CN112877026A - Brake pad containing adhesive layer and preparation process of brake pad - Google Patents

Brake pad containing adhesive layer and preparation process of brake pad Download PDF

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Publication number
CN112877026A
CN112877026A CN202110232512.0A CN202110232512A CN112877026A CN 112877026 A CN112877026 A CN 112877026A CN 202110232512 A CN202110232512 A CN 202110232512A CN 112877026 A CN112877026 A CN 112877026A
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modified
brake pad
adhesive layer
putting
solution
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不公告发明人
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Wenzhou Panhu New Energy Co ltd
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Wenzhou Panhu New Energy Co ltd
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Priority to CN202110232512.0A priority Critical patent/CN112877026A/en
Publication of CN112877026A publication Critical patent/CN112877026A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J179/00Adhesives based on 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 C09J161/00 - C09J177/00
    • C09J179/04Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C09J179/08Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16DCOUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D69/00Friction linings; Attachment thereof; Selection of coacting friction substances or surfaces
    • F16D69/02Composition of linings ; Methods of manufacturing
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2237Oxides; Hydroxides of metals of titanium
    • C08K2003/2241Titanium dioxide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16DCOUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D2200/00Materials; Production methods therefor
    • F16D2200/0034Materials; Production methods therefor non-metallic
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16DCOUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D2200/00Materials; Production methods therefor
    • F16D2200/0034Materials; Production methods therefor non-metallic
    • F16D2200/0039Ceramics
    • F16D2200/0043Ceramic base, e.g. metal oxides or ceramic binder
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16DCOUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D2200/00Materials; Production methods therefor
    • F16D2200/0034Materials; Production methods therefor non-metallic
    • F16D2200/0052Carbon
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16DCOUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D2200/00Materials; Production methods therefor
    • F16D2200/0082Production methods therefor
    • F16D2200/0086Moulding materials together by application of heat and pressure

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Braking Arrangements (AREA)

Abstract

The invention discloses a brake pad containing an adhesive layer, which comprises a friction layer, the adhesive layer and a steel backing; the bonding layer comprises the following raw materials in parts by weight: modified polyesterimide resin, modified graphene, a modified anti-aging agent and silicon carbide; putting the modified graphene and silicon carbide into a drying oven, drying for 2-3h at the temperature of 80-100 ℃, mixing and grinding the modified graphene and the silicon carbide for 1h, and sieving to obtain a solid mixture; adding the solid mixture into modified polyesterimide resin, adding an anti-aging agent, and stirring and mixing for 3-4h at the temperature of 300-350 ℃ to obtain an adhesive layer; controlling the mass ratio of the modified graphene to the silicon carbide to be 10-15: 8-12, and the invention has the advantages of good thermal stability, corrosion resistance and oxidation resistance.

Description

Brake pad containing adhesive layer and preparation process of brake pad
Technical Field
The invention belongs to the technical field of automobile parts, relates to a brake pad and a preparation process of the brake pad, and particularly relates to a brake pad containing an adhesive layer and a preparation process of the brake pad.
Background
The brake block generally comprises steel sheet, adhesive linkage and friction material layer, and the adhesive linkage is the bed charge layer of connecting steel sheet and friction material layer promptly, and bed charge layer thickness generally is between 1.5 ~ 2.5mm, plays the effect that bonds friction material increase shear strength in the brake block, and the bed charge layer of high-quality can also play noise reduction, quick radiating function. The working principle of the brake mainly comes from friction, and the kinetic energy of the vehicle is converted into heat energy after friction by using the friction between a brake pad and a brake disc (drum) and between a tire and the ground, so that the vehicle is stopped. A good and efficient braking system must provide a stable, sufficient and controllable braking force, and have good hydraulic transmission and heat dissipation capability, so as to ensure that the force applied by the driver from the brake pedal can be sufficiently and effectively transmitted to the master cylinder and the slave cylinders, and to avoid hydraulic failure and brake recession caused by high heat.
The reference CN105969307B discloses an adhesive layer of a brake pad, which is composed of the following materials in parts by weight: 6-10 parts of rubber powder, 5-10 parts of barium sulfate, 15-20 parts of steel wool, 3-6 parts of aluminum oxide, 2-6 parts of silicon carbide, 10-20 parts of resin, 6-12 parts of mica, 8-15 parts of friction powder and 3-7 parts of aramid fiber. The invention also provides a brake pad containing the bonding layer and a preparation process of the brake pad. The bonding layer provided by the invention can play a role in reminding a vehicle owner of replacing the brake pad, and meanwhile, the shearing strength of the brake pad is increased, so that the bonding layer has good heat dissipation and the product performance is improved.
In the prior art, the bonding layer of the brake pad has the problem of poor thermal stability, corrosion resistance, oxidation resistance and the like, and the service life of the bonding layer is influenced.
Disclosure of Invention
The invention aims to solve the problems that the bonding layer of the brake pad in the prior art is poor in thermal stability, corrosion resistance, oxidizability and the like and the service life of the bonding layer is influenced, and provides a brake pad containing the bonding layer and a preparation process of the brake pad.
The purpose of the invention can be realized by the following technical scheme:
a brake pad containing an adhesive layer comprises a friction layer, the adhesive layer and a steel backing;
the bonding layer comprises the following raw materials in parts by weight: 50-60 parts of modified polyesterimide resin, 10-15 parts of modified graphene, 12-16 parts of modified anti-aging agent and 8-12 parts of silicon carbide;
the preparation process of the brake pad comprises the following steps:
the first step is as follows: putting the modified graphene and silicon carbide into a drying oven, drying for 2-3h at the temperature of 80-100 ℃, mixing and grinding the modified graphene and the silicon carbide for 1h, and sieving to obtain a solid mixture; adding the solid mixture into modified polyesterimide resin, adding an anti-aging agent, and stirring and mixing for 3-4h at the temperature of 300-350 ℃ to obtain an adhesive layer; controlling the mass ratio of the modified graphene to the silicon carbide to be 10-15: 8-12, controlling the mass ratio of the solid mixture, the modified polyesterimide resin and the anti-aging agent to be 18-27:50-60: 12-16;
the second step is that: heating the hot press to 280-300 ℃ at 280-500 kgf/cm2Then, putting the friction layer into a cavity of a hot press, putting the bonding layer obtained in the first step into the cavity of the hot press after flattening, flattening the bonding layer, putting a steel backing on the bonding layer, and keeping the pressure for 4-10 minutes; obtaining a semi-finished brake pad; and then placing the semi-finished brake pad into a curing furnace, preserving the heat for 2-3 hours at the temperature of 220-260 ℃, and cooling to room temperature to obtain the brake pad containing the bonding layer.
Preferably, the preparation process of the modified polyesterimide resin comprises the following steps:
the first step is as follows: adding the modified nano titanium dioxide into N, N-dimethylformamide, and performing ultrasonic dispersion for 2 hours to obtain a mixed solution a;
step two, dripping m-phenylenediamine into the mixed solution a, stirring for 30min after dripping the m-phenylenediamine, continuously adding (4, 4' -isopropyldiphenoxy) diphthalic anhydride, and continuously stirring for 3 h; obtaining a mixed solution b;
the third step: carrying out ultrasonic treatment on the obtained mixed solution b for 10min, putting the treated mixed solution b into a vacuum drying oven, and vacuumizing the mixed solution b to remove bubbles in the mixed solution b;
the fourth step: pouring the treated mixed solution b onto a glass plate, and uniformly coating the mixed solution b onto the glass plate by using a film scraping machine; placing the scraped glass plate in a vacuum drying oven, vacuumizing for 4h at 80 ℃, and then heating to 40 ℃ from 120 ℃ each time, and preserving the heat of each temperature gradient for 45 min; taking out the cooled glass plate, transferring the cooled glass plate to a forced air drying oven, preserving the heat at 260 ℃ for 45min, preserving the heat at 280 ℃ for 0.5h, and naturally cooling to room temperature; and then stripping the film by water bath to remove the obtained modified polyesterimide resin from the glass plate.
Preferably, the mass ratio of the modified nano titanium dioxide to the N, N-dimethylformamide to the m-phenylenediamine to the (4, 4' -isopropyldiphenoxy) diphthalic anhydride is controlled to be 8-10: 30-40: 2-4: 3-5;
preferably, the preparation process of the modified nano titanium dioxide comprises the following steps:
the first step is as follows: putting the dried nano titanium dioxide into the oven again, and preserving the heat for 2 hours at 100 ℃;
the second step is that: adding absolute ethyl alcohol into a KH550 silane coupling agent to obtain solution A;
the third step: adding nano titanium dioxide into the solution A; carrying out condensation reflux and continuous stirring reaction for 4h in an ultrasonic cleaning machine in a constant-temperature water bath at 40 ℃; obtaining a solution B;
the fifth step: centrifuging the solution B by using a desk centrifuge to obtain a modified nano titanium dioxide coarse material; and then, cleaning the modified nano titanium dioxide coarse material by using ethanol, and drying to obtain the nano titanium dioxide.
Preferably, the mass ratio of the KH550 silane coupling agent to the absolute ethyl alcohol is controlled to be 5-8: 50-80; the mass ratio of the nano titanium dioxide to the A liquid is controlled to be 5-9: 60-90.
Preferably, the preparation process of the modified graphene comprises the following steps:
the first step is as follows: mixing and stirring aminopropyltriethoxysilane and toluene to obtain a solution a; then adding graphene and dicyclohexylcarbodiimide into the solution a, and ultrasonically dispersing for 1h at the temperature of 70-80 ℃ to obtain solution b; controlling the mass ratio of aminopropyltriethoxysilane to toluene to be 5-10: 20-30; controlling the mass ratio of the graphene dicyclohexylcarbodiimide to the liquid a to be 30-40:30-40: 25-40;
the second step is that: carrying out reduced pressure suction filtration on the solution b to obtain a filter cake, washing the filter cake by using absolute ethyl alcohol, and removing a silane monomer to obtain solid powder; and adding the solid powder into a drying oven, and drying at the temperature of 60-80 ℃ for 5h to obtain the modified graphene.
Preferably, the preparation process of the anti-aging agent comprises the following steps: mixing a coupling agent KH560 with p-aminodiphenylamine, and reacting for 5 hours at 120 ℃ under the protection of nitrogen to obtain a first mixed material; adding the first mixed material into ethanol for ultrasonic dispersion for 10 min; and (3) putting the dried white carbon black into a high-speed mixer, respectively spraying ethanol solution of the first mixed material, stirring for 5min, discharging, drying in vacuum at 120 ℃ for 6h, and washing with absolute ethanol to obtain the modified anti-aging agent.
Preferably, the molar ratio of the coupling agent KH560 to the p-aminodiphenylamine is controlled to be 1: 1-1.3; the mass ratio of the first mixed material to the ethanol is controlled to be 20-30: 55-60.
A preparation process of a brake pad containing an adhesive layer comprises the following steps:
the first step is as follows: putting the modified graphene and silicon carbide into a drying oven, drying for 2-3h at the temperature of 80-100 ℃, mixing and grinding the modified graphene and the silicon carbide for 1h, and sieving to obtain a solid mixture; adding the solid mixture into modified polyesterimide resin, adding an anti-aging agent, and stirring and mixing for 3-4h at the temperature of 300-350 ℃ to obtain an adhesive layer; controlling the mass ratio of the modified graphene to the silicon carbide to be 10-15: 8-12, controlling the mass ratio of the solid mixture, the modified polyesterimide resin and the anti-aging agent to be 18-27:50-60: 12-16;
the second step is that: heating the hot press to 280-300 ℃ at 280-500 kgf/cm2Then, putting the friction layer into a cavity of a hot press, putting the bonding layer obtained in the first step into the cavity of the hot press after flattening, flattening the bonding layer, putting a steel backing on the bonding layer, and keeping the pressure for 4-10 minutes; obtaining a semi-finished brake pad; and then placing the semi-finished brake pad into a curing furnace, preserving the heat for 2-3 hours at the temperature of 220-260 ℃, and cooling to room temperature to obtain the brake pad containing the bonding layer.
Compared with the prior art, the invention has the beneficial effects that:
the brake pad comprises a friction layer, an adhesive layer and a steel backing; the bonding layer comprises the following raw materials in parts by weight: 50-60 parts of modified polyesterimide resin, 10-15 parts of modified graphene, 12-16 parts of modified anti-aging agent and 8-12 parts of silicon carbide; wherein carborundum texture is very hard for the brake block in case the wearing and tearing reach the adhesive linkage, will send similar metal contact brake disc and the noise that produces, remind the car owner to change the brake block. Therefore, certain potential safety hazards caused by untimely replacement of the brake pad can be avoided; and the production process is simple
The modified polyesterimide resin is prepared by taking m-phenylenediamine as a diamine monomer, taking (4, 4' -isopropyldiphenoxy) diphthalic anhydride as a dianhydride monomer and taking modified nano titanium dioxide as an additive through an in-situ polymerization method; the nano titanium dioxide has strong polarity, and meanwhile, the particles of the nano particles are micronized; the inorganic nano material of nano titanium dioxide has better dispersion effect in a non-organic phase, and is not easy to disperse and easy to agglomerate in an organic phase; the problem is solved by modifying the nano titanium dioxide; the addition of the modified nano titanium dioxide greatly improves the thermal stability of the polyester-imide resin, and the introduction of the nano titanium dioxide also greatly improves the hydrophobicity of the polyimide film; thereby improving the thermal stability and the hydrophobicity of the bonding layer of the brake pad;
the temperature resistance of the bonding layer can be improved by introducing the modified graphene; the modified graphene sheet layer has a huge two-dimensional structure and a good gas barrier structure, so that decomposed gas or a ring body is prevented from overflowing out of the system, and the bonding layer of the brake pad has high thermal stability; the introduction of the modified graphene can improve the uniformity of the bonding layer, reduce the cracks of the material, form a compact barrier structure by the graphene which is dispersed in the polymer in a disordered manner, and obviously increase the diffusion path of a corrosive medium, so that less corrosive medium can permeate the surface of the steel backing, and the phenomenon that the steel backing and the bonding layer are corroded is avoided; the modified graphene has a plurality of reactive groups, and the modified graphene increases the crosslinking density, so that the barrier effect is enhanced;
the modified anti-aging agent with the coupling effect and the anti-aging effect is prepared by the reaction of the coupling agent and the p-aminodiphenylamine, so that the aging phenomenon of the bonding layer can be effectively relieved; the problem that in the prior art, when the anti-aging agent in the bonding layer is used in a high-temperature environment, the anti-aging agent is reduced or loses the protection effect due to volatilization is solved.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A brake pad containing an adhesive layer comprises a friction layer, the adhesive layer and a steel backing;
the bonding layer comprises the following raw materials in parts by weight: 50-60 parts of modified polyesterimide resin, 10-15 parts of modified graphene, 12-16 parts of modified anti-aging agent and 8-12 parts of silicon carbide;
the preparation process of the brake pad comprises the following steps:
the first step is as follows: putting the modified graphene and silicon carbide into a drying oven, drying for 2-3h at the temperature of 80-100 ℃, mixing and grinding the modified graphene and the silicon carbide for 1h, and sieving to obtain a solid mixture; adding the solid mixture into modified polyesterimide resin, adding an anti-aging agent, and stirring and mixing for 3-4h at the temperature of 300-350 ℃ to obtain an adhesive layer; controlling the mass ratio of the modified graphene to the silicon carbide to be 10-15: 8-12, controlling the mass ratio of the solid mixture, the modified polyesterimide resin and the anti-aging agent to be 18-27:50-60: 12-16;
the second step is that: heating the hot press to 280-300 ℃ at 280-500 kgf/cm2Then, putting the friction layer into a cavity of a hot press, putting the bonding layer obtained in the first step into the cavity of the hot press after flattening, flattening the bonding layer, putting a steel backing on the bonding layer, and keeping the pressure for 4-10 minutes; obtaining a semi-finished brake pad; and then placing the semi-finished brake pad into a curing furnace, preserving the heat for 2-3 hours at the temperature of 220-260 ℃, and cooling to room temperature to obtain the brake pad containing the bonding layer.
The preparation process of the modified polyester-imide resin comprises the following steps:
the first step is as follows: adding the modified nano titanium dioxide into N, N-dimethylformamide, and performing ultrasonic dispersion for 2 hours to obtain a mixed solution a;
step two, dripping m-phenylenediamine into the mixed solution a, stirring for 30min after dripping the m-phenylenediamine, continuously adding (4, 4' -isopropyldiphenoxy) diphthalic anhydride, and continuously stirring for 3 h; obtaining a mixed solution b;
the third step: carrying out ultrasonic treatment on the obtained mixed solution b for 10min, putting the treated mixed solution b into a vacuum drying oven, and vacuumizing the mixed solution b to remove bubbles in the mixed solution b;
the fourth step: pouring the treated mixed solution b onto a glass plate, and uniformly coating the mixed solution b onto the glass plate by using a film scraping machine; placing the scraped glass plate in a vacuum drying oven, vacuumizing for 4h at 80 ℃, and then heating to 40 ℃ from 120 ℃ each time, and preserving the heat of each temperature gradient for 45 min; taking out the cooled glass plate, transferring the cooled glass plate to a forced air drying oven, preserving the heat at 260 ℃ for 45min, preserving the heat at 280 ℃ for 0.5h, and naturally cooling to room temperature; and then stripping the film by water bath to remove the obtained modified polyesterimide resin from the glass plate.
Controlling the mass ratio of the modified nano titanium dioxide, the N, N-dimethylformamide, the m-phenylenediamine and the (4, 4' -isopropyl diphenoxy) diphthalic anhydride to be 8-10: 30-40: 2-4: 3-5;
the preparation process of the modified nano titanium dioxide comprises the following steps:
the first step is as follows: putting the dried nano titanium dioxide into the oven again, and preserving the heat for 2 hours at 100 ℃;
the second step is that: adding absolute ethyl alcohol into a KH550 silane coupling agent to obtain solution A;
the third step: adding nano titanium dioxide into the solution A; carrying out condensation reflux and continuous stirring reaction for 4h in an ultrasonic cleaning machine in a constant-temperature water bath at 40 ℃; obtaining a solution B;
the fifth step: centrifuging the solution B by using a desk centrifuge to obtain a modified nano titanium dioxide coarse material; and then, cleaning the modified nano titanium dioxide coarse material by using ethanol, and drying to obtain the nano titanium dioxide.
Controlling the mass ratio of the KH550 silane coupling agent to the absolute ethyl alcohol to be 5-8: 50-80; the mass ratio of the nano titanium dioxide to the A liquid is controlled to be 5-9: 60-90.
The preparation process of the modified graphene comprises the following steps:
the first step is as follows: mixing and stirring aminopropyltriethoxysilane and toluene to obtain a solution a; then adding graphene and dicyclohexylcarbodiimide into the solution a, and ultrasonically dispersing for 1h at the temperature of 70-80 ℃ to obtain solution b; controlling the mass ratio of aminopropyltriethoxysilane to toluene to be 5-10: 20-30; controlling the mass ratio of the graphene dicyclohexylcarbodiimide to the liquid a to be 30-40:30-40: 25-40;
the second step is that: carrying out reduced pressure suction filtration on the solution b to obtain a filter cake, washing the filter cake by using absolute ethyl alcohol, and removing a silane monomer to obtain solid powder; and adding the solid powder into a drying oven, and drying at the temperature of 60-80 ℃ for 5h to obtain the modified graphene.
The preparation process of the anti-aging agent comprises the following steps: mixing a coupling agent KH560 with p-aminodiphenylamine, and reacting for 5 hours at 120 ℃ under the protection of nitrogen to obtain a first mixed material; adding the first mixed material into ethanol for ultrasonic dispersion for 10 min; and (3) putting the dried white carbon black into a high-speed mixer, respectively spraying ethanol solution of the first mixed material, stirring for 5min, discharging, drying in vacuum at 120 ℃ for 6h, and washing with absolute ethanol to obtain the modified anti-aging agent.
Controlling the molar ratio of the coupling agent KH560 to the p-aminodiphenylamine to be 1: 1-1.3; the mass ratio of the first mixed material to the ethanol is controlled to be 20-30: 55-60.
Example 2
A brake pad containing an adhesive layer comprises a friction layer, the adhesive layer and a steel backing;
the bonding layer comprises the following raw materials in parts by weight: 50-60 parts of modified polyesterimide resin, 10-15 parts of modified graphene, 12-16 parts of modified anti-aging agent and 8-12 parts of silicon carbide;
the preparation process of the brake pad comprises the following steps:
the first step is as follows: putting the modified graphene and silicon carbide into a drying oven, drying for 2-3h at the temperature of 80-100 ℃, mixing and grinding the modified graphene and the silicon carbide for 1h, and sieving to obtain a solid mixture; adding the solid mixture into modified polyesterimide resin, adding an anti-aging agent, and stirring and mixing for 3-4h at the temperature of 300-350 ℃ to obtain an adhesive layer; controlling the mass ratio of the modified graphene to the silicon carbide to be 10-15: 8-12, controlling the mass ratio of the solid mixture, the modified polyesterimide resin and the anti-aging agent to be 18-27:50-60: 12-16;
the second step is that: heating the hot press to 280-300 ℃ at 280-500 kgf/cm2Then, putting the friction layer into a cavity of a hot press, putting the bonding layer obtained in the first step into the cavity of the hot press after flattening, flattening the bonding layer, putting a steel backing on the bonding layer, and keeping the pressure for 4-10 minutes; obtaining a semi-finished brake pad; and then placing the semi-finished brake pad into a curing furnace, preserving the heat for 2-3 hours at the temperature of 220-260 ℃, and cooling to room temperature to obtain the brake pad containing the bonding layer.
The preparation process of the modified polyester-imide resin comprises the following steps:
the first step is as follows: adding the modified nano titanium dioxide into N, N-dimethylformamide, and performing ultrasonic dispersion for 2 hours to obtain a mixed solution a;
step two, dripping m-phenylenediamine into the mixed solution a, stirring for 30min after dripping the m-phenylenediamine, continuously adding (4, 4' -isopropyldiphenoxy) diphthalic anhydride, and continuously stirring for 3 h; obtaining a mixed solution b;
the third step: carrying out ultrasonic treatment on the obtained mixed solution b for 10min, putting the treated mixed solution b into a vacuum drying oven, and vacuumizing the mixed solution b to remove bubbles in the mixed solution b;
the fourth step: pouring the treated mixed solution b onto a glass plate, and uniformly coating the mixed solution b onto the glass plate by using a film scraping machine; placing the scraped glass plate in a vacuum drying oven, vacuumizing for 4h at 80 ℃, and then heating to 40 ℃ from 120 ℃ each time, and preserving the heat of each temperature gradient for 45 min; taking out the cooled glass plate, transferring the cooled glass plate to a forced air drying oven, preserving the heat at 260 ℃ for 45min, preserving the heat at 280 ℃ for 0.5h, and naturally cooling to room temperature; and then stripping the film by water bath to remove the obtained modified polyesterimide resin from the glass plate.
Controlling the mass ratio of the modified nano titanium dioxide, the N, N-dimethylformamide, the m-phenylenediamine and the (4, 4' -isopropyl diphenoxy) diphthalic anhydride to be 8-10: 30-40: 2-4: 3-5;
the preparation process of the modified nano titanium dioxide comprises the following steps:
the first step is as follows: putting the dried nano titanium dioxide into the oven again, and preserving the heat for 2 hours at 100 ℃;
the second step is that: adding absolute ethyl alcohol into a KH550 silane coupling agent to obtain solution A;
the third step: adding nano titanium dioxide into the solution A; carrying out condensation reflux and continuous stirring reaction for 4h in an ultrasonic cleaning machine in a constant-temperature water bath at 40 ℃; obtaining a solution B;
the fifth step: centrifuging the solution B by using a desk centrifuge to obtain a modified nano titanium dioxide coarse material; and then, cleaning the modified nano titanium dioxide coarse material by using ethanol, and drying to obtain the nano titanium dioxide.
Controlling the mass ratio of the KH550 silane coupling agent to the absolute ethyl alcohol to be 5-8: 50-80; the mass ratio of the nano titanium dioxide to the A liquid is controlled to be 5-9: 60-90.
The preparation process of the modified graphene comprises the following steps:
the first step is as follows: mixing and stirring aminopropyltriethoxysilane and toluene to obtain a solution a; then adding graphene and dicyclohexylcarbodiimide into the solution a, and ultrasonically dispersing for 1h at the temperature of 70-80 ℃ to obtain solution b; controlling the mass ratio of aminopropyltriethoxysilane to toluene to be 5-10: 20-30; controlling the mass ratio of the graphene dicyclohexylcarbodiimide to the liquid a to be 30-40:30-40: 25-40;
the second step is that: carrying out reduced pressure suction filtration on the solution b to obtain a filter cake, washing the filter cake by using absolute ethyl alcohol, and removing a silane monomer to obtain solid powder; and adding the solid powder into a drying oven, and drying at the temperature of 60-80 ℃ for 5h to obtain the modified graphene.
The preparation process of the anti-aging agent comprises the following steps: mixing a coupling agent KH560 with p-aminodiphenylamine, and reacting for 5 hours at 120 ℃ under the protection of nitrogen to obtain a first mixed material; adding the first mixed material into ethanol for ultrasonic dispersion for 10 min; and (3) putting the dried white carbon black into a high-speed mixer, respectively spraying ethanol solution of the first mixed material, stirring for 5min, discharging, drying in vacuum at 120 ℃ for 6h, and washing with absolute ethanol to obtain the modified anti-aging agent.
Controlling the molar ratio of the coupling agent KH560 to the p-aminodiphenylamine to be 1: 1-1.3; the mass ratio of the first mixed material to the ethanol is controlled to be 20-30: 55-60.
Example 3
A brake pad containing an adhesive layer comprises a friction layer, the adhesive layer and a steel backing;
the bonding layer comprises the following raw materials in parts by weight: 50-60 parts of modified polyesterimide resin, 10-15 parts of modified graphene, 12-16 parts of modified anti-aging agent and 8-12 parts of silicon carbide;
the preparation process of the brake pad comprises the following steps:
the first step is as follows: putting the modified graphene and silicon carbide into a drying oven, drying for 2-3h at the temperature of 80-100 ℃, mixing and grinding the modified graphene and the silicon carbide for 1h, and sieving to obtain a solid mixture; adding the solid mixture into modified polyesterimide resin, adding an anti-aging agent, and stirring and mixing for 3-4h at the temperature of 300-350 ℃ to obtain an adhesive layer; controlling the mass ratio of the modified graphene to the silicon carbide to be 10-15: 8-12, controlling the mass ratio of the solid mixture, the modified polyesterimide resin and the anti-aging agent to be 18-27:50-60: 12-16;
the second step is that: heating the hot press to 280-300 ℃ at 280-500 kgf/cm2Then, putting the friction layer into a cavity of a hot press, putting the bonding layer obtained in the first step into the cavity of the hot press after flattening, flattening the bonding layer, putting a steel backing on the bonding layer, and keeping the pressure for 4-10 minutes; obtaining a semi-finished brake pad; and then placing the semi-finished brake pad into a curing furnace, preserving the heat for 2-3 hours at the temperature of 220-260 ℃, and cooling to room temperature to obtain the brake pad containing the bonding layer.
The preparation process of the modified polyester-imide resin comprises the following steps:
the first step is as follows: adding the modified nano titanium dioxide into N, N-dimethylformamide, and performing ultrasonic dispersion for 2 hours to obtain a mixed solution a;
step two, dripping m-phenylenediamine into the mixed solution a, stirring for 30min after dripping the m-phenylenediamine, continuously adding (4, 4' -isopropyldiphenoxy) diphthalic anhydride, and continuously stirring for 3 h; obtaining a mixed solution b;
the third step: carrying out ultrasonic treatment on the obtained mixed solution b for 10min, putting the treated mixed solution b into a vacuum drying oven, and vacuumizing the mixed solution b to remove bubbles in the mixed solution b;
the fourth step: pouring the treated mixed solution b onto a glass plate, and uniformly coating the mixed solution b onto the glass plate by using a film scraping machine; placing the scraped glass plate in a vacuum drying oven, vacuumizing for 4h at 80 ℃, and then heating to 40 ℃ from 120 ℃ each time, and preserving the heat of each temperature gradient for 45 min; taking out the cooled glass plate, transferring the cooled glass plate to a forced air drying oven, preserving the heat at 260 ℃ for 45min, preserving the heat at 280 ℃ for 0.5h, and naturally cooling to room temperature; and then stripping the film by water bath to remove the obtained modified polyesterimide resin from the glass plate.
Controlling the mass ratio of the modified nano titanium dioxide, the N, N-dimethylformamide, the m-phenylenediamine and the (4, 4' -isopropyl diphenoxy) diphthalic anhydride to be 8-10: 30-40: 2-4: 3-5;
the preparation process of the modified nano titanium dioxide comprises the following steps:
the first step is as follows: putting the dried nano titanium dioxide into the oven again, and preserving the heat for 2 hours at 100 ℃;
the second step is that: adding absolute ethyl alcohol into a KH550 silane coupling agent to obtain solution A;
the third step: adding nano titanium dioxide into the solution A; carrying out condensation reflux and continuous stirring reaction for 4h in an ultrasonic cleaning machine in a constant-temperature water bath at 40 ℃; obtaining a solution B;
the fifth step: centrifuging the solution B by using a desk centrifuge to obtain a modified nano titanium dioxide coarse material; and then, cleaning the modified nano titanium dioxide coarse material by using ethanol, and drying to obtain the nano titanium dioxide.
Controlling the mass ratio of the KH550 silane coupling agent to the absolute ethyl alcohol to be 5-8: 50-80; the mass ratio of the nano titanium dioxide to the A liquid is controlled to be 5-9: 60-90.
The preparation process of the modified graphene comprises the following steps:
the first step is as follows: mixing and stirring aminopropyltriethoxysilane and toluene to obtain a solution a; then adding graphene and dicyclohexylcarbodiimide into the solution a, and ultrasonically dispersing for 1h at the temperature of 70-80 ℃ to obtain solution b; controlling the mass ratio of aminopropyltriethoxysilane to toluene to be 5-10: 20-30; controlling the mass ratio of the graphene dicyclohexylcarbodiimide to the liquid a to be 30-40:30-40: 25-40;
the second step is that: carrying out reduced pressure suction filtration on the solution b to obtain a filter cake, washing the filter cake by using absolute ethyl alcohol, and removing a silane monomer to obtain solid powder; and adding the solid powder into a drying oven, and drying at the temperature of 60-80 ℃ for 5h to obtain the modified graphene.
The preparation process of the anti-aging agent comprises the following steps: mixing a coupling agent KH560 with p-aminodiphenylamine, and reacting for 5 hours at 120 ℃ under the protection of nitrogen to obtain a first mixed material; adding the first mixed material into ethanol for ultrasonic dispersion for 10 min; and (3) putting the dried white carbon black into a high-speed mixer, respectively spraying ethanol solution of the first mixed material, stirring for 5min, discharging, drying in vacuum at 120 ℃ for 6h, and washing with absolute ethanol to obtain the modified anti-aging agent.
Controlling the molar ratio of the coupling agent KH560 to the p-aminodiphenylamine to be 1: 1-1.3; the mass ratio of the first mixed material to the ethanol is controlled to be 20-30: 55-60.
Comparative example 1
Comparative example 1 is a brake pad on the market;
the samples obtained from the various groups of examples and comparative examples were subjected to performance tests:
pyrolysis activation energy (KJ/mol) Adhesion layer to Metal efficiency (%)
Example 1 968 94.61
Example 2 979 95.63
Example 3 1021 97.25
Comparative example 1 513 30.48
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise forms disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims (9)

1. A brake pad containing an adhesive layer is characterized in that: the brake pad comprises a friction layer, an adhesive layer and a steel backing;
the bonding layer comprises the following raw materials in parts by weight: 50-60 parts of modified polyesterimide resin, 10-15 parts of modified graphene, 12-16 parts of modified anti-aging agent and 8-12 parts of silicon carbide;
the preparation process of the brake pad comprises the following steps:
the first step is as follows: putting the modified graphene and silicon carbide into a drying oven, drying for 2-3h at the temperature of 80-100 ℃, mixing and grinding the modified graphene and the silicon carbide for 1h, and sieving to obtain a solid mixture; adding the solid mixture into modified polyesterimide resin, adding an anti-aging agent, and stirring and mixing for 3-4h at the temperature of 300-350 ℃ to obtain an adhesive layer; controlling the mass ratio of the modified graphene to the silicon carbide to be 10-15: 8-12, controlling the mass ratio of the solid mixture, the modified polyesterimide resin and the anti-aging agent to be 18-27:50-60: 12-16;
the second step is that: heating the hot press to 280-300 ℃ at 280-500 kgf/cm2Then, putting the friction layer into a cavity of a hot press, putting the bonding layer obtained in the first step into the cavity of the hot press after flattening, flattening the bonding layer, putting a steel backing on the bonding layer, and keeping the pressure for 4-10 minutes; obtaining a semi-finished brake pad; and then placing the semi-finished brake pad into a curing furnace, preserving the heat for 2-3 hours at the temperature of 220-260 ℃, and cooling to room temperature to obtain the brake pad containing the bonding layer.
2. The brake pad with the adhesive layer according to claim 1, wherein the preparation process of the modified polyester-imide resin comprises the following steps:
the first step is as follows: adding the modified nano titanium dioxide into N, N-dimethylformamide, and performing ultrasonic dispersion for 2 hours to obtain a mixed solution a;
step two, dripping m-phenylenediamine into the mixed solution a, stirring for 30min after dripping the m-phenylenediamine, continuously adding (4, 4' -isopropyldiphenoxy) diphthalic anhydride, and continuously stirring for 3 h; obtaining a mixed solution b;
the third step: carrying out ultrasonic treatment on the obtained mixed solution b for 10min, putting the treated mixed solution b into a vacuum drying oven, and vacuumizing the mixed solution b to remove bubbles in the mixed solution b;
the fourth step: pouring the treated mixed solution b onto a glass plate, and uniformly coating the mixed solution b onto the glass plate by using a film scraping machine; placing the scraped glass plate in a vacuum drying oven, vacuumizing for 4h at 80 ℃, and then heating to 40 ℃ from 120 ℃ each time, and preserving the heat of each temperature gradient for 45 min; taking out the cooled glass plate, transferring the cooled glass plate to a forced air drying oven, preserving the heat at 260 ℃ for 45min, preserving the heat at 280 ℃ for 0.5h, and naturally cooling to room temperature; and then stripping the film by water bath to remove the obtained modified polyesterimide resin from the glass plate.
3. The brake pad with the adhesive layer according to claim 2, wherein the mass ratio of the modified nano titanium dioxide, the N, N-dimethylformamide, the m-phenylenediamine, the (4, 4' -isopropyldiphenoxy) diphthalic anhydride is controlled to be 8-10: 30-40: 2-4:3-5.
4. The brake pad containing the adhesive layer according to claim 1, wherein the preparation process of the modified nano titanium dioxide comprises the following steps:
the first step is as follows: putting the dried nano titanium dioxide into the oven again, and preserving the heat for 2 hours at 100 ℃;
the second step is that: adding absolute ethyl alcohol into a KH550 silane coupling agent to obtain solution A;
the third step: adding nano titanium dioxide into the solution A; carrying out condensation reflux and continuous stirring reaction for 4h in an ultrasonic cleaning machine in a constant-temperature water bath at 40 ℃; obtaining a solution B;
the fifth step: centrifuging the solution B by using a desk centrifuge to obtain a modified nano titanium dioxide coarse material; and then, cleaning the modified nano titanium dioxide coarse material by using ethanol, and drying to obtain the nano titanium dioxide.
5. The brake pad with the adhesive layer according to claim 4, wherein the mass ratio of the KH550 silane coupling agent to the absolute ethyl alcohol is controlled to be 5-8: 50-80; the mass ratio of the nano titanium dioxide to the A liquid is controlled to be 5-9: 60-90.
6. The brake pad with the adhesive layer according to claim 1, wherein the preparation process of the modified graphene comprises the following steps:
the first step is as follows: mixing and stirring aminopropyltriethoxysilane and toluene to obtain a solution a; then adding graphene and dicyclohexylcarbodiimide into the solution a, and ultrasonically dispersing for 1h at the temperature of 70-80 ℃ to obtain solution b; controlling the mass ratio of aminopropyltriethoxysilane to toluene to be 5-10: 20-30; controlling the mass ratio of the graphene dicyclohexylcarbodiimide to the liquid a to be 30-40:30-40: 25-40;
the second step is that: carrying out reduced pressure suction filtration on the solution b to obtain a filter cake, washing the filter cake by using absolute ethyl alcohol, and removing a silane monomer to obtain solid powder; and adding the solid powder into a drying oven, and drying at the temperature of 60-80 ℃ for 5h to obtain the modified graphene.
7. The brake pad with the adhesive layer according to claim 1, wherein the process for preparing the anti-aging agent comprises the following steps: mixing a coupling agent KH560 with p-aminodiphenylamine, and reacting for 5 hours at 120 ℃ under the protection of nitrogen to obtain a first mixed material; adding the first mixed material into ethanol for ultrasonic dispersion for 10 min; and (3) putting the dried white carbon black into a high-speed mixer, respectively spraying ethanol solution of the first mixed material, stirring for 5min, discharging, drying in vacuum at 120 ℃ for 6h, and washing with absolute ethanol to obtain the modified anti-aging agent.
8. The brake pad with the adhesive layer according to claim 7, wherein the molar ratio of the coupling agent KH560 to the p-aminodiphenylamine is controlled to be 1: 1-1.3; the mass ratio of the first mixed material to the ethanol is controlled to be 20-30: 55-60.
9. A preparation process of a brake pad containing an adhesive layer is characterized by comprising the following steps:
the first step is as follows: putting the modified graphene and silicon carbide into a drying oven, drying for 2-3h at the temperature of 80-100 ℃, mixing and grinding the modified graphene and the silicon carbide for 1h, and sieving to obtain a solid mixture; adding the solid mixture into modified polyesterimide resin, adding an anti-aging agent, and stirring and mixing for 3-4h at the temperature of 300-350 ℃ to obtain an adhesive layer; controlling the mass ratio of the modified graphene to the silicon carbide to be 10-15: 8-12, controlling the mass ratio of the solid mixture, the modified polyesterimide resin and the anti-aging agent to be 18-27:50-60: 12-16;
the second step is that: heating the hot press to 280-300 DEG CAt 280 to 500kgf/cm2Then, putting the friction layer into a cavity of a hot press, putting the bonding layer obtained in the first step into the cavity of the hot press after flattening, flattening the bonding layer, putting a steel backing on the bonding layer, and keeping the pressure for 4-10 minutes; obtaining a semi-finished brake pad; and then placing the semi-finished brake pad into a curing furnace, preserving the heat for 2-3 hours at the temperature of 220-260 ℃, and cooling to room temperature to obtain the brake pad containing the bonding layer.
CN202110232512.0A 2021-03-03 2021-03-03 Brake pad containing adhesive layer and preparation process of brake pad Pending CN112877026A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
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JP2002266915A (en) * 2001-03-06 2002-09-18 Hitachi Chem Co Ltd Automobile non-asbestos disc brake pad
CN105505288A (en) * 2015-12-04 2016-04-20 中南大学 Polyimide tackiness agent and preparation method thereof
CN105715720A (en) * 2016-01-31 2016-06-29 瑞阳汽车零部件(仙桃)有限公司 Environment-friendly brake block with double-layer composite structure
CN105969307A (en) * 2016-06-03 2016-09-28 青岛基宏汽车部件有限公司 Bonding layer of brake pad, brake pad with bonding layer and preparation process of brake pad
CN108895102A (en) * 2018-07-11 2018-11-27 薛向东 A kind of preparation method of heat resistant and wear resistant type brake block
CN109135345A (en) * 2018-08-01 2019-01-04 安徽锦华氧化锌有限公司 A kind of method of the rubber product anti-old coupling agent modified Nano carbon white of ionic liquid-
CN109824895A (en) * 2019-02-27 2019-05-31 济南大学 A kind of preparation and its application of modified ultra-branching polyimide resin
CN110382654A (en) * 2017-03-06 2019-10-25 日立化成株式会社 Friction material composition, friction material and friction member

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002266915A (en) * 2001-03-06 2002-09-18 Hitachi Chem Co Ltd Automobile non-asbestos disc brake pad
CN105505288A (en) * 2015-12-04 2016-04-20 中南大学 Polyimide tackiness agent and preparation method thereof
CN105715720A (en) * 2016-01-31 2016-06-29 瑞阳汽车零部件(仙桃)有限公司 Environment-friendly brake block with double-layer composite structure
CN105969307A (en) * 2016-06-03 2016-09-28 青岛基宏汽车部件有限公司 Bonding layer of brake pad, brake pad with bonding layer and preparation process of brake pad
CN110382654A (en) * 2017-03-06 2019-10-25 日立化成株式会社 Friction material composition, friction material and friction member
CN108895102A (en) * 2018-07-11 2018-11-27 薛向东 A kind of preparation method of heat resistant and wear resistant type brake block
CN109135345A (en) * 2018-08-01 2019-01-04 安徽锦华氧化锌有限公司 A kind of method of the rubber product anti-old coupling agent modified Nano carbon white of ionic liquid-
CN109824895A (en) * 2019-02-27 2019-05-31 济南大学 A kind of preparation and its application of modified ultra-branching polyimide resin

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