CN106589313A - Unsaturated acid modified epoxy resin universal carbon fiber sizing agent, and preparation method and application thereof - Google Patents
Unsaturated acid modified epoxy resin universal carbon fiber sizing agent, and preparation method and application thereof Download PDFInfo
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- CN106589313A CN106589313A CN201510664767.9A CN201510664767A CN106589313A CN 106589313 A CN106589313 A CN 106589313A CN 201510664767 A CN201510664767 A CN 201510664767A CN 106589313 A CN106589313 A CN 106589313A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/14—Polycondensates modified by chemical after-treatment
- C08G59/1433—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
- C08G59/1438—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
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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
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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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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The invention discloses an unsaturated acid modified epoxy resin universal carbon fiber sizing agent, and a preparation method and an application thereof. The universal carbon fiber sizing agent comprises the following components: bisphenol A based epoxy resin, aliphatic binary monounsaturated acid with double end groups which are carboxyl, an aromatic active diluent containing one epoxide group in molecule, an inorganic polymerization inhibitor, and a quaternary ammonium bromide catalyst. The sizing agent is suitable for sizing 1K-12K small filament bundle carbon fiber for aerospace, the maximum decomposition peak temperature of reaction products is higher than 325 DEG C, sized carbon fiber and epoxy resin, phenolic resin, bismaleimide resin and other thermosetting resin substrates have good interface bonding strength with good versatility, and especially interface bonding strength of phenolic resin is substantially improved.
Description
Technical field
The invention belongs to carbon fiber sizing agent field, on more particularly to a kind of unsaturated acids modified epoxy common carbon fiber
Slurry agent, preparation method and applications.
Background technology
Carbon fiber enhancement resin base composite material has various excellent physics such as lightweight, high-strength, heatproof, conduction and mechanical property
Can, the carbon fiber enhancement resin base composite material with the little tow carbon fiber of 1K～12K high-performance as representative is in aerospace field
Have been obtained for extensively application.It is in the airborne vehicle with fighter plane and airline carriers of passengers as representative, with fields such as rocket-powered missile satellites
In prepared by the spacecraft of representative, fibre reinforced epoxy radicals, phenolic aldehyde base, dimaleoyl imino composite are fabulous because of its
Weight loss effect, can significantly replace traditional metal materials to do primary load bearing, secondary load-carrying construction part, improve the work of aerospace vehicle
Make effectiveness and scope.As carbon fibre composite is in the deep application of aerospace field, the user in the field is to carbon fiber
Propose further requirement：On the one hand wish high temperature resistant, the wet-hot aging performance raising of starching carbon fiber and its multiple material, meet
The special environmental requirement of aerospace field；On the other hand wish that carbon fiber is improved with multiple material interface performance, versatility is higher,
Holistic cost is reduced.In the preparation process of carbon fibre composite, carbon fiber is multiple with the two-phase interface performance of matrix resin
Can condensation material have the key of excellent physical and mechanical property, wherein the sizing agent for being coated in carbon fiber surface is the master at interface
Arrying main body is wanted, carbon fiber surface and the prerequisite process based prediction model of resin body is given.
Phenolic resin has higher mechanical strength because of it, heat-resist, fire retardant, low toxicity, low smoke, can be with other polies
Thing blending realizes high performance and is widely used in aerospace field.The carbon fiber sizing agent being widely used at present is with epoxy
Resin is main body, is aided with partial emulsifier, auxiliary agent and deionized water, by the emulsion that the method for Phase inversion emulsification is prepared from
Slurry agent.Patent 102828416A disclose it is a kind of with the epoxy resin containing 2-50%, the water of 35-97%, 0.5-15% table
The emulsion type carbon fiber sizing agent of the inorganic ammonium salt of face activating agent and 0.1-2.0%, the sizing agent stability is very high, and its interlayer is cut
Shearing stress strengthens more than 10% relative to existing carbon fibre composite, but such sizing agent is general to the adaptability of phenolic resin.
It is the carbon fiber sizing agent of main body by phenolic resin that patent 102912637A is disclosed a kind of, by 2～25 parts of phenolic resin, is answered
With 1～5 part of resin, 0.01～5 part of antistatic additive, 100 parts of compositions of solvent, wherein described phenolic resin is thermoplastic phenolic
Resin or phenol-formaldehyde resin modified, the carbon fiber sizing agent described in the invention can be preferably compatible with thermoplastic matrix resin, multiple
The stretching of condensation material, bending strength are higher, but its application is mainly thermoplastic matrix resin, it is impossible on preferably improving
Slurry agent and thermosetting phenolic resin, epoxy resin, the boundary strength of bimaleimide resin.Disclosure satisfy that Aero-Space are led
Domain high temperature resistant requires, at the same with conventional thermoset substrate resin, especially there is good interface intensity with thermosetting phenolic resin
Carbon fiber sizing agent has not yet to see relevant report.
The content of the invention
In order to solve current little tow carbon fiber sizing agent, the problem of single type matrix resin, the purpose of the present invention are only applicable to
It is that a kind of being applied on the unsaturated acids modified epoxy common carbon fiber of multiple types basic resin system is provided
Slurry agent, preparation method and applications.The unsaturated acids modified epoxy common carbon fiber sizing agent of the present invention is applied to boat
The empty space flight starching of the little tow carbon fibers of 1K～12K, sizing agent thermostability is high, starching carbon fiber and epoxy resin, phenolic aldehyde
The thermosetting resin matrix such as resin, bimaleimide resin are respectively provided with good interface bond strength, its highly versatile, especially
The interface bond strength of itself and phenolic resin has and more significantly improves.
Carbon fiber sizing agent of the present invention carries out open loop using binary aliphatic list unsaturated acids to bisphenol A type epoxy resin
Reaction, introduces a certain amount of unsaturated functional group on modified molecules main chain, improve sizing agent and different matrix interlaminar resin point
Sub- intermolecular forces, enable starching carbon fiber and epoxy resin, phenolic resin, bimaleimide resin to be respectively provided with good
Boundary strength.
The present invention provides a kind of unsaturated acids modified epoxy common carbon fiber sizing agent, percentage, its group
Dividing includes：
The gross weight of said components meets 100%；Wherein：
The bisphenol A type epoxy resin polycondensation that is diphenol propane and epoxychloropropane under base catalyst effect forms,
Two end groups are the bisphenol A type epoxy resin of epoxy radicals, and it has following formula：
Wherein, n is average degree of polymerization, n=0～5；
The unsaturated acids are to be the binary aliphatic list unsaturation of carboxyl containing 4～10 C atoms, both-end base on main chain
Acid, it has following structure formula：
Wherein, R1Selected from comprising 2～8 carbon atoms and comprising the monounsaturated fatty acid race group of a unsaturated double-bond；
The diluent is the aromatic active diluent containing an epoxy radicals in molecule, and it has following structure formula：
Wherein, R2For the aromatic group of 1～2 phenyl ring, including phenyl, tolyl, ethylphenyl, n-butylphenyl or
Isobutyl phenenyl, the epoxide equivalent scope of the diluent be at 150～300,25 DEG C viscosity between 0.001～0.1Pas；
The quaternary ammonium bromide salt catalyst has following structure formula：
Wherein, R3It is selected from the aliphatic group comprising 8～20 carbon atoms, R4It is selected from the fat comprising 1～4 carbon atom
Fat race straight chain group.
Preferably, the bisphenol A type epoxy resin selected from Shell Co. Ltd of U.S. EPON 820, EPON 828, EPON 834,
Any one in EPON 1001, EPON 1002 or EPON 1004.
Preferably, the unsaturated acids are selected from 3- hexene diacids, 2- methyl -2- hexene diacids, 2- methyl -2- heptylene diacids or 2,5-
One kind in dimethyl -2- heptylene diacids.
Preferably, the diluent is selected from phenyl glycidyl ether, cresylglycidylether, to ethylphenyl glycidyl ether
Or to the one kind in isobutyl phenenyl glycidyl ether.
Preferably, the one kind or two kinds of the inorganic polymerization inhibitor in Cu-lyt., ferric chloride.
Preferably, the quaternary ammonium bromide salt catalyst selected from ten alkyl trimethyl ammonium bromides, Dodecyl trimethyl ammonium chloride,
Any one in dodecyltriethylammonium ammonium bromide or cetyl trimethylammonium bromide.
The present invention also provides a kind of preparation method of unsaturated acids modified epoxy common carbon fiber sizing agent, concrete steps
Including：
(1) vacuum dehydration：By bisphenol A type epoxy resin, at high temperature evacuation is dehydrated to bubble-free generation, its vacuum dehydration
Temperature is 90～120 DEG C, and the vacuum pressure of dehydration is 100-0.1mmHg, then by the bisphenol A-type obtained by vacuum dehydration
Epoxy resin is gradually cooled to 60～80 DEG C；
(2) low-temp reaction：Under drying nitrogen protection, diluent, inorganic polymerization inhibitor, unsaturated acids and bromination are sequentially added
Quaternary ammonium salt catalyst, control material temperature in 60～80 DEG C, stirring reaction 5～10 hours；
(3) pyroreaction：Above-mentioned temperature of reaction system is gradually heating to into 100～140 DEG C, reaction stops anti-after 1～4 hour
Should, take out when material is down to room temperature, unsaturated acids modified epoxy sizing agent is obtained.
Preferably, in step (1), dehydration temperaturre is 110 DEG C；Vacuum pressure is 10-0.5mmHg；In step (2),
Low-temp reaction temperature is 65～75 DEG C；Response time is 6～8 hours；
In step (3), pyroreaction temperature is 105～125 DEG C, and the response time is 2～3 hours.
The present invention furthermore provides a kind of application process of unsaturated acids modified epoxy common carbon fiber sizing agent, tool
Body step includes：
1. sizing agent is prepared：The carbon fiber sizing agent resin of above-mentioned preparation is taken, acetone is added, 1～2 is stood in confined conditions
Hour, then it is slowly stirred, until all solids dissolve in acetone, it is configured to the starching dilution agent that concentration is 0.5～3wt%
Liquid；
2. online starching is dried：The sizing agent diluent for preparing is placed in sizing groove, non-starching carbon fiber passes through sizing groove
Dipping completes starching；Carbon fiber after starching is dried using room temperature wind, and dry starching carbon fiber is obtained after winding；
Wherein：The non-starching carbon fiber is the 1K～12K Jing after the process of low-temperature carbonization, high temperature cabonization, surface treatment and washing process
Carbon fiber.
Preferably, step 1. in, the concentration of the sizing agent diluent is 1.0～2.0wt%.
Preferably, step 2. in, the starching time be 5～60s；Drying time is 0.5～2.5min.Further preferred：On
The slurry time is 15～35s；Drying time is 1～2min.
Preferably, step 2. in, starching carbon fiber starching amount control in 1.5～2.5wt%.
The beneficial effects of the present invention is：
(1) present invention adopts unsaturated acids modified epoxy, while introducing aromatic active dilution during the course of the reaction
Agent, can effectively alleviate the high viscosity of reaction system, and reaction conversion ratio is high.Prepared sizing agent can be applied little with 1～12K
The online starching of tow carbon fiber, starching carbon fiber convergence is good, and lousiness amount is few, excellent combination property.
(2) invention introduces the more excellent inorganic polymerization inhibitor of temperature tolerance and aromatic active diluent, starching carbon fiber
Thermostability is high, can be used in the preparation of low high temperature different curing system and processing technique composite, meets Aero-Space use
The application requirement of carbon fibre composite.
(3) the sizing agent highly versatile prepared by the present invention, goes for epoxy resin, phenolic resin, double maleoyl
The preparation of imide resin based composites.Quaternary ammonium bromide salt catalyst is introduced in reaction system as potential curing agent, is made
The Interface adhesive strength of starching carbon fiber and phenolic resin has and more significantly improves.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, art technology
Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Fixed scope.
Embodiment
First, the preparation of sizing agent
During quantitative bisphenol A type epoxy resin (Shell Co. Ltd of the U.S.) is placed in into the four-hole boiling flask with mechanical stirring device,
110 DEG C are heated to, 10～0.5mmHg of vacuum pressure dehydration 2h are kept, are produced to the complete bubble-free of system.70 DEG C are cooled to,
99.999% high pure nitrogen is passed through, while removing vacuum equipment.Quantitative diluent, inorganic resistance are sequentially added in four-hole boiling flask
Poly- agent, unsaturated acids, quaternary ammonium bromide salt catalyst (picking up from Chemical Reagent Co., Ltd., Sinopharm Group), control material
Temperature 70 DEG C react 7 hours, then heat to 120 DEG C reaction 2.5 hours after stop heating.Treat that system temperature is down to often
Stop stirring when warm, the unsaturated acids modified epoxy sizing agent is obtained.
The bisphenol A type epoxy resin, unsaturated acids, diluent, inorganic polymerization inhibitor, the product of quaternary ammonium bromide salt catalyst
Plant and consumption is shown in Table 1～table 2.Obtained sizing agent the performance test results are shown in Table 3.From result in table, embodiment institute
The maximum peak temperature that decomposes of the sizing agent resin of preparation is all higher than 325 DEG C, is improved largely compared with comparative example, more conducively aviation boat
It uses the processing and application of carbon fibre composite.
Sizing agent resin mean molecule quantity prepared by the present embodiment is tested using GPC gel permeation chromatographies, and thermostability is adopted
Tested with TGA thermal gravimetric analyzers, using weightless maximum peak temperature as maximum decomposition temperature.
The raw material variety table of table 1
* comparative example 1：Sizing agent resin is made up of pure epoxy resin EPON 1001, does not carry out any modified or other process.
Raw material dosage table (g) of table 2
| Epoxy resin | Unsaturated acids | Diluent | Polymerization inhibitor | Catalyst | |
| Comparative example 1 | 100 | 0 | 0 | 0 | 0 |
| Embodiment 1 | 50.0 | 28.6 | 20.0 | 0.14 | 1.26 |
| Embodiment 2 | 52.3 | 30.0 | 15.6 | 0.10 | 2.00 |
| Embodiment 3 | 56.4 | 26.7 | 15.4 | 0.12 | 1.38 |
| Embodiment 4 | 59.4 | 25.2 | 14.3 | 0.14 | 0.96 |
| Embodiment 5 | 62.0 | 24.4 | 12.1 | 0.17 | 1.33 |
| Embodiment 6 | 65.2 | 22.7 | 11.5 | 0.10 | 0.50 |
| Embodiment 7 | 67.9 | 23.0 | 8.0 | 0.20 | 0.90 |
| Embodiment 8 | 70.0 | 20.0 | 8.7 | 0.05 | 1.25 |
The sizing agent resin property of table 3 tests table
| Number-average molecular weight | Maximum decomposition temperature (DEG C) | |
| Comparative example 1 | 950 | 243.0 |
| Embodiment 1 | 1872 | 333.6 |
| Embodiment 2 | 1900 | 335.0 |
| Embodiment 3 | 1834 | 331.7 |
| Embodiment 4 | 1804 | 330.2 |
| Embodiment 5 | 1788 | 329.4 |
| Embodiment 6 | 1754 | 327.7 |
| Embodiment 7 | 1760 | 328.0 |
| Embodiment 8 | 1700 | 325.1 |
2nd, the application of sizing agent
The quantitative sizing agent resin for preparing and acetone is added with this in 1000ml beakers, beaker is closed.After 1.5 hours
Locking device is opened, is slowly stirred, until all sizing agent resins are dissolved in acetone, system is transparent without muddiness, starching is obtained
Dilution agent liquid.
The good sizing agent diluent of above-mentioned configuration is placed in sizing groove, using filament tow quetsch, will non-starching 12K carbon
Fiber is impregnated by sizing groove, then by blowing device, is dried using room temperature wind, is then carried out by receive silk machine
Winding, obtains dry starching carbon fiber, and gained starching carbon fiber Evaluation results are shown in Table 4.From result in table,
The interlaminar shear strength of starching carbon fiber and epoxy resin, phenolic resin, bimaleimide resin prepared by embodiment compared with
Comparative example is improved, and the interlaminar shear strength of its neutralization phenolic resin improves the most notable.
The present embodiment reference《GB/T 3357-1982 unidirectional fibre reinforced plastics interlayer shear strength test methods》Test starching
The one-way slabss interlaminar shear strength ILSS of carbon fiber, selected matrix resin be respectively thermosetting epoxy resin AG80 (on
Extra large synthetic resin institute), thermosetting phenolic resin 2123 (SUMITOMO CHEMICAL KCC), thermosetting bismaleimide
Polyimide resin 6421 (Beijing Research Inst. of Aeronautic Material, abbreviation bismaleimide resin).
Shear strength test tables of data (Mpa) between the starching carbon fiber layer of table 4
| Epoxy resin | Phenolic resin | Bismaleimide resin | |
| Comparative example 1 | 94.5 | 60.7 | 89.8 |
| Embodiment 1 | 122.4 | 92.2 | 111.5 |
| Embodiment 2 | 123.0 | 93.1 | 112.5 |
| Embodiment 3 | 124.9 | 91.0 | 110.8 |
| Embodiment 4 | 126.2 | 90.1 | 110.2 |
| Embodiment 5 | 127.4 | 89.6 | 109.9 |
| Embodiment 6 | 128.8 | 88.6 | 109.2 |
| Embodiment 7 | 130.1 | 88.8 | 108.9 |
| Embodiment 8 | 131.0 | 87.0 | 108.1 |
Although the present invention discloses preferred embodiment as above, so it is not limited to present disclosure, any to be familiar with this
Those skilled in the art, without departing from the present invention main spirits and context in, when can make it is various change with retouching, therefore invent
Protection domain should be defined by the basic right claimed range applied for a patent.
Claims (13)
1. a kind of unsaturated acids modified epoxy common carbon fiber sizing agent, it is characterised in that percentage, its
Component includes：
The gross weight of said components meets 100%；Wherein：
The bisphenol A type epoxy resin polycondensation that is diphenol propane and epoxychloropropane under base catalyst effect forms,
Two end groups are the bisphenol A type epoxy resin of epoxy radicals, and it has following formula：
Wherein, n is average degree of polymerization, n=0～5；
The unsaturated acids are to be the binary aliphatic list unsaturation of carboxyl containing 4～10 C atoms, both-end base on main chain
Acid, it has following structure formula：
Wherein, R1Selected from comprising 2～8 carbon atoms and comprising the monounsaturated fatty acid race group of a unsaturated double-bond；
The diluent is the aromatic active diluent containing an epoxy radicals in molecule, and it has following structure formula：
Wherein, R2For the aromatic group of 1～2 phenyl ring, including phenyl, tolyl, ethylphenyl, normal-butyl
Phenyl or isobutyl phenenyl, the epoxide equivalent scope of the diluent be at 150～300,25 DEG C viscosity in 0.001～0.1Pas
Between；
The quaternary ammonium bromide salt catalyst has following structure formula：
Wherein, R3It is selected from the aliphatic group comprising 8～20 carbon atoms, R4It is selected from the fat comprising 1～4 carbon atom
Fat race straight chain group.
2. unsaturated acids modified epoxy common carbon fiber sizing agent according to claim 1, it is characterised in that：Institute
State bisphenol A type epoxy resin selected from Shell Co. Ltd of U.S. EPON 820, EPON 828, EPON 834, EPON 1001,
Any one in EPON 1002 or EPON 1004.
3. unsaturated acids modified epoxy common carbon fiber sizing agent according to claim 1, it is characterised in that：Institute
Unsaturated acids are stated selected from 3- hexene diacids, 2- methyl -2- hexene diacids, 2- methyl -2- heptylene diacids or 2,5- dimethyl -2- heptene
One kind in diacid.
4. unsaturated acids modified epoxy common carbon fiber sizing agent according to claim 1, it is characterised in that：Institute
Diluent is stated selected from phenyl glycidyl ether, cresylglycidylether, to ethylphenyl glycidyl ether or to isobutyl phenenyl
One kind in glycidyl ether.
5. unsaturated acids modified epoxy common carbon fiber sizing agent according to claim 1, it is characterised in that：Institute
State the one kind or two kinds of inorganic polymerization inhibitor in Cu-lyt., ferric chloride.
6. unsaturated acids modified epoxy common carbon fiber sizing agent according to claim 1, it is characterised in that：Institute
Quaternary ammonium bromide salt catalyst is stated selected from ten alkyl trimethyl ammonium bromides, Dodecyl trimethyl ammonium chloride, the second of dodecyl three
Any one in base ammonium bromide or cetyl trimethylammonium bromide.
7. a kind of preparation method of unsaturated acids modified epoxy common carbon fiber sizing agent, it is characterised in that concrete steps
Including：
(1) vacuum dehydration：By bisphenol A type epoxy resin, at high temperature evacuation is dehydrated to bubble-free generation, its vacuum dehydration
Temperature is 90～120 DEG C, and the vacuum pressure of dehydration is 100-0.1mmHg, then by the bisphenol A-type obtained by vacuum dehydration
Epoxy resin is gradually cooled to 60～80 DEG C；
(2) low-temp reaction：Under drying nitrogen protection, diluent, inorganic polymerization inhibitor, unsaturated acids and bromination are sequentially added
Quaternary ammonium salt catalyst, control material temperature in 60～80 DEG C, stirring reaction 5～10 hours；
(3) pyroreaction：Above-mentioned temperature of reaction system is gradually heating to into 100～140 DEG C, reaction stops anti-after 1～4 hour
Should, take out when material is down to room temperature, unsaturated acids modified epoxy sizing agent is obtained.
8. preparation method according to claim 7, it is characterised in that：In step (1), dehydration temperaturre is 110 DEG C；Very
Pneumatics power is 10-0.5mmHg；In step (2), low-temp reaction temperature is 65～75 DEG C；Response time is 6～8 hours；
In step (3), pyroreaction temperature is 105～125 DEG C, and the response time is 2～3 hours.
9. a kind of application process of unsaturated acids modified epoxy common carbon fiber sizing agent, it is characterised in that concrete steps
Including：
1. sizing agent is prepared：The carbon fiber sizing agent resin of above-mentioned preparation is taken, acetone is added, 1～2 is stood in confined conditions
Hour, then it is slowly stirred, until all solids dissolve in acetone, it is configured to the starching dilution agent that concentration is 0.5～3wt%
Liquid；
2. online starching is dried：The sizing agent diluent for preparing is placed in sizing groove, non-starching carbon fiber passes through sizing groove
Dipping completes starching；Carbon fiber after starching is dried using room temperature wind, and dry starching carbon fiber is obtained after winding；
Wherein：The non-starching carbon fiber is the 1K～12K Jing after the process of low-temperature carbonization, high temperature cabonization, surface treatment and washing process
Carbon fiber.
10. application process according to claim 9, it is characterised in that：Step 1. in, the concentration of the sizing agent diluent
For 1.0～2.0wt%.
11. application processes according to claim 9, it is characterised in that：Step 2. in, the starching time be 5～60s；When being dried
Between be 0.5～2.5min.
12. application processes according to claim 9 or 11, it is characterised in that：Step 2. in, the starching time be 15～35s；
Drying time is 1～2min.
13. application processes according to claim 9, it is characterised in that：Step 2. in, starching carbon fiber starching amount control exist
1.5～2.5wt%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109722745A (en) * | 2017-10-27 | 2019-05-07 | 中国石油化工股份有限公司 | A kind of polyetherimide resin based composites carbon fiber and preparation method thereof |
| CN115341391A (en) * | 2022-07-11 | 2022-11-15 | 浙江理工大学 | Water-based sizing agent suitable for recycling carbon fibers and sizing method |
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