CN109134900B - Prepreg and preparation method thereof - Google Patents
Prepreg and preparation method thereof Download PDFInfo
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- CN109134900B CN109134900B CN201710500186.0A CN201710500186A CN109134900B CN 109134900 B CN109134900 B CN 109134900B CN 201710500186 A CN201710500186 A CN 201710500186A CN 109134900 B CN109134900 B CN 109134900B
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- resin
- film
- prepreg
- coating
- steel roller
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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
- B29B15/00—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
- B29B15/08—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
- B29B15/10—Coating or impregnating independently of the moulding or shaping step
- B29B15/12—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length
- B29B15/122—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length with a matrix in liquid form, e.g. as melt, solution or latex
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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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- 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
- B29B11/00—Making preforms
- B29B11/14—Making preforms characterised by structure or composition
- B29B11/16—Making preforms characterised by structure or composition comprising fillers or reinforcement
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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
- C08J2363/00—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
- 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
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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
-
- 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
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Reinforced Plastic Materials (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention provides a prepreg and a preparation method thereof, wherein the prepreg comprises the following steps: preparing a film coating steel roller; heating the resin, and coating the heated resin on a film coating steel roller to prepare a film; and impregnating the adhesive film and the fiber fabric or yarn to obtain the prepreg. The prepreg prepared by the method has low porosity and simple preparation process, greatly reduces the production cost and improves the production efficiency of the prepreg.
Description
Technical Field
The invention relates to the field of materials, in particular to a prepreg and a preparation method thereof.
Background
During prepreg manufacturing, at lower forming pressures, porosity is often too high during curing due to poor air conduction between layers. At present, the common method is to control the pressure to immerse the resin adhesive film into a part of the dry fiber layer and realize the air guide function through the part which is not immersed, but in the method, the adjustment of the pressure is related to the state of the resin, the requirements on the state of the resin and the precision of equipment are high, the process is difficult to control, the porosity of the prepared prepreg is high, and a product with uniform infiltration is difficult to obtain.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a prepreg, which realizes air guide by controlling the width and height of a micro strip protruding on a film coating steel roller and the viscosity of resin and by using a method of patterning the film coating steel roller, prepares an adhesive film with regularly changed surface density in a micro area range, and further improves the uniformity of the adhesive film by using a spin coating process; and then, air guide can be further realized through the raised micro-strips during impregnation by controlling the viscosity of the adhesive film, so that the adhesive film can complete the preparation of the prepreg with high air guide under low forming pressure, and the prepared prepreg has low porosity.
The invention provides a method for preparing a prepreg, which comprises the following steps:
preparing a film coating steel roller; heating the resin, and coating the heated resin on a film coating steel roller to prepare a film; and impregnating the adhesive film and the fiber fabric or yarn to obtain the prepreg.
In the above method, the coated steel roll is made of a film and a steel roll.
In the above method, the film includes one or both of a polyethylene film and a polyimide film.
In the above method, the coated steel roll has raised micro-strips.
In the method, the width of the raised micro-strip is 1-100 microns.
In the method, the height of the raised micro-strip is 1-50 microns.
In the method, the resin is heated, and the viscosity of the resin is controlled to be 8000-20000 centipoises.
In the above method, after the heated resin is coated on the coated steel roll, the coated steel roll is patterned.
In the above method, the heated resin is coated on the coated steel roll by a spin coating process.
In the method, when the adhesive film and the fiber fabric or the yarn are impregnated, the viscosity of the adhesive film is controlled to be 4000-10000 centipoises.
In the above method, the resin includes one or more of a bismaleimide resin, a cyanate ester resin, and an epoxy resin.
In the above method, the fiber fabric comprises one or more of basalt fiber, aramid fabric, quartz fabric, and glass fabric.
The invention also provides a prepreg prepared according to the method.
The prepreg prepared by the method realizes high air guide of the prepreg during low-pressure forming, so that the porosity of the prepared prepreg is reduced, and the quality of the prepared prepreg is improved; the method is simple and easy to implement, and the manufacturing cost is greatly reduced while the efficiency is improved.
Drawings
FIG. 1 is a schematic representation of the prepared glue film (1-steel roller; 2-raised micro-strip; 3-glue film; 4-micro-groove).
Detailed Description
The following examples will allow one skilled in the art to more fully understand the present invention, but do not limit the invention in any way.
The film coating steel roller is prepared by coating a polyethylene film and/or a polyimide film on a steel roller, and is provided with a raised micro-strip, wherein the width of the raised micro-strip is 1-100 micrometers, and the height of the raised micro-strip is 1-50 micrometers;
heating the resin, controlling the viscosity of the resin to be 8000-20000 centipoises (including end points), and coating the heated resin on a coating steel roller by adopting a spin coating process to prepare a glue film; wherein, the resin can be one or more of bismaleimide resin, cyanate resin and epoxy resin; and
impregnating the adhesive film and the fiber fabric or yarn, and controlling the viscosity of the adhesive film to be 4000-10000 centipoises (inclusive) to prepare a prepreg; wherein the fiber fabric is selected from one or more of basalt fiber, aramid fabric, quartz fabric and glass fiber fabric.
Example 1
Coating a polyethylene film on a steel roller to form a film-coated steel roller with raised micro-strips, wherein the raised micro-strips have a width of 50 microns and a height of 50 microns;
then, heating the bismaleimide resin until the viscosity of the bismaleimide resin is 10000 centipoises, and coating the heated resin on a coating steel roller by adopting a spin coating process to prepare a coating film; and
impregnating the adhesive film and the yarns, and controlling the viscosity of the adhesive film to be 8000 centipoises to prepare a prepreg; the results of the porosity measurements of the prepregs are shown in table 1 below.
Example 2
Coating a polyethylene film on a steel roller to form a coated steel roller having raised micro-strips, the raised micro-strips having a width of 20 microns and a height of 30 microns;
then, heating the bismaleimide resin until the viscosity of the bismaleimide resin is 8000 centipoise, and coating the heated resin on a coating steel roller by adopting a spin coating process to prepare a coating film; and
impregnating the adhesive film and the glass fiber cloth, and controlling the viscosity of the adhesive film to be 6000 centipoise to prepare a prepreg; the results of the porosity measurements of the prepregs are shown in table 1 below.
Example 3
Coating a polyethylene film on a steel roller to form a coated steel roller having raised micro-strips, the raised micro-strips having a width of 70 microns and a height of 20 microns;
then, heating the bismaleimide resin until the viscosity of the bismaleimide resin is 12000 centipoises, and coating the heated resin on a coating steel roller by adopting a spin coating process to prepare a coating film; and
impregnating the adhesive film and the yarns, and controlling the viscosity of the adhesive film to be 4000 centipoises to prepare a prepreg; the results of the porosity measurements of the prepregs are shown in table 1 below.
Example 4
Coating a polyethylene film on a steel roller to prepare a film-coated steel roller with a raised micro-strip, wherein the raised micro-strip has the width of 1 micrometer and the height of 1 micrometer;
then, heating the bismaleimide resin until the viscosity of the bismaleimide resin is 16000 centipoises, and coating the heated resin on a coating steel roller by adopting a spin coating process to prepare a glue film; and
impregnating the adhesive film and aramid cloth, and controlling the viscosity of the adhesive film to be 10000 centipoises to prepare prepreg; the results of the porosity measurements of the prepregs are shown in table 1 below.
Example 5
Coating a polyethylene film on a steel roller to form a coated steel roller having raised micro-strips, the raised micro-strips having a width of 100 microns and a height of 50 microns;
then, heating the epoxy resin until the viscosity of the epoxy resin is 20000 centipoises, and coating the heated resin on a coating steel roller by adopting a spin coating process to prepare a glue film; and
impregnating the glue film and basalt fibers, and controlling the viscosity of the glue film to be 8000 centipoises to prepare a prepreg; the results of the porosity measurements of the prepregs are shown in table 1 below.
Example 6
Coating a polyethylene film on a steel roller to form a coated steel roller having raised micro-strips, the raised micro-strips having a width of 50 microns and a height of 40 microns;
then, heating the cyanate ester resin until the viscosity of the cyanate ester resin is 15000 centipoises, and coating the heated resin on a coating steel roller by adopting a spin coating process to prepare a glue film; and
impregnating the adhesive film and quartz cloth, and controlling the viscosity of the adhesive film to be 5000 centipoises to prepare a prepreg; the results of the porosity measurements of the prepregs are shown in table 1 below.
The porosities of the prepregs of examples 1 to 6 were determined using the relevant standards and the results of the measurements are shown in table 1 below:
TABLE 1
As can be seen from table 1, the method of the present invention controls the width and height of the micro-strips protruding from the coated steel roller and the viscosity of the resin, and uses the patterned coated steel roller to conduct air guide, so as to form an adhesive film with regularly changing surface density in the micro-area range, and further conduct air guide through the protruding micro-strips when the adhesive film with a certain viscosity is impregnated with the fiber fabric or yarn, and the prepreg prepared by the method of the present invention has a porosity of less than 1.1%.
In addition, in the invention, the performance required by the final product can be realized only by combining equipment and a simple process, so that the production cost is greatly reduced, the production efficiency of the prepreg is improved, and the large-scale production of the prepreg is facilitated.
Those skilled in the art will appreciate that the above embodiments are merely exemplary embodiments and that various changes, substitutions, and alterations can be made without departing from the spirit and scope of the invention.
Claims (10)
1. A method of making a prepreg comprising the steps of:
preparing a film coating steel roller;
heating the resin, and coating the heated resin on the coating steel roller to prepare a glue film; and
impregnating the adhesive film and a fiber fabric or yarn to obtain the prepreg,
the coating steel roller is provided with a protruding micro strip, the width of the protruding micro strip is 1-100 micrometers, and the height of the protruding micro strip is 1-50 micrometers.
2. The method of claim 1, wherein the coated steel roll is made of a film and a steel roll.
3. The method of claim 2, wherein the film comprises one or both of a polyethylene film and a polyimide film.
4. The method according to claim 1, wherein the resin is heated, and the viscosity of the resin is controlled to be 8000 to 20000 cps.
5. The method of claim 1, wherein the coated steel roll is patterned after the heated resin is coated on the coated steel roll.
6. The method of claim 1, wherein the heated resin is applied to the coated steel roll using a spin coating process.
7. The method according to claim 1, wherein the adhesive film is impregnated into the fiber fabric or the yarn, and the adhesive film has a viscosity of 4000 to 10000 cps.
8. The method of claim 1, wherein the resin comprises one or more of a bismaleimide resin, a cyanate resin, and an epoxy resin.
9. The method of claim 1, wherein the fiber fabric comprises one or more of basalt fiber, aramid fabric, quartz fabric, and fiberglass fabric.
10. A prepreg made according to the method of any one of claims 1-9.
Priority Applications (1)
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CN201710500186.0A CN109134900B (en) | 2017-06-27 | 2017-06-27 | Prepreg and preparation method thereof |
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CN201710500186.0A CN109134900B (en) | 2017-06-27 | 2017-06-27 | Prepreg and preparation method thereof |
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CN109134900B true CN109134900B (en) | 2022-06-07 |
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CN111057369A (en) * | 2019-12-12 | 2020-04-24 | 会通新材料股份有限公司 | Carbon fiber reinforced polyamide composite material pre-soaked basalt fiber cloth and preparation method thereof |
CN115181308A (en) * | 2022-07-12 | 2022-10-14 | 中航复合材料有限责任公司 | Preparation method of prepreg suitable for molding unidirectional tape outside tank |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5104718A (en) * | 1989-02-28 | 1992-04-14 | Mitsubishi Rayon Co., Ltd. | Prepreg and process for producing the same |
CN103429371A (en) * | 2011-03-30 | 2013-12-04 | 东丽株式会社 | Prepreg, fiber reinforced composite material, and manufacturing method for fiber reinforced composite material |
CN104647636A (en) * | 2015-01-16 | 2015-05-27 | 中国航空工业集团公司基础技术研究院 | Preparation method of gradient prepreg with air guiding passage in layer |
CN106273060A (en) * | 2016-08-09 | 2017-01-04 | 陕西天策新材料科技有限公司 | A kind of wide cut thermoplasticity prepreg preparation method and preparation hot-pressing roller thereof |
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2017
- 2017-06-27 CN CN201710500186.0A patent/CN109134900B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5104718A (en) * | 1989-02-28 | 1992-04-14 | Mitsubishi Rayon Co., Ltd. | Prepreg and process for producing the same |
CN103429371A (en) * | 2011-03-30 | 2013-12-04 | 东丽株式会社 | Prepreg, fiber reinforced composite material, and manufacturing method for fiber reinforced composite material |
CN104647636A (en) * | 2015-01-16 | 2015-05-27 | 中国航空工业集团公司基础技术研究院 | Preparation method of gradient prepreg with air guiding passage in layer |
CN106273060A (en) * | 2016-08-09 | 2017-01-04 | 陕西天策新材料科技有限公司 | A kind of wide cut thermoplasticity prepreg preparation method and preparation hot-pressing roller thereof |
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