CN109384984A - A kind of conductive fiber crosslinking rubber powder and preparation method thereof - Google Patents
A kind of conductive fiber crosslinking rubber powder and preparation method thereof Download PDFInfo
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- CN109384984A CN109384984A CN201811230443.4A CN201811230443A CN109384984A CN 109384984 A CN109384984 A CN 109384984A CN 201811230443 A CN201811230443 A CN 201811230443A CN 109384984 A CN109384984 A CN 109384984A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L19/00—Compositions of rubbers not provided for in groups C08L7/00 - C08L17/00
- C08L19/003—Precrosslinked rubber; Scrap rubber; Used vulcanised rubber
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2319/00—Characterised by the use of rubbers not provided for in groups C08J2307/00 - C08J2317/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of conductive fibers to be crosslinked rubber powder, it is composed of the following raw materials by weight: conductive fiber lotion 30-40, diisocyanate 1-2, waste rubber powder 110-120, anti-aging agent rd 2-3, nickel sulfamic acid 0.4-0.7, N-Methyl pyrrolidone 16-20, the crosslinked action that the present invention passes through diisocyanate, further improve the mechanical stability of finished-product material, rubber powder of the invention has good conductive stability, and comprehensive performance is superior.
Description
Technical field
The invention belongs to lithium ion battery electrode material fields, and in particular to a kind of conductive fiber crosslinking rubber powder and its preparation
Method.
Background technique
Lithium ion battery have energy density height, output power, self discharge is small, memory-less effect, has extended cycle life, ring
The advantages that border is friendly, lithium ion battery is in 3C such as mobile phone, notebook computer, digital camera, video cameras at present
Application in articles as high-energy density power supply is very mature, however, higher for having compared to above-mentioned 3C articles
The application fields such as the application of power, e.g. electric car, the application of lithium ion battery is then not yet mature, and reason is at present
The positive electrode material of lithium ion battery there are still electrical conductivities it is too low, cost is excessively high the problems such as.
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, passed in capacitor, the energy, anti-corrosion of metal and biology
It has a good application prospect in terms of sensor, the anode using conducting polymer as lithium ion battery has caused in the world at present
Extensive concern.And its key technology is still the conductive fiber that solve to have high mechanical property, high conductivity, low cost
Problem.
The all directly a large amount of purchase rubber powders of general reclaimed rubber factory, the yield of the annual reclaimed rubber in the whole nation is at 1,000,000 tons or more, each province
There is the reclaimed rubber factory for the scale of differing in size, rubber powder is the primary raw material of reclaimed rubber, is widely used, and low in cost.And
The most insulating properties of rubber material used at present is preferable, and some also serves as insulating sheath material, and therefore, the purpose of the present invention is to change
The service performance for becoming traditional rubber material, provides a kind of conductive polymer composite rubber material, which improve conductive fibers in glue
Dispersion compatibility between powder improves the conductive stability and mechanical stability of finished-product material, so that it is superior to obtain comprehensive performance
Anode material for lithium-ion batteries.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of conductive fiber crosslinking rubber powder and its
Preparation method.
To achieve the above object, the invention adopts the following technical scheme:
A kind of conductive fiber crosslinking rubber powder, it is composed of the following raw materials by weight:
Conductive fiber lotion 30-40, diisocyanate 1-2, waste rubber powder 110-120, anti-aging agent rd 2-3, nickel sulfamic acid
0.4-0.7, N-Methyl pyrrolidone 16-20.
What the conductive fiber lotion was made of the raw material of following weight parts:
Methylcellulose 4-6, pyrroles 50-60, ammonium persulfate 1-1.2, sym-closene 2-3, polysorbate 0.1-0.3.
The preparation method of the conductive fiber lotion, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly；
(2) methylcellulose, sym-closene mixing are taken, insulated and stirred 10-40 minutes at 50-55 DEG C, is added to mixing
In the deionized water of 3-10 times of weight of material, stirs evenly, obtain fiber solution；
(3) pyrroles is taken, is added in above-mentioned fiber solution, stirs evenly, be sent in reaction kettle, is passed through nitrogen, adjusts reaction
Kettle temperature degree is 65-70 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 3-4 hours, discharging was mixed with polysorbate, stirred
It mixes to room temperature to get the conductive fiber lotion.
A kind of preparation method of conductive fiber crosslinking rubber powder, comprising the following steps:
(1) anti-aging agent rd is taken, is added in the dehydrated alcohol of 10-14 times of its weight, stirs evenly, waste rubber powder is added, is risen
High-temperature is 50-60 DEG C, insulated and stirred 10-20 minutes, obtains alcohol dispersion liquid；
(2) diisocyanate is taken, is added in N-Methyl pyrrolidone, is stirred evenly, cross-linked disperse liquid is obtained；
(3) above-mentioned conductive fiber lotion, the mixing of alcohol dispersion liquid are taken, stirs evenly, is sent in reaction kettle, be passed through nitrogen, be added
Above-mentioned cross-linked disperse liquid, insulated and stirred 2-3 hours at 80-90 DEG C, discharging is mixed with nickel sulfamic acid, is stirred evenly, and is taken out
Filter, filter cake is washed, and is sent into baking oven, 20-49 minutes dry at 50-55 DEG C, and discharging is cooling to get conductive fiber friendship
Join rubber powder.
Advantages of the present invention:
The present invention is using pyrroles as monomer, using the fiber solution of sym-closene as solvent, polymerize under initiator effect, obtains
It is blended conductive fiber lotion with the alcoholic solution of rubber powder, and high temperature esterification introduces diisocyanate, not only in esterification process
Dispersion compatibility of the conductive fiber between rubber powder effectively is improved, and by the crosslinked action of diisocyanate, further
The mechanical stability of finished-product material is improved, rubber powder of the invention has good conductive stability, and comprehensive performance is superior.
Specific embodiment
Embodiment 1
A kind of conductive fiber crosslinking rubber powder, it is composed of the following raw materials by weight:
Conductive fiber lotion 30, diisocyanate 1, waste rubber powder 110, anti-aging agent rd 2, nickel sulfamic acid 0.4, N- methyl
Pyrrolidones 16.
What the conductive fiber lotion was made of the raw material of following weight parts:
Methylcellulose 4, pyrroles 50, ammonium persulfate 1, sym-closene 2, polysorbate 0.1.
The preparation method of the conductive fiber lotion, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 20 times of its weight, stirs evenly；
(2) methylcellulose, sym-closene mixing are taken, insulated and stirred 10 minutes at 50 DEG C are added to mixture weight 3
In deionized water again, stirs evenly, obtain fiber solution；
(3) pyrroles is taken, is added in above-mentioned fiber solution, stirs evenly, be sent in reaction kettle, is passed through nitrogen, adjusts reaction
Kettle temperature degree is 65 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 3 hours, discharging was mixed with polysorbate, and stirring is extremely
Room temperature is to get the conductive fiber lotion.
A kind of preparation method of conductive fiber crosslinking 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, increases temperature
Degree is 50 DEG C, insulated and stirred 10 minutes, obtains alcohol dispersion liquid；
(2) diisocyanate is taken, is added in N-Methyl pyrrolidone, is stirred evenly, cross-linked disperse liquid is obtained；
(3) above-mentioned conductive fiber lotion, the mixing of alcohol dispersion liquid are taken, stirs evenly, is sent in reaction kettle, be passed through nitrogen, be added
Above-mentioned cross-linked disperse liquid, insulated and stirred 2 hours at 80 DEG C, discharging are mixed with nickel sulfamic acid, are stirred evenly, and are filtered, will be filtered
Cake washing, is sent into baking oven, 20 minutes dry at 50 DEG C, and discharging is cooling to be crosslinked rubber powder to get the conductive fiber.
Embodiment 2
A kind of conductive fiber crosslinking rubber powder, it is composed of the following raw materials by weight:
Conductive fiber lotion 40, diisocyanate 2, waste rubber powder 120, anti-aging agent rd 3, nickel sulfamic acid 0.7, N- methyl
Pyrrolidones 20.
What the conductive fiber lotion was made of the raw material of following weight parts:
Methylcellulose 6, pyrroles 60, ammonium persulfate 1.2, sym-closene 3, polysorbate 0.3.
The preparation method of the conductive fiber lotion, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 30 times of its weight, stirs evenly；
(2) methylcellulose, sym-closene mixing are taken, insulated and stirred 40 minutes at 55 DEG C are added to mixture weight
It in 10 times of deionized water, stirs evenly, obtains fiber solution；
(3) pyrroles is taken, is added in above-mentioned fiber solution, stirs evenly, be sent in reaction kettle, is passed through nitrogen, adjusts reaction
Kettle temperature degree is 70 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 4 hours, discharging was mixed with polysorbate, and stirring is extremely
Room temperature is to get the conductive fiber lotion.
A kind of preparation method of conductive fiber crosslinking rubber powder, comprising the following steps:
(1) anti-aging agent rd is taken, is added in the dehydrated alcohol of 14 times of its weight, stirs evenly, waste rubber powder is added, increases temperature
Degree is 60 DEG C, insulated and stirred 20 minutes, obtains alcohol dispersion liquid；
(2) diisocyanate is taken, is added in N-Methyl pyrrolidone, is stirred evenly, cross-linked disperse liquid is obtained；
(3) above-mentioned conductive fiber lotion, the mixing of alcohol dispersion liquid are taken, stirs evenly, is sent in reaction kettle, be passed through nitrogen, be added
Above-mentioned cross-linked disperse liquid, insulated and stirred 2-3 hours at 90 DEG C, discharging is mixed with nickel sulfamic acid, is stirred evenly, and is filtered, will
Filter cake washing, is sent into baking oven, 49 minutes dry at 55 DEG C, and discharging is cooling to be crosslinked rubber powder to get the conductive fiber.
Performance test:
The conductive fiber of the embodiment of the present invention 1 is crosslinked rubber powder:
Tensile strength: 18.4Mpa；
70 DEG C × 70h air oven aging test:
Breaking strength reduced rate: 2.5%, elongation at break reduced rate: 2.1%；
Conductivity is 0.07 S/cm；
The conductive fiber of the embodiment of the present invention 2 is crosslinked rubber powder:
Tensile strength: 20.1Mpa；
70 DEG C × 70h air oven aging test:
Breaking strength reduced rate: 2.7%, elongation at break reduced rate: 2.5%；
Conductivity is 0.05S/cm.
Claims (4)
1. a kind of conductive fiber is crosslinked rubber powder, which is characterized in that it is composed of the following raw materials by weight:
Conductive fiber lotion 30-40, diisocyanate 1-2, waste rubber powder 110-120, anti-aging agent rd 2-3, nickel sulfamic acid
0.4-0.7, N-Methyl pyrrolidone 16-20.
2. a kind of conductive fiber according to claim 1 is crosslinked rubber powder, which is characterized in that the conductive fiber lotion is
It is made of the raw material of following weight parts:
Methylcellulose 4-6, pyrroles 50-60, ammonium persulfate 1-1.2, sym-closene 2-3, polysorbate 0.1-0.3.
3. a kind of conductive fiber according to claim 2 is crosslinked rubber powder, which is characterized in that the conductive fiber lotion
Preparation method, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly；
(2) methylcellulose, sym-closene mixing are taken, insulated and stirred 10-40 minutes at 50-55 DEG C, is added to mixing
In the deionized water of 3-10 times of weight of material, stirs evenly, obtain fiber solution；
(3) pyrroles is taken, is added in above-mentioned fiber solution, stirs evenly, be sent in reaction kettle, is passed through nitrogen, adjusts reaction
Kettle temperature degree is 65-70 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 3-4 hours, discharging was mixed with polysorbate, stirred
It mixes to room temperature to get the conductive fiber lotion.
4. a kind of preparation method of conductive fiber crosslinking rubber powder as described in claim 1, which is characterized in that including following step
It is rapid:
(1) anti-aging agent rd is taken, is added in the dehydrated alcohol of 10-14 times of its weight, stirs evenly, waste rubber powder is added, is risen
High-temperature is 50-60 DEG C, insulated and stirred 10-20 minutes, obtains alcohol dispersion liquid；
(2) diisocyanate is taken, is added in N-Methyl pyrrolidone, is stirred evenly, cross-linked disperse liquid is obtained；
(3) above-mentioned conductive fiber lotion, the mixing of alcohol dispersion liquid are taken, stirs evenly, is sent in reaction kettle, be passed through nitrogen, be added
Above-mentioned cross-linked disperse liquid, insulated and stirred 2-3 hours at 80-90 DEG C, discharging is mixed with nickel sulfamic acid, is stirred evenly, and is taken out
Filter, filter cake is washed, and is sent into baking oven, 20-49 minutes dry at 50-55 DEG C, and discharging is cooling to get conductive fiber friendship
Join rubber powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811230443.4A CN109384984A (en) | 2018-10-22 | 2018-10-22 | A kind of conductive fiber crosslinking rubber powder and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811230443.4A CN109384984A (en) | 2018-10-22 | 2018-10-22 | A kind of conductive fiber crosslinking rubber powder and preparation method thereof |
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| CN109384984A true CN109384984A (en) | 2019-02-26 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492372A (en) * | 2011-12-16 | 2012-06-13 | 中国人民解放军第三军医大学 | Static-free glue and preparation method thereof |
| CN105400007A (en) * | 2015-12-02 | 2016-03-16 | 安徽创奇乐智能游乐设备有限公司 | Oil-resistance anti-static composite rubber material |
| CA2983723A1 (en) * | 2016-10-26 | 2018-04-26 | J. Van Beugen Beheer B.V. | Inflatable stopper |
| CN108341934A (en) * | 2018-04-09 | 2018-07-31 | 南安市创培电子科技有限公司 | A kind of fiber composite polythiophene additives for battery and preparation method thereof |
| CN108559261A (en) * | 2018-05-12 | 2018-09-21 | 温州市赢创新材料技术有限公司 | Polypyrrole conductive additive and preparation method thereof is blended in a kind of rubber powder |
-
2018
- 2018-10-22 CN CN201811230443.4A patent/CN109384984A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492372A (en) * | 2011-12-16 | 2012-06-13 | 中国人民解放军第三军医大学 | Static-free glue and preparation method thereof |
| CN105400007A (en) * | 2015-12-02 | 2016-03-16 | 安徽创奇乐智能游乐设备有限公司 | Oil-resistance anti-static composite rubber material |
| CA2983723A1 (en) * | 2016-10-26 | 2018-04-26 | J. Van Beugen Beheer B.V. | Inflatable stopper |
| CN108341934A (en) * | 2018-04-09 | 2018-07-31 | 南安市创培电子科技有限公司 | A kind of fiber composite polythiophene additives for battery and preparation method thereof |
| CN108559261A (en) * | 2018-05-12 | 2018-09-21 | 温州市赢创新材料技术有限公司 | Polypyrrole conductive additive and preparation method thereof is blended in a kind of rubber powder |
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Application publication date: 20190226 |