CN106868865B - 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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- CN106868865B CN106868865B CN201710056915.8A CN201710056915A CN106868865B CN 106868865 B CN106868865 B CN 106868865B CN 201710056915 A CN201710056915 A CN 201710056915A CN 106868865 B CN106868865 B CN 106868865B
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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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Abstract
A kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent is related to a kind of method that carbon fiber surface sizing agent is modified.The present invention is the technical problem low for the interface bond strength for solving current fibre reinforced vinyl ester resin or unsaturated polyester resin composite material.The present invention: one, alcamines modifier solution is configured；Two, carbon fiber surface modification.The method of the present invention is simple and easy, and chemical graft is directly carried out on carbon fiber surface sizing agent, will not damage the intensity of carbon fiber itself, and modified sizing agent can also play the role of protecting carbon fiber.The interface shear strength and every mechanical property of modified carbon fiber and the composite material of unsaturated-resin preparation are all significantly improved.
Description
Technical field
The present invention relates to a kind of modified methods of carbon fiber surface sizing agent.
Background technique
Vinyl ester resin (VE) is a kind of thermosetting property tree as obtained from epoxy resin and unsaturated small molecule reaction
Rouge.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, with unsaturated polyester resin good process performance.So vinyl ester resin is in mechanical property
There is outstanding table in terms of energy, high temperature resistance, resistance to chemical corrosion and curing performance, processability and processing performance
It is existing, it is all widely used in fields such as automobile, sport, health cares.The curing mechanism of vinyl ester resin and insatiable hunger
It is identical with polyester resin, it is the cross moulding between the double bond in molecular resin and the double bond of diluent styrene, curing time is short,
Short molding cycle can satisfy the demand of the product batches such as composite material automobile parts production.
Starching is a procedure indispensable in carbon fiber preparation process, and the purpose is to draw between carbon fiber and matrix resin
Enter polymer transitional interlayer, i.e. coating one layer of polymeric protective glue.May be used also while improving carbon fiber and resin infiltration
To play the role of protecting fiber.Currently, the sizing agent of carbon fiber surface is mostly epoxy type sizing agent, with 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 epoxy group
Crosslinking.Which results in the interfaces of fibre reinforced vinyl ester resin or unsaturated polyester resin composite material to lack chemical bond
Connection so that interface become 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, has and is different from tree
The specific properties of aliphatic radical body and fiber are the third phases of composite material.Although interface is mutually in fiber-reinforced resin matrix compound material
In mass fraction played a crucial role less than 1%, but to the performance of composite material.When by external force, remove
Outside reinforcing fiber and matrix stress, interface also plays an important role, and only carries out stress transfer 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 material and hot
Energy.Interact between matrix and reinforcement it is insufficient or excessive be all it is unfavorable, interaction deficiency cannot obtain good knot
Close intensity；It is excessive then will lead to interfacial brittle, fiber is damaged, composite material strength and impact flexibility are reduced.Therefore, interface
Research becomes the important component of fibre reinforced vinyl ester resin or unsaturated polyester resin composite material design studies,
This technology is also rarely reported both at home and abroad.
Summary 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
:
One, it configures modifier solution: modifying agent being dissolved in solvent, modifier solution is obtained；The modifier solution
Mass concentration be 0.5%~5.0%；The modifying agent is the alcohol containing amino and unsaturated double-bond simultaneously in molecular structure
Amine small organic molecule；
Two, carbon fiber surface modification: by step 1 prepare modifier solution be adjusted to 50 DEG C~100 DEG C, with 50 DEG C~
100 DEG C of modifier solution carries out the carbon fiber that surface is modified, after being rinsed with water surface treatment to carbon fiber, is 50 DEG C in temperature
Dry 0.5h~6h, the carbon fiber after obtaining surface size agent grafting modification under conditions of~100 DEG C；The carbon fiber
For the unidirectional carbon fiber with epoxy type sizing agent, the carbon-fiber cloth with epoxy type sizing agent, there is epoxy type sizing agent
Fibrofelt or chopped carbon fiber with epoxy type sizing agent.
The principle of the sizing agent chemical graft of modifying agent and carbon fiber surface of the invention be amino in modifying agent with it is upper
Epoxy group in slurry agent chemically reacts, 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, thus in carbon
Chemistry key connection is formed between fiber and resin matrix, hence it is evident that improve the interface bond strength of composite material.
The method of the present invention is simple and easy, and chemical graft is directly carried out on carbon fiber surface sizing agent, will not damage carbon fiber
Tie up the intensity of itself.Every mechanical property of modified carbon fiber/unsaturated-resin interface shear strength and its composite material
All it is significantly improved.
Grafting modification of the invention
Without carrying out destarch processing to carbon fiber, chemical graft occurs between carbon fiber surface sizing agent and modifying agent,
Reaction principle is the chemical reaction of the epoxy group in amino and sizing agent molecule chain in modifier molecules, and reaction equation is shown in Fig. 2.
The present invention has the advantage that relative to traditional carbon fiber surface modification method
(1) processing method is simple and easy, without carrying out destarch processing to carbon fiber, to the performance undamaged wound of carbon fiber；
(2) sizing agent for retaining carbon fiber surface, improves the wellability of carbon fiber and resin, 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 key connection, can be improved the mechanical property of composite material.
Detailed description of the invention
Fig. 1 is the method schematic diagram that deflector roll is drawn in the specific embodiment of the invention four, and 1 is without present embodiment processing
Fiber roll, 2 be fiber, and 3 be deflector roll, and 4 be washing equipment, and 5 be modifier solution, and 6 be drying equipment, and 7 is through this embodiment party
The processed fiber roll of formula；
Fig. 2 is the chemical equation that the epoxy group in amino and sizing agent in modifying agent of the invention occurs；
Fig. 3 is the SEM figure for testing the carbon fiber in one before modified；
Fig. 4 is the SEM figure for testing modified carbon fiber in one.
Specific embodiment
Specific embodiment 1: present embodiment is a kind of side of alcamines solution graft copolymerization modified carbon fiber surface size agent
Method specifically carries out according to the following steps:
One, it configures modifier solution: modifying agent being dissolved in solvent, modifier solution is obtained；The modifier solution
Mass concentration be 0.5%~5.0%；The modifying agent is the alcohol containing amino and unsaturated double-bond simultaneously in molecular structure
Amine small organic molecule；
Two, carbon fiber surface modification: by step 1 prepare modifier solution be adjusted to 50 DEG C~100 DEG C, with 50 DEG C~
100 DEG C of modifier solution carries out the carbon fiber that surface is modified, after being rinsed with water surface treatment to carbon fiber, is 50 DEG C in temperature
Dry 0.5h~6h, the carbon fiber after obtaining surface size agent grafting modification under conditions of~100 DEG C；The carbon fiber
For the unidirectional carbon fiber with epoxy type sizing agent, the carbon-fiber cloth with epoxy type sizing agent, there is epoxy type sizing agent
Fibrofelt or chopped carbon fiber with epoxy type sizing agent.
It is continuous fiber that unidirectional carbon fiber peacekeeping with epoxy type sizing agent, which has the carbon-fiber cloth of epoxy type sizing agent,.
Specific embodiment 2: present embodiment is unlike specific embodiment one: dividing described in step 1
Hydramine organic micromolecule in minor structure simultaneously containing amino and unsaturated double-bond is 4- amino -2- butene-1-ol and 1- ammonia
The mixture of one or both of base-3- butene-2 -ol.It is other same as the specific embodiment one.
Specific embodiment 3: present embodiment is unlike specific embodiment one: molten described in step 1
Agent is water or organic solvent.It is other same as the specific embodiment one.
Specific embodiment 4: as described in Figure 1, present embodiment is unlike specific embodiment one: working 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 are as follows:
Carbon fiber is immersed in 50 DEG C~100 DEG C of modifier solution by the method that deflector roll is drawn, processing 5min~
30min.It is other same as the specific embodiment one.
Present embodiment is suitable for the on-line continuous processing of continuous carbon fibre, and the degree of automation is higher, can effectively reduce
Phenomena such as fluffing of carbon fiber caused by being surface-treated, fracture of wire, improve the convergence of modified carbon fiber.
Specific embodiment 5: present embodiment is unlike specific embodiment one: 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 are as follows:
Carbon fiber is totally immersed in 50 DEG C~100 DEG C of modifier solution, impregnates 5min~30min.Other and tool
Body embodiment one is identical.
Specific embodiment 6: present embodiment is unlike specific embodiment one: with 50 DEG C in step 2
~100 DEG C of modifier solution carries out carbon fiber to use ultrasonic treatment while surface is modified.Other and specific embodiment
One is identical.
Specific embodiment 7: present embodiment is unlike specific embodiment three: described in step 1
Organic solvent is the mixture of one or more of alcohol, ether and ketone.It is other to be the same as the specific implementation mode 3.
Effect of the invention is verified by following tests:
Test one: this test is a kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent, is specifically pressed
What following steps carried out:
One, modifier solution is configured: modifying agent is soluble in water, obtain modifier solution；The modifier solution
Mass concentration is 1.0%；The modifying agent is 4- amino -2- butene-1-ol；
Two, carbon fiber surface modification: modifier solution prepared by step 1 is heated to be 80 DEG C, the modifying agent with 80 DEG C is molten
Liquid carries out the carbon fiber that surface is modified, after being rinsed with water surface treatment to carbon fiber, dry 4h under conditions of temperature is 60 DEG C,
Carbon fiber after obtaining surface size agent grafting modification；The 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 are as follows: draw by deflector roll
Carbon fiber is immersed in 80 DEG C of modifier solution by method, handles 10min.
Elemental composition analysis is carried out to the carbon fiber and modified carbon fiber tested in one before modified respectively, as a result as schemed
1, it can be seen that modified carbon fiber N content obviously increases, this is because the amino in modifying agent contains N element, illustrates
Modified success.
Table 1
Respectively to the carbon fiber and modified carbon fiber progress Analysis of Surface Topography in test one before modified, Fig. 3 is to change
Property before carbon fiber SEM figure, Fig. 4 is the SEM figure of modified carbon fiber, as can be seen from Figure modified carbon fiber surface
Pattern does not have significant change, illustrates that the modification of this test does not destroy the structure of carbon fiber itself.
By test a surface size agent grafting modification after carbon fiber and vinyl ester resin prepare composite material, lead to
It crosses micro- unsticking method to characterize the interface shear strength of composite material, interface shear strength mentions after finding carbon fiber surface modification
It is high by 50% or more.
Claims (6)
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 carries out according to the following steps:
One, it configures modifier solution: modifying agent being dissolved in solvent, modifier solution is obtained；The matter of the modifier solution
Measuring concentration is 0.5%~5.0%；The modifying agent is the alcamines containing amino and unsaturated double-bond simultaneously in molecular structure
Small organic molecule；
Hydramine organic micromolecule in the molecular structure simultaneously containing amino and unsaturated double-bond is 4- amino -2- fourth
The mixture of one or both of the pure and mild 1- amino-3- butene-2 -ol of alkene-1-；
Two, carbon fiber surface modification: modifier solution prepared by step 1 is adjusted to 50 DEG C~100 DEG C, with 50 DEG C~100 DEG C
Modifier solution the carbon fiber that surface is modified, after being rinsed with water surface treatment is carried out to carbon fiber, be 50 DEG C~100 in temperature
Dry 0.5h~6h, the carbon fiber after obtaining surface size agent grafting modification under conditions of DEG C；The carbon fiber is tool
There are unidirectional carbon fiber, the carbon-fiber cloth with epoxy type sizing agent, the fibre with epoxy type sizing agent of epoxy type sizing agent
Tie up 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, feature
It is that solvent described in step 1 is water or organic solvent.
3. a kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent according to claim 1, feature
When being that the carbon fiber described in the step 2 is continuous fiber, with 50 DEG C~100 DEG C of modifier solution to carbon fiber in step 2
Dimension carries out the modified method in surface are as follows: the modifying agent that carbon fiber is immersed in 50 DEG C~100 DEG C by the method that deflector roll is drawn is molten
In liquid, 5min~30min is handled.
4. a kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent according to claim 1, feature
It is that working as carbon fiber described in step 2 is the chopped carbon fiber with epoxy type sizing agent or the fibre with epoxy type sizing agent
When tieing up felt, the modified method in surface is carried out to carbon fiber with 50 DEG C~100 DEG C of modifier solution in step 2 are as follows: by carbon fiber
It is totally immersed in 50 DEG C~100 DEG C of modifier solution, impregnates 5min~30min.
5. a kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent according to claim 1, feature
It is that carbon fiber is carried out to use ultrasonic treatment while surface is modified with 50 DEG C~100 DEG C of modifier solution in step 2.
6. a kind of method of alcamines solution graft copolymerization modified carbon fiber surface size agent according to claim 2, feature
It is that organic solvent described in step 1 is the mixture of one or more of 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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- 2017-01-24 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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