CN106868865A - A kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent - Google Patents
A kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent Download PDFInfo
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- CN106868865A CN106868865A CN201710056915.8A CN201710056915A CN106868865A CN 106868865 A CN106868865 A CN 106868865A CN 201710056915 A CN201710056915 A CN 201710056915A CN 106868865 A CN106868865 A CN 106868865A
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- carbon fiber
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- alcamines
- graft copolymerization
- sizing agent
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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
- 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
- D06M13/368—Hydroxyalkylamines; Derivatives thereof, e.g. Kritchevsky bases
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- 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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- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/40—Reduced friction resistance, lubricant properties; Sizing compositions
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
A kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent, a kind of method for being related to carbon fiber surface sizing agent modified.The present invention is the technical problem low in order to solve the interface bond strength of current fibre reinforced vinyl ester resin or unsaturated polyester resin composite material.The present invention：First, alcamines modifier solution is configured；2nd, carbon fiber surface modification.The inventive method is simple and easy to apply, and chemical graft is directly carried out on carbon fiber surface sizing agent, will not damage carbon fiber intensity in itself, and modified sizing agent may also operate as protecting the effect of carbon fiber.The interface shear strength of composite prepared by modified carbon fiber and unsaturated-resin and every mechanical property are all significantly improved.
Description
Technical field
The present invention relates to a kind of method that carbon fiber surface sizing agent is modified.
Background technology
Vinyl ester resin (VE) is a kind of thermosetting tree obtained from being reacted with unsaturated small molecule by epoxy resin
Fat.Vinyl ester resin had both remained the basic segment of epoxy resin, had adhered to the good characteristic of epoxy resin, and in strand
In introduce unsaturated double-bond, the good process performance with unsaturated polyester resin.So vinyl ester resin is in mechanical property
Energy, resistance to elevated temperatures, resistance to chemical corrosion and curing performance, processability and processing characteristics aspect have outstanding table
It is existing, it is obtained in fields such as automobile, physical culture, health cares and is widely applied.The curing mechanism of vinyl ester resin and insatiable hunger
It is identical with polyester resin, be double bond in molecular resin and diluent styrene double bond between cross moulding, hardening time is short,
Short molding cycle, disclosure satisfy that the demand of the products such as composite material automobile parts batch production.
Starching is a procedure of indispensability in carbon fiber preparation process, the purpose is to draw between carbon fiber and matrix resin
Enter polymer transitional interlayer, that is, coat one layer of polymeric Protection glue.May be used also while carbon fiber is improved with resin wellability
To play a part of to protect fiber.At present, the sizing agent of carbon fiber surface is generally epoxy type sizing agent, itself and vinyl ester resin
Or the molecular structure of unsaturated polyester resin is different, therefore curing mechanism is also different.The open loop that epoxy resin passes through epoxide group
Crosslinking.Interface which results in fibre reinforced vinyl ester resin or unsaturated polyester resin composite material lacks chemical bond
Connection so that interface turn into fibre reinforced Vinyl Ester Resin Composites weak link.
The interface of carbon fiber enhancement resin base composite material refers to the 3D region around reinforcing fiber, is had different from tree
The specific properties of aliphatic radical body and fiber, are the third phases of composite.Although interface is in fiber-reinforced resin matrix compound material
In mass fraction less than 1%, but performance to composite plays vital effect.When being acted on by external force, remove
Outside reinforcing fiber and matrix stress, interface also plays an important role, and only carries out stress transmission by interface, can just make
Fiber and matrix stress equiblibrium mass distribution, therefore interfacial property and state directly affect the comprehensive mechanical property of composite and hot
Energy.The interphase interaction of matrix and reinforcement is not enough or it is unfavorable to be all excessively, and interaction deficiency can not obtain good knot
Close intensity；It is excessive then interfacial brittle can be caused, fiber is damaged, reduce composite material strength and impact flexibility.Therefore, interface
Important component of the research as fibre reinforced vinyl ester resin or unsaturated polyester resin composite material design studies,
This technology is also rarely reported both at home and abroad.
The content of the invention
The present invention is to solve current fibre reinforced vinyl ester resin or unsaturated polyester resin composite material
The low technical problem of interface bond strength, and provide a kind of side of alcamines solution graft copolymerization modified carbon fiber surface size agent
Method.
A kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent of the invention is to carry out according to the following steps
's：
First, modifier solution is configured：Modifying agent is dissolved in solvent, modifier solution is obtained；Described modifier solution
Mass concentration be 0.5%~5.0%；Described modifying agent is the alcohol containing amino and unsaturated double-bond simultaneously in molecular structure
Amine organic molecule；
2nd, carbon fiber surface modification：Modifier solution prepared by step one is adjusted to 50 DEG C~100 DEG C, with 50 DEG C~
100 DEG C of modifier solution carries out surface to carbon fiber and is modified, the carbon fiber rinsed after surface treatment with water, is 50 DEG C in temperature
0.5h~6h is dried under conditions of~100 DEG C, the carbon fiber after surface size agent grafting modification is obtained；Described carbon fiber
Be the unidirectional carbon with epoxy type sizing agent, the carbon-fiber cloth with epoxy type sizing agent, with epoxy type sizing agent
Fibrofelt or the chopped carbon fiber with epoxy type sizing agent.
Modifying agent of the invention and the principle of the sizing agent chemical graft of carbon fiber surface be amino in modifying agent with it is upper
Epoxide group in slurry agent chemically reacts, so as to introduce unsaturated double-bond in carbon fiber surface.The unsaturated double-bond can be with
Double bond in vinyl ester resin or unsaturated polyester resin strand is chemically crosslinked in the curing process, so as in carbon
Chemical bond connection is formed between fiber and resin matrix, hence it is evident that improve the interface bond strength of composite.
The inventive method is simple and easy to apply, and chemical graft is directly carried out on carbon fiber surface sizing agent, will not damage carbon fine
The intensity of dimension itself.Every mechanical property of modified carbon fiber/unsaturated-resin interface shear strength and its composite
All it is significantly improved.
Grafting modification of the invention
Without carrying out destarch treatment to carbon fiber, chemical graft occurs between carbon fiber surface sizing agent and modifying agent,
Reaction principle is the chemical reaction of the epoxide group in amino and sizing agent molecule chain in modifier molecules, and reaction equation is shown in Fig. 2.
The present invention has advantages below relative to traditional carbon fiber surface modification method：
(1) processing method is simple and easy to apply, without carrying out destarch treatment to carbon fiber, to the performance undamaged wound of carbon fiber；
(2) retain the sizing agent of carbon fiber surface, the wellability of carbon fiber and resin is improved, while playing protection carbon fiber
Effect；
(3) unsaturated double-bond is introduced in carbon fiber surface, in carbon fiber and vinyl ester resin or unsaturated polyester resin
Between form covalent bond connection, it is possible to increase the mechanical property of composite.
Brief description of the drawings
Fig. 1 is the method schematic diagram of deflector roll traction in the specific embodiment of the invention four, and 1 is without present embodiment treatment
Fiber roll, 2 is fiber, and 3 is deflector roll, and 4 is washing equipment, and 5 is modifier solution, and 6 is drying equipment, and 7 is through this embodiment party
The treated fiber roll of formula；
Fig. 2 is the chemical equation that the epoxide group in amino and sizing agent in modifying agent of the invention occurs；
Fig. 3 is the SEM figures for testing the carbon fiber in before modified；
Fig. 4 is the SEM figures of the carbon fiber for testing modified in.
Specific embodiment
Specific embodiment one：Present embodiment is a kind of side of alcamines solution graft copolymerization modified carbon fiber surface size agent
Method, is specifically carried out according to the following steps：
First, modifier solution is configured：Modifying agent is dissolved in solvent, modifier solution is obtained；Described modifier solution
Mass concentration be 0.5%~5.0%；Described modifying agent is the alcohol containing amino and unsaturated double-bond simultaneously in molecular structure
Amine organic molecule；
2nd, carbon fiber surface modification：Modifier solution prepared by step one is adjusted to 50 DEG C~100 DEG C, with 50 DEG C~
100 DEG C of modifier solution carries out surface to carbon fiber and is modified, the carbon fiber rinsed after surface treatment with water, is 50 DEG C in temperature
0.5h~6h is dried under conditions of~100 DEG C, the carbon fiber after surface size agent grafting modification is obtained；Described carbon fiber
Be the unidirectional carbon with epoxy type sizing agent, the carbon-fiber cloth with epoxy type sizing agent, with epoxy type sizing agent
Fibrofelt or the chopped carbon fiber with epoxy type sizing agent.
It is continuous fiber that unidirectional carbon fiber peacekeeping with epoxy type sizing agent has the carbon-fiber cloth of epoxy type sizing agent.
Specific embodiment two：This specific embodiment from unlike specific embodiment one：Dividing described in step one
Hydramine organic micromolecule in minor structure simultaneously containing amino and unsaturated double-bond is 4- amino -2- butene-1-ols and 1- ammonia
One or two mixture in base-3- butene-2 -ol.Other are identical with specific embodiment one.
Specific embodiment three：This specific embodiment from unlike specific embodiment one：It is molten described in step one
Agent is water or organic solvent.Other are identical with specific embodiment one.
Specific embodiment four：As described in Figure 1, this specific embodiment from unlike specific embodiment one：Work as step
When carbon fiber described in rapid two is continuous fiber, table is carried out to carbon fiber with 50 DEG C~100 DEG C of modifier solution in step 2
The modified method in face is：
Be immersed in carbon fiber in 50 DEG C~100 DEG C of modifier solution by the method drawn by deflector roll, and treatment 5min~
30min.Other are identical with specific embodiment one.
Present embodiment is suitable for the on-line continuous treatment of continuous carbon fibre, and automaticity is higher, can effectively reduce
The phenomenon such as carbon fiber fluffing, fracture of wire caused by surface treatment, improves the convergence of modified carbon fiber.
Specific embodiment five：This specific embodiment from unlike specific embodiment one：When described in step 2
When carbon fiber is chopped carbon fiber with epoxy type sizing agent or the fibrofelt with epoxy type sizing agent, with 50 in step 2
DEG C~100 DEG C of modifier solution carries out the modified method in surface to carbon fiber and is：
Carbon fiber is totally immersed in 50 DEG C~100 DEG C of modifier solution, 5min~30min is soaked.Other and tool
Body implementation method one is identical.
Specific embodiment six：This specific embodiment from unlike specific embodiment one：With 50 DEG C in step 2
~100 DEG C of modifier solution carries out using ultrasonically treated while surface is modified to carbon fiber.Other and specific embodiment
One is identical.
Specific embodiment seven：This specific embodiment from unlike specific embodiment three：Described in step
Organic solvent is the mixture of one or more in alcohol, ether and ketone.Other are identical with specific embodiment three.
Effect of the invention is verified by tests below：
Experiment one：This experiment is a kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent, is specifically pressed
What following steps were carried out：
First, modifier solution is configured：Modifying agent is soluble in water, obtain modifier solution；Described modifier solution
Mass concentration is 1.0%；Described modifying agent is 4- amino -2- butene-1-ols；
2nd, carbon fiber surface modification：Modifier solution prepared by step one is heated to be 80 DEG C, the modifying agent with 80 DEG C is molten
Liquid carries out surface to carbon fiber and is modified, the carbon fiber rinsed after surface treatment with water, and 4h is dried under conditions of being 60 DEG C in temperature,
Obtain the carbon fiber after surface size agent grafting modification；Described carbon fiber is the unidirectional carbon fiber with epoxy type sizing agent
Dimension.
The modified method in surface is carried out to carbon fiber with 80 DEG C of modifier solution in step 2 is：Drawn by deflector roll
Be immersed in carbon fiber in 80 DEG C of modifier solution by method, processes 10min.
Elemental composition analysis is carried out to the carbon fiber and modified carbon fiber in experiment one before modified respectively, as a result as schemed
1, it can be seen that modified carbon fiber N content substantially increases, because the amino in modifying agent contains N element, illustrates
Modified success.
Table 1
Analysis of Surface Topography is carried out to the carbon fiber and modified carbon fiber in experiment one before modified respectively, Fig. 3 is to change
Property before carbon fiber SEM figures, Fig. 4 is the SEM figures of modified carbon fiber, as can be seen from Figure modified carbon fiber surface
Pattern does not have significant change, illustrates the modified structure for not destroying carbon fiber itself of this experiment.
Carbon fiber and vinyl ester resin after a surface size agent grafting modification will be tested and prepare composite, led to
Cross micro- unsticking method to characterize the interface shear strength of composite, interface shear strength is carried after finding carbon fiber surface modification
It is high by more than 50%.
Claims (7)
1. a kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent, it is characterised in that alcamines solution graft copolymerization changes
The method of property carbon fiber surface sizing agent is carried out according to the following steps：
First, modifier solution is configured：Modifying agent is dissolved in solvent, modifier solution is obtained；The matter of described modifier solution
Amount concentration is 0.5%~5.0%；Described modifying agent is the alcamines containing amino and unsaturated double-bond simultaneously in molecular structure
Organic molecule；
2nd, carbon fiber surface modification：Modifier solution prepared by step one is adjusted to 50 DEG C~100 DEG C, with 50 DEG C~100 DEG C
Modifier solution carbon fiber is carried out surface be modified, with water rinse surface treatment after carbon fiber, temperature be 50 DEG C~100
0.5h~6h is dried under conditions of DEG C, the carbon fiber after surface size agent grafting modification is obtained；Described carbon fiber is tool
There are unidirectional carbon, the carbon-fiber cloth with epoxy type sizing agent, the fibre with epoxy type sizing agent of epoxy type sizing agent
Dimension felt or the chopped carbon fiber with epoxy type sizing agent.
2. a kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent according to claim 1, its feature
Be the hydramine organic micromolecule in the molecular structure described in step one simultaneously containing amino and unsaturated double-bond for 4- amino-
One or two mixture in 2- butene-1-ols and 1- amino-3- butene-2 -ol.
3. a kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent according to claim 1, its feature
It is that the solvent described in step one is water or organic solvent.
4. a kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent according to claim 1, its feature
It is that, when the carbon fiber described in step 2 is continuous fiber, the modifier solution in step 2 with 50 DEG C~100 DEG C is fine to carbon
Dimension carries out the modified method in surface：The modifying agent that carbon fiber is immersed in 50 DEG C~100 DEG C by the method drawn by deflector roll is molten
In liquid, 5min~30min is processed.
5. a kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent according to claim 1, its feature
It is when the carbon fiber described in step 2 is the chopped carbon fiber with epoxy type sizing agent or the fibre with epoxy type sizing agent
The modified method in surface is carried out to carbon fiber with 50 DEG C~100 DEG C of modifier solution during dimension felt, in step 2 is：By carbon fiber
It is totally immersed in 50 DEG C~100 DEG C of modifier solution, soaks 5min~30min.
6. a kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent according to claim 1, its feature
Be carbon fiber is carried out with 50 DEG C~100 DEG C of modifier solution in step 2 surface it is modified while using ultrasonically treated.
7. a kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent according to claim 3, its feature
It is that the organic solvent described in step one is the mixture of one or more in alcohol, ether and ketone.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102926204A (en) * | 2012-11-16 | 2013-02-13 | 金发科技股份有限公司 | Sizing agent for emulsion type carbon fiber, preparation method and application of sizing agent |
| JP2014074255A (en) * | 2012-09-14 | 2014-04-24 | Toray Ind Inc | Siding agent application carbon fiber, production method of siding agent application carbon fiber, prepreg, and carbon fiber reinforced composite material |
| JP2014108990A (en) * | 2012-12-03 | 2014-06-12 | Mitsubishi Rayon Co Ltd | Carbon fiber-reinforced polypropylene resin composition |
| CN104195824A (en) * | 2014-09-15 | 2014-12-10 | 哈尔滨工业大学 | Carbon fiber surface modification method |
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2017
- 2017-01-24 CN CN201710056915.8A patent/CN106868865B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014074255A (en) * | 2012-09-14 | 2014-04-24 | Toray Ind Inc | Siding agent application carbon fiber, production method of siding agent application carbon fiber, prepreg, and carbon fiber reinforced composite material |
| CN102926204A (en) * | 2012-11-16 | 2013-02-13 | 金发科技股份有限公司 | Sizing agent for emulsion type carbon fiber, preparation method and application of sizing agent |
| JP2014108990A (en) * | 2012-12-03 | 2014-06-12 | Mitsubishi Rayon Co Ltd | Carbon fiber-reinforced polypropylene resin composition |
| CN104195824A (en) * | 2014-09-15 | 2014-12-10 | 哈尔滨工业大学 | Carbon fiber surface modification method |
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