CN108660742A - A kind of preparation method of polyimide fiber surface chemical modification carbon nanotube - Google Patents
A kind of preparation method of polyimide fiber surface chemical modification carbon nanotube Download PDFInfo
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- C08G73/0666—Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms
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- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
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- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
The invention discloses a kind of preparation methods of polyimides (PI) fiber surface carbon nanometer tube with chemical decoration, it is characterised in that：It will be dispersed in trishydroxymethylaminomethane hydrochloric acid buffer solution with dopamine by the PI fibers of surface cleaning processing, react at room temperature, poly-dopamine clad is formed on the surfaces PI.Then a certain amount of polyethyleneimine is added in above-mentioned reaction solution, the functionalized PI fibers of surface amino groups are formed by being reacted with poly-dopamine, it is eventually adding carboxyl-functional multi-walled carbon nano-tube, it is reacted with PI fiber surface amido functional groups by carbon nano tube surface carboxyl functional group, obtains the PI fibers of surface chemical modification multi-walled carbon nanotube.Method through the invention can effectively increase the surface roughness of polyimide fiber, reduce surface energy, improve its hydrophily and specific surface area, the interfacial combined function for improving fiber and matrix resin simultaneously is modified to be conducive to it applied to the enhancing of thermoplastic.
Description
Technical field
The present invention relates to field of compound material, are specifically related to a kind of carbon nano tube surface chemical modification polyimides (PI)
The preparation method of fiber.
Background technology
PI fibers have both the wider array of feature of fiber applicability, PI fibers on the basis of retaining original PI outstanding properties
The big modulus height of intensity, high temperature resistant, chemical mediator corrosion are mainly used for high temperature fume dust removal filter bag, the anti-soda acid fabric of weaving, resistance to
The fields such as fiery fabric, the flame-retardant and thermal-insulated proximate matter material of industry, multielement functionality advanced composite material (ACM).But PI fiber surfaces do not have
Active function groups, performance are stablized, and structure is smooth, poor with matrix binding performance, limits composite materials property and machinery
Performance further increases.
The excellent properties such as high and low temperature resistance, radiation resistance, high intensity and high-modulus that PI fibers have can be made with it
Make fibrous composite, to apply in the application fields such as high-low temperature resistant and radiation hardness, it is more representational be exactly national defence and
Aerospace field.PI fibers can be stabilized a few hours at high temperature, can make the parts and aerospace of rocket with it
Some parts of device, for coping with the harsh temperatures environment of the outer space, the Lear Suo Te companies of Russia by PI fibers with it is other
Light heat-resisting cable shield sheath has been made to apply on special purpose aviation in metal wire together.
The unique structure of carbon nanotube determines that it has many unique physical properties and chemical property.Because of carbon nanometer
C=C covalent bonds in pipe are considered as the chemical bond stablized the most in nature, so carbon nanotube has excellent mechanical property
Can, while can be obtained by theoretical calculation, carbon nanotube also has extremely excellent intensity and toughness, and carbon nanotube is in addition to power
Outside haveing excellent performance also have good conductive property.By adulterating micro carbon nanotube in the composite, then carbon is received
Mitron is suitably orientated so that the thermal conductivity of composite material has prodigious improvement.
The performance of composite material depends not only on the performance of its basis material simultaneously, while also significantly depending on
Interface cohesion situation between each component.The interface of composite material is the intermediate bridge between reinforced phase and matrix phase, and
The transmitter of energy and information, good interfacial bonding property can effectively transmit load to improve the mechanical property of composite material
Energy.Therefore the superiority of good interface effect is made full use of, the roughness and specific surface area of PI fiber surfaces are improved, it is fine to improve PI
The interfacial combined function of dimension and basis material, can significantly improve the mechanical property and mechanical performance of composite material.
Invention content
Problem to be solved by this invention is to change PI fiber surface inertia, improves surface roughness, the drop of PI fibers
Low-surface-energy improves its hydrophily and specific surface area, while improving the interfacial combined function of fiber and matrix resin, to have
It is applied to the enhancing of thermoplastic conducive to it to be modified.
The present invention is achieved through the following technical solutions：
(1) PI fibers are cleaned；(2) will be dispersed in by PI fibers and the dopamine of surface cleaning processing buffer it is molten
In liquid, poly-dopamine clad is formed on the surfaces PI after reaction；(3) that a certain amount of polyethyleneimine is added to above-mentioned reaction is molten
In liquid, the functionalized PI fibers of surface amino groups are formed by being reacted with poly-dopamine；(4) carboxy-functionalized multi-wall carbon nano-tube is added
Pipe, is reacted by carbon nano tube surface carboxyl functional group with PI fiber surface amido functional groups, and surface chemical modification multi wall is obtained
The PI fibers of carbon nanotube.
The PI fibers are a kind of high-strength and high-modulus and surface inactive organic synthetic fibers, and form can be continuous length
Fiber can also be chopped strand.
Tris solution and a concentration of 1mol/L of the buffer solution by a concentration of 1.2mg/mL
Hydrochloric acid solution configures, pH value 8.5.A concentration of 1.0~5.0mg/mL of dopamine, reaction temperature are in reaction solution
Room temperature, reaction time 2h.
The volume fraction of the polyethyleneimine is 1.0~5.0vol.%, and reaction temperature is room temperature, and the reaction time is
30min。
The carbon nanotube is carboxyl-functional multi-walled carbon nano-tube, and mass fraction is：1.0~2.0wt.%, instead
It is room temperature, reaction time 6h to answer temperature.
The PI fibers of carbon nano tube chemical decoration have been obtained by method as above, have improved the rough surface of PI fibers
Degree reduces surface energy, improves its hydrophily and specific surface area, while improving the interfacial combined function of fiber and matrix resin,
It is modified applied to the enhancing of thermoplastic to be conducive to it.
Specific implementation mode
It is the preparation method for the PI fiber surface carbon nanometer tube with chemical decoration for combining technical solution of the present invention to be provided below
The embodiment done, the present invention is explained further.
Example 1
Chopping processing is carried out to PI fibers, makes the length of 1mm, it is then that the PI fibers of 5.0g is ultrasonic in acetone solvent
Cleaning 2h is carried out under environment.It after acetone cleans, is respectively washed 3 times with ethyl alcohol and deionized water, clean PI fibers is put
Enter in blast dry oven and dries；The trishydroxymethylaminomethane for weighing 0.6g is added in 500mL deionized waters, configuration concentration
For the solution of 1.2mg/mL, pH value is measured with acidometer, then uses the hydrochloric acid solution of 1mol/L that trishydroxymethylaminomethane is molten
The pH value of liquid is adjusted to 8.5, obtains trishydroxymethylaminomethane-hydrochloric acid buffer solution；1.0g dopamine powder is weighed to be added to
In trishydroxymethylaminomethane-hydrochloric acid buffer solution, the processed PI fibers of 5.0g are added in reaction system therewith, by it
After stirring evenly, 2h is reacted under room temperature.The polyethyleneimine for measuring 1mL, is added in reaction system, at ambient temperature
Carry out copolyreaction 30min；0.05g carboxyl-functional multi-walled carbon nano-tubes are weighed, are added in reaction system, in room temperature condition
Lower progress copolyreaction 6h, is cleaned 3 times with deionized water, and the PI fibers of clean carbon nano tube modified mistake are put into forced air drying
It is dry in baking oven, then it is sealed with valve bag.Static Contact is carried out to the PI fibers of obtained graphene oxide modified
Angle is tested, and test result shows that the contact angle of PI fibers is reduced to 67.5 ° by 120.4 °, and the hydrophily of PI fibers obtains greatly
It improves.
Example 2
Chopping processing is carried out to PI fibers, makes the length of 3mm, it is then that the PI fibers of 5.0g is ultrasonic in acetone solvent
Cleaning 2h is carried out under environment.It after acetone cleans, is respectively washed 3 times with ethyl alcohol and deionized water, clean PI fibers is put
Enter in blast dry oven and dries；The trishydroxymethylaminomethane for weighing 0.6g is added in 500mL deionized waters, configuration concentration
For the solution of 1.2mg/mL, pH value is measured with acidometer, then uses the hydrochloric acid solution of 1mol/L that trishydroxymethylaminomethane is molten
The pH value of liquid is adjusted to 8.5, obtains trishydroxymethylaminomethane-hydrochloric acid buffer solution；0.5g dopamine powder is weighed to be added to
In trishydroxymethylaminomethane-hydrochloric acid buffer solution, the processed PI fibers of 5.0g are added in reaction system therewith, by it
After stirring evenly, 2h is reacted under room temperature.The polyethyleneimine for measuring 0.5mL, is added in reaction system, in room temperature condition
Lower progress copolyreaction 30min；0.05g carboxyl-functional multi-walled carbon nano-tubes are weighed, are added in reaction system, in room temperature item
Copolyreaction 6h is carried out under part, is cleaned 3 times with deionized water, and the PI fibers of clean carbon nano tube modified mistake, which are put into air blast, to be done
It is dry in dry baking oven, then it is sealed with valve bag.Static state is carried out to the PI fibers of obtained graphene oxide modified to connect
Feeler is tested, and test result shows that the contact angle of PI fibers is reduced to 71.7 ° by 120.4 °, and the hydrophily of PI fibers obtains pole
It is big to improve.
Example 3
Chopping processing is carried out to PI fibers, makes the length of 5mm, it is then that the PI fibers of 5.0g is ultrasonic in acetone solvent
Cleaning 2h is carried out under environment.It after acetone cleans, is respectively washed 3 times with ethyl alcohol and deionized water, clean PI fibers is put
Enter in blast dry oven and dries；The trishydroxymethylaminomethane for weighing 0.6g is added in 500mL deionized waters, configuration concentration
For the solution of 1.2mg/mL, pH value is measured with acidometer, then uses the hydrochloric acid solution of 1mol/L that trishydroxymethylaminomethane is molten
The pH value of liquid is adjusted to 8.5, obtains trishydroxymethylaminomethane-hydrochloric acid buffer solution；2.0g dopamine powder is weighed to be added to
In trishydroxymethylaminomethane-hydrochloric acid buffer solution, the processed PI fibers of 5.0g are added in reaction system therewith, by it
After stirring evenly, 2h is reacted under room temperature.The polyethyleneimine for measuring 2mL, is added in reaction system, at ambient temperature
Carry out copolyreaction 30min；0.05g carboxyl-functional multi-walled carbon nano-tubes are weighed, are added in reaction system, in room temperature condition
Lower progress copolyreaction 6h, is cleaned 3 times with deionized water, and the PI fibers of clean carbon nano tube modified mistake are put into forced air drying
It is dry in baking oven, then it is sealed with valve bag.Static Contact is carried out to the PI fibers of obtained graphene oxide modified
Angle is tested, and test result shows that the contact angle of PI fibers is reduced to 63.1 ° by 120.4 °, and the hydrophily of PI fibers obtains greatly
It improves.
Example 4
Chopping processing is carried out to PI fibers, makes the length of 1mm, it is then that the PI fibers of 5.0g is ultrasonic in acetone solvent
Cleaning 2h is carried out under environment.It after acetone cleans, is respectively washed 3 times with ethyl alcohol and deionized water, clean PI fibers is put
Enter in blast dry oven and dries；The trishydroxymethylaminomethane for weighing 0.6g is added in 500mL deionized waters, configuration concentration
For the solution of 1.2mg/mL, pH value is measured with acidometer, then uses the hydrochloric acid solution of 1mol/L that trishydroxymethylaminomethane is molten
The pH value of liquid is adjusted to 8.5, obtains trishydroxymethylaminomethane-hydrochloric acid buffer solution；It weighs 2g dopamine powder and is added to three
In hydroxymethyl aminomethane-hydrochloric acid buffer solution, the processed PI fibers of 5.0g are added in reaction system therewith, are stirred
After mixing uniformly, 2h is reacted under room temperature.Measure 2mL polyethyleneimine, be added in reaction system, at ambient temperature into
Row copolyreaction 30min；0.1g carboxyl-functional multi-walled carbon nano-tubes are weighed, are added in reaction system, at ambient temperature
Copolyreaction 6h is carried out, is cleaned 3 times with deionized water, the PI fibers of clean carbon nano tube modified mistake, which are put into forced air drying, to be dried
It is dry in case, then it is sealed with valve bag.Static contact angle is carried out to the PI fibers of obtained graphene oxide modified
Test, test result show that the contact angle of PI fibers is reduced to 61.9 ° by 120.4 °, and the hydrophily of PI fibers is greatly carried
It is high.
Example 5
Chopping processing is carried out to PI fibers, makes the length of 3mm, it is then that the PI fibers of 5.0g is ultrasonic in acetone solvent
Cleaning 2h is carried out under environment.It after acetone cleans, is respectively washed 3 times with ethyl alcohol and deionized water, clean PI fibers is put
Enter in blast dry oven and dries；The trishydroxymethylaminomethane for weighing 0.6g is added in 500mL deionized waters, configuration concentration
For the solution of 1.2mg/mL, pH value is measured with acidometer, then uses the hydrochloric acid solution of 1mol/L that trishydroxymethylaminomethane is molten
The pH value of liquid is adjusted to 8.5, obtains trishydroxymethylaminomethane-hydrochloric acid buffer solution；1.0g dopamine powder is weighed to be added to
In trishydroxymethylaminomethane-hydrochloric acid buffer solution, the processed PI fibers of 5.0g are added in reaction system therewith, by it
After stirring evenly, 2h is reacted under room temperature.The polyethyleneimine for measuring 1mL, is added in reaction system, at ambient temperature
Carry out copolyreaction 30min；0.1g carboxyl-functional multi-walled carbon nano-tubes are weighed, are added in reaction system, in room temperature condition
Lower progress copolyreaction 6h, is cleaned 3 times with deionized water, and the PI fibers of clean carbon nano tube modified mistake are put into forced air drying
It is dry in baking oven, then it is sealed with valve bag.Static Contact is carried out to the PI fibers of obtained graphene oxide modified
Angle is tested, and test result shows that the contact angle of PI fibers is reduced to 67.4 ° by 120.4 °, and the hydrophily of PI fibers obtains greatly
It improves.
Example 6
Chopping processing is carried out to PI fibers, makes the length of 1mm, it is then that the PI fibers of 5.0g is ultrasonic in acetone solvent
Cleaning 2h is carried out under environment.It after acetone cleans, is respectively washed 3 times with ethyl alcohol and deionized water, clean PI fibers is put
Enter in blast dry oven and dries；The trishydroxymethylaminomethane for weighing 0.6g is added in 500mL deionized waters, configuration concentration
For the solution of 1.2mg/mL, pH value is measured with acidometer, then uses the hydrochloric acid solution of 1mol/L that trishydroxymethylaminomethane is molten
The pH value of liquid is adjusted to 8.5, obtains trishydroxymethylaminomethane-hydrochloric acid buffer solution；0.5g dopamine powder is weighed to be added to
In trishydroxymethylaminomethane-hydrochloric acid buffer solution, the processed PI fibers of 5.0g are added in reaction system therewith, by it
After stirring evenly, 2h is reacted under room temperature.The polyethyleneimine for measuring 0.5mL, is added in reaction system, in room temperature condition
Lower progress copolyreaction 30min；1.0g carboxyl-functional multi-walled carbon nano-tubes are weighed, are added in reaction system, in room temperature item
Copolyreaction 6h is carried out under part, is cleaned 3 times with deionized water, and the PI fibers of clean carbon nano tube modified mistake, which are put into air blast, to be done
It is dry in dry baking oven, then it is sealed with valve bag.Static state is carried out to the PI fibers of obtained graphene oxide modified to connect
Feeler is tested, and test result shows that the contact angle of PI fibers is reduced to 72.5 ° by 120.4 °, and the hydrophily of PI fibers obtains pole
It is big to improve.
A kind of technological innovation of the preparation method of PI fiber surfaces carbon nanometer tube with chemical decoration of aforementioned present invention is for existing
Many saving graces are all had for modern technical staff of the same trade.The PI of the carbon nano tube chemical decoration obtained through the invention
Fiber, surface roughness are greatly improved, and hydrophily and specific surface area improve significantly, and the boundary of fiber and matrix resin
Face binding performance enhancing, to be conducive to enhancing modification and the composite material system that PI fibers are preferably applied to thermoplastic
The related fields such as standby.
The length being prepared using the technology of the present invention is the chopped PI fibers of the carbon nano tube chemical decoration of 5mm, when
, when mass fraction is 20wt.% in enhancing modified PC/ABS composite materials, tensile strength is up to 145MPa, bending modulus for it
Up to 7.0GPa or so, the comprehensive mechanical property of PC/ABS is significantly improved.The carbon nanotube chemical prepared using the present invention
The PI fiber reinforced thermolplastic composite materials of modification can be widely applied to electric product, component of machine and other to high-tensile strength
Learn the manufacture for the structure member that performance has higher requirements.
The above is only preferable examples prepared by the present invention, and non-present invention makes any form of restriction, though
So the present invention is disclosed above with preferred embodiments, however, it is not intended to limit the invention people or those skilled in the art,
Without departing from the scope of the present invention, when the technology contents using the disclosure above make a little variation or are modified to
With variation equivalent embodiment, as long as being the content without departing from technical solution of the present invention, according to the technical essence of the invention to
Any simple modification, equivalent change and modification that upper embodiment is done, belong in the range of technical solution of the present invention.
Claims (6)
1. a kind of preparation method of polyimides (PI) fiber surface carbon nanometer tube with chemical decoration, it is characterised in that：Using chemistry
Graft Method is carbon nano tube modified to the progress of PI fiber surfaces, to enhance its surface roughness, reduction surface energy, improve its parent
Aqueous and specific surface area.
2. a kind of preparation method of PI fiber surfaces carbon nanometer tube with chemical decoration as described in claim 1, it is characterised in that：By
Following steps are prepared：(1) PI fibers are cleaned；(2) by the PI fibers and dopamine point by surface cleaning processing
It is dispersed in buffer solution, reacts at room temperature, the surfaces PI form poly-dopamine clad；(3) by a certain amount of polyethyleneimine
It is added in above-mentioned reaction solution, the functionalized PI fibers of surface amino groups is formed by being reacted with poly-dopamine；(4) carboxyl is added
Function multi-walled carbon nano-tube is reacted by carbon nano tube surface carboxyl functional group with PI fiber surface amido functional groups, is obtained
The PI fibers of surface chemical modification multi-walled carbon nanotube.
3. a kind of preparation method of PI fiber surfaces carbon nanometer tube with chemical decoration as claimed in claim 2, it is characterised in that：Step
Suddenly the PI fibers described in (1) are a kind of high-strength and high-modulus and surface inactive organic synthetic fibers, and form can be continuous length
Fiber can also be chopped strand.
4. a kind of preparation method of PI fiber surfaces carbon nanometer tube with chemical decoration as claimed in claim 2, it is characterised in that：Step
Suddenly the buffer solution described in (2) by a concentration of 1.2mg/mL tris solution and a concentration of 1mol/L salt
Acid solution configures, pH value 8.5.A concentration of 1.0~5.0mg/mL of dopamine, reaction temperature are room in reaction solution
Temperature, reaction time 2h.
5. a kind of preparation method of PI fiber surfaces carbon nanometer tube with chemical decoration as claimed in claim 2, it is characterised in that：Step
Suddenly the volume fraction of the polyethyleneimine described in (3) is 1.0~5.0vol.%, and reaction temperature is room temperature, and the reaction time is
30min。
6. a kind of preparation method of PI fiber surfaces carbon nanometer tube with chemical decoration as claimed in claim 2, it is characterised in that：Step
Suddenly the carbon nanotube described in (4) is carboxyl-functional multi-walled carbon nano-tube, and mass fraction is：1.0~2.0wt.%, reaction
Temperature is room temperature, reaction time 6h.
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| CN201810488735.1A CN108660742A (en) | 2018-05-21 | 2018-05-21 | A kind of preparation method of polyimide fiber surface chemical modification carbon nanotube |
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| CN201810488735.1A CN108660742A (en) | 2018-05-21 | 2018-05-21 | A kind of preparation method of polyimide fiber surface chemical modification carbon nanotube |
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