CN108395533A - A kind of anti-oxidant Polypyrrole Conducting Materials - Google Patents
A kind of anti-oxidant Polypyrrole Conducting Materials Download PDFInfo
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- CN108395533A CN108395533A CN201810353019.2A CN201810353019A CN108395533A CN 108395533 A CN108395533 A CN 108395533A CN 201810353019 A CN201810353019 A CN 201810353019A CN 108395533 A CN108395533 A CN 108395533A
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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
- C08K9/04—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
- 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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Abstract
The invention discloses a kind of anti-oxidant Polypyrrole Conducting Materials, it is made of the raw material of following weight parts：2 0.7 1 parts of mercapto benzimidazoles, 140 200 parts of anti-oxidant modified pyrrole monomer, 57 parts of initiator, 0.1 0.3 parts of bis-phenol a diglycidyl ethers, 34 parts of polyamide wax micropowder, 10 13 parts of graphene, 12 parts of cyanuric acid zinc.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 composite material that inoxidizability is strong, mechanical stability is high.
Description
Technical field
The invention belongs to Material Fields, and in particular to a kind of anti-oxidant Polypyrrole Conducting Materials.
Background technology
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 anti-oxidant polypyrrole conduction materials
Material.
To achieve the above object, the present invention uses following technical scheme：
A kind of anti-oxidant Polypyrrole Conducting Materials, it is made of the raw material of following weight parts：
0.7-1 parts of 2- mercapto benzimidazoles, modified pyrrole monomer 140-200 parts anti-oxidant, 5-7 parts of initiator, bis-phenol a bis- contract
0.1-0.3 parts of water glycerin ether, 3-4 parts of polyamide wax micropowder, 10-13 parts of graphene, 1-2 parts of cyanuric acid zinc.
What anti-oxidant modified pyrrole monomer of the present invention was made of the raw material of following weight parts：
Dialkyl group is 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.
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.
Initiator of the present invention is cumyl peroxide.
Anti-oxidant Polypyrrole Conducting Materials of the present invention, are made by following steps：
（1）Initiator is taken, is added in the isopropanol of 18-20 times of its weight, stirs evenly, obtain initiator solution；
（2）Cyanuric acid zinc is taken, is added in 10-17 times of absolute ethyl alcohol of its weight, stirs evenly, 2- mercapto benzene a pair of horses going side by side miaows are added
Azoles increases temperature to 55-60 DEG C, and insulated and stirred 30-40 minutes obtains alcohol dispersion liquid；
（3）Polyamide wax micropowder is taken, is added in the dimethylformamide of 3-5 times of its weight, 130-140 DEG C of oil bath is sent to
In, it stirs 20-30 minutes, discharging mixes with above-mentioned alcohol dispersion liquid, stirs evenly, obtain amide solution；
（4）Graphene is taken, is added in above-mentioned amide solution, bis-phenol a diglycidyl ethers are added, it is 5-10 minutes ultrasonic, obtain stone
Black acrylamide dispersion liquid；
（5）Anti-oxidant modified pyrrole monomer is taken, is added in above-mentioned graphite acrylamide dispersion liquid, stirs evenly, be sent to reaction
In kettle, it is passed through nitrogen, it is 65-70 DEG C to adjust temperature of reaction kettle, and above-mentioned initiator solution, insulated and stirred 4-5 hours, discharging is added
It is cooling, obtain anti-oxidant modified polypyrrole solution；
（6）Above-mentioned anti-oxidant modified polypyrrole solution is filtered, filter cake is washed, air drying is to get the anti-oxidant poly- pyrrole
Cough up conductive material.
Advantages of the present invention：
The anti-oxidant modified pyrrole monomer that the present invention is added uses dialkyl group to handle pyrrole monomer to biphenol, passes through boron first
The esterification of acid and pentaerythrite, it is effective to improve the reactivity of pyrrole monomer, while imparting the good antioxygen of monomer
Change performance；
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 composite material that inoxidizability is strong, mechanical stability is high.
Specific implementation mode
Embodiment 1
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
It counts in parts by weight, weighs each raw material：1 part of 2- mercaptos benzimidazole, step 1）Anti-oxidant modified pyrroles obtained is single
200 parts of body, 7 parts of initiator cumyl peroxide, 0.3 part of bis-phenol a diglycidyl ethers, 4 parts of polyamide wax micropowder, graphene
13 parts, 2 parts of cyanuric acid zinc.
Initiator is taken, is added in the isopropanol of 20 times of its weight, is stirred evenly, obtain initiator solution；
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；
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；
Graphene is taken, is added in above-mentioned amide solution, bis-phenol a diglycidyl ethers are added, ultrasound 10 minutes obtains graphite amide
Dispersion liquid；
Anti-oxidant modified pyrrole monomer is taken, is added in above-mentioned graphite acrylamide dispersion liquid, is stirred evenly, be sent to reaction kettle
In, it is passed through nitrogen, it is 70 DEG C to adjust temperature of reaction kettle, and above-mentioned initiator solution, insulated and stirred 5 hours is added, and discharging cooling obtains
Anti-oxidant modified polypyrrole solution；
Above-mentioned anti-oxidant modified polypyrrole solution is filtered, filter cake is washed, air drying is led to get the anti-oxidant polypyrrole
Electric material.
Embodiment 2
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
It counts in parts by weight, weighs each raw material：0.7 part of 2- mercaptos benzimidazole, draws 140 parts of anti-oxidant modified pyrrole monomer
Send out 5 parts of agent cumyl peroxide, 0.1 part of bis-phenol a diglycidyl ethers, 3 parts of polyamide wax micropowder, 10 parts of graphene, cyanogen urine
1 part of sour zinc.
Initiator is taken, is added in the isopropanol of 18 times of its weight, is stirred evenly, obtain initiator solution；
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；
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；
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；
Anti-oxidant modified pyrrole monomer is taken, is added in above-mentioned graphite acrylamide dispersion liquid, is stirred evenly, be sent to reaction kettle
In, it is passed through nitrogen, it is 65 DEG C to adjust temperature of reaction kettle, and above-mentioned initiator solution, insulated and stirred 4 hours is added, and discharging cooling obtains
Anti-oxidant modified polypyrrole solution；
Above-mentioned anti-oxidant modified polypyrrole solution is filtered, filter cake is washed, air drying is led to get the anti-oxidant polypyrrole
Electric material.
Performance test：
The tensile strength 130.7Mpa of the anti-oxidant Polypyrrole Conducting Materials of the embodiment of the present invention 1 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 2 is heat-treated 200 points at 70 DEG C
Clock, tensile strength reduced rate are 0.27%.
Claims (5)
1. a kind of anti-oxidant Polypyrrole Conducting Materials, it is characterised in that：It is made of the raw material of following weight parts：
0.7-1 parts of 2- mercapto benzimidazoles, modified pyrrole monomer 140-200 parts anti-oxidant, 5-7 parts of initiator, bis-phenol a bis- contract
0.1-0.3 parts of water glycerin ether, 3-4 parts of polyamide wax micropowder, 10-13 parts of graphene, 1-2 parts of cyanuric acid zinc.
2. a kind of anti-oxidant Polypyrrole Conducting Materials according to claim 1, it is characterised in that：The anti-oxidant modification
Pyrrole monomer is made of the raw material of following weight parts：
Dialkyl group is 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.
3. a kind of anti-oxidant Polypyrrole Conducting Materials according to claim 2, it is characterised in that：The anti-oxidant modification
Pyrrole monomer 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.
4. a kind of anti-oxidant Polypyrrole Conducting Materials according to claim 1, it is characterised in that：The initiator was
Aoxidize diisopropylbenzene (DIPB).
5. a kind of anti-oxidant Polypyrrole Conducting Materials according to claim 1, it is characterised in that：The anti-oxidant polypyrrole is led
Electric material is made by following steps：
1）Initiator is taken, is added in the isopropanol of 18-20 times of its weight, stirs evenly, obtain initiator solution；
2）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,
Temperature is increased to 55-60 DEG C, insulated and stirred 30-40 minutes obtains alcohol dispersion liquid；
3）Polyamide wax micropowder is taken, is added in the dimethylformamide of 3-5 times of its weight, 130-140 DEG C of oil bath is sent to
In, it stirs 20-30 minutes, discharging mixes with above-mentioned alcohol dispersion liquid, stirs evenly, obtain amide solution；
4）Graphene is taken, is added in above-mentioned amide solution, bis-phenol a diglycidyl ethers are added, it is 5-10 minutes ultrasonic, obtain graphite
Acrylamide dispersion liquid；
5）Anti-oxidant modified pyrrole monomer is taken, is added in above-mentioned graphite acrylamide dispersion liquid, is stirred evenly, be sent to reaction kettle
In, it is passed through nitrogen, it is 65-70 DEG C to adjust temperature of reaction kettle, and above-mentioned initiator solution is added, and insulated and stirred 4-5 hours discharges cold
But, anti-oxidant modified polypyrrole solution is obtained；
6）Above-mentioned anti-oxidant modified polypyrrole solution is filtered, filter cake is washed, air drying is to get the anti-oxidant polypyrrole
Conductive material.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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- 2018-04-19 CN CN201810353019.2A patent/CN108395533A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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Application publication date: 20180814 |