CN107200844A - A kind of preparation method of polypyrrole magnetic conductance composite - Google Patents

A kind of preparation method of polypyrrole magnetic conductance composite Download PDF

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Publication number
CN107200844A
CN107200844A CN201710600592.4A CN201710600592A CN107200844A CN 107200844 A CN107200844 A CN 107200844A CN 201710600592 A CN201710600592 A CN 201710600592A CN 107200844 A CN107200844 A CN 107200844A
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composite
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张娟
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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
    • 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
    • C08K3/08—Metals
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • 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
    • 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
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • 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
    • C08K3/08—Metals
    • C08K2003/0856—Iron
    • 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
    • C08K2201/001—Conductive additives
    • 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
    • C08K2201/01—Magnetic additives
    • 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 preparation method of polypyrrole magnetic conductance composite, the composite of the present invention, in the polymerisation that CNT is participated in pyrrole monomer, dispersiveness of the CNT between polymer is effectively raised, reunion is effectively reduced, the stability_intensity of finished-product material is improved, the ferrocene added simultaneously is the hydroxylating iron of raw material, it can assign finished-product material good magnetic, expand the use scope of finished-product material, enhance its feature.

Description

A kind of preparation method of polypyrrole magnetic conductance composite
Technical field
The invention belongs to Material Field, and in particular to a kind of preparation method of polypyrrole magnetic conductance composite.
Background technology
Conducting polymer composite is with conducting function（Including semiconduction, metallic conductivity and superconductivity）, conductance Polymeric material of the rate in more than 10S/m.Macromolecule conducting material have small density, easy processing, it is corrosion-resistant, can large area into Film and electrical conductivity can be used as various metals material and nothing the features such as being adjusted in the range of more than ten orders of magnitude The substitute of machine conductive material, and turned into the indispensable class material of many advanced industrial departments and sophisticated technology field Material, by worldwide for many years widely studied, application of the conducting polymer in terms of new energy materialses has obtained very big Development, but also have a certain distance from actual large-scale application.It is bad not high with stability that this is primarily due to its processability Cause, seriously hinder the application of conductive polymer material industrially.Application especially in electric elements is, it is necessary to conduction material Material has good intensity, stability, otherwise, can not also be applied even if other performance is good again；
Application number：201610885928.1 disclose the electrically-conducting paint of a kind of, including 45-55 parts of polyaniline, polypyrrole 18-20 Part, 25-40 parts of carbon fiber, 7-12 parts of petroleum coke, 8-16 parts of carborundum, 20-25 parts of graphite, 6-9 parts of silver powder, 7-11 parts of nickel powder, 20-22 parts of single-walled carbon nanotube, 36-40 parts of tin oxide, 23-25 parts of zinc oxide, 22-24 parts of sodium pyrophosphate, triethyl group hexyl phosphorus Sour 4-8 parts, 16-20 parts of calgon, 7-9 parts of sodium carboxymethylcellulose, 11-15 parts of OPE, polyvinyl chloride tree 3-5 parts of fat, 12-16 parts of BMI, 20-25 parts of ethyl acrylate, 6-10 parts of NC Nitroncellulose and terpinol 13-16 Part, it is to be pre-mixed polypyrrole, single-walled carbon nanotube, then passes through point of calgon, sodium carboxymethylcellulose etc. It is scattered to act on improving compatibility of the inorganic fillers such as single-walled carbon nanotube between polymer；But this inorganic scattered mode is very Hardly possible improves the agglomeration of inorganic filler, is easily reduced the stability of finished product.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of polypyrrole magnetic conductance composite Preparation method.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of polypyrrole magnetic conductance composite, comprises the following steps：
（1）Ferrocene is taken, in the deionized water for being added to 40-50 times of its weight, trimethylolpropane is added, rise temperature is 50-60 DEG C, add to phenoxy benzoic acid, insulated and stirred 1-2 hours, filtering, precipitation is washed, air drying obtains carboxylated Iron；
（2）Pyrroles is taken, in the tetrahydrofuran for being added to 30-44 times of its weight, is stirred, 60-70 DEG C of thermostatted water is sent to In bath, metallic potassium is added, insulated and stirred 30-40 minutes, discharging cooling adds paratoluensulfonyl chloride, magnetic agitation 20-24 is small When, product is added in deionized water, stirred, 10-15 hours are stood, filtering washes precipitation, 60-70 DEG C of vacuum Lower dry 1-2 hours, obtain sulphonylpyrroles；
（3）Take in above-mentioned carboxylated iron, sulphonylpyrroles mixing, the tetrahydrofuran for being added to 2-3 times of compound weight, in 80- Insulated and stirred 1-2 hours at 85 DEG C, composite dispersion liquid is obtained；
（4）CNT is taken, in sulfuric acid solution that be added to 40-50 times of its weight, 96-98%, is incubated and stirs at 50-60 DEG C Mix 1-2 hours, filter, precipitation is washed, air drying, in the absolute ethyl alcohol for being added to 4-6 times of its weight, stirred, plus Enter aminopropyl triethoxysilane, it is ultrasonic 10-20 minutes, obtain silane carbon nano tube alcoholic solution；
（5）Above-mentioned silane carbon nano tube alcoholic solution, composite dispersion liquid mixing are taken, stirs, is sent in reactor, be passed through Nitrogen, regulation temperature of reaction kettle is 4-6 DEG C, and insulation reaction 4-5 hours discharges, and precipitation is washed in filtering, at 70-75 DEG C of vacuum Dry 20-23 hours, be cooled to normal temperature, produce the polypyrrole magnetic conductance composite.
Advantages of the present invention：
The present invention is carried out carboxylated, then using pyridine as raw material, carried out by paratoluensulfonyl chloride using ferrocene as raw material Sulfonylation, then by carboxylated iron and sulfonylation pyridine blended cross linking, obtains pyrrole monomer dispersion liquid, then with surface organic CNT mixing, carry out polymerisation, obtain polypyrrole magnetic conductance composite；
In the composite of the present invention, the polymerisation that CNT is participated in pyrrole monomer, carbon nanometer is effectively raised Dispersiveness of the pipe between polymer, effectively reduces reunion, improves the stability_intensity of finished-product material, while add two Luxuriant iron is the hydroxylating iron of raw material, can assign finished-product material good magnetic, expand the use scope of finished-product material, is strengthened Its feature.
Embodiment
Embodiment 1
A kind of preparation method of polypyrrole magnetic conductance composite, comprises the following steps：
（1）Ferrocene is taken, in the deionized water for being added to 50 times of its weight, trimethylolpropane is added, rise temperature is 50-60 DEG C, add to phenoxy benzoic acid, insulated and stirred 2 hours, filtering, precipitation is washed, air drying obtains carboxylated iron；
（2）Pyrroles is taken, in the tetrahydrofuran for being added to 30 times of its weight, is stirred, in the water bath with thermostatic control for being sent to 60 DEG C, plus Enter metallic potassium, insulated and stirred 30 minutes, discharging cooling adds paratoluensulfonyl chloride, product is added to by magnetic agitation 20 hours In deionized water, stir, stand 10 hours, precipitation is washed in filtering, is dried 1 hour at 60-70 DEG C of vacuum, is obtained sulphonyl Base pyrroles；
（3）Take in above-mentioned carboxylated iron, sulphonylpyrroles mixing, the tetrahydrofuran for being added to 2-3 times of compound weight, at 85 DEG C Lower insulated and stirred 1 hour, obtains composite dispersion liquid；
（4）CNT is taken, is added in 50 times of its weight, 98% sulfuric acid solution, insulated and stirred 2 hours, mistake at 60 DEG C Filter, precipitation is washed, air drying, in the absolute ethyl alcohol for being added to 4 times of its weight, is stirred, and adds the ethoxy of aminopropyl three Base silane, ultrasound 20 minutes, obtains silane carbon nano tube alcoholic solution；
（5）Above-mentioned silane carbon nano tube alcoholic solution, composite dispersion liquid mixing are taken, stirs, is sent in reactor, be passed through Nitrogen, regulation temperature of reaction kettle is 6 DEG C, and insulation reaction 4 hours discharges, and precipitation is washed in filtering, and 23 are dried at 75 DEG C of vacuum Hour, normal temperature is cooled to, the polypyrrole magnetic conductance composite is produced.

Claims (1)

1. a kind of preparation method of polypyrrole magnetic conductance composite, it is characterised in that comprise the following steps：
（1）Ferrocene is taken, in the deionized water for being added to 40-50 times of its weight, trimethylolpropane is added, rise temperature is 50-60 DEG C, add to phenoxy benzoic acid, insulated and stirred 1-2 hours, filtering, precipitation is washed, air drying obtains carboxylated Iron；
（2）Pyrroles is taken, in the tetrahydrofuran for being added to 30-44 times of its weight, is stirred, 60-70 DEG C of thermostatted water is sent to In bath, metallic potassium is added, insulated and stirred 30-40 minutes, discharging cooling adds paratoluensulfonyl chloride, magnetic agitation 20-24 is small When, product is added in deionized water, stirred, 10-15 hours are stood, filtering washes precipitation, 60-70 DEG C of vacuum Lower dry 1-2 hours, obtain sulphonylpyrroles；
（3）Take in above-mentioned carboxylated iron, sulphonylpyrroles mixing, the tetrahydrofuran for being added to 2-3 times of compound weight, in 80- Insulated and stirred 1-2 hours at 85 DEG C, composite dispersion liquid is obtained；
（4）CNT is taken, in sulfuric acid solution that be added to 40-50 times of its weight, 96-98%, is incubated and stirs at 50-60 DEG C Mix 1-2 hours, filter, precipitation is washed, air drying, in the absolute ethyl alcohol for being added to 4-6 times of its weight, stirred, plus Enter aminopropyl triethoxysilane, it is ultrasonic 10-20 minutes, obtain silane carbon nano tube alcoholic solution；
（5）Above-mentioned silane carbon nano tube alcoholic solution, composite dispersion liquid mixing are taken, stirs, is sent in reactor, be passed through Nitrogen, regulation temperature of reaction kettle is 4-6 DEG C, and insulation reaction 4-5 hours discharges, and precipitation is washed in filtering, at 70-75 DEG C of vacuum Dry 20-23 hours, be cooled to normal temperature, produce the polypyrrole magnetic conductance composite.
CN201710600592.4A 2017-07-21 2017-07-21 A kind of preparation method of polypyrrole magnetic conductance composite Pending CN107200844A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108047716A (en) * 2018-01-23 2018-05-18 宿州市微腾知识产权运营有限公司 A kind of preparation method of carbon nanotubes reinforcement Polypyrrole Conducting Materials
CN112142973A (en) * 2020-09-28 2020-12-29 浙江大学 Ferrocene-modified multi-walled carbon nanotube-polypyrrole nanotube wave-absorbing material and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104592514A (en) * 2015-01-07 2015-05-06 合肥师范学院 Preparation method of polypyrrole/carbon fiber composite electromagnetic wave absorbing material
CN105778089A (en) * 2016-03-18 2016-07-20 赵守彬 Inorganic particle modified magnetic composite material and preparation method thereof
CN106280288A (en) * 2016-08-31 2017-01-04 烟台南山学院 A kind of conductivity high molecule nanometer composite and preparation method thereof
CN106432721A (en) * 2016-09-30 2017-02-22 同济大学 Method for preparing carbon nano-tubes/polypyrrole nano-particles with performance of metamaterials

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104592514A (en) * 2015-01-07 2015-05-06 合肥师范学院 Preparation method of polypyrrole/carbon fiber composite electromagnetic wave absorbing material
CN105778089A (en) * 2016-03-18 2016-07-20 赵守彬 Inorganic particle modified magnetic composite material and preparation method thereof
CN106280288A (en) * 2016-08-31 2017-01-04 烟台南山学院 A kind of conductivity high molecule nanometer composite and preparation method thereof
CN106432721A (en) * 2016-09-30 2017-02-22 同济大学 Method for preparing carbon nano-tubes/polypyrrole nano-particles with performance of metamaterials

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108047716A (en) * 2018-01-23 2018-05-18 宿州市微腾知识产权运营有限公司 A kind of preparation method of carbon nanotubes reinforcement Polypyrrole Conducting Materials
CN112142973A (en) * 2020-09-28 2020-12-29 浙江大学 Ferrocene-modified multi-walled carbon nanotube-polypyrrole nanotube wave-absorbing material and preparation method thereof

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Application publication date: 20170926