CN108656423B - Preparation method of polyimide prepreg - Google Patents
Preparation method of polyimide prepreg Download PDFInfo
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- CN108656423B CN108656423B CN201810384316.3A CN201810384316A CN108656423B CN 108656423 B CN108656423 B CN 108656423B CN 201810384316 A CN201810384316 A CN 201810384316A CN 108656423 B CN108656423 B CN 108656423B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/24—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of indefinite length
- B29C41/28—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of indefinite length by depositing flowable material on an endless belt
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B13/00—Conditioning or physical treatment of the material to be shaped
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/40—Shaping or impregnating by compression not applied
- B29C70/50—Shaping or impregnating by compression not applied for producing articles of indefinite length, e.g. prepregs, sheet moulding compounds [SMC] or cross moulding compounds [XMC]
- B29C70/504—Shaping or impregnating by compression not applied for producing articles of indefinite length, e.g. prepregs, sheet moulding compounds [SMC] or cross moulding compounds [XMC] using rollers or pressure bands
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B13/00—Conditioning or physical treatment of the material to be shaped
- B29B2013/002—Extracting undesirable residual components, e.g. solvents, unreacted monomers, from material to be moulded
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Abstract
The invention relates to a preparation method of a polyimide prepreg, and belongs to the technical field of prepreg preparation. Firstly, obtaining proper resin solution viscosity through resin solution pretreatment, laying a fiber reinforcement after coating resin glue solution on release paper through a tape casting process, realizing impregnation of resin of the fiber reinforcement by using a pressure roller, then removing redundant volatile matters through drying, and finally carrying out film coating and winding. The preparation method adopts a double-roller meshing casting process to effectively solve the technical problem of high-efficiency impregnation of the low-viscosity polyimide resin solution, realizes the batch stable preparation of the polyimide prepreg and lays a good foundation for the engineering application and popularization.
Description
Technical Field
The invention relates to a preparation method of a polyimide prepreg, and belongs to the technical field of prepreg preparation.
Background
The flying Mach number of the advanced high-speed missile is continuously improved in the future, the missile is endowed with quick response capability, strong penetration and high survival capability, high-value maneuvering targets and time-sensitive targets can be effectively struck, and the method plays an important role in future wars. The high-speed missile flies in the dense atmosphere in an engine mode and can be subjected to complex environments such as severe aerodynamic heat, heavy overload and the like. The important missile components such as missile wings, air rudders, antenna covers and air inlet channels are in a low-heat-flow and long-time heating severe environment, the surface temperature is as high as more than 300 ℃ for a short time, and the traditional epoxy composite material and bismaleimide composite material cannot meet the use requirements.
The fiber reinforced polyimide composite material is one of resin-based structural composite materials which can be used for a long time in a high-temperature environment of more than 300 ℃ in the current engineering application. The polyimide composite material is prepared by adopting a layering curing method. When the polyimide structure composite material is prepared by laying, polyimide prepreg is prepared firstly, then the prepreg is laid according to a certain laying mode and a certain laying angle, and the polyimide composite material is obtained after curing. Therefore, quality control of prepregs for polyimide composite layup becomes an important factor in the performance of composites. At present, polyimide prepreg is mainly prepared by directly impregnating a fiber reinforcement with a polyimide resin solution, namely, the fiber reinforcement is coated and impregnated with the polyimide resin solution through a glue solution tank for placing a certain amount of the polyimide resin solution under a set tension, and then the fiber reinforcement is naturally dried to obtain a final prepreg product, or the polyimide resin solution is directly and manually coated on a fiber fabric reinforcement placed on a plane. However, the polyimide resin solution used at present has a low solid content (about 50 wt%), and the resin undergoes a polycondensation reaction in the subsequent composite material curing process to release a large amount of small molecules, so that the polyimide prepreg has a higher initial gel content than epoxy and bismaleimide prepregs, and the resin solution has a low viscosity, and the resin solution flows to some extent in the fiber reinforcement impregnation process, thereby causing uneven distribution of the resin content. On the other hand, the resin solution with lower solid content has the problem of insufficient sizing amount in one-time dipping in the gluing process, and needs sizing for many times, thus leading to low preparation efficiency. In addition, after the polyimide resin solution is impregnated into the fiber reinforcement, the product needs to be dried, and redundant low-boiling-point solvent (ethanol or methanol) is removed to reduce the volatile content of the subsequent composite material during molding and curing, so that the porosity of the composite material is effectively controlled to improve the molding quality of the composite material, and meanwhile, proper low-boiling-point solvent needs to be remained to ensure that the prepreg has certain viscosity, and the prepreg is convenient to bond between layers in the prepreg laying process. The prior art adopts natural airing, the final volatile content and viscosity control of the prepreg are greatly influenced by the environmental temperature, and the preparation efficiency is low.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method for preparing the polyimide prepreg overcomes the defects of the prior art, adopts a vacuum filtration to control the viscosity of a resin solution and a double-roller meshing casting process, solves the technical problem of high-efficiency preparation of a low-viscosity resin solution adhesive film, realizes high-efficiency continuous preparation of the polyimide prepreg, utilizes the control of the advancing speed and the temperature of a drying tunnel in the prepreg arranging process, realizes effective control of the volatile content and the paving property of the prepreg, and improves the qualification rate and the quality consistency of subsequent polyimide composite material members.
The technical solution of the invention is as follows:
a preparation method of polyimide prepreg, the preparation raw material of the polyimide prepreg comprises polyimide resin solution and fiber reinforcement; the method comprises the following steps:
(1) putting the polyimide resin solution into a reaction kettle for vacuum filtration;
(2) placing the polyimide resin solution obtained in the step (1) in a glue solution tank, and forming a polyimide resin glue film on release paper by adopting a tape casting process;
(3) drawing the fiber reinforcement body above the polyimide resin adhesive film in the step (2), and impregnating the polyimide resin adhesive film into the fiber reinforcement body;
(4) drying the product obtained in the step (3);
(5) placing an isolation film above the dried product in the step (4);
(6) and (5) rolling the product in the step (5) by using a rolling device to obtain the prepreg.
In the step (1), the polyimide resin solution is a PMR type polyimide resin solution, and the initial solid content of the resin solution is 45-60 wt%; the polyimide resin is subjected to vacuum filtration, the temperature during the filtration is 30-50 ℃, and the specific gravity of the resin solution after the filtration is 1.05-1.08.
In the step (2), the casting process adopts a double-roller meshing casting process.
The device used by the double-roller meshing casting process comprises a glue solution tank, a gluing round roller and a traction round roller, wherein the glue solution tank is used for containing polyimide resin solution;
one part of the gluing round roller is positioned in the polyimide resin solution in the gluing tank;
the gap between the traction round roller and the gluing round roller is 0.36-0.38 mm;
the traction round roller is used for driving the release paper to move from a gap between the gluing round roller and the traction round roller under the traction action of set tension.
The method of the twin-roll meshing casting process comprises the following steps: placing polyimide resin solution into a glue solution tank, then immersing a part of a gluing round roller into the polyimide resin solution, enabling release paper to pass through a gluing round roller and a traction round roller under the traction action of set tension, starting the gluing round roller and the traction round roller to rotate, enabling the polyimide resin solution to be uniformly coated on the surface of the gluing round roller when the gluing round roller rotates, and enabling the traction round roller to drive the release paper to pass through a gap between the gluing round roller and the release round roller under the traction action of set tension to enable the polyimide resin solution on the surface of the gluing round roller to be uniformly coated on the release paper to form a polyimide resin glue film.
In the step (3), the fiber reinforcement is one or a mixture of more than two of carbon fiber yarn, glass fiber yarn, quartz fiber yarn, carbon fiber fabric, glass fiber fabric and quartz fiber fabric.
In the step (3), the fiber reinforcement is drawn above the polyimide resin adhesive film in the step (2) through a set tension, and the polyimide resin adhesive film is impregnated into the fiber reinforcement through a compression roller; the set tension is 240-260N, and the pressure of the compression roller is 0.05-0.1 MPa.
In the step (4), the product obtained in the step (3) is dried by passing through a drying tunnel at a constant speed at a set advancing speed under the traction of a set tension; the drying temperature is 70-80 ℃, and the advancing speed is 2.0-3 m/min.
In the step (5), the isolating film is placed above the dried product in the step (4) under the action of set tension, and pressure is applied through a compression roller to increase the attaching degree between the isolating film and the product; the set tension is 120-150N, and the compression roller pressure is 0.05-0.1 MPa.
In the step (6), the winding tension in winding is 150-170N.
Compared with the prior art, the invention has the beneficial effects that:
(1) the control of the viscosity of the initial resin solution is realized by a resin solution vacuum filtration mode, and the problem of high-efficiency coating of the low-viscosity polyimide resin adhesive film is solved.
(2) The even coating of the low-viscosity resin glue solution is realized by adopting a double-roller meshing impregnation process;
(3) the accurate control of the resin content is realized through the reasonable control of the glue spreader gap;
(4) tension control before impregnation of the reinforcement is realized through pressure control of the compression roller, so that the wrinkle defect of the prepreg is reduced, and the flatness of the prepreg is improved;
(5) the drying tunnel temperature and the advancing speed of the prepreg are adjusted to control the volatile content and the paving manufacturability of the prepreg, so that the porosity of a subsequent polyimide composite material product can be effectively reduced, and the process control difficulty in the subsequent composite material forming process is reduced.
(6) The polyimide composite material prepared by the prepreg paving layer prepared by the method is cured, and the use temperature is up to 300-500 ℃.
(6) The invention relates to a preparation method of a polyimide prepreg, which comprises the following steps: firstly, obtaining proper resin solution viscosity through resin solution pretreatment, laying a fiber reinforcement after coating resin glue solution on release paper through a tape casting process, realizing impregnation of resin of the fiber reinforcement by using a pressure roller, then removing redundant volatile matters through drying, and finally carrying out film coating and winding. The preparation method adopts a double-roller meshing casting process to effectively solve the technical problem of high-efficiency impregnation of the low-viscosity polyimide resin solution, realizes the batch stable preparation of the polyimide prepreg and lays a good foundation for the engineering application and popularization.
Drawings
FIG. 1 is a schematic flow chart of the method of the present invention.
FIG. 2 is a schematic view of a twin roll kiss casting process.
Detailed Description
As shown in fig. 1, a method for preparing a high temperature resistant polyimide prepreg, the raw materials for preparing the high temperature resistant polyimide prepreg include a polyimide resin solution and a fiber reinforcement; the method comprises the following steps:
(1) putting the polyimide resin solution into a reaction kettle for vacuum filtration, and removing redundant solvent;
(2) placing the treated polyimide resin solution obtained in the step (1) in a glue solution tank, and uniformly coating the polyimide resin solution on release paper by adopting a tape casting process to form a polyimide resin glue film on the release paper;
(3) drawing the fiber reinforcement body above the polyimide resin adhesive film in the step (2) through set tension, and impregnating the polyimide resin adhesive film into the fiber reinforcement body through a compression roller;
(4) drying the product obtained in the step (3) at a set travelling speed and a set uniform speed through a drying tunnel under the traction of a set tension;
(5) placing the isolating film above the dried product in the step (4) under the action of set tension, and applying pressure by a compression roller to increase the attaching degree between the isolating film and the product;
(6) and (5) rolling the product in the step (5) by using a rolling device to obtain the prepreg.
In the step (1), the polyimide resin solution is a PMR type polyimide resin solution, and the initial solid content of the resin solution is 45-60 wt%;
in the step (1), the polyimide resin is subjected to vacuum filtration, the temperature during the filtration is 30-50 ℃, and the specific gravity of the resin solution after the filtration is 1.05-1.08;
as shown in fig. 2, in the step (2), a twin-roll casting process is adopted for the casting process, a device used in the twin-roll casting process comprises a glue solution tank, a gluing round roll and a traction round roll, glue solution is contained in the glue solution tank, a part of the gluing round roll is located in the glue solution tank, the gap between the traction round roll and the gluing round roll is 0.36-0.38 mm, and the traction round roll is used for driving release paper to move; the process of the twin-roll meshing casting technology is as follows: loading glue solution into a glue solution tank, then immersing a part of a gluing round roller into the glue solution, enabling release paper to pass through between the gluing round roller and a traction round roller under the action of set tension, starting the gluing round roller and the traction round roller to rotate, enabling polyimide resin solution on the surface of the gluing round roller to be uniformly coated on the surface of the gluing round roller when the gluing round roller rotates, and enabling the traction round roller to drive the release paper to pass through a gap between the gluing round roller and the release round roller under the traction action of the set tension to enable the polyimide resin solution on the surface of the gluing round roller to be uniformly coated on the release paper to form a polyimide resin adhesive film;
in the step (3), the fiber reinforcement is carbon fiber yarn, glass fiber yarn, quartz fiber yarn, carbon fiber fabric, glass fiber fabric or quartz fiber fabric;
in the step (3), the set tension is 240-260N, and the pressure of the compression roller is 0.05-0.1 MPa;
in the step (4), the drying temperature is 70-80 ℃, and the advancing speed is 2.0-3 m/min;
in the step (5), the set tension is 120-150N, and the pressure of the compression roller is 0.05-0.1 MPa;
in the step (6), the winding tension in winding is 150-170N.
In order to solve the technical problem of high-efficiency coating of a low-viscosity polyimide resin solution, resin solution vacuum filtration and a double-roller meshing casting impregnation process method are adopted, so that the coating efficiency and uniformity of a resin solution adhesive film are improved, meanwhile, the control of volatile matters and the spreading performance of the prepreg is realized by controlling the temperature of a drying tunnel and the advancing speed of the prepreg, the content of the volatile matters in the prepreg is reduced, the quality consistency of the prepreg is improved, and the control of the quality and the consistency of subsequent polyimide composite material products is facilitated.
The forming process flow of the invention is shown in figure 1 and comprises the following steps:
(1) resin solution pretreatment
And (2) placing the PMR type polyimide resin solution into a reaction kettle by adopting a vacuum filtration mode, carrying out vacuum filtration at the temperature of between 30 and 50 ℃, removing redundant solvent, and controlling the specific gravity of the final resin solution to be between 1.05 and 1.08, wherein the initial solid content of the resin solution is between 45 and 60 percent by weight.
(2) Resin glue solution coating
Pouring the pumped and filtered resin glue solution into a glue solution tank, uniformly coating the resin solution in the glue solution tank on release paper by adopting a double-roller meshing casting process, and controlling the gap between double rollers within the range of 0.36-0.38 mm.
(3) Impregnation with prepreg
Drawing a reinforcement body above the resin adhesive liquid film through tension of 240-260N, and applying pressure of 0.05-0.1 MPa through a compression roller to realize impregnation, wherein the reinforcement body is carbon fiber, glass fiber, quartz fiber yarn or fabric thereof;
(4) drying prepreg
And (3) drying the impregnated prepreg through a drying tunnel under the traction of 240-260N tension, wherein the drying temperature is 70-80 ℃, and the advancing speed is 2.0-3 m/min.
(5) Prepreg surface coating film
Placing an isolation film above the prepreg under the action of 120-150N tension, and applying pressure of 0.05-0.1 MPa through a compression roller to increase the bonding degree between the isolation film and the prepreg;
(6) prepreg winding
And winding the prepreg by using a winding device, wherein the winding tension is 150-170N.
The present invention will be described in further detail with reference to the following examples.
Example 1
The prepreg is prepared by adopting unidirectional carbon fiber reinforced PMR type 906 resin, firstly, 906 polyimide resin solution with the solid content of 50 wt% is placed in a reaction kettle, the temperature of the reaction kettle is set to be 40 ℃, after vacuum filtration is carried out until the specific gravity of the resin solution is 1.07, resin glue solution is taken out and poured into a glue solution tank, the resin solution in the glue solution tank is uniformly coated on release paper by adopting a double-roller meshing casting process, and the gap between the double rollers is adjusted to be 0.37 mm. The method comprises the steps of drawing arranged carbon fiber tows to the position above a resin adhesive film under the tension action of 260N, applying pressure of 0.05MPa through a compression roller to realize impregnation, drying the prepreg at a constant speed of 2.5m/min through a drying tunnel with the temperature set to 70 ℃, removing redundant solvent, laminating the surface of the prepreg after passing through the drying tunnel, drawing a surface isolation film to the position above the prepreg under the tension action of 150N, applying pressure of 0.05MPa through the compression roller to increase the bonding degree between the isolation film and the prepreg, and rolling the prepreg by a rolling device under the tension action of 150N to obtain the flat and wrinkle-free prepreg surface. Sampling 10 different areas of the obtained prepreg to test the resin content, the fiber surface density and the volatile content of the prepreg, wherein the resin content is 32-37%, and the fiber surface density is 162-167 g/m2And the content of volatile components is 8.5-10.1%. The prepared prepreg is used for preparing the polyimide composite material, and the porosity of the composite material is tested according to GB/T3365-2008, wherein the porosity is 0.02%.
Example 2
The prepreg is prepared by adopting unidirectional carbon fiber reinforced PMR type 906 resin, firstly, 906 polyimide resin solution with the solid content of 50 wt% is placed in a reaction kettle, the temperature of the reaction kettle is set to be 30 ℃, after vacuum filtration is carried out until the specific gravity of the resin solution is 1.05, resin glue solution is taken out and poured into a glue solution tank, the resin solution in the glue solution tank is uniformly coated on release paper by adopting a double-roller meshing casting process, and the gap between the double rollers is adjusted to be 0.38 mm. Drawing the arranged carbon fiber tows above a resin adhesive liquid film under the action of 260N tension, applying 0.05MPa pressure through a compression roller to realize impregnation, then drying the prepreg at a uniform speed of 2m/min through a drying channel with the temperature set to 70 ℃, removing redundant solvent, and passing through a drying channelAfter the drying tunnel, the surface of the prepreg is covered with a film, a surface isolation film is pulled to the upper part of the prepreg under the action of 150N tension, 0.05MPa pressure is applied through a compression roller, the attaching degree between the isolation film and the prepreg is increased, the prepreg is wound by a winding device under the action of 150N tension, and the prepared prepreg is smooth in surface and free of wrinkles. Sampling 10 different areas of the obtained prepreg to test the resin content, the fiber surface density and the volatile content of the prepreg, wherein the resin content is 31-36%, and the fiber surface density is 160.8-166.7 g/m2The content of volatile components is 10.5-11.7%. The prepared prepreg is used for preparing the polyimide composite material, and the porosity of the composite material is tested according to GB/T3365-2008, wherein the porosity is 0.06%.
Example 3
The prepreg is prepared by adopting unidirectional carbon fiber reinforced PMR type 906 resin, firstly, 906 polyimide resin solution with solid content of 45 wt% is placed in a reaction kettle, the temperature of the reaction kettle is set to be 50 ℃, after vacuum filtration is carried out until the specific gravity of the resin solution is 1.05, resin glue solution is taken out and poured into a glue solution tank, the resin solution in the glue solution tank is uniformly coated on release paper by adopting a double-roller meshing casting process, and the gap between the double rollers is adjusted to be 0.38 mm. The method comprises the steps of drawing arranged carbon fiber tows to the position above a resin adhesive film under the action of 260N tension, applying 0.05MPa pressure to the prepreg through a compression roller to achieve impregnation, then drying the prepreg at a constant speed of 2m/min through a drying tunnel with the temperature set to 70 ℃, removing redundant solvent, laminating the surface of the prepreg after passing through the drying tunnel, drawing a surface isolation film to the position above the prepreg under the action of 150N tension, applying 0.05MPa pressure through the compression roller to increase the bonding degree between the isolation film and the prepreg, and rolling the prepreg by a rolling device under the action of 150N tension to obtain the flat and wrinkle-free prepreg surface. Sampling 10 different areas of the obtained prepreg to test the resin content, the fiber surface density and the volatile content of the prepreg, wherein the resin content is 32-36%, and the fiber surface density is 162.4-167.1 g/m2The content of volatile components is 9.8-11.1%. The prepared prepreg is used for preparing the polyimide composite material, and the porosity of the composite material is tested according to GB/T3365-2008, wherein the porosity is 0.05%.
Example 4
The prepreg is prepared by adopting unidirectional carbon fiber reinforced PMR type 906 resin, firstly, 906 polyimide resin solution with the solid content of 60 wt% is placed in a reaction kettle, the temperature of the reaction kettle is set to be 40 ℃, after vacuum filtration is carried out until the specific gravity of the resin solution is 1.08, resin glue solution is taken out and poured into a glue solution tank, the resin solution in the glue solution tank is uniformly coated on release paper by adopting a double-roller meshing casting process, and the gap between the double rollers is adjusted to be 0.36 mm. The method comprises the steps of drawing arranged carbon fiber tows to the position above a resin adhesive film under the action of 260N tension, applying 0.05MPa pressure to the prepreg through a compression roller to achieve impregnation, then drying the prepreg at a constant speed of 3m/min through a drying tunnel with the temperature set to 70 ℃, removing redundant solvent, laminating the surface of the prepreg after passing through the drying tunnel, drawing a surface isolation film to the position above the prepreg under the action of 150N tension, applying 0.05MPa pressure through the compression roller to increase the bonding degree between the isolation film and the prepreg, and rolling the prepreg by a rolling device under the action of 150N tension to obtain the flat and wrinkle-free prepreg surface. Sampling 10 different areas of the obtained prepreg to test the resin content, the fiber surface density and the volatile content of the prepreg, wherein the resin content is 33-37%, and the fiber surface density is 161.4-165.8 g/m2And the content of volatile components is 8.8-10.1%. The prepared prepreg is used for preparing the polyimide composite material, the porosity of the composite material is tested according to GB/T3365-2008, and no pore is detected.
Example 5
The prepreg is prepared by adopting unidirectional carbon fiber reinforced PMR type 906 resin, firstly, 906 polyimide resin solution with the solid content of 50 wt% is placed in a reaction kettle, the temperature of the reaction kettle is set to be 40 ℃, after vacuum filtration is carried out until the specific gravity of the resin solution is 1.07, resin glue solution is taken out and poured into a glue solution tank, the resin solution in the glue solution tank is uniformly coated on release paper by adopting a double-roller meshing casting process, and the gap between the double rollers is adjusted to be 0.38 mm. Drawing the carbon fiber fabric above the resin adhesive liquid film under the tension of 240N, applying 0.1MPa pressure by a compression roller to realize impregnation, and then drying the prepreg at a uniform speed of 2m/min through a drying tunnel with the temperature set at 75 ℃ to remove muchResidual solvent is coated on the surface of the prepreg after passing through the drying tunnel, the surface isolation film is pulled above the prepreg under the action of 120N tension, 0.1MPa pressure is applied through the compression roller, the attaching degree between the isolation film and the prepreg is increased, the prepreg is wound by the winding device under the action of 170N tension, and the prepared prepreg is smooth in surface and free of wrinkles. Sampling 10 different areas of the obtained prepreg to test the resin content, the fiber surface density and the volatile content of the prepreg, wherein the resin content is 33-37%, and the fiber surface density is 270-278 g/m2And the content of volatile components is 7.8-9.2%. The prepared prepreg is used for preparing the polyimide composite material, the porosity of the composite material is tested according to GB/T3365-2008, and no pore is detected.
Example 6
The prepreg is prepared by adopting unidirectional carbon fiber reinforced PMR type 906 resin, firstly, 906 polyimide resin solution with the solid content of 50 wt% is placed in a reaction kettle, the temperature of the reaction kettle is set to be 40 ℃, after vacuum filtration is carried out until the specific gravity of the resin solution is 1.07, resin glue solution is taken out and poured into a glue solution tank, the resin solution in the glue solution tank is uniformly coated on release paper by adopting a double-roller meshing casting process, and the gap between the double rollers is adjusted to be 0.38 mm. The method comprises the steps of drawing a glass fiber fabric to the position above a resin adhesive liquid film under the tension of 250N, applying pressure of 0.1MPa by a compression roller to realize impregnation, then drying the prepreg at a constant speed of 3m/min through a drying tunnel with the temperature set at 80 ℃, removing redundant solvent, laminating the surface of the prepreg after passing through the drying tunnel, drawing a surface isolation film to the position above the prepreg under the tension of 130N, applying pressure of 0.1MPa by the compression roller to increase the bonding degree between the isolation film and the prepreg, and rolling the prepreg by a rolling device under the tension of 160N to obtain the flat and wrinkle-free prepreg surface. Sampling 10 different areas of the obtained prepreg to test the resin content, the fiber surface density and the volatile content of the prepreg, wherein the resin content is 30-35%, and the fiber surface density is 215.4-221.6 g/m2The content of volatile components is 6.8-8.1%. The prepared prepreg is used for preparing the polyimide composite material, the porosity of the composite material is tested according to GB/T3365-2008, and no pore is detected.
Example 7
The prepreg is prepared by adopting unidirectional carbon fiber reinforced PMR type 906 resin, firstly, 906 polyimide resin solution with the solid content of 50 wt% is placed in a reaction kettle, the temperature of the reaction kettle is set to be 40 ℃, after vacuum filtration is carried out until the specific gravity of the resin solution is 1.07, resin glue solution is taken out and poured into a glue solution tank, the resin solution in the glue solution tank is uniformly coated on release paper by adopting a double-roller meshing casting process, and the gap between the double rollers is adjusted to be 0.38 mm. The method comprises the steps of drawing a quartz fiber fabric to the position above a resin adhesive liquid film under the tension of 250N, applying pressure of 0.1MPa through a compression roller to realize impregnation, then drying the prepreg at a constant speed of 3m/min through a drying tunnel with the temperature set at 80 ℃, removing redundant solvent, laminating the surface of the prepreg after passing through the drying tunnel, drawing a surface isolation film to the position above the prepreg under the tension of 130N, applying pressure of 0.1MPa through the compression roller to increase the bonding degree between the isolation film and the prepreg, and rolling the prepreg by using a rolling device under the tension of 160N to obtain the flat and wrinkle-free prepreg surface. The obtained prepreg was tested for resin content, fiber areal density and volatile content, the resin content was 34.1%, and the fiber areal density was 219.2g/m2The volatile content was 8.2%. Sampling 10 different areas of the obtained prepreg to test the resin content, the fiber surface density and the volatile content of the prepreg, wherein the resin content is 32-36%, and the fiber surface density is 216.3-223.1 g/m2The content of volatile components is 9.7-11.2%. The prepared prepreg is used for preparing the polyimide composite material, and the porosity of the composite material is tested according to GB/T3365-2008, wherein the porosity is 0.02%.
The invention is not described in detail and is within the knowledge of a person skilled in the art.
Claims (6)
1. A preparation method of polyimide prepreg is characterized by comprising the following steps: the raw materials for preparing the polyimide prepreg comprise a polyimide resin solution and a fiber reinforcement; the method comprises the following steps:
(1) putting the polyimide resin solution into a reaction kettle for vacuum filtration;
(2) placing the polyimide resin solution obtained in the step (1) in a glue solution tank, and forming a polyimide resin glue film on release paper by adopting a tape casting process;
(3) drawing the fiber reinforcement body above the polyimide resin adhesive film in the step (2), and impregnating the polyimide resin adhesive film into the fiber reinforcement body;
(4) drying the product obtained in the step (3);
(5) placing an isolation film above the dried product in the step (4);
(6) winding the product in the step (5) by using a winding device to obtain a prepreg;
in the step (1), the polyimide resin solution is a PMR type polyimide resin solution, and the initial solid content of the resin solution is 45-60 wt%; performing vacuum filtration on the polyimide resin, wherein the temperature during the filtration is 30-50 ℃, and the specific gravity of the resin solution after the filtration is 1.05-1.08;
in the step (2), a double-roller meshing casting process is adopted as a casting process;
the device used by the double-roller meshing casting process comprises a glue solution tank, a gluing round roller and a traction round roller, wherein the glue solution tank is used for containing polyimide resin solution;
one part of the gluing round roller is positioned in the polyimide resin solution in the gluing tank;
the gap between the traction round roller and the gluing round roller is 0.36-0.38 mm;
the traction round roller is used for driving the release paper to move from a gap between the gluing round roller and the traction round roller under the traction action of set tension;
the method of the twin-roll meshing casting process comprises the following steps: placing polyimide resin solution in a glue solution tank, then immersing a part of a gluing round roller into the polyimide resin solution, enabling release paper to pass through a gap between the gluing round roller and a traction round roller under the set tension traction effect, starting the gluing round roller and the traction round roller to rotate, enabling the polyimide resin solution on the surface of the gluing round roller to be uniformly coated when the gluing round roller rotates, and enabling the traction round roller to drive the release paper to pass through the gap between the gluing round roller and the release round roller under the set tension traction effect to form a polyimide resin adhesive film on the release paper.
2. The method for producing a polyimide prepreg according to claim 1, characterized in that: in the step (3), the fiber reinforcement is one or a mixture of more than two of carbon fiber yarn, glass fiber yarn, quartz fiber yarn, carbon fiber fabric, glass fiber fabric and quartz fiber fabric.
3. The method for producing a polyimide prepreg according to claim 1, characterized in that: in the step (3), the fiber reinforcement is drawn above the polyimide resin adhesive film in the step (2) through a set tension, and the polyimide resin adhesive film is impregnated into the fiber reinforcement through a compression roller; the set tension is 240-260N, and the pressure of the compression roller is 0.05-0.1 MPa.
4. The method for producing a polyimide prepreg according to claim 1, characterized in that: in the step (4), the product obtained in the step (3) is dried by passing through a drying tunnel at a constant speed at a set advancing speed under the traction of a set tension; the drying temperature is 70-80 ℃, and the advancing speed is 2.0-3 m/min.
5. The method for producing a polyimide prepreg according to claim 1, characterized in that: in the step (5), the isolating film is placed above the dried product in the step (4) under the action of set tension, and pressure is applied through a compression roller to increase the attaching degree between the isolating film and the product; the set tension is 120-150N, and the compression roller pressure is 0.05-0.1 MPa.
6. The method for producing a polyimide prepreg according to claim 1, characterized in that: in the step (6), the winding tension in winding is 150-170N.
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| US5078934A (en) * | 1988-03-29 | 1992-01-07 | Nippon Shokubai Kagaku Kogyo Co., Ltd. | Method for production of fiber-reinforced thermosetting resin molding material |
| CN1339536A (en) * | 2000-08-22 | 2002-03-13 | 上海市合成树脂研究所 | Short-cut fiber reinforced moleded polyimide plastic and its preparing method |
| CN102503182A (en) * | 2011-11-08 | 2012-06-20 | 大连橡胶塑料机械股份有限公司 | Online gluing production line for carbon (glass) fibers |
| CN105882077A (en) * | 2016-04-27 | 2016-08-24 | 航天材料及工艺研究所 | Method using coating technology to prepare solution-method phenolic aldehyde prepreg |
| CN106273143A (en) * | 2016-09-22 | 2017-01-04 | 青岛理工大学 | The manufacturing system of a kind of embedded co-curing composite damping thin film and method |
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| US5078934A (en) * | 1988-03-29 | 1992-01-07 | Nippon Shokubai Kagaku Kogyo Co., Ltd. | Method for production of fiber-reinforced thermosetting resin molding material |
| CN1339536A (en) * | 2000-08-22 | 2002-03-13 | 上海市合成树脂研究所 | Short-cut fiber reinforced moleded polyimide plastic and its preparing method |
| CN102503182A (en) * | 2011-11-08 | 2012-06-20 | 大连橡胶塑料机械股份有限公司 | Online gluing production line for carbon (glass) fibers |
| CN105882077A (en) * | 2016-04-27 | 2016-08-24 | 航天材料及工艺研究所 | Method using coating technology to prepare solution-method phenolic aldehyde prepreg |
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