CN106317786A - Method for preparing polyester fiber reinforced epoxy composite material based on ultraviolet radiation modification - Google Patents
Method for preparing polyester fiber reinforced epoxy composite material based on ultraviolet radiation modification Download PDFInfo
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- CN106317786A CN106317786A CN201510814620.3A CN201510814620A CN106317786A CN 106317786 A CN106317786 A CN 106317786A CN 201510814620 A CN201510814620 A CN 201510814620A CN 106317786 A CN106317786 A CN 106317786A
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- terylene
- ultraviolet radiation
- reinforced epoxy
- epoxy composite
- method based
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Abstract
The invention provides a method for preparing a polyester fiber reinforced epoxy composite material based on ultraviolet radiation modification and relates to a resin-matrix composite material. The method comprises the following steps of: grafting active groups including acylamino and carboxyl to the surface of the polyester fiber by virtue of ultraviolet radiation modification; compositing epoxy resin with a polyester fiber fabric by virtue of a vacuum flow guide technique; and curing the resin, thereby obtaining the polyester fiber reinforced epoxy composite material. The method provided by the invention is simple, convenient, free from pollution and practicable.
Description
Technical field
The invention belongs to polyester modified be applied to field of compound material, particularly to one based on ultraviolet
The method of radiation modification terylene reinforced epoxy composite.
Background technology
Terylene is an important kind in synthetic fibers, is the trade name of China's polyester fiber.
It is to be that raw material is through ester with para Toluic Acid (PTA) or dimethyl terephthalate (DMT) (DMT) and ethylene glycol (EG)
Change or ester exchange and polycondensation reaction and prepared fiber-forming polymer one polyethylene terephthalate (PET),
Through the fiber that spinning and post processing are made.Polyster fibre is hydrophobic synthetic organic fibre, due to interior part
Closely, surface is the most smooth, and Nature comparison is stable in son arrangement.Terylene surface does not has can be with other substance reactions
Active group, so it seldom can directly occur chemical reaction.So the study on the modification of terylene is not had always
There is breakthrough.To polyester modified prepare epoxy composite material research then do not have.And corresponding, research
Comparison many be that the modified of carbon fiber, glass fibre, polypropylene fibre, aramid fiber etc. preparing is combined
Material.This is due to the performance of these fibers itself, and the surface such as carbon fiber is easy to by oxidation processes
Its surface forms the oxy radical being combined with resin matrix, and glass fibre can pass through at heat treatment, soda acid etching
Method and the corresponding inorganic reagent generation chemical reactions such as reason, coupling agent treatment, thus generate active group and enter
And prepare composite with epoxy bond.Such method for modifying fibers such as carbon fiber and glass fibre is sent out
Exhibition comparative maturity, method of modifying is fairly simple simultaneously.Accordingly, terylene can be grafted by certain method
Upper active groups, then in grafting, the polyster fibre of active group just can react preparation with epoxy resin
Composite.The polyester modified composite prepared with epoxy bond has the advantage that one is intensity
Height, good springiness, thermostability, thermoplasticity are good, wearability is good, light resistance is good, corrosion-resistant.Two is that raw material is easy
, cheap, it is easy to industrialized production.On composite prepared after polyester modified not only has
State the performance of excellence, but also there is the advantages such as good, the light quality of water resistance, be other composite institutes
Can not be substituted.
Summary of the invention
Owing to terylene smooth surface and chemically inert shortcoming make the interface between itself and epoxy resin
Imperfect bonding, limits its application in every field.Use ultraviolet irradiation technology for this this patent, washing
Such as hydroxyl, carboxyl, amide groups, sulfonic acid group, hydrogen-based isoreactivity group on synthetic fibre surface grafting.Modified
Terylene can prepare composite with epoxy resin reaction.Terylene is carried out irradiation grafting study on the modification, carries
High microsteping and the interfacial bond property of resin matrix.By optimizing design irradiation technique parameter and irradiation grafting list
Body, realizes fiber surface modification on the premise of not reducing fiber bodies intensity, thus to improve terylene multiple comprehensively
The combination property of condensation material.
The features such as irradiation technique is efficient with it, energy-conservation and environmental protection, obtain wide on material modified surface
General application.Ultraviolet irradiation can evoke the activity of fiber surface functional group, and these active function groups can be with matrix
There is physical action or chemical reaction, thus increase fiber and basal body interface binding ability；We can wash
Active group on synthetic fibre surface grafting, the other end of these active groups can also be grafted on resin matrix, have
It is beneficial to resin matrix to the infiltration of fiber and crosslinking；Fiber surface can also be performed etching, make fiber surface
Roughness increase, thus increase the surface area of fiber, make the mechanical snap between fiber and resin strengthen, from
And increase interface bond strength therebetween.Generally speaking ultraviolet irradiation can increase the coarse of fiber surface
Degree, the activity of the group of excitation fiber own and introducing active group, this active group can react with resin matrix,
Improve the resin wellability to fiber so that physics and chemical bond intensity therebetween increase, finally
Reach the more preferable combination between fiber and resin matrix.
The present invention is in liquid medium, terylene to be carried out radiation modification with ultraviolet irradiation, changes further
The surface property of kind fiber, thus improve the interface bond strength of fiber and epoxy resin-base, to greatest extent
Ground plays terylene and strengthens the combination property of composite.Under ultraviolet irradiation, all liquid with coupling agent function
There is graft reaction, and the idol being capable of between fiber and resin matrix in body medium and terylene top layer functional group
Connection reaction, all can be as graft.This patent use ultraviolet irradiation technology, on terylene surface grafting hydroxyl,
Carboxyl, amide groups, sulfonic acid group, hydrogen-based isoreactivity group.And epoxy resin can with alcohols, phenols,
Hydroxy acid class, mercaptan, amide, ureas, urea ester etc. react.Modified terylene can react with epoxy resin
Prepare composite.Irradiation bomb has the advantages that power is high, preparation is simple, use safety.The present invention has
Easy and simple to handle, process stabilizing, reliable product quality, environmental protection, and the advantage being suitable to industrialized production.Change
Can obtain after property: terylene interlaminar shear strength potentiation of composite after ultraviolet irradiation processes is obvious, not
The composite interlayer shear strength prepared time treated only has 63.75MPa, after ultraviolet irradiation processes
Interlaminar shear strength starts to increase, and increases along with the rising for the treatment of temperature.
Process of the present invention is: being placed in special glass container by the most dried terylene, addition can
It is completely soaked the grafting liquid of fiber consumption, soaks a period of time, then evacuation, inject liquid, finally lead to
Entering nitrogen and accept the radiation treatment of various dose to atmospheric pressure sealed, sealing, the fiber after irradiation is close in container
Close placement a period of time.Taking-up is dried naturally, and then heat drying is to remove residual solvent, close in exsiccator
Seal up for safekeeping and put.Graft selection principle is to have coupling agent function, and under ultraviolet irradiation, graft can be with fiber
Surface molecules generation graft reaction, and then the coupling reaction being capable of between terylene and resin matrix.Changing
Epoxy composite material made by terylene before and after property, the monofilament tensile strength contrast various dose radiation treatment of fiber
Rear polyester circular O compoiste material interlaminar shear strength.Result shows: after radiation treatment, the filament stretch of fiber is strong
Degree loss is the least, i.e. the bulk strength of fiber is basically unchanged, and reason is the skin that graft reaction only occurs in fiber
On layer, little molecule graft does not enters in the cored structure of fiber, so the orientation texture of strand is not by shadow
Ringing, the mechanical property change of fiber is little.Coupling agent solution and terylene are impregnated simultaneously and place a period of time,
Same prepared terylene reinforced epoxy composite.After impregnation process, the interlayer of terylene reinforced epoxy composite is cut
Shearing stress is almost roughly the same with the interlaminar shear strength of untreated terylene reinforced epoxy composite.This says
The raising of bright composite material interface is fiber result of mutual radiation effect in coupling agent solution.
Detailed description of the invention:
Detailed description of the invention one: graft acrylamide:
The first step: in fume hood, cleans PET non-weaving cloth acetone, the most in an oven
Dry 1 hour；
Second step: at monomer concentration be by the PET non-weaving cloth dried again after acetone cleans
2mol/L acrylamide and initiator concentration are the prepreg solution that proportioning is 1: 1 that 0.15mol/L Benzoinum is made into
Middle dipping two hours；
3rd step: take out the PET non-weaving cloth after dipping and clamp with two pieces of quartz glass plates, it is to avoid
The inhibition of oxygen, puts it into ultraviolet source wavelength and is about in 320nm ultraviolet reactor, ultraviolet light
Two sides uv photo initiated grafting process is carried out through quartz glass.Time of ultraviolet irradiation is 10min, and irradiation distance is 20
cm；Ultraviolet source be Shanghai Ya Ming electric bulbs factory produce model be GGZ500, power is the high pressure of 500W
Mercury lamp；
4th step: modified PET non-weaving cloth dries 15 minutes, uses the side of vacuum diversion
Method, prepares composite with epoxy resin E-51.
Detailed description of the invention two: graft acrylic acid
The first step: boiled in beaker by PET non-weaving cloth 15 minutes, extraction, then at 105 DEG C
Lower drying 1 hour；
Second step: the PET non-weaving cloth 25mL mass fraction after processing is 40% sweller
Metacresol soaks 2h, swelling temperature 60 DEG C, washing, removes metacresol, and naturally dries；
3rd step: be the third of 0.2mol/L benzophenone by swelling PET non-weaving cloth concentration
Ketone solution soaking 1.0h, natural drying；
4th step: be the acrylic acid of 0.58mol/L the PET non-weaving cloth handled well and concentration
Being placed in quartz test tube, logical nitrogen removes oxygen；
5th step: PET is non-woven lays people with 3.0 × 10 handling well-3Potassium permanganate with
The sulphuric acid of 0.02mol/L is as glycerol polymerization in the ultraviolet radiation facility of initiator, and light application time is that 2.0h takes
Go out PET non-weaving cloth, boil removal homopolymer, until constant weight；
6th step: modified PET non-weaving cloth dries 15 minutes, uses the side of vacuum diversion
Method, prepares composite with epoxy resin E-51.
Detailed description of the invention three: grafted with maleic anhydride
The first step: polyester fabric is placed in the clear water containing 1% detergent and washs 15 minutes, then use
Clear water rinses 15 minutes, dries 4 hours in 50 DEG C of baking ovens；
Second step: soaked 3 hours in dichloromethane by the polyester fabric handled well, takes out and divides
Dehydrated alcohol and deionized water Yong not clean twice, dry stand-by.
3rd step: maleic anhydride grafting radiation treatment, radiation parameter: wavelength 222nm, frequently
Rate 100HZ, electric current 1.6A, power 15KW, fluorescent tube is 3cm with the space of process fabric, radiation treatment
Time is advisable with 0.5min.
4th step: modified PET non-weaving cloth dries 15 minutes, uses the side of vacuum diversion
Method, is combined with epoxy resin E-51 and prepares composite.
Claims (8)
1. section method based on ultraviolet radiation modified terylene reinforced epoxy composite, it is characterised in that: by purple
External irradiation is amide groups, hydrogen-based, carboxyl isoreactivity group on the surface grafting of polyster fibre, and epoxy resin
Can react with alcohols, hydroxy acid class, amide-type etc., so the terylene of the upper active group of grafting can be with epoxy resin
Composite is prepared in reaction.
2. a kind of method based on ultraviolet radiation modified terylene reinforced epoxy composite, its feature described in claim 1
Being: be placed in washing dried terylene in advance in special glass container, addition can be completely soaked terylene and use
The grafting liquid of amount, soaks a period of time, then evacuation, is finally passed through nitrogen and connects to atmospheric pressure sealed, sealing
By the radiation treatment of various dose, the terylene after irradiation is airtight placement a period of time in container, then the most permissible
Some such as amide groups, carboxyl isoreactivity group in grafting.
A kind of method based on ultraviolet radiation modified terylene reinforced epoxy composite, its
Be characterised by: the irradiation dose of selection be respectively 0.1kGy, 100kGy, 500kGy, 1000kGy, 3000
KGy, exposure time is respectively 12h, 13h, 14h, 15h.
A kind of method based on ultraviolet radiation modified terylene reinforced epoxy composite, its
It is characterised by: be nitrogen, noble gas, air to the gas medium in the processing method of terylene surface modification
In the mixing of one or more gases.
A kind of method based on ultraviolet radiation modified terylene reinforced epoxy composite,
It is characterized in that: during ultraviolet irradiation, select different initiators, such as Benzoinum, potassium permanganate/sulphuric acid.
A kind of method based on ultraviolet radiation modified terylene reinforced epoxy composite,
It is characterized in that: can be acrylic acid, acryloyl through the ultraviolet radiation modified monomer being grafted to terylene surface
Amine, maleic anhydride.
A kind of method based on ultraviolet radiation modified terylene reinforced epoxy composite,
It is characterized in that: can be cloth through ultraviolet radiation modified terylene, it is also possible to be fiber.
A kind of method based on ultraviolet radiation modified terylene reinforced epoxy composite,
It is characterized in that: the terylene after ultraviolet modification is grafted, be provided with the active group reacted with epoxy resin,
The method using vacuum diversion prepares polymer matrix composites.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510814620.3A CN106317786A (en) | 2015-11-19 | 2015-11-19 | Method for preparing polyester fiber reinforced epoxy composite material based on ultraviolet radiation modification |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510814620.3A CN106317786A (en) | 2015-11-19 | 2015-11-19 | Method for preparing polyester fiber reinforced epoxy composite material based on ultraviolet radiation modification |
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| CN201510814620.3A Pending CN106317786A (en) | 2015-11-19 | 2015-11-19 | Method for preparing polyester fiber reinforced epoxy composite material based on ultraviolet radiation modification |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108505336A (en) * | 2018-04-04 | 2018-09-07 | 苏州经贸职业技术学院 | Mass sports outdoor garment material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103147290A (en) * | 2013-03-07 | 2013-06-12 | 中国科学院上海应用物理研究所 | Functional nano textile and preparation method thereof |
-
2015
- 2015-11-19 CN CN201510814620.3A patent/CN106317786A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103147290A (en) * | 2013-03-07 | 2013-06-12 | 中国科学院上海应用物理研究所 | Functional nano textile and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| BENGT RANBY: """Surface photografting" onto polymers - a new method for adhesion control"", 《JOURNAL OF ADHESION SCIENCE AND TECHNOLOGY》 * |
| 朱伟敏等: ""聚酯纤维非织造布紫外光表面接枝改性研究"", 《化学与粘合》 * |
| 袁茂全等: ""紫外辐照表面接枝纤维的表征"", 《中国纺织大学学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108505336A (en) * | 2018-04-04 | 2018-09-07 | 苏州经贸职业技术学院 | Mass sports outdoor garment material |
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