CN109666297B - Ultraviolet fluorescent bismaleimide resin carbon fiber prepreg for sacrificial layer - Google Patents
Ultraviolet fluorescent bismaleimide resin carbon fiber prepreg for sacrificial layer Download PDFInfo
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- CN109666297B CN109666297B CN201811462560.3A CN201811462560A CN109666297B CN 109666297 B CN109666297 B CN 109666297B CN 201811462560 A CN201811462560 A CN 201811462560A CN 109666297 B CN109666297 B CN 109666297B
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- ultraviolet fluorescent
- bismaleimide resin
- carbon fiber
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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
- 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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- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The invention belongs to the technical field of high polymer materials, and relates to an ultraviolet fluorescent bismaleimide resin carbon fiber prepreg for a sacrificial layer. The ultraviolet fluorescent bismaleimide resin carbon fiber prepreg is prepared from the following raw materials in parts by weight: 100 parts of bismaleimide resin matrix, 60-100 parts of process modifier, 0-50 parts of composite curing agent, 0-50 parts of auxiliary agent and 1-50 parts of ultraviolet fluorescent powder. According to the invention, the bismaleimide resin carbon fiber prepreg is prepared by adding the ultraviolet fluorescent powder into the sacrificial layer, so that the sacrificial layer and the body can be distinguished only by irradiation of an ultraviolet lamp when the composite material member is milled, the problem that the sacrificial layer of the carbon fiber prepreg is difficult to distinguish is solved, the problem that the body is easy to damage and difficult to measure if the feeding amount is improperly controlled when the carbon fiber prepreg is used as the sacrificial layer during assembling and milling is avoided, and the surface quality of the large composite material member is greatly improved.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and relates to an ultraviolet fluorescent bismaleimide resin carbon fiber prepreg for a sacrificial layer.
Background
At present, the composite material is widely applied to main load-bearing structures of military and civil aircrafts, such as wing skins, wing spars and the like. In the manufacturing and assembling process, the problem of assembling out-of-tolerance is inevitable, the preparation process of the composite material is complex, and the problem of assembling out-of-tolerance is more prominent due to easy occurrence of curing deformation. According to the traditional method, a method of adding a gasket/forcing assembly is generally adopted to solve the problem of assembly out-of-tolerance, however, the gasket can reduce the strength of the connecting structure and is easy to generate sealing problems, and the forcing assembly can cause larger local assembly stress and has adverse effects on the structure.
According to the current advanced design concept, for the surface of a resin-based composite material structure with an assembly relation, a plurality of sacrificial layers can be paved outside the body structure during preparation, and the sacrificial layers are milled according to actual conditions during assembly so as to ensure the assembly quality. When the carbon fiber composite material structure is prepared, the glass fiber prepreg is used as a sacrificial layer, so that the resolution is easy, the body is not easy to be damaged during milling, and severe thermal stress can be caused; the carbon fiber prepreg which is the same as the body is used, so that the problem of thermal deformation does not exist, however, the sacrificial layer is completely the same as the body, and if the feeding amount is improperly controlled during assembling and milling, the body is easily damaged, and the measurement is not easy.
Disclosure of Invention
The invention aims to provide an ultraviolet fluorescent bismaleimide resin carbon fiber prepreg for a sacrificial layer, aiming at the defects in the prior art.
The technical scheme of the invention is that the ultraviolet fluorescent bismaleimide resin carbon fiber prepreg for the sacrificial layer comprises the following raw materials in percentage by mass:
the bismaleimide resin matrix is one or a mixture of more than two of N, N ' - (4,4 ' -methylene diphenyl) bismaleimide, N ' - (4-methyl-1, 3-methylene) bismaleimide and 2,2, 4-trimethyl-1, 6-hexamethylene diamine bismaleimide.
The process modifier is one or more of diallyl bisphenol A, diallyl bisphenol S, 2' -diisopropenyl bisphenol A, diallyl bisphenol A ether, allyl phenol and allyl cresol.
The composite curing agent is one or a combination of an amine curing agent, an anhydride curing agent or an imidazole curing agent.
The particle size of the ultraviolet fluorescent powder is 1 um-20 um, and the ultraviolet fluorescent powder can be developed under ultraviolet light with the wavelength ranging from 200nm to 400 nm.
The auxiliary agent is one or a mixture of more than two of coupling agent, flame retardant, plasticizer and inorganic filler.
The method for preparing the ultraviolet fluorescent bismaleimide resin carbon fiber prepreg for the sacrificial layer comprises the following steps,
1) preparing ultraviolet fluorescent bismaleimide resin:
(1) the bismaleimide resin matrix and a modifier are heated to 80-150 ℃ under the stirring action to form a uniform and stable component;
(2) dispersing a composite curing agent and an auxiliary agent in the bismaleimide resin in the step (1) to form a uniform and stable mixture;
(3) uniformly dispersing an ultraviolet fluorescent agent in the mixture obtained in the step (2) to prepare ultraviolet fluorescent bismaleimide resin;
2) preparation of ultraviolet fluorescent bismaleimide resin film
Coating ultraviolet fluorescent bismaleimide resin on release paper or other carriers on a film coating machine at the temperature of 60-100 ℃ to prepare an ultraviolet fluorescent bismaleimide resin film;
3) preparation of ultraviolet fluorescent bismaleimide resin carbon fiber prepreg
Spreading a resin adhesive film on carbon fibers or carbon fiber woven fabrics by using a hot-melt pre-dipping machine, carrying out hot-pressing, dipping and compounding on the ultraviolet fluorescent bismaleimide resin adhesive film and the carbon fibers or the carbon fiber woven fabrics in the pre-dipping machine, controlling the temperature of a heating roller of the hot-melt pre-dipping machine and the speed of the heating roller, wherein the temperature of the heating roller is 70-100 ℃, and the speed of the heating roller is 3-10 m/min, so as to prepare the ultraviolet fluorescent bismaleimide resin carbon fiber pre-dipped material.
The invention has the advantages and beneficial effects
According to the invention, the ultraviolet fluorescent bismaleimide resin carbon fiber prepreg prepared by adding the ultraviolet fluorescent powder into the sacrificial layer is adopted, the sacrificial layer prepared by the prepreg is paved on the surface of the body structure, when the composite material member is milled, the sacrificial layer and the body can be distinguished only by adopting ultraviolet lamp irradiation, the problem that the sacrificial layer of the carbon fiber prepreg is difficult to distinguish is solved, the problem that the body is easy to damage if the feeding amount is improperly controlled during assembling and milling of the carbon fiber prepreg as the sacrificial layer and the measurement is difficult is avoided, the problem of the assembling out-of-tolerance of large composite material members such as wing skins and wing spars is improved, and the surface quality of the large composite material member is greatly improved.
Detailed Description
The ultraviolet fluorescent bismaleimide resin prepreg for the sacrificial layer comprises the following raw materials in parts by weight:
the bismaleimide resin matrix in the invention is one or a mixture of more than two of N, N ' - (4,4 ' -methylene diphenyl) bismaleimide, N ' - (4-methyl-1, 3-methylene) bismaleimide and 2,2, 4-trimethyl-1, 6-hexamethylene diamine bismaleimide.
The process modifier in the invention is one or more than two of diallyl bisphenol A, diallyl bisphenol S, 2' -diisopropenyl bisphenol A, diallyl bisphenol A ether, allyl phenol and allyl cresol.
The composite curing agent in the invention is one or a combination of an amine curing agent, an anhydride curing agent or an imidazole curing agent.
The ultraviolet fluorescent powder has the particle size of 1-20 um, and can be developed under the ultraviolet light with the wavelength of 200-400 nm.
The auxiliary agent in the invention is one or more than two of coupling agent, flame retardant, plasticizer and inorganic filler.
The invention discloses an ultraviolet fluorescent bismaleimide resin prepreg for a sacrificial layer, which comprises the following components:
preparing an ultraviolet fluorescent bismaleimide resin mixture;
preparing the mixture into a glue film; and
and carrying out hot-pressing infiltration on the carbon fiber or the carbon fiber fabric and the adhesive film to prepare the ultraviolet fluorescent bismaleimide resin prepreg for the sacrificial layer.
The preparation method of the ultraviolet fluorescent bismaleimide resin comprises the following steps:
(1) the bismaleimide resin matrix and a modifier are heated to 80-150 ℃ under the stirring action to form a uniform and stable component;
(2) dispersing a curing agent, a coupling agent, a flame retardant, a plasticizer, an inorganic filler and other auxiliaries in the bismaleimide resin in the step (1) to form a uniform and stable mixture;
(3) and (3) uniformly dispersing the ultraviolet fluorescent agent in the mixture obtained in the step (2) to prepare the ultraviolet fluorescent bismaleimide resin.
Coating the ultraviolet fluorescent bismaleimide resin on release paper or other carriers on a film coating machine at the temperature of 60-100 ℃ to prepare the ultraviolet fluorescent bismaleimide resin film.
Spreading a resin adhesive film on the carbon fiber/carbon fiber woven fabric by using a hot-melt pre-dipping machine, carrying out hot-pressing, dipping and compounding on the ultraviolet fluorescent bismaleimide resin adhesive film and the carbon fiber or the carbon fiber woven fabric in the pre-dipping machine, controlling the temperature of a heating roller of the hot-melt pre-dipping machine and the speed of the heating roller, wherein the temperature of the heating roller is 70-100 ℃, and the speed of the heating roller is 3-10 m/min, so as to prepare the ultraviolet fluorescent bismaleimide resin carbon fiber pre-dip material.
Example 1
Weighing the raw materials according to the following mass ratio, and uniformly mixing to prepare the ultraviolet fluorescent bismaleimide resin: bismaleimide resin matrix: the process modifier comprises the following steps: compound curing agent: a toughening agent: ultraviolet fluorescent powder is 100: 70: 20: 40: 10. wherein the bismaleimide resin is N, N ' - (4,4 ' -methylenediphenyl) bismaleimide and N, N ' - (4-methyl-1, 3-methylene) bismaleimide, and the proportion is 1: 1; the process modifier is diallyl bisphenol A and diallyl bisphenol A ether, and the proportion of the diallyl bisphenol A and the diallyl bisphenol A ether is 2: 1; the curing agent is an amine curing agent. Mixing and stirring a bismaleimide resin matrix and a process modifier in a reaction kettle or other containers, simultaneously heating to 90-130 ℃, stopping heating after observing that the resin is uniform and transparent in color, continuously adding a toughening agent and a composite curing agent, stirring uniformly, adding ultraviolet fluorescent powder with the particle size of 10 mu m, and stirring uniformly at a high speed to ensure that the resin mixture is stirred uniformly.
And coating the mixed ultraviolet fluorescent bismaleimide resin on release paper on a film coating machine at the temperature of 60-70 ℃ to prepare the ultraviolet fluorescent bismaleimide resin film.
The prepared resin adhesive film is laid on the carbon fiber woven fabric in a sandwich mode by adopting a hot-melting pre-dipping machine, the ultraviolet fluorescent bismaleimide resin adhesive film and the carbon fiber woven fabric are subjected to hot-pressing, dipping and compounding on the pre-dipping machine, the temperature of a heating roller of the hot-melting pre-dipping machine and the vehicle speed are controlled, the temperature of the heating roller is 60-80 ℃, and the vehicle speed is 4-6 m/min, so that the ultraviolet fluorescent bismaleimide resin carbon fiber pre-dipping material is prepared.
When a part is prepared, ultraviolet fluorescent bismaleimide resin carbon fiber prepreg is paved on the surface of a bismaleimide resin carbon fiber composite material member body, after curing and molding, an ultraviolet lamp is installed above a milling worktable during the assembling and milling process, and the light is irradiated on the surface of the part, so that the surface of the part shows fluorescence, and milling is carried out according to a normal milling procedure.
Example 2
Weighing the raw materials according to the following mass ratio, and uniformly mixing to prepare the ultraviolet fluorescent bismaleimide resin: bismaleimide resin matrix: the process modifier comprises the following steps: a toughening agent: ultraviolet fluorescent powder is 100: 80: 10: 5. wherein the bismaleimide resin is N, N ' - (4,4 ' -methylene diphenyl) bismaleimide and N, N ' - (4-methyl-1, 3-methylene) bismaleimide, and the proportion is 2: 1; the process modifier is diallyl bisphenol A, and the curing agent is an amine curing agent. Mixing and stirring a bismaleimide resin matrix and a process modifier in a reaction kettle, simultaneously heating to 110-130 ℃, stopping heating after observing that the resin is uniform and transparent in color, continuously adding a toughening agent, uniformly stirring, adding ultraviolet fluorescent powder with the particle size of 15um, and stirring at a high speed to uniformly stir the resin mixture.
And coating the mixed ultraviolet fluorescent bismaleimide resin on release paper on a film coating machine at the temperature of 60-70 ℃ to prepare the ultraviolet fluorescent bismaleimide resin film.
The prepared resin adhesive film is laid on the carbon fiber woven fabric in a sandwich mode by adopting a hot-melting pre-dipping machine, the ultraviolet fluorescent bismaleimide resin adhesive film and the carbon fiber woven fabric are subjected to hot-pressing, dipping and compounding on the pre-dipping machine, the temperature of a heating roller of the hot-melting pre-dipping machine and the vehicle speed are controlled, the temperature of the heating roller is 60-80 ℃, and the vehicle speed is 4-6 m/min, so that the ultraviolet fluorescent bismaleimide resin carbon fiber pre-dipping material is prepared.
When a part is prepared, ultraviolet fluorescent bismaleimide resin carbon fiber prepreg is paved on the surface of a bismaleimide resin carbon fiber composite material member body, after curing and molding, an ultraviolet lamp is installed above a milling worktable during the assembling and milling process, and the light is irradiated on the surface of the part, so that the surface of the part shows fluorescence, and milling is carried out according to a normal milling procedure.
Claims (4)
1. An application method of ultraviolet fluorescent bismaleimide resin carbon fiber prepreg as a sacrificial layer is characterized in that: the ultraviolet fluorescent bismaleimide resin carbon fiber prepreg is prepared from the following raw materials in parts by weight:
100 parts of bismaleimide resin matrix
60-100 parts of process modifier
0-50 parts of composite curing agent
0-50 parts of auxiliary agent
1-50 parts of ultraviolet fluorescent powder
The composite curing agent is one or a combination of an amine curing agent, an anhydride curing agent or an imidazole curing agent; the process modifier is one or more than two of diallyl bisphenol A, diallyl bisphenol S, 2' -diisopropenyl bisphenol A, diallyl bisphenol A ether, allyl phenol and allyl cresol;
the preparation method of the ultraviolet fluorescent bismaleimide resin carbon fiber prepreg for the sacrificial layer comprises the following steps:
1) preparing ultraviolet fluorescent bismaleimide resin:
(1) under the stirring action, the bismaleimide resin matrix and a process modifier are heated to 80-150 ℃ to form uniform and stable components;
(2) dispersing a composite curing agent and an auxiliary agent in the bismaleimide resin in the step (1) to form a uniform and stable mixture;
(3) uniformly dispersing ultraviolet fluorescent powder in the mixture obtained in the step (2) to prepare ultraviolet fluorescent bismaleimide resin;
2) preparation of ultraviolet fluorescent bismaleimide resin film
Coating ultraviolet fluorescent bismaleimide resin on release paper or other carriers on a film coating machine at the temperature of 60-100 ℃ to prepare an ultraviolet fluorescent bismaleimide resin film;
3) preparation of ultraviolet fluorescent bismaleimide resin carbon fiber prepreg
Spreading a resin adhesive film on carbon fibers or carbon fiber woven fabrics by using a hot-melt pre-dipping machine, carrying out hot-pressing, dipping and compounding on an ultraviolet fluorescent bismaleimide resin adhesive film and the carbon fibers or the carbon fiber woven fabrics in the pre-dipping machine, controlling the temperature and the speed of a heating roller of the hot-melt pre-dipping machine, wherein the temperature of the heating roller is 70-100 ℃, and the speed of the heating roller is 3-10 m/min, so as to prepare the ultraviolet fluorescent bismaleimide resin carbon fiber pre-dip material;
the application method of the ultraviolet fluorescent bismaleimide resin carbon fiber prepreg comprises the following steps: the ultraviolet fluorescent bismaleimide resin carbon fiber prepreg is used for preparing a sacrificial layer to be paved on the surface of a body structure, and when a composite material component is milled, the sacrificial layer and the body can be distinguished by ultraviolet lamp irradiation.
2. The application method of the ultraviolet fluorescent bismaleimide resin carbon fiber prepreg as a sacrificial layer according to claim 1 is characterized in that: the bismaleimide resin matrix is one or a mixture of more than two of N, N ' - (4,4 ' -methylene diphenyl) bismaleimide, N ' - (4-methyl-1, 3-phenylene) bismaleimide and 2,2, 4-trimethyl-1, 6-hexamethylene diamine bismaleimide.
3. The application method of the ultraviolet fluorescent bismaleimide resin carbon fiber prepreg as a sacrificial layer according to claim 1 is characterized in that: the particle size of the ultraviolet fluorescent powder is 0.5-50 um, and the ultraviolet fluorescent powder can be developed under ultraviolet light with the wavelength within the range of 200-400 nm.
4. The application method of the ultraviolet fluorescent bismaleimide resin carbon fiber prepreg as a sacrificial layer according to claim 1 is characterized in that: the auxiliary agent is one or a mixture of more than two of coupling agent, flame retardant, plasticizer and inorganic filler.
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