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CN117887212A - Preparation method of high-strength fiber-reinforced synthetic resin composite material - Google Patents

Preparation method of high-strength fiber-reinforced synthetic resin composite material Download PDF

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CN117887212A
CN117887212A CN202410059428.7A CN202410059428A CN117887212A CN 117887212 A CN117887212 A CN 117887212A CN 202410059428 A CN202410059428 A CN 202410059428A CN 117887212 A CN117887212 A CN 117887212A
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synthetic resin
composite material
resin composite
reinforced synthetic
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CN117887212B (en
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许德仲
李伟
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Shenzhen Shensaier Co Ltd
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Shenzhen Shensaier Co Ltd
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    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
    • C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
    • 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
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
    • 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
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/046—Reinforcing macromolecular compounds with loose or coherent fibrous material with synthetic macromolecular fibrous material
    • 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
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/047—Reinforcing macromolecular compounds with loose or coherent fibrous material with mixed fibrous material
    • 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
    • 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
    • C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
    • C08J2433/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C08J2433/08—Homopolymers or copolymers of acrylic acid esters
    • C—CHEMISTRY; METALLURGY
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    • 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
    • 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
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    • 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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Abstract

The invention discloses a preparation method of a high-strength fiber-reinforced synthetic resin composite material, which comprises the steps of synthesizing slurry composed of polyamide-imide copolymer solution, polyacrylate with a siloxane structure and an organosilicon defoamer, weaving a skeleton by using glass fibers and silicon carbide fiber bundles, wherein the lower surface of the skeleton is an aramid fiber layer, the upper surface of the skeleton is slurry, discharging air, coating an aramid fiber layer on the uppermost surface, feeding the aramid fiber layer into a rolling device, spraying epoxy resin for rolling and pressing, and curing to obtain the high-strength fiber-reinforced synthetic resin composite material.

Description

Preparation method of high-strength fiber-reinforced synthetic resin composite material
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a preparation method of a high-strength fiber-reinforced synthetic resin composite material.
Background
The polyamide-imide synthetic resin has the characteristics of high strength, high wear resistance and the like, and is often applied to the industries of aerospace, military industry, automobiles and the like, such as manufacturing aircraft parts, engine shells and the like. However, the production cost is too high, the production process is difficult to control accurately, the performance of the generated polyamide imide is often influenced by the production conditions and the external environment, the expected result of research personnel is often not obtained, the performances such as the shearing force of the polyamide imide are weakened, and the polyamide imide is easy to deform when the polyamide imide is subjected to impact extrusion and other conditions. In addition, when a polyamide-imide synthetic resin with high hardness and high rigidity is pursued by research and development personnel, toughness is easy to be reduced, resin becomes brittle, stretching capability is reduced, and epoxy resin and the like are usually added for modification, but the amount of the modified resin is difficult to control, and the performance of the synthetic resin is easy to be reduced. The invention relates to a preparation method of a high-strength fiber-reinforced synthetic resin composite material, which is characterized in that the high-strength fiber-reinforced synthetic resin composite material prepared by the preparation method is modified by using a filler, different resins are added to expand the performance of polyamide imide, and a structure containing a framework interlayer is designed to resist impact force caused by impact and extrusion.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a preparation method of a high-strength fiber-reinforced synthetic resin composite material.
The invention provides a preparation method of a high-strength fiber-reinforced synthetic resin composite material, which is used for preparing a skeleton woven by middle glass fibers and silicon carbide fibers, slurry on the upper layer of the skeleton, an aramid layer below the skeleton and an aramid layer on the slurry.
Further, the preparation of the slurry raw material comprises: polyacrylate, calcium stearate, polyamideimide copolymer, and silicone defoamer.
Further, the raw materials for preparing the slurry comprise, by weight, 20 parts of polyacrylate, 5 parts of calcium stearate, 40 parts of polyamide-imide copolymer and 2 parts of organosilicon defoamer.
Further, the preparation of the polyamideimide copolymer raw material comprises: n, N-dimethylacetamide, 2 '-bis (trifluoromethyl) benzidine, 4' - (hexafluoroisopropylidene) diphthalic anhydride, terephthaloyl chloride, N-dimethylacetamide, pyridine, acetic anhydride, and propylene oxide.
Further, the preparation of the polyamideimide copolymer comprises the following raw materials in parts by weight: 45 to 55 parts of N, N-dimethylacetamide, 3 to 4 parts of 2,2 '-bis (trifluoromethyl) benzidine, 1.5 to 2 parts of 4,4' - (hexafluoroisopropylidene) diphthalic anhydride, 1.6 to 1.65 parts of terephthaloyl chloride, 3 to 8 parts of N, N-dimethylacetamide, 1 to 1.3 parts of pyridine, 0.2 to 0.6 part of acetic anhydride and 1.7 to 1.8 parts of propylene oxide.
Further, the preparation of the polyacrylate material comprises: toluene, xylene, azobisisoheptonitrile, methyl methacrylate, ethyl methacrylate, butyl acrylate, octyl acrylate and vinyltrimethoxysilane.
Further, the preparation of the polyacrylate comprises the following raw materials in parts by weight: 80 to 120 parts of toluene, 30 to 50 parts of xylene, 1 to 2 parts of azodiisoheptonitrile, 15 to 25 parts of methyl methacrylate, 15 to 25 parts of ethyl methacrylate, 50 to 70 parts of butyl acrylate, 70 to 90 parts of octyl acrylate and 4 to 8 parts of vinyl trimethoxy silane.
Further, the skeleton is composed of glass fiber bundles and silicon carbide fiber bundles.
Further, the high-strength fiber-reinforced synthetic resin composite material is formed by weaving glass fiber bundles and silicon carbide fiber bundles respectively serving as warp yarns and weft yarns, and forming a skeleton structure after weaving is completed; coating an aramid fiber layer on the lower surface of the framework structure, and spraying slurry on the upper surface of the framework structure; the sizing agent is as follows: placing the ground polyacrylate and calcium stearate in a polyamide-imide copolymer solution, adding an organosilicon defoamer, and preparing a suspension by ultrasonic dispersion; drying after spraying, discharging air in the skeleton structure through ultrasonic oscillation after drying, and coating an aramid fiber layer on the upper surface after discharging to obtain a semi-finished product; and (3) feeding the semi-finished product into a rolling device, spraying atomized epoxy resin at 160 ℃ and in a vacuum state, rolling and pressing, and curing for 3 hours at 240 ℃ after pressing to obtain the high-strength fiber-reinforced synthetic resin composite material.
Further, after the lamination, curing is carried out for 3 hours at 240 ℃ to obtain the high-strength fiber reinforced synthetic resin composite material.
The high-strength fiber reinforced synthetic resin composite material provided by the invention has the thermal deformation temperature of more than or equal to 294 ℃, the tensile strength of more than or equal to 838MPa, the bending strength of more than or equal to 283MPa and the compression strength of more than or equal to 286MPa.
The preparation method of the high-strength fiber-reinforced synthetic resin composite material provided by the invention has the following beneficial effects:
1. the invention prepares the high-strength fiber-reinforced synthetic resin composite material with a four-layer structure by utilizing various fibers: glass fiber, aramid fiber and silicon carbide fiber are used as fillers to form a structure with a framework sandwich; filling a skeleton with slurry formed by polyacrylate, calcium stearate, polyamide-imide copolymer and an organosilicon defoamer, and finally curing and crosslinking by using epoxy resin and the polyamide-imide copolymer, wherein the rigidity and hardness of the filler physical structure are modified, and the toughness and flexibility of the polyamide-imide copolymer are modified by using the polyacrylate, the organosilicon defoamer and the epoxy resin, so that the prepared synthetic resin has the characteristic of high strength;
2. the polyamide-imide copolymer produced by the invention does not need additional filtration and purification processes;
3. the polyacrylate and the organosilicon defoamer in the formed slurry have a siloxane structure, have high viscosity, high strength and high abrasion resistance, and also have excellent heat conduction and high temperature resistance, calcium stearate and polyamide imide can be tightly bonded, and simultaneously the slurry can quickly transfer the high temperature of the aramid fiber layer to the skeleton and the bottom aramid fiber layer during reaction, and the applied external force can be quickly connected and diffused,
4. the added epoxy resin and polyamide imide are crosslinked and cured, and the organic silicon defoamer and the ultrasonic vibration method reduce the influence of bubbles formed in the reaction on the resin performance in sequence, so that the synthetic resin structure is more compact.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention.
Unless otherwise indicated, the examples and comparative examples are parallel tests of the same components, component contents, preparation steps, preparation parameters, and the experimental methods in the following examples are conventional methods unless otherwise specified; the test materials used in the examples described below, unless otherwise specified, were purchased from commercial sources.
The sources of the materials mentioned in the present invention are as follows: the organosilicon defoamer is purchased from all companies of new materials research in Dongguan City, the content is 99%, and the model is DU-159; the epoxy resin was bisphenol A type epoxy resin (product name NPEL-127L) purchased from New Material Co., ltd.
All reagents were used as received without further purification unless otherwise indicated. The flask was equipped with a mechanical stirrer, nitrogen inlet and reflux condenser. The N, N-dimethylacetamide and gamma-butyrolactone are all chromatographic pure reagent grade, and other reagents are all analytically pure unless specified. All of the 4,4'- (hexafluoroisopropylidene) diphthalic anhydride, 4' - (hexafluoroisopropylidene) diphthalic anhydride and terephthaloyl chloride used were placed in the reaction vessel in powder form at one time in each step to avoid contact with air as much as possible.
The fineness of the aramid fiber is 1000D-2000D; in the aramid fiber layer, gaps between the aramid fibers are smaller than 50 mu m.
In the preparation examples and examples of the present invention, the "parts" are parts by weight unless otherwise specified.
Example 1
50 parts of N, N-dimethylacetamide, 3.6 parts of 2,2 '-bis (trifluoromethyl) benzidine and 1.8 parts of 4,4' - (hexafluoroisopropylidene) diphthalic anhydride were added to the flask under a nitrogen flow at room temperature, and the mixture was stirred for 2 hours. After immersing the flask in an ice bath to cool to 0 ℃, 1.62 parts of terephthaloyl chloride was added and stirred for 10 minutes. 6 parts of N, N-dimethylacetamide are added and stirred for 3 hours while the ambient temperature is brought to room temperature. 1.18 parts of pyridine and 0.43 part of acetic anhydride are then added, stirred at room temperature for 30 minutes, and heated to 70℃and stirred for a further 60 minutes. After cooling to room temperature, 1.74 parts of propylene oxide was added and stirred for 12 hours to obtain a polyamideimide copolymer solution.
1 part of initiator azodiisoheptanenitrile is added into 100 parts of toluene and 40 parts of dimethylbenzene, 20 parts of methyl methacrylate, 20 parts of ethyl methacrylate, 60 parts of butyl acrylate and 80 parts of octyl acrylate are sequentially added, the reaction is carried out for 10 hours at 70 ℃, and then 6 parts of vinyl trimethoxysilane is added, so that the polyacrylate containing a siloxane structure can be obtained.
Weaving 13 parts of glass fiber bundles and 15 parts of silicon carbide fiber bundles respectively serving as warp yarns and weft yarns to prepare the fiber with the surface density of 140g/m 2 Forming a skeleton structure after knitting is completed; coating an aramid fiber layer on the lower surface of the framework structure, and spraying slurry on the upper surface of the framework structure; the sizing agent is as follows: 20 parts of polyacrylate containing a siloxane structure is ground to 10-15 mu m, 5 parts of calcium stearate is ground to 10-15 mu m, placed in 40 parts of polyamideimide copolymer solution, and then prepared into a suspension by ultrasonic dispersion. And (3) drying after the spraying is finished, discharging air in the skeleton structure through ultrasonic oscillation after the drying is finished, and coating an aramid fiber layer on the upper surface after the discharging is finished to obtain a semi-finished product. And (3) delivering 30 parts of the semi-finished product into a rolling device, spraying 60 parts of atomized epoxy resin at 140 ℃ and in a vacuum state, rolling and pressing, and curing for 3 hours at 240 ℃ after pressing to obtain the high-strength fiber-reinforced synthetic resin composite material.
The rolling device includes: the device comprises an encapsulation vacuum cavity, a compression roller group, an infrared radiation temperature regulation group, a temperature monitoring group, an epoxy resin heating tank, an epoxy resin pump, a heat-insulation epoxy resin conduit, an epoxy resin atomizing nozzle and a rolling process control processor; the outer layer of the rolling device is covered with the sealed vacuum chamber, the sealed vacuum chamber is vacuumized by a vacuum pump, the material inlet and outlet are opened when the material is fed and discharged, the material inlet and outlet are closed after the feeding and discharging are completed, and sealing strips are arranged at the edges of the material inlet and outlet and the edges of the material contact edges; the infrared radiation temperature regulation group includes: preheating an infrared radiation source and curing and heating the infrared radiation source for the semi-finished product; the temperature monitoring group monitors the temperature of the semi-finished product, the temperature of the epoxy resin and the curing temperature after lamination through a first temperature sensor, a second temperature sensor and a third temperature sensor respectively; the temperature monitoring group temperature signal is fed back to the rolling process control processor; the rolling process control processor controls the infrared radiation intensity of the infrared radiation temperature adjusting group and the heating of the epoxy resin heating tank according to the temperature signal of the temperature monitoring group, and adjusts the preheating temperature of the semi-finished product, the epoxy resin temperature and the curing temperature after pressing; the epoxy resin heating tank is communicated with an epoxy resin pump through a heat-insulating epoxy resin conduit, and the epoxy resin pump is communicated with an epoxy resin atomizing nozzle through the heat-insulating epoxy resin conduit; the insulating epoxy resin conduit comprises: the catheter comprises a catheter outer heat insulation layer, a catheter anti-folding protection layer and a catheter inner layer; the outer heat-insulating layer of the catheter is made of flexible heat-insulating materials and is wrapped outside the anti-folding protective layer of the catheter; the inner layer of the conduit is an oxidation-resistant surface passivation copper pipe; the catheter anti-folding protective layer is a stainless steel wire woven net and is wrapped outside the inner wall of the catheter; the flexible thermal insulation material comprises: diene foam, hydrocarbon foam elastomer or nitrile rubber foam;
more accurate temperature control can be performed; the vacuum degree in the rolling process is higher by fully sealing and wrapping the sealed vacuum cavity; the epoxy resin atomization is more precise in temperature and more accurate, so that the temperature loss of the epoxy resin conduit in the conveying temperature and the temperature difference in the atomization spraying process are greatly reduced;
vacuumizing through a vacuum pump, and completely vacuumizing an encapsulated vacuum cavity which is fully encapsulated at the outer layer of the rolling device; preheating the semi-finished product to a semi-finished product preheating set temperature through first infrared radiation of a semi-finished product preheating infrared radiation source; heating the epoxy resin to a first set temperature through an epoxy resin heating tank; an epoxy pump pumps and pumps the epoxy to an epoxy atomizing nozzle; spraying a preset part of atomized epoxy resin through an epoxy resin atomizing nozzle, and then sending the atomized epoxy resin into a press roller group for rolling and pressing; after the lamination, the material is sent into an infrared radiation temperature adjusting group to be laminated and then is solidified into an infrared radiation area, a third temperature sensor monitors the solidification temperature after lamination, and the laminated material is heated to a set solidification temperature through the second infrared radiation of a solidification heating infrared radiation source; solidifying the high-strength fiber reinforced synthetic resin composite material for a set solidifying time at a set solidifying temperature to obtain a high-strength fiber reinforced synthetic resin composite material; the semi-finished product preheating set temperature comprises: 140 ℃ or 160 ℃; the first set temperature includes: 142 ℃ or 162 ℃, wherein 142 ℃ is a temperature reduction compensation set temperature of the atomized epoxy resin due to the reduction of the external temperature when the preheating set temperature of the semi-finished product is 140 ℃, and the atomization temperature of the epoxy resin is kept to be not lower than 140 ℃ accurately; when the temperature of 162 ℃ is 160 ℃ of the preheating set temperature of the semi-finished product, the temperature of the atomized epoxy resin is reduced due to the external temperature, and the temperature of the atomized epoxy resin is kept to be accurately controlled to be not lower than 160 ℃;
the control of the rolling process is more accurate, the actual preheating temperature of the semi-finished product is obviously improved, and compared with the prior art that the object is difficult to heat in the full vacuum state by hot air heating or electric heating wire heating, the infrared radiation heating is more suitable for the accurate heating in the full vacuum environment, the heating efficiency and the heating accuracy of the vacuum environment are greatly improved, and the constant temperature degree of the curing process is greatly improved; the full-closed roller vacuum cavity enables the curing process to still keep a vacuum state, avoids the influence of external air dust impurities and the like in the curing process on the curing process, and remarkably improves the cleanliness of materials in the curing process.
Example 2
45 parts of N, N-dimethylacetamide, 3 parts of 2,2 '-bis (trifluoromethyl) benzidine and 1.5 parts of 4,4' - (hexafluoroisopropylidene) diphthalic anhydride were added to the flask under a nitrogen flow at room temperature, and the mixture was stirred for 2 hours. After immersing the flask in an ice bath to cool to 0 ℃, 1.6 parts of terephthaloyl chloride was added and stirred for 8 minutes. 3 parts of N, N-dimethylacetamide are added and stirred for 2 hours while the ambient temperature is brought to room temperature. Then 1 part pyridine and 0.2 part acetic anhydride were added and stirred at room temperature for 25 minutes and further stirred at 55℃for 60 minutes. After cooling to room temperature, 1.7 parts of propylene oxide was added and stirred for 12 hours to give a polyamideimide copolymer solution.
1 part of initiator azobisisoheptonitrile is added into 80 parts of toluene and 30 parts of dimethylbenzene, 15 parts of methyl methacrylate, 15 parts of ethyl methacrylate, 15 parts of butyl acrylate and 50 parts of octyl acrylate are sequentially added, the mixture is reacted for 9 hours at 70 ℃, and then 4 parts of vinyl trimethoxysilane is added, so that the polyacrylate containing a siloxane structure can be obtained.
Weaving 13 parts of glass fiber bundles and 15 parts of silicon carbide fiber bundles respectively serving as warp yarns and weft yarns to prepare the fiber with the surface density of 140g/m 2 Forming a skeleton structure after knitting is completed; coating an aramid fiber layer on the lower surface of the framework structure, and spraying slurry on the upper surface of the framework structure; the sizing agent is as follows: 20 parts of polyacrylate containing a siloxane structure is ground to 10-15 mu m, 5 parts of calcium stearate is ground to 10-15 mu m, placed in 40 parts of polyamideimide copolymer solution, and then prepared into a suspension by ultrasonic dispersion. And (3) drying after the spraying is finished, discharging air in the skeleton structure through ultrasonic oscillation after the drying is finished, and coating an aramid fiber layer on the upper surface after the discharging is finished to obtain a semi-finished product. And (3) delivering 30 parts of the semi-finished product into a rolling device, spraying 60 parts of atomized epoxy resin at 160 ℃ under vacuum, rolling and pressing, and curing for 3 hours at 240 ℃ after pressing to obtain the high-strength fiber-reinforced synthetic resin composite material.
Example 3
55 parts of N, N-dimethylacetamide, 4 parts of 2,2 '-bis (trifluoromethyl) benzidine and 2 parts of 4,4' - (hexafluoroisopropylidene) diphthalic anhydride were added to the flask under a nitrogen flow at room temperature, and the mixture was stirred for 2 hours. After immersing the flask in an ice bath to cool to 0 ℃, 1.65 parts of terephthaloyl chloride was added and stirred for 12 minutes. 8 parts of N, N-dimethylacetamide are added and stirred for 4 hours while the ambient temperature is brought to room temperature. 1.3 parts of pyridine and 0.6 part of acetic anhydride are then added and stirred at room temperature for 40 minutes, warmed to 70℃and stirred for a further 70 minutes. After cooling to room temperature, 1.8 parts of propylene oxide was added and stirred for 12 hours to give a polyamideimide copolymer solution.
2 parts of initiator azobisisoheptonitrile is added into 120 parts of toluene and 50 parts of dimethylbenzene, 25 parts of methyl methacrylate, 25 parts of ethyl methacrylate, 70 parts of butyl acrylate and 90 parts of octyl acrylate are sequentially added, the mixture is reacted for 10 hours at 70 ℃, and then 8 parts of vinyl trimethoxy silane is added, so that the polyacrylate containing a siloxane structure can be obtained.
Weaving 13 parts of glass fiber bundles and 15 parts of silicon carbide fiber bundles respectively serving as warp yarns and weft yarns to prepare the fiber with the surface density of 140g/m 2 Forming a skeleton structure after knitting is completed; coating an aramid fiber layer on the lower surface of the framework structure, and spraying slurry on the upper surface of the framework structure; the sizing agent is as follows: 20 parts of polyacrylate containing a siloxane structure is ground to 10-15 mu m, 5 parts of calcium stearate is ground to 10-15 mu m, placed in 40 parts of polyamideimide copolymer solution, and then prepared into a suspension by ultrasonic dispersion. And (3) drying after the spraying is finished, discharging air in the skeleton structure through ultrasonic oscillation after the drying is finished, and coating an aramid fiber layer on the upper surface after the discharging is finished to obtain a semi-finished product. And (3) delivering 30 parts of the semi-finished product into a rolling device, spraying 60 parts of atomized epoxy resin under the vacuum state of 160 ℃ and 0.05MPa, rolling and pressing, wherein the pressure is 0.05MPa, and curing for 3 hours at 240 ℃ after pressing to obtain the high-strength fiber-reinforced synthetic resin composite material.
Comparative example 1 differs from example 1 in that no silicone oil defoamer was added.
Comparative example 2 differs from example 1 in that 20 parts of polyacrylate containing a siloxane structure were ground to 50-60 μm and 5 parts of calcium stearate were ground to 50-60 μm.
Comparative example 3 differs from example 1 in that 10 parts of polyacrylate containing a siloxane structure were milled to 10-15 μm and 5 parts of calcium stearate were milled to 10-15 μm.
Comparative example 4 differs from example 1 in that 30 parts of polyacrylate containing a siloxane structure were milled to 10-15 μm and 5 parts of calcium stearate were milled to 10-15 μm.
Comparative example 5 differs from example 1 in that the polyacrylate containing a siloxane structure in example 1 was replaced by an equal weight part of polyacrylate containing no siloxane structure.
Performance testing
1. Thermal weight loss (TGA) test
The cured products prepared in examples 1 to 3 and comparative example 1 were tested for thermal weight loss under air and nitrogen, respectively, under the following specific conditions: the results are shown in Table 1 with 50℃as the initial temperature, then with a 20℃/min temperature rise to 800℃and with nitrogen or air as the carrier gas at a flow rate of 20 mL/min.
TABLE 1
As can be seen from Table 1, examples 1-3 were better in thermal stability, and the higher the temperature results under the same test conditions, the better the thermal stability.
2. Other Performance test
Other tests were performed on examples 1 to 3 and comparative examples 1 to 5, and the results are shown in Table 2.
TABLE 2
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.

Claims (10)

1. A preparation method of a high-strength fiber reinforced synthetic resin composite material is characterized by comprising the following steps: the high-strength fiber reinforced synthetic resin composite material is prepared from a skeleton woven by middle glass fibers and silicon carbide fibers, slurry on the upper layer of the skeleton, an aramid fiber layer below the skeleton and an aramid fiber layer on the slurry.
2. The method of producing a high-strength fiber-reinforced synthetic resin composite material according to claim 1, wherein the preparing the slurry raw material comprises: polyacrylate, calcium stearate, polyamideimide copolymer, and silicone defoamer.
3. The method for preparing a high-strength fiber-reinforced synthetic resin composite material according to claim 1 or 2, wherein the raw materials for preparing the slurry comprise, in parts by weight, 20 parts of polyacrylate, 5 parts of calcium stearate, 40 parts of polyamideimide copolymer and 2 parts of silicone defoamer.
4. A method for preparing a high strength fiber reinforced synthetic resin composite material according to any one of claims 1 to 3, wherein preparing the polyamideimide copolymer raw material comprises: n, N-dimethylacetamide, 2 '-bis (trifluoromethyl) benzidine, 4' - (hexafluoroisopropylidene) diphthalic anhydride, terephthaloyl chloride, N-dimethylacetamide, pyridine, acetic anhydride, and propylene oxide.
5. The method for preparing a high-strength fiber-reinforced synthetic resin composite material according to any one of claims 1 to 4, wherein the preparation of the polyamideimide copolymer raw material comprises, in parts by weight: 45 to 55 parts of N, N-dimethylacetamide, 3 to 4 parts of 2,2 '-bis (trifluoromethyl) benzidine, 1.5 to 2 parts of 4,4' - (hexafluoroisopropylidene) diphthalic anhydride, 1.6 to 1.65 parts of terephthaloyl chloride, 3 to 8 parts of N, N-dimethylacetamide, 1 to 1.3 parts of pyridine, 0.2 to 0.6 part of acetic anhydride and 1.7 to 1.8 parts of propylene oxide.
6. The method for producing a high-strength fiber-reinforced synthetic resin composite material according to any one of claims 1 to 5, wherein the production of the polyacrylate raw material comprises: toluene, xylene, azobisisoheptonitrile, methyl methacrylate, ethyl methacrylate, butyl acrylate, octyl acrylate and vinyltrimethoxysilane.
7. The method for producing a high-strength fiber-reinforced synthetic resin composite material according to any one of claims 1 to 6, characterized in that: the preparation of the polyacrylate comprises the following raw materials in parts by weight: 80 to 120 parts of toluene, 30 to 50 parts of xylene, 1 to 2 parts of azodiisoheptonitrile, 15 to 25 parts of methyl methacrylate, 15 to 25 parts of ethyl methacrylate, 50 to 70 parts of butyl acrylate, 70 to 90 parts of octyl acrylate and 4 to 8 parts of vinyl trimethoxy silane.
8. The method for producing a high-strength fiber-reinforced synthetic resin composite material according to any one of claims 1 to 7, characterized in that: the framework consists of glass fiber bundles and silicon carbide fiber bundles.
9. The method for producing a high-strength fiber-reinforced synthetic resin composite material according to any one of claims 1 to 8, characterized in that: the high-strength fiber reinforced synthetic resin composite material is formed by respectively weaving glass fiber bundles and silicon carbide fiber bundles as warp yarns and weft yarns, and forming a skeleton structure after weaving; coating an aramid fiber layer on the lower surface of the framework structure, and spraying slurry on the upper surface of the framework structure; the sizing agent is as follows: placing the ground polyacrylate and calcium stearate in a polyamide-imide copolymer solution, adding an organosilicon defoamer, and preparing a suspension by ultrasonic dispersion; drying after spraying, discharging air in the skeleton structure through ultrasonic oscillation after drying, and coating an aramid fiber layer on the upper surface after discharging to obtain a semi-finished product; and (3) feeding the semi-finished product into a rolling device, spraying atomized epoxy resin at 160 ℃ under a vacuum state, rolling and pressing, and curing after pressing to obtain the high-strength fiber-reinforced synthetic resin composite material.
10. The method for producing a high-strength fiber-reinforced synthetic resin composite material according to any one of claims 1 to 9, characterized in that: and (3) curing the mixture for 3 hours at 240 ℃ after pressing, so as to obtain the high-strength fiber-reinforced synthetic resin composite material.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5100713A (en) * 1989-06-06 1992-03-31 Toray Industries, Inc. Reinforcing woven fabric and preformed material, fiber reinforced composite material and beam using it
CN107868270A (en) * 2016-09-23 2018-04-03 中国科学院化学研究所 A kind of aerogel material constructed by fiber and adhesive and its preparation method and application
US20220194863A1 (en) * 2020-07-09 2022-06-23 Nanjing University Of Aeronautics And Astronautics Hybrid woven fiber preform-reinforced composite material and preparation method thereof
CN115493455A (en) * 2022-09-27 2022-12-20 江苏领瑞新材料科技有限公司 High-strength fiber material with bulletproof function and preparation method thereof
KR20230018871A (en) * 2021-07-30 2023-02-07 주식회사 한솔케미칼 Method for preparing polyamideimide varnish and film obtained therefrom

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5100713A (en) * 1989-06-06 1992-03-31 Toray Industries, Inc. Reinforcing woven fabric and preformed material, fiber reinforced composite material and beam using it
CN107868270A (en) * 2016-09-23 2018-04-03 中国科学院化学研究所 A kind of aerogel material constructed by fiber and adhesive and its preparation method and application
US20220194863A1 (en) * 2020-07-09 2022-06-23 Nanjing University Of Aeronautics And Astronautics Hybrid woven fiber preform-reinforced composite material and preparation method thereof
KR20230018871A (en) * 2021-07-30 2023-02-07 주식회사 한솔케미칼 Method for preparing polyamideimide varnish and film obtained therefrom
CN115493455A (en) * 2022-09-27 2022-12-20 江苏领瑞新材料科技有限公司 High-strength fiber material with bulletproof function and preparation method thereof

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