CN115260715A - High-strength fiber reinforced composite material for connecting piece and preparation method thereof - Google Patents

High-strength fiber reinforced composite material for connecting piece and preparation method thereof Download PDF

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CN115260715A
CN115260715A CN202211069372.0A CN202211069372A CN115260715A CN 115260715 A CN115260715 A CN 115260715A CN 202211069372 A CN202211069372 A CN 202211069372A CN 115260715 A CN115260715 A CN 115260715A
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composite material
reinforced composite
strength fiber
fiber
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熊进凤
刘程林
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Nanjing Sibeier Composite Material Yizheng Co ltd
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Nanjing Sibeier Composite Material Yizheng Co ltd
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Abstract

The invention provides a high-strength fiber reinforced composite material for connecting pieces and a preparation method thereof, wherein the high-strength fiber reinforced composite material is prepared from the following raw materials in parts by weight: 15-25 parts of glass fiber, 4-7 parts of waste polyaromatic oxadiazole fiber, 1-2 parts of coupling agent, 5-8 parts of sulfonated polybenzoxazole, 60-70 parts of PBT resin, 1-3 parts of graphene oxide fiber, 0.5-1.5 parts of compatilizer, 0.3-0.8 part of antioxidant, 1-3 parts of m-fluorobenzyl chloride ionized 4,4' -bis (N, N-dimethylamino) benzophenone, 1-2 parts of phosphorus pentoxide, 0.3-0.6 part of polyphosphoric acid and 10-15 parts of N-vinylcarbazole/2-acrylamide-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethylacrylate copolymer. The high-strength fiber reinforced composite material for the connecting piece disclosed by the invention is good in mechanical property, good in weather resistance and flame retardance and excellent in performance stability.

Description

High-strength fiber reinforced composite material for connecting piece and preparation method thereof
Technical Field
The invention relates to the technical field of composite materials, in particular to a high-strength fiber reinforced composite material for a connecting piece and a preparation method thereof.
Background
In recent years, with the promotion of global industrialization process, the mechanical equipment field is rapidly developed, the performance requirement on the connecting piece is driven to be higher and higher, and the market demand is larger and larger. The connecting piece is often used for connecting soft or hard pipelines and is manufactured by adopting iron castings or stainless steel, but the connecting piece has heavy weight and has inconvenience in manufacturing and installation, and although some existing connecting pieces are manufactured by adopting aluminum alloy, the existing connecting pieces have higher cost generally, and have certain difference in mechanical strength compared with the connecting pieces manufactured by the iron castings or the stainless steel, so that the large-scale application cannot be realized. In this situation, the high-strength fiber reinforced composite material for the connecting member has come to be used, and the emergence of the high-strength fiber reinforced composite material has attracted people's attention.
The high-strength fiber reinforced composite material for the connecting piece is usually formed by taking high-strength glass fibers as a reinforcing material, synthetic resin, an auxiliary agent and the like as a base material and performing pultrusion traction forming, has the excellent characteristics of light weight, high mechanical strength, good insulativity and corrosion resistance, good corrosion resistance and fatigue damage resistance and the like, is a mainstream trend of the development of the composite material industry in modern and future for a period of time, and has very high potential value. However, the existing high-strength fiber reinforced composite material for the connecting piece has the defects of relatively high price, poor wear resistance, mechanical properties, flame retardancy, weather resistance, environmental protection and performance stability which need to be further improved.
In order to solve the problems, patent CN104312094B discloses a novel composite material for making a connecting piece, which comprises, by weight, 4-8% of aluminum particles, 6-12% of carbon nanoparticles, 24-35% of low-viscosity polyamide, 13-25% of glass fibers, and 33-52% of epoxy resin. The connecting piece made of the composite material has the performances of mechanical strength, hardness and the like similar to those of an iron casting, the mass is reduced by 40-50%, the mechanical performance is excellent, the manufacturing and the installation are simple and convenient, the production cost is reduced, and the connecting piece is suitable for large-scale popularization. However, the weather resistance, flame retardancy and performance stability thereof are all to be further improved.
Therefore, the high-strength fiber reinforced composite material for connecting pieces with good mechanical properties, good weather resistance and flame retardance and excellent performance stability and the preparation method thereof are still needed in the field.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a high-strength fiber-reinforced composite material for connectors, which has excellent mechanical properties, good weather resistance and flame retardancy, and excellent performance stability, and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: a high-strength fiber reinforced composite material for connecting pieces is prepared from the following raw materials in parts by weight: 15-25 parts of glass fiber, 4-7 parts of waste polyaromatic oxadiazole fiber, 1-2 parts of coupling agent, 5-8 parts of sulfonated polybenzoxazole, 60-70 parts of PBT resin, 1-3 parts of graphene oxide fiber, 0.5-1.5 parts of compatilizer, 0.3-0.8 part of antioxidant, 1-3 parts of m-fluorobenzyl chloride ionized 4,4' -bis (N, N-dimethylamino) benzophenone, 1-2 parts of phosphorus pentoxide, 0.3-0.6 part of polyphosphoric acid and 10-15 parts of N-vinylcarbazole/2-acrylamide-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethylacrylate copolymer.
Preferably, the preparation method of the N-vinylcarbazole/2-acrylamido-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethyl acrylate copolymer comprises the following steps: adding N-vinylcarbazole, 2-acrylamido-2-methylpropanesulfonic acid, methylvinylsilfluorene, trifluoroethyl acrylate and an initiator into a high-boiling-point solvent, stirring and reacting at 50-65 ℃ for 3-5 hours in an inert gas atmosphere, then precipitating in water, washing the precipitated polymer with ethanol for 3-6 times, and finally drying in a vacuum drying oven at 85-95 ℃ to constant weight to obtain the N-vinylcarbazole/2-acrylamido-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethyl acrylate copolymer.
Preferably, the mass ratio of the N-vinyl carbazole to the 2-acrylamido-2-methylpropanesulfonic acid to the methylvinylsilfluorene to the trifluoroethyl acrylate to the initiator to the high-boiling-point solvent is (3-5) to (1) (0.8-1.2) to (0.06-0.09) to (20-40).
Preferably, the initiator is azobisisobutyronitrile; the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone; the inert gas is any one of nitrogen, helium, neon and argon.
Preferably, the preparation method of the m-fluorobenzyl ionized 4,4' -bis (N, N-dimethylamino) benzophenone comprises the following steps: adding m-fluorobenzyl chloride and 4,4 '-bis (N, N-dimethylamino) benzophenone into dimethyl sulfoxide, stirring and reacting for 4-6 hours at 70-80 ℃, then performing rotary evaporation to remove the dimethyl sulfoxide, washing with diethyl ether for 3-6 times, and then performing rotary evaporation to remove the diethyl ether to obtain the m-fluorobenzyl chloride ionized 4,4' -bis (N, N-dimethylamino) benzophenone.
Preferably, the molar ratio of the m-fluorobenzyl fluoride to the 4,4' -bis (N, N-dimethylamino) benzophenone to the dimethyl sulfoxide is 2.
Preferably, the antioxidant is at least one of antioxidant 9228, antioxidant 168, antioxidant 1010, antioxidant 1098 and antioxidant 1076.
Preferably, the compatilizer is at least one of PP-g-MAH, PE-g-MAH and EVA-g-MAH.
Preferably, the PBT resin is a high molecular weight PBT Celanex of tacona 1700A, usa.
Preferably, the source of the sulfonated polybenzoxazole is not particularly limited, and in one embodiment of the present invention, the sulfonated polybenzoxazole is prepared by the method of example 3 in patent CN 200410024691.5.
Preferably, the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
Preferably, the glass fiber is alkali-free chopped glass fiber, the diameter of each monofilament is 7-11 microns, and the length of each monofilament is 3-4.5 millimeters; the average diameter of the graphene oxide fiber is 3-9 μm, and the length-diameter ratio is (20-30): 1; the waste polyaryloxadiazole fiber is a waste product of polyester staple fiber; the average diameter is 5-10 μm and the length is 3-5mm.
Another object of the present invention is to provide a method for preparing a high-strength fiber-reinforced composite material for a connector, comprising the steps of: adding the raw materials into a high-speed stirrer according to the parts by weight, uniformly mixing, adding the mixture into a double-screw extruder, extruding and molding, soaking the mixture in water at the temperature of 50-70 ℃ for 8-10 hours, and drying the mixture in a vacuum drying oven at the temperature of 85-95 ℃ to constant weight to obtain the high-strength fiber reinforced composite material for the connecting piece.
Preferably, the extrusion molding temperature is 240-270 ℃, and the main screw rotating speed of the double-screw extruder is 120-220r/min.
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation method of the high-strength fiber reinforced composite material for the connecting piece, disclosed by the invention, can be realized by adopting a traditional extrusion molding process without complex process steps and flows and special equipment, so that the investment is low, the preparation efficiency and the finished product qualification rate are high, and the preparation method is suitable for industrial continuous production.
(2) The invention discloses a high-strength fiber reinforced composite material for connecting pieces, which adopts glass fibers, waste polyaromatic oxadiazole fibers and graphene oxide fibers as reinforcing fillers together, the glass fibers, the waste polyaromatic oxadiazole fibers and the graphene oxide fibers are matched with each other, the mechanical property and the wear resistance of the composite material can be better improved under the combined action, the compatibility between the graphene oxide fibers and a material resin substrate can be improved under the combined action of more active groups and a coupling agent, the waste polyaromatic oxadiazole fibers belong to organic fibers, the compatibility between the waste polyaromatic oxadiazole fibers and the resin substrate is good, the waste polyaromatic oxadiazole fibers belong to the recycling of wastes, and the waste polyaromatic oxadiazole fibers, the social value and the ecological value are high.
(3) The high-strength fiber reinforced composite material for the connecting piece disclosed by the invention takes PBT resin as a base material, and is supplemented with N-vinylcarbazole/2-acrylamide-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethyl acrylate copolymer and sulfonated polybenzoxazole, so that the final product combines the advantages of the PBT resin and the acrylamide-2-methylpropanesulfonic acid copolymer, and has excellent mechanical properties, weather resistance, flame retardance and performance stability.
(4) The high-strength fiber reinforced composite material for the connecting piece disclosed by the invention has the advantages that the sulfonic groups contained on the N-vinylcarbazole/2-acrylamide-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethylacrylate copolymer and the sulfonated polybenzoxazole can perform chemical reaction with the benzene ring in the molecular structure of the PBT resin under the catalytic action of phosphorus pentoxide and polyphosphoric acid, and can also perform ion exchange reaction with the quaternary ammonium salt in the molecular structure of m-fluorobenzyl chloride ionized 4,4' -bis (N, N-dimethylamino) benzophenone so as to form an interpenetrating network structure, so that the physical property and the performance stability of the material are effectively improved; the mechanical property, the weather resistance, the flame retardance and the performance stability of the final product are further improved.
(5) The high-strength fiber reinforced composite material for the connecting piece disclosed by the invention has the advantages that by reasonably selecting the raw materials and the proportion thereof, carbazole, amide, sulfonyl, silicon fluorenyl, fluorine-containing group, benzoxazolyl and ester structures are simultaneously introduced into the molecular structure of the material, and under the multiple actions of electronic effect, steric hindrance effect and conjugation effect, the prepared composite material has more excellent mechanical property, weather resistance, flame retardance and performance stability.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the following provides a detailed description of the product of the present invention with reference to the examples.
The sulfonated polybenzoxazole in the examples of the present invention is prepared by the method of example 3 in patent CN 200410024691.5.
Example 1
A high-strength fiber reinforced composite material for connecting pieces is prepared from the following raw materials in parts by weight: 15 parts of glass fiber, 4 parts of waste polyaromatic oxadiazole fiber, 1 part of coupling agent, 5 parts of sulfonated polybenzoxazole, 60 parts of PBT resin, 1 part of graphene oxide fiber, 0.5 part of compatilizer, 0.3 part of antioxidant, 1 part of m-fluorobenzyl chloride ionized 4,4' -bis (N, N-dimethylamino) benzophenone, 1 part of phosphorus pentoxide, 0.3 part of polyphosphoric acid, and 10 parts of N-vinylcarbazole/2-acrylamide-2-methylpropanesulfonic acid/methyl vinyl silafluorene/trifluoroethyl acrylate copolymer.
The preparation method of the N-vinylcarbazole/2-acrylamide-2-methylpropanesulfonic acid/methyl vinyl silafluorene/trifluoroethyl acrylate copolymer comprises the following steps: adding N-vinylcarbazole, 2-acrylamido-2-methylpropanesulfonic acid, methylvinylsilfluorene, trifluoroethyl acrylate and an initiator into a high-boiling-point solvent, stirring and reacting for 3 hours at 50 ℃ in an inert gas atmosphere, then precipitating in water, washing the precipitated polymer for 3 times by using ethanol, and finally drying in a vacuum drying oven at 85 ℃ to constant weight to obtain an N-vinylcarbazole/2-acrylamido-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethyl acrylate copolymer; the mass ratio of the N-vinylcarbazole, the 2-acrylamido-2-methylpropanesulfonic acid, the methylvinylsilfluorene, the trifluoroethyl acrylate, the initiator and the high-boiling point solvent is (3); the initiator is azobisisobutyronitrile; the high boiling point solvent is dimethyl sulfoxide; the inert gas is nitrogen; the M of the copolymer was determined by GPC testing, U.S. Waters 515-2410 n ＝14136g/mol，M W /M n =1.317; elemental analysis proves that the mass ratio of the structural units N-vinylcarbazole, 2-acrylamido-2-methylpropanesulfonic acid, methylvinylsilfluorene and trifluoroethyl acrylate in the copolymer is the same as the theoretical value.
The preparation method of the m-fluorobenzyl ionized 4,4' -bis (N, N-dimethylamino) benzophenone comprises the following steps: adding m-fluorobenzyl chloride and 4,4 '-bis (N, N-dimethylamino) benzophenone into dimethyl sulfoxide, stirring and reacting for 4 hours at 70 ℃, then performing rotary evaporation to remove the dimethyl sulfoxide, washing with diethyl ether for 3 times, and performing rotary evaporation to remove the diethyl ether to obtain m-fluorobenzyl ionized 4,4' -bis (N, N-dimethylamino) benzophenone; the mol ratio of m-fluorobenzyl, 4' -bis (N, N-dimethylamino) benzophenone to dimethyl sulfoxide is 2; the product is dispersed in silver nitrate aqueous solution with the mass fraction of 15%, white precipitate is generated, and the product is proved to contain a chloride ion structure, so that ionization is realized; the molar ratio of m-fluorobenzyl fluoride and 4,4' -bis (N, N-dimethylamino) benzophenone participating in the reaction was confirmed to be 2.
The antioxidant is 9228; the compatilizer is PP-g-MAH; the PBT resin is American Tycona 1700A high molecular weight PBT Celanex; the coupling agent is a silane coupling agent KH550; the glass fiber is alkali-free chopped glass fiber, the diameter of a monofilament is 7 micrometers, and the length of the monofilament is 3 millimeters; the average diameter of the graphene oxide fiber is 3 μm, and the length-diameter ratio is 20; the waste polyaryloxadiazole fiber is a waste product of polyester staple fiber; the average diameter was 5 μm and the length was 3mm.
A preparation method of the high-strength fiber reinforced composite material for the connecting piece comprises the following steps: adding the raw materials into a high-speed stirrer according to the parts by weight, uniformly mixing, adding the mixture into a double-screw extruder, extruding and molding, soaking the mixture in water at the temperature of 50 ℃ for 8 hours, and then placing the mixture in a vacuum drying oven to dry the mixture to constant weight at the temperature of 85 ℃ to obtain a high-strength fiber reinforced composite material for a connecting piece; the extrusion molding temperature is 240-270 ℃, and the main screw rotating speed of the double-screw extruder is 120r/min.
Example 2
A high-strength fiber reinforced composite material for connecting pieces is prepared from the following raw materials in parts by weight: 17 parts of glass fiber, 5 parts of waste polyaromatic oxadiazole fiber, 1.2 parts of coupling agent, 6 parts of sulfonated polybenzoxazole, 63 parts of PBT resin, 1.5 parts of graphene oxide fiber, 0.7 part of compatilizer, 0.5 part of antioxidant, 1.5 parts of m-fluorobenzyl ionized 4,4' -bis (N, N-dimethylamino) benzophenone, 1.2 parts of phosphorus pentoxide, 0.4 part of polyphosphoric acid and 12 parts of N-vinylcarbazole/2-acrylamide-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethylacrylate copolymer.
The preparation method of the N-vinylcarbazole/2-acrylamide-2-methylpropanesulfonic acid/methyl vinyl silafluorene/trifluoroethyl acrylate copolymer comprises the following steps: adding N-vinylcarbazole, 2-acrylamido-2-methylpropanesulfonic acid, methylvinylsilfluorene, trifluoroethyl acrylate and an initiator into a high-boiling-point solvent, stirring and reacting for 3.5 hours at 55 ℃ in an inert gas atmosphere, then precipitating in water, washing the precipitated polymer for 4 times by using ethanol, and finally drying in a vacuum drying oven at 87 ℃ to constant weight to obtain an N-vinylcarbazole/2-acrylamido-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethyl acrylate copolymer; the mass ratio of the N-vinyl carbazole to the 2-acrylamido-2-methylpropanesulfonic acid to the methylvinylsilfluorene to the trifluoroethyl acrylate to the initiator to the high-boiling-point solvent is 3.5; the initiator is azobisisobutyronitrile; the high boiling point solvent is N, N-dimethylformamide; the inert gas is helium.
The preparation method of the m-fluorobenzyl ionized 4,4' -bis (N, N-dimethylamino) benzophenone comprises the following steps: adding m-fluorobenzyl chloride and 4,4 '-bis (N, N-dimethylamino) benzophenone into dimethyl sulfoxide, stirring and reacting for 4.5 hours at 73 ℃, then performing rotary evaporation to remove the dimethyl sulfoxide, washing with diethyl ether for 4 times, and performing rotary evaporation to remove the diethyl ether to obtain m-fluorobenzyl ionized 4,4' -bis (N, N-dimethylamino) benzophenone; the molar ratio of m-fluorobenzyl, 4' -bis (N, N-dimethylamino) benzophenone and dimethyl sulfoxide is (2).
The antioxidant is antioxidant 168; the compatilizer is PE-g-MAH; the PBT resin is American Tycona 1700A high molecular weight PBT Celanex; the coupling agent is a silane coupling agent KH560; the glass fiber is alkali-free chopped glass fiber, the diameter of a monofilament is 8 microns, and the length of the monofilament is 3.5 millimeters; the graphene oxide fibers have an average diameter of 5 μm and an aspect ratio of 23; the waste polyaryloxadiazole fiber is a waste product of polyester staple fiber; the average diameter was 6.5 μm and the length was 3.5mm.
A preparation method of the high-strength fiber reinforced composite material for the connecting piece comprises the following steps: adding the raw materials into a high-speed stirrer according to the parts by weight, uniformly mixing, adding the mixture into a double-screw extruder, extruding and molding, soaking the mixture in water at the temperature of 55 ℃ for 8.5 hours, and drying the mixture in a vacuum drying oven at the temperature of 88 ℃ to constant weight to obtain a high-strength fiber reinforced composite material for a connecting piece; the extrusion molding temperature is 240-270 ℃, and the main screw rotating speed of the double-screw extruder is 150r/min.
Example 3
A high-strength fiber reinforced composite material for connecting pieces is prepared from the following raw materials in parts by weight: 20 parts of glass fiber, 5.5 parts of waste polyaromatic oxadiazole fiber, 1.5 parts of coupling agent, 6.5 parts of sulfonated polybenzoxazole, 65 parts of PBT resin, 2 parts of graphene oxide fiber, 1 part of compatilizer, 0.6 part of antioxidant, 2 parts of m-fluorobenzyl chloride ionized 4,4' -bis (N, N-dimethylamino) benzophenone, 1.5 parts of phosphorus pentoxide, 0.45 part of polyphosphoric acid and 13 parts of N-vinylcarbazole/2-acrylamide-2-methylpropanesulfonic acid/methylvinylsilfluorene/acrylic acid trifluoroethyl ester copolymer.
The preparation method of the N-vinylcarbazole/2-acrylamide-2-methylpropanesulfonic acid/methyl vinyl silafluorene/trifluoroethyl acrylate copolymer comprises the following steps: adding N-vinylcarbazole, 2-acrylamido-2-methylpropanesulfonic acid, methylvinylsilfluorene, trifluoroethyl acrylate and an initiator into a high-boiling-point solvent, stirring and reacting for 4 hours at 58 ℃ in an inert gas atmosphere, then precipitating in water, washing the precipitated polymer for 5 times by using ethanol, and finally drying in a vacuum drying oven at 90 ℃ to constant weight to obtain an N-vinylcarbazole/2-acrylamido-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethyl acrylate copolymer; the mass ratio of the N-vinyl carbazole to the 2-acrylamido-2-methylpropanesulfonic acid to the methylvinylsilfluorene to the trifluoroethyl acrylate to the initiator to the high-boiling-point solvent is 4; the initiator is azobisisobutyronitrile; the high boiling point solvent is N, N-dimethylacetamide; the inert gas is neon.
The preparation method of the m-fluorobenzyl ionized 4,4' -bis (N, N-dimethylamino) benzophenone comprises the following steps: adding m-fluorobenzyl chloride and 4,4 '-bis (N, N-dimethylamino) benzophenone into dimethyl sulfoxide, stirring and reacting for 5 hours at 75 ℃, then performing rotary evaporation to remove the dimethyl sulfoxide, washing with diethyl ether for 4 times, and then performing rotary evaporation to remove the diethyl ether to obtain m-fluorobenzyl chloride ionized 4,4' -bis (N, N-dimethylamino) benzophenone; the mol ratio of m-fluorobenzyl, 4' -bis (N, N-dimethylamino) benzophenone to dimethyl sulfoxide is 2.
The antioxidant is 1010; the compatilizer is EVA-g-MAH; the PBT resin is American Tycona 1700A high molecular weight PBT Celanex; the coupling agent is a silane coupling agent KH570; the glass fiber is alkali-free chopped glass fiber, the diameter of a monofilament is 9 micrometers, and the length of the monofilament is 4 millimeters; the graphene oxide fibers have an average diameter of 6 μm and an aspect ratio of 25; the waste polyaryl oxadiazole fibers are products obtained by discarding polyester staple fibers, the average diameter of the waste polyaryl oxadiazole fibers is 8 micrometers, and the length of the waste polyaryl oxadiazole fibers is 4mm.
A preparation method of the high-strength fiber reinforced composite material for the connecting piece comprises the following steps: adding the raw materials into a high-speed stirrer according to the parts by weight, uniformly mixing, adding the mixture into a double-screw extruder, extruding and molding, soaking the mixture in water at 60 ℃ for 9 hours, and drying the mixture in a vacuum drying oven at 90 ℃ to constant weight to obtain a high-strength fiber reinforced composite material for a connecting piece; the extrusion molding temperature is 240-270 ℃, and the main screw rotating speed of the double-screw extruder is 190r/min.
Example 4
A high-strength fiber reinforced composite material for connecting pieces is prepared from the following raw materials in parts by weight: 23 parts of glass fiber, 6.5 parts of waste polyaromatic oxadiazole fiber, 1.8 parts of coupling agent, 7.5 parts of sulfonated polybenzoxazole, 68 parts of PBT resin, 2.5 parts of graphene oxide fiber, 1.3 parts of compatilizer, 0.7 part of antioxidant, 2.5 parts of m-fluorobenzyl chloride ionized 4,4' -bis (N, N-dimethylamino) benzophenone, 1.8 parts of phosphorus pentoxide, 0.5 part of polyphosphoric acid and 14 parts of N-vinylcarbazole/2-acrylamide-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethylacrylate copolymer.
The preparation method of the N-vinylcarbazole/2-acrylamide-2-methylpropanesulfonic acid/methyl vinyl silafluorene/trifluoroethyl acrylate copolymer comprises the following steps: adding N-vinylcarbazole, 2-acrylamido-2-methylpropanesulfonic acid, methylvinylsilfluorene, trifluoroethyl acrylate and an initiator into a high-boiling-point solvent, stirring and reacting for 4.5 hours at 63 ℃ in an inert gas atmosphere, then precipitating in water, washing the precipitated polymer for 6 times by using ethanol, and finally drying in a vacuum drying oven at 93 ℃ to constant weight to obtain an N-vinylcarbazole/2-acrylamido-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethyl acrylate copolymer; the mass ratio of the N-vinyl carbazole to the 2-acrylamido-2-methylpropanesulfonic acid to the methylvinylsilfluorene to the trifluoroethyl acrylate to the initiator to the high-boiling-point solvent is 4.5; the initiator is azobisisobutyronitrile; the high boiling point solvent is a mixture formed by mixing dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone according to a mass ratio of 1; the inert gas is nitrogen.
The preparation method of the m-fluorobenzyl ionized 4,4' -bis (N, N-dimethylamino) benzophenone comprises the following steps: adding m-fluorobenzyl chloride and 4,4 '-bis (N, N-dimethylamino) benzophenone into dimethyl sulfoxide, stirring and reacting for 5.5 hours at 78 ℃, then performing rotary evaporation to remove the dimethyl sulfoxide, washing with diethyl ether for 5 times, and then performing rotary evaporation to remove the diethyl ether to obtain m-fluorobenzyl chloride ionized 4,4' -bis (N, N-dimethylamino) benzophenone; the molar ratio of m-fluorobenzyl, 4' -bis (N, N-dimethylamino) benzophenone to dimethyl sulfoxide is 2.
The antioxidant is an antioxidant 1076; the compatilizer is PP-g-MAH; the PBT resin is American Tycona 1700A high molecular weight PBT Celanex; the coupling agent is a silane coupling agent KH560; the glass fiber is alkali-free chopped glass fiber, the diameter of each monofilament is 10 micrometers, and the length of each monofilament is 4.3 millimeters; the graphene oxide fibers have an average diameter of 8 μm and an aspect ratio of 28; the waste polyaromatic oxadiazole fiber is a product obtained by discarding a polyester staple fiber; the average diameter was 9 μm and the length was 4.5mm.
A preparation method of the high-strength fiber reinforced composite material for the connecting piece comprises the following steps: adding the raw materials into a high-speed stirrer according to the parts by weight, uniformly mixing, adding the mixture into a double-screw extruder, extruding and molding, soaking the mixture in 65 ℃ water for 9.5 hours, and then placing the mixture in a vacuum drying oven for drying at 93 ℃ to constant weight to obtain a high-strength fiber reinforced composite material for a connecting piece; the extrusion molding temperature is 240-270 ℃, and the main screw rotating speed of the double-screw extruder is 210r/min.
Example 5
A high-strength fiber reinforced composite material for connecting pieces is prepared from the following raw materials in parts by weight: 25 parts of glass fiber, 7 parts of waste polyaromatic oxadiazole fiber, 2 parts of coupling agent, 8 parts of sulfonated polybenzoxazole, 70 parts of PBT resin, 3 parts of graphene oxide fiber, 1.5 parts of compatilizer, 0.8 part of antioxidant, 3 parts of m-fluorobenzyl chloride ionized 4,4' -bis (N, N-dimethylamino) benzophenone, 2 parts of phosphorus pentoxide, 0.6 part of polyphosphoric acid and 15 parts of N-vinylcarbazole/2-acrylamide-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethylacrylate copolymer.
The preparation method of the N-vinylcarbazole/2-acrylamide-2-methylpropanesulfonic acid/methyl vinyl silafluorene/trifluoroethyl acrylate copolymer comprises the following steps: adding N-vinylcarbazole, 2-acrylamido-2-methylpropanesulfonic acid, methylvinylsilfluorene, trifluoroethyl acrylate and an initiator into a high-boiling-point solvent, stirring and reacting for 5 hours at 65 ℃ in an inert gas atmosphere, then precipitating in water, washing the precipitated polymer for 6 times by using ethanol, and finally drying in a vacuum drying oven at 95 ℃ to constant weight to obtain an N-vinylcarbazole/2-acrylamido-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethyl acrylate copolymer; the mass ratio of the N-vinyl carbazole to the 2-acrylamido-2-methylpropanesulfonic acid to the methylvinylsilfluorene to the trifluoroethyl acrylate to the initiator to the high-boiling-point solvent is 5; the initiator is azobisisobutyronitrile; the high boiling point solvent is N-methyl pyrrolidone; the inert gas is nitrogen.
The preparation method of the m-fluorobenzyl ionized 4,4' -bis (N, N-dimethylamino) benzophenone comprises the following steps: adding m-fluorobenzyl chloride and 4,4 '-bis (N, N-dimethylamino) benzophenone into dimethyl sulfoxide, stirring and reacting for 6 hours at 80 ℃, then performing rotary evaporation to remove the dimethyl sulfoxide, washing with diethyl ether for 6 times, and performing rotary evaporation to remove the diethyl ether to obtain the m-fluorobenzyl ionized 4,4' -bis (N, N-dimethylamino) benzophenone; the molar ratio of m-fluorobenzyl, 4' -bis (N, N-dimethylamino) benzophenone to dimethyl sulfoxide is 2.
The antioxidant is an antioxidant 1076; the compatilizer is PP-g-MAH; the PBT resin is American Tycona 1700A high molecular weight PBT Celanex; the coupling agent is a silane coupling agent KH550; the glass fiber is alkali-free chopped glass fiber, the diameter of a monofilament is 11 micrometers, and the length of the monofilament is 4.5 millimeters; the graphene oxide fibers have an average diameter of 9 μm and an aspect ratio of 30; the waste polyaryloxadiazole fiber is a waste product of polyester staple fiber; the average diameter was 10 μm and the length was 5mm.
A preparation method of the high-strength fiber reinforced composite material for the connecting piece comprises the following steps: adding the raw materials into a high-speed stirrer according to the parts by weight, uniformly mixing, adding the mixture into a double-screw extruder, extruding and molding, soaking the mixture in 70 ℃ water for 10 hours, and then placing the mixture in a vacuum drying oven to dry the mixture to constant weight at 95 ℃ to obtain a high-strength fiber reinforced composite material for a connecting piece; the extrusion molding temperature is 240-270 ℃, and the main screw rotating speed of the double-screw extruder is 220r/min.
Comparative example 1
A high strength fiber reinforced composite for connectors, substantially the same as in example 1, except that no sulfonated polybenzoxazole was added and glass fibers were used in place of the waste polyaryloxadiazole fibers.
Comparative example 2
A high-strength fiber-reinforced composite material for connectors, which is substantially the same as in example 1, except that m-fluorobenzyl chloride was not added to ionize 4,4' -bis (N, N-dimethylamino) benzophenone, and glass fibers were used instead of the graphene oxide fibers.
To further illustrate the unexpected positive technical effects achieved by the products of the embodiments of the present invention, the high strength fiber reinforced composite material for connectors made in the embodiments of the present invention was subjected to the related performance tests, the test results are shown in table 1, and the test methods are as follows:
(1) Tensile strength: the test was carried out according to the standard GB/T1447-2005.
(2) Weather resistance: in a constant-humidity hot box, the humidity is set to be 85 percent, the temperature is set to be 60 ℃, the tensile strength is tested after the storage for 30 days, the retention rate of the tensile strength is calculated by taking the initial tensile strength as 100 percent, and the larger the value is, the better the weather resistance is.
(3) Flame retardancy: the flame retardant performance is tested according to UL94 standard.
As can be seen from table 1, the high-strength fiber-reinforced composite material for connecting members disclosed in the examples of the present invention has more excellent tensile properties, weather resistance and flame retardancy than the comparative example product.
TABLE 1
Item Tensile strength Weather resistance Flame retardancy
Unit of MPa ％ Stage
Example 1 188 98.87 V-0
Example 2 192 99.15 V-0
Example 3 198 99.40 V-0
Example 4 208 99.57 V-0
Example 5 213 99.89 V-0
Comparative example 1 155 95.76 V-2
Comparative example 2 162 93.21 V-1
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those of ordinary skill in the art can readily practice the present invention as described herein; however, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention; meanwhile, any equivalent changes, modifications and evolutions made to the above embodiments according to the substantial technology of the present invention are still within the protection scope of the technical solution of the present invention.

Claims (10)

1. The high-strength fiber reinforced composite material for the connecting piece is characterized by comprising the following raw materials in parts by weight: 15-25 parts of glass fiber, 4-7 parts of waste polyaromatic oxadiazole fiber, 1-2 parts of coupling agent, 5-8 parts of sulfonated polybenzoxazole, 60-70 parts of PBT resin, 1-3 parts of graphene oxide fiber, 0.5-1.5 parts of compatilizer, 0.3-0.8 part of antioxidant, 1-3 parts of m-fluorobenzyl chloride ionized 4,4' -bis (N, N-dimethylamino) benzophenone, 1-2 parts of phosphorus pentoxide, 0.3-0.6 part of polyphosphoric acid and 10-15 parts of N-vinylcarbazole/2-acrylamide-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethylacrylate copolymer.
2. The high-strength fiber-reinforced composite material for connecting pieces according to claim 1, wherein the preparation method of the N-vinylcarbazole/2-acrylamido-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethylacrylate copolymer comprises the following steps: adding N-vinylcarbazole, 2-acrylamido-2-methylpropanesulfonic acid, methylvinylsilfluorene, trifluoroethyl acrylate and an initiator into a high boiling point solvent, stirring and reacting at 50-65 ℃ for 3-5 hours in an inert gas atmosphere, then precipitating in water, washing the precipitated polymer with ethanol for 3-6 times, and finally drying in a vacuum drying oven at 85-95 ℃ to constant weight to obtain the N-vinylcarbazole/2-acrylamido-2-methylpropanesulfonic acid/methylvinylsilfluorene/trifluoroethyl acrylate copolymer.
3. The high-strength fiber reinforced composite material for connectors according to claim 2, wherein the mass ratio of the N-vinylcarbazole, the 2-acrylamido-2-methylpropanesulfonic acid, the methylvinylsilfluorene, the trifluoroethyl acrylate, the initiator and the high-boiling-point solvent is (3-5): 1, (0.8-1.2): 1, (0.06-0.09): 20-40).
4. The high-strength fiber-reinforced composite material for connectors according to claim 2, wherein the initiator is azobisisobutyronitrile; the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone; the inert gas is any one of nitrogen, helium, neon and argon.
5. The high strength fiber-reinforced composite material for connectors according to claim 1, wherein the m-fluorobenzyl chloride ionized 4,4' -bis (N, N-dimethylamino) benzophenone is prepared by a method comprising the steps of: adding m-fluorobenzyl chloride and 4,4 '-bis (N, N-dimethylamino) benzophenone into dimethyl sulfoxide, stirring and reacting for 4-6 hours at 70-80 ℃, then performing rotary evaporation to remove the dimethyl sulfoxide, washing with diethyl ether for 3-6 times, and then performing rotary evaporation to remove the diethyl ether to obtain the m-fluorobenzyl chloride ionized 4,4' -bis (N, N-dimethylamino) benzophenone.
6. The high-strength fiber-reinforced composite material for connectors according to claim 5, wherein the molar ratio of m-fluorobenzyl, 4' -bis (N, N-dimethylamino) benzophenone and dimethyl sulfoxide is 2.
7. The high-strength fiber-reinforced composite material for joints according to claim 1, wherein the antioxidant is at least one of antioxidant 9228, antioxidant 168, antioxidant 1010, antioxidant 1098, antioxidant 1076; the compatilizer is at least one of PP-g-MAH, PE-g-MAH and EVA-g-MAH; the PBT resin is American Tycona 1700A high molecular weight PBT Celanex; the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
8. The high-strength fiber-reinforced composite material for connectors according to claim 1, wherein the glass fibers are alkali-free chopped glass fibers, and the monofilaments have a diameter of 7 to 11 μm and a length of 3 to 4.5 mm; the average diameter of the graphene oxide fiber is 3-9 mu m, and the length-diameter ratio is (20-30): 1; the waste polyaryloxadiazole fiber is a waste product of polyester staple fiber; the average diameter is 5-10 μm and the length is 3-5mm.
9. A method for producing a high-strength fiber-reinforced composite material for connectors according to any one of claims 1 to 8, comprising the steps of: adding the raw materials into a high-speed stirrer according to the parts by weight, uniformly mixing, adding the mixture into a double-screw extruder, extruding and molding, soaking the mixture in water at the temperature of 50-70 ℃ for 8-10 hours, and then placing the mixture in a vacuum drying oven at the temperature of 85-95 ℃ to dry the mixture to constant weight to obtain the high-strength fiber reinforced composite material for the connecting piece.
10. The method of claim 9, wherein the extrusion temperature is 240-270 ℃ and the main screw rotation speed of the twin-screw extruder is 120-220r/min.
CN202211069372.0A 2022-09-02 2022-09-02 High-strength fiber reinforced composite material for connecting piece and preparation method thereof Pending CN115260715A (en)

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CN115821412A (en) * 2023-01-04 2023-03-21 盐城优和博新材料有限公司 Cutting-resistant ultra-high molecular weight polyethylene fiber and preparation method thereof
CN115926480B (en) * 2023-01-09 2023-09-29 江苏众成羽绒科技有限公司 Down composite thermal insulation material and preparation method thereof
CN117624851A (en) * 2023-12-15 2024-03-01 仪化东丽聚酯薄膜有限公司 High-strength polyester film and preparation method thereof
CN118388879A (en) * 2024-04-30 2024-07-26 江苏东峰电缆有限公司 Weather-resistant power cable material and preparation method thereof

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CN111234471A (en) * 2018-11-28 2020-06-05 合肥杰事杰新材料股份有限公司 PBT composite material with low linear thermal expansion coefficient and preparation method thereof
CN113861655A (en) * 2021-10-11 2021-12-31 安徽英力电子科技股份有限公司 Thermoplastic resin composite material notebook computer C shell and manufacturing process thereof
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CN117624851A (en) * 2023-12-15 2024-03-01 仪化东丽聚酯薄膜有限公司 High-strength polyester film and preparation method thereof
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Application publication date: 20221101