CN108731992A - A kind of preparation method of carbon fiber bundle filament test batten - Google Patents

A kind of preparation method of carbon fiber bundle filament test batten Download PDF

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Publication number
CN108731992A
CN108731992A CN201810250707.6A CN201810250707A CN108731992A CN 108731992 A CN108731992 A CN 108731992A CN 201810250707 A CN201810250707 A CN 201810250707A CN 108731992 A CN108731992 A CN 108731992A
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China
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preparation
fibre bundle
aqueous epoxy
maceration extract
aqueous
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CN201810250707.6A
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Inventor
童元建
徐樑华
曹维宇
李常清
高爱君
王宇
赵振文
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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Priority to CN201810250707.6A priority Critical patent/CN108731992A/en
Publication of CN108731992A publication Critical patent/CN108731992A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/30Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat

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  • General Health & Medical Sciences (AREA)
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  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Reinforced Plastic Materials (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The present invention relates to a kind of preparation methods of carbon fiber bundle filament test batten, using the aqueous solution of aqueous epoxy resins and aqueous epoxy resin curing agent as maceration extract, carbon fibre tow is subjected to pre-soaking processing with phosphoric acid ester adhesion promoter before dipping, and some tension is applied to carbon fibre tow in dipping process, obtain mechanical property test of carbon fiber batten after baking and curing.The present invention solves the disadvantage that the test of traditional carbon fibres synnema with batten preparation process is largely solvent using acetone, it is difficult to solve the problems, such as that aqueous epoxy resins aqueous solution adheres to as maceration extract simultaneously, it is quick with operation, it is simple and practicable, have many advantages, such as asepsis environment-protecting.

Description

A kind of preparation method of carbon fiber bundle filament test batten
Technical field
The present invention relates to a kind of preparation methods of carbon fiber bundle filament test batten, belong to testing research field.
Background technology
Carbon fiber has the characteristics that high specific strength, high ratio modulus, high temperature resistant, corrosion-resistant, electrical and thermal conductivity is good, is advanced multiple The important reinforcement of condensation material, is widely used in the fields such as space flight and aviation, communications and transportation, building energy and Leisure Sport.? In the preparation of carbon fiber, production and application process, the mechanical property of characterization carbon fiber accurately and timely and its important.Due to carbon fiber The tow that product is a large amount of carbon mono-filaments composition is tieed up, Mechanics Performance Testing is divided into monofilament method and synnema method, wherein monofilament method Sample prepares before need not particularly testing, and has the characteristics that simple and quick, but usual test result is discrete larger, test process Human factor is more, is gradually replaced by synnema method.Synnema method refer to test process fibre bundle as a whole into Row test to ensure all monofilament while stress in test process tow needs that carbon fibre tow is prepared into survey before testing Testing bar.Epoxy resin infusion process is generally used to carry out the preparation of carbon fiber bundle filament test batten at present, this method uses acetone For solvent dissolved epoxy, prepared batten can accurately reflect the mechanical property of carbon fiber.But acetone is a kind of easy Volatile organic solvent, itself has certain toxicity, and is that one kind easily system poison easily makes quick-fried chemicals, belongs to national strictly pipe The chemicals of control suffers from stringent management and control measures, to the timely of carbon fiber mechanical property to production, purchase, transport and use Accurate test brings many difficulties.Carbon fiber bundle filament test batten directly is prepared using aqueous epoxy resins, there are resins The problems such as, poor adhesive force poor to fiber coherent, batten test result accuracy are poor, discrete big.
Invention content
The object of the present invention is to provide a kind of using aqueous epoxy resins as the carbon fiber bundle filament test batten of impregnating agent Preparation method.Using the aqueous solution of aqueous epoxy resins and aqueous epoxy resin curing agent as maceration extract, by carbon before dipping Fibre bundle carries out pre-soaking processing with phosphoric acid ester adhesion promoter, and applies centainly to carbon fibre tow in dipping process Tension obtains mechanical property test of carbon fiber batten after baking and curing, solves traditional carbon fibres multifilament test batten system The shortcomings that standby process largely uses acetone to be solvent, while solving aqueous epoxy resins aqueous solution and adhering to difficulty as maceration extract The problem of.
For achieving the above object, concrete scheme is as follows:Via the configuration of maceration extract, the dipping of fibre bundle, solidification It is obtained with removing for fibre bundle, fibre bundle pre-soaking processing is carried out before fibre bundle dipping, the maceration extract is by aqueous Epoxy resin and aqueous epoxy resin curing agent composition.
The solid content of the aqueous epoxy resins is 40%~55%, and epoxide equivalent value is 0.16~0.25mol/ 100g, viscosity are 250~1000cps.
The solid content of the aqueous epoxy resin curing agent is 40%~55%, and amine hydrogen equivalent value is 150~280, is glued Degree is 1000~3000cps.
Specific steps include as follows:
(1) configuration of maceration extract:Deionized water will be added in aqueous epoxy resins, stir evenly, is configured to epoxy resin The aqueous solution that mass percent is 20%~38%;Then aqueous epoxy resin curing agent is added, stirs evenly, aqueous ring is made The mass ratio of oxygen resin maceration extract, curing agent and aqueous epoxy resins is 0.5~1:1;
(2) fibre bundle pre-treatment:Carbon fibre tow is wrapped on fixed frame, winding process applies of 1~10N Power is impregnated 1~5 minute in mass percent concentration is 1~5% adhesion promoter aqueous solution;
The adhesion promoter is phosphate compounds, is epoxy phosphate ester, methacrylic acid phosphoric acid ester, 2- hydroxyls One or several kinds in ethyl methacrylate phosphate.
Adhesion promoter effectively increases the interaction between carbon fibre tow and aqueous epoxy resins, increases carbon fiber The adhesion amount for tieing up epoxy resin on tow enhances epoxy resin and interfibrous interaction after solidification, improves filament The boundling effect of beam.
(3) dipping of fibre bundle:Step (2) treated fibre bundle is placed in the aqueous ring of step (1) together with frame It is impregnated 1~20 minute in oxygen resin maceration extract;
(4) solidification of fibre bundle:Carbon fibre tow is stood 1~5 minute after being taken out in maceration extract together with frame, is put Enter baking and curing 1~10 hour in 90~140 DEG C of baking oven;
(5) removing for fibre bundle refers to being removed carbon fibre tow from fixed frame using tools such as scissors.
The advantages of the present invention:
The present invention provides a kind of preparation methods of carbon fiber bundle filament test sample, solve the survey of traditional carbon fibres synnema The shortcomings that batten preparation process on probation largely uses acetone to be solvent, has test result accurate, and operation is quick, simple and practicable, Has many advantages, such as asepsis environment-protecting.
Specific implementation mode
Embodiment 1
(1) configuration of aqueous epoxy resins maceration extract:Aqueous epoxy resins F0404 (solid content 45%, epoxide equivalent Value be 0.18mol/100g, viscosity 300cps) in be added deionized water, stir evenly, be configured to epoxy resin quality percentage Than the aqueous solution for 30%;Aqueous epoxy resin curing agent F0405 is added, and (solid content 50%, amine hydrogen equivalent value are 200, viscosity For 1500cps), the mass ratio of aqueous epoxy resins and aqueous epoxy resin curing agent is 1:1;It stirs evenly, aqueous ring is made Oxygen resin maceration extract;
(2) fibre bundle pre-treatment:The T800 grade 12K carbon fibre tows that toray company produces are wrapped in fixed frame On, winding process applies the tension of 5N, is impregnated 3 minutes in mass ratio is 1% epoxy phosphate aqueous solution of ester;
(3) dipping of fibre bundle:Step (2) treated fibre bundle is placed in the water-base epoxy of step (1) together with frame It is impregnated 3 minutes in resin maceration extract;
(4) cure:Carbon fibre tow stands 2 minutes together with frame after being taken out in maceration extract, is put into 120 DEG C of baking oven Baking and curing 3 hours;
(5) fibre bundle is removed:Carbon fibre tow is removed from fixed frame using tools such as scissors.
Embodiment 2
(1) configuration of aqueous epoxy resins maceration extract:Aqueous epoxy resins F0404 (solid content 45%, epoxide equivalent value For 0.20mol/100g, viscosity 600cps) in be added deionized water, stir evenly, be configured to epoxy resin mass percent For 25% aqueous solution;Aqueous epoxy resin curing agent F0405 is added, and (solid content 50%, amine hydrogen equivalent value are 250, and viscosity is 1500cps), the mass ratio of aqueous epoxy resins and aqueous epoxy resin curing agent is 0.75:1, it stirs evenly, aqueous ring is made Oxygen resin maceration extract;
(2) fibre bundle pre-treatment:The T800 grade 12K carbon fibre tows that toray company produces are wrapped in fixed frame On, winding process applies the tension of 3N, is impregnated 1 minute in mass ratio is 2% methacrylic acid phosphoric acid ester aqueous solution;
(3) dipping of fibre bundle:Step (2) treated fibre bundle is placed in the water-base epoxy of step (1) together with frame It is impregnated 15 minutes in resin maceration extract;
(4) cure:Carbon fibre tow stands 4 minutes together with frame after being taken out in maceration extract, is put into 110 DEG C of baking oven Baking and curing 5 hours;
(5) fibre bundle is removed:Carbon fibre tow is removed from fixed frame using tools such as scissors.
Embodiment 3
(1) (2) are the same as embodiment 1;
(3) dipping of fibre bundle:Step (2) treated fibre bundle is placed in the water-base epoxy of step (1) together with frame It is impregnated 10 minutes in resin maceration extract;
(4) cure:Carbon fibre tow stands 2 minutes together with frame after being taken out in maceration extract, is put into 130 DEG C of baking oven Baking and curing 2 hours;
(5) fibre bundle is removed:Carbon fibre tow is removed from fixed frame using tools such as scissors.
Comparative example
(1) the recipe configuration maceration extract that GB/T3362-2005 recommends, in mass ratio, epoxy resin E51 are pressed:Triethylene four Amine:Acetone=10:1:20;
(2) the T800 grade 12K carbon fibre tows that toray company produces are wrapped on fixed frame, winding process is applied The tension for adding 8N is subsequently placed in the maceration extract of step (1) and impregnates 10 minutes;
(3) carbon fibre tow stands 2 minutes together with frame after being taken out in maceration extract, is put into 130 DEG C of baking oven and dries Solidification 2 hours;
(4) carbon fibre tow is removed from fixed frame using tools such as scissors.
After reinforced sheet is pasted at the carbon fiber batten both ends that above-described embodiment and comparative example are obtained, according to GB/T3362- 2005 test method carries out tensile property test, and test result is listed in table 1.Carbon fiber sample prepared by method using the present invention Item can accurately reflect intrinsic tensile mechanical properties.
Table 1

Claims (10)

1. a kind of preparation method of carbon fiber bundle filament test batten, via the configuration of maceration extract, fibre bundle dipping, solidification and Removing for fibre bundle is obtained, it is characterised in that the maceration extract is aqueous epoxy resins and aqueous epoxy resin curing agent Aqueous solution.
2. preparation method according to claim 1, it is characterised in that the solid content of the aqueous epoxy resins be 40%~ 55%, epoxide equivalent value is 0.16~0.25mol/100g, and viscosity is 250~1000cps.
3. preparation method according to claim 1, it is characterised in that the solid content of the aqueous epoxy resin curing agent is 40%~55%, amine hydrogen equivalent value is 150~280, and viscosity is 1000~3000cps.
4. preparation method according to claim 1, it is characterised in that the configuration of the maceration extract refers to by water-base epoxy Deionized water is added in resin, stirs evenly, is configured to the aqueous solution that epoxy resin mass percent is 20%~38%;Then Aqueous epoxy resin curing agent is added, stirs evenly, is made aqueous epoxy resins maceration extracts, curing agent and aqueous epoxy resins Mass ratio is 0.5~1:1.
5. preparation method according to claim 1, it is characterised in that first carry out fibre bundle preimpregnation before fibre bundle dipping Bubble processing.
6. preparation method according to claim 5, it is characterised in that the pre-soaking processing of the fibre bundle refers to by carbon Fibre bundle is wrapped on fixed frame, winding process apply 1~10N tension, be subsequently placed in mass percent concentration be 1~ It is impregnated 1~5 minute in 5% phosphoric acid ester adhesion promoter aqueous solution.
7. preparation method according to claim 6, it is characterised in that the phosphoric acid ester adhesion promoter is epoxy One or several kinds in phosphate, methacrylic acid phosphoric acid ester, 2- hydroxy ethyl methyl acrylated phosphates.
8. preparation method according to claim 1, it is characterised in that the dipping of the fibre bundle is to handle pre-soaking Fibre bundle afterwards impregnates 1~20 minute together with frame in aqueous epoxy resins maceration extract.
9. preparation method according to claim 1, it is characterised in that the solidification refers to by carbon fibre tow together with frame Frame from maceration extract take out after stand 1~after five minutes, at a temperature of 90~140 DEG C, baking and curing 1~10 hour.
10. preparation method according to claim 1, it is characterised in that removing for the fibre bundle refers to utilizing scissors Equal tools remove carbon fibre tow from fixed frame.
CN201810250707.6A 2018-03-26 2018-03-26 A kind of preparation method of carbon fiber bundle filament test batten Pending CN108731992A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111562279A (en) * 2020-05-11 2020-08-21 江苏恒神股份有限公司 Characterization method of skin-core structure of pre-oxidized fiber
CN111638112A (en) * 2020-05-29 2020-09-08 威海拓展纤维有限公司 Preparation method of carbon fiber bundle wire test sample strip

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CN102809499A (en) * 2012-08-15 2012-12-05 中国科学院宁波材料技术与工程研究所 Sample preparation method for carbon fiber tensile property test
CN104120605A (en) * 2014-07-16 2014-10-29 哈尔滨工业大学 Carbon nanotube modified emulsion sizing agent, preparation method and applications thereof
CN105043840A (en) * 2015-09-21 2015-11-11 核工业理化工程研究院 Large-tow carbon fiber tensile sample manufacturing method

Patent Citations (4)

* Cited by examiner, † Cited by third party
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
CN102809499A (en) * 2012-08-15 2012-12-05 中国科学院宁波材料技术与工程研究所 Sample preparation method for carbon fiber tensile property test
CN104120605A (en) * 2014-07-16 2014-10-29 哈尔滨工业大学 Carbon nanotube modified emulsion sizing agent, preparation method and applications thereof
CN105043840A (en) * 2015-09-21 2015-11-11 核工业理化工程研究院 Large-tow carbon fiber tensile sample manufacturing method

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111562279A (en) * 2020-05-11 2020-08-21 江苏恒神股份有限公司 Characterization method of skin-core structure of pre-oxidized fiber
CN111638112A (en) * 2020-05-29 2020-09-08 威海拓展纤维有限公司 Preparation method of carbon fiber bundle wire test sample strip

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Application publication date: 20181102