CN102735571A - Method for determining carbon fiber sizing agent content - Google Patents
Method for determining carbon fiber sizing agent content Download PDFInfo
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- CN102735571A CN102735571A CN2012102238138A CN201210223813A CN102735571A CN 102735571 A CN102735571 A CN 102735571A CN 2012102238138 A CN2012102238138 A CN 2012102238138A CN 201210223813 A CN201210223813 A CN 201210223813A CN 102735571 A CN102735571 A CN 102735571A
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Abstract
The invention discloses a method for determining a carbon fiber sizing agent content. Specifically, the invention discloses a rapid determining method of a sizing agent on the surface of carbon fiber through ultrasonic wave processing. The method comprises the steps that: the carbon fiber is soaked in an organic solvent; and ultrasonic wave processing is carried out in an ultrasonic instrument. The method provided by the invention is advantaged in simple operation, low cost, short detection period, and high applicability.
Description
Technical field
The present invention relates to the carbon fibre field, be specifically related to the method for testing of carbon fiber surface sizing agent content, promptly through using ultrasonic processing method fast measuring carbon fiber surface sizing agent content.
Background technology
Carbon fibre is meant that carbon fiber content is at the inorganic material fiber more than 90%; Mainly can be divided into polyacrylonitrile carbon fiber, asphalt base carbon fiber and viscose-based carbon fiber according to its material carbon fiber; The carbon fibre good combination property, the preparation technology that wherein prepare owing to the use polyacrylonitrile fibre are simple, so its output accounts for world's carbon fibre total production more than 90%.The carbon fibre excellent performance; Have that density is little, light weight, pulling strengrth and advantage such as stretch modulus is high, thermal expansivity is little, wear-resistant, corrosion-resistant; But it uses seldom separately; Usually as strengthening the occasion of body and function, like carbon fiber enhancement resin base composite material, carbon/carbon compound material, carbon fiber reinforced metal based composites etc. at fibre reinforced composites.
Starching is one important procedure in the carbon fiber production process, and its fundamental purpose is to make carbon fibre technology such as reel, weave in the later stage to be protected, and avoids the generation of lousiness and fracture of wire.Generally speaking, the market sale carbon fibre is the carbon fibre that obtains through starching.And sizing agent content is an important indicator in the sizing technique, generally need be controlled between the 0.4%-1.2%, and the sizing agent too high levels can cause tow stiff, is unfavorable for out fibre, expanding and deep processing.
At present, the measuring method of carbon fiber sizing agent content mainly comprises thermal decomposition method, extraction process.High temperature may damage the carbon fiber surface structure when using thermal decomposition method, therefore in practical operation, often uses extraction process to measure sizing agent content.Use acetone to reflux according to ISO 10548-2002 international standard and measured in 2 hours, and, calculated the phenomenon that increasing progressively appears in sizing agent content by the increase of discovering along with return time, this 2 hour time of prompting too short-range missile to cause the carbon fiber surface extraction unclean.In addition, need a large amount of loop solutions during owing to condensing reflux, therefore cause the waste of water resource.
In sum, this area presses for a kind of new method of measuring carbon fiber sizing agent content fast and accurately of research and development.
Summary of the invention
The object of the invention just provides a kind of method of measuring carbon fiber sizing agent content fast and accurately, and said method not only can effectively be removed the carbon fiber surface sizing agent fast, and practices thrift cost.
In first aspect of the present invention, a kind of method of measuring the sizing agent content of carbon fibre is provided, comprise step:
(a) mensuration has the dry weight of the carbon fibre to be measured of sizing agent, counts W1;
(b) carbon fibre to be measured is dipped in or places organic solvent, and with the said organic solvent that is impregnated with carbon fibre to be measured of ultrasonic Treatment, thereby impel sizing agent and carbon fibre to dissociate and be dissolved in said organic solvent;
(c) from said organic solvent, take out carbon fibre to be measured, and measure the dry weight of said carbon fibre, count W2; With
(d), obtain the sizing agent content of (calculating) said carbon fibre based on W1 and W2.
In another preference, ultrasonic treatment time is 3-60 minute in the step (b), preferably 5-30 minute.
In another preference, the frequency of described ultrasonic Treatment is 16,000-100,000Hz.
In another preference, described organic solvent comprises ketones solvent (acetone, butanone, MEK, espeleton, methylisobutylketone etc.), halogenated hydrocarbon solvent (methylene chloride, methenyl choloride, chlorobenzene etc.), alcohols solvent (methyl alcohol, ethanol, isopropyl alcohol etc.), fat hydrocarbon solvent (pentane, hexane, octane etc.) or its combination.
Preferably, described ketones solvent is selected from down group: acetone, butanone, MEK, espeleton, methylisobutylketone or its combination.
Preferably, described halogenated hydrocarbon solvent is selected from down group: methylene chloride, methenyl choloride, chlorobenzene or its combination.
Preferably, described alcohols solvent comprises methyl alcohol, ethanol, isopropyl alcohol or its combination.
Preferably, described fat hydrocarbon solvent comprises pentane, hexane, octane or its combination.
In another preference, described organic solvent comprises: acetone, butanone, methylene chloride or its combination.
In another preference, described organic solvent is a methylene chloride.
In another preference, also comprise in the step (c) carbon fibre to be measured that takes out is dried processing, weigh then.
In another preference, the condition that said oven dry is handled is 40-120 ℃ (preferably 50-120 a ℃), and the time is for being generally 10-100 minute.
In another preference, said carbon fibre comprises: PAN-based carbon fiber, viscose-based carbon fiber, and asphalt base carbon fiber.
In another preference, the treatment temperature of step (b) is 4 ℃ of reflux temperatures to organic solvent, preferably is 10-80 ℃.
In another preference, volume of organic solvent is 10-200ml:1-5g with the ratio of the weight of carbon fibre to be measured.Preferably, described ratio is 20-100ml:1-3g, more preferably 40-100ml:1-3g.
In another preference, in step (b), said organic solvent is arranged in the glass container of sealing.
In another preference, said method also comprises step: the carbon fibre to sloughing sizing agent carries out recycle.
In second aspect of the present invention; A kind of method of removing the sizing agent of carbon fibre is provided; Comprise step: carbon fibre to be measured is dipped in or places organic solvent; And, impel sizing agent and carbon fibre to dissociate and be dissolved in the said organic solvent, thereby remove the sizing agent of said carbon fibre with the said organic solvent that is impregnated with carbon fibre to be measured of ultrasonic Treatment.
In should be understood that within the scope of the present invention, above-mentioned each technical characterictic of the present invention and hereinafter can mutual combination between specifically described each technical characterictic in (like embodiment), thus constitute new or optimized technical scheme.As space is limited, this tired no longer one by one stating.
Embodiment
The inventor is through extensive and deep research; Be surprised to find that first; Carbon fibre to be measured is immersed in organic solvent and uses ultrasonic Treatment; Can impel sizing agent to dissociate extremely effectively and be dissolved in organic solvent, thereby significantly shorten the time of measuring sizing agent content, can foreshorten to about 20 minutes in many hours from 2-3.Accomplished the present invention on this basis.
Term
As used herein, term " is dipped in ", " being immersed in " or " place ... in " interchangeable use, point out carbon fibre to be determined is immersed in organic solvent fully.Certainly, a part that can first impregnation of carbon fibers, and then another part of impregnation of carbon fibers.As long as the each several part of carbon fibre was all flooded by organic solvent, then be regarded as this carbon fibre and be dipped in organic solvent.
The inventive method
Of the present invention a kind of method of measuring the sizing agent content of carbon fibre is provided; Comprise: the step of measuring the carbon fibre dry weight W1 that has sizing agent; Measure the step of the dry weight W2 of the carbon fibre of removing sizing agent; With the step of confirming sizing agent content based on dry weight W1 and W2; The main improvements of said method are: carbon fibre to be measured is dipped in or places organic solvent, and with the said organic solvent that is impregnated with carbon fibre to be measured of ultrasonic Treatment, thereby impel sizing agent and carbon fibre to dissociate and be dissolved in said organic solvent.
In another preference, said method comprises step:
(a) mensuration has the dry weight of the carbon fibre to be measured of sizing agent, counts W1;
(b) carbon fibre to be measured is dipped in or places organic solvent, and with the said organic solvent that is impregnated with carbon fibre to be measured of ultrasonic Treatment, thereby impel sizing agent and carbon fibre to dissociate and be dissolved in said organic solvent;
(c) from said organic solvent, take out carbon fibre to be measured, and measure the dry weight of said carbon fibre, count W2; With
(d), obtain the sizing agent content of said carbon fibre through following formula based on W1 and W2:
Carbon fibre
Can be used for the not special restriction of carbon fibre of the inventive method, can be the various carbon fibres that have or have sizing agent.Representational carbon fibre example comprises (but being not limited to): PAN-based carbon fiber, asphalt base carbon fiber or viscose-based carbon fiber.
The diameter of carbon fibre or length is restriction not, can be various stock sizes.Generally, the diameter of carbon fibre is 5-10 μ m or bigger.The not special restriction of used carbon fibre sample to be measured during measurement, its total length is generally 1-20m.In addition, when measuring, also can fiber be cut short into the staple fibre of the about 1-20cm of length.Fiber can be single or many, also can bunchy.
Organic solvent
Said organic solvent can be used for the not special restriction of organic solvent of the inventive method, as long as can dissolve carbon fiber sizing agent.Representational organic solvent example comprises (but being not limited to): the combination of ketones solvent (acetone, butanone, MEK, espeleton, methylisobutylketone or its combination), halogenated hydrocarbon solvent (methylene chloride, methenyl choloride, chlorobenzene or its combination), alcohols solvent (methyl alcohol, ethanol, isopropyl alcohol or its combination), fat hydrocarbon solvent (pentane, hexane, octane or its combination) or above-mentioned solvent.
Generally, the not special restriction of the consumption of organic solvent is as long as the organic solution of this consumption can the submergence carbon fibre or is enough to flood and the sizing agent on the dissolved carbon fiber fully.Usually, volume of organic solvent is 10-200ml:1-5g with the ratio of the weight of carbon fibre to be measured; Preferably, described ratio is 20-100ml:1-3g; More preferably, said ratio is 40-100ml:1-3g.
Ultrasonic Treatment
Can be used for the not special restriction of ultrasonic frequency of the inventive method, can be positioned at 16 for various frequencies, 000-200,000Hz, preferably 20,000-200,000Hz more preferably is 30,000-100, the ultrasound wave of 000Hz.
Can be used for the not special restriction of ultrasonic treatment time of the inventive method, be generally 3-60 minute, preferably 5-30 minute more preferably is 5-15 minute.
During ultrasonic Treatment, temperature preferably is 10-80 ℃ for being generally the reflux temperature of room temperature (as 4 ℃) to organic solvent.
Main beneficial effect of the present invention comprises:
1. measurement quick and precisely: Measuring Time shortened to about 15-20 minute from more than 2 hours, and removed slurry fully so measurement is more accurate.
2. easy and simple to handle: as, to overcome complex process in traditional extraction process owing to use ultrasonic Treatment.
3. save the energy and environmental protection: compare with circumfluence method and needn't use the required energy of heating that refluxes, and can avoid the waste of water resource.
4. remove slurry fully: under the ultrasonic Treatment condition, make surperficial sizing agent to be dissolved in rapidly in the organic solvent, therefore solve problem in the past.
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.Unless otherwise indicated, otherwise number percent and umber are percentage by weight and parts by weight.
Embodiment 1-4, ultrasonic frequency is 20000Hz; Embodiment 5-7, ultrasonic frequency is 30000Hz; Embodiment 8-10, ultrasonic frequency is 35000Hz.
Embodiment 1
In glass container, add the 80.0ml acetone soln; Take by weighing 2.2223g (being accurate to 0.0001g) carbon fibre then, carbon fibre fully is immersed in the glass container, use ultrasonic unit under 80 ℃ of conditions of temperature, to carry out sonicated; Processing time is 10min; Take out dryly then, measure and remove slurry back weight 2.1978g, and to calculate sizing agent content be 1.10wt%.
Embodiment 2
Adopt the step identical with embodiment 1, same carbon fibre sample is tested, remove heavy 2.2306g before the slurry, remove slurry back 2.2071g, calculating sizing agent content is 1.05%;
Embodiment 3
Adopt the step identical with embodiment 1, same carbon fibre sample is tested, the sonicated time is 20min, removes heavy 2.2662g before the slurry, removes slurry back 2.2398g, and calculating sizing agent content is 1.16%.
Embodiment 4
Adopt the step identical with embodiment 1, same carbon fibre sample is tested, the sonicated time is 40min, removes heavy 2.2632g before the slurry, removes slurry back 2.2365g, and calculating sizing agent content is 1.18%.
Embodiment 5
Adopt the step identical with embodiment 1, same carbon fibre sample is tested, the sonicated time is 50min, removes heavy 2.1440g before the slurry, removes slurry back 2.1192g, and calculating sizing agent content is 1.16%.
Embodiment 6
Adopt the step identical with embodiment 1, same carbon fibre sample is tested, the sonicated time is 10min, and the sonicated temperature is 70 ℃, removes heavy 2.2525g before the slurry, removes slurry back 2.2260g, and calculating sizing agent content is 1.18%.
Embodiment 7
Adopt the step identical with embodiment 1, same carbon fibre sample is tested, employings butanone is a solvent, and the sonicated time is 10min, removes heavy 2.2618g before the slurry, removes 2.2358g behind the slurry, and calculating sizing agent content is 1.15%.
Embodiment 8
Adopt the step identical with embodiment 1, same carbon fibre sample is tested, adopt methylene chloride to make solvent, the sonicated time is 60min, removes heavy 2.2669g before the slurry, removes slurry back 2.2419g, and calculating sizing agent content is 1.10%.
Embodiment 9
Adopt mixed solvent (acetone and methylene chloride volume are than the being 2:1) 60mL that adds acetone and methylene chloride in the glass container; Take by weighing the 2.2555g carbon fibre then, carbon fibre fully is immersed in the glass container, use ultrasonic unit under 60 ℃ of conditions of temperature, to carry out sonicated; Processing time is 20min; Take out dryly then, measure and remove slurry back weight 2.2313g, and to calculate sizing agent content be 1.07%.
Embodiment 10
Adopt and add methylene chloride 60mL in the glass container as solvent; Take by weighing the 2.3622g carbon fibre then, carbon fibre fully is immersed in the glass container, use ultrasonic unit under 80 ℃ of conditions of temperature, to carry out sonicated; Processing time is 10min; Take out dryly then, measure and remove slurry back weight 2.3351g, and to calculate sizing agent content be 1.15%.
Comparative Examples 1
Adopting traditional extraction process, is 80 ℃ in temperature, and return time is 3h, and the ratio of carbon fibre and acetone solvent use amount is: 2g:100mL.Measure carbon fiber sizing agent content, use the acetone circumfluence method that same sample is carried out the sizing agent content measuring, weight 2.2451g before the extracting, 2.2214g behind the extracting 3h, calculating sizing agent content is 1.06%.
Comparative Examples 2
Adopt traditional extraction process to measure carbon fiber sizing agent content, use the acetone circumfluence method that same sample is carried out the sizing agent content measuring, remove the preceding 2.1833g of slurry, extracting 2.5h removes slurry back 2.1604g, calculates sizing agent content 1.05%.
Comparative Examples 3
Adopt traditional extraction process to measure carbon fiber sizing agent content, use the acetone circumfluence method that same sample is carried out the sizing agent content measuring, remove the preceding 2.2895g of slurry, extracting 2h removes slurry back 2.2666g, calculates sizing agent content 1.00%.
Table 1 embodiment data
Table 2 Comparative Examples data
Test result through contrast table 1 and table 2 can be found out: consuming time longer when using traditional acetone circumfluence method to measure the carbon fibre rate of sizing, the rate of sizing value of measuring during backflow 3h still is lower than the rate of sizing that ultrasonic method 20min measures.This points out traditional acetone circumfluence method abundant inadequately to the dissolving of sizing agent.
Conclusion
Can find out that from the mensuration result of embodiment 1-9 the sizing agent content average out to of this carbon fibre is about 1.10%, and the mensuration result when ultrasonic Treatment 5 minutes, 10 minutes or 30 minutes differs very little.
In contrast, when measuring, extraction process, therefore need at least 3 hours consuming time ability to obtain testing result more accurately along with the time increases increase gradually.
This shows that the inventive method can impel sizing agent fully to be dissolved in the organic solvent apace, and it is accurate to measure the result.
All documents in that the present invention mentions are all quoted as a reference in this application, are just quoted such as a reference separately as each piece document.Should be understood that in addition after having read above-mentioned teachings of the present invention, those skilled in the art can do various changes or modification to the present invention, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Claims (10)
1. a method of measuring the sizing agent content of carbon fibre is characterized in that, comprises step:
(a) mensuration has the dry weight of the carbon fibre to be measured of sizing agent, counts W1;
(b) carbon fibre to be measured is dipped in or places organic solvent, and with the said organic solvent that is impregnated with carbon fibre to be measured of ultrasonic Treatment, thereby impel sizing agent and carbon fibre to dissociate and be dissolved in said organic solvent;
(c) from said organic solvent, take out carbon fibre to be measured, and measure the dry weight of said carbon fibre, count W2; With
(d), obtain the sizing agent content of said carbon fibre based on W1 and W2.
2. the method for claim 1 is characterized in that, ultrasonic treatment time is 3-60 minute in the step (b), preferably 5-30 minute.
3. the method for claim 1 is characterized in that, the frequency of described ultrasonic Treatment is 16,000-100,000Hz.
4. the method for claim 1 is characterized in that, described organic solvent comprises ketones solvent, halogenated hydrocarbon solvent, alcohols solvent, fat hydrocarbon solvent or its combination;
Preferably, described organic solvent comprises: acetone, butanone, methylene chloride or its combination.
5. method as claimed in claim 4 is characterized in that, described ketones solvent is selected from down group: acetone, butanone, MEK, espeleton, methylisobutylketone or its combination;
Described halogenated hydrocarbon solvent is selected from down group: methylene chloride, methenyl choloride, chlorobenzene or its combination;
Described alcohols solvent comprises methyl alcohol, ethanol, isopropyl alcohol or its combination;
Described fat hydrocarbon solvent comprises pentane, hexane, octane or its combination.
6. the method for claim 1 is characterized in that, in step (c), also comprises the carbon fibre to be measured that takes out is dried processing, weighs then.
7. the method for claim 1 is characterized in that, said carbon fibre comprises: PAN-based carbon fiber, asphalt base carbon fiber, viscose-based carbon fiber.
8. the method for claim 1 is characterized in that, the treatment temperature of step (b) is 4 ℃ of reflux temperatures to organic solvent, preferably is 10-80 ℃; And/or
Volume of organic solvent is 10-200ml:1-5g with the ratio of the weight of carbon fibre to be measured.
9. the method for claim 1 is characterized in that, in step (b), said organic solvent is arranged in the glass container of sealing.
10. method of removing the sizing agent of carbon fibre; It is characterized in that; Comprise step: carbon fibre to be measured is dipped in or places organic solvent; And, impel sizing agent and carbon fibre to dissociate and be dissolved in the said organic solvent, thereby remove the sizing agent of said carbon fibre with the said organic solvent that is impregnated with carbon fibre to be measured of ultrasonic Treatment.
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| CN103940695A (en) * | 2014-04-14 | 2014-07-23 | 四川城际轨道交通材料有限责任公司 | Method for testing microbial fixation strength of carbon fiber carrier |
| CN105136605A (en) * | 2015-10-09 | 2015-12-09 | 上海市环境科学研究院 | Method for measuring sizing agent content on carbon fiber and graphite fiber |
| CN105300978A (en) * | 2015-11-18 | 2016-02-03 | 北京市政路桥建材集团有限公司 | Method for detecting whether warm mix asphalt contains oil-soluble amine surfactant warm mix agent |
| CN105527373A (en) * | 2016-01-08 | 2016-04-27 | 中简科技股份有限公司 | Detection method for ammonia content of polyacrylonitrile-based carbon fiber spinning solution |
| CN107407043A (en) * | 2015-03-06 | 2017-11-28 | 东丽株式会社 | Apply the manufacture method of sizing agent carbon fiber, the manufacture method for applying sizing agent carbon fiber, carbon fibre reinforced composite and carbon fibre reinforced composite |
| CN112432877A (en) * | 2020-12-11 | 2021-03-02 | 湖北三江航天江河化工科技有限公司 | Method for measuring content of glue in heat-insulating material |
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| CN103940695A (en) * | 2014-04-14 | 2014-07-23 | 四川城际轨道交通材料有限责任公司 | Method for testing microbial fixation strength of carbon fiber carrier |
| CN107407043A (en) * | 2015-03-06 | 2017-11-28 | 东丽株式会社 | Apply the manufacture method of sizing agent carbon fiber, the manufacture method for applying sizing agent carbon fiber, carbon fibre reinforced composite and carbon fibre reinforced composite |
| CN107407043B (en) * | 2015-03-06 | 2018-06-22 | 东丽株式会社 | Apply the manufacturing method of sizing agent carbon fiber, the manufacturing method for applying sizing agent carbon fiber, carbon fibre reinforced composite and carbon fibre reinforced composite |
| CN105136605A (en) * | 2015-10-09 | 2015-12-09 | 上海市环境科学研究院 | Method for measuring sizing agent content on carbon fiber and graphite fiber |
| CN105136605B (en) * | 2015-10-09 | 2018-07-13 | 上海市环境科学研究院 | A method of measuring carbon fiber and graphite fibre starching agent content |
| CN105300978A (en) * | 2015-11-18 | 2016-02-03 | 北京市政路桥建材集团有限公司 | Method for detecting whether warm mix asphalt contains oil-soluble amine surfactant warm mix agent |
| CN105300978B (en) * | 2015-11-18 | 2018-02-09 | 北京市政路桥建材集团有限公司 | Containing oil soluble amine surfactants warm-mixing agent detection method in a kind of warm-mixed asphalt |
| CN105527373A (en) * | 2016-01-08 | 2016-04-27 | 中简科技股份有限公司 | Detection method for ammonia content of polyacrylonitrile-based carbon fiber spinning solution |
| CN112432877A (en) * | 2020-12-11 | 2021-03-02 | 湖北三江航天江河化工科技有限公司 | Method for measuring content of glue in heat-insulating material |
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Application publication date: 20121017 |