CN102899901A - High-temperature-resistant emulsion type carbon fiber sizing agent and preparation and applications of carbon fiber sizing agent - Google Patents
High-temperature-resistant emulsion type carbon fiber sizing agent and preparation and applications of carbon fiber sizing agent Download PDFInfo
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- CN102899901A CN102899901A CN2012104056878A CN201210405687A CN102899901A CN 102899901 A CN102899901 A CN 102899901A CN 2012104056878 A CN2012104056878 A CN 2012104056878A CN 201210405687 A CN201210405687 A CN 201210405687A CN 102899901 A CN102899901 A CN 102899901A
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Abstract
The invention discloses a high-temperature-resistant emulsion type carbon fiber sizing agent and a preparation method and applications of the carbon fiber sizing agent. The high-temperature-resistant emulsion type carbon fiber sizing agent contains 2-40% of high-temperature-resistant epoxy resin, 0-97.5% of water and 0.5-15% of surface active agent, wherein the high-temperature-resistant epoxy resin is a compound containing at least two epoxy groups in the molecule. The sizing agent has the characteristic of high-temperature resistance; and after the carbon fiber composite material is prepared by carbon fibers sized by the sizing agent, a sizing agent layer for playing the role of interface connection between the carbon fiber and matrix resin has extremely strong environmental adaptation, and the carbon fiber composite material still keeps high interlaminar shear strength under the condition of high temperature being 200 DEG C, so that the high integral performance of the carbon fiber composite material under high temperature condition can be ensured, the environmental adaptation of the carbon fiber composite material is enhanced, and the application range of the carbon fiber composite material is enlarged.
Description
Technical field
The invention belongs to the carbon fiber production field, be specifically related to a kind of resistant to elevated temperatures emulsion type carbon fiber sizing agent and its production and use.
Background technology
In carbon fibre reinforced composite, for using sizing agent as transition zone between the carbon fiber that strengthens and the matrix resin, sizing agent can connect carbon fiber well, can connect well matrix resin again, make carbon fibre reinforced composite become as a whole, have very strong overall performance.
Patent CN1318686C discloses a kind of carbon fiber sizing agent, this carbon fiber contains with sizing agent, (A) have at least the compound of an epoxy radicals in the molecule, (B) have with ammonium ion as the anionic surfactant to ion, (C) nonionic surface active agent.
But, use the composite that the carbon fiber after the above-mentioned carbon fiber sizing agent starching is made, because the environmental suitability as the sizing agent of transition articulamentum is not strong, raising along with temperature, its interlaminar shear strength (ILSS) fast-descending, thus the whole mechanical property of carbon fibre composite under hot conditions greatly affected.
Summary of the invention
In order to overcome the defective of existing carbon fiber sizing agent its interlaminar shear strength (ILSS) fast-descending under hot environment, primary and foremost purpose of the present invention is to provide a kind of resistant to elevated temperatures emulsion type carbon fiber sizing agent, carbon fiber through this sizing agent starching, after making carbon fibre composite, the sizing agent layer that plays the interface connection function between carbon fiber and the matrix resin has extremely strong environmental suitability, carbon fibre composite still maintains higher interlaminar shear strength under hot conditions, has guaranteed that carbon fibre composite has higher overall performance under hot conditions.
Another object of the present invention is to provide the preparation method of above-mentioned resistant to elevated temperatures emulsion type carbon fiber sizing agent.
A further object of the present invention is to provide the purposes of above-mentioned resistant to elevated temperatures emulsion type carbon fiber sizing agent.
Purpose of the present invention is achieved through the following technical solutions:
A kind of resistant to elevated temperatures emulsion type carbon fiber sizing agent, contain the composition of following mass percent:
Resistant to elevated temperatures epoxy resin: 2-40%
Water: 0-97.5%
Surfactant: 0.5-15%;
Described resistant to elevated temperatures epoxy resin refers to contain in the molecule compound of at least two epoxy radicals, the preferred many epoxy resin of phenolic aldehyde, resorcinol-formaldehyde type epoxy resin, four phenolic group ethane type epoxy resin, three hydroxyphenyl methane type epoxy resin, 4, more than one in 4 '-diaminodiphenylmethane epoxy resin (TGDDM), para-aminophenol epoxy resin (TGPAP), tricyanic epoxy resin, bicyclopentadiene dioxide (6207 resins or R-122 resin) or the titanium dioxide double cyclopentenyl ether.
The structure of above-mentioned various resistant to elevated temperatures epoxy resin is as follows:
The many epoxy resin of phenolic aldehyde (n is greater than 1 in the formula)
Resorcinol-formaldehyde type epoxy resin
Four phenolic group ethane type epoxy resin
Three hydroxyphenyl methane type epoxy resin
4,4 '-diaminodiphenylmethane epoxy resin (TGDDM)
Para-aminophenol epoxy resin (TGPAP)
Tricyanic epoxy resin
Bicyclopentadiene dioxide (6207 resins or R-122 resin)
Titanium dioxide double cyclopentenyl ether
The preferred deionized water of described water.
Surfactant is the effect of playing emulsification, and described surfactant is anion surfactant and/or non-ionic surface active agent;
Described anion surfactant is organic ammonium (ammonia) salt and/or aminated compounds, contains suc as formula 1, the hydrophobic grouping shown in formula 2, formula 3 or the formula 4:
Formula 1
Formula 2
Formula 3
Formula 4
In formula 1-4, R
1, R
2, R
3It is the chain alkyl of H or C1-C3; R
4Be the divalent aliphatic alkyl; M is the integer of 1-3.
Described non-ionic surface active agent is the polyalkylene oxide Addition on ethylene thing of senior alcohol ether type, the polyalkylene oxide Addition on ethylene thing of higher fatty acids type, polyalkylene oxide Addition on ethylene thing or the PO/EO block type polyethers of alkyl phenyl ether type; The preferred polyethylene oxide alkyl ethers of described non-ionic surface active agent, polyethylene glycol oxide alkyl phenylate, polyoxyethylene fatty acid esters, polyethylene glycol oxide aliphatic acid amino ethers, polyol fatty acid ester, polyethylene glycol oxide polyol fatty acid ester, sucrose fatty ester, alkylolamides or polyoxygenated alkyl block virtue polymers.
The preparation method of above-mentioned resistant to elevated temperatures emulsion type carbon fiber sizing agent may further comprise the steps:
Get surfactant and be added to the water, mixing; Add again epoxy resin, stir 60-100min under the rotating speed of 500-1000r/min; Then under the rotating speed of 5000-10000r/min, stir emulsification pretreatment 15-35min; At last under the rotating speed of 500-1000r/min, stir 15-25min, obtain resistant to elevated temperatures emulsion type carbon fiber sizing agent;
Described stirring all is to carry out under 40-80 ℃.
Above-mentioned resistant to elevated temperatures emulsion type carbon fiber sizing agent can be used in the carbon fibre composite, connects carbon fiber and matrix resin as transition zone.
A kind of carbon fiber contains above-mentioned resistant to elevated temperatures emulsion type carbon fiber sizing agent, and the quality of resistant to elevated temperatures emulsion type carbon fiber sizing agent is the 0.1-5% of carbon fiber gross mass.
A kind of carbon fibre composite contains above-mentioned carbon fiber.
The present invention has following advantage and effect with respect to prior art:
Sizing agent of the present invention has resistant to elevated temperatures characteristic, carbon fiber with sizing agent starching of the present invention, after making carbon fibre composite, the sizing agent layer that plays the interface connection function between carbon fiber and the matrix resin has extremely strong environmental suitability, carbon fibre composite still maintains higher interlaminar shear strength under about 200 ℃ hot conditions, guaranteed that carbon fibre composite has higher overall performance under hot conditions, strengthen the environment-adaptive type of carbon fibre composite, enlarged the scope of application of carbon fibre composite.
The specific embodiment
The present invention is described in further detail below in conjunction with embodiment, but embodiments of the present invention are not limited to this.
Embodiment 1
A kind of resistant to elevated temperatures emulsion type carbon fiber sizing agent is prepared by following steps:
The surfactant of 0.5g (Japanese emulsifying agent company/Nikon you 707-SF) is added in the deionized water of 97.5g, and agitation as appropriate mixes it; The many epoxy resin of phenolic aldehyde that add again 2g, the rotating speed with 1000r/min under 40 ℃ stirs 100min; Then under 40 ℃ with the rotating speed high speed shear emulsification 35min of 10000r/min; Rotating speed with 1000r/min stirs 25min under 40 ℃ at last, namely gets resistant to elevated temperatures emulsion type carbon fiber sizing agent.
The structure of surfactant is as follows:
Japan emulsifying agent company/Nikon that 707-SF
Embodiment 2
A kind of resistant to elevated temperatures emulsion type carbon fiber sizing agent is prepared by following steps:
With the surfactant of 1.5g (0.75g mitsubishi rayon/BPEO20SON, 0.75g mitsubishi rayon/SPEO120SON) add in the deionized water of 93.5g, agitation as appropriate mixes it; The resistant to elevated temperatures epoxy resin (2.5g resorcinol-formaldehyde type epoxy resin, 2.5g four phenolic group ethane type epoxy resin) that adds again 5g, the rotating speed with 750r/min under 60 ℃ stirs 80min; Then under 60 ℃ with the rotating speed high speed shear emulsification 25min of 7500r/min; Rotating speed with 750r/min stirs 20min under 60 ℃ at last, namely gets resistant to elevated temperatures emulsion type carbon fiber sizing agent.
The structure of surfactant is as follows:
Mitsubishi rayon/BPEO20SON
Mitsubishi rayon/SPEO120SON
Embodiment 3
A kind of resistant to elevated temperatures emulsion type carbon fiber sizing agent is prepared by following steps:
The surfactant (2.0g polyethylene oxide alkyl ethers, 1.5g polyethylene glycol oxide alkyl phenylate) of 3.5g is added in the deionized water of 86.5g, and agitation as appropriate mixes it; Add the resistant to elevated temperatures epoxy resin of 10g (5g three hydroxyphenyl methane type epoxy resin, 5g4,4 '-diaminodiphenylmethane epoxy resin), the rotating speed with 500r/min under 60 ℃ stirs 60min again; Then under 60 ℃ with the rotating speed high speed shear emulsification 15min of 5000r/min; Rotating speed with 500r/min stirs 15min under 60 ℃ at last, namely gets resistant to elevated temperatures emulsion type carbon fiber sizing agent.
Embodiment 4
A kind of resistant to elevated temperatures emulsion type carbon fiber sizing agent is prepared by following steps:
The surfactant (4g polyoxyethylene fatty acid esters, 4g polyethylene glycol oxide aliphatic acid amino ethers) of 8.0g is added in the deionized water of 72g, and agitation as appropriate mixes it; Add the resistant to elevated temperatures epoxy resin of 20g (10g para-aminophenol epoxy resin, 10g tricyanic epoxy resin), the rotating speed with 500r/min under 80 ℃ stirs 60min again; Then under 80 ℃ with the rotating speed high speed shear emulsification 15min of 5000r/min; Rotating speed with 500r/min stirs 15min under 80 ℃ at last, namely gets resistant to elevated temperatures emulsion type carbon fiber sizing agent.
Embodiment 5
A kind of resistant to elevated temperatures emulsion type carbon fiber sizing agent is prepared by following steps:
The surfactant (6g Mitsui NPES3030P, 6g polyol fatty acid ester) of 12g is added in the deionized water of 58g, and agitation as appropriate mixes it; The bicyclopentadiene dioxide that adds again 30g, the rotating speed with 750r/min under 40 ℃ stirs 100min; Then under 40 ℃ with the rotating speed high speed shear emulsification 35min of 7500r/min; Rotating speed with 750r/min stirs 25min under 40 ℃ at last, namely gets resistant to elevated temperatures emulsion type carbon fiber sizing agent.
The structure of surfactant is as follows:
Mitsui NPES3030P
Embodiment 6
A kind of resistant to elevated temperatures emulsion type carbon fiber sizing agent is prepared by following steps:
The surfactant (5g Japan emulsifying agent company/Nikon you 723-SF, 5g produce chemical industrial company/FO180EO6SON, 5g polyethylene glycol oxide polyol fatty acid ester daily) of 15g is added in the deionized water of 45g, and agitation as appropriate mixes it; The titanium dioxide double cyclopentenyl ether that adds again 40g, the rotating speed with 1000r/min under 80 ℃ stirs 80min; Then under 80 ℃ with the rotating speed high speed shear emulsification 25min of 10000r/min; Rotating speed with 1000r/min stirs 20min under 80 ℃ at last, namely gets resistant to elevated temperatures emulsion type carbon fiber sizing agent.
The structure of surfactant is as follows:
Japan emulsifying agent company/Nikon that 723-SF
Daily output chemical industrial company/FO180EO6SON
Comparative Examples 1
A kind of emulsion type carbon fiber sizing agent is prepared by following steps:
The surfactant of 0.5g (Japanese emulsifying agent company/Nikon you 707-SF) is added in the deionized water of 97.5g, and agitation as appropriate mixes it; The bisphenol A type epoxy resin that adds again 2g, the rotating speed with 1000r/min under 40 ℃ stirs 100min; Then under 40 ℃ with the rotating speed high speed shear emulsification 35min of 10000r/min; Rotating speed with 1000r/min stirs 25min under 40 ℃ at last, namely gets emulsion type carbon fiber sizing agent.
Comparative Examples 2
A kind of emulsion type carbon fiber sizing agent is prepared by following steps:
With the surfactant of 1.5g (0.75g mitsubishi rayon/BPEO20SON, 0.75g mitsubishi rayon/SPEO120SON) add in the deionized water of 93.5g, agitation as appropriate mixes it; The bisphenol A type epoxy resin that adds again 5g, the rotating speed with 750r/min under 60 ℃ stirs 80min; Then under 60 ℃ with the rotating speed high speed shear emulsification 25min of 7500r/min; Rotating speed with 750r/min stirs 20min under 60 ℃ at last, namely gets emulsion type carbon fiber sizing agent.
Comparative Examples 3
A kind of emulsion type carbon fiber sizing agent is prepared by following steps:
The surfactant (2.0g polyethylene oxide alkyl ethers, 1.5g polyethylene glycol oxide alkyl phenylate) of 3.5g is added in the deionized water of 86.5g, and agitation as appropriate mixes it; The bisphenol A type epoxy resin that adds again 10g, the rotating speed with 500r/min under 60 ℃ stirs 60min; Then under 60 ℃ with the rotating speed high speed shear emulsification 15min of 5000r/min; Rotating speed with 500r/min stirs 15min under 60 ℃ at last, namely gets emulsion type carbon fiber sizing agent.
Comparative Examples 4
A kind of emulsion type carbon fiber sizing agent is prepared by following steps:
The surfactant (4g polyoxyethylene fatty acid esters, 4g polyethylene glycol oxide aliphatic acid amino ethers) of 8.0g is added in the deionized water of 72g, and agitation as appropriate mixes it; The bisphenol A type epoxy resin that adds again 20g, the rotating speed with 500r/min under 80 ℃ stirs 60min; Then under 80 ℃ with the rotating speed high speed shear emulsification 15min of 5000r/min; Rotating speed with 500r/min stirs 15min under 80 ℃ at last, namely gets emulsion type carbon fiber sizing agent.
Comparative Examples 5
A kind of emulsion type carbon fiber sizing agent is prepared by following steps:
The surfactant (6g Mitsui NPES3030P, 6g polyol fatty acid ester) of 12g is added in the deionized water of 58g, and agitation as appropriate mixes it; The bisphenol A type epoxy resin that adds again 30g, the rotating speed with 750r/min under 40 ℃ stirs 100min; Then under 40 ℃ with the rotating speed high speed shear emulsification 35min of 7500r/min; Rotating speed with 750r/min stirs 25min under 40 ℃ at last, namely gets emulsion type carbon fiber sizing agent.
Comparative Examples 6
A kind of emulsion type carbon fiber sizing agent is prepared by following steps:
The surfactant (5g Japan emulsifying agent company/Nikon you 723-SF, 5g produce chemical industrial company/FO180EO6SON, 5g polyethylene glycol oxide polyol fatty acid ester daily) of 15g is added in the deionized water of 45g, and agitation as appropriate mixes it; The bisphenol A type epoxy resin that adds again 40g, the rotating speed with 1000r/min under 80 ℃ stirs 80min; Then under 80 ℃ with the rotating speed high speed shear emulsification 25min of 10000r/min; Rotating speed with 1000r/min stirs 20min under 80 ℃ at last, namely gets emulsion type carbon fiber sizing agent.
Use respectively the carbon fiber after the sizing agent starching of the sizing agent of embodiment and Comparative Examples to make epoxy resin base carbon fiber composite material, measure the gained carbon fibre composite under normal temperature condition and 200 ℃ of temperature conditions under interlaminar shear strength (ILSS), list in the table 1.The detection method of composite interlayer shear strength is that JC/T773-2010 fibre reinforced plastics short beam method is measured interlaminar shear strength.
Table 1 carbon fibre composite interlaminar shear strength
| The embodiment sequence number | 1 | 2 | 3 | 4 | 5 | 6 |
| Interlayer shear strength/MPa under the normal temperature | 91.28 | 92.55 | 91.47 | 92.36 | 91.77 | 92.57 |
| 200 ℃ of lower interlayer shear strength/MPa | 90.14 | 91.87 | 90.55 | 91.34 | 90.23 | 91.25 |
| The Comparative Examples sequence number | 1 | 2 | 3 | 4 | 5 | 6 |
| Interlayer shear strength/MPa under the normal temperature | 85.35 | 86.57 | 85.26 | 85.78 | 86.42 | 85.17 |
| 200 ℃ of lower interlayer shear strength/MPa | 46.78 | 47.35 | 46.36 | 46.12 | 47.58 | 46.89 |
All use resistant to elevated temperatures epoxy resin among all embodiment, and all use bisphenol A type epoxy resin in the Comparative Examples, all the other component ratios are identical.Can find out by table 1, use the sizing agent of resistant to elevated temperatures epoxy resin preparation, the carbon fibre composite that uses the carbon fiber after its starching to make, its interlayer shear strength under 200 ℃ hot conditions is substantially constant; And use the sizing agent of common bisphenol A type epoxy resin preparation, and the carbon fibre composite that uses the carbon fiber after its starching to make, its interlayer shear strength under 200 ℃ hot conditions has significantly and descends.
Above-described embodiment is the better embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under Spirit Essence of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (7)
1. resistant to elevated temperatures emulsion type carbon fiber sizing agent is characterized in that containing the composition of following mass percent:
Resistant to elevated temperatures epoxy resin: 2-40%
Water: 0-97.5%
Surfactant: 0.5-15%;
Described resistant to elevated temperatures epoxy resin refers to contain in the molecule compound of at least two epoxy radicals.
2. resistant to elevated temperatures emulsion type carbon fiber sizing agent according to claim 1, it is characterized in that: described resistant to elevated temperatures epoxy resin is the many epoxy resin of phenolic aldehyde, resorcinol-formaldehyde type epoxy resin, four phenolic group ethane type epoxy resin, three hydroxyphenyl methane type epoxy resin, 4, more than one in 4 '-diaminodiphenylmethane epoxy resin, para-aminophenol epoxy resin, tricyanic epoxy resin, bicyclopentadiene dioxide or the titanium dioxide double cyclopentenyl ether.
3. resistant to elevated temperatures emulsion type carbon fiber sizing agent according to claim 1, it is characterized in that: described surfactant is anion surfactant and/or non-ionic surface active agent.
4. the preparation method of each described resistant to elevated temperatures emulsion type carbon fiber sizing agent of claim 1-3 is characterized in that may further comprise the steps: get surfactant and be added to the water, mixing; Add again epoxy resin, stir 60-100min under the rotating speed of 500-1000r/min; Then under the rotating speed of 5000-10000r/min, stir emulsification pretreatment 15-35min; At last under the rotating speed of 500-1000r/min, stir 15-25min, obtain resistant to elevated temperatures emulsion type carbon fiber sizing agent.
5. each described resistant to elevated temperatures emulsion type carbon fiber sizing agent application in carbon fibre composite of claim 1-3.
6. carbon fiber, it is characterized in that: contain each described resistant to elevated temperatures emulsion type carbon fiber sizing agent of claim 1-3, the quality of resistant to elevated temperatures emulsion type carbon fiber sizing agent is the 0.1-5% of carbon fiber gross mass.
7. a carbon fibre composite is characterized in that: contain carbon fiber claimed in claim 6.
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| CN104294602A (en) * | 2014-09-18 | 2015-01-21 | 济南大学 | Temperature-resistant type emulsion sizing agent for carbon fiber, as well as preparation method and application of sizing agent |
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| CN106133235A (en) * | 2014-04-07 | 2016-11-16 | 陶氏环球技术有限责任公司 | Glueing composition for carbon fiber |
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| CN110273209A (en) * | 2019-07-03 | 2019-09-24 | 江苏先诺新材料科技有限公司 | A kind of high-strength fire-retarding high temperature resistant type polyimides yarn and preparation method thereof |
| CN110273209B (en) * | 2019-07-03 | 2021-01-01 | 江苏先诺新材料科技有限公司 | High-strength flame-retardant high-temperature-resistant polyimide yarn and preparation method thereof |
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Application publication date: 20130130 |