CN105586778B - A kind of low contact angle and low regain carbon fiber Wesy's emulsion pasting agent and its preparation and application - Google Patents
A kind of low contact angle and low regain carbon fiber Wesy's emulsion pasting agent and its preparation and application Download PDFInfo
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Abstract
The invention discloses a kind of low contact angle and low regain carbon fiber Wesy emulsion pasting agent, including host agent and deionized water, host agent and deionized water quality ratio are (35:65)~(55:45), and the host agent is made up of:Using after carbon fiber Wesy emulsion pasting agent starching of the invention carbon fiber and matrix resin contact angle it is small, wetting velocity is fast, and adsorption capacity is strong, and composite material interface bond strength is high.Regain is extremely low, requires carbon fiber storage condition low, long-term preservation and can not influence the physical property of fiber；Moisture-proof thermal energy power is high simultaneously, can apply under the conditions of the various complicateds such as aviation, operation on the sea.The invention also discloses the preparation methods and application method of above-mentioned carbon fiber Wesy emulsion pasting agent.
Description
Technical field
The invention belongs to carbon fiber chemical fields, and in particular to a kind of low contact angle and low regain carbon fiber emulsion starching
Agent and its preparation and application.
Background technique
Carbon fibre composite is not only aerospace and the essential new material of war industry, and transports in traffic
There is social and economic benefit outstanding in the civilian industries such as defeated, infrastructure, new energy and environmental improvement field.It is compound in carbon fiber
In the forming process of material, every process performance index of carbon fiber has the physical synthesis performance and its stability of composite material
Great influence determines the practicability and economy of composite material.
The contact angle of carbon fiber and matrix resin is to influence composite material preparation complexity and Interface adhesive strength power
An important factor for.The contact angle of carbon fiber and matrix resin is smaller, and matrix resin wetting velocity is faster when preparing composite material, system
Standby technique is simpler and more direct, economical and have selectivity；Carbon fiber adsorption resin capacity is more preferable simultaneously, the bond strength between two-phase interface
It is higher.Carbon fiber regain has the multinomial performances such as long-term storage, the humidity resistance of carbon fiber and made composite material important
It influences.The regain of starching carbon fiber is smaller, and the carbon fiber of preparation can keep quality to stablize in longer Storage period, reduces
Requirement to storage condition；Meanwhile the ability of prepared composite material moisture-proof thermal environment improves, and extends composite material and is navigating
The application range and efficiency in the fields such as sky, ocean operation.
Ideal carbon fiber sizing agent, it should make matrix resin that there is good infiltration in carbon fiber surface and sprawl energy
Power, and can have bonds well effect, interlaminar shear strength with higher with matrix resin.Prepared carbon fiber simultaneously
Regain is lower, can prepare the carbon fiber with high stability and high humidity calorific intensity.
Patent CN 101736593A is provided to be made using aqueous epoxy resins, water-soluble epoxy resin curing agent, auxiliary agent etc.
At aqueous epoxy resins sizing agent.Patent CN 1302172A removes Shui Shan using polyoxyethylene nonyl phenolic ether and polyoxyethylene
Pears alcohol monoleate is that emulsifier, potassium peroxydisulfate and sodium sulfite are that initiator prepares epoxy resin base carbon fiber cementing agent.This
Class sizing agent pays close attention to deficiency to carbon fiber and matrix resin contact angle, and due to being prepared using the method for outer emulsification, table in formula
The components such as face activating agent, curing agent are excessive, and carbon fiber regain is higher.
Summary of the invention
For above-mentioned problem, the present invention provides one kind by aromatic polyester polyol, bisphenol A epoxide resin and anion
The carbon fiber Wesy emulsion pasting agent as principal component such as surfactant, and corresponding preparation, application method.The carbon fiber
Wesy's emulsion pasting agent can improve the contact angle and regain of carbon fiber and resin after starching, make and use process without any
Organic solvent.
Specifically, the present invention provides a kind of carbon fiber Wesy emulsion pasting agent, including host agent and deionized water, host agent with
Deionized water quality ratio is (35:65)~(55:45), and the host agent is made up of:
It is preferred that the aromatic polyester polyol, can be indicated with formula (I):
Wherein, R14Selected from following one or more: the saturated or unsaturated fat of the divalent containing 1~12 carbon atom
Race's group, the O divalent aromatic group containing 6~10 carbon atoms；R15Selected from following one or more: containing 2~12 carbon
The saturated or unsaturated aliphatic group of the divalent of atom, the O divalent aromatic group containing 6~10 carbon atoms, and R14With
R15It cannot simultaneously be aliphatic group.The aromatic polyester polyol can for saturation/unsaturated aliphatic binary acid or
Its derivative, aromatic acid or derivatives thereof and saturation/unsaturated aliphatic dihydric alcohol or derivatives thereof, aromatic dicarboxylic
Alcohol or derivatives thereof is made.The present invention is not particularly limited the preparation method of aromatic polyester polyol.
It is further preferred that the aromatic polyester polyol, is selected from polyethylene terephthalate, poly- phthalic acid second two
Alcohol ester, polypropylene terephthalate, poly- O-phthalic acid propylene glycol ester, gathers to benzene two polyethylene glycol isophthalate
Formic acid butanediol ester, poly- phthalic acid butanediol ester.Most preferably, the aromatic polyester polyol is selected from poly- terephthaldehyde
Sour glycol ester, polyethylene glycol phthalate, polybutylene terephthalate (PBT).
It is further preferred that the aromatic polyester polyol, can be one or more of mixing of above-mentioned polyester polyol
Object.
It is preferred that the polymerization degree n range of the aromatic polyester polyol is 1~25, more preferably 2~12.
It is preferred that the acid value of the polyester polyol, is less than or equal to 5mg KOH/g.
It is preferred that the bisphenol A epoxide resin molecular weight ranges are 250~3500, more preferable 300~1500.
It is preferred that the bisphenol A epoxide resin is EPON 820, EPON 828, EPON 834, EPON 1001, EPON
1002, one or more in EPON 1004 (U.S.'s shell).It is preferred that the bisphenol A epoxide resin is EPON 834, EPON
1001, one or more in EPON 1002.
It is preferred that the anionic surfactant is selected to cumyl polyether-based sulfonate.It is described to cumyl polyether-based sulphur
Hydrochlorate, including but not limited to cumyl polyoxyethylene poly-oxygen propylene aether sulfonate, to cumyl polyethenoxy ether sulphonate.It is preferred that
Cumyl polyoxyethylene poly-oxygen propylene aether sulfonate is selected from disclosed in 103897172 A of Chinese patent CN to cumyl polyoxyethylene
Polyoxypropylene ether sulfonate；Described is selected from SIOC-S (n) series anionic surface-active to cumyl polyethenoxy ether sulphonate
Agent.SIOC-S (n) the series anionic surfactant such as formula (II) is shown, wherein n=6~15.
It is preferred that the antioxidant is 2,6-di-tert-butyl p-cresol.
It is preferred that the levelling agent is Siloxane-Oxyalkylene Copolymers BNK-LK380.
It is preferred that the pH value of the deionized water is 6.0~8.0, resistance is greater than 1 megohm.It is further preferred that it is described go from
The pH value of sub- water is 6.5~7.5, and resistance is greater than 10 megohms.
It is emphasized that some involved in bisphenol A epoxide resin of the invention, anionic surfactant, levelling agent
The product of the concrete model of company, it is and upper it is not intended that the component in the present invention is defined in the product of these concrete models
The product for stating other comparable manufacturers of specific model properties of product is also within the scope of the present invention.
The present invention also provides a kind of low contact angle and low regain carbon fiber Wesy emulsion pasting agent preparation method, packet
It includes:
(1) aromatic polyester polyol, bisphenol A epoxide resin, antioxidant are added in reaction vessel, 70~130
Stirring to component is completely dispersed at DEG C, configures premixed liquid；
(2) anionic surfactant, levelling agent are added in above-mentioned premixed liquid, stir 10~50min, gradually decreases body
It is temperature to 50~90 DEG C；
(3) deionized water is gradually added dropwise into said mixture, and continues to stir, carbon fiber Wesy emulsion pasting agent is made.
It is preferred that mixing temperature control is at 80~120 DEG C in step (1).
It is preferred that premixed liquid mixing time is 10~100min, more preferably 30~50min in step (1).
It is preferred that mixing time is 15~30min in step (2).
Concrete mode, the mixing time that deionized water is added dropwise to step (3) in the present invention are not particularly limited, and can be used
The modes such as lasting dropwise addition, segmentation are added dropwise, interval is added dropwise.
It will be apparent that the mixing speed, whipping temp and mixing time are only in preparation method provided by the present invention
Have an impact to sizing agent preparation time, on prepared sizing agent performance without influence.
The present invention also provides the application method of a kind of low contact angle and low regain carbon fiber Wesy emulsion pasting agent, packets
It includes:
(a) it prepares dilution: above-mentioned sizing agent is add to deionized water, it is stirring while adding, until emulsion dispersion is equal
Even bubble-free generates；
(b) carbon fiber starching: under tension, unsized carbon fiber bundle is passed through into the dipping equipped with above-mentioned dilution
Slot, after the carbon fiber bundle drying after starching on roller.
It is preferred that the concentration of host agent is 0.5~3.5wt% in sizing agent dilution described in step (a).
It is preferred that non-starching carbon fiber bundle described in step (b) is by the non-starching carbon fiber group of T300~T1000 grades of 3K~12K
At.
It is preferred that the dip time in dipping tank of non-starching carbon fiber bundle described in step (b) is 10~50s, more preferably
15~30s.
It is preferred that the carbon fiber bundle drying mode in step (b) after starching is hot-air seasoning, temperature is 100~170 DEG C, more
Preferably 120~160 DEG C；Drying time is 1~5 minute, more preferably 1.5~3 minutes.
It is preferred that acted in step (b) non-starching carbon fiber bundle tension be 100~1000cN, preferably 200~
500cN。
It is preferred that the control of carbon fiber starching amount is in 0.2~5.0wt% in step (b).
It is preferred that starching carbon fiber and matrix resin surface contact angle < 25 ° obtained in step (b), regain <
0.15%.
It will be apparent that present invention only provides one of the application method of the carbon fiber Wesy emulsion pasting agent,
The technological parameters such as middle host agent concentration, dip time, drying temperature and time, fiber tension are to prepared starching carbon fiber performance
Without influence.
Beneficial effect
1. the contact angle of carbon fiber and matrix resin after the starching of this sizing agent is small, matrix resin wetting velocity can be improved
And adsorption capacity, prepared composite material interface bond strength are high.
2. the carbon fiber regain after the starching of this sizing agent is low, Storage period is longer, and economic benefit is more preferably；It is prepared compound
The wet-hot aging performance of material is strong, can apply under the conditions of various complicated.
Detailed description of the invention
Fig. 1 SIOC-S7 anionic surfactant1H-NMR nuclear magnetic spectrum
Specific embodiment
The present invention is specifically described by the following examples, it will help the understanding of the present invention, but be not intended to limit
The contents of the present invention.
Raw material in following embodiment, are such as not particularly illustrated, and are commercially available.
The testing performance index method of starching carbon fiber:
1, the contact angle of starching carbon fiber and matrix resin
It tests to obtain with surface tension instrument using German DataPhysics company DCAT21 type dynamic contact angle, matrix tree
Rouge selects epoxy resin ON 828.
2, starching carbon fiber interlaminar shear strength (ILSS)
Select epoxy AG80 resin, sample preparation and test referring to " GB 3357-1982 unidirectional fibre reinforced plastics interlayer shearing
Strength Testing Methods " test obtain.
3, the regain of starching carbon fiber
It tests to obtain using weighting method after dried, normal pressure drying, 110 DEG C of drying temperature.
4, starching carbon fiber convergence
It is graded using feel ocular estimate, Index grading is ●-very well；Zero-is good；△-is bad；×-poor.
103897172 A of Chinese patent CN can refer to cumyl polyoxyethylene poly-oxygen propylene aether sulfonic acid salt production process.
SIOC-S (n) series anionic surfactant prepares embodiment
By equimolar p -cumylphenol (No. CAS: 599-64-4) and ethylene oxide (polymerization degree n=6~15) (No. CAS:
75-21-8) under the action of catalyst KOH (No. CAS: the 1310-58-3) of p -cumylphenol weight 1.3wt%, 130~
150 DEG C, 100~200min of opening is made to cumyl phenol polyethenoxy ether under pressure 0.9Mpa；Then it sequentially adds
Sulfur trioxide (No. CAS: 7446-11-9) and pyridine (No. CAS: 110-86-1) react 30~50min to hydroxyl at 50~90 DEG C
Base carries out sulfonation, wherein being 1:1:15 to cumyl phenol polyethenoxy ether and sulfur trioxide, pyridine molar ratio；It is eventually adding to cumyl
The ammonium hydroxide (No. CAS: 1336-21-6) that 1.2 times of phenol polyethenoxy ether molal quantity reacts 30~50min at 40~120 DEG C and carries out
Ammonium obtains SIOC-S (n) series anionic surfactant.Fig. 1 is SIOC-S7 anion surface active obtained
The 1H-NMR nuclear magnetic spectrum of agent.
One, prepared by sizing agent
Aromatic polyester polyol component is taken (to be synthesized by Shanghai Organic Chemistry Institute, Chinese Academy of Sciences, abbreviation Shanghai has
Machine institute), bisphenol A epoxide resin (being produced by Shell Co. Ltd, the U.S.), antioxidant DBPC 2,6 ditertiary butyl p cresol is (by Chinese medicines group
Production) it is added in 500ml four-hole boiling flask, 40min is stirred at a temperature of 110 DEG C to be completely dispersed to component.Then be added yin from
Sub- surfactant (see above-mentioned preparation example), levelling agent Siloxane-Oxyalkylene Copolymers BNK-LK380 are (raw by BNK company, the U.S.
Produce), after stirring 20min, gradually decrease temperature.When pot temperature is down to 75 DEG C, start that deionized water is added dropwise into flask
And continue to stir.When total amount of dripping reaches certain mass, stop reaction, carbon fiber Wesy emulsion pasting agent is made.
Each raw material component used is shown in Table 1 in above-mentioned preparation process, and the dosage of each raw material component is shown in Table 2.
1 raw material components table of table
2 raw material components scale of table
Two, sizing agent application
Take emulsion pasting agent obtained above, be slowly added into deionized water, it is stirring while adding until bubble-free generate,
The sizing agent dilution that host agent content is 2wt% is made.The above-mentioned sizing agent dilution of 500g is added in sizing groove, makes T800 grades
6K carbon fiber is impregnated in the case where keeping 300cN tension by sizing groove, and control makes dip time 30s by speed.Then
By hot-air drying stove, 2min is dried under 140 DEG C of high temperature, then winding is on plastic drum.
Prepared starching carbon fiber Evaluation results are shown in Table 3.
3 starching carbon fiber the performance test results of table
Although the present invention is disclosed above by preferred embodiment, however, it is not to limit the invention, any to be familiar with this skill
Skill person, without departing from the spirit and scope of the present invention, when can make it is various change and retouch, because the protection scope of the invention should be with
Subject to the scope of the claims applied for a patent.
Claims (20)
1. a kind of low contact angle and low regain carbon fiber Wesy emulsion pasting agent, which is characterized in that including host agent and deionized water,
Host agent and deionized water quality ratio are (35:65)~(55:45), and the host agent is made up of:
The polymerization degree n range of the aromatic polyester polyol is 1~25.
2. low contact angle according to claim 1 and low regain carbon fiber Wesy emulsion pasting agent, which is characterized in that described
Aromatic polyester polyol, with formula (I) indicate:
Wherein, R14Selected from following one or more: the saturated or unsaturated fatty group of the divalent containing 1~12 carbon atom
Group, the O divalent aromatic group containing 6~10 carbon atoms；R15Selected from following one or more: containing 2~12 carbon atoms
The saturated or unsaturated aliphatic group of divalent, the O divalent aromatic group containing 6~10 carbon atoms, and R14And R15No
It can simultaneously be aliphatic group.
3. low contact angle according to claim 2 and low regain carbon fiber Wesy emulsion pasting agent, which is characterized in that described
Aromatic polyester polyol, be polyethylene terephthalate, polyethylene glycol phthalate, poly- M-phthalic acid second
Diol ester, polypropylene terephthalate, poly- O-phthalic acid propylene glycol ester, polybutylene terephthalate (PBT), poly- adjacent benzene
It is one or more in dioctyl phthalate butanediol ester.
4. low contact angle according to claim 1-3 and low regain carbon fiber Wesy emulsion pasting agent, feature
It is, the acid value of the aromatic polyester polyol, is less than or equal to 5mg KOH/g.
5. carbon fiber Wesy according to claim 1 emulsion pasting agent, which is characterized in that the bisphenol A epoxide resin molecule
Measuring range is 250~3500.
6. low contact angle according to claim 5 and low regain carbon fiber Wesy emulsion pasting agent, which is characterized in that described
Bisphenol A epoxide resin is EPON 820, EPON 828, EPON 834, EPON 1001, EPON 1002, a kind of in EPON 1004
Or it is a variety of.
7. low contact angle according to claim 1 and low regain carbon fiber Wesy emulsion pasting agent, which is characterized in that described
Anionic surfactant is selected to cumyl polyether-based sulfonate.
8. low contact angle according to claim 1 and low regain carbon fiber Wesy emulsion pasting agent, which is characterized in that described
Antioxidant be DBPC 2,6 ditertiary butyl p cresol.
9. low contact angle according to claim 1 and low regain carbon fiber Wesy emulsion pasting agent, which is characterized in that described
Levelling agent be Siloxane-Oxyalkylene Copolymers BNK-LK380.
10. low contact angle according to claim 1 and low regain carbon fiber Wesy emulsion pasting agent, which is characterized in that institute
The pH value for stating deionized water is 6.0~8.0, and resistance is greater than 1 megohm.
11. a kind of prepare the described in any item low contact angles of claim 1-10 and emulsion pasting agent side, low regain carbon fiber Wesy
Method, comprising:
(1) aromatic polyester polyol, bisphenol A epoxide resin, antioxidant are added in reaction vessel, at 70~130 DEG C
Stirring to component is completely dispersed, and configures premixed liquid；
(2) anionic surfactant, levelling agent are added in above-mentioned premixed liquid, stir 10~50min, gradually decreases system temperature
Degree is to 50~90 DEG C；
(3) deionized water is gradually added dropwise into said mixture, and continues to stir, carbon fiber Wesy emulsion pasting agent is made.
12. preparation starching agent method according to claim 11, which is characterized in that premixed liquid mixing time in step (1)
For 10~100min.
13. a kind of use of the described in any item low contact angles of claim 1-10 and low regain carbon fiber Wesy emulsion pasting agent
Method, comprising:
(a) it prepares dilution: above-mentioned sizing agent is add to deionized water, it is stirring while adding, until the uniform nothing of emulsion dispersion
Bubble generates；
(b) carbon fiber starching: under tension, by unsized carbon fiber bundle by be equipped with above-mentioned dilution dipping tank,
After drying on roller.
14. sizing agent application method according to claim 13, which is characterized in that starching dilution agent described in step (a)
The concentration of host agent is 0.5~3.5wt% in liquid.
15. sizing agent application method according to claim 13, which is characterized in that non-starching carbon fiber described in step (b)
Dimension beam is made of the non-starching carbon fiber of T300~T1000 grades of 3K~12K.
16. sizing agent application method according to claim 13, which is characterized in that non-starching carbon fiber described in step (b)
Tieing up beam dip time in dipping tank is 10~50s.
17. sizing agent application method according to claim 13, which is characterized in that the carbon fiber in step (b) after starching
Beam drying mode is hot-air seasoning, and temperature is 100~170 DEG C；Drying time 1~5 minute.
18. sizing agent application method according to claim 13, which is characterized in that act on non-starching carbon in step (b)
The tension of fibre bundle is 100~1000cN.
19. sizing agent application method according to claim 13, which is characterized in that carbon fiber starching amount control in step (b)
System is in 0.2~5.0wt%.
20. sizing agent application method according to claim 13, which is characterized in that obtained starching carbon in step (b)
Fiber and matrix resin surface contact angle < 25 °, regain < 0.15%.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1701148A (en) * | 2001-05-25 | 2005-11-23 | 三菱丽阳株式会社 | Sizing agent for carbon fiber, aqueous dispersion thereof, carbon fiber treated by sizing, sheet-form object comprising the carbon fiber, and carbon fiber-reinforced composite material |
| CN103161073A (en) * | 2013-03-26 | 2013-06-19 | 金发科技股份有限公司 | Emulsion carbon fiber sizing agent and preparation method and application thereof |
| CN103890261A (en) * | 2011-10-21 | 2014-06-25 | 松本油脂制药株式会社 | Sizing agent for carbon fibers, carbon fiber strand, and fiber-reinforced composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4278970B2 (en) * | 2002-12-16 | 2009-06-17 | 三菱レイヨン株式会社 | Carbon fiber bundle and chopped carbon fiber bundle for fiber reinforced resin and carbon fiber reinforced resin composition exhibiting high mechanical properties and low electrical conductivity |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1701148A (en) * | 2001-05-25 | 2005-11-23 | 三菱丽阳株式会社 | Sizing agent for carbon fiber, aqueous dispersion thereof, carbon fiber treated by sizing, sheet-form object comprising the carbon fiber, and carbon fiber-reinforced composite material |
| CN103890261A (en) * | 2011-10-21 | 2014-06-25 | 松本油脂制药株式会社 | Sizing agent for carbon fibers, carbon fiber strand, and fiber-reinforced composite material |
| CN103161073A (en) * | 2013-03-26 | 2013-06-19 | 金发科技股份有限公司 | Emulsion carbon fiber sizing agent and preparation method and application thereof |
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