CN108342080A - A kind of intercalation polypyrrole nano material and preparation method thereof - Google Patents
A kind of intercalation polypyrrole nano material and preparation method thereof Download PDFInfo
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- CN108342080A CN108342080A CN201810317783.4A CN201810317783A CN108342080A CN 108342080 A CN108342080 A CN 108342080A CN 201810317783 A CN201810317783 A CN 201810317783A CN 108342080 A CN108342080 A CN 108342080A
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- intercalation
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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
- C08L79/00—Compositions 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 C08L61/00 - C08L77/00
- C08L79/04—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
- 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
- C08K5/00—Use of organic ingredients
- C08K5/02—Halogenated hydrocarbons
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1535—Five-membered rings
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a kind of intercalation polypyrrole nano materials and preparation method thereof, it is made of the raw material of following weight parts：Pyrroles 60 70, intercalation lotion 10 14, initiator 1.7 2, isocyanuric acid three-glycidyl ester 12, alkenyl succinic anhydride 0.7 1, vanadium acetylacetonate 0.1 0.2, nano silicon dioxide 7.5 9.The present invention ensure that conductive stability by intercalation, provides more attachment points for nano silicon dioxide, reduces the reunion of nano silicon dioxide.
Description
Technical field
The invention belongs to Material Fields, and in particular to a kind of intercalation polypyrrole nano material and preparation method thereof.
Background technology
Polypyrrole is common black, insoluble, molten, conductive polymer, polypyrrole are not aoxidized by pyrrole monomer usually poly-
Conjunction obtains, and electrochemical anodic oxidation pyrroles is also the effective means for preparing polypyrrole；Polypyrrole can be used for biology, ion detection,
The electrode material of the modified electrode of electrochemical capacitance and antistatic material and photoelectrochemical cell, accumulator.Further, it is also possible to as electricity
Magnetic shielding material and gas separation membrane material, for electrolytic capacitor, electro-catalysis, conducting polymer composite material etc., application range
It is very wide, the concern of people has been constantly subjected to since being found；However the stability and poor mechanical property of electric polypyrrole material,
In order to improve the performance of polypyrrole, a large number of researchers by sight concentrate on polypyrrole and other materials it is compound on, closely
The compound extensive expansion of the carbon materials such as Nian Laiyu carbon nanotubes, result of study shows can be significantly with the compound of carbon nanotube
Improve the performance of ultracapacitor, however the poor compatibility of polypyrrole and carbon nanotube, it is compound after material conductive stability compared with
It is low, therefore how to improve the mechanical stability of compound polypyrrole material and the research of its electric conductivity will not be reduced and just seem have very much
It is necessary.
Invention content
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of intercalation polypyrrole nano material and
Preparation method.
To achieve the above object, the present invention uses following technical scheme：
A kind of intercalation polypyrrole nano material, it is made of the raw material of following weight parts：
Pyrroles 60-70, intercalation lotion 10-14, initiator 1.7-2, isocyanuric acid three-glycidyl ester 1-2, alkenyl succinic anhydride
0.7-1, vanadium acetylacetonate 0.1-0.2, nano silicon dioxide 7.5-9.
A kind of intercalation polypyrrole nano material, the initiator are ammonium persulfate.
A kind of intercalation polypyrrole nano material, the intercalation lotion are made of the raw material of following weight parts
's：
Ethyl cellulose 10-14, bromohexane 1-2, tetrahydrofurfuryl alcohol 0.1-0.3, trimethyl hydroxyethylammonium ethylenediamine 1-2；
The preparation method of the intercalation lotion, includes the following steps：
（1）Ethyl cellulose is taken, is added in the deionized water of 14-20 times of its weight, stirs evenly, obtain fiber dispersion；
（2）Take trimethyl hydroxyethylammonium ethylenediamine, be added in the absolute ethyl alcohol of 3-5 times of its weight, stir evenly, be added bromine oneself
Alkane, it is 50-60 DEG C to increase temperature, and insulated and stirred 10-20 minutes obtains bromination alcoholic solution；
（3）Above-mentioned fiber dispersion, the mixing of bromination alcoholic solution are taken, is stirred evenly, tetrahydrofurfuryl alcohol is added, it is 4-10 minutes ultrasonic, i.e.,
Obtain the intercalation lotion.
A kind of preparation method of the intercalation polypyrrole nano material, includes the following steps：
（1）Initiator is taken, is added in the deionized water of 15-20 times of its weight, stirs evenly；
（2）Alkenyl succinic anhydride, pyrroles's mixing are taken, is added in the deionized water of 30-40 times of mixture weight, levulinic is added
Ketone vanadium, stirs evenly, and is sent in reaction kettle, is passed through nitrogen, and above-mentioned intercalation lotion is added, and adjusting temperature of reaction kettle is 70-75
DEG C, above-mentioned initiator solution, insulated and stirred 4-5 hours is added dropwise, discharging obtains intercalation polypyrrole solution；
（3）Take nano silicon dioxide, isocyanuric acid three-glycidyl ester mixing, be added to 30-45 times of mixture weight go from
It is 10-20 minutes ultrasonic in sub- water, obtain nano dispersion fluid；
（4）Above-mentioned intercalation polypyrrole solution, nano dispersion fluid mixing are taken, stirs evenly, filters, precipitation is washed, vacuum 50-60
It is 1-2 hours dry at DEG C, it is cooled to room temperature to get the intercalation polypyrrole nano material.
Advantages of the present invention：
The present invention is realized by trimethyl hydroxyethylammonium ethylenediamine peptizaiton and is blended with bromohexane using ethyl cellulose as raw material
Dispersion, using pyrroles as monomer, using alkenyl succinic anhydride as dopant, gathers then as intercalation solution under initiator effect
It closes, realizes bromination intercalation in the course of the polymerization process, be then blended with nano silicon dioxide, improve nano silicon dioxide and polypyrrole
Between compatibility, to improve the stability_intensity of finished product, the present invention ensure that conductive stability by intercalation, be nanometer
Silica provides more attachment points, reduces the reunion of nano silicon dioxide, to improve finished product nano material
Mechanical stability intensity.
Specific implementation mode
Embodiment 1
A kind of intercalation polypyrrole nano material, it is made of the raw material of following weight parts：
Pyrroles 70, intercalation lotion 14, initiator 2, isocyanuric acid three-glycidyl ester 2, alkenyl succinic anhydride 1, vanadium acetylacetonate
0.2, nano silicon dioxide 9.
A kind of intercalation polypyrrole nano material, the initiator are ammonium persulfate.
A kind of intercalation polypyrrole nano material, the intercalation lotion are made of the raw material of following weight parts
's：
Ethyl cellulose 14, bromohexane 2, tetrahydrofurfuryl alcohol 0.3, trimethyl hydroxyethylammonium ethylenediamine 2；
The preparation method of the intercalation lotion, includes the following steps：
（1）Ethyl cellulose is taken, is added in the deionized water of 20 times of its weight, is stirred evenly, obtain fiber dispersion；
（2）Trimethyl hydroxyethylammonium ethylenediamine is taken, is added in the absolute ethyl alcohol of 5 times of its weight, stirs evenly, bromohexane is added,
It is 60 DEG C to increase temperature, and insulated and stirred 20 minutes obtains bromination alcoholic solution；
（3）Take above-mentioned fiber dispersion, bromination alcoholic solution mixing, stir evenly, be added tetrahydrofurfuryl alcohol, ultrasound 10 minutes to get
The intercalation lotion.
A kind of preparation method of the intercalation polypyrrole nano material, includes the following steps：
（1）Initiator is taken, is added in the deionized water of 20 times of its weight, stirs evenly；
（2）Alkenyl succinic anhydride, pyrroles's mixing are taken, is added in the deionized water of 40 times of mixture weight, acetylacetone,2,4-pentanedione is added
Vanadium stirs evenly, and is sent in reaction kettle, is passed through nitrogen, and above-mentioned intercalation lotion is added, and it is 75 DEG C to adjust temperature of reaction kettle, drop
In addition stating initiator solution, insulated and stirred 5 hours, discharging obtains intercalation polypyrrole solution；
（3）Nano silicon dioxide, isocyanuric acid three-glycidyl ester mixing are taken, the deionized water of 45 times of mixture weight is added to
In, ultrasound 20 minutes obtains nano dispersion fluid；
（4）Above-mentioned intercalation polypyrrole solution, nano dispersion fluid mixing are taken, stirs evenly, filters, precipitation is washed, 60 DEG C of vacuum
Lower drying 2 hours is cooled to room temperature to get the intercalation polypyrrole nano material.
Embodiment 2
A kind of intercalation polypyrrole nano material, it is made of the raw material of following weight parts：
Pyrroles 60, intercalation lotion 10, initiator 1.7, isocyanuric acid three-glycidyl ester 1, alkenyl succinic anhydride 0.7, levulinic
Ketone vanadium 0.1, nano silicon dioxide 7.5.
A kind of intercalation polypyrrole nano material, the initiator are ammonium persulfate.
A kind of intercalation polypyrrole nano material, the intercalation lotion are made of the raw material of following weight parts
's：
Ethyl cellulose 10, bromohexane 1, tetrahydrofurfuryl alcohol 0.1, trimethyl hydroxyethylammonium ethylenediamine 1；
The preparation method of the intercalation lotion, includes the following steps：
（1）Ethyl cellulose is taken, is added in the deionized water of 14 times of its weight, is stirred evenly, obtain fiber dispersion；
（2）Trimethyl hydroxyethylammonium ethylenediamine is taken, is added in the absolute ethyl alcohol of 3 times of its weight, stirs evenly, bromohexane is added,
It is 50 DEG C to increase temperature, and insulated and stirred 10 minutes obtains bromination alcoholic solution；
（3）Above-mentioned fiber dispersion, the mixing of bromination alcoholic solution are taken, is stirred evenly, tetrahydrofurfuryl alcohol is added, ultrasonic 4 minutes to get institute
State intercalation lotion.
A kind of preparation method of the intercalation polypyrrole nano material, includes the following steps：
（1）Initiator is taken, is added in the deionized water of 15 times of its weight, stirs evenly；
（2）Alkenyl succinic anhydride, pyrroles's mixing are taken, is added in the deionized water of 30 times of mixture weight, acetylacetone,2,4-pentanedione is added
Vanadium stirs evenly, and is sent in reaction kettle, is passed through nitrogen, and above-mentioned intercalation lotion is added, and it is 70 DEG C to adjust temperature of reaction kettle, drop
In addition stating initiator solution, insulated and stirred 4 hours, discharging obtains intercalation polypyrrole solution；
（3）Take nano silicon dioxide, isocyanuric acid three-glycidyl ester mixing, be added to 30-45 times of mixture weight go from
In sub- water, ultrasound 10 minutes obtains nano dispersion fluid；
（4）Above-mentioned intercalation polypyrrole solution, nano dispersion fluid mixing are taken, stirs evenly, filters, precipitation is washed, 50 DEG C of vacuum
Lower drying 1 hour is cooled to room temperature to get the intercalation polypyrrole nano material.
Performance test：
The intercalation polypyrrole nano material of the embodiment of the present invention 1：
Charge-discharge test is carried out, specific capacitance under the conditions of 0.2A/g charge and discharge is 146.3F/g；Tensile strength is
173.8MPa；
The intercalation polypyrrole nano material of the embodiment of the present invention 2：
Charge-discharge test is carried out, specific capacitance under the conditions of 0.2A/g charge and discharge is 141.5F/g；Tensile strength 162.9MPa；
Commercially available pure polypyrrole：
Charge-discharge test is carried out, specific capacitance under the conditions of 0.2A/g charge and discharge is 100-110F/g；Tensile strength is 80-
100MPa；As can be seen that the material of the present invention has better conductive stability and mechanical property, comprehensive performance superior.
Claims (4)
1. a kind of intercalation polypyrrole nano material, which is characterized in that it is made of the raw material of following weight parts：
Pyrroles 60-70, intercalation lotion 10-14, initiator 1.7-2, isocyanuric acid three-glycidyl ester 1-2, alkenyl succinic anhydride
0.7-1, vanadium acetylacetonate 0.1-0.2, nano silicon dioxide 7.5-9.
2. a kind of intercalation polypyrrole nano material according to claim 1, which is characterized in that the initiator is over cure
Sour ammonium.
3. a kind of intercalation polypyrrole nano material according to claim 1, which is characterized in that the intercalation lotion be by
The raw material composition of following weight parts：
Ethyl cellulose 10-14, bromohexane 1-2, tetrahydrofurfuryl alcohol 0.1-0.3, trimethyl hydroxyethylammonium ethylenediamine 1-2；
The preparation method of the intercalation lotion, includes the following steps：
（1）Ethyl cellulose is taken, is added in the deionized water of 14-20 times of its weight, stirs evenly, obtain fiber dispersion；
（2）Take trimethyl hydroxyethylammonium ethylenediamine, be added in the absolute ethyl alcohol of 3-5 times of its weight, stir evenly, be added bromine oneself
Alkane, it is 50-60 DEG C to increase temperature, and insulated and stirred 10-20 minutes obtains bromination alcoholic solution；
（3）Above-mentioned fiber dispersion, the mixing of bromination alcoholic solution are taken, is stirred evenly, tetrahydrofurfuryl alcohol is added, it is 4-10 minutes ultrasonic, i.e.,
Obtain the intercalation lotion.
4. a kind of preparation method of intercalation polypyrrole nano material as described in claim 1, which is characterized in that including following step
Suddenly：
（1）Initiator is taken, is added in the deionized water of 15-20 times of its weight, stirs evenly；
（2）Alkenyl succinic anhydride, pyrroles's mixing are taken, is added in the deionized water of 30-40 times of mixture weight, levulinic is added
Ketone vanadium, stirs evenly, and is sent in reaction kettle, is passed through nitrogen, and above-mentioned intercalation lotion is added, and adjusting temperature of reaction kettle is 70-75
DEG C, above-mentioned initiator solution, insulated and stirred 4-5 hours is added dropwise, discharging obtains intercalation polypyrrole solution；
（3）Take nano silicon dioxide, isocyanuric acid three-glycidyl ester mixing, be added to 30-45 times of mixture weight go from
It is 10-20 minutes ultrasonic in sub- water, obtain nano dispersion fluid；
（4）Above-mentioned intercalation polypyrrole solution, nano dispersion fluid mixing are taken, stirs evenly, filters, precipitation is washed, vacuum 50-60
It is 1-2 hours dry at DEG C, it is cooled to room temperature to get the intercalation polypyrrole nano material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109767858A (en) * | 2018-12-28 | 2019-05-17 | 朱雪梅 | A kind of polyalcohol intercalation conductive material and preparation method thereof |
| CN110655768A (en) * | 2017-12-06 | 2020-01-07 | 雷珊珊 | Polylactic acid fiber fused polypyrrole material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101120047A (en) * | 2004-12-02 | 2008-02-06 | 克里奥瓦克公司 | Intercalated layered silicates |
| CN106146886A (en) * | 2016-06-30 | 2016-11-23 | 常州第六元素材料科技股份有限公司 | A kind of composite of Graphene intercalation silicate and preparation method thereof |
| CN108410168A (en) * | 2018-03-08 | 2018-08-17 | 查公祥 | A kind of intercalation polypyrrole nano material and preparation method thereof |
-
2018
- 2018-04-10 CN CN201810317783.4A patent/CN108342080A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101120047A (en) * | 2004-12-02 | 2008-02-06 | 克里奥瓦克公司 | Intercalated layered silicates |
| CN106146886A (en) * | 2016-06-30 | 2016-11-23 | 常州第六元素材料科技股份有限公司 | A kind of composite of Graphene intercalation silicate and preparation method thereof |
| CN108410168A (en) * | 2018-03-08 | 2018-08-17 | 查公祥 | A kind of intercalation polypyrrole nano material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110655768A (en) * | 2017-12-06 | 2020-01-07 | 雷珊珊 | Polylactic acid fiber fused polypyrrole material and preparation method thereof |
| CN109767858A (en) * | 2018-12-28 | 2019-05-17 | 朱雪梅 | A kind of polyalcohol intercalation conductive material and preparation method thereof |
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