CN108004779A - A kind of carbon fiber ketone-grouped resin base suspension sizing agent and preparation method thereof - Google Patents
A kind of carbon fiber ketone-grouped resin base suspension sizing agent and preparation method thereof Download PDFInfo
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- CN108004779A CN108004779A CN201610966290.4A CN201610966290A CN108004779A CN 108004779 A CN108004779 A CN 108004779A CN 201610966290 A CN201610966290 A CN 201610966290A CN 108004779 A CN108004779 A CN 108004779A
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- ketone
- carbon fiber
- sizing agent
- grouped resin
- resin base
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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
- D06M15/53—Polyethers
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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
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/285—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides
-
- 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 & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a kind of carbon fiber ketone-grouped resin base suspension sizing agent and preparation method thereof.The suspension sizing agent of the present invention is made of ketone-grouped resin, dispersant, stabilizer and deionized water.The suspension sizing agent property of the present invention is stablized, and available for carbon fiber is prepared, obtained starching carbon fiber is suitable for the intermediates such as ketone-grouped resin based composites carbon fibre fabric, prepreg, has good processing performance and Interface adhesive strength.
Description
Technical field
The invention belongs to carbon fiber sizing agent technical field, more particularly to a kind of ketone-grouped resin base suspension-type starching
Agent and preparation method thereof.
Background technology
Composite material is by two or more material of different nature, passes through the tool of method composition physically or chemically
There is the material of new capability.Carbon fiber is most common at present due to its high intensity, high-modulus, heat safe new fiber materials
One of multiple material enhancing phase.Contain rigid phenyl ring in ketone-grouped resin molecular structure, there is prominent high-temperature behavior, excellent
Mechanical property, electrical insulating property, the performance such as can process, and be that important high temperature resistant answers material matrix resin.Since both are respective excellent
Performance, fibre reinforced ketone-grouped resin based composites are commonly used to aerospace, the contour performance neck of electronic car industry
Domain, is the Typical Representative in tip materials field, important heatproof is tough engineering material.
The interface of fibre reinforced ketone-grouped resin based composites is an important factor for influencing its physical and chemical performance.
Carbon fiber surface is typically coated with one layer of sizing agent, to improve fibre technology performance, strengthens multiple material two-phase interface.It is industrial at present normal
With epoxy resin-matrix sizing agent, prepared carbon fiber answers material commonly used in thermosetting properties such as epoxy resin-matrix, phenolic resin bases, such as
Chinese patent (Application No. 201010522312.0) proposes one kind and uses modified epoxy amine curing agent and asphalt mixtures modified by epoxy resin
The carbon fiber emulsion pasting agent of the compound preparation of fat, answers material interface binding intensity to epoxy resin-matrix and improves.But on this kind of
Slurry agent has following key issue to be difficult to solve：First, the interfacial adhesion ability of carbon fiber surface epoxy resin and ketone-grouped resin
Generally, it is difficult to play the excellent properties that fibre reinforced polyarylether ketone group answers material；Second, use epoxy resin-matrix sizing agent starching
Carbon fiber, when left between long or processing temperature it is higher when, epoxy resin can be caused due to curing reaction fiber reunite or become
Firmly, it is difficult to scattered to sprawl；And the melt viscosity of thermoplastic poly aryl ether ketone is big, when preparing multiple material to carbon fiber bundle internal flow
Resistance is very big, and the carbon fiber of epoxy starching causes extreme difficulties due to impregnation processability of the cure hard to ketone-grouped resin.Cause
This, it is necessary to develop dedicated ketone-grouped resin based carbon fiber sizing agent.
The research of ketone-grouped resin base carbon fibre sizing agent is concentrated mainly on solvent-borne type and emulsion-type two types at present.
Since ketone-grouped resin is not soluble in water, partial solvent is only soluble in, therefore the method for adding solvent can be used to be prepared, but
Security is poor, and stability is poor, and industrial circle is seldom applied.Chinese patent (Application No. 201210464424.4) provides one kind
The modified epoxy class emulsion pasting agent being prepared by modifying agent, epoxy resin, surface modifier etc., to polyether-ether-ketone tree
The boundary strength that fat answers material improves.But its main body is still epoxy resin, it stores problem of aging, processing wellability is asked
Topic etc. is not resolved.
The content of the invention
In view of the above problems, it is an object of the invention to provide a kind of ketone-grouped resin base suspension starching of carbon fiber
Agent and preparation method thereof.Preparation method of the present invention is simple, obtained carbon fiber ketone-grouped resin base suspension sizing agent
Matter is stablized, its bulk composition is ketone-grouped resin powder, without epoxy resin ingredient, without any organic solvent, it is not necessary to
Any chemical modification.The starching carbon fiber prepared using the sizing agent of the present invention can be used for preparing ketone-grouped resin base composite wood
The material intermediates such as prepreg, fabric, have good processability and Interface adhesive strength.
The present invention uses industrial ketone-grouped resin powder, its preparation process relative maturity, cost is relatively low, is adapted to
Sizable application.To solve ketone-grouped resin powder dispersiveness in water and stability problem, invention introduces dispersant,
Preferably, polyacrylamide dispersant is selected, it can rely on molecular separating force and hydrogen bond action, with poly aryl ether ketone polymer chain
Section, which produces, to be adsorbed and is mutually mixed, and loses certain free degree.Meanwhile the dispersant has water solubility, molecule segment can be
Freely stretched in WATER AS FLOW MEDIUM, produce stronger steric stabilization effect, hinder the close to each other of poly(aryl ether ketone) powder and aggregation, make to gather
Aryl oxide ketone powder reaches fine dispersion.Invention introduces stabilizer, it is preferred that is used as stabilization by the use of alkylphenol polyoxyethylene ether
Agent, it can have certain compatibility with aromatic yl group with poly(aryl ether ketone) powder.It has well amphipathic at the same time,
It can promote more to be stabilized in the micelle particle water that poly(aryl ether ketone) powder forms with polyacrylamide amine dispersant.
The present invention provides a kind of suspension-type carbon fiber sizing agent, it is by ketone-grouped resin, dispersant, stabilizer and goes
Ionized water forms；Counted according to the gross mass of solid constituent for 100wt%, wherein：Ketone-grouped resin accounts for 60~80wt%, disperses
Agent accounts for 5~15wt%, and stabilizer accounts for 15~25wt%.
In the present invention, solid constituent account for carbon fiber ketone-grouped resin base suspension sizing agent gross weight 5%~
30%.
In the present invention, the ketone-grouped resin is selected from polyether-ketone PEK (formula I), polyether-ether-ketone PEEK (Formula II), polyethers
Ketone ketone PEKK (formula III) or polyether ether ketone ketone PEEKK (IV), in any one or a few.The present invention can be answered according to carbon fiber
The type of timber-used matrix resin adjusts accordingly, poly(aryl ether ketone) species preferably consistent with matrix resin.
In the present invention, the number-average molecular weight of the ketone-grouped resin is between 1.5 ten thousand~3.0 ten thousand；Its in powdered,
Its average diameter is between 20~50 microns.Preferably, the number-average molecular weight of the ketone-grouped resin is 2.0 ten thousand~2.5
Between ten thousand, powder average diameter is between 30~40 microns.
In the present invention, the dispersant is polyacrylamide, its number-average molecular weight is between 1.0 ten thousand~3.0 ten thousand, preferably
Between 1.5 ten thousand~2.0 ten thousand；The polyacrylamide, has such as the general structure of formula V.
Wherein n is the degree of polymerization of polyacrylamide.
In the present invention, the stabilizer is alkylphenol polyoxyethylene ether, is had such as the general structure of formula VI；
Wherein, R is selected from the saturated aliphatic groups for including 8~20 carbon atoms；Polyoxyethylene polymerization degree n scope for 30~
50。
A kind of preparation the present invention also provides above-mentioned carbon fiber with ketone-grouped resin base suspension-type carbon fiber sizing agent
Method, comprises the following steps that：By ketone-grouped resin, dispersant and deionized water after mixing, stabilizer is added thereto,
Discharge after being emulsified with high-speed emulsifying machine, obtain carbon fiber ketone-grouped resin base suspension-type carbon fiber sizing agent.
Compared to the prior art, the beneficial effects of the present invention are：
(1) the carbon fiber surface main body prepared using suspension sizing agent of the present invention contains poly(aryl ether ketone) resinoid,
Without epoxy resin, long-term storage and application will not produce ageing hardening phenomenon, have with ketone-grouped resin matrix resin good
Good processing performance and interface performance.
(2) suspension carbon fiber sizing agent of the present invention introduces polyacrylamide amine dispersant, while introduces with virtue
The alkylphenol polyoxyethylene ether stabilizer of base group, with the equally poly(aryl ether ketone) powder with a large amount of aromatic yl groups with certain
Compatibility.It has well amphipathic at the same time, poly(aryl ether ketone) powder can be promoted to be formed with polyacrylamide amine dispersant micro-
More it is stabilized in group's particle water, product storage application performance is good.
(3) suspension carbon fiber sizing agent preparation process of the present invention is without appointing ketone-grouped resin resin
What chemical modification, preparation process need not add any chemical solvent, and overall process does not produce correlation only with the method for physical mixed
Polluting waste, security and the feature of environmental protection are high.Sizing agent raw material is extensive, and technique is simple, common apparatus can be used to prepare, it is comprehensive into
This is low.
Embodiment
With reference to specific embodiment, the present invention is further explained.It is to be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Scope.
Comparative example 1
Using bisphenol-A/Bisphenol F composite epoxy resin base emulsion type carbon fiber sizing agent (production of Chinese Academy of Sciences Shanghai Institute of Organic Chemistry,
KTM-3 types) starching is carried out on carbon fiber test wire, starching agent concentration is 2.8%, dip time 30s, and receiving silk after dry prepares
Obtain epoxy resin-matrix starching carbon fiber.
Comparative example 2
Using bisphenol A epoxide resin base emulsion type carbon fiber sizing agent (Chinese Academy of Sciences's Shanghai Institute of Organic Chemistry production, KTM-1 types) in carbon
Starching is carried out on string proof test line, starching agent concentration is 4.8%, dip time 35s, and receiving silk after dry is prepared epoxy resin
Base starching carbon fiber.
Embodiment 1~8
Quantitative ketone-grouped resin powder, polyacrylamide are uniformly mixed spare；Added in stainless steel stirred tank A
Quantitative water simultaneously opens mechanical agitation, keeps under certain rotating speed, is gradually added into said mixture, continues to stir after being added completely into
Certain time；Above-mentioned aqueous mixture is transferred in stainless steel stirred tank B, quantitative alkylphenol polyoxyethylene ether is added, opens
High-speed emulsifying machine is opened, is discharged after a certain period of time with the emulsification of certain rotating speed.The ketone-grouped resin powder comes from France A Kema
Limited company, the polyacrylamide, alkylphenol polyoxyethylene ether come from BASF AG.Embodiment 1~8
Prepared suspension sizing agent solid constituent is shown in Table 1, and sizing agent composition dosage is shown in Table 2, and sizing agent preparation technology parameter is shown in Table
3。
Using the ketone-grouped resin resin-based carbon fiber sizing agent prepared by above-described embodiment on carbon fiber test wire
Starching is carried out, dip time 30s, receives silk after dry and starching carbon fiber is prepared.
1 sizing agent solid constituent of table
2 sizing agent of table forms dosage
3 sizing agent preparation technology parameter of table
Test analysis
Whether the present invention has obvious layering using the prepared sizing agent of ocular estimate observation；It is public using U.S. BROOKFIELD
Department's DV Pro VISCOMETER viscosity apparatus tests the viscosity of prepared sizing agent；Using weighting method after dried to prepared
The concentration of suspension is tested, and the steady of prepared sizing agent is characterized relative to the change rate of upper strata concentration with lower floor's concentration
It is qualitative, calculated according to the following equation：
Lower floor's change rate of concentration=(lower floor's concentration-upper strata concentration)/upper strata concentration * 100%
Test to obtain the contact angle of ketone-grouped resin and carbon fiber using OCA20 contact angle measurements；Using Japanese east
Flourish industry companies MODEL HM410 interface performance evaluating apparatus tests to obtain ketone-grouped resin and the interface shearing of carbon fiber is strong
Degree.
Gained suspension sizing agent performance is shown in Table 4 with starching carbon fiber Evaluation results.It can be seen from result in table
Suspension sizing agent has no layering, the change rate very little of lower floor's concentration upper layer concentration, and emulsion-type sizing agent in level of approximation,
Show to be evenly distributed inside suspension, stability is good.Suspension sizing agent overall viscosity is low, good fluidity, easy to clean, online work
Skill is good.The contact angle smaller of starching carbon fiber and ketone-grouped resin prepared by embodiment, ketone-grouped resin are easier
Quickly being infiltrated to carbon fiber surface and painted inside, prepared carbon fibre fabric and prepreg uniformity are good, and fault gap is few,
Interface shear strength higher.
4 suspension sizing agent of table and starching carbon fiber Evaluation results
Although the present invention discloses preferred embodiment as above, so it is not limited to present disclosure, any ripe
Know this those skilled in the art, do not departing from the present invention main spirits and context in, when can make it is various change and retouch, because of the invention
Protection domain should be subject to the actual claim scope applied for a patent.
Claims (8)
1. a kind of carbon fiber ketone-grouped resin base suspension sizing agent, it is characterised in that it is by ketone-grouped resin, scattered
Agent, stabilizer and deionized water composition；It is 100% meter according to the gross mass of solid constituent, wherein：Ketone-grouped resin accounts for 60~
80wt%, dispersant account for 5~15wt%, and stabilizer accounts for 15~25wt%.
2. carbon fiber according to claim 1 ketone-grouped resin base suspension sizing agent, it is characterised in that：Solid group
Divide and account for the 5%~30% of carbon fiber ketone-grouped resin base suspension sizing agent gross weight.
3. carbon fiber according to claim 1 ketone-grouped resin base suspension sizing agent, it is characterised in that：Described
Ketone-grouped resin is any in polyether-ketone PEK, polyether-ether-ketone PEEK, polyether ketone ketone PEKK or polyether ether ketone ketone PEEKK
It is one or more of.
4. carbon fiber according to claim 1 ketone-grouped resin base suspension sizing agent, it is characterised in that：Described
The number-average molecular weight of ketone-grouped resin is between 1.5 ten thousand~3.0 ten thousand；It is in powdered, its average diameter is at 20~50 microns
Between.
5. carbon fiber according to claim 4 ketone-grouped resin base suspension sizing agent, it is characterised in that：Described
The number-average molecular weight of ketone-grouped resin is between 2.0 ten thousand~2.5 ten thousand, and average diameter is between 30~40 microns.
6. carbon fiber according to claim 1 ketone-grouped resin base suspension sizing agent, it is characterised in that：Described
Dispersant is polyacrylamide, its number-average molecular weight is between 1.0 ten thousand~3.0 ten thousand, between preferably 1.5 ten thousand~2.0 ten thousand.
7. carbon fiber according to claim 6 ketone-grouped resin base suspension sizing agent, it is characterised in that：Described
Stabilizer is alkylphenol polyoxyethylene ether, is had such as the general structure of formula VI；
Wherein, R is selected from the saturated aliphatic groups for including 8~20 carbon atoms；Polyoxyethylene polymerization degree n scope is 30~50.
A kind of 8. carbon fiber according to one of claim 1-7 ketone-grouped resin base suspension-type carbon fiber sizing agent
Preparation method, it is characterised in that comprise the following steps that：By ketone-grouped resin, dispersant and deionized water after mixing,
Stabilizer is added thereto, is discharged after being emulsified with high-speed emulsifying machine, obtains carbon fiber ketone-grouped resin base suspension-type carbon
Fiber sizing agent.
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| CN201610966290.4A CN108004779B (en) | 2016-10-28 | 2016-10-28 | Polyaryletherketone resin-based suspension sizing agent for carbon fibers and preparation method thereof |
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| CN201610966290.4A CN108004779B (en) | 2016-10-28 | 2016-10-28 | Polyaryletherketone resin-based suspension sizing agent for carbon fibers and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109505135A (en) * | 2018-11-28 | 2019-03-22 | 中国科学院宁波材料技术与工程研究所 | A kind of method that polyether ketone ketone sizing agent and its starching prepare carbon fibre composite |
| CN110820315A (en) * | 2019-12-11 | 2020-02-21 | 吉林大学 | Crystalline crosslinkable polyaryletherketone sizing agent modified carbon fiber and preparation method thereof |
| CN111472172A (en) * | 2020-06-05 | 2020-07-31 | 长春工业大学 | Aqueous amino modified polyaryletherketone sizing agent and preparation method thereof |
| CN113235304A (en) * | 2021-05-31 | 2021-08-10 | 哈尔滨工业大学 | Aqueous solution sizing agent based on polyether-ether-ketone, preparation method thereof and preparation method of carbon fiber cloth reinforced polyether-ether-ketone composite material |
| CN113430831A (en) * | 2021-07-14 | 2021-09-24 | 上海交通大学 | High-temperature-resistant universal sizing agent for water-based carbon fibers, and preparation method and application thereof |
| CN113718528A (en) * | 2021-08-24 | 2021-11-30 | 中国科学院山西煤炭化学研究所 | Sulfonated polyaryletherketone water sizing agent and preparation method and application thereof |
| CN114456539A (en) * | 2022-01-24 | 2022-05-10 | 华东理工大学 | Preparation method of high-solid-content polyether-ether-ketone aqueous suspension and composite fiber |
| CN114559685A (en) * | 2022-02-28 | 2022-05-31 | 中国科学院长春应用化学研究所 | Carbon fiber-polyaryletherketone composite material unidirectional prepreg tape and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109505135A (en) * | 2018-11-28 | 2019-03-22 | 中国科学院宁波材料技术与工程研究所 | A kind of method that polyether ketone ketone sizing agent and its starching prepare carbon fibre composite |
| CN110820315A (en) * | 2019-12-11 | 2020-02-21 | 吉林大学 | Crystalline crosslinkable polyaryletherketone sizing agent modified carbon fiber and preparation method thereof |
| CN111472172A (en) * | 2020-06-05 | 2020-07-31 | 长春工业大学 | Aqueous amino modified polyaryletherketone sizing agent and preparation method thereof |
| CN113235304A (en) * | 2021-05-31 | 2021-08-10 | 哈尔滨工业大学 | Aqueous solution sizing agent based on polyether-ether-ketone, preparation method thereof and preparation method of carbon fiber cloth reinforced polyether-ether-ketone composite material |
| CN113430831A (en) * | 2021-07-14 | 2021-09-24 | 上海交通大学 | High-temperature-resistant universal sizing agent for water-based carbon fibers, and preparation method and application thereof |
| CN113430831B (en) * | 2021-07-14 | 2022-10-25 | 上海交通大学 | High-temperature-resistant universal sizing agent for water-based carbon fibers, and preparation method and application thereof |
| CN113718528A (en) * | 2021-08-24 | 2021-11-30 | 中国科学院山西煤炭化学研究所 | Sulfonated polyaryletherketone water sizing agent and preparation method and application thereof |
| CN114456539A (en) * | 2022-01-24 | 2022-05-10 | 华东理工大学 | Preparation method of high-solid-content polyether-ether-ketone aqueous suspension and composite fiber |
| CN114559685A (en) * | 2022-02-28 | 2022-05-31 | 中国科学院长春应用化学研究所 | Carbon fiber-polyaryletherketone composite material unidirectional prepreg tape and preparation method thereof |
| CN114559685B (en) * | 2022-02-28 | 2024-03-26 | 中国科学院长春应用化学研究所 | Carbon fiber-polyaryletherketone composite material unidirectional prepreg tape and preparation method thereof |
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| CN108004779B (en) | 2022-02-08 |
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