CN108004779B - Polyaryletherketone resin-based suspension sizing agent for carbon fibers and preparation method thereof - Google Patents
Polyaryletherketone resin-based suspension sizing agent for carbon fibers and preparation method thereof Download PDFInfo
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- CN108004779B CN108004779B CN201610966290.4A CN201610966290A CN108004779B CN 108004779 B CN108004779 B CN 108004779B CN 201610966290 A CN201610966290 A CN 201610966290A CN 108004779 B CN108004779 B CN 108004779B
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- polyaryletherketone resin
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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
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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
Abstract
The invention discloses a polyaryletherketone resin-based suspension sizing agent for carbon fibers and a preparation method thereof. The suspension sizing agent consists of polyaryletherketone resin, a dispersing agent, a stabilizing agent and deionized water. The suspension sizing agent disclosed by the invention is stable in property, can be used for preparing carbon fibers, and the prepared sized carbon fibers are suitable for intermediates such as carbon fiber fabrics and prepreg for polyaryletherketone resin-based composite materials, and have good processing performance and interface bonding capability.
Description
Technical Field
The invention belongs to the technical field of carbon fiber sizing agents, and particularly relates to a polyaryletherketone resin-based suspension type sizing agent and a preparation method thereof.
Background
The composite material is a material with new performance which is composed of two or more materials with different properties by a physical or chemical method. Carbon fiber is one of the most commonly used composite reinforcing phases at present due to its novel fiber material with high strength, high modulus and high temperature resistance. The polyaryletherketone resin contains rigid benzene rings in the molecular structure, has outstanding high-temperature performance, excellent mechanical property, electrical insulation property, processability and other properties, and is important high-temperature-resistant composite matrix resin. Due to the respective excellent performances of the two, the carbon fiber reinforced polyaryletherketone resin matrix composite is widely applied to high-performance fields such as aerospace, electronic automobile industry and the like, is a typical representative of the field of advanced materials, and is an important temperature-resistant and toughness-resistant engineering material.
The interface of the carbon fiber reinforced polyaryletherketone resin-based composite material is an important factor influencing the physical and chemical properties of the carbon fiber reinforced polyaryletherketone resin-based composite material. The surface of the carbon fiber is usually coated with a layer of sizing agent to improve the processing performance of the fiber and enhance the two-phase interface of the composite material. Currently, epoxy resin-based sizing agents are commonly used in industry, and prepared carbon fibers are generally used for thermosetting composite materials such as epoxy resin-based composite materials and phenolic resin-based composite materials, for example, Chinese patent (application number 201010522312.0) provides a carbon fiber emulsion sizing agent prepared by compounding a modified epoxy resin amine curing agent and epoxy resin, and the interface bonding strength of the epoxy resin-based composite materials is improved to a certain extent. However, the sizing agent has the following key problems which are difficult to solve: firstly, the interfacial adhesion capability of the epoxy resin and the polyaryletherketone resin on the surface of the carbon fiber is general, and the excellent performance of the carbon fiber reinforced polyaryletherketone composite material is difficult to exert; secondly, the carbon fiber is sized by adopting the epoxy resin-based sizing agent, and when the carbon fiber is placed for a long time or the processing temperature is higher, the epoxy resin can cause fiber agglomeration or hardening due to ring-opening curing and is difficult to disperse and spread; the thermoplastic polyaryletherketone has high melt viscosity, and the resistance to flow into the carbon fiber bundles is high when the composite material is prepared, so that the impregnation processing of the polyaryletherketone resin is greatly difficult due to the solidification and hardening of the carbon fibers subjected to epoxy sizing. Therefore, it is necessary to develop a special sizing agent for carbon fibers of polyaryletherketone resin.
At present, the research on the polyaryletherketone resin-based carbon fiber sizing agent mainly focuses on two types, namely a solvent type sizing agent and an emulsion type sizing agent. The polyaryletherketone resin is insoluble in water and only soluble in partial solvent, so that the polyaryletherketone resin can be prepared by a method of adding the solvent, but the polyaryletherketone resin has poor safety and stability and is rarely applied in the industrial field. Chinese patent (application No. 201210464424.4) provides a modified epoxy resin emulsion sizing agent prepared from a modifier, epoxy resin, a surface modifier and the like, which has certain improvement on the interface strength of a polyether-ether-ketone resin composite material. However, the main body of the epoxy resin is still epoxy resin, and the problems of storage aging, processing wettability and the like are not solved.
Disclosure of Invention
In view of the above problems, the present invention provides a polyaryletherketone resin-based suspension sizing agent for carbon fibers and a preparation method thereof. The preparation method is simple, the obtained polyaryletherketone resin-based suspension sizing agent for the carbon fibers is stable in property, and the main component of the sizing agent is polyaryletherketone resin powder, does not contain epoxy resin components, does not contain any organic solvent, and does not need any chemical modification. The sizing carbon fiber prepared by the sizing agent can be used for preparing intermediates such as prepreg and fabric for polyaryletherketone resin matrix composite materials, and has good processability and interface bonding capability.
The invention adopts the industrial polyaryletherketone resin powder, has relatively mature preparation process and lower cost, and is suitable for large-scale application. In order to solve the problems of dispersibility and stability of polyaryletherketone resin powder in water, the invention introduces a dispersant, preferably selects a polyacrylamide dispersant, can adsorb and mix with a polyaryletherketone polymer chain segment by virtue of intermolecular force and hydrogen bond action, and loses a certain degree of freedom. Meanwhile, the dispersing agent has water solubility, and molecular chain segments can freely stretch in medium water to generate a strong steric stabilization effect to prevent polyaryletherketone powder from approaching and gathering each other, so that the polyaryletherketone powder can achieve good dispersion. The invention introduces a stabilizer, preferably, alkylphenol polyoxyethylene is used as the stabilizer, which has an aryl group and can have certain affinity with polyaryletherketone powder. Meanwhile, the polyether ketone/polyacrylamide composite material has good amphipathy, and can promote the micelle particle water formed by the polyether ketone powder and the polyacrylamide dispersant to exist more stably.
The invention provides a suspension type carbon fiber sizing agent, which consists of polyaryletherketone resin, a dispersant, a stabilizer and deionized water; according to the total mass of the solid components of 100 wt%, wherein: 60-80 wt% of polyaryletherketone resin, 5-15 wt% of dispersant and 15-25 wt% of stabilizer.
In the invention, the solid component accounts for 5-30% of the total weight of the sizing agent of the polyaryletherketone resin-based suspension for the carbon fibers.
In the invention, the polyaryletherketone resin is selected from any one or more of polyether ketone PEK (formula I), polyether ether ketone PEEK (formula II), polyether ketone PEKK (formula III) or polyether ether ketone PEEKK (IV). The invention can be correspondingly adjusted according to the type of the matrix resin for the carbon fiber composite material, and the polyaryletherketone type consistent with the matrix resin is preferred.
In the invention, the number average molecular weight of the polyaryletherketone resin is between 1.5 and 3.0 ten thousand; the powder is in a powder shape, and the average diameter of the powder is 20-50 microns. Preferably, the number average molecular weight of the polyaryletherketone resin is between 2.0 and 2.5 ten thousand, and the average diameter of powder is between 30 and 40 micrometers.
In the invention, the dispersant is polyacrylamide, and the number average molecular weight of the dispersant is between 1.0 ten thousand and 3.0 ten thousand, preferably between 1.5 ten thousand and 2.0 ten thousand; the polyacrylamide has a structural general formula shown in a formula V.
Wherein n is the degree of polymerization of polyacrylamide.
In the invention, the stabilizer is alkylphenol polyoxyethylene ether and has a structural general formula shown in formula VI;
wherein R is selected from saturated aliphatic groups containing 8-20 carbon atoms; the polymerization degree n of polyoxyethylene is in the range of 30 to 50.
The invention also provides a preparation method of the polyaryletherketone resin-based suspension type carbon fiber sizing agent for carbon fibers, which comprises the following specific steps: uniformly mixing the polyaryletherketone resin, the dispersing agent and the deionized water, adding the stabilizing agent, emulsifying by using a high-speed emulsifying machine, and discharging to obtain the polyaryletherketone resin-based suspension type carbon fiber sizing agent for carbon fibers.
Compared with the prior art, the invention has the beneficial effects that:
(1) the carbon fiber surface main body prepared by the suspension sizing agent contains polyaryletherketone resin, does not contain epoxy resin, does not generate aging hardening phenomenon after long-term storage and application, and has good processing performance and interface performance with polyaryletherketone resin matrix resin.
(2) The suspension carbon fiber sizing agent provided by the invention introduces a polyacrylamide dispersant, and simultaneously introduces an alkylphenol polyoxyethylene ether stabilizer with aryl groups, so that the suspension carbon fiber sizing agent has certain affinity with polyaryletherketone powder with a large number of aryl groups. Meanwhile, the polyether ketone/polyacrylamide composite material has good amphipathy, can promote micelle particle water consisting of polyaryletherketone powder and polyacrylamide dispersant to exist more stably, and has good storage and application performance.
(3) The preparation process of the suspension carbon fiber sizing agent does not need to carry out any chemical modification on polyaryletherketone resin, does not need to add any chemical solvent, only adopts a physical mixing method in the whole process, does not generate related pollution wastes, and has high safety and environmental protection. The sizing agent has the advantages of wide raw materials, simple process, capability of being prepared by adopting general equipment and low comprehensive cost.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Comparative example 1
The epoxy resin-based sizing carbon fiber is prepared by adopting a bisphenol A/bisphenol F composite epoxy resin-based emulsion type carbon fiber sizing agent (KTM-3 type produced by Shanghai organic of Chinese academy of sciences) to perform sizing on a carbon fiber test line, wherein the concentration of the sizing agent is 2.8 percent, the dipping time is 30s, and the epoxy resin-based sizing carbon fiber is prepared by drying and filament winding.
Comparative example 2
The epoxy resin-based sizing carbon fiber is prepared by adopting bisphenol A epoxy resin-based emulsion type carbon fiber sizing agent (KTM-1 type produced by Shanghai organic of Chinese academy of sciences) to perform sizing on a carbon fiber test line, wherein the concentration of the sizing agent is 4.8 percent, the dipping time is 35s, and the epoxy resin-based sizing carbon fiber is obtained by drying and filament winding.
Examples 1 to 8
Uniformly mixing quantitative polyaryletherketone resin powder and polyacrylamide for later use; adding a certain amount of water into a stainless steel stirring kettle A, starting mechanical stirring, gradually adding the mixture at a certain rotating speed, and continuously stirring for a certain time after the mixture is completely added; transferring the aqueous mixture to a stainless steel stirring kettle B, adding quantitative alkylphenol polyoxyethylene, starting a high-speed emulsifying machine, emulsifying for a certain time at a certain rotating speed, and discharging. The polyaryletherketone resin powder is from Achima corporation of France, and the polyacrylamide and alkylphenol polyoxyethylene ether are from Pasteur corporation. The solid components of the suspension sizing agents prepared in the examples 1 to 8 are shown in table 1, the composition and the dosage of the sizing agents are shown in table 2, and the preparation process parameters of the sizing agents are shown in table 3.
The polyaryletherketone resin-based carbon fiber sizing agent prepared by the embodiment is used for sizing on a carbon fiber test line, the dipping time is 30s, and the sizing carbon fiber is prepared by drying and reeling.
TABLE 1 solid components of sizing agent
TABLE 2 sizing agent composition amounts
TABLE 3 sizing agent preparation Process parameters
Test analysis
The invention adopts a visual method to observe whether the prepared sizing agent has obvious layering; the viscosity of the prepared sizing agent was tested using a DV Pro VISCOMETER VISCOMETER from BROOKFIELD, USA; the concentration of the prepared suspension is tested by adopting a drying and weighing method, the stability of the prepared sizing agent is characterized by the change rate of the concentration of the lower layer relative to the concentration of the upper layer, and the stability is calculated according to the following formula:
lower layer concentration change rate (lower layer concentration-upper layer concentration)/upper layer concentration 100%
Testing by using an OCA20 contact angle measuring instrument to obtain a contact angle between the polyaryletherketone resin and the carbon fiber; the interfacial shear strength of the polyaryletherketone resin and the carbon fiber is obtained by testing with a MODEL HM410 interfacial performance evaluation device of the Japan Dongrong industry company.
The evaluation results of the performance of the obtained suspension sizing agent and the performance of the sized carbon fiber are shown in Table 4. As can be seen from the results in the table, the suspension sizing agent has no layering, the change rate of the lower layer concentration compared with the upper layer concentration is very small, and the emulsion type sizing agent is approximately horizontal, which shows that the suspension has uniform internal distribution and good stability. The suspension sizing agent has low overall viscosity, good fluidity, easy cleaning and good on-line manufacturability. The contact angle between the sized carbon fiber and the polyaryletherketone resin prepared by the embodiment is smaller, the polyaryletherketone resin is easier to spread and infiltrate to the surface and the inside of the carbon fiber quickly, and the prepared carbon fiber fabric and prepreg have good uniformity, few defect gaps and higher interface shear strength.
TABLE 4 evaluation results of suspension sizing agent and sized carbon fiber
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. A polyaryletherketone resin-based suspension sizing agent for carbon fibers is characterized by comprising polyaryletherketone resin, a dispersing agent, a stabilizing agent and deionized water; according to the total mass of the solid components of 100 percent, wherein: 60-80 wt% of polyaryletherketone resin, 5-15 wt% of dispersant and 15-25 wt% of stabilizer;
the dispersant is polyacrylamide, and the number average molecular weight of the dispersant is between 1.0 ten thousand and 3.0 ten thousand;
the stabilizer is alkylphenol polyoxyethylene ether and has a structural general formula shown in a formula VI;
wherein R is selected from saturated aliphatic groups containing 8-20 carbon atoms; the polymerization degree n of polyoxyethylene is in the range of 30 to 50.
2. The polyaryletherketone resin-based suspension sizing agent for carbon fibers according to claim 1, wherein: the solid component accounts for 5-30% of the total weight of the sizing agent of the polyaryletherketone resin-based suspension for the carbon fibers.
3. The polyaryletherketone resin-based suspension sizing agent for carbon fibers according to claim 1, wherein: the polyaryletherketone resin is selected from one or more of polyether ketone PEK, polyetheretherketone PEEK, polyetherketone ketone PEKK or polyetheretherketone PEEKK.
4. The polyaryletherketone resin-based suspension sizing agent for carbon fibers according to claim 1, wherein: the number average molecular weight of the polyaryletherketone resin is between 1.5 and 3.0 ten thousand; the powder is in a powder shape, and the average diameter of the powder is 20-50 microns.
5. The polyaryletherketone resin-based suspension sizing agent for carbon fibers according to claim 4, wherein: the number average molecular weight of the polyaryletherketone resin is between 2.0 and 2.5 ten thousand, and the average diameter is between 30 and 40 micrometers.
6. The polyaryletherketone resin-based suspension sizing agent for carbon fibers according to claim 1, wherein: the dispersant is polyacrylamide, and the number average molecular weight of the dispersant is between 1.5 and 2.0 ten thousand.
7. A method for preparing a polyaryletherketone resin-based suspension type carbon fiber sizing agent for carbon fibers according to any one of claims 1 to 6, which comprises the following specific steps: uniformly mixing the polyaryletherketone resin, the dispersing agent and the deionized water, adding the stabilizing agent, emulsifying by using a high-speed emulsifying machine, and discharging to obtain the polyaryletherketone resin-based suspension type carbon fiber sizing agent for carbon fibers.
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| 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 |
| CN110820315B (en) * | 2019-12-11 | 2021-05-25 | 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 |
| CN113235304B (en) * | 2021-05-31 | 2022-05-17 | 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 |
| 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 |
| CN113718528B (en) * | 2021-08-24 | 2022-10-21 | 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 |
| 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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