CN107722595A - A kind of preparation method of the multiple dimensioned composite of graphite fiber olefinic thermoplastic polyarylether - Google Patents
A kind of preparation method of the multiple dimensioned composite of graphite fiber olefinic thermoplastic polyarylether Download PDFInfo
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- CN107722595A CN107722595A CN201710991858.2A CN201710991858A CN107722595A CN 107722595 A CN107722595 A CN 107722595A CN 201710991858 A CN201710991858 A CN 201710991858A CN 107722595 A CN107722595 A CN 107722595A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
- C08L71/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08L71/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
- C08L81/06—Polysulfones; Polyethersulfones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Abstract
A kind of preparation method of the multiple dimensioned composite of graphite fiber olefinic thermoplastic polyarylether, belongs to field of material technology, comprises the following steps：(1) add graphene oxide into solvent N, N dimethyl acetamide and disperse；(2) thermoplastic poly aryl ether resin is added in solvent N, N dimethyl acetamide and stirred；(3) graphene oxide dispersion soln and thermoplastic poly aryl ether resin solution are mixed into simultaneously ultrasonic disperse；(4) continuous fiber is placed in dipping solution, in 220 ± 10 DEG C of drying after being sufficiently impregnated, while makes graphene oxide thermal reduction in situ；(5) it is placed in die for molding.The preparation method of the present invention is scientific and reasonable, and process is simple, workable, greatly extends its application.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of fiber-graphene-thermoplastic poly aryl oxide is multiple dimensioned compound
The preparation method of material.
Background technology
PAEK (PEK-C) containing phenolphthalein side base, the polyether sulphone (PES-C) containing phenolphthalein side base and containing phenodiazine
The poly (aryl ether sulfone ketone) (PPESK) of miscellaneous naphthalenone biphenyl structural is the polyarylether class High performance plastic resin voluntarily researched and developed by China,
These resins have excellent mechanical property, resistance to elevated temperatures and processing characteristics, have obtained swift and violent development in recent years.
There is higher modulus of elasticity and water ratio limit using High performance plastic resin as the fibrous composite of matrix
Intensity, compared with same with thermosetting compound material, have high shock resistance damage performance, prepreg storage period length and recoverable etc. excellent
Point, is just more and more paid attention to.
Graphene is the Two-dimensional Carbon atomic crystal of monoatomic thickness, it is considered to be the base of fullerene, CNT and graphite
This construction unit.Because graphene has high rigidity, high intensity, low thermal coefficient of expansion, high conductivity, high-termal conductivity, high
The specific surface area of draw ratio and super large, preparation method is various in addition and relative maturity, therefore is generally considered preferable polymerization
Thing modified filler, it is more obvious to compare advantage with other carbon nanomaterials.
But graphene film interlayer has a strong π-π interactions, surface very torpescence, be not easy it is compatible with organic matter,
It is very easy to reunite in the polymer, its composite cannot also give full play to the superior performance of graphene.At present, both at home and abroad
What document was mainly reported is that research is modified to thermoplastic resin matrix using graphene oxide or functional graphene oxide,
And the high-performance polyarylether resin based composites of continuous lod are modified using graphene, also it is rarely reported.
The content of the invention
It is an object of the invention to provide a kind of preparation side of fiber-graphene-multiple dimensioned composite of thermoplastic poly aryl oxide
Method, mixed by the way that graphene oxide is disperseed in a solvent, then with thermoplastic poly aryl ether resin solution, leaching is formed after ultrasonic disperse
Stain solution, after fibrous material is sufficiently impregnated with dipping solution, graphene oxide is carried out while heating removes solvent former
Position thermal reduction, it is finally that obtained prepreg is hot-forming, improve fiber reinforcement high-performance thermoplastic polyarylether resin composite wood
The performance of material.
The method of the present invention comprises the following steps：
1st, add graphene oxide into solvent DMA, carry out 1~2h ultrasonic disperse, form oxygen
Graphite alkene dispersion soln；
2nd, thermoplastic poly aryl ether resin is added in solvent DMA, stirred, it is dense that quality is made
The thermoplastic poly aryl ether resin solution of degree 10~35%；Described thermoplastic poly aryl ether resin selects the poly- virtue containing phenolphthalein side base
Ether ketone resin, the polyaryl ether sulphone resin containing phenolphthalein side base or the PPESK containing diazanaphthalene terphenyl structure；
3rd, graphene oxide dispersion soln is mixed with thermoplastic poly aryl ether resin solution, stirs 1~2h, then ultrasound point
1~2h is dissipated, dipping solution is made；Graphene oxide is the 0.05~0.75% of polyarylether resin gross mass in dipping solution；
4th, continuous fiber is placed in dipping solution, the fiber being sufficiently impregnated into continuous fiber is infiltrated, and is then taken out
2~3h is dried at 220 ± 10 DEG C, while removing solvent, makes graphene oxide thermal reduction in situ, obtains containing the pre- of graphene
Leaching material；
5th, the prepreg containing graphene is placed in mould, by compression molding or autoclave molding, fiber-stone is made
Black alkene-multiple dimensioned the composite of thermoplastic poly aryl oxide.
Above-mentioned continuous fiber selects glass fibre, carbon fiber, aramid fiber or pbo fiber.
The filament diameter of above-mentioned continuous fiber is 2~18 μm.
The particle diameter of graphene is 5~400nm in above-mentioned fiber-graphene-thermoplastic poly aryl oxide composite.
In the above method, 310~440 DEG C, 0.5~10MPa of pressure of temperature when compression molding or autoclave molding, during shaping
Between 3~4h.
The supersonic frequency selected in above-mentioned step 1 and 3, during ultrasonic disperse is 40Hz.
The surface of graphene oxide that the present invention uses contains the substantial amounts of oxygen-containing functional group such as hydroxyl, carboxyl, epoxy, in water
With can be dispersed in DMA equal solvent, by way of solution blending, graphene oxide is uniformly divided
It is dispersed among the soluble polyaryl ether resin body such as PEK-C, PES-C or PPESK, after fiber impregnation, drying removes solvent
In-situ reducing is carried out to graphene oxide simultaneously, obtains the prepreg containing graphene, combination property is prepared using the prepreg
Excellent multiple dimensioned composite；Collectively formed in the composite by various sizes of micron order fiber and nanoscale graphite alkene
Reinforcement, form Multi-scale model.
The beneficial effect that is reached of the present invention is：(1) graphene oxide is dispersed in by N, N- dimethyl by ultrasound
In acetamide, after being mixed with resin solution, it is scattered in resin matrix to be greatly promoted graphene oxide；(2) will be even
Continuous fiber or fabric make graphite oxide after mixed resin solution is sufficiently impregnated while heating removes solvent in an oven
Alkene thermal reduction in situ, under conditions of without reducing agent, obtain the scattered prepreg of graphene uniform；(3) more chis prepared by
Degree composite property is excellent, and interlaminar shear strength, bending strength, bending modulus, impact flexibility are significantly increased；And prepare
Methodological science is reasonable, and process is simple, workable, greatly extends its application, has significant social economy effect
Benefit.
Brief description of the drawings
Fig. 1 is the thermogravimetric curve figure for the graphene oxide that the present invention uses.
Embodiment
The middle graphene oxide used is commercial products in the present invention is implemented.
The DMAC N,N' dimethyl acetamide used in the embodiment of the present invention is AR purchased in market.
The ketone-grouped resin (PEK-C) containing phenolphthalein side base that is used in the embodiment of the present invention, containing phenolphthalein side base
Polyaryl ether sulphone resin (PES-C) and PPESK (PPESK) containing diazanaphthalene terphenyl structure are commercial products.
Glass fibre, carbon fiber, aramid fiber and the pbo fiber used in the embodiment of the present invention is commercial products.
It is ASTM D2344 that interlaminar shear strength accepted standard is tested in the embodiment of the present invention.
It is GB/T 1449 that bending strength and bending modulus accepted standard are tested in the embodiment of the present invention.
It is GB/T1451 that impact flexibility accepted standard is tested in the embodiment of the present invention.
The filament diameter of continuous fiber is 2~18 μm in the embodiment of the present invention.
The particle diameter of graphene oxide is 5~400nm in the embodiment of the present invention.
In the embodiment of the present invention in fiber-graphene-thermoplastic poly aryl oxide composite the particle diameter of graphene for 5~
400nm。
The supersonic frequency selected in the embodiment of the present invention during ultrasonic disperse is 40Hz.
Same steps are used in the embodiment of the present invention but are added without graphene oxide (thermal reduction reaction in situ does not occur)
Scheme, unmodified fiber-thermoplastic poly aryl oxide composite is made, carries out performance comparison.
Embodiment 1
Add graphene oxide into solvent DMA, carry out 1h ultrasonic disperse, form oxidation stone
Black alkene dispersion soln；
Thermoplastic poly aryl ether resin is added in solvent DMA, stirred, mass concentration is made
10% thermoplastic poly aryl ether resin solution；Thermoplastic poly aryl ether resin is PEK-C；
Graphene oxide dispersion soln is mixed with thermoplastic poly aryl ether resin solution, stirs 2h, then ultrasonic disperse
1.5h, dipping solution is made；Graphene oxide is the 0.05% of polyarylether resin gross mass in dipping solution；
Continuous fiber is placed in dipping solution, the fiber being sufficiently impregnated into continuous fiber is infiltrated, and is then taken out
220 ± 10 DEG C of drying 2h, while removing solvent, make graphene oxide thermal reduction in situ, obtain the prepreg containing graphene；
Continuous fiber is glass fibre；
In in-situ heat reduction process, the thermogravimetric curve of graphene oxide is as shown in Figure 1, it can be seen that graphene oxide exists
Weight loss rate is most fast at 220 DEG C, shows that a large amount of oxy radicals of surface of graphene oxide are decomposed and removed, and graphene oxide occurs
Obvious reduction reaction；
Prepreg containing graphene is placed in mould, by compression molding, fiber-graphene-thermoplastic poly is made
The multiple dimensioned composite of aryl oxide；310 DEG C of temperature during compression molding, pressure 10MPa, molding time 4h；
The interlaminar shear strength of fiber-graphene of acquisition-multiple dimensioned composite of thermoplastic poly aryl oxide is 85.5MPa,
Bending strength is 1765MPa, bending modulus 68GPa, impact flexibility 14.8KJ/m2；With unmodified fiber -- thermoplasticity
Polyarylether composite is compared, and is respectively increased 31.1%, 23.9%, 23.6% and 42.3%.
Embodiment 2
With embodiment 1, difference is method：
(1) graphene oxide dispersion soln is made in ultrasonic disperse 1.5h；
(2) mass concentration 20% of thermoplastic poly aryl ether resin solution；Thermoplastic poly aryl ether resin is PES-C；
(3) graphene oxide dispersion soln and thermoplastic poly aryl ether resin solution are mixed into 1.5h, ultrasonic disperse 1h；
Graphene oxide is the 0.25% of polyarylether resin gross mass in dipping solution；
(4) continuous fiber is placed in dipping solution, is taken out after being sufficiently impregnated and dry 3h at 220 ± 10 DEG C；Continuous fiber
For by carbon fiber；
(5) fiber-graphene-multiple dimensioned composite of thermoplastic poly aryl oxide is made by autoclave molding；Forming temperature
350 DEG C, pressure 5MPa, time 3.5h；
(6) interlaminar shear strength of the fiber-graphene-multiple dimensioned composite of thermoplastic poly aryl oxide obtained
104.5MPa, bending strength 1868MPa, bending modulus 115Gpa, impact flexibility 13.2KJ/m2；With unmodified fiber -- heat
Plasticity polyarylether composite is compared, and is respectively increased 33.1%, 41.5%, 64.3% and 37.5%.
Embodiment 3
With embodiment 1, difference is method：
(1) graphene oxide dispersion soln is made in ultrasonic disperse 2h；
(2) mass concentration 30% of thermoplastic poly aryl ether resin solution；Thermoplastic poly aryl ether resin is PPESK；
(3) graphene oxide dispersion soln and thermoplastic poly aryl ether resin solution are mixed into 1h, ultrasonic disperse 2h；Leaching
Graphene oxide is the 0.5% of polyarylether resin gross mass in stain solution；
(4) continuous fiber is placed in dipping solution, is taken out after being sufficiently impregnated and dry 2.5h at 220 ± 10 DEG C；It is continuous fine
Tie up as aramid fiber；
(5) fiber-graphene-multiple dimensioned composite of thermoplastic poly aryl oxide is made by compression molding；Forming temperature 410
DEG C, pressure 2MPa, time 3h；
(6) the interlaminar shear strength 56.2MPa of the fiber-graphene-multiple dimensioned composite of thermoplastic poly aryl oxide obtained,
Bending strength 678MPa, bending modulus 60.2GPa, impact flexibility 21.5KJ/m2；With unmodified fiber -- thermoplastic poly aryl oxide
Composite is compared, and is respectively increased 43.3%, 30.3%, 41.6% and 22.9%.
Embodiment 4
With embodiment 1, difference is method：
(1) graphene oxide dispersion soln is made in ultrasonic disperse 1.5h；
(2) mass concentration 35% of thermoplastic poly aryl ether resin solution；Thermoplastic poly aryl ether resin is PEK-C；
(3) graphene oxide dispersion soln and thermoplastic poly aryl ether resin solution are mixed into 1.5h, ultrasonic disperse
1.5h；Graphene oxide is the 0.75% of polyarylether resin gross mass in dipping solution；
(4) continuous fiber is placed in dipping solution, is taken out after being sufficiently impregnated and dry 2.5h at 220 ± 10 DEG C；It is continuous fine
Tie up as pbo fiber；
(5) fiber-graphene-multiple dimensioned composite of thermoplastic poly aryl oxide is made by autoclave molding；Forming temperature
440 DEG C, pressure 0.5MPa, time 3.5h；
(6) the interlaminar shear strength 42.6MPa of the fiber-graphene-multiple dimensioned composite of thermoplastic poly aryl oxide obtained,
Bending strength 645MPa, bending modulus 48.6GPa, impact flexibility 19.8KJ/m2；With unmodified fiber -- thermoplastic poly aryl oxide
Composite is compared, and is respectively increased 59.6%, 40.2%, 51.8% and 26.9%.
Claims (5)
1. the preparation method of a kind of fiber-graphene-multiple dimensioned composite of thermoplastic poly aryl oxide, it is characterised in that including following
Step：
(1) add graphene oxide into solvent DMA, carry out 1~2h ultrasonic disperse, form oxidation
Graphene dispersion solution；
(2) thermoplastic poly aryl ether resin is added in solvent DMA, stirred, mass concentration 10 is made
~35% thermoplastic poly aryl ether resin solution；Described thermoplastic poly aryl ether resin selects the PAEK containing phenolphthalein side base
Resin, the polyaryl ether sulphone resin containing phenolphthalein side base or the PPESK containing diazanaphthalene terphenyl structure；
(3) graphene oxide dispersion soln is mixed with thermoplastic poly aryl ether resin solution, stirs 1~2h, then ultrasonic disperse 1
~2h, is made dipping solution；Graphene oxide is the 0.05~0.75% of polyarylether resin gross mass in dipping solution；
(4) continuous fiber is placed in dipping solution, the fiber being sufficiently impregnated into continuous fiber is infiltrated, and is then taken out
220 ± 10 DEG C of 2~3h of drying, while removing solvent, make graphene oxide thermal reduction in situ, obtain the preimpregnation containing graphene
Material；
(5) prepreg containing graphene is placed in mould, by compression molding or autoclave molding, fiber-graphite is made
Alkene-multiple dimensioned the composite of thermoplastic poly aryl oxide.
A kind of 2. preparation side of fiber-graphene-multiple dimensioned composite of thermoplastic poly aryl oxide according to claim 1
Method, it is characterised in that described continuous fiber selects glass fibre, carbon fiber, aramid fiber or pbo fiber.
A kind of 3. preparation side of fiber-graphene-multiple dimensioned composite of thermoplastic poly aryl oxide according to claim 1
Method, it is characterised in that the filament diameter of described continuous fiber is 2~18 μm.
A kind of 4. preparation side of fiber-graphene-multiple dimensioned composite of thermoplastic poly aryl oxide according to claim 1
Method, it is characterised in that the particle diameter of graphene is 5~400nm in described fiber-graphene-thermoplastic poly aryl oxide composite.
A kind of 5. preparation side of fiber-graphene-multiple dimensioned composite of thermoplastic poly aryl oxide according to claim 1
Method, it is characterised in that 310~440 DEG C of temperature when described compression molding or autoclave molding, 0.5~10MPa of pressure, during shaping
Between 3~4h.
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| CN109142478A (en) * | 2018-08-30 | 2019-01-04 | 浙江大学 | A kind of novel high molecular polymer film functionalization graphene modified electrode electrochemical sensor and preparation method and application |
| CN109177207A (en) * | 2018-07-09 | 2019-01-11 | 黄河科技学院 | Para-aramid fiber enhances unsaturated-resin board making and stress measuring method |
| CN109233241A (en) * | 2018-09-25 | 2019-01-18 | 沈阳航空航天大学 | A kind of graphene/poly (aryl ether sulfone ketone) conductive film and preparation method thereof |
| CN110323451A (en) * | 2019-04-28 | 2019-10-11 | 中国科学院山西煤炭化学研究所 | A kind of multifunctional composite and its preparation method and application based on graphene and macromolecular fibre |
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