CN108395576A - A kind of graphite acrylamide dispersion liquid and its application in anti-oxidant Polypyrrole Conducting Materials - Google Patents
A kind of graphite acrylamide dispersion liquid and its application in anti-oxidant Polypyrrole Conducting Materials Download PDFInfo
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- CN108395576A CN108395576A CN201810353163.6A CN201810353163A CN108395576A CN 108395576 A CN108395576 A CN 108395576A CN 201810353163 A CN201810353163 A CN 201810353163A CN 108395576 A CN108395576 A CN 108395576A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- C08G73/0605—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0611—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring, e.g. polypyrroles
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
- H01B1/124—Intrinsically conductive polymers
- H01B1/127—Intrinsically conductive polymers comprising five-membered aromatic rings in the main chain, e.g. polypyrroles, polythiophenes
Abstract
The invention belongs to Material Fields, and in particular to a kind of graphite acrylamide dispersion liquid and its application in anti-oxidant Polypyrrole Conducting Materials.The graphite acrylamide dispersion liquid is made by following steps：1）The preparation of alcohol dispersion liquid；2）The preparation of amide solution；3）The preparation of graphite acrylamide dispersion liquid.The present invention prepares amide solution by raw material of 2 mercapto benzimidazoles, then dispersed graphite alkene is come with this, so as to improve the reactivity of graphene surface, the graphene is participated in the polymerisation of anti-oxidant monomer later, to obtain the anti-oxidant Polypyrrole Conducting Materials that inoxidizability is strong, mechanical stability is high.
Description
Technical field
The invention belongs to Material Fields, and in particular to a kind of graphite acrylamide dispersion liquid and its in anti-oxidant polypyrrole conduction
Application in material.
Background technology
Graphene is a kind of material for the monatomic layer structure being made of hexagonal honeycomb lattice carbon atom, is had very excellent
Different conduction, heat conduction and mechanical performance, can be widely used in each field.But graphene is as a kind of two-dimensional nano material
Material is very easy to reunite, and graphene is changed into graphite-structure again after reuniting, it is difficult to play its unique performance.
Therefore it is to solve current graphene application urgent problem how by the dispersion of graphene uniform.
Polypyrrole is a kind of typical silver type conducting polymer altogether, has good light, electricity, magnetic characteristic, and with opposite
The features such as being easy each system and preferable environmental stability, receives the extensive concern of researcher.Currently, the research of polypyrrole and answering
With very extensive, be directed not only to the fields such as sensor, capacitor, electroluminescent, electrochromism and electromagnetic shielding, and with life
Object, nanotechnology combine, and apply also for the intellectual materials neck such as controlled release of manufacture molecular wire, artificial-muscle and drug
Domain；However the inoxidizability of polypyrrole material is not high at present, bin stability is poor, has seriously affected its using effect.
Invention content
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of graphite acrylamide dispersion liquid and its
Application in anti-oxidant Polypyrrole Conducting Materials.
To achieve the above object, the present invention uses following technical scheme：
A kind of graphite acrylamide dispersion liquid, the graphite acrylamide dispersion liquid are made by following steps：
1）The preparation of alcohol dispersion liquid
Cyanuric acid zinc is taken, is added in 10-17 times of absolute ethyl alcohol of its weight, stirs evenly, 2- mercapto benzimidazoles are added, is risen
For high-temperature to 55-60 DEG C, insulated and stirred 30-40 minutes obtains alcohol dispersion liquid；
2）The preparation of amide solution
Polyamide wax micropowder is taken, is added in the dimethylformamide of 3-5 times of its weight, is sent in 130-140 DEG C of oil bath,
Stirring 20-30 minutes, discharging, mixes with above-mentioned alcohol dispersion liquid, stirs evenly, obtain amide solution；
3）Graphite acrylamide dispersion liquid
Graphene is taken, is added in above-mentioned amide solution, bis-phenol a diglycidyl ethers are added, it is 5-10 minutes ultrasonic, obtain graphene
Amide dispersion liquid.
Wherein, it counts in parts by weight, each raw material is：1-2 parts of cyanuric acid zinc, 0.7-1 parts of 2- mercapto benzimidazoles, polyamides
3-4 parts of amine wax micro mist, 10-13 parts of graphene, 0.1-0.3 parts of bis-phenol a diglycidyl ethers.
A kind of graphite acrylamide dispersion liquid and its application in anti-oxidant Polypyrrole Conducting Materials, concrete application step
It is：Anti-oxidant modified pyrrole monomer is taken, is added in claim 1 in gained graphite acrylamide dispersion liquid, is stirred evenly, be sent to
In reaction kettle, it is passed through nitrogen, it is 65-70 DEG C to adjust temperature of reaction kettle, and initiator solution, insulated and stirred 4-5 hours, discharging is added
It is cooling, obtain anti-oxidant modified polypyrrole solution；Anti-oxidant modified polypyrrole solution is filtered, filter cake is washed, air drying, is made
Obtain anti-oxidant Polypyrrole Conducting Materials.
Wherein, count in parts by weight, described anti-oxidant modified pyrrole monomer 140-200 parts, initiator solution be by 5-7 parts
Initiator cumyl peroxide is added to stirred evenly in the isopropanol of 18-20 times of its weight after be made.
Preferably, anti-oxidant modified pyrrole monomer of the present invention, is made by following steps：
1）The 60-70% of above-mentioned toluene by weight is taken, dialkyl group is added to biphenol, is sent in 40-50 DEG C of water bath with thermostatic control, adds
Enter pyrroles, insulated and stirred 1-2 hours, discharging cooling obtains pyrroles's dispersion liquid；
2）Boric acid is taken, is added in remaining toluene, stirs evenly, be sent in reaction kettle, is passed through nitrogen, Ji Wusi is added
Alcohol increases temperature to 55-60 DEG C, and insulated and stirred 30-40 minutes, discharging cooling obtains ester raw material；
3）Above-mentioned ester raw material is taken, is added in pyrroles's dispersion liquid, stirs evenly, it is 10-20 minutes ultrasonic, toluene is distilled off, i.e.,
Obtain the anti-oxidant modified pyrrole monomer.
Wherein, it counts in parts by weight, each raw material：Dialkyl group to 3-4 parts of biphenol, 100-120 parts of pyrroles, 3-5 parts of boric acid,
3-4 parts of pentaerythrite, 40-54 parts of toluene.
Advantages of the present invention：
The present invention prepares amide solution by raw material of 2- mercaptos benzimidazole, then carrys out dispersed graphite alkene with this, so as to improve
The reactivity of graphene surface, participates in the graphene in the polymerisation of anti-oxidant monomer, later to obtain
The anti-oxidant Polypyrrole Conducting Materials that inoxidizability is strong, mechanical stability is high.
The anti-oxidant modified pyrrole monomer that the present invention is added uses dialkyl group to handle pyrrole monomer to biphenol first, leads to
The esterification of perboric acid and pentaerythrite, the effective reactivity for improving pyrrole monomer, while it is good to impart monomer
Antioxygenic property.
Specific implementation mode
Embodiment 1
1）The preparation of alcohol dispersion liquid
Cyanuric acid zinc is taken, is added in 17 times of absolute ethyl alcohols of its weight, stirs evenly, 2- mercapto benzimidazoles are added, is increased
Temperature is 60 DEG C, and insulated and stirred 40 minutes obtains alcohol dispersion liquid；
2）The preparation of amide solution
Polyamide wax micropowder is taken, is added in the dimethylformamide of 5 times of its weight, is sent in 140 DEG C of oil bath, is stirred
230 minutes, discharging mixed with above-mentioned alcohol dispersion liquid, stirs evenly, obtain amide solution；
3）Graphite acrylamide dispersion liquid
Graphene is taken, is added in above-mentioned amide solution, bis-phenol a diglycidyl ethers are added, ultrasound 10 minutes obtains graphene acyl
Amine dispersion liquid.
Embodiment 2
1）The preparation of alcohol dispersion liquid
Cyanuric acid zinc is taken, is added in 10 times of absolute ethyl alcohols of its weight, stirs evenly, 2- mercapto benzimidazoles are added, is increased
Temperature is 55 DEG C, and insulated and stirred 30 minutes obtains alcohol dispersion liquid；
2）The preparation of amide solution
Polyamide wax micropowder is taken, is added in the dimethylformamide of 3 times of its weight, is sent in 130 DEG C of oil bath, stirring 20
Minute, discharging mixes with above-mentioned alcohol dispersion liquid, stirs evenly, obtain amide solution；
3）Graphite acrylamide dispersion liquid
Graphene is taken, is added in above-mentioned amide solution, bis-phenol a diglycidyl ethers are added, ultrasound 5 minutes obtains graphene acyl
Amine dispersion liquid.
Embodiment 3
Graphite acrylamide dispersion liquid obtained in embodiment 1 is applied to and is prepared in anti-oxidant Polypyrrole Conducting Materials.
The specific method is as follows：
1）The preparation of anti-oxidant modified pyrrole monomer
It counts in parts by weight, weighs each raw material：Dialkyl group to 4 parts of biphenol, 120 parts of pyrroles, 5 parts of boric acid, 4 parts of pentaerythrite,
54 parts of toluene.
The 70% of above-mentioned toluene by weight is taken, dialkyl group is added to biphenol, is sent in 50 DEG C of water bath with thermostatic control, pyrrole is added
It coughs up, insulated and stirred 2 hours, discharging cooling obtains pyrroles's dispersion liquid；
Boric acid is taken, is added in remaining toluene, stirs evenly, be sent in reaction kettle, is passed through nitrogen, pentaerythrite is added,
It is 60 DEG C to increase temperature, insulated and stirred 40 minutes, and discharging cooling obtains ester raw material；
Above-mentioned ester raw material is taken, is added in pyrroles's dispersion liquid, stirs evenly, toluene is distilled off to get described in ultrasound 20 minutes
Anti-oxidant modified pyrrole monomer.
2）The preparation of anti-oxidant Polypyrrole Conducting Materials
Take step 1）200 parts of anti-oxidant modified pyrrole monomer obtained, is added to graphite acrylamide dispersion liquid made from embodiment 1
In, it stirs evenly, is sent in reaction kettle, be passed through nitrogen, it is 70 DEG C to adjust temperature of reaction kettle, and it is different that initiator peroxidating two is added
Propyl benzene solution, insulated and stirred 5 hours, discharging cooling obtain anti-oxidant modified polypyrrole solution；It filters, filter cake is washed, room temperature is dry
It is dry to get the anti-oxidant Polypyrrole Conducting Materials.
Wherein, initiator cumyl peroxide solution is to be added to its weight for 7 parts by initiator cumyl peroxide
In 20 times of isopropanol, stirs evenly and be made.
Embodiment 4
Graphite acrylamide dispersion liquid obtained in embodiment 2 is applied to and is prepared in anti-oxidant Polypyrrole Conducting Materials.
1）The preparation of anti-oxidant modified pyrrole monomer
It counts in parts by weight, weighs each raw material：Dialkyl group to 3 parts of biphenol, 100 parts of pyrroles, 3 parts of boric acid, 3 parts of pentaerythrite,
40 parts of toluene.
The 60% of above-mentioned toluene by weight is taken, dialkyl group is added to biphenol, is sent in 40 DEG C of water bath with thermostatic control, pyrrole is added
It coughs up, insulated and stirred 1 hour, discharging cooling obtains pyrroles's dispersion liquid；
Boric acid is taken, is added in remaining toluene, stirs evenly, be sent in reaction kettle, is passed through nitrogen, pentaerythrite is added,
It is 55 DEG C to increase temperature, insulated and stirred 30 minutes, and discharging cooling obtains ester raw material；
Above-mentioned ester raw material is taken, is added in pyrroles's dispersion liquid, stirs evenly, toluene is distilled off to get described in ultrasound 10 minutes
Anti-oxidant modified pyrrole monomer.
2）The preparation of anti-oxidant Polypyrrole Conducting Materials
Take step 1）140 parts of anti-oxidant modified pyrrole monomer obtained, is added to graphite acrylamide dispersion liquid made from embodiment 2
In, it stirs evenly, is sent in reaction kettle, be passed through nitrogen, it is 65 DEG C to adjust temperature of reaction kettle, and it is different that initiator peroxidating two is added
Propyl benzene solution, insulated and stirred 4 hours, discharging cooling obtain anti-oxidant modified polypyrrole solution；It filters, filter cake is washed, room temperature is dry
It is dry to get the anti-oxidant Polypyrrole Conducting Materials.
Wherein, initiator cumyl peroxide solution is to be added to its weight for 5 parts by initiator cumyl peroxide
It in 18 times of isopropanol, stirs evenly, obtains initiator solution；
In the embodiment of the present invention 1 and 2, amide solution is prepared by raw material of 2- mercaptos benzimidazoles, stone is then disperseed with this
Black alkene improves the reactivity of graphene surface, which is participated in the polymerisation of anti-oxidant monomer, to
The anti-oxidant Polypyrrole Conducting Materials that inoxidizability is strong, mechanical stability is high are arrived.
Specific performance test is as follows：
The tensile strength 130.7Mpa of the anti-oxidant Polypyrrole Conducting Materials of the embodiment of the present invention 3 is heat-treated 200 points at 70 DEG C
Clock, tensile strength reduced rate are 0.31%；
The tensile strength 136.3Mpa of the anti-oxidant Polypyrrole Conducting Materials of the embodiment of the present invention 4 is heat-treated 200 points at 70 DEG C
Clock, tensile strength reduced rate are 0.27%.
Claims (6)
1. a kind of graphite acrylamide dispersion liquid, it is characterised in that：The graphite acrylamide dispersion liquid is made by following steps：
1）The preparation of alcohol dispersion liquid
Cyanuric acid zinc is taken, is added in 10-17 times of absolute ethyl alcohol of its weight, stirs evenly, 2- mercapto benzimidazoles are added, is risen
For high-temperature to 55-60 DEG C, insulated and stirred 30-40 minutes obtains alcohol dispersion liquid；
2）The preparation of amide solution
Polyamide wax micropowder is taken, is added in the dimethylformamide of 3-5 times of its weight, is sent in 130-140 DEG C of oil bath,
Stirring 20-30 minutes, discharging, mixes with above-mentioned alcohol dispersion liquid, stirs evenly, obtain amide solution；
3）Graphite acrylamide dispersion liquid
Graphene is taken, is added in above-mentioned amide solution, bis-phenol a diglycidyl ethers are added, it is 5-10 minutes ultrasonic, obtain graphene
Amide dispersion liquid.
2. a kind of graphite acrylamide dispersion liquid according to claim 1, it is characterised in that：
It counts in parts by weight, each raw material is：1-2 parts of cyanuric acid zinc, 0.7-1 parts of 2- mercapto benzimidazoles, polyamide wax micropowder
3-4 parts, 10-13 parts of graphene, 0.1-0.3 parts of bis-phenol a diglycidyl ethers.
3. a kind of application of graphite acrylamide dispersion liquid as claimed in claim 1 or 2 in anti-oxidant Polypyrrole Conducting Materials,
It is characterized in that：Anti-oxidant modified pyrrole monomer is taken, is added in claim 1 in gained graphite acrylamide dispersion liquid, stirs evenly,
It is sent in reaction kettle, is passed through nitrogen, it is 65-70 DEG C to adjust temperature of reaction kettle, and initiator solution is added, and insulated and stirred 4-5 is small
When, discharging cooling obtains anti-oxidant modified polypyrrole solution；Anti-oxidant modified polypyrrole solution is filtered, filter cake is washed, room temperature
It is dry, anti-oxidant Polypyrrole Conducting Materials are made.
4. application of a kind of graphite acrylamide dispersion liquid in anti-oxidant Polypyrrole Conducting Materials according to claim 3,
It is characterized in that：Count in parts by weight, described anti-oxidant modified pyrrole monomer 140-200 parts, initiator solution be by 5-7 parts cause
Agent cumyl peroxide is added to stirred evenly in the isopropanol of 18-20 times of its weight after be made.
5. according to a kind of application of the graphite acrylamide dispersion liquid of claim 3 or 4 in anti-oxidant Polypyrrole Conducting Materials,
It is characterized in that：The anti-oxidant modified pyrrole monomer, is made by following steps：
1）The 60-70% of toluene by weight is taken, dialkyl group is added to biphenol, is sent in 40-50 DEG C of water bath with thermostatic control, pyrrole is added
It coughs up, insulated and stirred 1-2 hours, discharging cooling obtains pyrroles's dispersion liquid；
2）Boric acid is taken, is added in remaining toluene, stirs evenly, be sent in reaction kettle, is passed through nitrogen, Ji Wusi is added
Alcohol increases temperature to 55-60 DEG C, and insulated and stirred 30-40 minutes, discharging cooling obtains ester raw material；
3）Above-mentioned ester raw material is taken, is added in pyrroles's dispersion liquid, stirs evenly, it is 10-20 minutes ultrasonic, toluene is distilled off, i.e.,
Obtain the anti-oxidant modified pyrrole monomer.
6. application of a kind of graphite acrylamide dispersion liquid in anti-oxidant Polypyrrole Conducting Materials according to claim 5,
It is characterized in that：It counts in parts by weight, dialkyl group is to 3-4 parts of biphenol, 100-120 parts of pyrroles, 3-5 parts of boric acid, pentaerythrite 3-4
Part, 40-54 parts of toluene.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109932849A (en) * | 2018-11-08 | 2019-06-25 | 揭阳市宏光镀膜玻璃有限公司 | A kind of novel electrochromic glass |
| CN111334133A (en) * | 2020-04-02 | 2020-06-26 | 汉中木头人科技信息咨询有限公司 | Graphene antistatic coating and preparation method thereof |
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| CN106128799A (en) * | 2016-07-15 | 2016-11-16 | 武汉工程大学 | A kind of preparation method based on Graphene/polypyrrole nanotube composite film ultracapacitor |
| KR20170064371A (en) * | 2015-12-01 | 2017-06-09 | 전남대학교산학협력단 | Graphene-carbon nanofiber complex and method for preparing the same |
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2018
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Patent Citations (4)
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|---|---|---|---|---|
| CN102627768A (en) * | 2012-04-10 | 2012-08-08 | 上海交通大学 | Preparation method of grapheme/polypyrrole nanocomposite material for super capacitor electrode |
| CN103602065A (en) * | 2013-11-25 | 2014-02-26 | 中国科学院山西煤炭化学研究所 | Preparation method of reduced graphene and polyimide nano composite material |
| KR20170064371A (en) * | 2015-12-01 | 2017-06-09 | 전남대학교산학협력단 | Graphene-carbon nanofiber complex and method for preparing the same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109932849A (en) * | 2018-11-08 | 2019-06-25 | 揭阳市宏光镀膜玻璃有限公司 | A kind of novel electrochromic glass |
| CN111334133A (en) * | 2020-04-02 | 2020-06-26 | 汉中木头人科技信息咨询有限公司 | Graphene antistatic coating and preparation method thereof |
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