CN117924934A - Modified polyimide composite material, preparation method and application thereof - Google Patents
Modified polyimide composite material, preparation method and application thereof Download PDFInfo
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- 239000004642 Polyimide Substances 0.000 title claims abstract description 96
- 229920001721 polyimide Polymers 0.000 title claims abstract description 96
- 239000002131 composite material Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000835 fiber Substances 0.000 claims abstract description 93
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 71
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 71
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 70
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 68
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 68
- 229910052582 BN Inorganic materials 0.000 claims abstract description 65
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 65
- 238000002156 mixing Methods 0.000 claims abstract description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000006229 carbon black Substances 0.000 claims abstract description 15
- 230000001050 lubricating effect Effects 0.000 claims abstract description 14
- 239000000945 filler Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000001746 injection moulding Methods 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 17
- 239000011812 mixed powder Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 8
- 238000002347 injection Methods 0.000 claims description 8
- 239000007924 injection Substances 0.000 claims description 8
- 230000004048 modification Effects 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 239000002861 polymer material Substances 0.000 abstract description 3
- 238000005461 lubrication Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 25
- 238000012360 testing method Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 229920006259 thermoplastic polyimide Polymers 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions 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 C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08L79/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The invention belongs to the technical field of high polymer materials, and in particular relates to a modified polyimide composite material, a preparation method thereof and application thereof in sealing products, wherein the modified polyimide composite material comprises the following raw material components in parts by weight: 70-80 parts of polyimide; 1-5 parts of modified polytetrafluoroethylene; 1-5 parts of graphene; 0.2-1 parts of boron nitride; 2-5 parts of white carbon black; the modified polytetrafluoroethylene is modified polytetrafluoroethylene by blending boron nitride fibers and graphene fibers, wherein the inorganic lubricating filler accounts for 8-12% of the mass of the modified polytetrafluoroethylene. The composite material prepared by the invention has the advantages of good compatibility among components, high mechanical strength, self-lubrication, corrosion resistance, wear resistance, high toughness and the like, and the preparation method is simple, quick in injection molding, easy to process and beneficial to industrial application.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a modified polyimide composite material, a preparation method and application thereof.
Background
Polyimide (PI) is a high-performance polymer material with excellent thermal stability, chemical stability, mechanical strength and electrical insulation properties. Because of its unique molecular structure and physicochemical properties, polyimide has been widely used in the fields of aerospace, electronic and electrical appliances, automobile manufacturing, and the like. However, polyimide materials are susceptible to frictional wear in high-speed sliding or high-temperature environments, limiting their application to some particular fields.
Although polyimide has many advantages, it has relatively poor self-lubricating properties, resulting in the tendency to frictional wear phenomenon in practical use. This is mainly because the interaction force between polyimide molecular chains is strong, so that it is difficult to form an effective lubricating film during sliding, thereby increasing the friction coefficient and wear rate. In addition, polyimide materials are relatively hard, which can also easily lead to increased wear during rubbing.
In order to improve the self-lubricating properties of polyimide materials, researchers have tried many methods such as adding nanoparticles, changing the molecular structure, and the like. These methods improve the self-lubricating properties of polyimide materials to some extent, but still have some problems. For example, the addition of nanoparticles may affect the mechanical strength and thermal stability of polyimide materials; changing the molecular structure may lead to an increase in production cost, which is disadvantageous for large-scale application.
Disclosure of Invention
For the above reasons, it is necessary to provide a formulation and a preparation method thereof which can effectively improve the self-lubricity of polyimide while maintaining the original advantages thereof.
The invention aims at providing a modified polyimide composite material.
The modified polyimide composite material comprises the following raw material components in parts by weight:
70-80 parts of polyimide;
1-5 parts of modified polytetrafluoroethylene;
1-5 parts of graphene;
0.2-1 parts of boron nitride;
White carbon black 2-5 parts.
Preferably, the modified polytetrafluoroethylene is inorganic lubricating filler blended modified polytetrafluoroethylene, wherein the inorganic lubricating filler accounts for 8-12% of the mass of the modified polytetrafluoroethylene; the inorganic lubricating filler comprises boron nitride fibers and graphene fibers.
Preferably, the mass ratio of the boron nitride fiber to the graphene fiber is 1.20-1.35:1.
Preferably, the length-diameter ratio of the boron nitride fiber is 40-60:1, and the diameter is 4-6 mu m.
Preferably, the length-diameter ratio of the graphene fiber is 80-120:1, and the diameter is 0.5-5 mu m.
Preferably, the polytetrafluoroethylene has an average particle diameter of 2 μm to 10. Mu.m.
Preferably, the particle size of the polyimide ranges from 25 mu m to 35 mu m, the sheet diameter of the graphene ranges from 2 mu m to 5 mu m, and the thickness of the graphene ranges from 0.8nm to 1.2nm; the particle size of the boron nitride is 5-8 mu m, and the particle size of the white carbon black is 5-8 mu m.
The invention further aims at providing a preparation method of the modified polyimide composite material.
The preparation method of the modified polyimide composite material comprises the following preparation steps:
s1, fully drying boron nitride fibers, graphene fibers and polytetrafluoroethylene, carrying out resonance mixing on the boron nitride fibers and the graphene fibers, and then adding polytetrafluoroethylene which is placed in advance at 3-6 ℃ and stands for 6-8 hours for resonance mixing to obtain mixed powder;
And S2, slowly heating the mixed powder to 350 ℃ and performing heat treatment for 5-8 min to finish modification of polytetrafluoroethylene, adding polyimide, performing high-speed blending, and granulating to obtain the modified polyimide composite material.
A third object of the present invention is to provide an application of the modified polyimide composite material.
The application of the modified polyimide composite material is that the modified polyimide composite material is taken as a raw material to be added into an injection mold for injection molding to form a sealing product.
Preferably, in the injection molding process, the temperature is increased to 280-320 ℃ from the room temperature at a heating rate of 5-10 ℃ per minute, and the heat preservation time is 2-4 hours; then heating to 350-360 ℃, preserving heat for 1.5-3 h, and then cooling to room temperature at a cooling rate of 5-10 ℃.
The beneficial effects are that:
The composite material prepared by the invention has the advantages of good compatibility among components, high mechanical strength, self-lubrication, corrosion resistance, wear resistance, high toughness and the like, and the preparation method is simple, quick in injection molding, easy to process and beneficial to industrial application.
The tensile strength of the modified polyimide composite material prepared by the invention is more than 80Mpa, the elongation at break is more than 6.8%, the toughness is excellent, the friction coefficient is less than 0.12, the wear rate is less than 0.08mm 3/(N.m), and the self-lubricating property and the wear resistance are excellent.
Detailed Description
The invention will be further illustrated by the following examples, which are not intended to limit the scope of the invention, in order to facilitate the understanding of those skilled in the art. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a modified polyimide composite material which comprises the following raw material components in parts by weight: 70-80 parts of polyimide; 1-5 parts of modified polytetrafluoroethylene; 1-5 parts of graphene; 0.2-1 parts of boron nitride; white carbon black 2-5 parts.
In the modified polyimide composite material provided by the invention, the modified polytetrafluoroethylene is inorganic lubricating filler blended modified polytetrafluoroethylene. The inorganic lubricating filler accounts for 8-12% of the mass of the modified polytetrafluoroethylene, and is preferably 10%; the inorganic lubricating filler comprises boron nitride fibers and graphene fibers. It should be noted that the physical state of the boron nitride fibers and graphene fibers used for the inorganic lubricating filler is different from that of boron nitride and graphene in the composition modified polyimide composite material, and this is not ambiguous here.
In the modified polyimide composite material provided by the invention, the mass part ratio of the boron nitride fiber to the graphene fiber is 1.20-1.35:1, preferably 1.20:1.
In the modified polyimide composite material provided by the invention, the length-diameter ratio of the boron nitride fiber is 40-60:1, and the diameter is 4-6 mu m.
In the modified polyimide composite material provided by the invention, the length-diameter ratio of the graphene fiber is 80-120:1, and the diameter is 0.5-5 mu m.
In the modified polyimide composite material provided by the invention, the average particle size of the polytetrafluoroethylene is 2-10 mu m.
In the modified polyimide composite material provided by the invention, the particle size range of polyimide is 25-35 mu m, the sheet diameter of graphene is 2-5 mu m, and the thickness is 0.8-1.2 nm; the particle size of the boron nitride is 5-8 mu m, and the particle size of the white carbon black is 5-8 mu m.
The invention provides a preparation method of a modified polyimide composite material, which comprises the following preparation steps:
s1, fully drying boron nitride fibers, graphene fibers and polytetrafluoroethylene, carrying out resonance mixing on the boron nitride fibers and the graphene fibers, and then adding polytetrafluoroethylene which is placed in advance at 3-6 ℃ and stands for 6-8 hours for resonance mixing to obtain mixed powder;
And S2, slowly heating the mixed powder to 350 ℃ and performing heat treatment for 5-8 min to finish modification of polytetrafluoroethylene, adding polyimide, performing high-speed blending, and granulating to obtain the modified polyimide composite material.
The invention provides an application of a modified polyimide composite material, which is characterized in that the modified polyimide composite material is taken as a raw material and added into an injection mold to be injection molded to form a sealing product, and in the injection molding process, the temperature is raised to 280-320 ℃ from room temperature at a heating rate of 5-10 ℃/min, and the heat preservation time is 2-4 h; then heating to 350-360 ℃, preserving heat for 1.5-3 h, and then cooling to room temperature at a cooling rate of 5-10 ℃.
The tensile strength of the modified polyimide composite material prepared by the invention is more than 80Mpa, the elongation at break is more than 6.8%, the toughness is excellent, the friction coefficient is less than 0.12, the wear rate is less than 0.08mm 3/(N.m), and the self-lubricating property and the wear resistance are excellent.
Polyimide is a high-performance engineering plastic, and is known for its excellent thermal stability, mechanical properties and chemical resistance. Polytetrafluoroethylene (PTFE) is also a high performance polymeric material that has excellent high and low temperature properties and chemical stability. Because the chemical structures and properties of polyimide and polytetrafluoroethylene are greatly different, the blending granulation of polyimide and polytetrafluoroethylene has a certain difficult problem. According to the invention, after the polytetrafluoroethylene is modified by adopting the graphene fiber and the boron nitride fiber, the modified polytetrafluoroethylene is used as a raw material to be compounded with polyimide, graphene particles, boron nitride particles and the like, so that the blending property is good, and excellent lubricating property, toughness and wear resistance are shown. On one hand, graphene is used as an auxiliary agent to improve the lubricating property and the wear resistance of polyimide, and boron nitride is used as another auxiliary agent possibly used for improving the self-lubricating property of polyimide, and has excellent biocompatibility, mechanical strength, high-temperature oxidation resistance and chemical stability, similar to the graphene in structure; the modified polyimide prepared by the method has such excellent performance as breaking the interfacial compatibility and breaking through the limitation, the internal reasons are presumed to be that polytetrafluoroethylene is modified by two fibers at the moment, a fibrous network is formed inside the polytetrafluoroethylene, and graphene and boron nitride particles are also present in a polyimide system in the mixing process with polyimide, so that the linkage is easy to generate between molecules of the same components or molecular acting force exists in the matching process of the fibrous network structure and the polyimide system, the specific surface area of the fibers is large, the activity is strong, the acting force between interfaces is further enhanced, the interface bonding strength is increased, and the blending between the two is realized.
The modified polytetrafluoroethylene is used as a reinforcing material, the properties of the length-diameter ratio, diameter and the like of the fibers formed in the composite material have important influence on the performance of the composite material, and the components are cooperatively influenced to improve the comprehensive performance of the modified polyimide composite material.
For clarity, the following examples are provided in detail.
Polytetrafluoroethylene adopted in the embodiment of the invention is purchased from polytetrafluoroethylene suspension resin M-18F produced by Japanese Dajinshi industries, inc.; polyimide is purchased in Shanghai synthetic resin factories; other sources not illustrated are commercially available.
Example 1
In the embodiment, the modified polyimide composite material comprises the following components in parts by weight: 73 parts of polyimide; 4 parts of modified polytetrafluoroethylene; 4 parts of graphene; 0.5 parts of boron nitride; 3 parts of white carbon black.
Wherein the grain diameter of polyimide is 25 μm, the sheet diameter of graphene is 2 μm-5 μm, and the thickness is 0.8nm-1.2nm; the grain size of the boron nitride is 5-8 mu m, and the grain size of the white carbon black is 5-8 mu m.
In the preparation of the modified polytetrafluoroethylene,
The amount of the boron nitride fiber and the graphene fiber accounts for 8% of the mass of the modified polytetrafluoroethylene;
the mass ratio of the boron nitride fiber to the graphene fiber is 1.2:1, a step of;
the length-diameter ratio of the boron nitride fiber is 40: 1. boron nitride fibers having a diameter of 4-6 μm;
The length-diameter ratio of the graphene fiber is 80: 1. graphene fibers with diameters of 0.5-2 μm;
The grain size of polytetrafluoroethylene is 2-6 μm.
The preparation method of the modified polyimide composite material comprises the following steps:
S1, placing polytetrafluoroethylene in an environment of 3-6 ℃ for standing for 6-8 hours for pretreatment for later use; sufficiently drying boron nitride fiber, graphene fiber and polytetrafluoroethylene at 25-35 ℃, carrying out resonance mixing on the boron nitride fiber and the graphene fiber for 120-180min, adding pretreated polytetrafluoroethylene, and carrying out resonance mixing for 120-180min to obtain mixed powder;
And S2, slowly heating the mixed powder to 350 ℃, performing heat treatment for 5-8 min to finish modification of polytetrafluoroethylene, adding polyimide, performing high-temperature melt mixing at 280 ℃ by using a double screw extruder, and granulating to obtain the modified polyimide composite material.
Example 2
In the embodiment, the modified polyimide composite material comprises the following components in parts by weight: 73 parts of polyimide; 4 parts of modified polytetrafluoroethylene; 4 parts of graphene; 0.5 parts of boron nitride; 3 parts of white carbon black.
Wherein the grain diameter of polyimide is 25 μm, the sheet diameter of graphene is 2 μm-5 μm, and the thickness is 0.8nm-1.2nm; the grain size of the boron nitride is 5-8 mu m, and the grain size of the white carbon black is 5-8 mu m.
In the preparation of the modified polytetrafluoroethylene,
The amount of the boron nitride fiber and the graphene fiber accounts for 8% of the mass of the modified polytetrafluoroethylene;
the mass ratio of the boron nitride fiber to the graphene fiber is 1.3:1, a step of;
the length-diameter ratio of the boron nitride fiber is 40: 1. boron nitride fibers having a diameter of 4-6 μm;
The length-diameter ratio of the graphene fiber is 80: 1. graphene fibers with diameters of 3-5 μm;
The grain size of polytetrafluoroethylene is 5-10 μm.
The preparation method of the modified polyimide composite material comprises the following steps:
S1, placing polytetrafluoroethylene in an environment of 3-6 ℃ for standing for 6-8 hours for pretreatment for later use; sufficiently drying boron nitride fiber, graphene fiber and polytetrafluoroethylene at 25-35 ℃, carrying out resonance mixing on the boron nitride fiber and the graphene fiber for 120-180min, adding pretreated polytetrafluoroethylene, and carrying out resonance mixing for 120-180min to obtain mixed powder;
And S2, slowly heating the mixed powder to 350 ℃, performing heat treatment for 5-8 min to finish modification of polytetrafluoroethylene, adding polyimide, performing high-temperature melt mixing at 280 ℃ by using a double screw extruder, and granulating to obtain the modified polyimide composite material.
Example 3
In the embodiment, the modified polyimide composite material comprises the following components in parts by weight: 73 parts of polyimide; 4 parts of modified polytetrafluoroethylene; 4 parts of graphene; 0.5 parts of boron nitride; 3 parts of white carbon black.
Wherein the grain diameter of polyimide is 25 μm, the sheet diameter of graphene is 2 μm-5 μm, and the thickness is 0.8nm-1.2nm; the grain size of the boron nitride is 5-8 mu m, and the grain size of the white carbon black is 5-8 mu m.
In the preparation of the modified polytetrafluoroethylene,
The amount of the boron nitride fiber and the graphene fiber accounts for 8% of the mass of the modified polytetrafluoroethylene;
the mass ratio of the boron nitride fiber to the graphene fiber is 1.35:1, a step of;
the length-diameter ratio of the boron nitride fiber is 40: 1. boron nitride fibers having a diameter of 4-6 μm;
The length-diameter ratio of the graphene fiber is 80: 1. graphene fibers with diameters of 3-5 μm;
The grain size of polytetrafluoroethylene is 4-8 μm.
The preparation method of the modified polyimide composite material comprises the following steps:
S1, placing polytetrafluoroethylene in an environment of 3-6 ℃ for standing for 6-8 hours for pretreatment for later use; sufficiently drying boron nitride fiber, graphene fiber and polytetrafluoroethylene at 25-35 ℃, carrying out resonance mixing on the boron nitride fiber and the graphene fiber for 120-180min, adding pretreated polytetrafluoroethylene, and carrying out resonance mixing for 120-180min to obtain mixed powder;
And S2, slowly heating the mixed powder to 350 ℃, performing heat treatment for 5-8 min to finish modification of polytetrafluoroethylene, adding polyimide, performing high-temperature melt mixing at 280 ℃ by using a double screw extruder, and granulating to obtain the modified polyimide composite material.
Example 4
The difference between this embodiment and embodiment 1 is that in this embodiment, the aspect ratio of the boron nitride fiber of this embodiment is selected to be 50: 1. boron nitride fibers having a diameter of 4-6 μm.
Example 5
The difference between this embodiment and embodiment 1 is that in this embodiment, the aspect ratio of the boron nitride fiber of this embodiment is selected to be 60: 1. boron nitride fibers having a diameter of 4-6 μm.
Example 6
The difference between this embodiment and embodiment 1 is that in this embodiment, the aspect ratio of the graphene fiber of this embodiment is selected to be 100: 1. graphene fibers with a diameter of 0.5-2 μm.
Example 7
The difference between the present embodiment and embodiment 1 is that in the present embodiment, the aspect ratio of the graphene fiber of the present embodiment is 120: 1. graphene fibers with a diameter of 3-5 μm.
Example 8
This example differs from example 1 in that in this example, the amounts of boron nitride fibers and graphene fibers account for 9% of the mass of the modified polytetrafluoroethylene.
Example 9
This example differs from example 1 in that in this example, the amounts of boron nitride fibers and graphene fibers account for 10% of the mass of the modified polytetrafluoroethylene.
Example 10
The difference between this example and example 1 is that in this example, the modified polyimide composite material comprises the following components in parts by weight: 70 parts of polyimide; 5 parts of modified polytetrafluoroethylene; 1 part of graphene; 0.2 parts of boron nitride; white carbon black 2 parts.
Example 11
The difference between this example and example 1 is that in this example, the modified polyimide composite material comprises the following components in parts by weight: 80 parts of polyimide; 1 part of modified polytetrafluoroethylene; 5 parts of graphene; 1 part of boron nitride; and 5 parts of white carbon black.
Comparative example 1
Thermoplastic polyimides are commercially available.
Comparative example 2
The difference between this comparative example and example 1 is that polytetrafluoroethylene in this comparative example was not modified.
Comparative example 3
The present comparative example differs from example 1 in that in the present comparative example, boron nitride having a particle diameter of 4 to 6 μm and graphene having a particle diameter of 3 to 5 μm were modified for polytetrafluoroethylene.
Comparative example 4
The present comparative example differs from example 1 in that in the present comparative example, the mass ratio of the boron nitride fiber to the graphene fiber is 1:1.
Comparative example 5
The present comparative example is different from example 1 in that the amounts of the boron nitride fiber and the graphene fiber in the present comparative example account for 6% of the mass of the modified polytetrafluoroethylene.
Comparative example 6
The present comparative example is different from example 1 in that the amounts of the boron nitride fiber and the graphene fiber in the present comparative example account for 13% of the mass of the modified polytetrafluoroethylene.
Application examples 1 to 11 and comparative application examples 1 to 6
The composite materials prepared in the examples 1-11 and the comparative examples 1-6 are added into an injection mold as raw materials, and the temperature is raised to 280-320 ℃ from room temperature at a heating rate of 5 ℃/min-10 ℃/min (in the test process, the heat preservation time of the examples 1-11 is in the range of 2-4 h, and the heat preservation time of the comparative examples 1-6 is required to exceed 4h, especially the heat preservation time of the comparative example 1 is close to 8 h); then heating to 350-360 deg.C (in the test process, the heat-preserving time of examples 1-11 is in the range of 1.5-3 h, and the heat-preserving time of comparative examples 1-6 is more than 5h, and the average heat-preserving time is about 8 h), then cooling to room temperature at the cooling rate of 5-10 deg.C, and injection moulding to form the sealed sample.
Performance detection
The samples prepared in examples 1-11 and comparative examples 1-6 were subjected to performance test.
In the test of tensile strength and breaking strength, the samples prepared in examples 1 to 11 and comparative examples 1 to 6 were injection molded and made into dumbbell shape for performance test.
For the friction coefficient and abrasion loss tests, samples of examples 1 to 11 and comparative examples 1 to 6 were injection molded into 30×7×6mm (length×width×thickness) plaques for testing.
The samples of examples 1-11 and comparative examples 1-6 were injection molded into 30 x 7 x 6mm (length x width x thickness) plaques for corrosion resistance testing: neutral salt fog detection: immersing the sample into 5% salt at room temperature to observe the change of appearance; alkali resistance detection: immersing the sample into sodium hydroxide with the concentration of 5% at room temperature, and observing the change of appearance; acid resistance detection: the sample pieces were immersed in a glacial acetic acid solution having a concentration of 3.1% at room temperature, and the change in appearance was observed.
The test results are shown in table 1 below.
Table 1 performance test table
As can be seen from the test results in Table 1, the modified polyimide composite material prepared by the invention has tensile strength of more than 80Mpa, elongation at break of more than 6.8%, excellent toughness, friction coefficient of less than 0.12, abrasion rate of less than 0.08mm 3/(N.m) and excellent self-lubricating property and abrasion resistance.
The foregoing is merely exemplary of the present invention, and those skilled in the art should not be considered as limiting the invention, since modifications may be made in the specific embodiments and application scope of the invention in light of the teachings of the present invention.
Claims (10)
1. The modified polyimide composite material is characterized by comprising the following raw material components in parts by weight:
70-80 parts of polyimide;
1-5 parts of modified polytetrafluoroethylene;
1-5 parts of graphene;
0.2-1 parts of boron nitride;
White carbon black 2-5 parts.
2. The modified polyimide composite material according to claim 1, wherein the modified polytetrafluoroethylene is an inorganic lubricating filler blended modified polytetrafluoroethylene, wherein the inorganic lubricating filler accounts for 8-12% of the mass of the modified polytetrafluoroethylene; the inorganic lubricating filler comprises boron nitride fibers and graphene fibers.
3. The modified polyimide composite material according to claim 2, wherein the mass ratio of the boron nitride fiber to the graphene fiber is 1.20-1.35:1.
4. A modified polyimide composite according to claim 3, wherein the boron nitride fiber has an aspect ratio of 40-60:1 and a diameter of 4-6 μm.
5. A modified polyimide composite according to claim 3, wherein the graphene fibers have an aspect ratio of 80-120:1 and a diameter of 0.5 μm-5 μm.
6. A modified polyimide composite according to claim 2, wherein the polytetrafluoroethylene has an average particle diameter of 2 μm to 10 μm.
7. The modified polyimide composite according to claim 1, wherein the polyimide has a particle size ranging from 25 μm to 35 μm, the graphene has a sheet size ranging from 2 μm to 5 μm, and the graphene has a thickness ranging from 0.8nm to 1.2nm; the particle size of the boron nitride is 5-8 mu m, and the particle size of the white carbon black is 5-8 mu m.
8. The method for preparing a modified polyimide composite material according to claim 2, comprising the following preparation steps:
s1, fully drying boron nitride fibers, graphene fibers and polytetrafluoroethylene, carrying out resonance mixing on the boron nitride fibers and the graphene fibers, and then adding polytetrafluoroethylene which is placed in advance at 3-6 ℃ and stands for 6-8 hours for resonance mixing to obtain mixed powder;
And S2, slowly heating the mixed powder to 350 ℃ and performing heat treatment for 5-8 min to finish modification of polytetrafluoroethylene, adding polyimide, performing high-speed blending, and granulating to obtain the modified polyimide composite material.
9. Use of a modified polyimide composite according to any of claims 1 to 7, wherein the modified polyimide composite is injection molded into a sealing product by injection molding using the modified polyimide composite as a raw material.
10. The use of a modified polyimide composite according to any one of claims 9, wherein during injection molding, the temperature is raised from room temperature to 280 ℃ to 320 ℃ at a heating rate of 5 ℃/min to 10 ℃/min, and the heat preservation time is 2h to 4h; then heating to 350-360 ℃, preserving heat for 1.5-3 h, and then cooling to room temperature at a cooling rate of 5-10 ℃.
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