CN106928488B - Fabric enhances blending resin base composite laminate of phthalonitrile containing Phthalazinone and preparation method thereof - Google Patents
Fabric enhances blending resin base composite laminate of phthalonitrile containing Phthalazinone and preparation method thereof Download PDFInfo
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- CN106928488B CN106928488B CN201710226765.0A CN201710226765A CN106928488B CN 106928488 B CN106928488 B CN 106928488B CN 201710226765 A CN201710226765 A CN 201710226765A CN 106928488 B CN106928488 B CN 106928488B
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/04—Layered products comprising a layer of synthetic resin as impregnant, bonding, or embedding substance
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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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
- C08K7/10—Silicon-containing compounds
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Reinforced Plastic Materials (AREA)
Abstract
The invention belongs to advanced compound materials science domains.Disclose a kind of fabric enhancing blending resin base composite laminate of phthalonitrile containing Phthalazinone and preparation method thereof.Its main feature is that resin matrix is the blending resin that the phthalonitrile-terminated cross-linking Phthalazinone independently prepared is total to poly (arylene ether nitrile) resin and cross-linking bisphenol type phthalonitrile compound BP Ph；Above-mentioned resin matrix is dissolved in specific organic solvent, and 4 are added for the first time, 4 diaminodiphenylsulfones/zinc chloride mixture is as curing agent.By solution homogeneous impregnation in fabric, solvent is removed through hot-fluid drying channel, after being cooled to room temperature, preliminary-dip piece is made；Preliminary-dip piece is put in mold, through certain hot-press solidifying technological forming, the composite material laminated board with good comprehensive performance is obtained after cooling and demolding.Innovation of the present invention is to have designed and synthesized a kind of o-phthalonitrile resin containing Phthalazinone and cyanophenyl structure, can realize that solution prepreg method prepares composite laminate using the resin as matrix；In addition, the design by being mixed into BP Ph and Novel curing agent, realizes the raising of o-phthalonitrile resin curing performance and the reduction of processing cost.And by presoaking design and optimization with laminating technology, prepare the composite laminate with good comprehensive performance.The present invention has practical value in the development and expansion thermosetting resin based composites for pushing high-performance composite materials in the application aspect of aerospace field.
Description
Technical field
The invention discloses a kind of fabrics to enhance the blending resin base composite wood of phthalonitrile containing Phthalazinone
Material and preparation method thereof more particularly to uses the o-phthalonitrile resin containing Phthalazinone of autonomous Design by being blended, molten
Liquid preimpregnated process, composite crosslinking curing agent accelerate ratio of hot press forming technology, regulation and control blending resin etc. to regulate and control composite material
Physical property and processing performance.Belong to advanced compound materials science domain.
Background technology
Thermosetting resin based composites have been widely used in navigating due to the advantages that its high intensity, high-modulus, light specific gravity
Empty space industry, but with the fast development of aeronautical and space technology, to the mechanical performance of thermosetting resin based composites, heat-resisting
Performance, dielectric properties made higher requirement.In order to further increase the comprehensive performance of thermosetting resin based composites,
Be a series of high intensity of matrix with crosslinkable aryne resin, cyanic acid resin, o-phthalonitrile resin etc., high thermal stability and
The composite material of low-k is successfully prepared.Wherein, o-phthalonitrile resin has due to that can be formed in crosslinking
The s-triazine ring and phthalocyanine structure of good thermal stability and high degree of rigidity so that go out excellent heat resistance with its composite material exhibits
Energy and mechanical performance.In recent years, o-phthalonitrile resin composite material receives more and more extensive concern.However, such tree
The high processing viscosity of fat and harsh condition of cure make its related application be restricted, and the heat resistance of its composite material has
It waits further increasing.
Poly (arylene ether nitrile) resin (Yu Guipeng et al, Polymer, 2010,51 (1) containing Phthalazinone:540-
549) it is an analog thermoplastic high-performance resin matrix by Dalian University of Technology's independent development, since Phthalazinone makes its tool
There is excellent heat resistance, and be dissolvable in water proton polar solvent, when poly (arylene ether nitrile) resin and the adjacent benzene two of Phthalazinone
Nitrile structure is combined, and by forming triazine ring and/or phthalocyanine structure after the crosslinking curing of dintrile structure, makes the material of gained after solidification
Material has superior performance (Yu Guipeng et al, High Performance Polymers, 2014,26 (5):
1233-1239).The present invention uses poly (arylene ether nitrile) phthalic nitrile resin and biphenyl structural phthalic nitrile list containing Phthalazinone
Body forms blending resin matrix, and the prepreg of fabric reinforced composites is prepared using solution dipping method, wherein containing miscellaneous naphthalene
The poly (arylene ether nitrile) phthalic nitrile resin of biphenyl structural can guarantee the heat resistance of gained composite material, biphenyl structural neighbour's benzene of addition
Two nitrile monomers can improve the mobile performance of resin matrix in thermoforming solidification process, using composite crosslinking curing agent to above-mentioned adjacent benzene
Dintrile resin carries out curing reaction, makes the active higher of curing reaction, can shorten hardening time, improves curing efficiency.
It retrieves existing disclosure or authorizes in patent of invention, patent related to the present invention has, patent of invention
CN2012105551 32.1 and ZL 201010217662.6 individually discloses the bi-phthalonitrile tree of poly (arylene ether nitrile) containing bisphenol A-type
Fat and phthalonitrile-terminated polyimide resin containing phthalazinone structure, corresponding solidfied material and preparation method thereof.
The resin matrix that above-mentioned patent is related to is different from the structure of resin matrix of the present invention, and preparation method is also different.Vertical rate of ancestor etc.
It reports and uses the thermosetting property Phthalazinone o-phthalonitrile resin of s-triazine structure containing aryl for matrix, using solution dipping method
Be prepared for carbon cloth reinforced resin based composites (ancestor founds rate etc., composite material journal, 2013,30：59-64).With this hair
Bright blending resin matrix is compared, and the resin matrix configuration of documents is different from the present invention, and curative systems are also different.This
Invention uses the poly (arylene ether nitrile) phthalic nitrile resin of Phthalazinone and tree is blended in biphenyl structural phthalic nitrile monomer composition
Aliphatic radical body, and the single aromatic diamines of crosslinking and curing agent used become aromatic diamines/zinc chloride mixed curing agent, so completely
It is different.
Invention content
The purpose of the present invention is the o-phthalonitrile resin based composites for report due to processing difficulties, curing process
The problems such as condition is harsh, heat resistance is to be improved provides a kind of fabric enhancing phthalonitrile containing Phthalazinone
Blending resin base composite laminate and preparation method thereof.
Technical scheme of the present invention,
Fabric enhances the thermoplastic blends matrix composite of phthalonitrile containing Phthalazinone, using containing Phthalazinone
The poly (arylene ether nitrile) phthalic nitrile resin and biphenyl structural phthalic nitrile monomer composition blending resin matrix of structure, wherein joining containing miscellaneous naphthalene
The poly (arylene ether nitrile) phthalic nitrile resin of benzene structure has good dissolubility energy, heat resistance and processing performance, the biphenyl of addition
Structure phthalic nitrile monomer can improve the mobile performance of resin matrix in thermoforming solidification process, using composite crosslinking curing agent pair
Phthalic nitrile resin carries out curing reaction, makes the active higher of curing reaction, can shorten hardening time, improves curing efficiency.In advance
The preparation for soaking piece uses solution dipping method, is easy to control, is easy to make fabric by solution homogeneous immersion.
A kind of fabric enhancing blending resin base composite laminate of phthalonitrile containing Phthalazinone, including fiber
Fabric and the blending resin matrix of phthalonitrile containing Phthalazinone are according to mass percentage composition：
Fabric：50~70 parts；
The blending resin of phthalonitrile containing Phthalazinone：30~50 parts；
The blending resin of phthalonitrile containing Phthalazinone includes two kinds of components, the quality of component 1 and component 2
Than being 4:1~1:4；
The structural formula of component 1 is as follows：
Wherein,
R1It is hydrogen, halogenic substituent, phenyl, phenoxy group, alkyl or alkoxy,
R2It is hydrogen, halogenic substituent, phenyl, phenoxy group, alkyl or alkoxy,
R3It is hydrogen, halogenic substituent, phenyl, phenoxy group, alkyl or alkoxy,
R4It is hydrogen, halogenic substituent, phenyl, phenoxy group, alkyl or alkoxy,
Above-mentioned R1、R2、R3And R4In alkyl or alkoxy be contain at least one carbon atom, R1、R2、R3And R4Structure phase
It is same or different；n≥1.
The structural formula of component 2 is as follows：
The fabric is quartz fiber cloth, glass fabric, carbon cloth, aryl fiber cloth, basalt fibre
One kind in cloth.
A kind of preparation side of the fabric enhancing blending resin base composite laminate of phthalonitrile containing Phthalazinone
Method, steps are as follows：
The dissolving of Phthalazinone phthalonitrile blending resin will be contained in organic solvent, addition accounts for knot containing Phthalazinone
The crosslinking and curing agent of structure phthalonitrile blending resin content 8wt%, is configured to Solid content (O-phthalic containing Phthalazinone
Nitrile blending resin and crosslinking and curing agent) mass percent concentration be 25~40% resin solution, fabric is immersed in tree
In lipoprotein solution, make the surface homogeneous impregnation resin solution of fabric, solvent, hot-fluid drying channel are removed through hot-fluid drying channel
Temperature is 100~200 DEG C, and drying time is 8~12h, and prepreg tape is made after naturally cooling to room temperature；By prepreg tape be cut into
The matched preliminary-dip piece of mold size, the preliminary-dip piece of the corresponding number of plies is laid with according to the thickness of composite material laminated board, obtains prepreg；
Prepreg is put in mold technique through hot press molding, completes curing reaction, is joined containing miscellaneous naphthalene up to fabric enhancing after demoulding
Benzene structure phthalonitrile blending resin base composite laminate.
The crosslinking and curing agent is 4,4`- diaminodiphenylmethane, two methyl phenyl ethers anisole of 4,4`- diamino, 4,4`- diamino
One kind in diphenyl sulphone (DPS), the blend with anhydrous zinc chloride, the two mass ratio are 5:1~1:5.
The program of the hot press forming technology is：15~20min of heat preservation at a temperature of 50~120 DEG C, pressurization 8~
20MPa is vented 3 times；Release, after being warming up to 200~250 DEG C with the heating rate of 10~15 DEG C/min, pressurize 8~20MPa, with
The heating rate of 6~8 DEG C/min is warming up to 230~290 DEG C, and 2~3min is kept under the temperature condition；Pressure is risen to
15MPa is vented 1~2 time, by following procedure hot-press solidifying：265 DEG C of -2h, 295 DEG C of -2h, 375 DEG C of -2h；When keeping hot-press solidifying
Pressure, is cooled down with 2~3 DEG C/min rates, and temperature demoulds after being down to 50 DEG C.
The organic solvent is N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, dimethyl sulfoxide (DMSO), N- methyl pyrroles
One or more of pyrrolidone, chloroform mix.
The o-phthalonitrile resin matrix PBD-Ph in the bibliography on aforementioned composite material journal is compared, is being mixed into
After single aromatic diamines (4,4`- diaminodiphenylsulfones, DDS) curing agent, cure peak temperature is measured 325 by DSC scannings
DEG C or so, rheological curve shows that its viscosity just begins with apparent rising after 260 DEG C.And composite material using the present invention
The obtained corresponding temperature of preparation method is respectively at 260 DEG C and 230 DEG C or so, it was demonstrated that the cross-linking system designed herein has more
High crosslinking active.Meanwhile mentioning PBD-Ph in document and can only be dissolved in N-Methyl pyrrolidone under heating state, and this hair
The prepared o-phthalonitrile resin PPEN-Ph containing Phthalazinone and fragrant nitrile structure is completely soluble in chloroform, dichloro in bright
In methane, n,N-Dimethylformamide, N-Methyl pyrrolidone, dimethyl sulfoxide (DMSO) equal solvent, there is more excellent solution to process
Property.Further, since PBD-Ph processing viscosity is higher, cause it undesirable to the wellability of fiber cloth during hot-press solidifying,
Cause composite laminate shear strength relatively low.And PPEN-Ph prepared by the present invention has lower processing viscosity compared to PBD-Ph,
And due to biphenyl structural phthalic nitrile monomer (BP-Ph) (fusing point：232~235 DEG C) addition so that resin matrix is to fiber
The wellability of cloth, which has, to be obviously improved, and shear strength improves, and when crooked test shows apparent tension failure.With E- glass fibers
For this kind of resin base composite laminate for tieing up enhancing, the bending strength of such laminate at normal temperatures up to 650~670MPa,
Bending modulus is up to 28~34GPa.
By taking PB11 (PPEN-Ph/BP-Ph=1/1) blending resin as an example, the thermogravimetic analysis (TGA) knot of two kinds of resin matrixes is compared
Fruit (see Fig. 1, table 1) is as can be seen that there is PB11 more excellent thermal stability, 5% thermal weight loss temperature to be higher by compared with PBD-Ph
20~25 DEG C or so.From dynamic mechanical analysis result (DMA is shown in Fig. 2) as can be seen that quartz fibre enhances PB11 composite laminates
Glass transition is not had at 400 DEG C or less, it was demonstrated that crosslinking degree is high, and molecule chain rigidity is big, and prepared by bibliography
The loss tangent of composite material, which then takes place from 350 DEG C, to be significantly risen.In addition, composite material heating used prepared by the present invention
Program curing amounts to 6h, much smaller than the 14h (being to remove the heating time used) in document, illustrates the resin that the present invention designs
System and curing agent can improve the preparation efficiency of o-phthalonitrile resin base composite laminate to a certain extent.In addition, by
In the high-crosslinking-degree of resin matrix, composite laminate prepared by the present invention has lower dielectric constant.Enhanced with quartz fibre
PB11 resin base composite laminates for, in consistent electric field (voltage swing：Dielectric constant under 0.526KV) is 2.98；
For dielectric constant under 8-18GHz electromagnetic waves between 3.44~3.54, dielectric loss is less than 0.008.The present invention is for pushing
The development of advanced composite material and the application opened up in aerospace field have practical value.
Thermogravimetric curve related data (nitrogen atmosphere) after table 1.PB11 and PBD-Ph solidifications
Description of the drawings
Fig. 1 is thermogravimetric curve figure (nitrogen atmosphere) after PB11 resin solidifications.
Fig. 2 is PB11 composite laminate DMA test result figures.
Specific implementation mode
Below in conjunction with attached drawing and technical solution, the specific implementation mode that further illustrates the present invention.
Embodiment one
Using nucleophilic displacement process, synthesize the PPEN-Ph oligomers of n=10, and by it with BP-Ph by mass percentage
50：50 are dissolved in n,N-Dimethylformamide (DMF) solvent, are configured to the glue that mass percent concentration is 30%, simultaneously
Addition accounts for the mass mixings objects such as 8% 4,4- diaminodiphenylsulfones/zinc chloride of resin gross mass as curing agent, heating stirring
30min.Glass fabric is cut into 8 × 8cm sizes, amounts to 10 layers, is positioned on 60 DEG C of constant temperature glass plates, resin solution is equal
It is even to be impregnated in fiber cloth.It is put it to after standing a period of time in vacuum drying oven according in 125 DEG C of -2h, the temperature of 155 DEG C of -6h
It spends program and removes solvent.Then naturally cool to room temperature.
It is put into hot press after preliminary-dip piece is positioned in mold, closes film.At 80 DEG C, heat-insulation pressure keeping under conditions of 12MPa
15min.Subsequent release is pressurized to 4MPa after being rapidly heated to 220 DEG C with 15 DEG C/min, with the heating rate liter of 8 DEG C/min
Temperature melts 5min to 230 DEG C under the temperature condition.With final vacuum 2 times, pressure is risen into 12MPa, and carry out by following procedure
Hot-press solidifying：260 DEG C of -2h, 290 DEG C of -2h, 370 DEG C of -2h.After hot-press solidifying, heating is closed, keeps pressure constant, is started
Cooling, rate of temperature fall is 2 DEG C/min, and after temperature drops to 50 DEG C or less, release simultaneously demoulds the laminate for taking out and pressing.
Embodiment two
Using nucleophilic displacement process, synthesize the PPEN-Ph oligomers of n=20, and by it with BP-Ph by mass percentage
50：50 are dissolved in n,N-Dimethylformamide (DMF) solvent, are configured to the glue that mass percent concentration is 25%, simultaneously
Addition accounts for the mass mixings objects such as 8% 4,4- diaminodiphenylsulfones/zinc chloride of resin gross mass as curing agent, heating stirring
30min.Glass fabric is cut into 8 × 8cm sizes, amounts to 10 layers, is positioned on 60 DEG C of constant temperature glass plates, resin solution is equal
It is even to be impregnated in fiber cloth.It is put it to after standing a period of time in vacuum drying oven according in 135 DEG C of -2h, the temperature of 165 DEG C of -10h
It spends program and removes solvent.Then naturally cool to room temperature.
It is put into hot press after preliminary-dip piece is positioned in mold, closes film.At 100 DEG C, heat-insulation pressure keeping under conditions of 15MPa
15min.Subsequent release is pressurized to 5MPa after being rapidly heated to 230 DEG C with 12 DEG C/min, with the heating rate of 8 DEG C/min
240 DEG C are warming up to, 2min is melted under the temperature condition.With final vacuum 2 times, pressure is risen into 15MPa, and by following procedure into
Row hot-press solidifying：260 DEG C of -2h, 290 DEG C of -2h, 370 DEG C of -2h.After hot-press solidifying, heating is closed, keeps pressure constant, opens
Begin to cool down, rate of temperature fall is 2 DEG C/min, and after temperature drops to 50 DEG C or less, release simultaneously demoulds the laminate for taking out and pressing.
Embodiment three
By the PPEN-Ph of n=20 and BP-Ph by mass percentage 75：25 are dissolved in dimethyl sulfoxide (DMSO) (DMSO) solvent,
Be configured to the glue that mass percent concentration is 25%, at the same be added account for 8% 4,4- diaminodiphenylsulfones of resin gross mass/
The mass mixings such as zinc chloride object is as curing agent, heating stirring 30min.Quartz fiber cloth is cut into 8 × 8cm sizes, amounts to 10
Layer, is positioned on 80 DEG C of constant temperature glass plates, by resin solution homogeneous impregnation in fiber cloth.It is put it to after standing a period of time
In vacuum drying oven solvent is removed according to the temperature program(me) in 135 DEG C of -2h, 180 DEG C of -10h.Then naturally cool to room temperature.
It is put into hot press after preliminary-dip piece is positioned in mold, closes film.At 120 DEG C, heat-insulation pressure keeping under conditions of 20MPa
30min.Subsequent release is pressurized to 5MPa after being rapidly heated to 230 DEG C with 12 DEG C/min, with the heating rate liter of 8 DEG C/min
Temperature is to 240 DEG C, after temperature stabilization, pressure is risen to 20MPa, and carry out hot-press solidifying by following procedure：260 DEG C of -2h, 290
DEG C -2h, 370 DEG C of -2h.After hot-press solidifying, close heating, keep pressure it is constant, start to cool down, rate of temperature fall be 2 DEG C/
Min, after temperature drops to 50 DEG C or less, release simultaneously demoulds the laminate for taking out and pressing.
Claims (3)
1. a kind of preparation method of the fabric enhancing blending resin base composite laminate of phthalonitrile containing Phthalazinone,
It is characterized in that, the fabric enhancing blending resin base composite laminate of phthalonitrile containing Phthalazinone includes
Fabric and the blending resin matrix of phthalonitrile containing Phthalazinone are according to mass percentage composition：
Fabric：50~70 parts；
The blending resin of phthalonitrile containing Phthalazinone：30~50 parts；
The blending resin of phthalonitrile containing Phthalazinone includes two kinds of components, and the mass ratio of component 1 and component 2 is
4:1~1:4；
The structural formula of component 1 is as follows：
Wherein,
R1It is hydrogen, halogenic substituent, phenyl, phenoxy group, alkyl or alkoxy,
R2It is hydrogen, halogenic substituent, phenyl, phenoxy group, alkyl or alkoxy,
R3It is hydrogen, halogenic substituent, phenyl, phenoxy group, alkyl or alkoxy,
R4It is hydrogen, halogenic substituent, phenyl, phenoxy group, alkyl or alkoxy,
Above-mentioned R1、R2、R3And R4In alkyl or alkoxy be contain at least one carbon atom, R1、R2、R3And R4Structure it is identical or
It is different；n≥1；
The structural formula of component 2 is as follows：The fabric
For one kind in quartz fiber cloth, glass fabric, carbon cloth, aryl fiber cloth, basalt fiber cloth；
The preparation method of the fabric enhancing blending resin base composite laminate of phthalonitrile containing Phthalazinone,
Steps are as follows：
The dissolving of Phthalazinone phthalonitrile blending resin will be contained in organic solvent, addition is accounted for containing Phthalazinone neighbour
The crosslinking and curing agent of benzene dicarbonitrile blending resin content 8wt%, it is 25~40% to be configured to Solid content mass percent concentration
Fabric is immersed in resin solution by resin solution, is made the surface homogeneous impregnation resin solution of fabric, is dried through hot-fluid
Dry passage removes solvent, and hot-fluid drying channel temperature is 100~200 DEG C, and drying time is 8~12h, after naturally cooling to room temperature
Prepreg tape is made；By prepreg tape be cut into the matched preliminary-dip piece of mold size, according to the thickness of composite material laminated board be laid with
The preliminary-dip piece of the corresponding number of plies, obtains prepreg；Prepreg is put in mold technique through hot press molding, completes curing reaction, is taken off
Enhance the blending resin base composite laminate of phthalonitrile containing Phthalazinone after mould up to fabric；
The crosslinking and curing agent is 4,4`- diaminodiphenylmethane, two methyl phenyl ethers anisole of 4,4`- diamino, 4,4`- diamino hexichol
One kind in sulfone, the blend with anhydrous zinc chloride, the two mass ratio are 5:1~1:5.
2. preparation method according to claim 1, which is characterized in that the program of the hot press forming technology is：50
15~20min is kept the temperature at a temperature of~120 DEG C, pressurize 8~20MPa, is vented 3 times；Release, with the heating speed of 10~15 DEG C/min
After rate is warming up to 200~250 DEG C, pressurize 8~20MPa, and 230~290 DEG C are warming up to the heating rate of 6~8 DEG C/min, and
2~3min is kept under the temperature condition；Pressure is risen into 15MPa, is vented 1~2 time, by following procedure hot-press solidifying：265℃-
2h, 295 DEG C of -2h, 375 DEG C of -2h；Pressure when holding hot-press solidifying, is cooled down with 2~3 DEG C/min rates, and temperature takes off after being down to 50 DEG C
Mould.
3. preparation method according to claim 1 or 2, which is characterized in that the organic solvent is N, N- dimethyl methyls
One or more of amide, DMAC N,N' dimethyl acetamide, dimethyl sulfoxide (DMSO), N-Methyl pyrrolidone, chloroform mix.
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| CN107286649B (en) * | 2017-08-01 | 2020-03-31 | 四川理工学院 | Electromagnetic microwave shielding composite material and preparation method thereof |
| CN108454135B (en) * | 2018-01-31 | 2020-07-14 | 航天材料及工艺研究所 | Phthalonitrile resin prepreg, composite material and preparation method thereof |
| CN108442122B (en) * | 2018-04-26 | 2019-08-27 | 湖南师范大学 | Sizing agent for preparing quartz fiber/nitrile resin composite material |
| CN113234314B (en) * | 2021-04-14 | 2022-04-15 | 电子科技大学 | Preparation method of aramid fiber reinforced poly (arylene ether nitrile) composite material |
| CN113927920A (en) * | 2021-09-13 | 2022-01-14 | 湖北三江航天江北机械工程有限公司 | Composite material antenna housing forming method |
| CN114474778B (en) * | 2022-01-27 | 2024-05-24 | 中国航空工业集团公司济南特种结构研究所 | Preparation method of modified high-silicon-content aryne resin and composite material thereof |
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| CN101619131B (en) * | 2009-07-25 | 2012-07-25 | 大连理工大学 | O-phthalodinitrile end-blocked soluble polyarylether resin with phthalazinone structure and condensate and preparation method thereof |
| CN103834008B (en) * | 2014-03-10 | 2016-09-28 | 中国科学院化学研究所 | A kind of o-phthalonitrile resin and preparation method thereof |
| CN103965638B (en) * | 2014-05-14 | 2016-06-15 | 大连理工大学 | A kind of continuous lod Phthalazinone copolymerization aryl ether sulfone thermoplastic blends matrix composite and preparation method thereof |
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| CN106928488A (en) | 2017-07-07 |
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