CN116198144A - Fiber reinforced resin matrix composite material and preparation method thereof - Google Patents
Fiber reinforced resin matrix composite material and preparation method thereof Download PDFInfo
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- CN116198144A CN116198144A CN202310146827.2A CN202310146827A CN116198144A CN 116198144 A CN116198144 A CN 116198144A CN 202310146827 A CN202310146827 A CN 202310146827A CN 116198144 A CN116198144 A CN 116198144A
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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
- B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
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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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Abstract
The invention provides a fiber reinforced resin matrix composite material and a preparation method thereof, wherein the product comprises a fiber/resin composite material and a toughening layer inserted into the fiber/resin composite material, and the toughening layer is a flame-retardant nanofiber membrane; the preparation method comprises the following steps: taking fiber reinforced resin prepreg or fiber fabric as a receiving base material, forming the flame-retardant nanofiber membrane through electrostatic spinning to obtain a double-layer composite material, sequentially cutting the double-layer composite material according to the required size, overlapping and layering along the same direction, and curing according to a resin-based composite material forming process to obtain the fiber reinforced resin-based composite material; or alternately superposing and layering the fiber reinforced resin prepreg or fiber fabric and the flame-retardant nanofiber membrane, and solidifying according to a resin matrix composite molding process to obtain the fiber reinforced resin matrix composite. The method has simple process, and the product of the invention can endow the fiber reinforced resin matrix composite material with flame retardant property, does not increase the viscosity of the resin during molding, and ensures the mechanical strength of the composite material.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a fiber reinforced resin matrix composite material and a preparation method thereof.
Background
The fiber reinforced resin matrix composite material has the advantages of high specific strength, high specific rigidity, fatigue resistance, good chemical corrosion resistance, strong designability and the like, and is widely applied to the fields of automobiles, aerospace, civil infrastructures and the like. The fiber reinforced resin matrix composite material mainly comprises a resin matrix and a fiber reinforcement. The resin used as a matrix has high flammability generally, can destroy the integral strength of the composite material structure during combustion, and simultaneously releases a large amount of heat and toxic smoke to have adverse effects on personal safety and environment. The flammability problem limits the use of fiber reinforced resin based composites in certain specific applications.
The main solution to the flammability problem of fiber reinforced resin matrix composites is to directly add a large amount of flame retardants such as ammonium polyphosphate, DOPO derivatives, magnesium hydroxide, aluminum hydroxide, etc. into the resin matrix. Although this method can improve the flame retardance of the composite material, the existence of the flame retardant in the resin increases the drag coefficient of the particle group, increases the internal resistance of the fluid, and increases the viscosity of the resin glue solution, so that the molding process of the composite material is changed, and the resin cannot fully impregnate the fiber fabric. Meanwhile, the poor compatibility of the flame retardant and the resin leads to the reduction of the mechanical property of the composite material. The prior art uses a tape casting method to prepare a film containing a flame retardant, and places the film between layers of a composite material to endow the composite material with flame retardance. Although the technology can give consideration to the flame retardance and interlayer mechanical properties of the composite material, the casting film does not have air permeability, an additional mechanical punching procedure is needed to be used as a flame retardant layer of the composite material, and the film material is required to be dissolved in matrix resin at the curing process temperature, so that the method has poor universality. Therefore, it is required to impart flame retardant properties to the fiber-reinforced resin-based composite material without increasing the viscosity of the resin during molding, affecting the molding process of the composite material, and ensuring the mechanical strength of the composite material.
Disclosure of Invention
The invention aims to provide an excellent flame retardant property for a composite material when a flame retardant nanofiber membrane is used as an interlayer of a fiber reinforced resin matrix composite material, and the mechanical property of the composite material is maintained without changing the viscosity of the resin.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a fiber reinforced resin matrix composite material comprises a fiber/resin composite material and a toughening layer inserted into the fiber/resin composite material, wherein the toughening layer is a flame-retardant nanofiber membrane.
As a preferable technical scheme:
the fiber reinforced resin matrix composite material comprises the flame-retardant nanofiber membrane, wherein the nanofiber membrane is composed of nanofibers, and the nanofibers are composed of a thermoplastic polymer fiber body and a flame retardant with the content of 5-50wt% dispersed in the thermoplastic polymer fiber body.
The fiber reinforced resin matrix composite material comprises more than one thermoplastic polymer selected from phenoxy resin, polyaryletherketone, polycaprolactone, polyimide, polyetherimide, polysulfone, polyethersulfone, polyamide, polyphenylene oxide, polystyrene, polyacrylonitrile, polylactic acid, polyvinyl alcohol and polybutylene terephthalate; the flame retardant is one or more of phosphorus-containing flame retardant, nitrogen-containing flame retardant, metal hydroxide, halogen-containing flame retardant and metal salt flame retardant.
The preparation process of the fiber reinforced resin matrix composite material and the flame-retardant nanofiber membrane comprises the following steps: preparing spinning solution composed of thermoplastic polymer, flame retardant and solvent (more than one of ethanol, N-dimethylformamide, N-dimethylacetamide, N-methyl-2-pyrrolidone, dimethyl sulfoxide, tetrahydrofuran, methylene dichloride, pyridine, ethyl acetate, acetone, water, dimethylbenzene and cyclohexanone), and carrying out electrostatic spinning to obtain the flame-retardant nanofiber membrane; the technological parameters of the electrostatic spinning include: the voltage is 25-80KV, the receiving distance is 180-220mm, the temperature is 24 ℃, and the relative humidity is 10-60%.
The fiber-reinforced resin matrix composite material is characterized in that the fibers in the fiber/resin composite material are carbon fibers, glass fibers, aramid fibers, basalt fibers, PBO fibers, boron fibers, ultra-high molecular weight polyethylene fibers or mixed-woven fibers; the resin in the fiber/resin composite material is one or more of epoxy resin, vinyl resin, phenolic resin, urea resin, unsaturated polyester, cyanate resin and bismaleimide resin.
The fiber reinforced resin matrix composite material comprises 10-50wt% of resin in the fiber/resin composite material and 0.1-5wt% of flame-retardant nanofiber membrane in the fiber reinforced resin matrix composite material; the porosity of the flame-retardant nanofiber membrane is 40-80%, the thickness is 10-100 mu m, and the diameter of the nanofiber is 100-1000nm.
The limiting oxygen index of the fiber reinforced resin matrix composite is 23-40%, the bending strength is 400-1200MPa, the interlaminar shear strength is 20-80MPa, and the residual compression strength after impact is 100-350 MPa.
The invention also provides a method for preparing the fiber reinforced resin matrix composite material, which takes fiber reinforced resin prepreg or fiber fabric as a receiving base material, forms the flame-retardant nanofiber membrane through electrostatic spinning to obtain a double-layer composite material, sequentially cuts the double-layer composite material according to the required size, alternately stacks and laminates along the same direction, and cures according to a resin matrix composite material molding process to obtain the fiber reinforced resin matrix composite material;
or alternatively, alternately superposing and layering the fiber reinforced resin prepreg or fiber fabric and the flame-retardant nanofiber membrane, and curing according to a resin matrix composite molding process to obtain the fiber reinforced resin matrix composite.
As a preferable technical scheme:
the method is characterized in that the fiber fabric is one or more of unidirectional fabric, plain fabric, twill fabric and satin fabric.
The principle of the invention is as follows:
the flame retardant is placed between the layers of the composite materials in the form of the electrostatic spinning nanofiber membrane, the viscosity of the resin is not increased due to the addition of the flame retardant, the complete infiltration of the resin to the reinforced fiber fabric is not affected due to the uniform porous structure of the nanofiber membrane, no extra punching process is needed, and the method is suitable for various composite material forming processes.
The flame-retardant component in the nanofiber membrane can promote the fiber membrane and the interlayer region resin to form carbon during combustion, thereby isolating heat, oxygen and fuel from transferring between layers, inhibiting the combustion of the composite material and improving the flame-retardant grade of the composite material. The flame retardant can be uniformly distributed in the nanofiber, and can endow the composite material with higher flame retardant property under the condition of smaller flame retardant usage amount.
In addition, the flame-retardant nanofiber membrane benefits from the nanoscale fiber structure, can play a bridging toughening role between composite material layers, can absorb fracture energy when impacted, prevents the expansion of microcracks between layers, and eliminates the problem that the flame retardant is incompatible with a resin matrix because the flame retardant is dispersed and wrapped in a thermoplastic polymer.
Advantageous effects
(1) The preparation method of the fiber reinforced resin matrix composite material has simple process;
(2) The fiber reinforced resin matrix composite material provided by the invention has the advantages that the flame retardant property of the fiber reinforced resin matrix composite material is endowed, the viscosity of the resin during molding is not increased, and the mechanical strength of the composite material is ensured.
Drawings
FIG. 1 is a schematic illustration of a preparation flow of a fiber reinforced resin matrix composite of the present invention;
FIG. 2 is an interlayer SEM image of the composite material of example 1 after combustion;
FIG. 3 is an interlayer SEM image of the composite material of example 2 after combustion;
FIG. 4 is an interlayer SEM image of the composite material of example 3 after combustion;
FIG. 5 is an interlayer SEM image of the composite material of example 4 after combustion;
FIG. 6 is an SEM image of a nanofiber membrane prepared according to example 5;
FIG. 7 is an SEM image of a nanofiber membrane prepared according to example 6;
FIG. 8 is a thermogravimetric curve of the nanofiber membranes prepared in example 5 and example 6.
Detailed Description
The invention is further described below in conjunction with the detailed description. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
The manufacturer and brand information for the related substances in the following examples are as follows:
phenoxy resin: manufacturer is united carbon, and the brand is PKHH;
polycaprolactone: manufacturer is Suwei, USA, brand 6800;
polylactic acid: the manufacturer is Zhejiang sea biological materials, inc., with the brand name REVODE713;
polyvinyl alcohol: the manufacturer is Shandong Youcao chemical technology Co., ltd, and the brand is PVA1788L;
polybutylene terephthalate: the manufacturer is vinca chemical industry (Jiangsu) limited company with the trade mark of 1100-211M;
polysulfone: vendor Amoxic, U.S. with trade name Udel P-1700;
pentaerythritol phosphate: the manufacturer is WUHANKEMIKE biological medicine technology Co., ltd, and the brand is kmk-23;
bisphenol a bis (diphenyl phosphate): the manufacturer is the Wuhan Kamick science and technology Co., ltd, and the brand is BDP;
tetrabromobisphenol a: the manufacturer is Guangzhou Yuanzha New Material Co., ltd, and the brand is TBBPA
Melamine cyanurate: the manufacturer is Qiao Feng chemical technology Co., ltd, and the brand is MCA;
aluminum diethylphosphinate: the manufacturer is Jiaxing city fine drill new material technology Co., ltd, and the brand is JZ-F200;
ammonium polyphosphate: the manufacturer is Jinan Haobang chemical industry Co., ltd, and the brand is APP2000;
nano magnesium hydroxide: the manufacturer is Weifang Lihe powder science and technology Co., ltd, and the brand is Q-KB-GX2;
zinc stannate: the manufacturer is Yunnan tin industry Co., ltd, and CAS is 12036-37-2;
n, N-dimethylformamide: the manufacturer is national medicine group chemical reagent limited company, and the analytical purity is more than or equal to 99.5 percent;
tetrahydrofuran: the manufacturer is national medicine group chemical reagent limited company, and the analytical purity is more than or equal to 99.8 percent;
pyridine: the manufacturer is national medicine group chemical reagent limited company, and the analytical purity is more than or equal to 99.5 percent;
cyclohexanone: the manufacturer is national medicine group chemical reagent limited company, and the analytical purity is more than or equal to 99.5 percent;
dichloromethane: the manufacturer is national medicine group chemical reagent Co., ltd, and the analytical purity is more than or equal to 99.5 percent.
The method for detecting the relevant performance of the fiber reinforced resin matrix composite material prepared in the following examples is as follows:
the method for detecting the limiting oxygen index comprises the following steps: detection is carried out according to standard GB/T8924-2005;
the method for detecting the bending strength comprises the following steps: detection is carried out according to standard GB/T1447-2005;
the method for detecting the interlayer shear strength comprises the following steps: detecting according to standard GB/T30969-2014;
the method for detecting the viscosity of the resin during molding comprises the following steps: detecting according to a standard GB/T2794-2013;
the method for detecting the residual compressive strength after impact comprises the following steps: the samples were first subjected to an impact test (20J impact energy) with reference to the standard ASTM D7136/D7136M-2015, and then subjected to a compression test with reference to the standard ASTM D7137/D7137M-17.
Example 1
A method for preparing a fiber reinforced resin matrix composite material comprises the following specific steps:
(1) Preparing raw materials:
receiving a substrate: carbon fiber plain weave (manufacturer: zhongfushen eagle carbon fiber Co., ltd., brand: 3K240 g);
thermoplastic polymer: a phenoxy resin;
flame retardant: pentaerythritol phosphate;
solvent: n, N-dimethylformamide;
(2) Preparing spinning solution composed of thermoplastic polymer, flame retardant and solvent, and forming a flame-retardant nanofiber membrane on a receiving substrate through electrostatic spinning to obtain a double-layer composite material; wherein, the voltage of electrostatic spinning is 50KV, the receiving distance is 220mm, the temperature is 24 ℃, the relative humidity is 30%, and the concentration of thermoplastic polymer in spinning solution is 28wt%;
the flame-retardant nanofiber membrane formed consists of nanofibers with the average diameter of 557nm, wherein the nanofibers consist of a thermoplastic polymer fiber body and a flame retardant with the content of 40 weight percent dispersed in the thermoplastic polymer fiber body; the porosity of the flame-retardant nanofiber membrane is 72.1 percent, and the thickness is 100 mu m;
(3) Cutting the double-layer composite material according to the required size, alternately overlapping and layering along the same direction, and curing according to the resin matrix composite material molding process to obtain the fiber reinforced resin matrix composite material.
The finally prepared fiber reinforced resin matrix composite is composed of a fiber/resin composite and a flame-retardant nanofiber membrane inserted into the fiber/resin composite; wherein the resin in the fiber/resin composite (i.e., vinyl resin, manufacturer is Huachang Polymer Co., university of Huadong, trade name is
30-200P) accounts for 37.8wt% of the fiber reinforced resin matrix composite material, and the flame-retardant nanofiber membrane accounts for 3.8wt% of the fiber reinforced resin matrix composite material;
the limiting oxygen index of the fiber reinforced resin matrix composite is 32.1%, the bending strength is 598.3MPa, the interlaminar shear strength is 47.3MPa, the resin viscosity is 293.2cps during molding, and the residual compression strength after impact is 154.3MPa.
Example 2
A method for preparing a fiber reinforced resin matrix composite material comprises the following specific steps:
(1) Preparing raw materials:
receiving a substrate: carbon fiber plain weave (manufacturer: zhongfushen eagle carbon fiber Co., ltd., brand: 3K240 g);
thermoplastic polymer: a phenoxy resin;
flame retardant: bisphenol a bis (diphenyl phosphate);
solvent: n, N-dimethylformamide;
(2) Preparing spinning solution composed of thermoplastic polymer, flame retardant and solvent, and forming a flame-retardant nanofiber membrane on a receiving substrate through electrostatic spinning to obtain a double-layer composite material; wherein, the voltage of electrostatic spinning is 50KV, the receiving distance is 220mm, the temperature is 24 ℃, the relative humidity is 30%, and the concentration of thermoplastic polymer in spinning solution is 28wt%;
the formed flame-retardant nanofiber membrane consists of nanofibers with the average diameter of 468nm, wherein the nanofibers consist of a thermoplastic polymer fiber body and a flame retardant with the content of 40 weight percent dispersed in the thermoplastic polymer fiber body; the porosity of the flame-retardant nanofiber membrane is 68.3%, and the thickness is 100 mu m;
(3) Cutting the double-layer composite material according to the required size, alternately overlapping and layering along the same direction, and curing according to the resin matrix composite material molding process to obtain the fiber reinforced resin matrix composite material.
The finally prepared fiber reinforced resin matrix composite is composed of a fiber/resin composite and a flame-retardant nanofiber membrane inserted into the fiber/resin composite; wherein the resin in the fiber/resin composite (i.e., vinyl resin, manufacturer is Huachang Polymer Co., university of Huadong, trade name is
30-200P) accounts for 38.7wt% of the fiber reinforced resin matrix composite material, and the flame-retardant nanofiber membrane accounts for 3.7wt% of the fiber reinforced resin matrix composite material;
the limiting oxygen index of the fiber reinforced resin matrix composite is 31.8%, the bending strength is 654.1MPa, the interlaminar shear strength is 48.5MPa, the resin viscosity is 291.5cps during molding, and the residual compression strength after impact is 147.6MPa.
Example 3
A method for preparing a fiber reinforced resin matrix composite material comprises the following specific steps:
(1) Preparing raw materials:
receiving a substrate: carbon fiber plain weave (manufacturer: zhongfushen eagle carbon fiber Co., ltd., brand: 3K240 g);
thermoplastic polymer: a phenoxy resin;
flame retardant: pentaerythritol phosphate and nano magnesium hydroxide mixture with the mass ratio of 3:1;
solvent: n, N-dimethylformamide;
(2) Preparing spinning solution composed of thermoplastic polymer, flame retardant and solvent, and forming a flame-retardant nanofiber membrane on a receiving substrate through electrostatic spinning to obtain a double-layer composite material; wherein, the voltage of electrostatic spinning is 50KV, the receiving distance is 220mm, the temperature is 24 ℃, the relative humidity is 30%, and the concentration of thermoplastic polymer in spinning solution is 28wt%;
the flame-retardant nanofiber membrane formed consists of nanofibers with the average diameter of 447nm, wherein the nanofibers consist of a thermoplastic polymer fiber body and a flame retardant with the content of 40 weight percent dispersed in the thermoplastic polymer fiber body; the porosity of the flame-retardant nanofiber membrane is 67%, and the thickness is 100 mu m;
(3) Cutting the double-layer composite material according to the required size, alternately overlapping and layering along the same direction, and curing according to the resin matrix composite material molding process to obtain the fiber reinforced resin matrix composite material.
The finally prepared fiber reinforced resin matrix composite is composed of a fiber/resin composite and a flame-retardant nanofiber membrane inserted into the fiber/resin composite; wherein the resin in the fiber/resin composite (i.e., vinyl resin, manufacturer is Huachang Polymer Co., university of Huadong, trade name is
30-200P) in the fiber reinforced resin matrix composite material is 36.9wt percent, and the flame-retardant nanofiber membrane is in the fiber reinforced resinThe ratio of the base composite material was 4.21wt%;
the limiting oxygen index of the fiber reinforced resin matrix composite is 32.7%, the bending strength is 587.2MPa, the interlaminar shear strength is 47.9MPa, the resin viscosity is 288.1cps during molding, and the residual compression strength after impact is 153.4MPa.
Example 4
(1) Preparing raw materials:
receiving a substrate: carbon fiber plain weave (manufacturer: zhongfushen eagle carbon fiber Co., ltd., brand: 3K240 g);
thermoplastic polymer: a phenoxy resin;
flame retardant: pentaerythritol phosphate and zinc stannate mixture with a mass ratio of 3:1;
solvent: n, N-dimethylformamide;
(2) Preparing spinning solution composed of thermoplastic polymer, flame retardant and solvent, and forming a flame-retardant nanofiber membrane on a receiving substrate through electrostatic spinning to obtain a double-layer composite material; wherein, the voltage of electrostatic spinning is 50KV, the receiving distance is 220mm, the temperature is 24 ℃, the relative humidity is 30%, and the concentration of thermoplastic polymer in spinning solution is 28wt%;
the flame-retardant nanofiber membrane formed consists of nanofibers with the average diameter of 445nm, wherein the nanofibers consist of a thermoplastic polymer fiber body and a flame retardant with the content of 40 weight percent dispersed in the thermoplastic polymer fiber body; the porosity of the flame-retardant nanofiber membrane is 63.2%, and the thickness is 100 mu m;
(3) Cutting the double-layer composite material according to the required size, alternately overlapping and layering along the same direction, and curing according to the resin matrix composite material molding process to obtain the fiber reinforced resin matrix composite material.
The finally prepared fiber reinforced resin matrix composite is composed of a fiber/resin composite and a flame-retardant nanofiber membrane inserted into the fiber/resin composite; wherein the resin in the fiber/resin composite (i.e., vinyl resin, manufacturer is Huachang Polymer Co., university of Huadong, trade name is
30-200P) accounts for 38.1wt% of the fiber reinforced resin matrix composite material, and the flame-retardant nano fiber membrane accounts for 3.86wt% of the fiber reinforced resin matrix composite material;
the limiting oxygen index of the fiber reinforced resin matrix composite is 32.4%, the bending strength is 624.5MPa, the interlaminar shear strength is 48.2MPa, the resin viscosity is 296.8cps during molding, and the residual compression strength after impact is 145.5MPa.
Example 5
A method for preparing a fiber reinforced resin matrix composite material comprises the following specific steps:
(1) Preparing raw materials:
receiving a substrate: carbon fiber plain weave (manufacturer: zhongfushen eagle carbon fiber Co., ltd., brand: 3K240 g);
thermoplastic polymer: a phenoxy resin;
flame retardant: pentaerythritol phosphate;
solvent: n, N-dimethylformamide;
(2) Preparing spinning solution composed of thermoplastic polymer, flame retardant and solvent, and forming a flame-retardant nanofiber membrane on a receiving substrate through electrostatic spinning to obtain a double-layer composite material; wherein, the voltage of electrostatic spinning is 40KV, the receiving distance is 220mm, the temperature is 24 ℃, the relative humidity is 30%, and the concentration of thermoplastic polymer in spinning solution is 28wt%;
the flame-retardant nanofiber membrane formed consists of nanofibers with the average diameter of 446nm, wherein the nanofibers consist of a thermoplastic polymer fiber body and a flame retardant with the content of 40 weight percent dispersed in the thermoplastic polymer fiber body; the porosity of the flame-retardant nanofiber membrane is 55.8%, and the thickness is 30 mu m;
(3) Cutting the double-layer composite material according to the required size, alternately overlapping and layering along the same direction, and curing according to the resin matrix composite material molding process to obtain the fiber reinforced resin matrix composite material.
The finally prepared fiber reinforced resin matrix composite is composed of a fiber/resin composite and a flame-retardant nanofiber membrane inserted into the fiber/resin composite; wherein the resin in the fiber/resin composite (i.e., epoxy resinThe manufacturer is Huadong university Huachang polymer Limited company with the trade mark of
3312A/B) 28.1wt% of the fiber reinforced resin matrix composite, and 1.58wt% of the flame retardant nanofiber membrane in the fiber reinforced resin matrix composite;
the limiting oxygen index of the fiber reinforced resin matrix composite is 32.4%, the bending strength is 894.4MPa, the interlaminar shear strength is 58.6MPa, the resin viscosity is 237.1cps during molding, and the residual compression strength after impact is 219.4MPa.
Example 6
A method for preparing a fiber reinforced resin matrix composite material comprises the following specific steps:
(1) Preparing raw materials:
receiving a substrate: carbon fiber plain weave (manufacturer: zhongfushen eagle carbon fiber Co., ltd., brand: 3K240 g);
thermoplastic polymer: a phenoxy resin;
flame retardant: pentaerythritol phosphate;
solvent: n, N-dimethylformamide;
(2) Preparing spinning solution composed of thermoplastic polymer, flame retardant and solvent, and forming a flame-retardant nanofiber membrane on a receiving substrate through electrostatic spinning to obtain a double-layer composite material; wherein, the voltage of electrostatic spinning is 40KV, the receiving distance is 220mm, the temperature is 24 ℃, the relative humidity is 30%, and the concentration of thermoplastic polymer in spinning solution is 28wt%;
the flame-retardant nanofiber membrane formed consists of nanofibers with the average diameter of 447nm, wherein the nanofibers consist of a thermoplastic polymer fiber body and 50wt% of flame retardant dispersed therein; the porosity of the flame-retardant nanofiber membrane is 60.2%, and the thickness is 30 mu m;
(3) Cutting the double-layer composite material according to the required size, alternately overlapping and layering along the same direction, and curing according to the resin matrix composite material molding process to obtain the fiber reinforced resin matrix composite material.
The finally prepared fiber reinforced resin matrix composite is composed of a fiber/resin composite and a flame-retardant nanofiber membrane inserted into the fiber/resin composite; wherein the resin in the fiber/resin composite material (i.e., epoxy resin, manufacturer is Huachang Polymer Co., ltd., trade name: huadong university)
3312A/B) 29.6wt% of the fiber reinforced resin matrix composite, and 1.53wt% of the flame-retardant nanofiber membrane;
the limiting oxygen index of the fiber reinforced resin matrix composite is 34.7%, the bending strength is 885.5MPa, the interlaminar shear strength is 58.4MPa, the resin viscosity is 239.5cps during molding, and the residual compression strength after impact is 204.5MPa.
Example 7
A method for preparing a fiber reinforced resin matrix composite material comprises the following specific steps:
(1) Preparing raw materials:
receiving a substrate: carbon fiber plain weave (manufacturer: zhongfushen eagle carbon fiber Co., ltd., brand: 3K240 g);
thermoplastic polymer: a phenoxy resin;
flame retardant: tetrabromobisphenol a;
solvent: n, N-dimethylformamide;
(2) Preparing spinning solution composed of thermoplastic polymer, flame retardant and solvent, and forming a flame-retardant nanofiber membrane on a receiving substrate through electrostatic spinning to obtain a double-layer composite material; wherein, the voltage of electrostatic spinning is 50KV, the receiving distance is 220mm, the temperature is 24 ℃, the relative humidity is 30%, and the concentration of thermoplastic polymer in spinning solution is 28wt%;
the flame-retardant nanofiber membrane formed consists of nanofibers with average diameter of 475nm, wherein the nanofibers consist of a thermoplastic polymer fiber body and a flame retardant with the content of 30 weight percent dispersed in the thermoplastic polymer fiber body; the porosity of the flame-retardant nanofiber membrane is 63.6%, and the thickness is 80 mu m;
(3) Cutting the double-layer composite material according to the required size, alternately overlapping and layering along the same direction, and curing according to the resin matrix composite material molding process to obtain the fiber reinforced resin matrix composite material.
The finally prepared fiber reinforced resin matrix composite is composed of a fiber/resin composite and a flame-retardant nanofiber membrane inserted into the fiber/resin composite; wherein the resin in the fiber/resin composite material (i.e., epoxy resin, manufacturer is Huachang Polymer Co., ltd., trade name: huadong university)
3312A/B) in the fiber reinforced resin matrix composite at a ratio of 37.9wt%, and the flame retardant nanofiber membrane in the fiber reinforced resin matrix composite at a ratio of 3.43wt%;
the limiting oxygen index of the fiber reinforced resin matrix composite is 31.2%, the bending strength is 844.6MPa, the interlaminar shear strength is 57.5MPa, the resin viscosity is 226.4cps during molding, and the residual compression strength after impact is 205.6MPa.
Example 8
A method for preparing a fiber reinforced resin matrix composite material comprises the following specific steps:
(1) Preparing raw materials:
receiving a substrate: fiber reinforced resin prepregs (manufacturer: yixing city Ci Yi Xin Ji carbon fiber products Co., ltd., brand: H-CP 3200);
thermoplastic polymer: a phenoxy resin;
flame retardant: pentaerythritol phosphate;
solvent: n, N-dimethylformamide;
(2) Preparing spinning solution composed of thermoplastic polymer, flame retardant and solvent, and forming a flame-retardant nanofiber membrane on a receiving substrate through electrostatic spinning to obtain a double-layer composite material; wherein, the voltage of electrostatic spinning is 40KV, the receiving distance is 180mm, the temperature is 24 ℃, the relative humidity is 20%, and the concentration of thermoplastic polymer in spinning solution is 28wt%;
the flame-retardant nanofiber membrane formed consists of nanofibers with an average diameter of 445nm, wherein the nanofibers consist of a thermoplastic polymer fiber body and a flame retardant with a content of 30wt% dispersed therein; the porosity of the flame-retardant nanofiber membrane is 77.2%, and the thickness is 80 mu m;
(3) Cutting the double-layer composite material according to the required size, alternately overlapping and layering along the same direction, and curing according to the resin matrix composite material molding process to obtain the fiber reinforced resin matrix composite material.
The finally prepared fiber reinforced resin matrix composite is composed of a fiber/resin composite and a flame-retardant nanofiber membrane inserted into the fiber/resin composite; wherein, the resin in the fiber/resin composite material (the resin in the fiber reinforced resin prepreg) accounts for 39.5wt% of the fiber reinforced resin matrix composite material, and the flame-retardant nano fiber film accounts for 3.45wt% of the fiber reinforced resin matrix composite material;
the limiting oxygen index of the fiber reinforced resin matrix composite is 30.6%, the bending strength is 1163.2MPa, the interlaminar shear strength is 74.5MPa, and the residual compression strength after impact is 241.3MPa.
Example 9
A method for preparing a fiber reinforced resin matrix composite material comprises the following specific steps:
(1) Preparing raw materials:
fiber reinforced resin prepregs (manufacturer: yixing city Ci Yi Xin Ji carbon fiber products Co., ltd., brand: H-CP 3200);
thermoplastic polymer: polysulfone;
flame retardant: melamine cyanurate;
solvent: a mixture of N, N-dimethylformamide and tetrahydrofuran in a volume ratio of 5:5;
(2) Preparing a flame-retardant nanofiber membrane:
preparing spinning solution composed of thermoplastic polymer, flame retardant and solvent, and then carrying out electrostatic spinning to obtain the flame-retardant nanofiber membrane; wherein, the voltage of electrostatic spinning is 25KV, the receiving distance is 190mm, the temperature is 24 ℃, and the relative humidity is 60%;
the flame-retardant nanofiber membrane formed consists of nanofibers with an average diameter of 956nm, wherein the nanofibers consist of a thermoplastic polymer fiber body and a flame retardant with the content of 20wt% dispersed in the thermoplastic polymer fiber body; the porosity of the flame-retardant nanofiber membrane is 72.6%, and the thickness is 60 mu m;
(3) And (3) alternately superposing and layering the fiber reinforced resin prepreg and the flame-retardant nanofiber membrane prepared in the step (2), and curing according to a resin matrix composite molding process to obtain the fiber reinforced resin matrix composite.
The finally prepared fiber reinforced resin matrix composite is composed of a fiber/resin composite and a flame-retardant nanofiber membrane inserted into the fiber/resin composite; wherein, the resin in the fiber/resin composite material (the resin in the fiber reinforced resin prepreg) accounts for 39.3wt% of the fiber reinforced resin matrix composite material, and the flame-retardant nano fiber film accounts for 2.93wt% of the fiber reinforced resin matrix composite material;
the limiting oxygen index of the fiber reinforced resin matrix composite is 28.8%, the bending strength is 1012.6MPa, the interlaminar shear strength is 72.1MPa, and the residual compression strength after impact is 238.4MPa.
Example 10
A method for preparing a fiber reinforced resin matrix composite material comprises the following specific steps:
(1) Preparing raw materials:
fiber reinforced resin prepregs (manufacturer: yixing city Ci Yi Xin Ji carbon fiber products Co., ltd., brand: H-CP 3200);
thermoplastic polymer: polycaprolactone;
flame retardant: aluminum diethylphosphinate;
solvent: a mixture of N, N-dimethylformamide and dichloromethane in a volume ratio of 7:3;
(2) Preparing a flame-retardant nanofiber membrane:
preparing spinning solution composed of thermoplastic polymer, flame retardant and solvent, and then carrying out electrostatic spinning to obtain the flame-retardant nanofiber membrane; wherein, the voltage of electrostatic spinning is 80KV, the receiving distance is 190mm, the temperature is 24 ℃, and the relative humidity is 40%;
the flame-retardant nanofiber membrane formed consists of nanofibers with the average diameter of 322nm, wherein the nanofibers consist of a thermoplastic polymer fiber body and a flame retardant with the content of 20 weight percent dispersed in the thermoplastic polymer fiber body; the porosity of the flame-retardant nanofiber membrane is 52.3%, and the thickness is 60 mu m;
(3) And (3) alternately superposing and layering the fiber reinforced resin prepreg and the flame-retardant nanofiber membrane prepared in the step (2), and curing according to a resin matrix composite molding process to obtain the fiber reinforced resin matrix composite.
The finally prepared fiber reinforced resin matrix composite is composed of a fiber/resin composite and a flame-retardant nanofiber membrane inserted into the fiber/resin composite; wherein, the resin in the fiber/resin composite material (the resin in the fiber reinforced resin prepreg) accounts for 38.9wt% of the fiber reinforced resin matrix composite material, and the flame-retardant nano fiber film accounts for 3.05wt% of the fiber reinforced resin matrix composite material;
the limiting oxygen index of the fiber reinforced resin matrix composite is 30.6%, the bending strength is 1058.3MPa, the interlaminar shear strength is 73.5MPa, and the residual compressive strength after impact is 232.7MPa.
Example 11
A method for preparing a fiber reinforced resin matrix composite material comprises the following specific steps:
(1) Preparing raw materials:
fiber reinforced resin prepregs (manufacturer: yixing city Ci Yi Xin Ji carbon fiber products Co., ltd., brand: H-CP 3200);
thermoplastic polymer: polylactic acid;
flame retardant: bisphenol a bis (diphenyl phosphate) and zinc stannate in a mass ratio of 3:1;
solvent: a mixture of dichloromethane and pyridine in a volume ratio of 5:5;
(2) Preparing a flame-retardant nanofiber membrane:
preparing spinning solution composed of thermoplastic polymer, flame retardant and solvent, and then carrying out electrostatic spinning to obtain the flame-retardant nanofiber membrane; wherein, the voltage of electrostatic spinning is 40KV, the receiving distance is 180mm, the temperature is 24 ℃, and the relative humidity is 40%;
the flame-retardant nanofiber membrane formed by the method consists of nanofibers with the average diameter of 685nm, wherein the nanofibers consist of a thermoplastic polymer fiber body and a flame retardant with the content of 30 weight percent dispersed in the thermoplastic polymer fiber body; the porosity of the flame-retardant nanofiber membrane is 63.1 percent, and the thickness is 60 mu m;
(3) And (3) alternately superposing and layering the fiber reinforced resin prepreg and the flame-retardant nanofiber membrane prepared in the step (2), and curing according to a resin matrix composite molding process to obtain the fiber reinforced resin matrix composite.
The finally prepared fiber reinforced resin matrix composite is composed of a fiber/resin composite and a flame-retardant nanofiber membrane inserted into the fiber/resin composite; wherein, the resin in the fiber/resin composite material (the resin in the fiber reinforced resin prepreg) accounts for 39.6wt% in the fiber reinforced resin matrix composite material, and the flame-retardant nano fiber film accounts for 3.12wt% in the fiber reinforced resin matrix composite material;
the limiting oxygen index of the fiber reinforced resin matrix composite is 29.3%, the bending strength is 1025.7MPa, the interlaminar shear strength is 72.8MPa, and the residual compressive strength after impact is 234.2MPa.
Example 12
A method for preparing a fiber reinforced resin matrix composite material comprises the following specific steps:
(1) Preparing raw materials:
glass fiber plain weave (manufacturer: hezhou city Ruishan new material science and technology company, trade mark: EWR-200);
thermoplastic polymer: polyvinyl alcohol;
flame retardant: ammonium polyphosphate;
solvent: water;
(2) Preparing a flame-retardant nanofiber membrane:
preparing spinning solution composed of thermoplastic polymer, flame retardant and solvent, and then carrying out electrostatic spinning to obtain the flame-retardant nanofiber membrane; wherein, the voltage of electrostatic spinning is 35KV, the receiving distance is 200mm, the temperature is 24 ℃, and the relative humidity is 20%;
the flame-retardant nanofiber membrane formed consists of nanofibers with the average diameter of 421nm, wherein the nanofibers consist of a thermoplastic polymer fiber body and a flame retardant with the content of 5 weight percent dispersed in the thermoplastic polymer fiber body; the porosity of the flame-retardant nanofiber membrane is 74.4 percent, and the thickness is 50 mu m;
(3) And (3) alternately superposing and layering the glass fiber plain weave and the flame-retardant nanofiber membrane prepared in the step (2), and curing according to a resin matrix composite molding process to obtain the fiber reinforced resin matrix composite.
The finally prepared fiber reinforced resin matrix composite is composed of a fiber/resin composite and a flame-retardant nanofiber membrane inserted into the fiber/resin composite; wherein the resin in the fiber/resin composite (i.e., vinyl resin, manufacturer is Huachang Polymer Co., university of Huadong, trade name is
30-200P) accounts for 28.3wt% of the fiber reinforced resin matrix composite material, and the flame-retardant nano fiber membrane accounts for 2.76wt% of the fiber reinforced resin matrix composite material;
the limiting oxygen index of the fiber reinforced resin matrix composite is 28.2%, the bending strength is 574.6MPa, the interlaminar shear strength is 57.2MPa, the resin viscosity is 238.5cps during molding, and the residual compression strength after impact is 168.2MPa.
Example 13
A method for preparing a fiber reinforced resin matrix composite material comprises the following specific steps:
(1) Preparing raw materials:
glass fiber plain weave (manufacturer: hezhou city Ruishan new material science and technology company, trade mark: EWR-200);
thermoplastic polymer: polybutylene terephthalate;
flame retardant: aluminum diethylphosphinate;
solvent: a mixture of dichloromethane and cyclohexanone in a volume ratio of 5:5;
(2) Preparing a flame-retardant nanofiber membrane:
preparing spinning solution composed of thermoplastic polymer, flame retardant and solvent, and then carrying out electrostatic spinning to obtain the flame-retardant nanofiber membrane; wherein, the voltage of electrostatic spinning is 50KV, the receiving distance is 200mm, the temperature is 24 ℃, and the relative humidity is 10%;
the flame-retardant nanofiber membrane formed consists of nanofibers with the average diameter of 464nm, wherein the nanofibers consist of a thermoplastic polymer fiber body and a flame retardant with the content of 20 weight percent dispersed in the thermoplastic polymer fiber body; the porosity of the flame-retardant nanofiber membrane is 44.7%, and the thickness is 50 μm;
(3) And (3) alternately superposing and layering the glass fiber plain weave and the flame-retardant nanofiber membrane prepared in the step (2), and curing according to a resin matrix composite molding process to obtain the fiber reinforced resin matrix composite.
The finally prepared fiber reinforced resin matrix composite is composed of a fiber/resin composite and a flame-retardant nanofiber membrane inserted into the fiber/resin composite; wherein the resin in the fiber/resin composite (i.e., vinyl resin, manufacturer is Huachang Polymer Co., university of Huadong, trade name is
30-200P) accounts for 28.9wt% of the fiber reinforced resin matrix composite material, and the flame-retardant nano fiber membrane accounts for 2.81wt% of the fiber reinforced resin matrix composite material;
the limiting oxygen index of the fiber reinforced resin matrix composite is 31.2%, the bending strength is 556.4MPa, the interlaminar shear strength is 56.3MPa, the resin viscosity is 232.8cps during molding, and the residual compression strength after impact is 175.1MPa.
Claims (10)
1. The fiber reinforced resin matrix composite material comprises a fiber/resin composite material and a toughening layer inserted into the fiber/resin composite material, and is characterized in that the toughening layer is a flame-retardant nanofiber membrane.
2. A fiber reinforced resin matrix composite according to claim 1, wherein the flame retardant nanofiber membrane is comprised of nanofibers comprised of a thermoplastic polymer fiber body and a flame retardant dispersed therein in an amount of 5 to 50 wt%.
3. The fiber reinforced resin matrix composite according to claim 2, wherein the thermoplastic polymer is one or more of phenoxy resin, polyaryletherketone, polycaprolactone, polyimide, polyetherimide, polysulfone, polyethersulfone, polyamide, polyphenylene oxide, polystyrene, polyacrylonitrile, polylactic acid, polyvinyl alcohol, and polybutylene terephthalate; the flame retardant is one or more of phosphorus-containing flame retardant, nitrogen-containing flame retardant, metal hydroxide, halogen-containing flame retardant and metal salt flame retardant.
4. The fiber reinforced resin matrix composite of claim 2, wherein the flame retardant nanofiber membrane is prepared by the steps of: preparing spinning solution composed of thermoplastic polymer, flame retardant and solvent, and then carrying out electrostatic spinning to obtain the flame-retardant nanofiber membrane; the technological parameters of the electrostatic spinning include: the voltage is 25-80KV, the receiving distance is 180-220mm, the temperature is 24 ℃, and the relative humidity is 10-60%.
5. The fiber reinforced resin matrix composite of claim 1, wherein the fibers in the fiber/resin composite are carbon fibers, glass fibers, aramid fibers, basalt fibers, PBO fibers, boron fibers, ultra high molecular weight polyethylene fibers, or co-woven fibers; the resin in the fiber/resin composite material is one or more of epoxy resin, vinyl resin, phenolic resin, urea resin, unsaturated polyester, cyanate resin and bismaleimide resin.
6. The fiber reinforced resin matrix composite according to claim 5, wherein the ratio of resin in the fiber/resin composite to the fiber reinforced resin matrix composite is 10-50wt%, and the ratio of the flame retardant nanofiber membrane to the fiber reinforced resin matrix composite is 0.1-5wt%; the porosity of the flame-retardant nanofiber membrane is 40-80%, the thickness is 10-100 mu m, and the diameter of the nanofiber is 100-1000nm.
7. The fiber reinforced resin matrix composite according to claim 6, wherein the fiber reinforced resin matrix composite has a limiting oxygen index of 23 to 40%, a flexural strength of 400 to 1200MPa, an interlaminar shear strength of 20 to 80MPa, and a residual compressive strength after impact of 100 to 350MPa.
8. A method for preparing the fiber reinforced resin matrix composite according to any one of claims 1 to 7, wherein the fiber reinforced resin matrix composite is prepared by forming the flame-retardant nanofiber membrane by electrostatic spinning with fiber reinforced resin prepreg or fiber fabric as a receiving substrate, obtaining a double-layer composite, sequentially cutting the double-layer composite according to a required size, alternately overlapping and layering along the same direction, and curing according to a resin matrix composite molding process.
9. A method for preparing the fiber reinforced resin matrix composite according to any one of claims 1 to 7, wherein after the fiber reinforced resin prepreg or fiber fabric and the flame retardant nanofiber membrane are alternately overlapped and laid, the fiber reinforced resin matrix composite is obtained by curing according to a resin matrix composite molding process.
10. The method of claim 8 or 9, wherein the fiber fabric is one or more of a unidirectional fabric, a plain weave fabric, a twill weave fabric, and a satin weave fabric.
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