CN109524668A - A kind of anti-aging conduction rubber powder and preparation method thereof - Google Patents
A kind of anti-aging conduction rubber powder and preparation method thereof Download PDFInfo
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- CN109524668A CN109524668A CN201811233906.2A CN201811233906A CN109524668A CN 109524668 A CN109524668 A CN 109524668A CN 201811233906 A CN201811233906 A CN 201811233906A CN 109524668 A CN109524668 A CN 109524668A
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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
- H01M4/624—Electric conductive fillers
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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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- 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 discloses a kind of anti-aging conduction rubber powders, it is composed of the following raw materials by weight: ammonium persulfate 0.8-1, waste rubber powder 120-130, anti-aging agent rd2-3, acetic anhydride 3-5, catalyst 0.01-0.02, aniline 30-40, organic filler 10-12, dodecyl trimethyl ammonium chloride 1-2, zinc stearate 3-4, rubber powder of the invention has good anti-aging property, good weatherability, and also there is certain electric conductivity, enhance the application range of rubber powder.
Description
Technical field
The invention belongs to lithium ion battery electrode material fields, and in particular to a kind of anti-aging conduction rubber powder and its preparation side
Method.
Background technique
Now, for not discharging any polluted gas such as CO2、NOx, hydrocarbon etc electric car, compel to be essential
Develop a kind of rechargeable battery of high-energy density.Moreover, there is a perceived need to develop a kind of the chargeable of miniature efficient and light weight
Battery, for use as the power supply of portable device such as small personal computers, digital camera and mobile phone etc..
As the efficient rechargeable battery of this small, light, it has been suggested that a variety of lithium ion batteries, lithium ion battery is by having
Can reversibly the property of deintercalate lithium ions anode and cathode Yu nonaqueous electrolytic constitute.Battery electrode is as lithium-ion electric
The core building block in pond, it is also higher and higher to its performance requirement, however, there are still power for existing lithium ion battery electrode material
Learn the problems such as performance is poor, and electric conductivity is not high, easy to aging, preparation cost is higher.
Conducting polymer is a kind of macromolecule containing conjugated structure, is adulterated by modes such as chemistry, electrochemistry or ions
The level of conductivity of polymer can be made to reach metal rank from insulation rank, and the most insulating properties of rubber material used at present
Preferably, some also serves as insulating sheath material, therefore, the purpose of the present invention is to change the service performance of traditional rubber material, mentions
For a kind of conductive polymer composite rubber material, which raises the mechanical strength of finished product and conductive stabilities, and have good
Anti-aging property, good weatherability enhance the application range of rubber powder.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide one kind to be used for lithium ion cell positive material
Anti-aging conduction rubber powder of material and preparation method thereof.
To achieve the above object, the invention adopts the following technical scheme:
A kind of anti-aging conduction rubber powder, it is composed of the following raw materials by weight:
Ammonium persulfate 0.8-1, waste rubber powder 120-130, anti-aging agent rd2-3, acetic anhydride 3-5, catalyst 0.01-0.02, benzene
Amine 30-40, organic filler 10-12, dodecyl trimethyl ammonium chloride 1-2, zinc stearate 3-4.
The organic filler is made of the raw material of following weight parts:
Powdered whiting 20-30, silane coupling agent kh550 2-4, polytetrafluoroethylwax wax 3-5, thionyl chloride 17-20, ricinoleic acid
Calcium 1-2.
The preparation method of the organic filler, comprising the following steps:
(1) polytetrafluoroethylwax wax is taken, is added in thionyl chloride, increasing temperature is 50-55 DEG C, insulated and stirred 20-30 minutes, is obtained
Thionyl chloride solution；
(2) calcium ricinoleate is taken, is added in the dehydrated alcohol of 6-9 times of its weight, stirs evenly, silane coupling agent kh550 is added,
Increasing temperature is 60-70 DEG C, insulated and stirred 1-2 hours, obtains silanol solution；
(3) above-mentioned thionyl chloride solution, silanol solution mixing are taken, stirs evenly, powdered whiting, ultrasonic 100-140 is added
Minute, it filters, filter cake is washed, air drying is to get the organic filler.
The catalyst is the sulfuric acid that concentration is 96-98%.
A kind of preparation method of anti-aging conduction rubber powder, comprising the following steps:
(1) anti-aging agent rd is taken, is added in the dehydrated alcohol of 6-10 times of its weight, stirs evenly, waste rubber powder is added,
Insulated and stirred 20-30 minutes at 50-60 DEG C, alcohol dispersion liquid is obtained；
(2) acetic anhydride, aniline mixing are taken, is added in the deionized water of 4-10 times of mixture weight, stirs evenly, catalysis is added
Agent, it is 10-40 minutes ultrasonic, obtain aniline solution；
(3) ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly；
(4) dodecyl trimethyl ammonium chloride is taken, is added in the deionized water of 16-20 times of its weight, stirs evenly, addition has
Machine filler, it is 4-5 minutes ultrasonic, it mixes, is sent in reaction kettle with above-mentioned aniline solution, be passed through nitrogen, adjust temperature of reaction kettle
It is 65-70 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 4-5 hours, discharging cooling obtained organic polymer soln；
(5) above-mentioned alcohol dispersion liquid, organic polymer soln mixing is taken to filter, will sink insulated and stirred 1-2 hours at 90-95 DEG C
It forms sediment and washes, air drying obtains polymer-modified rubber powder；
(6) above-mentioned polymer-modified rubber powder is taken, mixes, stirs evenly with zinc stearate, be sent in extruder, melting extrusion,
Cooling is to get the anti-aging conduction rubber powder.
Advantages of the present invention:
The present invention uses amino silane modified calcium carbonate first, then uses acetic anhydride process aniline, makees in the catalysis of the concentrated sulfuric acid
Acetylization reaction is carried out under, is polymerize under initiator effect later, is introduced amino modified calcium carbonate in the course of the polymerization process, from
And dispersion compatibility of the calcium carbonate between polyaniline is improved, so that the mechanical strength and conductive stability of finished product are improved, this
The rubber powder of invention has good anti-aging property, good weatherability, and also has certain electric conductivity, is being used for lithium ion battery
When the filler of positive electrode, the service life of electrode can be improved, improve the service life of lithium ion battery.
Specific embodiment
Embodiment 1
A kind of anti-aging conduction rubber powder, it is composed of the following raw materials by weight:
Ammonium persulfate 0.8, waste rubber powder 120, anti-aging agent rd2, acetic anhydride 3, catalyst 0.01, aniline 30, organic filler 10,
Dodecyl trimethyl ammonium chloride 1, zinc stearate 3.
The organic filler is made of the raw material of following weight parts:
Powdered whiting 20, silane coupling agent kh550 2, polytetrafluoroethylwax wax 3, thionyl chloride 17, calcium ricinoleate 1.
The preparation method of the organic filler, comprising the following steps:
(1) polytetrafluoroethylwax wax is taken, is added in thionyl chloride, increasing temperature is 50 DEG C, insulated and stirred 20 minutes, obtains protochloride
Sulfolane solution；
(2) calcium ricinoleate is taken, is added in the dehydrated alcohol of 6 times of its weight, stirs evenly, silane coupling agent kh550 is added, is risen
High-temperature is 60 DEG C, insulated and stirred 1 hour, obtains silanol solution；
(3) above-mentioned thionyl chloride solution, silanol solution mixing are taken, is stirred evenly, powdered whiting is added, it is 100 minutes ultrasonic,
It filters, filter cake is washed, air drying is to get the organic filler.
The catalyst is the sulfuric acid that concentration is 96%.
A kind of preparation method of anti-aging conduction rubber powder, comprising the following steps:
(1) anti-aging agent rd is taken, is added in the dehydrated alcohol of 6 times of its weight, stirs evenly, waste rubber powder is added, at 50 DEG C
Lower insulated and stirred 20 minutes, obtains alcohol dispersion liquid；
(2) acetic anhydride, aniline mixing are taken, is added in 4 times of mixture weight of deionized water, stirs evenly, catalyst is added,
Ultrasound 10 minutes, obtains aniline solution；
(3) ammonium persulfate is taken, is added in the deionized water of 20 times of its weight, stirs evenly；
(4) dodecyl trimethyl ammonium chloride is taken, is added in the deionized water of 16 times of its weight, stirs evenly, is added organic
Filler, ultrasound 4 minutes, mixes with above-mentioned aniline solution, is sent in reaction kettle, is passed through nitrogen, and adjusting temperature of reaction kettle is 65
DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 4 hours, discharging cooling obtained organic polymer soln；
(5) above-mentioned alcohol dispersion liquid, organic polymer soln mixing are taken, insulated and stirred 1 hour at 90 DEG C filters, will precipitate water
It washes, air drying, obtains polymer-modified rubber powder；
(6) above-mentioned polymer-modified rubber powder is taken, mixes, stirs evenly with zinc stearate, be sent in extruder, melting extrusion,
Cooling is to get the anti-aging conduction rubber powder.
Embodiment 2
A kind of anti-aging conduction rubber powder, it is composed of the following raw materials by weight:
Ammonium persulfate 1, waste rubber powder 130, anti-aging agent rd3, acetic anhydride 5, catalyst 0.02, aniline 40, organic filler 12, ten
Dialkyl group trimethyl ammonium chloride 2, zinc stearate 4.
The organic filler is made of the raw material of following weight parts:
Powdered whiting 30, silane coupling agent kh550 4, polytetrafluoroethylwax wax 5, thionyl chloride 20, calcium ricinoleate 2.
The preparation method of the organic filler, comprising the following steps:
(1) polytetrafluoroethylwax wax is taken, is added in thionyl chloride, increasing temperature is 55 DEG C, insulated and stirred 20-30 minutes, obtains chlorine
Change sulfoxide solution；
(2) calcium ricinoleate is taken, is added in the dehydrated alcohol of 9 times of its weight, stirs evenly, silane coupling agent kh550 is added, is risen
High-temperature is 70 DEG C, insulated and stirred 2 hours, obtains silanol solution；
(3) above-mentioned thionyl chloride solution, silanol solution mixing are taken, is stirred evenly, powdered whiting is added, it is 140 minutes ultrasonic,
It filters, filter cake is washed, air drying is to get the organic filler.
The catalyst is the sulfuric acid that concentration is 98%.
A kind of preparation method of anti-aging conduction rubber powder, comprising the following steps:
(1) anti-aging agent rd is taken, is added in the dehydrated alcohol of 10 times of its weight, stirs evenly, waste rubber powder is added, at 60 DEG C
Lower insulated and stirred 30 minutes, obtains alcohol dispersion liquid；
(2) acetic anhydride, aniline mixing are taken, mixture is added to and weighs in 10 times of deionized water, stir evenly, catalyst is added,
Ultrasound 40 minutes, obtains aniline solution；
(3) ammonium persulfate is taken, is added in the deionized water of 30 times of its weight, stirs evenly；
(4) dodecyl trimethyl ammonium chloride is taken, is added in the deionized water of 20 times of its weight, stirs evenly, is added organic
Filler, ultrasound 5 minutes, mixes with above-mentioned aniline solution, is sent in reaction kettle, is passed through nitrogen, and adjusting temperature of reaction kettle is 70
DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 5 hours, discharging cooling obtained organic polymer soln；
(5) above-mentioned alcohol dispersion liquid, organic polymer soln mixing are taken, insulated and stirred 2 hours at 95 DEG C filter, will precipitate water
It washes, air drying, obtains polymer-modified rubber powder；
(6) above-mentioned polymer-modified rubber powder is taken, mixes, stirs evenly with zinc stearate, be sent in extruder, melting extrusion,
Cooling is to get the anti-aging conduction rubber powder.
Performance test:
The anti-aging conduction rubber powder of the embodiment of the present invention 1:
Tensile strength: 19.1Mpa；
70 DEG C × 70h air oven aging test:
Breaking strength reduced rate: 4.4%, elongation at break reduced rate: 3.9%；
Conductivity is 0.02 S/cm；
The anti-aging conduction rubber powder of the embodiment of the present invention 2:
Tensile strength: 18.6Mpa；
70 DEG C × 70h air oven aging test:
Breaking strength reduced rate: 4.7%, elongation at break reduced rate: 3.2%；
Conductivity is 0.04S/cm.
Claims (5)
1. a kind of anti-aging conduction rubber powder, it is composed of the following raw materials by weight:
Ammonium persulfate 0.8-1, waste rubber powder 120-130, anti-aging agent rd2-3, acetic anhydride 3-5, catalyst 0.01-0.02, benzene
Amine 30-40, organic filler 10-12, dodecyl trimethyl ammonium chloride 1-2, zinc stearate 3-4；It is characterized in that, described organic
Filler includes powdered whiting.
2. a kind of anti-aging conduction rubber powder according to claim 1, which is characterized in that the organic filler is by following
The raw material composition of parts by weight:
Powdered whiting 20-30, silane coupling agent kh550 2-4, polytetrafluoroethylwax wax 3-5, thionyl chloride 17-20, ricinoleic acid
Calcium 1-2.
3. a kind of anti-aging conduction rubber powder according to claim 2, which is characterized in that the preparation side of the organic filler
Method, comprising the following steps:
(1) polytetrafluoroethylwax wax is taken, is added in thionyl chloride, increasing temperature is 50-55 DEG C, insulated and stirred 20-30 minutes, is obtained
Thionyl chloride solution；
(2) calcium ricinoleate is taken, is added in the dehydrated alcohol of 6-9 times of its weight, stirs evenly, silane coupling agent kh550 is added,
Increasing temperature is 60-70 DEG C, insulated and stirred 1-2 hours, obtains silanol solution；
(3) above-mentioned thionyl chloride solution, silanol solution mixing are taken, stirs evenly, powdered whiting, ultrasonic 100-140 is added
Minute, it filters, filter cake is washed, air drying is to get the organic filler.
4. a kind of anti-aging conduction rubber powder according to claim 1, which is characterized in that the catalyst is that concentration is
The sulfuric acid of 96-98%.
5. a kind of preparation method of anti-aging conduction rubber powder as described in claim 1, which comprises the following steps:
(1) anti-aging agent rd is taken, is added in the dehydrated alcohol of 6-10 times of its weight, stirs evenly, waste rubber powder is added,
Insulated and stirred 20-30 minutes at 50-60 DEG C, alcohol dispersion liquid is obtained；
(2) acetic anhydride, aniline mixing are taken, is added in the deionized water of 4-10 times of mixture weight, stirs evenly, catalysis is added
Agent, it is 10-40 minutes ultrasonic, obtain aniline solution；
(3) ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly；
(4) dodecyl trimethyl ammonium chloride is taken, is added in the deionized water of 16-20 times of its weight, stirs evenly, addition has
Machine filler, it is 4-5 minutes ultrasonic, it mixes, is sent in reaction kettle with above-mentioned aniline solution, be passed through nitrogen, adjust temperature of reaction kettle
It is 65-70 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 4-5 hours, discharging cooling obtained organic polymer soln；
(5) above-mentioned alcohol dispersion liquid, organic polymer soln mixing is taken to filter, will sink insulated and stirred 1-2 hours at 90-95 DEG C
It forms sediment and washes, air drying obtains polymer-modified rubber powder；
(6) above-mentioned polymer-modified rubber powder is taken, mixes, stirs evenly with zinc stearate, be sent in extruder, melting extrusion,
Cooling is to get the anti-aging conduction rubber powder.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811233906.2A CN109524668A (en) | 2018-10-23 | 2018-10-23 | A kind of anti-aging conduction rubber powder and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811233906.2A CN109524668A (en) | 2018-10-23 | 2018-10-23 | A kind of anti-aging conduction rubber powder and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102532892A (en) * | 2012-01-20 | 2012-07-04 | 北京师范大学 | Conductive polymer film and preparation method thereof |
| CN107118555A (en) * | 2017-06-22 | 2017-09-01 | 常州大学 | The method that solution blended process prepares polyamideimide-based antistatic film |
| CN107418111A (en) * | 2017-08-01 | 2017-12-01 | 中国科学技术大学 | For strain and/or the preparation method of pressure sensing conductive polymer composite |
-
2018
- 2018-10-23 CN CN201811233906.2A patent/CN109524668A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102532892A (en) * | 2012-01-20 | 2012-07-04 | 北京师范大学 | Conductive polymer film and preparation method thereof |
| CN107118555A (en) * | 2017-06-22 | 2017-09-01 | 常州大学 | The method that solution blended process prepares polyamideimide-based antistatic film |
| CN107418111A (en) * | 2017-08-01 | 2017-12-01 | 中国科学技术大学 | For strain and/or the preparation method of pressure sensing conductive polymer composite |
Non-Patent Citations (1)
| Title |
|---|
| 胡桢等: "《新型高分子合成与制备工艺》", 30 May 2014 * |
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Application publication date: 20190326 |