CN108485231A - A kind of epoxidation polyphenylene oxide conductive film and preparation method thereof - Google Patents

A kind of epoxidation polyphenylene oxide conductive film and preparation method thereof Download PDF

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CN108485231A
CN108485231A CN201810417792.0A CN201810417792A CN108485231A CN 108485231 A CN108485231 A CN 108485231A CN 201810417792 A CN201810417792 A CN 201810417792A CN 108485231 A CN108485231 A CN 108485231A
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polyphenylene oxide
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carbon nano
tube
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饶素芳
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Wuhu Tian Ke Biological Technology Co Ltd
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Wuhu Tian Ke Biological Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2371/00Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
    • C08J2371/08Polyethers derived from hydroxy compounds or from their metallic derivatives
    • C08J2371/10Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
    • C08J2371/12Polyphenylene oxides
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/327Aluminium phosphate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K2201/011Nanostructured additives
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • C08K3/041Carbon nanotubes
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/36Sulfur-, selenium-, or tellurium-containing compounds
    • C08K5/37Thiols
    • C08K5/378Thiols containing heterocyclic rings
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances

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  • Manufacturing & Machinery (AREA)
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Abstract

The invention discloses a kind of epoxidation polyphenylene oxide conductive films, it is made of the raw material of following weight parts:Ammonium hydroxide 17 20, the Sucrose acetoisobutyrate 12 of polyphenylene oxide 100 120, aluminium triphosphate 12, carbon nanotube 68, methacrylic acid 34, propylene oxide 24, alkanolamide 12,2 mercaptobenzimidazoles 0.4 1,10 12%, it is compatible that the present invention realizes effectively dispersion of the carbon nanotube between polyphenylene oxide, the thin film mechanics stability of the present invention is good, electric conductivity is strong, and comprehensive performance is superior.

Description

A kind of epoxidation polyphenylene oxide conductive film and preparation method thereof
Technical field
The invention belongs to conductive film fields, and in particular to a kind of epoxidation polyphenylene oxide conductive film and preparation method thereof.
Background technology
Conductive film is a kind of very important photoelectric material, it has the characteristics that low-resistance, is widely used in solar energy In the various photoelectric materials such as battery, electrode material, display, apply at present more for inorganic oxide film, translucency Good, resistivity is low, and chemical temperatures are good, but as inorganic filler, and the brittleness of film is larger, toughness is poor, synthesis temperature Higher, these all limit their further development, and therefore, market has gradually appeared macromolecule conducting material, including polyphenyl Amine, polypyridine etc., polyaniline is since its aerial stability is good, and raw material is easy to get, monomer is cheap, synthetic method is simple Just, conductivity is easy the advantages that adjusting and is widely used, such as electrode material, electrochromic material, anti-corrosion of metal material, electricity Magnetic shielding material, antistatic material, molecular device etc. are led however, due to the poor compatibility of inorganic raw material and high molecular polymer It is difficult that film forming, the mechanical property relative reduction of the single organic film obtained from is blended to cause composite material.
Invention content
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of epoxidation polyphenylene oxide conductive films And preparation method thereof.
To achieve the above object, the present invention uses following technical scheme:
A kind of epoxidation polyphenylene oxide conductive film, it is made of the raw material of following weight parts:
Polyphenylene oxide 100-120, aluminium triphosphate 1-2, carbon nanotube 6-8, methacrylic acid 3-4, propylene oxide 2-4, alkane Alkylolamides 1-2, the ammonium hydroxide 17-20 of 2-mercaptobenzimidazole 0.4-1,10-12%, Sucrose acetoisobutyrate 1-2.
A kind of preparation method of epoxidation polyphenylene oxide conductive film, includes the following steps:
(1) 2-mercaptobenzimidazole is taken, is added in the absolute ethyl alcohol of 10-12 times of its weight, stirs evenly, it is molten to obtain alcohol Liquid;
(2) carbon nanotube is taken, it is 3-5 hours ultrasonic in sulfuric acid solution that be added to 14-20 times of its weight, 96-98%, Precipitation is washed, mixes, be added in above-mentioned alcoholic solution with propylene oxide by filtering, insulated and stirred 10-20 points at 50-55 DEG C Ethyl alcohol is distilled off in clock, obtains activated carbon nano-tube;
(3) methacrylic acid is taken, is added in the chloroform of 20-30 times of its weight, stirs evenly, polyphenylene oxide, stirring is added 1-2 hours, chloroform is distilled off, obtains acidification polyphenylene oxide;
(4) aluminium triphosphate, alkanolamide mixing are taken, is added in the deionized water of 15-20 times of mixture weight, stirs Uniformly, amide solution is obtained;
(5) above-mentioned activated carbon nano-tube is taken, is added in amide solution, is stirred evenly, 65-70 DEG C of thermostatted water is sent to In bath, the ammonium hydroxide of 10-12%, insulated and stirred 3-5 hours is added, discharging cooling obtains modified carbon nano-tube;
(6) above-mentioned modified carbon nano-tube is taken, is mixed with above-mentioned acidification polyphenylene oxide, Sucrose acetoisobutyrate, stirring is added 30-40 minutes, precipitation was washed in filtering, and air drying obtains carbon nano-tube modification polyphenylene oxide;
(7) above-mentioned carbon nano-tube modification polyphenylene oxide is taken, is added in the dimethylformamide of 30-40 times of its weight, ultrasound It 1-2 hours, pours into culture dish, is put into vacuum drying chamber, be dried in vacuo 20-30 hours at 70-85 DEG C, after film molding, It is put into 95-105 DEG C of thermostatic drying chamber to handle 1-2 hours, takes off film, film water is washed, air drying is to get the epoxidation polyphenyl Ether conductive film.
Advantages of the present invention:
The present invention handles polyphenylene oxide using methacrylic acid, then propylene oxide is used to handle carbon nanotube, by what is obtained Activated carbon nano-tube is distributed in alkanolamide aqueous solution, and using ammonium hydroxide as catalyst, catalysis epoxy is reacted with amide, Zhi Houzai With acidification polyphenylether blending, realize that effectively dispersion of the carbon nanotube between polyphenylene oxide is compatible, thin film mechanics of the invention are stablized Property is good, and electric conductivity is strong, and comprehensive performance is superior.
Specific implementation mode
Embodiment 1
A kind of epoxidation polyphenylene oxide conductive film, it is made of the raw material of following weight parts:
Polyphenylene oxide 100, aluminium triphosphate 1, carbon nanotube 6, methacrylic acid 3, propylene oxide 2, alkanolamide 1,2- mercaptos Ammonium hydroxide 17, the Sucrose acetoisobutyrate 1 of base benzimidazole 0.4,10%.
A kind of preparation method of epoxidation polyphenylene oxide conductive film, includes the following steps:
(1) 2-mercaptobenzimidazole is taken, is added in the absolute ethyl alcohol of 10 times of its weight, is stirred evenly, obtain alcoholic solution;
(2) carbon nanotube is taken, is added in 14 times of its weight, 96% sulfuric acid solution, ultrasound 3 hours, filtering will sink It forms sediment and washes, mix, be added in above-mentioned alcoholic solution with propylene oxide, insulated and stirred 10 minutes, are distilled off ethyl alcohol at 50 DEG C, Obtain activated carbon nano-tube;
(3) methacrylic acid is taken, is added in the chloroform of 20 times of its weight, stirs evenly, polyphenylene oxide is added, stirring 1 is small When, chloroform is distilled off, obtains acidification polyphenylene oxide;
(4) aluminium triphosphate, alkanolamide mixing are taken, is added in the deionized water of 15 times of mixture weight, stirring is equal It is even, obtain amide solution;
(5) above-mentioned activated carbon nano-tube is taken, is added in amide solution, is stirred evenly, 65 DEG C of water bath with thermostatic control is sent to In, 10% ammonium hydroxide, insulated and stirred 3 hours is added, discharging cooling obtains modified carbon nano-tube;
(6) above-mentioned modified carbon nano-tube is taken, is mixed with above-mentioned acidification polyphenylene oxide, Sucrose acetoisobutyrate, stirring is added 30 minutes, precipitation was washed in filtering, and air drying obtains carbon nano-tube modification polyphenylene oxide;
(7) above-mentioned carbon nano-tube modification polyphenylene oxide is taken, is added in the dimethylformamide of 30 times of its weight, ultrasound 1 is small When, it pours into culture dish, is put into vacuum drying chamber, be dried in vacuo 20 hours at 70 DEG C, after film molding, be put into 95 DEG C of perseverance Warm drying box is handled 1 hour, takes off film, film water is washed, air drying is to get the epoxidation polyphenylene oxide conductive film.
Embodiment 2
A kind of epoxidation polyphenylene oxide conductive film, it is made of the raw material of following weight parts:
Polyphenylene oxide 120, aluminium triphosphate 2, carbon nanotube 8, methacrylic acid 4, propylene oxide 4, alkanolamide 1,2- mercaptos Ammonium hydroxide 20, the Sucrose acetoisobutyrate 2 of base benzimidazole 1,12%.
A kind of preparation method of epoxidation polyphenylene oxide conductive film, includes the following steps:
(1) 2-mercaptobenzimidazole is taken, is added in the absolute ethyl alcohol of 12 times of its weight, is stirred evenly, obtain alcoholic solution;
(2) take carbon nanotube, be added to its heavy 20 times, in 98% sulfuric acid solution, ultrasound 5 hours, filtering will precipitate Washing, mixes with propylene oxide, is added in above-mentioned alcoholic solution, insulated and stirred 20 minutes, are distilled off ethyl alcohol at 55 DEG C, obtain Activated carbon nano-tube;
(3) methacrylic acid is taken, is added in the chloroform of 30 times of its weight, stirs evenly, polyphenylene oxide is added, stirring 2 is small When, chloroform is distilled off, obtains acidification polyphenylene oxide;
(4) aluminium triphosphate, alkanolamide mixing are taken, is added in the deionized water of 20 times of mixture weight, stirring is equal It is even, obtain amide solution;
(5) above-mentioned activated carbon nano-tube is taken, is added in amide solution, is stirred evenly, 70 DEG C of water bath with thermostatic control is sent to In, 12% ammonium hydroxide, insulated and stirred 5 hours is added, discharging cooling obtains modified carbon nano-tube;
(6) above-mentioned modified carbon nano-tube is taken, is mixed with above-mentioned acidification polyphenylene oxide, Sucrose acetoisobutyrate, stirring is added 40 minutes, precipitation was washed in filtering, and air drying obtains carbon nano-tube modification polyphenylene oxide;
(7) above-mentioned carbon nano-tube modification polyphenylene oxide is taken, is added in the dimethylformamide of 40 times of its weight, ultrasound 2 is small When, it pours into culture dish, is put into vacuum drying chamber, be dried in vacuo 30 hours at 85 DEG C, after film molding, be put into 105 DEG C Thermostatic drying chamber is handled 2 hours, takes off film, film water is washed, air drying is to get the epoxidation polyphenylene oxide conductive film.
Performance test:
The conductivity of the epoxidation polyphenylene oxide conductive film of the present invention is 1.6-2.0 × 10-2Scm-1, mechanical mechanics property 30-33.6Mpa。

Claims (2)

1. a kind of epoxidation polyphenylene oxide conductive film, which is characterized in that it is made of the raw material of following weight parts:
Polyphenylene oxide 100-120, aluminium triphosphate 1-2, carbon nanotube 6-8, methacrylic acid 3-4, propylene oxide 2-4, alkanol acyl Amine 1-2, the ammonium hydroxide 17-20 of 2-mercaptobenzimidazole 0.4-1,10-12%, Sucrose acetoisobutyrate 1-2.
2. a kind of preparation method of epoxidation polyphenylene oxide conductive film as described in claim 1, which is characterized in that including following step Suddenly:
(1) 2-mercaptobenzimidazole is taken, is added in the absolute ethyl alcohol of 10-12 times of its weight, stirs evenly, obtain alcoholic solution;
(2) carbon nanotube is taken, 3-5 hours ultrasonic in sulfuric acid solution that be added to 14-20 times of its weight, 96-98%, filtering, Precipitation is washed, mixes, is added in above-mentioned alcoholic solution with propylene oxide, insulated and stirred 10-20 minutes at 50-55 DEG C, is steamed Ethyl alcohol is removed in distillation, obtains activated carbon nano-tube;
(3) methacrylic acid is taken, is added in the chloroform of 20-30 times of its weight, stirs evenly, polyphenylene oxide is added, stirring 1-2 is small When, chloroform is distilled off, obtains acidification polyphenylene oxide;
(4) aluminium triphosphate, alkanolamide mixing are taken, is added in the deionized water of 15-20 times of mixture weight, stirring is equal It is even, obtain amide solution;
(5) above-mentioned activated carbon nano-tube is taken, is added in amide solution, is stirred evenly, 65-70 DEG C of water bath with thermostatic control is sent to In, the ammonium hydroxide of 10-12%, insulated and stirred 3-5 hours is added, discharging cooling obtains modified carbon nano-tube;
(6) above-mentioned modified carbon nano-tube is taken, is mixed with above-mentioned acidification polyphenylene oxide, Sucrose acetoisobutyrate is added, stirs 30-40 Minute, precipitation is washed in filtering, and air drying obtains carbon nano-tube modification polyphenylene oxide;
(7) above-mentioned carbon nano-tube modification polyphenylene oxide is taken, is added in the dimethylformamide of 30-40 times of its weight, ultrasonic 1-2 is small When, it pours into culture dish, is put into vacuum drying chamber, be dried in vacuo 20-30 hours at 70-85 DEG C, after film molding, is put into 95-105 DEG C of thermostatic drying chamber is handled 1-2 hours, takes off film, film water is washed, air drying is led to get the epoxidation polyphenylene oxide Conductive film.
CN201810417792.0A 2018-05-04 2018-05-04 A kind of epoxidation polyphenylene oxide conductive film and preparation method thereof Withdrawn CN108485231A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109608780A (en) * 2018-12-31 2019-04-12 王爱绿 A kind of flame-retardant expanded insulating board for building and preparation method thereof
CN109777078A (en) * 2018-12-28 2019-05-21 朱雪梅 A kind of polyphenylene oxide graphene proton membrane and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109777078A (en) * 2018-12-28 2019-05-21 朱雪梅 A kind of polyphenylene oxide graphene proton membrane and preparation method thereof
CN109608780A (en) * 2018-12-31 2019-04-12 王爱绿 A kind of flame-retardant expanded insulating board for building and preparation method thereof

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Application publication date: 20180904