CN108587085A - A kind of preparation method of carbon nano-fiber base polyester film - Google Patents

A kind of preparation method of carbon nano-fiber base polyester film Download PDF

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CN108587085A
CN108587085A CN201810515445.1A CN201810515445A CN108587085A CN 108587085 A CN108587085 A CN 108587085A CN 201810515445 A CN201810515445 A CN 201810515445A CN 108587085 A CN108587085 A CN 108587085A
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carbon
polyester film
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powder
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邹峰
赵必花
朱彩娣
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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
    • C08J2367/00Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/02Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • 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
    • 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
    • C08K3/02Elements
    • C08K3/04Carbon
    • 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
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/06Elements
    • 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
    • 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
    • C08K9/02Ingredients treated with inorganic substances
    • 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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  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
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  • Artificial Filaments (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)

Abstract

The invention discloses a kind of preparation methods of carbon nano-fiber base polyester film, belong to field of polymer material preparing technology.Surface modification is carried out to carbon fiber first with nitric acid supersonic synergic, oxide etch and cavitation effect are combined, the ketone acid anhydride containing flexible group is added into carbon fiber again, the systematicness of carbon fiber molecule interchain is set to destroy, carbon nanotube ground in the present invention to obtain carbon nanotube powder, it passes through acid oxidase, a series of chemical treatments such as chloride and nucleophilic displacement of fluorine, so that hexamethylene diamine molecule is grafted to carbon nanotube powder surface, enhance the dispersibility and chemism of carbon nanotube powder, again since carbon nanotube grafting carbon fiber is as reinforcement, mechanical anchor ingot power intensity is occurred into resin matrix interface in it and is apparently higher than traditional carbon fibres and resin matrix, so that with oxygen radical reaction will not occur for resin matrix, to improve the uvioresistant performance of polyester film, it is with a wide range of applications.

Description

A kind of preparation method of carbon nano-fiber base polyester film
Technical field
The invention discloses a kind of preparation methods of carbon nano-fiber base polyester film, belong to high molecular material technology of preparing Field.
Background technology
Polyester film(PET)It is sheet to be made using extrusion molding, then through double using polyethylene terephthalate as raw material To thin-film material made of stretching.Usually water white transparency, glossiness film, good mechanical performance are common barriers One of laminated film base material, but corona resistance is bad.Polyester film is a kind of macromolecule plastic film, because of its high comprehensive performance And increasingly favored by consumers in general.Since the characteristic of polyester film determines its different purposes.Different purposes Requirement and processing technology of the polyester film to raw material and additive have different requirements, thickness and technical indicator also to differ Sample;In addition, only BOPET just serves many purposes, therefore all it is BOPET according to the film of purpose classification.Polyester film is one Kind macromolecule plastic film, is increasingly favored by consumers in general because of its high comprehensive performance.Due to China's output Cannot still meet the needs of market with technical merit, partly still need to rely on import.
It can be divided into drawing process difference according to raw material used by production polyester film following two:Biaxial stretching polyester Film is to utilize to have light material(Also referred to as have light material greatly, be raw material polyester slice content of titanium dioxide be 0.1%, through overdrying Dry, melting squeezes out, the high-grade film of slab and vertically and horizontally stretching, widely used.Simple tension polyester film is to utilize semi-dull Material, by the film of drying, melting, extrusion, slab and longitudinal stretching, the class and price in polyester film are minimum, mainly It is packed for drug tablet.According to the purpose classification of polyester film:Since the characteristic of polyester film determines its different purposes. Requirement and processing technology of the polyester film of different purposes to raw material and additive have different requirements, thickness and technology Index is also different, can be divided into following several:Electrical insulation film.Since it is with good electric appliance, machinery, thermally and chemically lazy Property, good insulation preformance, anti-breakdown voltage are high, are exclusively used in electronics, electrical insulating material.With packages printing, decoration material in the market The development of the fashions trend such as material, label, this specialty polyesters with texture and soft view effect of dumb light polyester film are thin Film demand is increasing year by year, and in rapid growth.That there are tensile strengths is low for the polyester film being commonly used, uvioresistant effect Fruit is poor.Therefore, the polyester film that a kind of tensile strength is high and uvioresistant effect is good is invented to lead high molecular material technology of preparing Domain has positive effect.
Invention content
The technical problems to be solved by the invention:For current conventional polyester film there are tensile strengths low, ultraviolet-resistent property Can be poor, it can not meet the defect of market demands, provide a kind of preparation method of carbon nano-fiber base polyester film.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of preparation method of carbon nano-fiber base polyester film, it is characterised in that specifically preparation process is:
(1)It weighs 0.12~0.15kg carbon nanotubes to pour into grinder, be ground under conditions of rotating speed is 100~115r/min It crushes, obtains carbon nanotube powder, then the sulfuric acid solution that carbon nanotube powder and mass fraction are 98% is mixed and is placed in beaker Middle stirring, and beaker is placed in thermostat water bath and is stirred to react, acid oxidase nanometer powder is obtained, sour oxygen is washed with deionized Change nanometer powder, dry discharging obtains dry oxidation nanometer powder;
(2)Dry oxidation nanometer powder, thionyl chloride and n,N-Dimethylformamide are mixed to be placed in ultrasonic wave separating apparatus and surpassed Sound disperses, and obtains dispersion liquid, then dispersion liquid and hexamethylene diamine are mixed, and be stirred to react, cooling discharging obtains modified carbon nano-tube Powder;
(3)Carbon fiber, absolute ethyl alcohol and acetone are mixed, mixture is obtained, washs mixture with acetone, be put into after washing It is dry in baking oven, dried object is obtained, the mixing of dried object, ketone acid anhydride and concentrated nitric acid is placed in ultrasonic wave separating apparatus and is ultrasonically treated, is done Dry discharging, obtains modified carbon fiber;
(4)It counts in parts by weight, weighs 12~15 parts of modified carbon nano tube pipe powders, 10~12 parts of modified carbon fibers, 2~4 respectively Part n,N-Dimethylformamide, 42~45 parts of polyethylene terephthalates, 2~4 parts of carbon blacks and 3~5 parts of absolute ethyl alcohols, first Modified carbon nano tube pipe powder, modified carbon fiber and n,N-Dimethylformamide are mixed to be placed in blender and are stirred to react, then is added Addition polymerization ethylene glycol terephthalate, carbon black and absolute ethyl alcohol continue heat preservation under conditions of rotating speed is 210~240r/min and stir It mixes, obtains mixture, continue mixture being put into film extrusion in double screw extruder, sizing discharging is to get carbon nano-fiber Base polyester film.
Step(1)The time that grinds is 18~21min, the sulphur that carbon nanotube powder and mass fraction are 98% The mass ratio of acid solution is 1:4, mixing time is 10~12min, and it is 85~90 DEG C to be stirred to react temperature, is stirred to react the time and is 2~3h, washing times are 4~5 times.
Step(2)The mass ratio of the drying carbon nanotube powder, thionyl chloride and n,N-Dimethylformamide is 5: 2:1, ultrasonic disperse 32~36kHz of frequency, ultrasonic disperse time are 1~2h, and the mass ratio of dispersion liquid and hexamethylene diamine is 3:1, it stirs It is 55~60 DEG C to mix reaction temperature, and it is 1~2h to be stirred to react the time.
Step(3)The mass ratio of the carbon fiber, absolute ethyl alcohol and acetone is 4:1:2, mixing time be 21~ 24min, washing times are 3~5 times, and drying temperature is 85~90 DEG C, and drying time is 15~18min, dried object, ketone acid anhydride and matter The mass ratio for measuring the concentrated nitric acid that score is 80% is 2:1:4, be ultrasonically treated temperature be 88~92 DEG C, be ultrasonically treated frequency be 20~ 22kHz, sonication treatment time are 1~2h.
Step(4)The temperature that is stirred to react is 65~70 DEG C, and it is 3~4h to be stirred to react the time, continues mixing time For 10~12min, extrusion pressure is 4~6MPa, and extrusion temperature is 215~220 DEG C.
Compared with other methods, advantageous effects are the present invention:
(1)The present invention is using polyethylene terephthalate as resin matrix, modified carbon nano tube pipe powder, modified carbon fiber conduct Reinforcing agent, and be aided with carbon black and absolute ethyl alcohol etc. and carbon nano-fiber base polyester film is prepared, it is assisted first with nitric acid-ultrasound Surface modification is carried out with to carbon fiber, oxide etch and cavitation effect are combined, improve the surface polarity of carbon fiber and is divided Property is dissipated, so that carbon fiber surface is become coarse, surface oxygen-containing functional group quantity and increases, the crystallite dimension of carbon fiber is also promoted to subtract Small, crystallinity improves, and to enhance the physics or mechanism between carbon fiber and filler interface, forms disorderly arranged Physical Network Shape structure has spread the stress of resin matrix, and the tensile strength for being conducive to polyester film is improved, then is added into carbon fiber Ketone acid anhydride containing flexible group, when tensile deformation occurs, the fracture that the rigid phenyl ring of intramolecular can deform with key, to The stress applied is absorbed, so that the systematicness of carbon fiber molecule interchain is destroyed, to improve the tensile strength of polyester film;
(2)Carbon nanotube ground in the present invention to obtain carbon nanotube powder, by acid oxidase, chloride and nucleophilic displacement of fluorine etc. A series of chemical treatments so that hexamethylene diamine molecule is grafted to carbon nanotube powder surface, and introduces amidine functional group in its end, Carbon nanotube powder surface polarity is enhanced, agglomeration weakens between making carbon nanotube powder, enhances carbon nanotube powder Dispersibility and chemism, continuation are grafted to carbon fiber surface under Action of Surfactant so that carbon nanotube powder Intrinsic silicon is extended to by carbon fiber surface, amido class functional group is contained in wherein modified carbon nano tube pipe powder end, in resin base Resin matrix solidification can be participated in body solidification process, make have very high connection strong between carbon nanotube powder and resin matrix Degree, and since carbon nanotube grafting carbon fiber is as reinforcement, mechanical anchor ingot power intensity is occurred into for itself and resin matrix interface Traditional carbon fibres and resin matrix are apparently higher than, and do not damage the tensile strength of carbon fiber, further increase the drawing of polyester film Intensity is stretched, continues to add carbon black to resin matrix, under the high temperature conditions so that carbon black is melted in resin matrix, purple can be absorbed The radiation energy on resin matrix surface is irradiated in outside line so that with oxygen radical reaction will not occur for resin matrix, to improve polyester The uvioresistant performance of film, is with a wide range of applications.
Specific implementation mode
It weighs 0.12~0.15kg carbon nanotubes to pour into grinder, be ground under conditions of rotating speed is 100~115r/min Be milled broken 18~21min, obtains carbon nanotube powder, then the sulfuric acid solution that carbon nanotube powder and mass fraction are 98% is pressed Mass ratio is 1:4 mixing are placed in beaker after 10~12min of stirring, and beaker is placed in thermostat water bath, are 85 in temperature It is stirred to react 2~3h under conditions of~90 DEG C, obtains acid oxidase nanometer powder, acid oxidase nanometer powder 4 is washed with deionized ~5 times, dry discharging obtains dry oxidation nanometer powder;It will dry oxidation nanometer powder, thionyl chloride and N, N- dimethyl methyl Amide is 5 in mass ratio:2:1 mixing be placed in ultrasonic wave separating apparatus, under conditions of 32~36kHz of frequency ultrasonic disperse 1~ 2h, obtains dispersion liquid, then by dispersion liquid and hexamethylene diamine is 3 in mass ratio:1 mixing, and under conditions of temperature is 55~60 DEG C It is stirred to react 1~2h, cooling discharging obtains modified carbon nano tube pipe powder;It is 4 in mass ratio:1:2 by carbon fiber, absolute ethyl alcohol 21~24min is mixed with acetone, obtains mixture, washs mixture 3~5 times with acetone, be put into baking oven after washing, Temperature is dry 15~18min at 85~90 DEG C, obtains dried object, is in mass ratio 2:1:4 divide dried object, ketone acid anhydride and quality Number is placed in for 80% concentrated nitric acid mixing in ultrasonic wave separating apparatus, in the condition that temperature is 88~92 DEG C, frequency is 20~22kHz 1~2h of lower supersound process, dry discharging, obtains modified carbon fiber;It counts in parts by weight, weighs 12~15 parts of carbon modifieds respectively and receive Mitron powder, 10~12 parts of modified carbon fibers, 2~4 parts of n,N-Dimethylformamide, 42~45 parts of polyethylene terephthalates Ester, 2~4 parts of carbon blacks and 3~5 parts of absolute ethyl alcohols, first by modified carbon nano tube pipe powder, modified carbon fiber and N, N- dimethyl formyls Amine mixing is placed in blender, is stirred to react 3~4h under conditions of temperature is 65~70 DEG C, then add poly terephthalic acid second Diol ester, carbon black and absolute ethyl alcohol continue 10~12min of insulated and stirred under conditions of rotating speed is 210~240r/min, obtain Mixture continues mixture being put into double screw extruder, in the condition that pressure is 4~6MPa, temperature is 215~220 DEG C Lower film extrusion, sizing discharging is to get carbon nano-fiber base polyester film.
Example 1
It weighs 0.12kg carbon nanotubes to pour into grinder, grinds 18min under conditions of rotating speed is 100r/min, obtain Carbon nanotube powder, then by the sulfuric acid solution that carbon nanotube powder and mass fraction are 98% be 1 in mass ratio:4 mixing are placed in After stirring 10min in beaker, and beaker is placed in thermostat water bath, is stirred to react 2h under conditions of temperature is 85 DEG C, obtains To acid oxidase nanometer powder, acid oxidase nanometer powder is washed with deionized 4 times, dry discharging obtains dry oxidation nanometer powder End;It is 5 in mass ratio by dry oxidation nanometer powder, thionyl chloride and n,N-Dimethylformamide:2:1 mixing is placed in ultrasonic wave In separating apparatus, ultrasonic disperse 1h under conditions of frequency 32kHz obtains dispersion liquid, then in mass ratio by dispersion liquid and hexamethylene diamine It is 3:1 mixing, and it is stirred to react 1h under conditions of temperature is 55 DEG C, cooling discharging obtains modified carbon nano tube pipe powder;By matter Amount is than being 4:1:21min is mixed in carbon fiber, absolute ethyl alcohol and acetone by 2, obtains mixture, mixture 3 is washed with acetone It is secondary, it is put into baking oven after washing, dry 15min at being 85 DEG C in temperature obtains dried object, is in mass ratio 2:1:4 will dry The concentrated nitric acid mixing that object, ketone acid anhydride and mass fraction are 80% is placed in ultrasonic wave separating apparatus, temperature is 88 DEG C, frequency is 1h is ultrasonically treated under conditions of 20kHz, dry discharging obtains modified carbon fiber;It counts in parts by weight, weighs 12 parts of modifications respectively Carbon nanotube powder, 10 parts of modified carbon fibers, 2 parts of n,N-Dimethylformamide, 42 parts of polyethylene terephthalates, 2 parts Modified carbon nano tube pipe powder, modified carbon fiber and n,N-Dimethylformamide first are mixed to be placed in and be stirred by carbon black and 3 parts of absolute ethyl alcohols It mixes in machine, is stirred to react 3h under conditions of temperature is 65 DEG C, then add polyethylene terephthalate, carbon black and anhydrous second Alcohol continues insulated and stirred 10min under conditions of rotating speed is 210r/min, obtains mixture, continues mixture being put into double spiral shells In bar extruder, film extrusion under conditions of pressure is 4MPa, temperature is 215 DEG C, sizing discharging is to get carbon nano-fiber base Polyester film.
Example 2
It weighs 0.14kg carbon nanotubes to pour into grinder, grinds 20min under conditions of rotating speed is 110r/min, obtain Carbon nanotube powder, then by the sulfuric acid solution that carbon nanotube powder and mass fraction are 98% be 1 in mass ratio:4 mixing are placed in After stirring 11min in beaker, and beaker is placed in thermostat water bath, 2.5h is stirred to react under conditions of temperature is 87 DEG C, Acid oxidase nanometer powder is obtained, acid oxidase nanometer powder is washed with deionized 4 times, dry discharging obtains dry oxidation nanometer Powder;It is 5 in mass ratio by dry oxidation nanometer powder, thionyl chloride and n,N-Dimethylformamide:2:1 mixing is placed in ultrasound In wave separating apparatus, ultrasonic disperse 1.5h under conditions of frequency 34kHz obtains dispersion liquid, then dispersion liquid and hexamethylene diamine is pressed matter Amount is than being 3:1 mixing, and it is stirred to react 1.5h under conditions of temperature is 57 DEG C, cooling discharging obtains modified carbon nano-tube powder End;It is 4 in mass ratio:1:23min is mixed in carbon fiber, absolute ethyl alcohol and acetone by 2, is obtained mixture, is washed with acetone Mixture 4 times, is put into after washing in baking oven, and dry 17min at being 87 DEG C in temperature obtains dried object, is in mass ratio 2:1:4 The concentrated nitric acid that dried object, ketone acid anhydride and mass fraction are 80% is mixed and is placed in ultrasonic wave separating apparatus, is 90 DEG C, frequency in temperature To be ultrasonically treated 1.5h under conditions of 21kHz, dry discharging obtains modified carbon fiber;It counts in parts by weight, weighs 14 parts respectively Modified carbon nano tube pipe powder, 11 parts of modified carbon fibers, 3 parts of n,N-Dimethylformamide, 44 parts of polyethylene terephthalates, Modified carbon nano tube pipe powder, modified carbon fiber and n,N-Dimethylformamide are first mixed and are set by 3 parts of carbon blacks and 4 parts of absolute ethyl alcohols In blender, temperature be 67 DEG C under conditions of be stirred to react 3.5h, then add polyethylene terephthalate, carbon black and Absolute ethyl alcohol continues insulated and stirred 11min under conditions of rotating speed is 230r/min, obtains mixture, continue to put mixture Enter in double screw extruder, film extrusion under conditions of pressure is 5MPa, temperature is 217 DEG C, sizing discharging is to get carbon nanometer Fiber base polyester film.
Example 3
It weighs 0.15kg carbon nanotubes to pour into grinder, grinds 21min under conditions of rotating speed is 115r/min, obtain Carbon nanotube powder, then by the sulfuric acid solution that carbon nanotube powder and mass fraction are 98% be 1 in mass ratio:4 mixing are placed in After stirring 12min in beaker, and beaker is placed in thermostat water bath, 3h is stirred to react under the conditions of at a temperature of 90 °C, is obtained To acid oxidase nanometer powder, acid oxidase nanometer powder is washed with deionized 5 times, dry discharging obtains dry oxidation nanometer powder End;It is 5 in mass ratio by dry oxidation nanometer powder, thionyl chloride and n,N-Dimethylformamide:2:1 mixing is placed in ultrasonic wave In separating apparatus, ultrasonic disperse 2h under conditions of frequency 36kHz obtains dispersion liquid, then in mass ratio by dispersion liquid and hexamethylene diamine It is 3:1 mixing, and it is stirred to react 2h under conditions of temperature is 60 DEG C, cooling discharging obtains modified carbon nano tube pipe powder;By matter Amount is than being 4:1:24min is mixed in carbon fiber, absolute ethyl alcohol and acetone by 2, obtains mixture, mixture 5 is washed with acetone It is secondary, it is put into baking oven after washing, dry 18min at being 90 DEG C in temperature obtains dried object, is in mass ratio 2:1:4 will dry The concentrated nitric acid mixing that object, ketone acid anhydride and mass fraction are 80% is placed in ultrasonic wave separating apparatus, temperature is 92 DEG C, frequency is 2h is ultrasonically treated under conditions of 22kHz, dry discharging obtains modified carbon fiber;It counts in parts by weight, weighs 15 parts of modifications respectively Carbon nanotube powder, 12 parts of modified carbon fibers, 4 parts of n,N-Dimethylformamide, 45 parts of polyethylene terephthalates, 4 parts Modified carbon nano tube pipe powder, modified carbon fiber and n,N-Dimethylformamide first are mixed to be placed in and be stirred by carbon black and 5 parts of absolute ethyl alcohols It mixes in machine, is stirred to react 4h under conditions of temperature is 70 DEG C, then add polyethylene terephthalate, carbon black and anhydrous second Alcohol continues insulated and stirred 12min under conditions of rotating speed is 240r/min, obtains mixture, continues mixture being put into double spiral shells In bar extruder, film extrusion under conditions of pressure is 6MPa, temperature is 220 DEG C, sizing discharging is to get carbon nano-fiber base Polyester film.
Comparative example
With the carbon nano-fiber base polyester film of Changzhou company production as a comparison case to carbon nano-fiber produced by the present invention Carbon nano-fiber base polyester film in base polyester film and comparative example carries out performance detection, and testing result is as shown in table 1:
Test method:
Tensile strength test is detected using polyester film tensile strength tester;
Elongation at break test is detected using Tai'an LDS plastic film elongation at break detectors;
Tensile strength test is detected using polyester film instron;
Elasticity modulus test is detected using elastic modulus tester;
The test of ultraviolet isolating rate is detected using the portable solar film testers of LS162A.
1 polyester film performance measurement result of table
Note:It is reference with the film of 50mm thickness
High according to the tensile strength produced by the present invention of data among the above, elongation at break is high, and tensile strength is high, ultraviolet light resistance Every rate height, anti-ultraviolet property is good, has broad application prospects.

Claims (5)

1. a kind of preparation method of carbon nano-fiber base polyester film, it is characterised in that specifically preparation process is:
(1)It weighs 0.12~0.15kg carbon nanotubes to pour into grinder, be ground under conditions of rotating speed is 100~115r/min It crushes, obtains carbon nanotube powder, then the sulfuric acid solution that carbon nanotube powder and mass fraction are 98% is mixed and is placed in beaker Middle stirring, and beaker is placed in thermostat water bath and is stirred to react, acid oxidase nanometer powder is obtained, sour oxygen is washed with deionized Change nanometer powder, dry discharging obtains dry oxidation nanometer powder;
(2)Dry oxidation nanometer powder, thionyl chloride and n,N-Dimethylformamide are mixed to be placed in ultrasonic wave separating apparatus and surpassed Sound disperses, and obtains dispersion liquid, then dispersion liquid and hexamethylene diamine are mixed, and be stirred to react, cooling discharging obtains modified carbon nano-tube Powder;
(3)Carbon fiber, absolute ethyl alcohol and acetone are mixed, mixture is obtained, washs mixture with acetone, be put into after washing It is dry in baking oven, dried object is obtained, the mixing of dried object, ketone acid anhydride and concentrated nitric acid is placed in ultrasonic wave separating apparatus and is ultrasonically treated, is done Dry discharging, obtains modified carbon fiber;
(4)It counts in parts by weight, weighs 12~15 parts of modified carbon nano tube pipe powders, 10~12 parts of modified carbon fibers, 2~4 respectively Part n,N-Dimethylformamide, 42~45 parts of polyethylene terephthalates, 2~4 parts of carbon blacks and 3~5 parts of absolute ethyl alcohols, first Modified carbon nano tube pipe powder, modified carbon fiber and n,N-Dimethylformamide are mixed to be placed in blender and are stirred to react, then is added Addition polymerization ethylene glycol terephthalate, carbon black and absolute ethyl alcohol continue heat preservation under conditions of rotating speed is 210~240r/min and stir It mixes, obtains mixture, continue mixture being put into film extrusion in double screw extruder, sizing discharging is to get carbon nano-fiber Base polyester film.
2. a kind of preparation method of carbon nano-fiber base polyester film according to claim 1, it is characterised in that:Step (1)The time that grinds is 18~21min, the quality for the sulfuric acid solution that carbon nanotube powder and mass fraction are 98% Than being 1:4, mixing time is 10~12min, and it is 85~90 DEG C to be stirred to react temperature, and it is 2~3h, washing time to be stirred to react the time Number is 4~5 times.
3. a kind of preparation method of carbon nano-fiber base polyester film according to claim 1, it is characterised in that:Step (2)The mass ratio of the drying carbon nanotube powder, thionyl chloride and n,N-Dimethylformamide is 5:2:1, ultrasonic disperse 32~36kHz of frequency, ultrasonic disperse time are 1~2h, and the mass ratio of dispersion liquid and hexamethylene diamine is 3:1, being stirred to react temperature is 55~60 DEG C, it is 1~2h to be stirred to react the time.
4. a kind of preparation method of carbon nano-fiber base polyester film according to claim 1, it is characterised in that:Step (3)The mass ratio of the carbon fiber, absolute ethyl alcohol and acetone is 4:1:2, mixing time is 21~24min, washing times 3 ~5 times, drying temperature be 85~90 DEG C, drying time be 15~18min, dried object, ketone acid anhydride and mass fraction be 80% it is dense The mass ratio of nitric acid is 2:1:4, it is 88~92 DEG C to be ultrasonically treated temperature, and supersounds process frequency is 20~22kHz, when supersound process Between be 1~2h.
5. a kind of preparation method of carbon nano-fiber base polyester film according to claim 1, it is characterised in that:Step (4)The temperature that is stirred to react is 65~70 DEG C, and it is 3~4h to be stirred to react the time, and continuation mixing time is 10~12min, Extrusion pressure is 4~6MPa, and extrusion temperature is 215~220 DEG C.
CN201810515445.1A 2018-05-25 2018-05-25 A kind of preparation method of carbon nano-fiber base polyester film Pending CN108587085A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111549391A (en) * 2020-06-15 2020-08-18 杨旺姣 Preparation method of antibacterial polyester fiber
CN114149666A (en) * 2021-12-28 2022-03-08 会通新材料股份有限公司 PBT composite material and preparation method thereof
CN117165047A (en) * 2023-08-29 2023-12-05 苏州怀仁化纤有限公司 Polyester film with release function for prepreg

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Application publication date: 20180928