CN107447522A - A kind of preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent - Google Patents

A kind of preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent Download PDF

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Publication number
CN107447522A
CN107447522A CN201710811737.5A CN201710811737A CN107447522A CN 107447522 A CN107447522 A CN 107447522A CN 201710811737 A CN201710811737 A CN 201710811737A CN 107447522 A CN107447522 A CN 107447522A
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China
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poss
epoxy resin
carbon fiber
sizing agent
preparation
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Inventor
黄玉东
张鸶鹭
郑晓强
龙军
黎俊
张炫烽
刘丽
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Harbin Institute of Technology
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Harbin Institute of Technology
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Priority to CN201710811737.5A priority Critical patent/CN107447522A/en
Publication of CN107447522A publication Critical patent/CN107447522A/en
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/55Epoxy resins
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/647Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing polyether sequences
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/40Fibres of carbon

Abstract

A kind of preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent, belongs to sizing agent preparation field.Its step is as follows:1st, first with POSS modified surface active's agent:Specifically, POSS, surfactant and coupling agent are dissolved in organic solvent according to specific addition sequence, reacted, after go out organic solvent, that is, obtain the surfactant of POSS modifications;2nd, the preparation of epoxy resin latex type carbon fiber sizing agent:Epoxy resin is added in the surfactant modified to POSS, carries out emulsifying process, deionized water is added dropwise, the epoxy resin latex type carbon fiber sizing agent on nanoscale is finally given after phase reversal.It is an advantage of the invention that:Used POSS compares other inorganic nano-particles, has the advantages of being not easy to reunite that be evenly distributed.POSS is in the case where dosage is less, and resistance to elevated temperatures, which just has, to have greatly improved, the cost substantially reduced.

Description

A kind of preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent
Technical field
The invention belongs to sizing agent preparation field, and in particular to a kind of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent Preparation method.
Background technology
High-performance carbon fibre is indispensable critical material in the Important Project such as Aero-Space and energy petrochemical field, mesh The extensive use in major aircraft, automotive material, wind electricity blade, field drilling and part sports goods of preceding carbon fiber, This, which benefits from carbon fiber, has the premium properties such as lightweight, high-module high-strength, low bulk and highly corrosion resistant, while again because it has Standby soft machinability, it can be made into the composite of carbon fiber as reinforcing material, further expand the application of carbon fiber Field.But because carbon fiber belongs to fragile material, it wears no resistance, " fluffing " easily occurs in the technological operations such as winding weaving And phenomenon of rupture, therefore, sizing agent arises at the historic moment as " protective layer " of carbon fiber.
Originally carbon fiber sizing agent is only the solution of resin, and it is poly- that resin is generally polyurethane, epoxy resin, unsaturation Ester, vinyl acetate polymer and polyethylene glycol, even and if solvent is generally organic solvent that it can protect carbon fiber to exist well Phenomena such as fracture of wire fluffing in production process, but due to it on deflector roll easy cull, and the volatilization pole of solvent is not environmentally, because This, emulsion-type sizing agent instead of solution-type sizing agent extensively as the new protective layer in carbon fiber production process.Emulsion-type Sizing agent refers to using a kind of resin as matrix, in addition a certain amount of emulsifying agent, crosslinking agent and needs qualitative to change a certain performance Filler and auxiliary agent, through the emulsion obtained by emulsion process.It is advantageous that the residual volume on deflector roll is few, and because not molten Agent and it is pollution-free, due to there is part surface activating agent to cause machine easy cleaning in system, and can greatly improve and carbon fiber The wellability on surface, auxiliary agent and filler in system can also improve the interlaminar shear strength of carbon fibre composite simultaneously (ILSS).
With industrial expansions such as Aero-Space and automobile, wind energies, the resistance to elevated temperatures of carbon fibre composite is carried Go out higher requirement, because, at relatively high temperatures, breaking polymer chains, cause resin to be glued with carbon fiber interface Power is tied to decline.In spacecraft carbon fiber sizing agent, especially based on epoxy type sizing agent, but its heat resisting temperature is usually no more than 180 DEG C, and required tolerable temperature reaches more than 250 DEG C on its field, carbon fiber and resin matrix can reach required substantially Tolerable temperature, and the tolerable temperature of sizing agent is relatively low, therefore, it is to prepare high-temperature resistance carbon fiber to improve sizing agent resistance to elevated temperatures The key of composite.In the preparation process of sizing agent, due to having used substantial amounts of surfactant, and most surfaces are lived Property agent temperature tolerance it is relatively low so that the final temperature tolerance of sizing agent declines, therefore how to improve carbon fiber sizing agent production process The temperature tolerance of the middle surfactant used turns into the most important thing for preparing high temperature resistant sizing agent.
And the carbon fiber sizing agent in China goes modified method to be concentrated mainly on modified tree in terms of resistance to elevated temperatures at present Fat or addition nano-particle.Su Yu celerys et al. are reacted using polyethylene glycol and epoxy resin E51, have prepared carbon fiber breast Liquid type sizing agent, and demonstrated by testing and testing, the particle diameter of its emulsion is smaller, and stability is good, and TG results are shown, on The heat decomposition temperature for starching agent is 428 DEG C, good thermal stability, and the interface shearing with the sizing agent to fiber after carbon fiber starching Intensity improves 33.48%, and the lousiness amount of fiber substantially reduces.
Li Xiaofei etc., as matrix resin, is added the cooperation of emulsifying agent and auxiliary agent, has prepared PEEK from PEEK resins The carbon fiber sizing agent of base, and the sizing agent film forming and stability that prepare are all preferable, its decomposition temperature of TG analysis shows Higher than the carbon fiber sizing agent of epoxy resin, there is outstanding resistance to elevated temperatures, and improve the synthesis mechanics of composite Performance, with the raising of forming temperature, the mechanical property of the composite also increases, under conditions of 370 DEG C With higher boundary strength.
Cao Xia et al. is prepared for carbon fiber sizing agent using TPI and thermosetting epoxy resin 618, and adopts The methods of being tested with heat analysis, grain size analysis, acid base titration, contact angle determination, interface shear strength studies sizing agent performance.Knot Fruit shows that the compound sizing agent emulsion particle diameter is small, has good stability and resistance to acids and bases, at the compound starching emulsion The carbon fiber anti-wear performance of reason is improved, and the interface shear strength of carbon fiber and Bmi In Fiber Composites after starching Compared with improving 97% before starching.Sizing agent is in 350 DEG C of high temperature, when its compound interface shear strength conservation rate is up to room temperature 75.62%。
In sizing agent system, the heat resistance of epoxy resin can not show a candle to bimaleimide resin base body, and in epoxy Its chief component is emulsifying agent and epoxy resin in resin sizing agent, and the structure of emulsifying agent majority is hydrophilic polyethers Segment and hydroxyl, its heat resistance belongs to minimum in fact in whole systems, and dosage is more, therefore improves the heat resistance of emulsifying agent Compared with improving, epoxy resin heat resistance is extremely more urgent.
It is polymer-modified important method by the use of nano-particle as filler, the presence of inorganic particulate can effectively change The heat endurance of property high polymer material, inoxidizability and intensity, and can be modified and obtain excellent from molecular level Physics and chemical characteristic.And polyhedral oligomeric silsesquioxane(POSS)It is to develop most hot a kind of inorganic/organic receive in recent years Rice corpuscles, the advantage on POSS nano-scale can be such that it disperses well in the polymer, the rigidity of its cage type skeleton compared with By force, good heat-resisting quantity and oxidative resistance are made it have, and if POSS connect in a manner of chemical bond on polymer, not only It is capable of the motion of restriction molecule chain, and physical crosslinking can be produced with caused free segment after polymer decomposition, so as to increases The heat endurance of strength polymer, in addition, again because POSS three closed structures have particle diameter small, specific surface area is big, and has quantum Dimensional effect, quantum tunneling effect and interfacial effect, so as to have excellent physical property, therefore POSS is widely used in In the modification of the resin composite materials such as polyacrylic acid, polyurethane, epoxy resin.
The content of the invention
The invention aims to solve at this stage domestic carbon fibre sizing agent at high temperature molecular chain rupture and cause The problem of decline with carbon fiber interface cohesive force, there is provided a kind of system of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent Preparation Method, so as to improve the heat resistance of sizing agent, the method can effectively improve the resistance to heat decomposition temperature of sizing agent, so as to answer Among production for domestic carbon fibre composite.
To achieve the above object, the technical scheme that the present invention takes is as follows:
A kind of preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent, methods described step are as follows:
Step 1:Prepare POSS modified surface active's agent:At room temperature, by the POSS of 10 ~ 20 mass parts and the surface of 100 mass parts Activating agent is dissolved in organic solvent, and both are dispersed in organic solvent using ultrasound, and ultrasonic time is 10 ~ 20min, after Temperature is promoted to 50 ~ 120 DEG C, the coupling agent for adding 10 ~ 20 mass parts reacts 2 ~ 5h, after question response terminates, is steamed by decompression Evaporate, remove organic solvent, obtain the surfactant of POSS modifications;
Step 2:The preparation of epoxy resin carbon emulsion type carbon fiber sizing agent:Ring is added in the surfactant being modified to POSS Oxygen tree fat, the mass fraction for controlling POSS is 1% ~ 20%, between 30 ~ 70 DEG C, deionized water is added dropwise, by Phase Inversion Emulsification mistake Journey obtains the epoxy resin latex type carbon fiber sizing agent of nano-scale, wherein, the mass fraction of deionized water accounts for sizing agent 30~80%。
A kind of preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent, methods described step are as follows:
Step 1:Prepare POSS modified surface active's agent:The surfactant of 100 mass parts is put into organic solvent, 50 ~ The coupling agent of 5 ~ 15 mass parts is added under the conditions of 80 DEG C, after reacting 1 ~ 3h, the POSS of 10 ~ 20 mass parts is added and divides in ultrasound 10 ~ 20min is dissipated, is warming up to 90 ~ 120 DEG C, adds the coupling agent of 5 ~ 10 mass parts, after reacting 2 ~ 5h, through being evaporated under reduced pressure, removing has Solvent, obtain the surfactant of POSS modifications;
Step 2:The preparation of epoxy resin carbon emulsion type carbon fiber sizing agent:Ring is added in the surfactant being modified to POSS Oxygen tree fat, the mass fraction for controlling POSS is 1% ~ 20%, between 30 ~ 70 DEG C, deionized water is added dropwise, by Phase Inversion Emulsification mistake Journey obtains the epoxy resin latex type carbon fiber sizing agent of nano-scale, wherein, the mass fraction of deionized water accounts for sizing agent 30~80%。
It is of the invention to be relative to the beneficial effect of prior art:
1st, used POSS compares other inorganic nano-particles, has the advantages of being not easy to reunite that be evenly distributed.
2nd, POSS amounts used in the present invention are in the case of less, and quality accounts for resin 1%, and resistance to elevated temperatures just has Larger improvement, the cost substantially reduced.
3rd, the present invention in using introduce chemical bond energy compared to other blending inorganic nano-particles can be good at keep starching The stability of agent emulsion.
4th, by introducing POSS nano-particles, it can be good at improving the mechanical property of carbon fiber, and significantly improve starching Agent and the interface performance of carbon fiber, the carbon fiber interface shear strength after starching can improve 20%.
5th, it is small to remain to holding granularity after POSS is introduced by the present invention, the advantages of narrowly distributing.
6th, the present invention can effectively improve the resistance to elevated temperatures of carbon fiber resin matrix composite, about 280 DEG C, make its extensive Among process applied to carbon fiber production.
Embodiment
Technical scheme is further described with reference to embodiment, but is not limited thereto, it is every right Technical solution of the present invention is modified or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention, all should contain Cover in protection scope of the present invention.
Embodiment one:What present embodiment was recorded is a kind of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent Preparation method, methods described step is as follows:
Step 1:Prepare POSS modified surface active's agent:At room temperature, by the POSS of 10 ~ 20 mass parts and the surface of 100 mass parts Activating agent is dissolved in organic solvent, and both are dispersed in organic solvent using ultrasound, and ultrasonic time is 10 ~ 20min, after Temperature is promoted to 50 ~ 120 DEG C, the coupling agent for adding 10 ~ 20 mass parts reacts 2 ~ 5h, after question response terminates, is steamed by decompression Evaporate, remove organic solvent, obtain the surfactant of POSS modifications;
Step 2:The preparation of epoxy resin carbon emulsion type carbon fiber sizing agent:Ring is added in the surfactant being modified to POSS Oxygen tree fat, the mass fraction for controlling POSS is 1% ~ 20%, between 30 ~ 70 DEG C, deionized water is added dropwise, by Phase Inversion Emulsification mistake Journey obtains the epoxy resin latex type carbon fiber sizing agent of nano-scale, wherein, the mass fraction of deionized water accounts for sizing agent 30~80%。
Embodiment two:On a kind of high-temperature-resistant epoxy resin emulsion type carbon fiber described in embodiment one The preparation method of agent is starched, in step 1, the surfactant used is APES;The POSS used is epoxy radicals Cage type POSS or hydroxyl cage type POSS.
Embodiment three:On a kind of high-temperature-resistant epoxy resin emulsion type carbon fiber described in embodiment one The preparation method of agent is starched, in step 1, the organic solvent used is one kind in acetone, butanone or tetrahydrofuran;The idol used It is aliphatic diamine or aromatic diamines to join agent.
Embodiment four:On a kind of high-temperature-resistant epoxy resin emulsion type carbon fiber described in embodiment one The preparation method of agent is starched, in step 2, the epoxy resin used is epoxy resin E51 or epoxy resin E44.
Embodiment five:What present embodiment was recorded is a kind of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent Preparation method, methods described step is as follows:
Step 1:Prepare POSS modified surface active's agent:The surfactant of 100 mass parts is put into organic solvent, 50 ~ The coupling agent of 5 ~ 15 mass parts is added under the conditions of 80 DEG C, after reacting 1 ~ 3h, the POSS of 10 ~ 20 mass parts is added and divides in ultrasound 10 ~ 20min is dissipated, is warming up to 90 ~ 120 DEG C, adds the coupling agent of 5 ~ 10 mass parts, after reacting 2 ~ 5h, through being evaporated under reduced pressure, removing has Solvent, obtain the surfactant of POSS modifications;
Step 2:The preparation of epoxy resin carbon emulsion type carbon fiber sizing agent:Ring is added in the surfactant being modified to POSS Oxygen tree fat, the mass fraction for controlling POSS is 1% ~ 20%, between 30 ~ 70 DEG C, deionized water is added dropwise, by Phase Inversion Emulsification mistake Journey obtains the epoxy resin latex type carbon fiber sizing agent of nano-scale, wherein, the mass fraction of deionized water accounts for sizing agent 30~80%。
Embodiment six:On a kind of high-temperature-resistant epoxy resin emulsion type carbon fiber described in embodiment five The preparation method of agent is starched, in step 1, the surfactant used is APES;The POSS used is epoxy radicals Cage type POSS or hydroxyl cage type POSS.
Embodiment seven:On a kind of high-temperature-resistant epoxy resin emulsion type carbon fiber described in embodiment five The preparation method of agent is starched, in step 1, the organic solvent used is one kind in acetone, butanone or tetrahydrofuran;The idol used It is aliphatic diamine or aromatic diamines to join agent.
Embodiment eight:On a kind of high-temperature-resistant epoxy resin emulsion type carbon fiber described in embodiment five The preparation method of agent is starched, in step 2, the epoxy resin used is epoxy resin E51 or epoxy resin E44.
Embodiment 1:
The system for the high temperature resistant nano POSS modified epoxy type carbon fiber sizing agent surfactants that the present embodiment provides Preparation Method is divided to following two step to carry out:
First, POSS modified surface active's agent is prepared:
The POSS of 10 mass parts and 100 mass parts surfactant are dissolved in organic solvent, it is using ultrasound that both are uniform It is scattered in organic solvent, time 10min, after reaction temperature is promoted to 60 DEG C, add the coupling agent reaction of 15 mass parts 2h, after question response terminates, by being evaporated under reduced pressure, organic solvent is removed, obtains the surfactant of POSS modifications.
2nd, the preparation of carbon fiber epoxy emulsion pasting agent:
Epoxy resin E51 is added in the surfactant being modified to POSS, the mass fraction for controlling POSS is 1%, and adjustment temperature is 50 DEG C, deionized water is added dropwise, the epoxy resin latex type carbon fiber sizing agent of nano-scale is obtained by Phase Inversion Emulsification process, Wherein, the mass fraction of deionized water accounts for the 60% of sizing agent.
By carbon fiber sizing agent manufactured in the present embodiment, its particle diameter reaches 220nm.
Embodiment 2:
The present embodiment is as different from Example 1:The surfactant of 100 mass parts is put into organic solvent in step 1, The coupling agent of 5 mass parts is added under the conditions of 60 DEG C, after reacting 2h, the POSS of 10 mass parts is added and disperses in ultrasound 10min, 90 DEG C are warming up to, add the coupling agent of 10 mass parts, after reacting 2h, through being evaporated under reduced pressure, Separation of Organic and POSS Modified surfactant.
Embodiment 3:
The present embodiment is as different from Example 1:In step 2, the mass fraction of deionized water accounts for the 50% of sizing agent.
Embodiment 4:
The present embodiment is as different from Example 1:In step 2, the mass fraction of deionized water accounts for the 70% of sizing agent.
Embodiment 5:
The present embodiment is as different from Example 1:In step 2, the mass fraction for controlling POSS is 3%.
Embodiment 6:
The present embodiment is as different from Example 1:In step 2, the mass fraction for controlling POSS is 5%.
Embodiment 5 and embodiment 6 are contrasted, the results showed that, with the increase of POSS contents, its heat resistance gradually carries Rise.
Embodiment 7:
The present embodiment is as different from Example 1:In step 1, the ultrasonic disperse time is 20min.
Embodiment 8:
The present embodiment is as different from Example 1:In step 2, the epoxy resin model used is E44..

Claims (8)

  1. A kind of 1. preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent, it is characterised in that:Methods described step It is as follows:
    Step 1:Prepare POSS modified surface active's agent:At room temperature, by the POSS of 10 ~ 20 mass parts and the surface of 100 mass parts Activating agent is dissolved in organic solvent, and both are dispersed in organic solvent using ultrasound, and ultrasonic time is 10 ~ 20min, after Temperature is promoted to 50 ~ 120 DEG C, the coupling agent for adding 10 ~ 20 mass parts reacts 2 ~ 5h, after question response terminates, is steamed by decompression Evaporate, remove organic solvent, obtain the surfactant of POSS modifications;
    Step 2:The preparation of epoxy resin carbon emulsion type carbon fiber sizing agent:Ring is added in the surfactant being modified to POSS Oxygen tree fat, the mass fraction for controlling POSS is 1% ~ 20%, between 30 ~ 70 DEG C, deionized water is added dropwise, by Phase Inversion Emulsification mistake Journey obtains the epoxy resin latex type carbon fiber sizing agent of nano-scale, wherein, the mass fraction of deionized water accounts for sizing agent 30~80%。
  2. 2. according to a kind of preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent described in claim 1, its It is characterised by:In step 1, the surfactant used is APES;The POSS used is the cage type of epoxy radicals POSS or hydroxyl cage type POSS.
  3. 3. according to a kind of preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent described in claim 1, its It is characterised by:In step 1, the organic solvent used is one kind in acetone, butanone or tetrahydrofuran;The coupling agent used is Aliphatic diamine or aromatic diamines.
  4. 4. according to a kind of preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent described in claim 1, its It is characterised by:In step 2, the epoxy resin used is epoxy resin E51 or epoxy resin E44.
  5. A kind of 5. preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent, it is characterised in that:Methods described step It is as follows:
    Step 1:Prepare POSS modified surface active's agent:The surfactant of 100 mass parts is put into organic solvent, 50 ~ The coupling agent of 5 ~ 15 mass parts is added under the conditions of 80 DEG C, after reacting 1 ~ 3h, the POSS of 10 ~ 20 mass parts is added and divides in ultrasound 10 ~ 20min is dissipated, is warming up to 90 ~ 120 DEG C, adds the coupling agent of 5 ~ 10 mass parts, after reacting 2 ~ 5h, through being evaporated under reduced pressure, removing has Solvent, obtain the surfactant of POSS modifications;
    Step 2:The preparation of epoxy resin carbon emulsion type carbon fiber sizing agent:Ring is added in the surfactant being modified to POSS Oxygen tree fat, the mass fraction for controlling POSS is 1% ~ 20%, between 30 ~ 70 DEG C, deionized water is added dropwise, by Phase Inversion Emulsification mistake Journey obtains the epoxy resin latex type carbon fiber sizing agent of nano-scale, wherein, the mass fraction of deionized water accounts for sizing agent 30~80%。
  6. 6. according to a kind of preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent described in claim 5, its It is characterised by:In step 1, the surfactant used is APES;The POSS used is the cage type of epoxy radicals POSS or hydroxyl cage type POSS.
  7. 7. according to a kind of preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent described in claim 5, its It is characterised by:In step 1, the organic solvent used is one kind in acetone, butanone or tetrahydrofuran;The coupling agent used is Aliphatic diamine or aromatic diamines.
  8. 8. according to a kind of preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent described in claim 5, its It is characterised by:In step 2, the epoxy resin used is epoxy resin E51 or epoxy resin E44.
CN201710811737.5A 2017-09-11 2017-09-11 A kind of preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent Pending CN107447522A (en)

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN110128034A (en) * 2019-02-12 2019-08-16 吉林化工学院 It nano-oxide fabricated in situ and is applied in polyester-type carbon fiber sizing agent and basalt fibre/glass fiber infiltration agent
CN110184821A (en) * 2019-05-05 2019-08-30 宜兴市新立织造有限公司 A kind of alumina fibre flexible modifying agent and preparation method thereof
CN111978514A (en) * 2020-08-25 2020-11-24 哈尔滨工业大学 Preparation method of high-temperature-resistant nonionic waterborne epoxy curing agent emulsion
CN114561811A (en) * 2022-03-02 2022-05-31 安徽弋尚纺织科技有限公司 Wear-resistant cloth and preparation method thereof
CN115341392A (en) * 2022-09-23 2022-11-15 哈尔滨工业大学 Preparation method of high-temperature-resistant epoxy resin emulsion carbon fiber sizing agent

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CN105178025A (en) * 2015-09-02 2015-12-23 哈尔滨工业大学 High-temperature resistance type nanometer POSS modified epoxy emulsion carbon fiber sizing agent preparation method
CN106065528A (en) * 2016-08-18 2016-11-02 江苏恒神股份有限公司 A kind of aqueous epoxy emulsion type carbon fiber sizing agent and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN101736593A (en) * 2010-01-08 2010-06-16 哈尔滨工业大学 Preparation method of water-base epoxy resin sizing agent for carbon fiber
CN105178025A (en) * 2015-09-02 2015-12-23 哈尔滨工业大学 High-temperature resistance type nanometer POSS modified epoxy emulsion carbon fiber sizing agent preparation method
CN105178025B (en) * 2015-09-02 2017-07-04 哈尔滨工业大学 A kind of preparation method of high temperature resistant nano POSS modified epoxy emulsion carbon fiber sizing agents
CN106065528A (en) * 2016-08-18 2016-11-02 江苏恒神股份有限公司 A kind of aqueous epoxy emulsion type carbon fiber sizing agent and preparation method thereof

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110128034A (en) * 2019-02-12 2019-08-16 吉林化工学院 It nano-oxide fabricated in situ and is applied in polyester-type carbon fiber sizing agent and basalt fibre/glass fiber infiltration agent
CN110184821A (en) * 2019-05-05 2019-08-30 宜兴市新立织造有限公司 A kind of alumina fibre flexible modifying agent and preparation method thereof
CN110184821B (en) * 2019-05-05 2022-02-11 宜兴市新立织造有限公司 Alumina fiber flexible modifier and preparation method thereof
CN111978514A (en) * 2020-08-25 2020-11-24 哈尔滨工业大学 Preparation method of high-temperature-resistant nonionic waterborne epoxy curing agent emulsion
CN111978514B (en) * 2020-08-25 2022-11-29 哈尔滨工业大学 Preparation method of high-temperature-resistant nonionic waterborne epoxy curing agent emulsion
CN114561811A (en) * 2022-03-02 2022-05-31 安徽弋尚纺织科技有限公司 Wear-resistant cloth and preparation method thereof
CN114561811B (en) * 2022-03-02 2023-09-08 安徽弋尚纺织科技有限公司 Wear-resistant cloth and preparation method thereof
CN115341392A (en) * 2022-09-23 2022-11-15 哈尔滨工业大学 Preparation method of high-temperature-resistant epoxy resin emulsion carbon fiber sizing agent
CN115341392B (en) * 2022-09-23 2023-03-10 哈尔滨工业大学 Preparation method of high-temperature-resistant epoxy resin emulsion carbon fiber sizing agent

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Application publication date: 20171208