CN107955371A - The preparation method of bimaleimide resin epoxy resin composite material - Google Patents
The preparation method of bimaleimide resin epoxy resin composite material Download PDFInfo
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- CN107955371A CN107955371A CN201711337737.2A CN201711337737A CN107955371A CN 107955371 A CN107955371 A CN 107955371A CN 201711337737 A CN201711337737 A CN 201711337737A CN 107955371 A CN107955371 A CN 107955371A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08J2471/10—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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
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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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
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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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5435—Silicon-containing compounds containing oxygen containing oxygen in a ring
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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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/544—Silicon-containing compounds containing nitrogen
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
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- Epoxy Resins (AREA)
Abstract
The present invention relates to polymeric material field, specifically a kind of preparation method of bimaleimide resin epoxy resin composite material.Comprise the following steps：By weight, by 50~100 parts of bimaleimide resins, 20~100 parts of allylic compounds, 1~30 part of toughener, stirred at 50~200 DEG C, after melting is uniformly dispersed, cool to 70~150 DEG C, add 0.1~10 part of antioxidant, 0.1~20 part of UV absorbers, after melting is uniformly dispersed, cool to 70~150 DEG C, add 1~50 part of epoxy resin, 0.1~10 part of coupling agent, 0.1~10 part of thixotropic agent, after being uniformly dispersed, obtain resin combination, resin combination is carried out to apply membrane process and fiber composite process, bimaleimide resin epoxy resin composite material is obtained after curing.
Description
Technical field
The present invention relates to polymeric material field, specifically a kind of illumination aging resisting performance bimaleimide resin
The preparation method of epoxy resin composite material.
Background technology
It is well known that bimaleimide resin is with its excellent humidity resistance, hygroscopicity is low, radiation hardness, anti-flammability, it is excellent
The features such as different mechanical performance, it is widely used in the fields such as aerospace, electronics, track traffic lamp.While plurality of advantages,
There is also many deficiencies, the problems such as solidification temperature is high, brittleness is big, poor dimensional stability, hardness are low, generally require modification.It is common
Method of modifying have allyl compound modification, aromatic diamine modification, epoxy resin modification, epoxy resin modification, thermoplasticity
Resin modified and addition inorganic filler modification etc..
Epoxy resin have excellent bonding, it is corrosion-resistant, insulation etc. performance, be widely used in adhesive, coating, electrically absolutely
In edge material and composite material.Since epoxy resin composite material has the characteristics that intensity is higher, low density, gradually into
For one of indispensable basic material of industrial circle.But epoxy composite material heat resistance, wearability, dimensional stability,
Brittleness etc. Shortcomings, are limited by very large its application.Especially long-term exposure in the sun, accelerates resin
Aging.
Ultra-violet absorber be it is a kind of can suppress or weaken degradation of the light to plastics, improve plastic material light resistance
Material, and most of they can absorb ultraviolet.Ultraviolet in sunlight is to produce aging action to high molecular material
Main cause.Although ultraviolet only accounts for 5% of sunlight or so, energy is but very big, its energy is enough the chemistry for destroying polymer
Key, makes its molecular chain rupture, crosslinking, causes its mechanical property that canceration occurs, meanwhile, its color also changes.
The effect of antioxidant is to eliminate free radical, or promotes the decomposition of hydroperoxides, prevents the progress of chain reaction.
The thermal oxidation process of organic compound is a series of free chain reaction, under the action of heat, light or oxygen, organic molecule
Chemical bond is broken, and generates active free radical and hydroperoxides.Hydroperoxides are decomposed reaction, also generate hydrocarbon oxygen
Free radical and hydroxyl radical free radical.These free radicals can trigger a series of free chain reaction, cause organic compound
Basic change occurs for structure and property.
The content of the invention
The purpose of the present invention is exactly to overcome the deficiencies of the prior art and provide a kind of bimaleimide resin asphalt mixtures modified by epoxy resin
The comprehensive performance such as the preparation method of resin composite material, heat endurance, craftsmanship, wearability, illumination aging resisting significantly improves.
The present invention solves the technical solution that above-mentioned technical problem uses：A kind of bimaleimide resin epoxy resin is answered
The preparation method of condensation material, it is characterised in that comprise the following steps：
By weight, by 50~100 parts of bimaleimide resins, 20~100 parts of allylic compounds, 1~30 part of toughness reinforcing
Agent, is stirred at 50~200 DEG C, after melting is uniformly dispersed, cools to 70~150 DEG C, add 0.1~10 part of antioxidant, 0.1~
20 parts of UV absorbers, after melting is uniformly dispersed, cool to 70~150 DEG C, add 1~50 part of epoxy resin, 0.1~10 part
Coupling agent, 0.1~10 part of thixotropic agent, after being uniformly dispersed, obtain resin combination, and resin combination is carried out to apply membrane process and fibre
Compound working procedure is tieed up, bimaleimide resin epoxy resin composite material is obtained after curing.
The bimaleimide resin is 4,4,- diphenyl methane dimaleimide, N, penylene span carrys out acyl between N-
Imines, 4,4,- Diphenyl Ether Bismaleimide, 4,4,The mixing of one kind or its arbitrary proportion in-diphenyl sulphone (DPS) bismaleimide
Thing.
The antioxidant for antioxidant 1010, antioxidant 1076 or with one kind in the compound of irgasfos 168.
The toughener for poly(aryl ether ketone), polyether sulphone, polyetherimide, polyphenylene oxide, polyphenylene sulfide, nitrile rubber,
The mixture of one kind or its arbitrary proportion in makrolon.
The ultra-violet absorber is that UV-328, UV-327, UV-531, UV-9, UV-O, UV-P are a kind of or its is any
The mixture of ratio.
The coupling agent is the mixture of one kind or its arbitrary proportion in KH550, KH560.
The fiber for carbon fiber, glass fibre, quartz fibre, aramid fiber, one kind in basalt fibre or its
The blended fabric arbitrarily arranged in pairs or groups.
The thixotropic agent is aerosil, organobentonite, rilanit special, one kind in polyamide wax or several
Kind.
The allylic compound is diallyl bisphenol, in diallyl bisphenol ether, diallyl bisphenol S
A kind of or its arbitrary proportion mixture.
The epoxy resin is one in bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-s epoxy resin
The mixture of kind or its arbitrary proportion.
The invention has the advantages that ultra-violet absorber and antioxidant are added to bimaleimide resin epoxy resin
In system so that the composite material of preparation has more preferable illumination aging resisting characteristic.Toughener is added to bismaleimide tree
In alicyclic ring epoxy resin system, the brittleness of resin is improved so that the composite material of preparation has certain toughness.The span of preparation
Bismaleimide resin epoxy-resin systems, have good craftsmanship, can carry out film and combination process, to prepare preimpregnation
Material.Standby bimaleimide resin epoxy-resin systems, preparation process is simple, production cost is low, excellent combination property.
Embodiment
With reference to embodiment, the present invention will be further described：
Embodiment 1：
Stock up by following formulas：
4,4,80 mass parts of-diphenyl methane dimaleimide；
60 mass parts of diallyl bisphenol；
20 mass parts of bisphenol F type epoxy；
0.2 mass parts of antioxidant 1010；
0.2 mass parts of irgasfos 168；
0.4 mass parts of UV-9；
6 mass parts of poly(aryl ether ketone)；
0.5 mass parts of KH560；
1.5 mass parts of aerosil.
By 80 part 4,4 ,-diphenyl methane dimaleimide, 60 parts of diallyl bisphenols, 6 parts of poly(aryl ether ketone), 150
Stirred at DEG C, after melting is uniformly dispersed, cool to 110 DEG C, addition, 0.2 part of antioxidant 1010,0.2 part of irgasfos 168,0.4
Part UV-9, after melting is uniformly dispersed, cools to 80 DEG C, adds 20 parts of bisphenol F type epoxies, 0.5 part of KH560,1.5 parts of gas phase dioxies
SiClx, after being uniformly dispersed, the resin mixed is directly poured into the glue groove of film applicator, carries out painting membrane process, then multiple
Compound working procedure is carried out on conjunction machine, resin is combined with fiber, obtains prepreg.Prepreg is cut, laying, be put into autoclave into
Row elevated cure, curing process are 180 DEG C/1h+200 DEG C/3h, are then cooled down, the demoulding, up to a kind of illumination aging resisting performance
Bismaleimide resin composite material.Meanwhile resin combination is poured into flat plate mold, it is put into baking oven, curing process 180
DEG C/1h+200 DEG C/3h, cure pure resin model and be tested for the property.
Test result：Tensile strength is 62MPa, stretch modulus 3.1GPa, bending strength 86MPa, and bending modulus is
3.5GPa, light resistance grade are 4 grades.
Embodiment 2：
Stock up by following formulas：
4,4,80 mass parts of-diphenyl methane dimaleimide；
50 mass parts of diallyl bisphenol；
10 mass parts of Diallyl Bisphenol Sulfone Ether；
20 mass parts of bisphenol F type epoxy；
0.2 mass parts of antioxidant 1076；
0.2 mass parts of irgasfos 168；
0.4 mass parts of UV-327；
6 mass parts of polyether sulphone；
0.5 mass parts of KH550；
1.5 mass parts of aerosil.
By 80 part 4,4 ,-diphenyl methane dimaleimide, 50 parts of diallyl bisphenols, 10 parts of diallyl bisphenol Ss
Ether, 6 parts of polyether sulphones, are stirred at 150 DEG C, after melting is uniformly dispersed, are cooled to 110 DEG C, are added 0.2 part of antioxidant
1010th, 0.2 part of irgasfos 168,0.4 part of UV-327, after melting is uniformly dispersed, cool to 80 DEG C, add 20 parts of Bisphenol F type rings
The resin mixed, after being uniformly dispersed, is directly poured into the glue of film applicator by oxygen, 0.5 part of KH550,1.5 parts of aerosils
In groove, painting membrane process is carried out, compound working procedure is then carried out on compounding machine, resin is combined with fiber, obtains prepreg.Will be pre-
Leaching material is cut, laying, is put into autoclave and is carried out elevated cure, and curing process is 180 DEG C/1h+200 DEG C/3h, is then cooled down, and is taken off
Mould, up to a kind of bismaleimide resin composite material of illumination aging resisting performance.Meanwhile resin combination is poured into tablet
Mould, is put into baking oven, and curing process is 180 DEG C/1h+200 DEG C/3h, cures pure resin model and is tested for the property.
Test result：Tensile strength is 68MPa, stretch modulus 3.2GPa, bending strength 93MPa, and bending modulus is
3.3GPa, light resistance grade are 4 grades.
Comparative example：
Stock up by following formulas：
4,4,80 mass parts of-diphenyl methane dimaleimide；
60 mass parts of diallyl bisphenol；
20 mass parts of bisphenol F type epoxy；
6 mass parts of polyether sulphone；
0.5 mass parts of KH550；
1.5 mass parts of aerosil.
By 80 part 4,4 ,-diphenyl methane dimaleimide, 60 parts of diallyl bisphenols, 6 parts of polyether sulphones, at 150 DEG C
Lower stirring, after melting is uniformly dispersed, cools to 80 DEG C, adds 20 parts of bisphenol F type epoxies, 0.5 part of KH550,1.5 parts of gas phases two
Silica, after being uniformly dispersed, the resin mixed is directly poured into the glue groove of film applicator, carries out painting membrane process, Ran Hou
Compound working procedure is carried out on compounding machine, resin is combined with fiber, obtains prepreg.Prepreg is cut, laying, be put into autoclave
Elevated cure is carried out, curing process is 180 DEG C/1h+210 DEG C/3h, is then cooled down, the demoulding, up to a kind of illumination aging resisting performance
Bismaleimide resin composite material.Meanwhile resin combination is poured into flat plate mold, baking oven is put into, curing process is
180 DEG C/1h+210 DEG C/3h, cure pure resin model and be tested for the property.
Test result：Tensile strength is 88MPa, stretch modulus 3.5GPa, bending strength 115MPa, and bending modulus is
3.3GPa, light resistance grade are 3 grades.
It can be seen that from the contrast of embodiment 1,2 and comparative example and add antioxidant and ultra-violet absorber, resin system
Illumination aging resisting performance significantly improves, but the mechanical property of composite material is declined slightly.
Claims (10)
1. a kind of preparation method of bimaleimide resin epoxy resin composite material, it is characterised in that comprise the following steps：
By weight, by 50~100 parts of bimaleimide resins, 20~100 parts of allylic compounds, 1~30 part of toughness reinforcing
Agent, is stirred at 50~200 DEG C, after melting is uniformly dispersed, cools to 70~150 DEG C, add 0.1~10 part of antioxidant, 0.1~
20 parts of UV absorbers, after melting is uniformly dispersed, cool to 70~150 DEG C, add 1~50 part of epoxy resin, 0.1~10 part
Coupling agent, 0.1~10 part of thixotropic agent, after being uniformly dispersed, obtain resin combination, and resin combination is carried out to apply membrane process and fibre
Compound working procedure is tieed up, bimaleimide resin epoxy resin composite material is obtained after curing.
2. the preparation method of bimaleimide resin epoxy resin composite material according to claim 1, it is characterised in that
The bimaleimide resin is 4,4,- diphenyl methane dimaleimide, N, penylene bismaleimide, 4,4 between N-,-
Diphenyl Ether Bismaleimide, 4,4,The mixture of one kind or its arbitrary proportion in-diphenyl sulphone (DPS) bismaleimide.
3. the preparation method of bimaleimide resin epoxy resin composite material according to claim 1, it is characterised in that
The antioxidant for antioxidant 1010, antioxidant 1076 or with one kind in the compound of irgasfos 168.
4. the preparation method of bimaleimide resin epoxy resin composite material according to claim 1, it is characterised in that
The toughener is poly(aryl ether ketone), polyether sulphone, polyetherimide, polyphenylene oxide, polyphenylene sulfide, nitrile rubber, makrolon
In one kind or its arbitrary proportion mixture.
5. the preparation method of bimaleimide resin epoxy resin composite material according to claim 1, it is characterised in that
The ultra-violet absorber for UV-328, UV-327, UV-531, UV-9, UV-O, UV-P be a kind of or its arbitrary proportion it is mixed
Compound.
6. the preparation method of bimaleimide resin epoxy resin composite material according to claim 1, it is characterised in that
The coupling agent is the mixture of one kind or its arbitrary proportion in KH550, KH560.
7. the preparation method of bimaleimide resin epoxy resin composite material according to claim 1, it is characterised in that
The fiber is carbon fiber, glass fibre, quartz fibre, aramid fiber, one kind in basalt fibre or its any collocation
Blended fabric.
8. the preparation method of bimaleimide resin epoxy resin composite material according to claim 1, it is characterised in that
The thixotropic agent is aerosil, the one or more in organobentonite, rilanit special, polyamide wax.
9. the preparation method of bimaleimide resin epoxy resin composite material according to claim 1, it is characterised in that
The allylic compound for diallyl bisphenol, diallyl bisphenol ether, one kind in diallyl bisphenol S or its
The mixture of arbitrary proportion.
10. the preparation method of bimaleimide resin epoxy resin composite material according to claim 1, it is characterised in that
The epoxy resin for bisphenol A type epoxy resin, bisphenol f type epoxy resin, one kind in bisphenol-s epoxy resin or its
The mixture of meaning ratio.
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| CN201711337737.2A CN107955371A (en) | 2017-12-14 | 2017-12-14 | The preparation method of bimaleimide resin epoxy resin composite material |
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| CN201711337737.2A CN107955371A (en) | 2017-12-14 | 2017-12-14 | The preparation method of bimaleimide resin epoxy resin composite material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108587162A (en) * | 2018-05-02 | 2018-09-28 | 江苏恒神股份有限公司 | A kind of non-autoclave molding prepreg bismaleimide resin and preparation method thereof |
| CN111040163A (en) * | 2019-11-29 | 2020-04-21 | 航天特种材料及工艺技术研究所 | Bismaleimide resin, air bag for autoclave molding and preparation method thereof |
| CN114561101A (en) * | 2022-04-01 | 2022-05-31 | 焦作市天益科技有限公司 | Diallyl bisphenol A modified bismaleimide resin capable of prolonging shelf life and preparation method thereof |
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| CN105860522A (en) * | 2016-04-20 | 2016-08-17 | 威海光威复合材料股份有限公司 | Preparation method of modified bismaleimide resin |
| CN106046786A (en) * | 2016-08-22 | 2016-10-26 | 威海光威复合材料股份有限公司 | Method for preparing composite material from nanometer ceramic powder modified bismaleimide resin |
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| CN106221215A (en) * | 2016-08-22 | 2016-12-14 | 威海光威复合材料股份有限公司 | Cyanate ester resin composite material preparation method |
| CN107189435A (en) * | 2017-07-17 | 2017-09-22 | 威海光威复合材料股份有限公司 | The preparation method of bismaleimide resin composite material |
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| CN105860522A (en) * | 2016-04-20 | 2016-08-17 | 威海光威复合材料股份有限公司 | Preparation method of modified bismaleimide resin |
| CN106046786A (en) * | 2016-08-22 | 2016-10-26 | 威海光威复合材料股份有限公司 | Method for preparing composite material from nanometer ceramic powder modified bismaleimide resin |
| CN106046691A (en) * | 2016-08-22 | 2016-10-26 | 威海光威复合材料股份有限公司 | Nanometer ceramic modified cyanate resin/epoxy resin composite material preparation method |
| CN106189225A (en) * | 2016-08-22 | 2016-12-07 | 威海光威复合材料股份有限公司 | Nano-ceramic powder modified cyanic acid ester resin prepares the method for composite |
| CN106221215A (en) * | 2016-08-22 | 2016-12-14 | 威海光威复合材料股份有限公司 | Cyanate ester resin composite material preparation method |
| CN107189435A (en) * | 2017-07-17 | 2017-09-22 | 威海光威复合材料股份有限公司 | The preparation method of bismaleimide resin composite material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108587162A (en) * | 2018-05-02 | 2018-09-28 | 江苏恒神股份有限公司 | A kind of non-autoclave molding prepreg bismaleimide resin and preparation method thereof |
| CN111040163A (en) * | 2019-11-29 | 2020-04-21 | 航天特种材料及工艺技术研究所 | Bismaleimide resin, air bag for autoclave molding and preparation method thereof |
| CN114561101A (en) * | 2022-04-01 | 2022-05-31 | 焦作市天益科技有限公司 | Diallyl bisphenol A modified bismaleimide resin capable of prolonging shelf life and preparation method thereof |
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