CN108707317A - A kind of polyimides enhancing conductive material and preparation method thereof - Google Patents

A kind of polyimides enhancing conductive material and preparation method thereof Download PDF

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CN108707317A
CN108707317A CN201810548963.3A CN201810548963A CN108707317A CN 108707317 A CN108707317 A CN 108707317A CN 201810548963 A CN201810548963 A CN 201810548963A CN 108707317 A CN108707317 A CN 108707317A
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added
taken
stirred
stirs evenly
polyimides
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查公祥
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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
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1075—Partially aromatic polyimides
    • C08G73/1082—Partially aromatic polyimides wholly aromatic in the tetracarboxylic moiety
    • 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
    • C08G61/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
    • C08G61/12—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule
    • C08G61/122—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides
    • C08G61/123—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides derived from five-membered heterocyclic compounds
    • C08G61/126—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides derived from five-membered heterocyclic compounds with a five-membered ring containing one sulfur atom in the ring
    • 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
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1003—Preparatory processes
    • C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L65/00—Compositions of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Compositions of derivatives of such polymers
    • 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
    • C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
    • C08G2261/10—Definition of the polymer structure
    • C08G2261/11—Homopolymers
    • 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
    • C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
    • C08G2261/10—Definition of the polymer structure
    • C08G2261/18—Definition of the polymer structure conjugated
    • 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
    • C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
    • C08G2261/30—Monomer units or repeat units incorporating structural elements in the main chain
    • C08G2261/32—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain
    • C08G2261/322—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain non-condensed
    • C08G2261/3223—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain non-condensed containing one or more sulfur atoms as the only heteroatom, e.g. thiophene
    • 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
    • C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
    • C08G2261/50—Physical properties
    • C08G2261/51—Charge transport
    • 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
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)

Abstract

The invention discloses a kind of polyimides to enhance conductive material, it is made of the raw material of following weight parts：Pyromellitic acid anhydride 10-17, tetramethylethylenediamine 10-13, dimethylformamide 20-30, thiophene 100-140, ferric chloride (FeCl36H2O) 5-6, hexadecyltrimethylammonium chloride 0.7-1, sorbitan monooleate 1-2, tricalcium silicate 2-3, oxidized polyethylene wax 4-5, calcium stearate 1-2, the present invention is compound by polyimides, can effectively improve the mechanical stability and weatherability of finished-product material.

Description

A kind of polyimides enhancing conductive material and preparation method thereof
Technical field
The invention belongs to conductive material fields, and in particular to a kind of polyimides enhancing conductive material and preparation method thereof.
Background technology
Conducting polymer polythiophene has good photoelectric properties, with the phases such as other conjugated polymers such as polyaniline, polypyrrole Than there is better chemical stability.Especially its derivative poly- (3,4-ethylene dioxythiophene) (PEDOT), which has, easily prepares, is electrochemical It is high to learn activity, good electric conductivity and environmental stability, after doping the advantages that opposite height ratio capacity, ultracapacitor and lithium from There is larger application in terms of sub-electrode material.But it is inevitably present skeleton knot also as other conducting polymers Structure destructible, capacity attenuation clearly the case where, therefore, how to improve its conductive stability, enhance the stabilization of skeleton structure Property is the emphasis studied at present.
Invention content
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of polyimides to enhance conductive material And preparation method thereof.
To achieve the above object, the present invention uses following technical scheme：
A kind of polyimides enhancing conductive material, which is characterized in that it is made of the raw material of following weight parts：
Pyromellitic acid anhydride 10-17, tetramethylethylenediamine 10-13, dimethylformamide 20-30, thiophene 100-140, Ferric chloride (FeCl36H2O) 5-6, hexadecyltrimethylammonium chloride 0.7-1, sorbitan monooleate 1-2, tricalcium silicate 2-3, oxidation Polyethylene wax 4-5, calcium stearate 1-2.
A kind of preparation method of polyimides enhancing conductive material, includes the following steps：
(1) oxidized polyethylene wax is taken, is added in dimethylformamide, is sent in 70-80 DEG C of water bath with thermostatic control, is kept the temperature Stirring 1-2 hours, discharging, mixes with calcium stearate, stirs to room temperature, obtains amide solution；
(2) tricalcium silicate is taken, is added in the absolute ethyl alcohol of 10-12 times of its weight, stirs evenly, tetramethyl second two is added Ethyl alcohol is distilled off insulated and stirred 20-30 minutes at 50-55 DEG C in amine, obtains diamines raw material；
(3) ferric chloride (FeCl36H2O) is taken, is added in the deionized water of 15-20 times of its weight, stirs evenly；
(4) thiophene, pyromellitic acid anhydride mixing are taken, it is 60-65 DEG C to increase temperature, and insulated and stirred 10-20 minutes obtains sour Change monomer；
(5) diamines raw material, acidification monomer mixing are taken, is added in above-mentioned amide solution, stirs evenly, be sent to reaction kettle In, it is passed through nitrogen, is stirred to react at 3-5 DEG C 4-5 hours, discharges, obtains polymer modification monomer solution；
(6) hexadecyltrimethylammonium chloride is taken, is added in the deionized water of 17-20 times of its weight, stirs evenly, obtain Aqueous dispersions；
(7) above-mentioned polymer modification monomer solution is taken, is added in above-mentioned aqueous dispersions, stirs evenly, is sent to reaction In kettle, it is passed through nitrogen, it is 13-15 DEG C to adjust temperature of reaction kettle, and above-mentioned ferric chloride (FeCl36H2O) is added, is stirred to react 10-12 hours, Sorbitan monooleate is added, stirs evenly, filters, precipitation is washed, it is 1-2 hours dry at 50-55 DEG C of vacuum, it is cooled to often Temperature to get.
Advantages of the present invention：
The present invention handles thiophene using pyromellitic acid anhydride, obtains acidification monomer, and silicon is handled using tetramethylethylenediamine Sour tricalcium obtains diamines raw material, and then acidification monomer is blended with diamines raw material, using amide solution as solvent, obtains polyimides Then modified monomer polymerize under aqueous oxidizing agent solution effect, obtains polyimide modified polythiophene, the present invention passes through polyamides Imines is compound, can effectively improve the mechanical stability and weatherability of finished-product material.
Specific implementation mode
Embodiment 1
A kind of polyimides enhancing conductive material, it is made of the raw material of following weight parts：
Pyromellitic acid anhydride 10, tetramethylethylenediamine 10, dimethylformamide 20, thiophene 100, ferric chloride (FeCl36H2O) 5, Hexadecyltrimethylammonium chloride 0.7, sorbitan monooleate 1, tricalcium silicate 2, oxidized polyethylene wax 4, calcium stearate 1.
A kind of preparation method of polyimides enhancing conductive material, includes the following steps：
(1) oxidized polyethylene wax is taken, is added in dimethylformamide, is sent in 70 DEG C of water bath with thermostatic control, heat preservation is stirred It mixes 1 hour, discharges, mixed with calcium stearate, stir to room temperature, obtain amide solution；
(2) tricalcium silicate is taken, is added in the absolute ethyl alcohol of 10 times of its weight, stirs evenly, tetramethylethylenediamine is added, Insulated and stirred 20 minutes, are distilled off ethyl alcohol at 50 DEG C, obtain diamines raw material；
(3) ferric chloride (FeCl36H2O) is taken, is added in the deionized water of 15 times of its weight, stirs evenly；
(4) thiophene, pyromellitic acid anhydride mixing are taken, it is 60 DEG C to increase temperature, insulated and stirred 10 minutes, must be acidified single Body；
(5) diamines raw material, acidification monomer mixing are taken, is added in above-mentioned amide solution, stirs evenly, be sent to reaction kettle In, it is passed through nitrogen, is stirred to react at 3 DEG C 4 hours, discharges, obtains polymer modification monomer solution；
(6) hexadecyltrimethylammonium chloride is taken, is added in the deionized water of 17- times of its weight, stirs evenly, obtain water Dispersion liquid；
(7) above-mentioned polymer modification monomer solution is taken, is added in above-mentioned aqueous dispersions, stirs evenly, is sent to reaction In kettle, it is passed through nitrogen, it is 13 DEG C to adjust temperature of reaction kettle, and above-mentioned ferric chloride (FeCl36H2O) aqueous solution is added, is stirred to react 10 hours, Sorbitan monooleate is added, stirs evenly, filters, precipitation is washed, it is 1 hour dry at 50 DEG C of vacuum, it is cooled to room temperature, i.e., .
Embodiment 2
A kind of polyimides enhancing conductive material, it is made of the raw material of following weight parts：
Pyromellitic acid anhydride 17, tetramethylethylenediamine 13, dimethylformamide 30, thiophene 140, ferric chloride (FeCl36H2O) 6, Hexadecyltrimethylammonium chloride 1, sorbitan monooleate 2, silicic acid three -3, oxidized polyethylene wax 5, calcium stearate 2.
A kind of preparation method of polyimides enhancing conductive material, includes the following steps：
(1) oxidized polyethylene wax is taken, is added in dimethylformamide, is sent in 80 DEG C of water bath with thermostatic control, heat preservation is stirred It mixes 2 hours, discharges, mixed with calcium stearate, stir to room temperature, obtain amide solution；
(2) tricalcium silicate is taken, is added in the absolute ethyl alcohol of 12 times of its weight, stirs evenly, tetramethylethylenediamine is added, Insulated and stirred 30 minutes, are distilled off ethyl alcohol at 55 DEG C, obtain diamines raw material；
(3) ferric chloride (FeCl36H2O) is taken, is added in the deionized water of 20 times of its weight, stirs evenly；
(4) thiophene, pyromellitic acid anhydride mixing are taken, it is 65 DEG C to increase temperature, insulated and stirred 20 minutes, must be acidified single Body；
(5) diamines raw material, acidification monomer mixing are taken, is added in above-mentioned amide solution, stirs evenly, be sent to reaction kettle In, it is passed through nitrogen, is stirred to react at 5 DEG C 5 hours, discharges, obtains polymer modification monomer solution；
(6) hexadecyltrimethylammonium chloride is taken, is added in the deionized water of 20 times of its weight, is stirred evenly, obtain water Dispersion liquid；
(7) above-mentioned polymer modification monomer solution is taken, is added in above-mentioned aqueous dispersions, stirs evenly, is sent to reaction In kettle, it is passed through nitrogen, it is 15 DEG C to adjust temperature of reaction kettle, and above-mentioned ferric chloride (FeCl36H2O) aqueous solution is added, is stirred to react 12 hours, Sorbitan monooleate is added, stirs evenly, filters, precipitation is washed, it is 2 hours dry at 55 DEG C of vacuum, it is cooled to room temperature, i.e., .
Performance test：
The finished product conductive material of embodiment 1：
Density is 0.96g/cm3, tensile strength 17.6Mpa, conductivity 0.33S/cm；
The finished product conductive material of embodiment 2：
Density is 0.87g/cm3, tensile strength 16.4Mpa, conductivity 0.35S/cm.

Claims (2)

1. a kind of polyimides enhances conductive material, which is characterized in that it is made of the raw material of following weight parts：
Pyromellitic acid anhydride 10-17, tetramethylethylenediamine 10-13, dimethylformamide 20-30, thiophene 100-140, six water Ferric trichloride 5-6, hexadecyltrimethylammonium chloride 0.7-1, sorbitan monooleate 1-2, tricalcium silicate 2-3, the poly- second of oxidation Alkene wax 4-5, calcium stearate 1-2.
2. a kind of preparation method of polyimides enhancing conductive material as described in claim 1, which is characterized in that including following step Suddenly：
(1) oxidized polyethylene wax is taken, is added in dimethylformamide, is sent in 70-80 DEG C of water bath with thermostatic control, insulated and stirred 1-2 hours, discharging was mixed with calcium stearate, is stirred to room temperature, is obtained amide solution；
(2) tricalcium silicate is taken, is added in the absolute ethyl alcohol of 10-12 times of its weight, stirs evenly, tetramethylethylenediamine is added, Insulated and stirred 20-30 minutes at 50-55 DEG C, ethyl alcohol is distilled off, obtains diamines raw material；
(3) ferric chloride (FeCl36H2O) is taken, is added in the deionized water of 15-20 times of its weight, stirs evenly；
(4) thiophene, pyromellitic acid anhydride mixing are taken, it is 60-65 DEG C to increase temperature, insulated and stirred 10-20 minutes, must be acidified single Body；
(5) diamines raw material, acidification monomer mixing are taken, is added in above-mentioned amide solution, stirs evenly, be sent in reaction kettle, It is passed through nitrogen, is stirred to react at 3-5 DEG C 4-5 hours, discharges, obtains polymer modification monomer solution；
(6) hexadecyltrimethylammonium chloride is taken, is added in the deionized water of 17-20 times of its weight, stirs evenly, obtain moisture Dispersion liquid；
(7) above-mentioned polymer modification monomer solution is taken, is added in above-mentioned aqueous dispersions, stirs evenly, be sent in reaction kettle, It is passed through nitrogen, it is 13-15 DEG C to adjust temperature of reaction kettle, and above-mentioned ferric chloride (FeCl36H2O) aqueous solution is added, it is small to be stirred to react 10-12 When, sorbitan monooleate is added, stirs evenly, filters, precipitation is washed, it is 1-2 hours dry at 50-55 DEG C of vacuum, it is cooling To room temperature to get.
CN201810548963.3A 2018-05-31 2018-05-31 A kind of polyimides enhancing conductive material and preparation method thereof Pending CN108707317A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103665409A (en) * 2013-11-12 2014-03-26 华南理工大学 Preparation method of conductive poly(3,4-ethylenedioxythiophene) composite film
CN107189083A (en) * 2017-06-21 2017-09-22 中国科学院广州能源研究所 Conducting polymer PEDOT organic dispersions system and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103665409A (en) * 2013-11-12 2014-03-26 华南理工大学 Preparation method of conductive poly(3,4-ethylenedioxythiophene) composite film
CN107189083A (en) * 2017-06-21 2017-09-22 中国科学院广州能源研究所 Conducting polymer PEDOT organic dispersions system and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王璐莹著: "《渗透汽化膜及其应用原理》", 31 December 2017, 中南大学出版社 *

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