CN107446346B - Carbon fiber reinforced wear-resistant high-temperature nylon composite material and preparation method thereof - Google Patents
Carbon fiber reinforced wear-resistant high-temperature nylon composite material and preparation method thereof Download PDFInfo
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Abstract
A carbon fiber reinforced wear-resistant high-temperature nylon composite material comprises the following components in parts by weight: 35-85% of high-temperature nylon resin, 5-45% of carbon fiber, 5-20% of composite wear-resistant auxiliary agent and 0.2-0.6% of antioxidant, wherein the composite wear-resistant auxiliary agent is a mixed filler modified by a coupling agent, and the mixed filler is composed of a soft filler with the Mohs hardness of less than or equal to 2 and a hard filler with the Mohs hardness of more than or equal to 5. The carbon fiber reinforced wear-resistant high-temperature nylon composite material disclosed by the invention has the advantages of mechanical property, heat resistance, low friction coefficient, low wear loss and excellent comprehensive performance when being high in bearing capacity.
Description
Technical Field
The invention belongs to the technical field of high-temperature nylon materials, and particularly relates to a nylon composite material and a preparation method thereof.
Background
The high-temperature nylon resin generally refers to nylon engineering plastics with long-term use temperature of more than 150 ℃ after modification, and the main products of the current industrialization comprise aliphatic nylon PA46, semi-aromatic nylon PA4T, PA6T, PA9T, PA10T and the like. The high-temperature nylon resin has the advantages of good mechanical property, wear resistance, heat resistance, chemical resistance and the like, and the semi-aromatic high-temperature nylon resin also overcomes the defect of high water absorption of the nylon resin. The high-temperature nylon resin can be used for sliding parts such as gears, bearings, valves and the like, structural parts, fuel pipelines and the like, but if the unmodified high-temperature nylon resin is used as a wear-resistant material, particularly under the working conditions of poor lubricating conditions or large load, the high-temperature nylon resin has insufficient bearing capacity, poor self-lubricating property and large wear loss in high-speed friction, and is difficult to meet the use requirements of a self-lubricating engineering structural material with surface wear resistance and low friction property under high load for a long time. Generally, the performance of nylon resin can be improved by adding carbon fiber and wear-resisting auxiliary agent.
The carbon fiber is a high-strength high-modulus fiber with carbon content of more than 90 percent, and is a reinforcing material with excellent performance. The carbon fiber and carbon fiber composite material has the advantages of high strength, high modulus, high temperature resistance, light weight, wear resistance, creep resistance, low thermal expansion coefficient and the like, and can be widely applied to the field of composite materials. However, the surface of the carbon fiber is chemically inert, the compatibility with a thermoplastic resin matrix is poor, the carbon fiber is difficult to uniformly disperse in the matrix resin and is poor in adhesion with the matrix resin, and the comprehensive performance of the composite material is influenced.
The selection of the wear-resistant auxiliary agent plays a vital role in improving the friction coefficient of the wear-resistant material and reducing the wear loss of the wear-resistant material. It is believed that low hardness fillers, particularly those having a mohs hardness of less than 2, such as graphite, molybdenum disulfide, talc, mica, and polytetrafluoroethylene fines, reduce both the coefficient of friction of the material and the wear on mating materials. However, under a large load, when the wear-resistant materials slide relatively to the mating materials with higher hardness to rub against each other, local overheating is caused, and high temperature is caused, so that the wear-resistant materials are softened and sheared off due to the high temperature to form adhesive wear.
Patent document CN101343409B discloses a carbon fiber reinforced thermoplastic resin composite material, in which a surface-treated thermoplastic plastic such as carbon fiber reinforced nylon, polycarbonate, polyethylene terephthalate, polypropylene, and ABS is used, and polytetrafluoroethylene is added to reduce the friction coefficient, but this patent fails to solve the problem of excessive material wear at high load.
Patent document CN104744926A discloses a continuous long fiber reinforced high temperature resistant nylon composite material, which comprises the following components in parts by weight: 100 parts of high-temperature resistant nylon resin, 35-155 parts of continuous reinforced fiber, 1-15 parts of bismaleimide, 5-15 parts of compatilizer A, 1-3 parts of compatilizer B, 11-46 parts of composite reinforced antiwear agent, 10-40 parts of composite lubricating antifriction agent, 1.0-5.0 parts of processing aid and 0.1-0.5 part of curing agent. The continuous long fiber reinforced high temperature resistant nylon composite material prepared by the method has the advantages of mechanical property, high temperature resistance and size stability, but the continuous long fiber reinforced high temperature resistant nylon composite material has large fiber length, is not beneficial to reducing the friction coefficient and the abrasion of the material, and simultaneously has special requirements on forming equipment and complex process.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings in the background art, provides a carbon fiber reinforced wear-resistant high-temperature nylon composite material which has mechanical property, heat resistance and low friction coefficient and has low abrasion loss during high bearing, and correspondingly provides a preparation method thereof. In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a carbon fiber reinforced wear-resistant high-temperature nylon composite material comprises the following components in parts by weight: 35-85% of high-temperature nylon resin, 5-45% of carbon fiber, 5-20% of composite wear-resistant auxiliary agent and 0.2-0.6% of antioxidant, wherein the composite wear-resistant auxiliary agent is a mixed filler modified by a coupling agent, and the mixed filler is composed of a soft filler with the Mohs hardness of less than or equal to 2 and a hard filler with the Mohs hardness of more than or equal to 5.
In the carbon fiber reinforced wear-resistant high-temperature nylon composite material, preferably, the mass ratio of the soft filler to the hard filler is 3:1-9:1, and the mass of the coupling agent is 0.3-1% of the total mass of the soft filler and the hard filler.
In the research process, the inventor finds that the friction coefficient of the materials can be reduced and the abrasion to the mating materials can be reduced by adopting a single soft filler, but under a larger load, when the wear-resistant materials and the mating materials with higher hardness slide relatively to each other and are rubbed, local overheating can be caused, high temperature is caused, and the wear-resistant materials are softened at the high temperature and are sheared off to form adhesive abrasion. However, the inventors have found that the problem of a large abrasion loss can be solved by using a mixed filler comprising a soft filler and a hard filler at a mass ratio of 3:1 to 9:1 and treating the mixed filler with a coupling agent. The soft filler in the mixed filler treated by the coupling agent can form a stable, continuous and smooth transfer film on a friction interface in the friction process, so that the friction coefficient and the abrasion loss of the wear-resistant material can be effectively reduced; the hard filler in the mixed filler can improve the modulus, hardness and heat resistance of the wear-resistant material, mainly plays a role in bearing in the friction process, reduces adhesion, prevents the extension and thermoplastic deformation and softening of furrows and reduces the wear loss of the material, so that the mixed filler added with the coupling agent can effectively relieve the adhesion wear generated by the friction of the wear-resistant material and a mate material with higher hardness under a large load due to relative sliding, and can reduce the wear loss. However, the hard filler should not be too much, otherwise the friction coefficient of the composite material is increased, which is not beneficial to improving the comprehensive performance of the composite material.
In the carbon fiber reinforced wear-resistant high-temperature nylon composite material, preferably, the soft filler is one or more of graphite, molybdenum disulfide, talc, mica and polytetrafluoroethylene micro powder, and the hard filler is one or more of wollastonite, aluminum oxide and silicon carbide.
In the carbon fiber reinforced wear-resistant high-temperature nylon composite material, preferably, the coupling agent is one or more of a titanate coupling agent, an aluminate coupling agent and a zirconate coupling agent.
In the carbon fiber reinforced wear-resistant high-temperature nylon composite material, preferably, the high-temperature nylon resin is one or more of semi-aromatic nylon resin or semi-aromatic nylon resin copolymer with a melting point of 280-330 ℃. For example, it may be selected from polytridecylene terephthalamide (PA13T), polyterephthalamide undecamethylene (PA11T), polyterephthalamide dodecadiamine (PA12T), polyhexamethylene terephthalamide-co-polycaprolactam copolymer (PA6T/6), polyhexamethylene terephthalamide-co-polyhexamethylene adipamide copolymer (PA6T/66), and polyterephthalamide nonanediamide-co-polyhexamethylene terephthalamide copolymer (PA 9T/10T). The composite material can generate a large amount of heat under the high-pressure and high-speed friction working condition, and the material with poor heat resistance is easy to soften and is worn quickly. The matrix resin has good wear resistance, heat resistance, chemical resistance and mechanical property, and can meet the use conditions of severe working conditions such as high bearing capacity, high temperature, poor lubrication and the like.
In the carbon fiber reinforced wear-resistant high-temperature nylon composite material, preferably, the carbon fibers are PAN-based ground carbon fibers treated by a nitric acid liquid phase oxidation method, the monofilament diameter of the PAN-based ground carbon fibers is 5-8 μm, and the average fiber length is 50-200 μm. The ground carbon fiber has the advantages of uniform length distribution, excellent dispersibility and the like, can effectively improve the dispersion problem of the carbon fiber in matrix resin, improves the mechanical property and the friction property of the material, can improve the bonding force between the carbon fiber and high-temperature nylon resin by performing liquid-phase oxidation treatment before use, and has more excellent modification effect.
In the carbon fiber reinforced wear-resistant high-temperature nylon composite material, preferably, the antioxidant is a mixture of N, N-bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexamethylenediamine and tris (2, 4-tert-butylphenyl) phosphite in a weight ratio of 0.5:1-2: 1.
As a general technical concept, the invention also provides a preparation method of the carbon fiber reinforced wear-resistant high-temperature nylon composite material, which comprises the following steps:
(1) drying and uniformly mixing the soft filler and the hard filler to obtain a mixed filler, spraying a coupling agent solution on the surface of the mixed filler under stirring, and drying to obtain the composite wear-resistant auxiliary agent;
(2) putting the carbon fiber into a nitric acid solution for heating treatment, washing and drying to obtain liquid-phase oxidized carbon fiber;
(3) drying the high-temperature nylon resin, uniformly mixing the high-temperature nylon resin, the composite wear-resistant auxiliary agent and the antioxidant, adding the mixture from a main feeding port of a screw extruder, adding the carbon fiber from a side feeding port of the screw extruder, melting, extruding, cooling, granulating and drying to obtain the carbon fiber reinforced wear-resistant high-temperature nylon composite material.
In the preparation method of the carbon fiber reinforced wear-resistant high-temperature nylon composite material, preferably, the coupling agent solution is prepared by adding the coupling agent into isopropanol and keeping the mass of the isopropanol to be 10-30 times of that of the coupling agent. The isopropanol may also be replaced by an alcoholic solvent having a melting point of 60-85 ℃, but is preferably isopropanol.
In the preparation method of the carbon fiber reinforced wear-resistant high-temperature nylon composite material, the mass fraction of the nitric acid solution is preferably 30-65%, and the heating treatment condition is that the heating treatment is carried out in a water bath at the temperature of 60-80 ℃ for 0.5-3 h.
Specifically, the preparation method of the carbon fiber reinforced wear-resistant high-temperature nylon composite material comprises the following steps:
(1) placing the soft filler and the hard filler in an electric hot blast drying box, drying for 6-8h at 80-120 ℃, uniformly mixing to obtain a mixed filler, dissolving a coupling agent in isopropanol to prepare a coupling agent solution, keeping the mass of the isopropanol to be 10-30 times of that of the coupling agent, placing the mixed filler in a stirrer for stirring, spraying the coupling agent solution on the surface of the mixed filler in the stirring process for 10-20min, finally placing the mixed filler sprayed with the coupling agent solution in the electric hot blast drying box, and drying for 3-6h at 80-100 ℃ to obtain the composite wear-resistant auxiliary agent;
(2) putting carbon fibers into nitric acid with the mass fraction of 30-65%, heating in a water bath at 60-80 ℃ for 0.5-3h, washing the carbon fibers treated by the nitric acid with distilled water until the pH value of the distilled water is about 7, finally putting the carbon fibers into an oven, and drying at 75-85 ℃ for 8-12h to obtain carbon fibers subjected to liquid phase oxidation;
(3) putting the high-temperature nylon resin into an oven, drying for 4-6h at the temperature of 110-130 ℃, uniformly mixing the high-temperature nylon resin, the composite wear-resistant auxiliary agent and the antioxidant in a high-speed mixer, adding the mixture from a main feeding port of a screw extruder, adding the carbon fiber from a side feeding port of the screw extruder, keeping the extrusion temperature at 290-335 ℃, the screw rotation speed at 200-500 r/min, melting, extruding, cooling, granulating and drying to obtain the carbon fiber reinforced wear-resistant high-temperature nylon composite material.
Compared with the prior art, the invention has the advantages that:
1. the high-temperature-resistant nylon resin is used as the matrix resin of the composite material, has good wear resistance, heat resistance, chemical resistance and mechanical properties, and can meet the use conditions of severe working conditions such as high bearing capacity, high temperature, poor lubrication and the like.
2. The composite wear-resistant additive can effectively relieve the adhesive wear caused by the friction of the wear-resistant material and a mating material with higher hardness under a large load, and reduce the wear amount. In addition, the binding force between the wear-resistant auxiliary agent and matrix resin after being treated by the coupling agent is obviously improved, and the mechanical property of the material can be improved.
3. The advantages of the high-temperature-resistant nylon resin, the composite wear-resistant auxiliary agent and the carbon fiber are complementary, and the prepared carbon fiber reinforced wear-resistant high-temperature-resistant nylon composite material has mechanical property, heat resistance, low friction coefficient, low abrasion loss and excellent comprehensive performance during high bearing.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the components and the content of the carbon fiber reinforced wear-resistant high-temperature nylon composite material are shown in the following table 1, wherein the Mohs hardness of a soft filler is less than or equal to 2, the Mohs hardness of a hard filler is greater than or equal to 5, the carbon fiber is PAN-based ground carbon fiber treated by a nitric acid liquid phase oxidation method, the monofilament diameter of the PAN-based ground carbon fiber before being treated by the nitric acid liquid phase oxidation method is 7 micrometers, and the average fiber length is 100 micrometers.
The preparation method of the carbon fiber reinforced wear-resistant high-temperature nylon composite material comprises the following steps:
(1) placing a soft filler and a hard filler in an electric heating forced air drying oven, drying for 8 hours at 100 ℃, uniformly mixing to obtain a mixed filler, dissolving a coupling agent in isopropanol to prepare a coupling agent solution, keeping the mass of the isopropanol to be 20 times of that of the coupling agent, placing the mixed filler in a stirrer to stir, spraying the coupling agent solution on the surface of the mixed filler in the stirring process for 15min, finally placing the mixed filler sprayed with the coupling agent solution in the electric heating forced air drying oven, and drying for 4 hours at 90 ℃ to obtain the composite wear-resistant auxiliary agent;
(2) putting carbon fibers into nitric acid with the mass fraction of 60%, heating in a water bath at 70 ℃ for 1h, washing the carbon fibers treated by the nitric acid with distilled water until the pH value of the distilled water is about 7, and finally putting the carbon fibers into an oven to be dried at 80 ℃ for 10h to obtain carbon fibers subjected to liquid phase oxidation;
(3) putting high-temperature nylon resin into an oven, drying for 6 hours at 120 ℃, uniformly mixing the high-temperature nylon resin, the composite wear-resistant auxiliary agent and the antioxidant in a high-speed mixer, adding the mixture from a main feeding port of a screw extruder, adding carbon fiber from a side feeding port of the screw extruder, keeping the extrusion temperature at 300 ℃, controlling the rotation speed of the screw at 400r/min, melting, extruding, cooling, granulating and drying to obtain the carbon fiber reinforced wear-resistant high-temperature nylon composite material.
The carbon fiber reinforced wear-resistant high-temperature nylon composite material prepared in the embodiment is subjected to performance test, and the test results are shown in table 1 below.
Examples 2 to 4:
compared with example 1, the carbon fiber reinforced wear-resistant high-temperature nylon composite material is different in the content of the components, and the specific difference is shown in table 1 below. The preparation method of this example is the same as example 1.
Comparative examples 1 to 3:
compared with examples 1-4, the carbon fiber reinforced wear-resistant high-temperature nylon composite material is different in the content of the components, and the specific difference is shown in the following table 1.
Table 1: raw materials and performance data for examples 1-4 and comparative examples 1-3
As can be seen from the above table, the composite materials prepared in examples 1 to 4 have significantly better overall properties than the composite materials prepared in comparative examples 1 to 3, especially the abrasion resistance is significantly better.
In the above table, the tensile strength and modulus are tested according to GB/T1040-; the bending strength and the modulus are tested according to the GB/T9341 + 2008 standard, and the testing speed of the tensile strength and the modulus is 2 mm/min; the notch impact strength and the unnotched impact strength of the simply supported beam are tested according to the GB/T1043-2008 standard, the energy of a notch impact strength pendulum is 1J, and the energy of an unnotched impact strength pendulum is 7.5J; the thermal deformation temperature is tested according to GB/T1643-2004 standard, and the load is 1.8 MPa; the friction coefficient and the abrasion are tested according to the national standard GB/T3960-2016, 1250N force is applied, and the 45# steel is used as a grinding ring with the area of 125mm2。
Claims (8)
1. The carbon fiber reinforced wear-resistant high-temperature nylon composite material is characterized by comprising the following components in parts by weight: 35-85% of high-temperature nylon resin, 5-45% of carbon fiber, 5-20% of composite wear-resistant auxiliary agent and 0.2-0.6% of antioxidant, wherein the composite wear-resistant auxiliary agent is a mixed filler modified by a coupling agent, and the mixed filler is composed of a soft filler with the Mohs hardness of less than or equal to 2 and a hard filler with the Mohs hardness of more than or equal to 5;
wherein the soft filler is one or more of graphite, molybdenum disulfide, talc, mica and polytetrafluoroethylene micro powder, and the hard filler is one or more of wollastonite, aluminum oxide and silicon carbide;
the carbon fiber is PAN-based ground carbon fiber treated by a nitric acid liquid phase oxidation method, the monofilament diameter of the PAN-based ground carbon fiber is 5-8 μm, and the average fiber length is 50-200 μm;
the mass ratio of the soft filler to the hard filler is 3:1-9: 1.
2. The carbon fiber reinforced wear-resistant high-temperature nylon composite material as claimed in claim 1, wherein the mass of the coupling agent is 0.3-1% of the total mass of the soft filler and the hard filler.
3. The carbon fiber reinforced abrasion-resistant high-temperature nylon composite material according to claim 1 or 2, wherein the coupling agent is one or more of a titanate coupling agent, an aluminate coupling agent and a zirconate coupling agent.
4. The carbon fiber reinforced wear-resistant high-temperature nylon composite material as claimed in claim 1 or 2, wherein the high-temperature nylon resin is one or more of semi-aromatic nylon resin or semi-aromatic nylon resin copolymer with a melting point of 280-330 ℃.
5. The carbon fiber reinforced abrasion-resistant high-temperature nylon composite material as claimed in claim 1 or 2, wherein the antioxidant is a mixture of N, N-bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexamethylenediamine and tris (2, 4-tert-butylphenyl) phosphite in a weight ratio of 0.5:1 to 2: 1.
6. A method for preparing the carbon fiber reinforced abrasion-resistant high-temperature nylon composite material as claimed in any one of claims 1 to 5, wherein the method comprises the following steps:
(1) drying and uniformly mixing the soft filler and the hard filler to obtain a mixed filler, spraying a coupling agent solution on the surface of the mixed filler under stirring, and drying to obtain the composite wear-resistant auxiliary agent;
(2) putting the carbon fiber into a nitric acid solution for heating treatment, washing and drying to obtain liquid-phase oxidized carbon fiber;
(3) drying the high-temperature nylon resin, uniformly mixing the high-temperature nylon resin, the composite wear-resistant auxiliary agent and the antioxidant, adding the mixture from a main feeding port of a screw extruder, adding the carbon fiber from a side feeding port of the screw extruder, melting, extruding, cooling, granulating and drying to obtain the carbon fiber reinforced wear-resistant high-temperature nylon composite material.
7. The method according to claim 6, wherein the coupling agent solution is prepared by adding the coupling agent to isopropanol and maintaining the mass of the isopropanol at 10-30 times that of the coupling agent.
8. The preparation method according to claim 6, wherein the mass fraction of the nitric acid solution is 30-65%, and the heating treatment is performed in a water bath at 60-80 ℃ for 0.5-3 h.
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