CN107383762A - A kind of preparation method of enhanced phenolic aldehyde friction resistance material for automobile - Google Patents

A kind of preparation method of enhanced phenolic aldehyde friction resistance material for automobile Download PDF

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CN107383762A
CN107383762A CN201710536315.1A CN201710536315A CN107383762A CN 107383762 A CN107383762 A CN 107383762A CN 201710536315 A CN201710536315 A CN 201710536315A CN 107383762 A CN107383762 A CN 107383762A
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sesame oil
resistance material
friction resistance
phenolic aldehyde
automobile
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王海燕
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Dongguan Jia Xin New Mstar Technology Ltd
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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
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    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G8/00Condensation polymers of aldehydes or ketones with phenols only
    • C08G8/04Condensation polymers of aldehydes or ketones with phenols only of aldehydes
    • C08G8/08Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
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    • C08G8/00Condensation polymers of aldehydes or ketones with phenols only
    • C08G8/04Condensation polymers of aldehydes or ketones with phenols only of aldehydes
    • C08G8/08Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
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Abstract

The invention discloses a kind of preparation method of the enhanced phenolic aldehyde friction resistance material for automobile, comprise the following steps:Phenol and sesame oil are mixed, partial catalyst reaction is added under certain temperature, obtains sesame oil phenol mixture, heating, part formaldehyde is added, follow-up continuous temperature reaction is mixed, adds remaining formaldehyde and catalyst, reaction system cools down when occurring muddy, 45 50 DEG C of vacuum dehydrations are cooled to, stop dehydration when reaction system becomes transparent, add absolute ethyl alcohol and stirring dissolving, room temperature discharging is cooled to, obtains sesame oil modified phenolic resin;Prepare organo montmorillonite;By sesame oil modified phenolic resin, organo montmorillonite, sepiolite fibre, hollow carbon fiber, calcium carbonate, graphite, dispersant, obtained mixture 35min of pressurize 15 in hydraulic forming machine, then room temperature is stripped in natural cooling, heat treatment, enhanced phenolic aldehyde friction resistance material is made, the material friction wear properties are good, excellent in mechanical performance, free phenol content is small, environmental protection.

Description

A kind of preparation method of enhanced phenolic aldehyde friction resistance material for automobile
Technical field:
The present invention relates to field of compound material, is specifically related to a kind of system of the enhanced phenolic aldehyde friction resistance material for automobile Preparation Method.
Background technology:
At present, with automobile at a high speed, heavily loaded, comfortable and safe direction develop, there is an urgent need to high performance for traffic department Friction resistance material, such as higher heat decomposition temperature, good hot restorability, enough friction factors, preferable wearability and compared with Low noise.This synthesis friction resistance material is typically made up of components such as matrix resin, reinforcing fiber, frictional property regulators.Base The effect of body resin mainly bonds together each component in material, makes organic whole, therefore the property of matrix resin The combination property of friction resistance material can be just determined significantly.Phenolic resin is that one kind finds and obtains wide variety of synthesis tree earliest Fat, and raw material is easy to get, cost is cheap, and its backbone structure contains substantial amounts of phenyl ring, has that heat-resist, mechanics is strong after cured The advantages that spending height, stable performance, hard wear resistant, resistance to most of chemical reagent, therefore by the widely matrix as friction resistance material Resin.As the application environment of friction resistance material becomes increasingly harsher, common phenolic resin can not meet many high-new skills The requirement in art field, thus using various technologies and method phenolic aldehyde is carried out the improvement of synthesis technique and the exploitation of new technology and Modification to synthetic resin improves the combination property of friction resistance material, it has also become the core of friction resistance material matrix phenolic resin research Intracardiac appearance.
Chinese patent (201010123740.6) discloses a kind of boron, linseed oil double-modification phenolic resin-based friction resistance composite wood Material and preparation method thereof, blending phenolic resin as matrix resin, mass fraction 20-24% of the composite by mass fraction 36-40% Glass fibre, mass fraction 16-19% nitrile rubber, mass fraction be 4-6 silica, mass fraction 8-10% Carborundum, mass fraction 3-6% molybdenum disulfide and mass fraction 2-4% copper powder composition, the blending phenolic resin base Body by mass fraction 28-32% modification of flax oil phenolic resin and mass fraction 68-72% boron modified phenolic resin it is pre- Polymers mixes.Although the addition of nitrile rubber can improve the impact strength of matrix, also cause the abrasion loss of material Increase.
Chinese patent (201510472319.9) discloses a kind of preparation method of sepiolite fibre friction resistance material, first by sea Afrodite fiber, phenolic resin, carboxyl nitrsofluoro rubber, 2- thiol benzothiazoles are added in mixer, heating stirring, cooling To room temperature, then steel fibre, graphite, white carbon, barium sulfate, n-butyl boronate, diphenyl silicon two are added in gained mixture A Alcohol, it is passed through CO2, mixing, gained mixture B is finally subjected to precompressed, compression molding, heat treatment successively, produced.The material is same Also a certain amount of rubber is added to improve the mechanical property of material, and adds a certain amount of organic solvent, is had to environment necessarily Harm.
The content of the invention:
The invention discloses a kind of preparation method of the enhanced phenolic aldehyde friction resistance material for automobile, phenol made from this method Aldehyde friction resistance material mechanical property is good, and friction and wear behavior is excellent, and free phenol content is environment-protecting and non-poisonous less than 0.05%.
To achieve the above object, the present invention uses following technical scheme:
A kind of preparation method of enhanced phenolic aldehyde friction resistance material for automobile, comprises the following steps:
(1) phenol and sesame oil are mixed evenly, are to slowly warm up to 130-150 DEG C, after stirring 10min, add 1/2 Catalyst, isothermal reaction 1-4h, reaction are cooled to room temperature after terminating, obtain sesame oil-phenol mixture;
(2) sesame oil-phenol mixture warming while stirring is added into 2/3 formaldehyde into reaction system to 50-80 DEG C, After being stirred 30min, stirring is warming up to 100-120 DEG C, reacts 10min, remaining formaldehyde and catalyst is continuously added, when anti- When answering system appearance muddy, cooled down, be cooled to 45-50 DEG C of beginning vacuum dehydration, when reaction system becomes transparent, stopped de- Water, absolute ethyl alcohol and stirring dissolving is added, be cooled to room temperature discharging, obtain sesame oil modified phenolic resin;
(3) dimethyldimethoxysil,ne and isopropanol are mixed evenly, nano imvite are then added, after mixing Ultrasonic 3-6h under 1000W power, per ultrasonic 30min, stop 30min, filtered after the completion of supersound process, solid is dried to obtain organic Montmorillonite;
(4) by sesame oil modified phenolic resin obtained above, organo montmorillonite, sepiolite fibre, hollow carbon fiber, carbon Sour calcium, graphite, dispersant are added in mixer and mixed, obtained mixture pressurize 15-35min in hydraulic forming machine, so Room temperature is stripped in natural cooling afterwards, heat treatment, enhanced phenolic aldehyde friction resistance material is made.
As the preferred of above-mentioned technical proposal, in step (1), the phenol, sesame oil, the mass ratio of catalyst are 1: (0.3-0.6):(0.0012-0.0017).
As the preferred of above-mentioned technical proposal, the catalyst is the mixed liquor of p-methyl benzenesulfonic acid and glacial acetic acid, the two matter It is (2-3.5) to measure ratio:1.
As the preferred of above-mentioned technical proposal, in step (2), the addition of the formaldehyde is sesame oil-phenol mixture The 73% of quality.
As the preferred of above-mentioned technical proposal, in step (3), dimethyldimethoxysil,ne, isopropanol, nano imvite Mass ratio be (0.3-0.5):50:3.
As the preferred of above-mentioned technical proposal, in step (4), each component content is respectively in parts by weight:Sesame Oil modified phenolic resin 40-65 parts, organo montmorillonite 7-13 parts, sepiolite fibre 4-9 parts, hollow carbon fiber 2-5 parts, calcium carbonate 5-10 parts, graphite 5-10 parts, dispersant 1-4 parts.
As the preferred of above-mentioned technical proposal, in step (4), the condition of the pressurize is that pressure is 25-40MPa, temperature For 155-175 DEG C.
As the preferred of above-mentioned technical proposal, in step (4), the dispersant is sodium metasilicate.
As the preferred of above-mentioned technical proposal, in step (4), the condition of the heat treatment is first from room temperature with 10 DEG C of speed Rate is warming up to 220 DEG C, is incubated 1h, is then cooled to 150 DEG C with 5 DEG C/min speed, 1h is incubated, then with 15 DEG C/min speed Rate is warming up to 410 DEG C, is incubated 1h, is cooled to 150 DEG C, is incubated 1.5h.
The invention has the advantages that:
The present invention is modified using the more cheap sesame oil of price to phenolic resin, and sesame oil main component is 3,4- Methylenedioxyphenol, it can react with the phenolic hydroxyl group on phenol with formaldehyde, and obtained phenol-formaldehyde resin modified stability is good, Toughness is big, and heat resistance is good.
The present invention adds appropriate organo montmorillonite, its piece in the modification phenolic resin-based body material of obtained sesame oil Thickness degree is small, and layer surface is coated using dimethylformamide dimethyl epoxide, the good dispersion in matrix material, and the present invention also addition sea Afrodite fiber, hollow carbon fiber, graphite etc., effectively improve the friction and wear behavior of phenolic resin material.
Embodiment:
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving The present invention is released, any restriction will not be formed to the present invention.
Embodiment 1
A kind of preparation method of enhanced phenolic aldehyde friction resistance material for automobile, comprises the following steps:
(1) phenol and sesame oil are mixed evenly, are to slowly warm up to 130 DEG C, after stirring 10min, add 1/2 catalysis Agent, isothermal reaction 1h, reaction are cooled to room temperature after terminating, obtain sesame oil-phenol mixture;Wherein, phenol, sesame oil, urge The mass ratio of agent is 1:0.3:0.0012;The catalyst is the mixed liquor of p-methyl benzenesulfonic acid and glacial acetic acid, the two mass ratio For 2:1;
(2) by sesame oil-phenol mixture warming while stirring to 50 DEG C, 2/3 formaldehyde is added into reaction system, is stirred After mixing 30min, stirring is warming up to 100 DEG C, reacts 10min, remaining formaldehyde and catalyst is continuously added, when reaction system goes out When existing muddy, cooled down, be cooled to 45-50 DEG C of beginning vacuum dehydration, when reaction system becomes transparent, stop dehydration, add Absolute ethyl alcohol and stirring dissolves, and is cooled to room temperature discharging, obtains sesame oil modified phenolic resin;Wherein, the addition of formaldehyde is sesame The 73% of sesame oil-phenol mixture quality;
(3) dimethyldimethoxysil,ne and isopropanol are mixed evenly, nano imvite are then added, after mixing Ultrasonic 3h under 1000W power, per ultrasonic 30min, stop 30min, filtered after the completion of supersound process, solid is dried to obtain organic illiteracy De- soil;Wherein, dimethyldimethoxysil,ne, isopropanol, the mass ratio of nano imvite are 0.3:50:3;
(4) by sesame oil modified phenolic resin obtained above, organo montmorillonite, sepiolite fibre, hollow carbon fiber, carbon Sour calcium, graphite, dispersant are added in mixer and mixed, obtained mixture pressurize 15min in hydraulic forming machine, then certainly So room temperature is stripped in cooling, heat treatment, enhanced phenolic aldehyde friction resistance material is made;
Wherein, each component content is respectively in parts by weight:40 parts of sesame oil modified phenolic resin, 7 parts of organo montmorillonite, 4 parts of sepiolite fibre, 2 parts of hollow carbon fiber, 5 parts of calcium carbonate, 5 parts of graphite, 1 part of dispersant;
The condition of pressurize is that pressure is 25MPa, and temperature is 155 DEG C;
The condition of heat treatment is incubated 1h, then with 5 DEG C/min's to be first warming up to 220 DEG C from room temperature with 10 DEG C of speed Speed is cooled to 150 DEG C, is incubated 1h, is then warming up to 410 DEG C with 15 DEG C/min speed, is incubated 1h, is cooled to 150 DEG C, protects Warm 1.5h.
Embodiment 2
A kind of preparation method of enhanced phenolic aldehyde friction resistance material for automobile, comprises the following steps:
(1) phenol and sesame oil are mixed evenly, are to slowly warm up to 150 DEG C, after stirring 10min, add 1/2 catalysis Agent, isothermal reaction 4h, reaction are cooled to room temperature after terminating, obtain sesame oil-phenol mixture;Wherein, phenol, sesame oil, urge The mass ratio of agent is 1:0.6:0.0017;The catalyst is the mixed liquor of p-methyl benzenesulfonic acid and glacial acetic acid, the two mass ratio For 3.5:1;
(2) by sesame oil-phenol mixture warming while stirring to 80 DEG C, 2/3 formaldehyde is added into reaction system, is stirred After mixing 30min, stirring is warming up to 120 DEG C, reacts 10min, remaining formaldehyde and catalyst is continuously added, when reaction system goes out When existing muddy, cooled down, be cooled to 45-50 DEG C of beginning vacuum dehydration, when reaction system becomes transparent, stop dehydration, add Absolute ethyl alcohol and stirring dissolves, and is cooled to room temperature discharging, obtains sesame oil modified phenolic resin;Wherein, the addition of formaldehyde is sesame The 73% of sesame oil-phenol mixture quality;
(3) dimethyldimethoxysil,ne and isopropanol are mixed evenly, nano imvite are then added, after mixing Ultrasonic 6h under 1000W power, per ultrasonic 30min, stop 30min, filtered after the completion of supersound process, solid is dried to obtain organic illiteracy De- soil;Wherein, dimethyldimethoxysil,ne, isopropanol, the mass ratio of nano imvite are 0.5:50:3;
(4) by sesame oil modified phenolic resin obtained above, organo montmorillonite, sepiolite fibre, hollow carbon fiber, carbon Sour calcium, graphite, dispersant are added in mixer and mixed, obtained mixture pressurize 35min in hydraulic forming machine, then certainly So room temperature is stripped in cooling, heat treatment, enhanced phenolic aldehyde friction resistance material is made;
Wherein, each component content is respectively in parts by weight:65 parts of sesame oil modified phenolic resin, organo montmorillonite 13 Part, 9 parts of sepiolite fibre, 5 parts of hollow carbon fiber, 10 parts of calcium carbonate, 10 parts of graphite, 4 parts of dispersant;
The condition of pressurize is that pressure is 40MPa, and temperature is 175 DEG C;
The condition of heat treatment is incubated 1h, then with 5 DEG C/min's to be first warming up to 220 DEG C from room temperature with 10 DEG C of speed Speed is cooled to 150 DEG C, is incubated 1h, is then warming up to 410 DEG C with 15 DEG C/min speed, is incubated 1h, is cooled to 150 DEG C, protects Warm 1.5h.
Embodiment 3
A kind of preparation method of enhanced phenolic aldehyde friction resistance material for automobile, comprises the following steps:
(1) phenol and sesame oil are mixed evenly, are to slowly warm up to 135 DEG C, after stirring 10min, add 1/2 catalysis Agent, isothermal reaction 1-4h, reaction are cooled to room temperature after terminating, obtain sesame oil-phenol mixture;Wherein, phenol, sesame oil, The mass ratio of catalyst is 1:0.4:0.0014;The catalyst is the mixed liquor of p-methyl benzenesulfonic acid and glacial acetic acid, the two quality Than for 2.5:1;
(2) by sesame oil-phenol mixture warming while stirring to 60 DEG C, 2/3 formaldehyde is added into reaction system, is stirred After mixing 30min, stirring is warming up to 105 DEG C, reacts 10min, remaining formaldehyde and catalyst is continuously added, when reaction system goes out When existing muddy, cooled down, be cooled to 45-50 DEG C of beginning vacuum dehydration, when reaction system becomes transparent, stop dehydration, add Absolute ethyl alcohol and stirring dissolves, and is cooled to room temperature discharging, obtains sesame oil modified phenolic resin;Wherein, the addition of formaldehyde is sesame The 73% of sesame oil-phenol mixture quality;
(3) dimethyldimethoxysil,ne and isopropanol are mixed evenly, nano imvite are then added, after mixing Ultrasonic 4h under 1000W power, per ultrasonic 30min, stop 30min, filtered after the completion of supersound process, solid is dried to obtain organic illiteracy De- soil;Wherein, dimethyldimethoxysil,ne, isopropanol, the mass ratio of nano imvite are 0.35:50:3;
(4) by sesame oil modified phenolic resin obtained above, organo montmorillonite, sepiolite fibre, hollow carbon fiber, carbon Sour calcium, graphite, dispersant are added in mixer and mixed, obtained mixture pressurize 20min in hydraulic forming machine, then certainly So room temperature is stripped in cooling, heat treatment, enhanced phenolic aldehyde friction resistance material is made;
Wherein, each component content is respectively in parts by weight:50 parts of sesame oil modified phenolic resin, 8 parts of organo montmorillonite, 5 parts of sepiolite fibre, 3 parts of hollow carbon fiber, 6 parts of calcium carbonate, 6 parts of graphite, 2 parts of dispersant;
The condition of pressurize is that pressure is 30MPa, and temperature is 160 DEG C;
The condition of heat treatment is incubated 1h, then with 5 DEG C/min's to be first warming up to 220 DEG C from room temperature with 10 DEG C of speed Speed is cooled to 150 DEG C, is incubated 1h, is then warming up to 410 DEG C with 15 DEG C/min speed, is incubated 1h, is cooled to 150 DEG C, protects Warm 1.5h.
Embodiment 4
A kind of preparation method of enhanced phenolic aldehyde friction resistance material for automobile, comprises the following steps:
(1) phenol and sesame oil are mixed evenly, are to slowly warm up to 140 DEG C, after stirring 10min, add 1/2 catalysis Agent, isothermal reaction 3h, reaction are cooled to room temperature after terminating, obtain sesame oil-phenol mixture;Wherein, phenol, sesame oil, urge The mass ratio of agent is 1:0.5:0.0014;The catalyst is the mixed liquor of p-methyl benzenesulfonic acid and glacial acetic acid, the two mass ratio For 3:1;
(2) by sesame oil-phenol mixture warming while stirring to 70 DEG C, 2/3 formaldehyde is added into reaction system, is stirred After mixing 30min, stirring is warming up to 110 DEG C, reacts 10min, remaining formaldehyde and catalyst is continuously added, when reaction system goes out When existing muddy, cooled down, be cooled to 45-50 DEG C of beginning vacuum dehydration, when reaction system becomes transparent, stop dehydration, add Absolute ethyl alcohol and stirring dissolves, and is cooled to room temperature discharging, obtains sesame oil modified phenolic resin;Wherein, the addition of formaldehyde is sesame The 73% of sesame oil-phenol mixture quality;
(3) dimethyldimethoxysil,ne and isopropanol are mixed evenly, nano imvite are then added, after mixing Ultrasonic 5h under 1000W power, per ultrasonic 30min, stop 30min, filtered after the completion of supersound process, solid is dried to obtain organic illiteracy De- soil;Wherein, dimethyldimethoxysil,ne, isopropanol, the mass ratio of nano imvite are 0.4:50:3;
(4) by sesame oil modified phenolic resin obtained above, organo montmorillonite, sepiolite fibre, hollow carbon fiber, carbon Sour calcium, graphite, dispersant are added in mixer and mixed, obtained mixture pressurize 25min in hydraulic forming machine, then certainly So room temperature is stripped in cooling, heat treatment, enhanced phenolic aldehyde friction resistance material is made;
Wherein, each component content is respectively in parts by weight:55 parts of sesame oil modified phenolic resin, organo montmorillonite 10 Part, 6 parts of sepiolite fibre, 4 parts of hollow carbon fiber, 7 parts of calcium carbonate, 7 parts of graphite, 3 parts of dispersant;
The condition of pressurize is that pressure is 35MPa, and temperature is 165 DEG C;
The condition of heat treatment is incubated 1h, then with 5 DEG C/min's to be first warming up to 220 DEG C from room temperature with 10 DEG C of speed Speed is cooled to 150 DEG C, is incubated 1h, is then warming up to 410 DEG C with 15 DEG C/min speed, is incubated 1h, is cooled to 150 DEG C, protects Warm 1.5h.
Embodiment 5
A kind of preparation method of enhanced phenolic aldehyde friction resistance material for automobile, comprises the following steps:
(1) phenol and sesame oil are mixed evenly, are to slowly warm up to 145 DEG C, after stirring 10min, add 1/2 catalysis Agent, isothermal reaction 3.5h, reaction are cooled to room temperature after terminating, obtain sesame oil-phenol mixture;Wherein, phenol, sesame oil, The mass ratio of catalyst is 1:0.55:0.0016;The catalyst is the mixed liquor of p-methyl benzenesulfonic acid and glacial acetic acid, the two quality Than for 3:1;
(2) by sesame oil-phenol mixture warming while stirring to 75 DEG C, 2/3 formaldehyde is added into reaction system, is stirred After mixing 30min, stirring is warming up to 115 DEG C, reacts 10min, remaining formaldehyde and catalyst is continuously added, when reaction system goes out When existing muddy, cooled down, be cooled to 45-50 DEG C of beginning vacuum dehydration, when reaction system becomes transparent, stop dehydration, add Absolute ethyl alcohol and stirring dissolves, and is cooled to room temperature discharging, obtains sesame oil modified phenolic resin;Wherein, the addition of formaldehyde is sesame The 73% of sesame oil-phenol mixture quality;
(3) dimethyldimethoxysil,ne and isopropanol are mixed evenly, nano imvite are then added, after mixing Ultrasonic 5.5h under 1000W power, per ultrasonic 30min, stop 30min, filtered after the completion of supersound process, solid is dried to obtain organic Montmorillonite;Wherein, dimethyldimethoxysil,ne, isopropanol, the mass ratio of nano imvite are 0.45:50:3;
(4) by sesame oil modified phenolic resin obtained above, organo montmorillonite, sepiolite fibre, hollow carbon fiber, carbon Sour calcium, graphite, dispersant are added in mixer and mixed, obtained mixture pressurize 30min in hydraulic forming machine, then certainly So room temperature is stripped in cooling, heat treatment, enhanced phenolic aldehyde friction resistance material is made;
Wherein, each component content is respectively in parts by weight:60 parts of sesame oil modified phenolic resin, organo montmorillonite 11 Part, 8 parts of sepiolite fibre, 4.5 parts of hollow carbon fiber, 9 parts of calcium carbonate, 8 parts of graphite, 3.5 parts of dispersant;
The condition of pressurize is that pressure is 35MPa, and temperature is 170 DEG C;
The condition of heat treatment is incubated 1h, then with 5 DEG C/min's to be first warming up to 220 DEG C from room temperature with 10 DEG C of speed Speed is cooled to 150 DEG C, is incubated 1h, is then warming up to 410 DEG C with 15 DEG C/min speed, is incubated 1h, is cooled to 150 DEG C, protects Warm 1.5h.
The performance of phenolic resin material produced by the present invention is tested below.
Test result is as follows:
The normal temperature of table 1, during load 20kg, the relation of phenolic aldehyde friction resistance material coefficient of friction and rotating speed
Rotating speed/r/min 200 400 600 800
Coefficient of friction 0.553 0.532 0.511 0.508
The normal temperature of table 2, during rotating speed 400r/min, the relation of phenolic aldehyde friction resistance material coefficient of friction and load
Load/kg 10 15 20 25
Coefficient of friction 0.609 0.537 0.532 0.512
The relation of the load 20kg of table 3, rotating speed 400r/min phenolic aldehyde friction resistance material coefficient of friction and temperature
Temperature 100 150 200 250
Coefficient of friction 0.529 0.523 0.515 0.508
The hardness and impact property of the phenolic aldehyde friction resistance material of table 4
Hardness Impact strength kI/m2
Embodiment 1 78.8 5.12
Embodiment 2 79.5 5.25
Embodiment 3 78.6 5.19
Embodiment 4 79.5 5.17
Embodiment 5 78.9 5.25
From the point of view of above table data, phenolic aldehyde friction resistance material coefficient of friction produced by the present invention is good, and coefficient of friction by turn The influence of speed, temperature and load is small, and hardness is big, and shock resistance is good.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to the present invention Equivalent transformation, or be directly or indirectly used in other related technical areas, the patent protection of the invention similarly included In the range of.

Claims (9)

1. the preparation method of a kind of enhanced phenolic aldehyde friction resistance material for automobile, it is characterised in that comprise the following steps:
(1) phenol and sesame oil are mixed evenly, are to slowly warm up to 130-150 DEG C, after stirring 10min, add 1/2 catalysis Agent, isothermal reaction 1-4h, reaction are cooled to room temperature after terminating, obtain sesame oil-phenol mixture;
(2) by sesame oil-phenol mixture warming while stirring to 50-80 DEG C, 2/3 formaldehyde is added into reaction system, is stirred After mixing 30min, stirring is warming up to 100-120 DEG C, reacts 10min, continuously adds remaining formaldehyde and catalyst, work as reactant When system occurs muddy, cooled down, be cooled to 45-50 DEG C of beginning vacuum dehydration, when reaction system becomes transparent, stop dehydration, Absolute ethyl alcohol and stirring dissolving is added, room temperature discharging is cooled to, obtains sesame oil modified phenolic resin;
(3) dimethyldimethoxysil,ne and isopropanol are mixed evenly, nano imvite are then added, after mixing Ultrasonic 3-6h under 1000W power, per ultrasonic 30min, stop 30min, filtered after the completion of supersound process, solid is dried to obtain organic Montmorillonite;
(4) by sesame oil modified phenolic resin obtained above, organo montmorillonite, sepiolite fibre, hollow carbon fiber, carbonic acid Calcium, graphite, dispersant are added in mixer and mixed, obtained mixture pressurize 15-35min in hydraulic forming machine, then Room temperature is stripped in natural cooling, heat treatment, enhanced phenolic aldehyde friction resistance material is made.
A kind of 2. preparation method of enhanced phenolic aldehyde friction resistance material for automobile as claimed in claim 1, it is characterised in that: In step (1), the phenol, sesame oil, the mass ratio of catalyst are 1:(0.3-0.6):(0.0012-0.0017).
A kind of 3. preparation method of enhanced phenolic aldehyde friction resistance material for automobile as claimed in claim 1, it is characterised in that: The catalyst is the mixed liquor of p-methyl benzenesulfonic acid and glacial acetic acid, and the two mass ratio is (2-3.5):1.
A kind of 4. preparation method of enhanced phenolic aldehyde friction resistance material for automobile as claimed in claim 1, it is characterised in that: In step (2), the addition of the formaldehyde is the 73% of sesame oil-phenol mixture quality.
A kind of 5. preparation method of enhanced phenolic aldehyde friction resistance material for automobile as claimed in claim 1, it is characterised in that: In step (3), dimethyldimethoxysil,ne, isopropanol, the mass ratio of nano imvite are (0.3-0.5):50:3.
A kind of 6. preparation method of enhanced phenolic aldehyde friction resistance material for automobile as claimed in claim 1, it is characterised in that: In step (4), each component content is respectively in parts by weight:Sesame oil modified phenolic resin 40-65 parts, organo montmorillonite 7-13 parts, sepiolite fibre 4-9 parts, hollow carbon fiber 2-5 parts, calcium carbonate 5-10 parts, graphite 5-10 parts, dispersant 1-4 parts.
A kind of 7. preparation method of enhanced phenolic aldehyde friction resistance material for automobile as claimed in claim 1, it is characterised in that: In step (4), the condition of the pressurize is that pressure is 25-40MPa, and temperature is 155-175 DEG C.
A kind of 8. preparation method of enhanced phenolic aldehyde friction resistance material for automobile as claimed in claim 1, it is characterised in that: In step (4), the dispersant is sodium metasilicate.
A kind of 9. preparation method of enhanced phenolic aldehyde friction resistance material for automobile as claimed in claim 1, it is characterised in that: In step (4), the condition of the heat treatment is incubated 1h to be first warming up to 220 DEG C from room temperature with 10 DEG C of speed, then with 5 DEG C/ Min speed is cooled to 150 DEG C, is incubated 1h, is then warming up to 410 DEG C with 15 DEG C/min speed, is incubated 1h, is cooled to 150 DEG C, it is incubated 1.5h.
CN201710536315.1A 2017-07-04 2017-07-04 A kind of preparation method of enhanced phenolic aldehyde friction resistance material for automobile Withdrawn CN107383762A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108644270A (en) * 2018-05-10 2018-10-12 浙江科马摩擦材料股份有限公司 A kind of aramid fiber clutch surface and its preparation process
CN116640278A (en) * 2023-06-06 2023-08-25 郑州轻工业大学 Modified phenolic resin and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1752122A (en) * 2005-09-29 2006-03-29 江苏大学 Linseed oil modified phenol formaldehyde resin for friction material and its preparation method
CN101250272A (en) * 2008-03-25 2008-08-27 武汉理工大学 Formaldehyde-phenol resin/vermiculite nano composite friction material and preparation method thereof
CN106633861A (en) * 2016-12-13 2017-05-10 苏州赛斯德工程设备有限公司 High-strength friction material for vehicles

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1752122A (en) * 2005-09-29 2006-03-29 江苏大学 Linseed oil modified phenol formaldehyde resin for friction material and its preparation method
CN101250272A (en) * 2008-03-25 2008-08-27 武汉理工大学 Formaldehyde-phenol resin/vermiculite nano composite friction material and preparation method thereof
CN106633861A (en) * 2016-12-13 2017-05-10 苏州赛斯德工程设备有限公司 High-strength friction material for vehicles

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王文广: "《塑料配方设计》", 31 July 2004, 化学工业出版社 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108644270A (en) * 2018-05-10 2018-10-12 浙江科马摩擦材料股份有限公司 A kind of aramid fiber clutch surface and its preparation process
CN116640278A (en) * 2023-06-06 2023-08-25 郑州轻工业大学 Modified phenolic resin and preparation method thereof
CN116640278B (en) * 2023-06-06 2024-06-07 郑州轻工业大学 Modified phenolic resin and preparation method thereof

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