CN109021232A - A kind of carbon nanotube composite conducting material and preparation method thereof - Google Patents

A kind of carbon nanotube composite conducting material and preparation method thereof Download PDF

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Publication number
CN109021232A
CN109021232A CN201810773332.1A CN201810773332A CN109021232A CN 109021232 A CN109021232 A CN 109021232A CN 201810773332 A CN201810773332 A CN 201810773332A CN 109021232 A CN109021232 A CN 109021232A
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China
Prior art keywords
carbon nanotube
pyridine
added
dispersion liquid
taken
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CN201810773332.1A
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Chinese (zh)
Inventor
孙艺宾
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Hefei Ai Feixin Materials Co Ltd
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Hefei Ai Feixin Materials Co Ltd
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Priority to CN201810773332.1A priority Critical patent/CN109021232A/en
Publication of CN109021232A publication Critical patent/CN109021232A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular 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
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/0622Polycondensates containing six-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
    • C08G73/0627Polycondensates containing six-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring
    • 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
    • C08K3/02Elements
    • C08K3/04Carbon
    • C08K3/041Carbon nanotubes
    • 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
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

Abstract

The invention discloses a kind of carbon nanotube composite conducting materials and preparation method thereof, and the composite conducting material is made of the raw material of following weight parts: sodium carbonate 0.1-0.2, sodium acrylate 10-20, ammonium persulfate 1-1.8, pyridine 40-60, carbon nanotube 100-130, propylene oxide 6-8, methyl methacrylate 10-14, aluminium dihydrogen phosphate 2-3, catalyst 0.01-0.013.The present invention is reacted under the catalysis of sodium carbonate by the alcoholic extract hydroxyl group of carbon nano tube surface with epoxy group, so as to improve the compatibility of pyridine and carbon nanotube, finally it polymerize under initiator effect, obtain the composite material of polypyridine and carbon nanotube, Compound Material Engineering and conductive stability of the invention is good, and comprehensive performance is superior.

Description

A kind of carbon nanotube composite conducting material and preparation method thereof
Technical field
The invention belongs to conductive material fields, and in particular to a kind of carbon nanotube composite conducting material and preparation method thereof.
Background technique
In carbon nano-material, carbon nanotube (CNTs) because have special one-dimentional structure and physicochemical properties, especially its Excellent mechanical performance and chemical property, makes it all have wide practical use in many fields, such as functional composite material, Energy stores and switching device, sensor, Flied emission, semiconductor devices etc., wherein carbon nanotube is formed with conducting polymer High-conductivity composite material is increasingly becoming research hotspot;However, since the compatibility of carbon nanotube and conducting polymer is poor, such as Fruit conducting polymer is reunited on the surface of carbon nanotube, it is possible to the electron transmission of carbon nanotube is blocked, to reduce its electricity Capacity.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of carbon nanotube composite conducting materials And preparation method thereof.
To achieve the above object, the invention adopts the following technical scheme:
A kind of carbon nanotube composite conducting material, it is composed of the following raw materials by weight: sodium carbonate 0.1-0.2, Sodium acrylate 10-20, ammonium persulfate 1-1.8, pyridine 40-60, carbon nanotube 100-130, propylene oxide 6-8, methacrylic acid Methyl esters 10-14, aluminium dihydrogen phosphate 2-3, catalyst 0.01-0.013.
The catalyst is lithium methoxide.
The preparation method of the carbon nanotube composite conducting material, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly;
(2) pyridine is taken, is added in the deionized water of 10-15 times of its weight, stirs evenly, obtains pyridine dispersion liquid;
(3) methyl methacrylate, epoxy prapanol mixing are taken, is sent in stainless steel cauldron, is passed through nitrogen, is adjusted anti- Answering kettle temperature degree is 95-105 DEG C, is stirred to react 1-2 hours, and catalyst is added, and adjusting temperature of reaction kettle is 150-160 DEG C, is added Above-mentioned pyridine dispersion liquid, insulation reaction 3-4 hours, discharging cooling obtained epoxy-modified pyridine solution;
(4) aluminium dihydrogen phosphate, carbon nanotube are taken, is heated 20-50 minutes at 140-160 DEG C, is mixed, add with sodium acrylate Enter into 10-13 times of mixture weight of deionized water, it is 1-2 hours ultrasonic, obtain carbon nano tube dispersion liquid;
(5) above-mentioned epoxy-modified pyridine solution, carbon nano tube dispersion liquid mixing are taken, is stirred evenly, raising temperature is 130- 150 DEG C, sodium carbonate is added, insulated and stirred 4-6 hours, is cooled to room temperature, obtains modified carbon nano-tube dispersion liquid;
(6) above-mentioned modified carbon nano-tube dispersion liquid is taken, is sent in reaction kettle, nitrogen is passed through, adjusting temperature of reaction kettle is 50-75 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 3-5 hours, precipitating was washed in filtering, at 75-80 DEG C of vacuum It is 1-2 hours dry, it is cooled to room temperature to get the carbon nanotube composite conducting material.
Advantages of the present invention:
The present invention is modified pyridine using lithium methoxide as catalyst using methyl methacrylate, epoxy prapanol as raw material, Epoxy-modified pyridine solution is obtained, then carbon nanotube, sodium acrylate are blended, obtain carbon nano tube dispersion liquid, then receive by carbon The alcoholic extract hydroxyl group of nanotube surface reacts under the catalysis of sodium carbonate with epoxy group, so as to improve the compatible of pyridine and carbon nanotube Property, finally it polymerize under initiator effect, obtains the composite material of polypyridine and carbon nanotube, Compound Material Engineering of the invention Good with conductive stability, conducting polymer is not easy to reunite, and capacitance is high, and comprehensive performance is superior.
Specific embodiment
Embodiment 1
A kind of carbon nanotube composite conducting material, it is composed of the following raw materials by weight:
Sodium carbonate 0.1, sodium acrylate 10, ammonium persulfate 1, pyridine 40, carbon nanotube 100, propylene oxide 6, metering system Sour methyl esters 10, aluminium dihydrogen phosphate 2, catalyst 0.01.
The catalyst is lithium methoxide.
The preparation method of the carbon nanotube composite conducting material, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 20 times of its weight, stirs evenly;
(2) pyridine is taken, is added in the deionized water of 10 times of its weight, stirs evenly, obtain pyridine dispersion liquid;
(3) methyl methacrylate, epoxy prapanol mixing are taken, is sent in stainless steel cauldron, is passed through nitrogen, is adjusted anti- Answering kettle temperature degree is 95 DEG C, is stirred to react 1 hour, and catalyst is added, and adjusting temperature of reaction kettle is 150 DEG C, and above-mentioned pyridine point is added Dispersion liquid, insulation reaction 3 hours, discharging cooling obtained epoxy-modified pyridine solution;
(4) aluminium dihydrogen phosphate, carbon nanotube are taken, is heated 20 minutes at 140 DEG C, is mixed, be added to mixed with sodium acrylate It closes in the deionized water for expecting 10 times of weight, ultrasound 1 hour obtains carbon nano tube dispersion liquid;
(5) above-mentioned epoxy-modified pyridine solution, carbon nano tube dispersion liquid mixing are taken, is stirred evenly, increasing temperature is 130 DEG C, sodium carbonate is added, insulated and stirred 4 hours, is cooled to room temperature, obtains modified carbon nano-tube dispersion liquid;
(6) above-mentioned modified carbon nano-tube dispersion liquid is taken, is sent in reaction kettle, nitrogen is passed through, adjusting temperature of reaction kettle is 50 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 3 hours, precipitating was washed in filtering, and dry 1 is small at 75 DEG C of vacuum When, it is cooled to room temperature to get the carbon nanotube composite conducting material.
Embodiment 2
A kind of carbon nanotube composite conducting material, it is composed of the following raw materials by weight: sodium carbonate 0.2, propylene Sour sodium 20, ammonium persulfate 1.8, pyridine 60, carbon nanotube 130, propylene oxide 8, methyl methacrylate 14, aluminium dihydrogen phosphate 3, Catalyst 0.013.
The catalyst is lithium methoxide.
The preparation method of the carbon nanotube composite conducting material, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 30 times of its weight, stirs evenly;
(2) pyridine is taken, is added in the deionized water of 15 times of its weight, stirs evenly, obtain pyridine dispersion liquid;
(3) methyl methacrylate, epoxy prapanol mixing are taken, is sent in stainless steel cauldron, is passed through nitrogen, is adjusted anti- Answering kettle temperature degree is 105 DEG C, is stirred to react 2 hours, and catalyst is added, and adjusting temperature of reaction kettle is 160 DEG C, and above-mentioned pyridine point is added Dispersion liquid, insulation reaction 4 hours, discharging cooling obtained epoxy-modified pyridine solution;
(4) aluminium dihydrogen phosphate, carbon nanotube are taken, is heated 50 minutes at 160 DEG C, is mixed, be added to mixed with sodium acrylate It closes in the deionized water for expecting 13 times of weight, ultrasound 2 hours obtains carbon nano tube dispersion liquid;
(5) above-mentioned epoxy-modified pyridine solution, carbon nano tube dispersion liquid mixing are taken, is stirred evenly, increasing temperature is 150 DEG C, sodium carbonate is added, insulated and stirred 6 hours, is cooled to room temperature, obtains modified carbon nano-tube dispersion liquid;
(6) above-mentioned modified carbon nano-tube dispersion liquid is taken, is sent in reaction kettle, nitrogen is passed through, adjusting temperature of reaction kettle is 75 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 5 hours, precipitating was washed in filtering, and dry 2 is small at 80 DEG C of vacuum When, it is cooled to room temperature to get the carbon nanotube composite conducting material.
Performance test:
The carbon nanotube composite conducting material of the embodiment of the present invention 1:
Specific capacitance is 188.8F/g;
The carbon nanotube composite conducting material of the embodiment of the present invention 2:
Specific capacitance is 191.5F/g.

Claims (3)

1. a kind of carbon nanotube composite conducting material, which is characterized in that it is composed of the following raw materials by weight:
Sodium carbonate 0.1-0.2, sodium acrylate 10-20, ammonium persulfate 1-1.8, pyridine 40-60, carbon nanotube 100-130, epoxy Propane 6-8, methyl methacrylate 10-14, aluminium dihydrogen phosphate 2-3, catalyst 0.01-0.013.
2. a kind of carbon nanotube composite conducting material according to claim 1, which is characterized in that the catalyst is first Lithium alkoxide.
3. a kind of preparation method of carbon nanotube composite conducting material as described in claim 1, which is characterized in that including following step It is rapid:
(1) ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly;
(2) pyridine is taken, is added in the deionized water of 10-15 times of its weight, stirs evenly, obtains pyridine dispersion liquid;
(3) methyl methacrylate, epoxy prapanol mixing are taken, is sent in stainless steel cauldron, is passed through nitrogen, adjust reaction kettle Temperature is 95-105 DEG C, is stirred to react 1-2 hours, and catalyst is added, and adjusting temperature of reaction kettle is 150-160 DEG C, is added above-mentioned Pyridine dispersion liquid, insulation reaction 3-4 hours, discharging cooling obtained epoxy-modified pyridine solution;
(4) aluminium dihydrogen phosphate, carbon nanotube are taken, is heated 20-50 minutes at 140-160 DEG C, is mixed, be added to sodium acrylate It is 1-2 hours ultrasonic in the deionized water of 10-13 times of mixture weight, obtain carbon nano tube dispersion liquid;
(5) above-mentioned epoxy-modified pyridine solution, carbon nano tube dispersion liquid mixing are taken, is stirred evenly, raising temperature is 130-150 DEG C, sodium carbonate is added, insulated and stirred 4-6 hours, is cooled to room temperature, obtains modified carbon nano-tube dispersion liquid;
(6) above-mentioned modified carbon nano-tube dispersion liquid is taken, is sent in reaction kettle, nitrogen is passed through, adjusting temperature of reaction kettle is 50-75 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 3-5 hours, precipitating was washed in filtering, dry 1- at 75-80 DEG C of vacuum It 2 hours, is cooled to room temperature to get the carbon nanotube composite conducting material.
CN201810773332.1A 2018-07-14 2018-07-14 A kind of carbon nanotube composite conducting material and preparation method thereof Pending CN109021232A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109575682A (en) * 2018-12-28 2019-04-05 张展清 A kind of IML ink of resistance to red ink 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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CN1886808A (en) * 2003-09-29 2006-12-27 通用电气公司 Conductive thermoplastic compositions, methods of manufacture and articles derived from such compositions
WO2013105757A1 (en) * 2012-01-12 2013-07-18 Hanwha Chemical Corporation Resin composition for emi shielding, comprising carbon hydride composite
CN108940269A (en) * 2017-11-03 2018-12-07 深圳大学 A kind of Nanoalloy and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1886808A (en) * 2003-09-29 2006-12-27 通用电气公司 Conductive thermoplastic compositions, methods of manufacture and articles derived from such compositions
WO2013105757A1 (en) * 2012-01-12 2013-07-18 Hanwha Chemical Corporation Resin composition for emi shielding, comprising carbon hydride composite
CN108940269A (en) * 2017-11-03 2018-12-07 深圳大学 A kind of Nanoalloy and preparation method thereof

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109575682A (en) * 2018-12-28 2019-04-05 张展清 A kind of IML ink of resistance to red ink 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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Application publication date: 20181218