight, self discharge is small, has extended cycle life, storage life
It is portable that the advantages that length, discharge performance stabilization, memory-less effect, small environmental pollution, is widely used in mobile phone, laptop etc.
On formula electronic product.Binder is one of essential material in lithium ion battery, has bonding electrode and keeps activity
The effect of substance can enhance the electronic contact between electrode active material and conductive agent and active material and collector, more
Stablize the structure of pole piece well.Currently, the adhesive industrially used is mainly Kynoar (PVDF), but PVDF is knot
Crystalline substance polymer, crystallinity are generally 50% or so, lithium ion battery routine at use temperature, the crystallinity of PVDF makes to deposit
Crystallinity molecule be difficult to circulate, cause charge and discharge electric load increase, in addition to this mechanical performance and chemical stability are also paid no attention to
Think, so application range is relatively narrow.Based on this, the present invention proposes a kind of high-performance polyimide preparation method and its in lithium battery
Application in extremely.
Summary of the invention
High, use process that the purpose of the present invention is to solve the crystallinity of PVDF used in existing lithium ion battery is not
Problem smooth, charge and discharge electric load is big, mechanical performance and chemical stability are undesirable, and a kind of high-performance polyimide proposed
Preparation method and its application in electrode of lithium cell.
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of high-performance polyimide preparation method and its application in electrode of lithium cell, comprising the following steps:
S1, aromatic dianhydride is weighed, be placed in a reaction flask, nitrogen is passed through into reaction flask, continue 20~40min, add non-matter
Sub- property solvent, is stirred to aromatic dianhydride with the speed of 100~200r/min and is completely dissolved, obtain reaction solution I；
S2, the temperature for adjusting reaction solution I are 38~45 DEG C, and diamines is added into reaction solution I with the speed of 2~4g/min, to
After diamines is added, is kept for 35~45 DEG C and continue stirring 5~8 days to get high-performance polyimide.
Preferably, the molar ratio of the aromatic dianhydride, non-protonic solvent and diamines is 0.85~1:38~44:1.
Preferably, the molar ratio of the aromatic dianhydride, non-protonic solvent and diamines is 0.9:42:1.
Preferably, the aromatic dianhydride 3,3'4, bis- methyl phenyl ethers anisole tetracid dianhydride of 4-, 3,3', 4,4'- biphenyltetracarboxylic dianhydrides,
One of pyromellitic dianhydride.
Preferably, the non-protonic solvent is N-Methyl pyrrolidone, n,N-dimethylacetamide, N, N- dimethyl methyl
One of amide.
Preferably, the diamines is p-phenylenediamine, 1,10- diamino decane, 4, one in 4 '-methylene bis cyclohexane amine
Kind.
Preferably, in step S1, the aromatic dianhydride is not completely dissolved in 5min, then system temperature is risen to 30~35
DEG C or mixing speed is improved continue stirring to 250~300r/min and be completely dissolved to aromatic dianhydride.
The above-mentioned preparation-obtained high-performance polyimide of high-performance polyimide preparation method.
Preparation method proposed by the present invention, advantage is compared with prior art:
1, preparation method proposed by the present invention, it is easy to operate, it is easy to use, raw material sources are abundant, are with aromatic dianhydride and diamines
Raw material, in non-protonic solvent, aromatic dianhydride first dissolves in non-protonic solvent again under the protection of nitrogen, then is being suitable for
At a temperature of reacted with diamines, obtain polyimides with high performance, the polyimides obtained by the preparation method has
There are the excellent erasable property made, chemical property and mechanical performance, and corrosion-resistant, electrolyte resistance and bending resistance are good, effectively solves
Determined PVDF used in existing lithium ion battery crystallinity it is high, use process is not smooth, charge and discharge electric load is big, mechanical performance
The undesirable problem with chemical stability；
2, preparation method proposed by the present invention by choosing suitable reaction raw materials, and regulates and controls aromatic dianhydride, non-protonic solvent
With the ratio of diamines, with it is quick, efficiently obtain polyimides, and be prepared through testing the preparation method proposed according to the present invention
Polyimides can satisfy the application requirement of lithium battery various aspects, therefore field of lithium can be widely applied to, expanded
The use scope of polyimides.
Specific embodiment
Combined with specific embodiments below the present invention is made further to explain.
Embodiment 1
A kind of high-performance polyimide preparation method proposed by the present invention and its application in electrode of lithium cell, including following step
It is rapid:
S1,3,3'4,4-, bis- methyl phenyl ethers anisole tetracid dianhydride is weighed, is placed in a reaction flask, nitrogen is passed through into reaction flask, continued
20min adds n,N-dimethylacetamide, is stirred with the speed of 200r/min complete to 3,3'4,4-, bis- methyl phenyl ethers anisole tetracid dianhydride
System temperature is then risen to 30~35 DEG C if bis- methyl phenyl ethers anisole tetracid dianhydride of 3,3'4,4- is not completely dissolved in 5min by fully dissolved
Or mixing speed is improved to 280r/min and continues stirring to aromatic dianhydride 3,3'4, bis- methyl phenyl ethers anisole tetracid dianhydride of 4- is completely dissolved,
Obtain reaction solution I；
S2, the temperature for adjusting reaction solution I are 38 DEG C, and 1, the 10- diamino last of the ten Heavenly stems is added into reaction solution I with the speed of 2g/min
Alkane after being added to 1,10- diamino decane, is kept for 45 DEG C continue stirring 8 days to get high-performance polyimide；
The molar ratio of aromatic dianhydride, non-protonic solvent and diamines is 0.85:44:1 in the present invention.
Embodiment 2
A kind of high-performance polyimide preparation method proposed by the present invention and its application in electrode of lithium cell, including following step
It is rapid:
S1, it 3,3', 4,4'- biphenyltetracarboxylic dianhydrides is weighed is placed in a reaction flask, nitrogen is passed through into reaction flask, continue 0min,
Add N-Methyl pyrrolidone, with the speed of 150r/min stir to 3,3', 4,4'- biphenyltetracarboxylic dianhydride of aromatic dianhydride,
Pyromellitic dianhydride to being completely dissolved, if 3,3', 4,4'- biphenyltetracarboxylic dianhydrides are not completely dissolved in 5min, then by system
Temperature, which rises to 30~35 DEG C or improves mixing speed to 300r/min, continues stirring to 3,3', 4,4'- biphenyltetracarboxylic dianhydride
It is completely dissolved, obtains reaction solution I；
S2, the temperature for adjusting reaction solution I are 40 DEG C, and 1,10- diamino decane is added into reaction solution I with the speed of 3/min,
After being added to 1,10- diamino decane, kept for 40 DEG C continue stirring 7 days to get high-performance polyimide；
The molar ratio of 3,3' in the present invention, 4,4'- biphenyltetracarboxylic dianhydride, N-Methyl pyrrolidone and 1,10- diamino decane
For 0.9:42:1.
Embodiment 3
A kind of high-performance polyimide preparation method proposed by the present invention and its application in electrode of lithium cell, including following step
It is rapid:
S1,3,3'4,4-, bis- methyl phenyl ethers anisole tetracid dianhydride is weighed, is placed in a reaction flask, nitrogen is passed through into reaction flask, continued
40min adds n,N-dimethylacetamide, is stirred with the speed of 100r/min molten to 3,3'4,4-, bis- methyl phenyl ethers anisole tetracid dianhydride
System temperature is then risen to 35 DEG C or will stirred by solution if bis- methyl phenyl ethers anisole tetracid dianhydride of 3,3'4,4- is not completely dissolved in 5min
Speed is improved to 300r/min to continue to stir to 3,3'4,4-, bis- methyl phenyl ethers anisole tetracid dianhydride and is completely dissolved, and obtains reaction solution I；
S2, the temperature for adjusting reaction solution I are 38 DEG C, and are incorporated as p-phenylenediamine into reaction solution I with the speed of 2g/min, to for
After p-phenylenediamine is added, kept for 40 DEG C continue stirring 6 days to get high-performance polyimide；
The molar ratio of bis- methyl phenyl ethers anisole tetracid dianhydride of 3,3'4,4-, DMAC N,N' dimethyl acetamide and p-phenylenediamine is 1 in the present invention:
38:1.
Embodiment 4
A kind of high-performance polyimide preparation method proposed by the present invention and its application in electrode of lithium cell, including following step
It is rapid:
S1,3,3'4,4-, bis- methyl phenyl ethers anisole tetracid dianhydride is weighed, is placed in a reaction flask, nitrogen is passed through into reaction flask, continued
20min adds n,N-Dimethylformamide, is stirred with the speed of 150r/min complete to 3,3'4,4-, bis- methyl phenyl ethers anisole tetracid dianhydride
Fully dissolved, if 3,3', 4,4'- biphenyltetracarboxylic dianhydrides are not completely dissolved in 5min, then system temperature are risen to 30 DEG C or incited somebody to action
Mixing speed is improved to 300r/min to continue to stir to 3,3'4,4-, bis- methyl phenyl ethers anisole tetracid dianhydride and is completely dissolved, and obtains reaction solution I；
S2, the temperature for adjusting reaction solution I are 42 DEG C, and 4,4 '-methylene bis hexamethylenes are added into reaction solution I with the speed of 4g/min
Alkanamine after being added to 4,4 '-methylene bis cyclohexane amine, is kept for 45 DEG C continue stirring 6 days to get high-performance polyimide；
Bis- methyl phenyl ethers anisole tetracid dianhydride of 3,3'4,4- in the present invention, N,N-dimethylformamide and 4,4 '-methylene bis cyclohexane amine
Molar ratio is 1:44:1.
Embodiment 5
A kind of high-performance polyimide preparation method proposed by the present invention and its application in electrode of lithium cell, including following step
It is rapid:
S1, pyromellitic dianhydride is weighed, be placed in a reaction flask, nitrogen is passed through into reaction flask, continued 40min, add N, N-
Dimethyl acetamide is stirred to pyromellitic dianhydride with the speed of 100r/min and is completely dissolved, if pyromellitic dianhydride does not exist
It is completely dissolved in 5min, then system temperature is risen to 35 DEG C or improves mixing speed to 250r/min and continue stirring to equal benzene four
Formic anhydride；
S2, the temperature for adjusting reaction solution I are 38 DEG C, and 4,4 '-methylene bis hexamethylenes are added into reaction solution I with the speed of 4g/min
Alkanamine after being added to 4,4 '-methylene bis cyclohexane amine, is kept for 45 DEG C continue stirring 5 days to get high-performance polyimide；
The molar ratio of pyromellitic dianhydride, DMAC N,N' dimethyl acetamide and 4,4 '-methylene bis cyclohexane amine is 1:38 in the present invention:
1。
The high-performance polyimide that above-described embodiment 1~5 is prepared is applied in electrode of lithium cell bonding, and test is viscous
The tensile strength and elongation at break of rear sample are connect, then carries out acidproof, alkaline-resisting and salt tolerant test, acidproof survey respectively to sample
Strip part: impregnating 72h in 10% hydrochloric acid solution, and soaking temperature is 80 DEG C；Alkaline-resisting test condition: in 30% sodium hydroxide solution
Middle immersion 72h, soaking temperature are 80 DEG C；Salt tolerant test condition: 72h, soaking temperature 80 are impregnated in 40% sodium chloride solution
℃；The tensile strength and elongation at break of sample after detection is corroded again after test, tensile strength changes after calculating corrosion
Rate and elongation at break change rate, as a result see the table below:
Testing result shows, the high-performance polyimide that the preparation method proposed through the invention is prepared it is acidproof, alkaline-resisting
It is excellent with salt resistant character, corrosion resistance and good.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of high-performance polyimide preparation method and its application in electrode of lithium cell, which is characterized in that including following
Step:
S1, aromatic dianhydride is weighed, be placed in a reaction flask, nitrogen is passed through into reaction flask, continue 20~40min, add non-matter
Sub- property solvent, is stirred to aromatic dianhydride with the speed of 100~200r/min and is completely dissolved, obtain reaction solution I；
S2, the temperature for adjusting reaction solution I are 38~45 DEG C, and diamines is added into reaction solution I with the speed of 2~4g/min, to
After diamines is added, is kept for 35~45 DEG C and continue stirring 5~8 days to get high-performance polyimide.
2. a kind of high-performance polyimide preparation method according to claim 1 and its application in electrode of lithium cell,
It is characterized in that, the molar ratio of the aromatic dianhydride, non-protonic solvent and diamines is 0.85~1:38~44:1.
3. a kind of high-performance polyimide preparation method according to claim 1 and its application in electrode of lithium cell,
It is characterized in that, the molar ratio of the aromatic dianhydride, non-protonic solvent and diamines is 0.9:42:1.
4. a kind of high-performance polyimide preparation method according to claim 1 or 2 or 3 and its in electrode of lithium cell
Using, which is characterized in that the aromatic dianhydride 3,3'4, bis- methyl phenyl ethers anisole tetracid dianhydride of 4-, 3,3', 4,4'- biphenyltetracarboxyacid acids two
One of acid anhydride, pyromellitic dianhydride.
5. a kind of high-performance polyimide preparation method according to claim 1 or 2 or 3 and its in electrode of lithium cell
Using, which is characterized in that the non-protonic solvent is N-Methyl pyrrolidone, n,N-dimethylacetamide, N, N- dimethyl
One of formamide.
6. a kind of high-performance polyimide preparation method according to claim 1 or 2 or 3 and its in electrode of lithium cell
It is p-phenylenediamine, 1,10- diamino decane, 4 using, which is characterized in that the diamines, one in 4 '-methylene bis cyclohexane amine
Kind.
7. a kind of high-performance polyimide preparation method according to claim 1 and its application in electrode of lithium cell,
It is characterized in that, the aromatic dianhydride is not completely dissolved in 5min in step S1, then by system temperature rise to 30~35 DEG C or
Mixing speed is improved to 250~300r/min to continue to stir to aromatic dianhydride and is completely dissolved.
8. the high-performance that high-performance polyimide preparation method described in any one is prepared according to claim 1~7 is poly-
Application of the acid imide in electrode of lithium cell.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112194935A (en) * | 2020-08-28 | 2021-01-08 | 河北金力新能源科技股份有限公司 | PVDF (polyvinylidene fluoride) slurry, diaphragm and preparation method thereof |
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