CN111518300B - Preparation process of carbon fiber prepreg - Google Patents

Preparation process of carbon fiber prepreg Download PDF

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Publication number
CN111518300B
CN111518300B CN202010411648.3A CN202010411648A CN111518300B CN 111518300 B CN111518300 B CN 111518300B CN 202010411648 A CN202010411648 A CN 202010411648A CN 111518300 B CN111518300 B CN 111518300B
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carbon fiber
conductive powder
prepreg
pan
resin
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CN111518300A (en
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吴海宏
郭正民
杨向涛
蒋爱云
黄明
周应国
张洛明
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Zhengzhou Fanxian New Material Technology Co ltd
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Zhengzhou Fanxian New Material Technology Co ltd
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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
    • 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
    • C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
    • C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
    • C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
    • 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
    • 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
    • C08J2363/10—Epoxy resins modified by unsaturated compounds
    • 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
    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/06—Unsaturated polyesters
    • 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
    • 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
    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances

Abstract

The invention provides a preparation process of carbon fiber prepreg, which comprises the following steps: (1) Spreading the precursor carbon fiber to a certain width through a spreading device; (2) Adsorbing conductive powder on the carbon fiber dry belt after being spread by an electrostatic spraying method; (3) And compounding the carbon fiber attached with the conductive powder with resin to form a carbon fiber prepreg. The prepreg prepared by the process has the characteristics of high strength, small density, good plasticity, good formability, long service life and the like, and meanwhile, the conductive powder is attached to the surface, so that the Z-axis conductivity is enhanced, and the conductivity of the carbon fiber prepreg is integrally improved.

Description

Preparation process of carbon fiber prepreg
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a preparation process of carbon fiber prepreg.
Background
The carbon fiber is a microcrystalline graphite material obtained by carbonizing and graphitizing an organic fiber. The carbon fiber is a new material with excellent mechanical property, the specific gravity of the material is less than 1/4 of that of steel, and the tensile strength of the carbon fiber resin composite material is generally more than 3500Mpa and 7-9 times of that of steel. Meanwhile, the composite material has excellent conductivity, chemical inertness, corrosion resistance, high temperature resistance and the like, and is widely applied to the fields of civil use, military use, construction, chemical industry and aerospace, and the demand is increased year by year.
The carbon fiber prepreg is a semi-finished product prepared by compounding carbon fibers or fabrics with a resin matrix, and is a main intermediate material for manufacturing a composite structural member. At present, the carbon fiber prepreg has fast application development, is mostly produced by specialized factories, and has a large number of shaping products for users to select, so that the market and application fields can be further widened by improving the overall performance of the carbon fiber prepreg.
Disclosure of Invention
The invention aims to provide a preparation process of carbon fiber prepreg, which has the characteristics of high strength, small density, good plasticity, good formability, long service life and the like, and conductive powder is attached to the surface of the prepreg, so that the Z-axis conductivity is enhanced, and the conductivity of the carbon fiber prepreg is integrally improved.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a preparation process of carbon fiber prepreg comprises the following steps:
(1) Spreading the precursor carbon fiber to a certain width through a spreading device;
(2) Adsorbing conductive powder on the carbon fiber dry belt after being spread by an electrostatic spraying method;
(3) And compounding the carbon fiber attached with the conductive powder with resin to form a carbon fiber prepreg.
Further, the precursor carbon fiber is a carbon fiber or a plurality of carbon fibers which are regularly or irregularly arranged. Model number 6k or 12k.
Further, the precursor carbon fibers are PAN-based carbon fibers and pitch-based carbon fibers, and preferably PAN-based carbon fibers.
Further, in the step (1), the width of the precursor carbon fiber is 15mm to 100mm.
In the step (2), the conductive powder is led to pass through the concentration area of the electrostatic generator by a fan, and then the powder is electrified and mutually separated and dispersed, so that the powder is adsorbed on the surface of the carbon fiber.
Further, in the step (2), the conductive powder is one of gold, silver, copper, tin, nickel, titanium, and carbon.
Further, in the step (2), the average diameter of the conductive powder is 1 to 150 μm.
Further, in the step (3), the compounding process of the carbon fiber and the resin to which the conductive powder is attached is dry compounding or wet compounding, preferably wet compounding, specifically: the carbon fiber bundles attached with the conductive powder are immersed in the resin solution at a certain speed, and then dried and cured.
Further, in the step (3), the resin is a thermosetting resin, and the solvent of the resin solution is one of benzene, alcohol and ketone.
In the step (3), the resin in the resin solution accounts for 30% -60% of the total mass of the resin solution.
Further, in the step (3), the speed of passing the carbon fiber bundles attached with the conductive powder through the resin solution is 0.1 to 0.5 m/s.
Further, in the step (3), the gram weight of the conductive powder is 1-3 g/cm 2 。
The carbon fiber prepreg prepared by the preparation process has good conductivity and the resistivity can be as low as 0.8x10 -3 Omega cm, can be used for preparing functional prepreg in the aspects of high-performance electromagnetic shielding, wave absorption stealth and lightning protection.
Compared with the prior art, the invention has the beneficial effects that:
1. in the preparation process, the conductive powder is attached to the surface of the carbon fiber through an external electromagnetic field, so that the conductive powder is arranged on the Z axis, and the conductivity of the carbon fiber prepreg can be enhanced; while increasing the area quality and thickness of the carbon fiber prepreg.
2. The carbon fiber prepreg prepared by the process has the characteristics of high strength, small density, good corrosion resistance, softness and plasticity, good processing consistency and long service life, and meanwhile, the conductive powder is attached to the surface, so that the Z-axis conductivity is enhanced, and the conductivity of the carbon fiber prepreg is integrally improved.
Drawings
FIG. 1 is a flow chart of a preparation process of the carbon fiber prepreg of the present invention;
in the figure, 1-fibril carbon fiber; 2-expanding the device; 3-a fan; 4-conductive powder; 5-electrostatic generator concentration zone; 6-resin solution; 7-baking oven; 8-release paper; 9-prepreg.
Detailed Description
The invention provides a preparation process of carbon fiber prepreg, which is shown in figure 1, and specifically comprises the following steps: the precursor carbon fiber 1 is subjected to expansion through rollers with different rotating speeds in the expansion equipment 2, conductive powder 4 is blown into a static generator concentration zone 5 through a fan 3, so that the powder is electrified and mutually exclusive and dispersed, and can be adsorbed on the surface of the carbon fiber for a long time, a carbon fiber bundle is immersed in a resin solution 6 at a certain speed, the fiber enters an oven 7 for drying, then release paper 8 is attached to the upper surface and the lower surface of the carbon fiber, and finally prepreg 9 is formed and wound.
The present invention will be described in further detail with reference to examples.
Example 1
The process adopts T700 PAN-based high-strength carbon fiber, expands to 60mm, adopts epoxy resin as resin, adopts acetone as solvent, and has a resin ratio of 40% in resin solution, a fiber forward traction speed of 0.3m/s, carbon fiber powder as conductive powder, and a gram weight of 1.5g/cm 2 The resistivity of the prepreg prepared by the process is 1.0x10 -3 Ω·cm~1.1x10 -3 Omega cm, which can be made into small energy storage elements of specific structure by a molding process.
Example 2
The process adopts T800 PAN-based high-strength carbon fiber, expands to 80mm, adopts polyimide resin as resin, adopts methyl pyrrolidone as solvent,the resin in the resin solution accounts for 40 percent, the forward traction speed of the fiber is 0.4m/s, the conductive powder adopts carbon fiber powder, and the gram weight is 1g/cm 2 The resistivity of the prepreg prepared by the process is 1.1x10 -3 Ω·cm~1.3x10 -3 Omega cm, and the conductive paper is prepared by laminating the omega cm and common paper, so that the electromagnetic shielding effect can be achieved.
Example 3
The process adopts M40J PAN-based high-strength high-modulus carbon fiber, expands to 60mm, adopts epoxy resin, adopts acetone as a solvent, and has a resin ratio of 40% in resin solution, a forward traction speed of 0.3M/s, carbon fiber powder as conductive powder and a gram weight of 1.5g/cm 2 The resistivity of the prepreg prepared by the process is 0.8x10 -3 Ω·cm~1.0x10 -3 Omega cm, can be made into the unmanned aerial vehicle fuselage through mould pressing technology to reach the stealthy effect of wave-absorbing.
Example 4
The process adopts M60J PAN-based high-strength high-modulus carbon fiber, expands to 80mm, adopts polyimide resin, adopts methyl pyrrolidone as a solvent, and adopts carbon fiber powder with the weight of 1g/cm, wherein the resin ratio in a resin solution is 40%, the forward traction speed of the fiber is 0.4M/s, and the conductive powder is carbon fiber powder 2 The resistivity of the prepreg prepared by the process is 1.1x10 -3 Ω·cm~1.2x10 -3 Omega cm, and making the material into a ship body structure so as to achieve the effects of low radar signals and magnetic field signals and electromagnetic wave absorption.
Example 5
Unlike examples 1-4, T300, T1000, M55J PAN-based carbon fibers, other pitch-based carbon fibers, and the like can also be used in the present process.
Example 6
In contrast to examples 1-4, thermosetting resins such as unsaturated polyesters, vinyl esters, phenolic aldehyde, bismaleimides, and the like may also be used in the present process.
Example 7
Unlike examples 1 to 4, alcohols and benzenes can also be used as the resin solution solvent in the present process.
Example 8
Unlike examples 1-4, the conductive particles in the present process may also be gold, silver, copper, tin, nickel, titanium, or other metal particles.
Example 9
Unlike examples 1-4, the fiber spread width, the resin ratio in the resin solution, the gram weight of the conductive powder, and the fiber draw speed in the present process can all be modified in accordance with the scope of the appended claims.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (1)

1. The process for improving the conductivity of the carbon fiber prepreg is characterized in that conductive powder is attached to the surface of the carbon fiber prepreg, so that the Z-axis conductivity is enhanced, and the conductivity of the carbon fiber prepreg is integrally improved, and the process specifically comprises the following steps:
(1) Spreading the precursor carbon fiber to a certain width through a spreading device;
(2) Adsorbing conductive powder on the spread carbon fiber dry belt by an electrostatic spraying method, specifically blowing the conductive powder into a concentration area of an electrostatic generator by a fan through the spread carbon fiber, so that the powder is electrified, mutually exclusive and dispersed, and adsorbed on the surface of the carbon fiber for a long time;
(3) Impregnating carbon fibers attached with conductive powder into a resin solution at a certain speed, drying the fibers in an oven, attaching release paper to the upper and lower surfaces of the carbon fibers, and finally forming prepreg and winding;
the precursor carbon fiber is one of a T700 PAN-based high-strength carbon fiber, a T800 PAN-based high-strength carbon fiber, an M40J PAN-based high-strength high-modulus carbon fiber, an M60J PAN-based high-strength high-modulus carbon fiber, a T300 PAN-based carbon fiber, a T1000 PAN-based carbon fiber, an M55J PAN-based carbon fiber and an asphalt-based carbon fiber;
in the step (1), the width of the precursor carbon fiber is 15 mm-100 mm;
in the step (2), the conductive powder is one of gold, silver, copper, tin, nickel, titanium and carbon;
in the step (2), the average diameter of the conductive powder is 1-150 mu m;
in the step (3), the resin is thermosetting resin, and the solvent of the resin solution is one of benzene, alcohol and ketone;
in the step (3), the resin in the resin solution accounts for 30% -60% of the total mass of the resin solution;
in the step (3), the speed of the carbon fiber bundles attached with the conductive powder passing through the resin solution is 0.1-0.5 m/s;
in the step (3), the gram weight of the conductive powder is 1-3 g/cm 2 ；
The resistivity of the carbon fiber prepreg prepared by the process is as low as 0.8x10 -3 Omega cm, is used for preparing functional prepreg with high electromagnetic shielding, wave absorption stealth and lightning protection.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102838766A (en) * 2006-08-07 2012-12-26 东丽株式会社 Prepreg and carbon fiber-reinforced composite material
CN103554530A (en) * 2013-10-11 2014-02-05 中国航空工业集团公司北京航空材料研究院 Electric conductive continuous fiber-reinforced fabric or prepreg and electric conductive treatment method
CN103724813A (en) * 2012-10-16 2014-04-16 辽宁辽杰科技有限公司 Continuous-fiber-reinforced thermoplastic flame-retardant antistatic composite material and preparation method thereof
CN106317772A (en) * 2015-07-10 2017-01-11 深圳光启高等理工研究院 Antistatic composite material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
US9481145B2 (en) * 2011-03-17 2016-11-01 Toray Industries, Inc. Prepreg, method of manufacturing prepreg, and carbon fiber-reinforced composite material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102838766A (en) * 2006-08-07 2012-12-26 东丽株式会社 Prepreg and carbon fiber-reinforced composite material
CN103724813A (en) * 2012-10-16 2014-04-16 辽宁辽杰科技有限公司 Continuous-fiber-reinforced thermoplastic flame-retardant antistatic composite material and preparation method thereof
CN103554530A (en) * 2013-10-11 2014-02-05 中国航空工业集团公司北京航空材料研究院 Electric conductive continuous fiber-reinforced fabric or prepreg and electric conductive treatment method
CN106317772A (en) * 2015-07-10 2017-01-11 深圳光启高等理工研究院 Antistatic composite material and preparation method thereof

Non-Patent Citations (1)

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