CN105734977A - Carbon fiber emulsion sizing agent based on surface tension matching technology and preparation method - Google Patents

Carbon fiber emulsion sizing agent based on surface tension matching technology and preparation method Download PDF

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Publication number
CN105734977A
CN105734977A CN201610264050.XA CN201610264050A CN105734977A CN 105734977 A CN105734977 A CN 105734977A CN 201610264050 A CN201610264050 A CN 201610264050A CN 105734977 A CN105734977 A CN 105734977A
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carbon fiber
weight portion
epoxy resin
surface tension
bisphenol
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CN201610264050.XA
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CN105734977B (en
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叶明新
沈剑锋
李娜
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Fudan University
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Fudan University
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • 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
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/55—Epoxy resins
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/325—Amines
    • D06M13/332—Di- or polyamines
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • 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
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/53—Polyethers
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/40—Fibres of carbon

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention relates to a carbon fiber emulsion sizing agent based on the surface tension matching technology and a preparation method. The sizing agent is composed of main slurry and surfactant. The main slurry is composed of bisphenol epoxy resin and polypropylene glycol. By adjusting the proportion of bisphenol epoxy resin and polypropylene glycol to be matched with surface tension components of carbon fibers respectively, high compatible wettability is obtained. The sizing agent has special solubility parameters and surface tension. The sizing agent has the advantages of being simple in synthesis, low in cost, stable in performance, convenient to use and free of environment pollution.

Description

A kind of carbon fiber emulsion pasting agent based on surface tension matching technique and preparation method
Technical field
The present invention relates to field of compound material, be specifically related to a kind of carbon fiber emulsion pasting agent according to resinous substrates and carbon fiber surface surface tension matching technique and preparation method thereof.
Background technology
Carbon fiber has a series of excellent properties such as high specific strength, high ratio modulus, carbon fiber enhancement resin base composite material, have excellence shearing strength at intersection cut, shock resistance, damage tolerance, fracture toughness and reliability are superior to traditional composite.But because of carbon fiber poor toughness, rub is poor, producing and in the course of processing, opening can made unclear by snag broken end, easily produce the phenomenon such as lousiness and single wire fracture through mechanical friction so that it is intensity reduces.Due to the existence of lousiness, make matrix resin can not abundant moistening carbon fiber, thus can produce hole in the composite of preparation, affect the mechanical property of composite.It addition, working environment also can be produced impact by lousiness.Therefore, it is necessary to carbon fiber is carried out starching.Sizing agent can form protecting film on the surface of carbon fiber, reduces the phenomenons such as the friction produced in following process process, abrasion and lousiness, and its effect main manifestations is following 4 points: one, has boundling function, improves carbon fiber processing performance so that it is easily processes；Two, similar coupling agent, improves the chemical bond of carbon fiber and interlaminar resin, improves the interface performance of composite；Three, play the effect of lubricant, protect carbon fiber.Reduce mutual friction so that it is damage little as far as possible；Four, serve as wetting agent, improve the wetting property of carbon fiber, it is simple to resin infiltrates, reduce the preparation time of composite, improve product quality.Therefore, in order to improve the wettability of carbon fiber and interlaminar resin, the research that surface can be affected by carbon fibre surface energy and sizing agent need to be carried out.
According to surface tension matching theory, liquid there will be two kinds of phenomenons when the surface of solids contacts with each other: when the cohesiveness between fluid molecule is less than adhesive force between fluid molecule and molecular solids, liquid can automatic drawout on a solid surface, this shows that this liquid can moistening solid；When cohesiveness between fluid molecule is more than adhesive force between fluid molecule and molecular solids, liquid will not drawout automatically on a solid surface, and spherical drop can be formed, this shows that this liquid can not moistening solid.Two stages can be divided into: first stage during carbon fiber saturated ring epoxy resins, owing under capillarity, the weight of the resin of moistening carbon fiber is little, being difficult to become resistance, now epoxy resin mainly rapid moistening fiber under the additonal pressure effect of capillary tube, makes carbon fiber weight increase sharply；Second stage, increasing with weight resin, the weight that this part increases then becomes the resistance of the further adsorbent resin of carbon fiber, and resistance becomes larger, thus the speed of PAN-ACF resin is slack-off gradually, the final combined effect at the two is issued to adsorption equilibrium, and the weight of carbon fiber almost no longer changes.Theoretical according to Thermodynamic Basis, when sizing agent and carbon fiber surface tension difference between the two more hour, in theory, com-patibilising effect is more good.This point can be stated by below equation:
σ s l = σ s + σ l - 2 ( σ s d · σ l d + σ s p · σ l p ) = σ s d + σ s p + σ l d + σ l p - 2 ( σ s d · σ l d + σ s p · σ l p )
σ s l = ( σ l d σ l p + 1 ) · σ l p + ( σ s d σ s p + 1 ) · σ s p - 2 ( σ l d σ l p · σ s d σ s p + 1 ) σ l p · σ s p = ( σ s p σ s d σ s p + 1 - σ l p σ l d σ l p + 1 ) 2 + 2 σ s p · σ l p ( σ l d σ l p + 1 σ s d σ s p + 1 - σ l d σ l p · σ s d σ s p - 1 )
Wherein d represents capillary dispersive part, the corresponding capillary polar portion of p；S represents fibrous material, l correspondence solvent.For the left-half of formula, whenWhen being 0；For the right half part of formula, whenShi Keneng obtains minima.Therefore, when sizing agent and carbon fiber surface tension can not essentially equal, both surface tension dispersive component and polar component ratio closer to time, its wellability is more good.By this principle, when known carbon fiber surface surface tension, it is possible to design corresponding sizing agent component thus meeting its good wellability requirement.
At present, due to epoxy resin widely using in carbon fibre composite preparation process, existing carbon fiber sizing agent mostly is epoxy resin sizing agent (such as CN101886336, CN1271276, CN101858037, CN102828416, CN102206919, CN102212967, CN101858038, CN101736593, CN101845755 and CN101880967), to realize well compatible between sized fiber with epoxy resin and to mate.But for epoxy resin and stromal surface tension force with infiltrating mate, it is necessary to be modified thus being achieved by suitable approach.
Summary of the invention
It is an object of the invention to provide that a kind of cost is low, the carbon fiber emulsion pasting agent of stable performance and preparation method thereof.
A kind of carbon fiber emulsion pasting agent based on surface tension matching technique, mainly include main slurry and auxiliary agent, main slurry is made up of bisphenol-type epoxy resin and polypropylene glycol, described auxiliary agent is using ammonium ion as the anionic surfactant to ion, nonionic surfactant, or both mixture.
Further, described bisphenol-type epoxy resin includes bisphenol A type epoxy resin and bisphenol f type epoxy resin, comprises bisphenol group and hydroxyl in its strand, and one or both ends end group is epoxide group, and described polypropylene glycols weight range is 4000-10000.
Further, described main slurry is bisphenol A type epoxy resin E42, epoxy resin F-44 and polypropylene glycol, and described auxiliary agent is diethylenetriamine.
Further, wherein main slurry is 10-30 weight portion, it is preferred to 20-25 weight portion, and auxiliary agent is 0.1-0.5 weight portion, it is preferred to 0.2-0.4 weight portion.
Further, be mainly made up of following weight portion: the polypropylene glycol of epoxy resin F-44,5-10 weight portion of bisphenol A type epoxy resin E42,4-6 weight portion of 9-11 weight portion, 0.1-0.5 weight portion diethylenetriamine.
Further, the solubility parameters of described carbon fiber emulsion pasting agent ranges for: 10-25MPa1/2, and the surface tension when 25 DEG C is 20-45mN/m, and surface tension polarity phase and nonpolar phase ratio are at 0.2-1.6.
Further, it is provided that the preparation method of a kind of carbon fiber emulsion pasting agent based on surface tension matching technique, it is characterised in that, (1) main slurry is dissolved in dichloromethane, at 0-20 DEG C, react 10～30 hours, obtain modified epoxy solution；(2) in modified epoxy solution, add deionized water, dichloromethane is distilled off；(3) in modified epoxy aqueous solution, auxiliary agent, high speed shear 1～6 hour at temperature is 60-100 DEG C are then added.
Further, wherein the dichloromethane in (1st) step is 10-20 weight portion, and the deionized water in (2nd) step is 10-20 weight portion.
Further, the shearing rotating speed of described high speed shear is 5000-15000rpm.
Further, described sizing agent is the carbon filament of 0.3-0.8 for surface tension polarity phase and nonpolar phase ratio.
According to technique scheme, the beneficial effect comprise that the selection by component and ratio and the optimization of preparation method, mate respectively with the surface tension component of carbon fiber, thus obtaining high compatible wellability.Sizing agent of the present invention has specific solubility parameters and surface tension, can suppress carbon fiber generation of lousiness in the course of processing, improves carbon fiber wearability, can also improve the interfacial adhesion of carbon fiber and matrix resin simultaneously.The present invention has that synthesis is simple, cost is low, stable performance, advantage easy to use, free from environmental pollution.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1: embodiment 2 is the field emission scanning electron microscope figure of carbon fiber after starching processes；
Fig. 2: embodiment 2 is the wellability curve of carbon fiber and resin after starching processes；
Fig. 3: embodiment 3 is the field emission scanning electron microscope figure of carbon fiber after starching processes；
Fig. 4: embodiment 3 is the wellability curve of carbon fiber and resin after starching processes.
Detailed description of the invention
Embodiment 1
(1) it is the carbon filament of 0.35 for surface tension polarity phase and nonpolar phase ratio, by 1000 grams of bisphenol A type epoxy resin E42,500 grams of epoxy resin F-44,800 grams of polypropylene glycols (molecular weight 10000), it is dissolved in 1500 grams of dichloromethane, react 16 hours at 10 DEG C, obtain modified epoxy solution；(2) in modified epoxy solution, add 1500 grams of deionized waters, dichloromethane is distilled off；(3) adding auxiliary agent diethylenetriamine 30 grams in modified epoxy aqueous solution, shearing rotating speed is 10000rpm, and temperature is high speed shear 3 hours at 65 DEG C, namely prepares the carbon fiber emulsion pasting agent of coupling.
Embodiment 2
(1) it is the carbon filament of 0.76 for surface tension polarity phase and nonpolar phase ratio, by 1000 grams of bisphenol A type epoxy resin E42,500 grams of epoxy resin F-44,600 grams of polypropylene glycols (molecular weight 20000), it is dissolved in 1000 grams of dichloromethane, react 16 hours at 0 DEG C, obtain modified epoxy solution；(2) in modified epoxy solution, add 1500 grams of deionized waters, dichloromethane is distilled off；(3) adding auxiliary agent diethylenetriamine 30 grams in modified epoxy aqueous solution, shearing rotating speed is 10000rpm, and temperature is high speed shear 2 hours at 95 DEG C.Namely the carbon fiber emulsion pasting agent of coupling is prepared.Fig. 1 is the present embodiment field emission scanning electron microscope figure of carbon fiber after starching processes.Fig. 2 is the present embodiment wellability curve of carbon fiber and resin after starching processes.
Embodiment 3
(1) it is the carbon filament of 0.53 for surface tension polarity phase and nonpolar phase ratio, by 1000 grams of bisphenol A type epoxy resin E42,500 grams of epoxy resin F-44,500 grams of polypropylene glycols (molecular weight 10000), it is dissolved in 1000 grams of dichloromethane, react 16 hours at 5 DEG C, obtain modified epoxy solution；(2) in modified epoxy solution, add 1500 grams of deionized waters, dichloromethane is distilled off；(3) adding auxiliary agent diethylenetriamine 30 grams in modified epoxy aqueous solution, shearing rotating speed is 10000rpm, and temperature is high speed shear 3 hours at 75 DEG C.Namely carbon fiber emulsion pasting agent is prepared.Fig. 3 is the present embodiment field emission scanning electron microscope figure of carbon fiber after starching processes.Fig. 4 is the present embodiment wellability curve of carbon fiber and resin after starching processes.
Embodiment 4
(1) it is the carbon filament of 0.72 for surface tension polarity phase and nonpolar phase ratio, by 1000 grams of bisphenol A type epoxy resin E42,500 grams of epoxy resin F-44,1000 grams of polypropylene glycols (molecular weight 8000), it is dissolved in 1000 grams of dichloromethane, react 16 hours at 10 DEG C, obtain modified epoxy solution；(2) in modified epoxy solution, add 1500 grams of deionized waters, dichloromethane is distilled off；(3) auxiliary agent diethylenetriamine 30 grams in modified epoxy aqueous solution, shearing rotating speed is 10000rpm, and temperature is high speed shear 2 hours at 85 DEG C.Namely carbon fiber emulsion pasting agent is prepared.
The epoxy resin-base composite material mechanical property such as following table obtained in embodiment 1-4:
In sum, embodiments provide a kind of carbon fiber emulsion pasting agent based on surface tension matching technique and preparation method, this sizing agent has specific solubility parameters and surface tension, can suppress carbon fiber generation of lousiness in the course of processing, improves carbon fiber wearability, can also improve the interfacial adhesion of carbon fiber and matrix resin simultaneously.The present invention has that synthesis is simple, cost is low, stable performance, advantage easy to use, free from environmental pollution.
The above; being only the present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto, any those familiar with the art is in the technical scope that the invention discloses; the change that can readily occur in or replacement, all should be encompassed within protection scope of the present invention.

Claims (10)

1. the carbon fiber emulsion pasting agent based on surface tension matching technique, it is characterized in that, mainly include main slurry and auxiliary agent, main slurry is made up of bisphenol-type epoxy resin and polypropylene glycol, described auxiliary agent is using ammonium ion as the anionic surfactant to ion, nonionic surfactant, or both mixture.
2. carbon fiber emulsion pasting agent as claimed in claim 1, it is characterized in that, described bisphenol-type epoxy resin includes bisphenol A type epoxy resin and bisphenol f type epoxy resin, its strand comprises bisphenol group and hydroxyl, one or both ends end group is epoxide group, and described polypropylene glycols weight range is 4000-10000.
3. carbon fiber emulsion pasting agent as claimed in claim 2, it is characterised in that described main slurry is bisphenol A type epoxy resin E42, epoxy resin F-44 and polypropylene glycol, and described auxiliary agent is diethylenetriamine.
4. carbon fiber emulsion pasting agent as described in any claim in claim 1-3, it is characterised in that wherein main slurry is 10-30 weight portion, it is preferred to 20-25 weight portion, and auxiliary agent is 0.1-0.5 weight portion, it is preferred to 0.2-0.4 weight portion.
5. carbon fiber emulsion pasting agent as claimed in claim 3, it is characterized in that, be mainly made up of following weight portion: the polypropylene glycol of epoxy resin F-44,5-10 weight portion of bisphenol A type epoxy resin E42,4-6 weight portion of 9-11 weight portion, 0.1-0.5 weight portion diethylenetriamine.
6. carbon fiber emulsion pasting agent as claimed in claim 5, it is characterised in that the solubility parameters of described carbon fiber emulsion pasting agent ranges for: 10-25MPa1/2, the surface tension when 25 DEG C is 20-45mN/m, and surface tension polarity phase and nonpolar phase ratio are at 0.2-1.6.
7. the preparation method of the carbon fiber emulsion pasting agent based on surface tension matching technique as described in claim 1-6, it is characterized in that, main slurry is dissolved in dichloromethane by (1), at 0-20 DEG C, react 10～30 hours, obtain modified epoxy solution；(2) in modified epoxy solution, add deionized water, dichloromethane is distilled off；(3) in modified epoxy aqueous solution, auxiliary agent, high speed shear 1～6 hour at temperature is 60-100 DEG C are then added.
8. preparation method as claimed in claim 7, it is characterised in that wherein the dichloromethane in (1st) step is 10-20 weight portion, and the deionized water in (2nd) step is 10-20 weight portion.
9. preparation method as claimed in claim 7 or 8, it is characterised in that the shearing rotating speed of described high speed shear is 5000-15000rpm.
10. preparation method as described in any claim in claim 7-9, it is characterised in that described sizing agent is the carbon filament of 0.3-0.8 for surface tension polarity phase and nonpolar phase ratio.
CN201610264050.XA 2016-04-26 2016-04-26 A kind of carbon fiber emulsion pasting agent and preparation method based on surface tension matching technique Expired - Fee Related CN105734977B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6957070B1 (en) * 2021-06-04 2021-11-02 竹本油脂株式会社 Treatment agent for synthetic fibers and synthetic fibers
CN114481618A (en) * 2022-03-21 2022-05-13 江苏恒神股份有限公司 Carbon fiber sizing agent for water-based treatment and preparation method and application thereof
JP2023088243A (en) * 2021-12-14 2023-06-26 日本エイアンドエル株式会社 Composition for bundling fibers, and resin-impregnated fiber, thermoplastic resin composition, and molded article using the same

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CN102828416A (en) * 2012-09-20 2012-12-19 金发科技股份有限公司 Emulsion carbon fiber sizing agent as well as preparation method and application of sizing agent
JP2013133559A (en) * 2011-12-27 2013-07-08 Toray Ind Inc Sizing agent-applied carbon fiber and method for producing sizing agent-applied carbon fiber
CN104562693A (en) * 2013-10-11 2015-04-29 中国石油化工股份有限公司 A carbon fiber composite emulsion sizing agent having low surface tension and high particle size stability and a preparing method thereof

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JP2013133559A (en) * 2011-12-27 2013-07-08 Toray Ind Inc Sizing agent-applied carbon fiber and method for producing sizing agent-applied carbon fiber
CN102828416A (en) * 2012-09-20 2012-12-19 金发科技股份有限公司 Emulsion carbon fiber sizing agent as well as preparation method and application of sizing agent
CN104562693A (en) * 2013-10-11 2015-04-29 中国石油化工股份有限公司 A carbon fiber composite emulsion sizing agent having low surface tension and high particle size stability and a preparing method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6957070B1 (en) * 2021-06-04 2021-11-02 竹本油脂株式会社 Treatment agent for synthetic fibers and synthetic fibers
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JP2023088243A (en) * 2021-12-14 2023-06-26 日本エイアンドエル株式会社 Composition for bundling fibers, and resin-impregnated fiber, thermoplastic resin composition, and molded article using the same
JP7312888B2 (en) 2021-12-14 2023-07-21 日本エイアンドエル株式会社 Fiber bundling composition, resin-impregnated fiber, thermoplastic resin composition, molded article using the same
CN114481618A (en) * 2022-03-21 2022-05-13 江苏恒神股份有限公司 Carbon fiber sizing agent for water-based treatment and preparation method and application thereof
CN114481618B (en) * 2022-03-21 2023-10-24 江苏恒神股份有限公司 Carbon fiber sizing agent for water-based treatment, and preparation method and application thereof

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