CN101250272B - Formaldehyde-phenol resin/vermiculite nano composite friction material and preparation method thereof - Google Patents
Formaldehyde-phenol resin/vermiculite nano composite friction material and preparation method thereof Download PDFInfo
- Publication number
- CN101250272B CN101250272B CN2008100471428A CN200810047142A CN101250272B CN 101250272 B CN101250272 B CN 101250272B CN 2008100471428 A CN2008100471428 A CN 2008100471428A CN 200810047142 A CN200810047142 A CN 200810047142A CN 101250272 B CN101250272 B CN 101250272B
- Authority
- CN
- China
- Prior art keywords
- vermiculite
- parts
- resol
- nano composite
- composite material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Braking Arrangements (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention relates to friction material and a preparation process thereof. Phenol resin/vermiculite nano composite friction material is characterized in that the material is prepared by raw materials that phenol resin/vermiculite nano composite material, carbon fiber, steel fiber, barium sulfate, kaolin, silica dioxide, wollastonite, calcium carbonate, graphite, molybdenum disulphite, butadiene acrylonitrile rubber and hexamethylenetetramine, wherein of each raw material with parts by mass is: 10-20 phenol resin/vermiculite nano composite material, 1-5 carbon fiber, 2-5 steel fiber, 15-20 barium sulfate, 1-5 kaolin, 1-8 silica dioxide, 1-15 wollastonite, 1-15 calcium carbonate, 3-10 graphite, 2-5 molybdenum disulphite, 2-12 butadiene acrylonitrile rubber and 0.8-2 hexamethylenetetramine. Friction material which is prepared using phenol resin/vermiculite nano composite material as binding agent has the advantages of excellent heat resistance property, stable friction parameter, and small heat fading and low wear rate and the like, since the phenol resin/vermiculite nano composite material has the advantages of high heat decomposition temperature and excellent toughness.
Description
Technical field
The present invention relates to a kind of friction resistance material and preparation method thereof, particularly a kind of friction resistance material of making brake facing and preparation method thereof that is used to.
Background technology
Friction resistance material is an indispensable important materials in the modern industry.In the last few years,, friction resistance material was had higher requirement, as require friction resistance material to have the excellent high-temperature frictional behaviour, promptly kept stable at quite high temperature, pressure, velocity range coefficient of interal friction along with the high speed of vehicle and machinery; Good character of heat-fading and heat are restorative; Wear resistance is good, long service life etc.So far, fibrous magnesium silicate base frictional drag material, powder metallurgy inanimate matter metal friction resistance material, Semi-metal Friction Materials and carbon fiber friction resistance material have been developed.In these friction resistance materials, except that powder metallurgy friction materials, other three kinds all is the polymer-based carbon friction resistance composite material.The polymer-based carbon friction resistance composite material is to utilize polymer adhesive with the each several part of material uniformly, bond together securely, so tackiness agent affects the overall performance of friction resistance material.In friction resistance material was formed, matrix resin is the easiest being influenced by heat and degrading, thereby cause the inefficacy of whole goods.
Resol is that the use of polymer-based carbon friction resistance material at most also is a most important class body material.Usually the employed resol of friction resistance material is synthetic phenol formaldehyde resin under the acid catalysis effect.Resol contains more aromatic ring owing in this body structure, and has better heat-resisting performance and mechanical property.Yet the methyne key of resol oxidation scission under the thermooxidizing condition causes the oxygenolysis of resin easily.Common resol can steady in a long-termly use below 200 ℃, if surpass 250 ℃, can oxidation take place obviously, and the thermolysis phenomenon is quite serious when surpassing 300 ℃, has limited the application of resol in the high-performance friction resistance material, presses for its modification.Carried out both at home and abroad at present much about the heat resistance modified research of resol.As using boric acid, molybdic acid or wolframic acid with the phenolic hydroxyl group esterification; The methods such as hydrogen atom that substitute phenolic hydroxyl group with organosilicon, rare earth element, cyano group make the better resol of thermotolerance.
Clay of laminar silicate (polynite, talcum, vermiculite etc.) is a kind of silicate minerals of the laminate structure that is made of silicon-oxygen tetrahedron and aluminium-oxygen octahedra.Over past ten years, it is found that layered silicate/polymer nanocomposites all improves a lot than polymeric matrix at aspects such as mechanical property, thermotolerance and barriers.About the also existing bibliographical information of layered silicate/bakelite resin nano composite material.Employing in-situ polymerizations such as Guo Jiangshan have prepared resol/organic montmorillonoid nano composite material, but the heat decomposition temperature of hot analysis revealed matrix material only can be brought up to 370 ℃ by 353 ℃ of pure phenolic resin, and heat decomposition temperature improves limited.Application suspension polycondensation methods such as Zhou Chixing have prepared resol/Nano composite material of montmorillonite, and it is also very little that the heat decomposition temperature of hot analysis revealed bakelite resin nano composite material improves degree.Vermiculite has that heat rejection is good, fracture absorbs can height and advantage such as interlamellar spacing is bigger, but its interlayer charge height, relative difficulty with the organic cation exchange, the intractability that organises is big.We discover by adopting hydrochloric acid and sodium-chlor mixing solutions or sodium chloride solution that vermiculite is carried out interlayer structure and modify, and can reduce interlayer charge, with the vermiculite that organises of organic cation exchange preparation, can make most of positively charged ion (Mg between vermiculite layers again
2+, Ca
2+, Na
+, K
+Deng) replaced by organic cation, make vermiculite and resol form exfoliated nano-composite, thereby significantly improve the heat decomposition temperature of resol, its heat decomposition temperature can reach more than 500 ℃, has advantages such as resistance toheat is good, stable friction factor, character of heat-fading is little, wear rate is low with this vermiculite/bakelite resin nano composite material as the friction resistance material of adhesive preparation.
Summary of the invention
The object of the present invention is to provide good compound base frictional drag material of resol/vermiculite nano of a kind of resistance toheat and preparation method thereof.
To achieve these goals, technical scheme of the present invention is: the compound base frictional drag material of a kind of resol/vermiculite nano, it is characterized in that it is by resol/vermiculite nano composite material, carbon fiber, steel fiber, barium sulfate, kaolin, silicon-dioxide, wollastonite, lime carbonate, graphite, molybdenumdisulphide, paracril and hexamethylenetetramine feedstock production form, the shared mass fraction of each raw material is: resol/vermiculite nano composite material 10~20, carbon fiber 1~5, steel fiber 2~5, barium sulfate 15~20, kaolin 1~5, silica 1~8, wollastonite 1~15, lime carbonate 1~15, graphite 3~10, molybdenumdisulphide 2~5, paracril 2~12, hexamethylenetetramine 0.8~2.
Described resol/vermiculite nano composite material organises vermiculite and resol by the melting intercalation method preparation, or organise vermiculite and phenol, formaldehyde and acid catalyst prepare by in-situ inserted method.
The described vermiculite that organises with the common vermiculite of 200~300 orders or expanded vermiculite through cetyl trimethylammonium bromide solution or the octadecyl dimethyl benzyl brometo de amonio Processing of Preparation that organises.Preferably the common vermiculite of 200~300 orders is handled in hydrochloric acid/sodium chloride solution, hydrochloric acid and sodium-chlor mass ratio are 1: 2~1: 3, again through cetyl trimethylammonium bromide solution or the octadecyl dimethyl benzyl brometo de amonio Processing of Preparation that organises; Or 200~300 order expanded vermiculites are handled in sodium chloride solution, the NaCl mass concentration is 1~3%, again through cetyl trimethylammonium bromide solution or the octadecyl dimethyl benzyl brometo de amonio solution Processing of Preparation that organises.
The preparation method of the compound base frictional drag material of above-mentioned a kind of resol/vermiculite nano is characterized in that carrying out as follows:
(1) mass ratio by each raw material is: resol/vermiculite nano composite material 10~20, carbon fiber 1~5, steel fiber 2~5, barium sulfate 15~20, kaolin 1~5, silica 1~8, wollastonite 1~15, lime carbonate 1~15, graphite 3~10, molybdenumdisulphide 2~5, paracril 2~12, hexamethylenetetramine 0.8~2 is chosen resol/vermiculite nano composite material, carbon fiber, steel fiber, barium sulfate, kaolin, silicon-dioxide, wollastonite, lime carbonate, graphite, molybdenumdisulphide, paracril and hexamethylenetetramine raw material, pour stirrer into, mix;
(2) with above-mentioned compound in mould, compression molding, forming pressure is 20~30MPa, molding temperature is under 160~180 ℃, behind the 30s venting once, heat-insulation pressure keeping 15~30min then;
(3) goods that the demoulding is made are put into baking oven, rise to 120 ℃ from room temperature, insulation 1h; Be warmed up to 130 ℃, insulation 1h; Be warmed up to 140 ℃, insulation 1h; Be warmed up to 155 ℃, insulation 1h; Be warmed up to 165 ℃, insulation 2h; Be warmed up to 175 ℃, insulation 2h; Be warmed up to 180 ℃, insulation 1h; Then, take out goods and be cooled to room temperature, promptly obtain product.
The preparation of described resol/vermiculite nano composite material:
(1) processing that organises of vermiculite: the mass fraction by each raw material is: 10 part of 200~300 common vermiculite of order and 3 parts of mass concentrations are 36~38% hydrochloric acid, 3 parts of sodium-chlor, 100 parts of deionized water centrifugations after stirring 5h under 50 ℃ of constant temperatures, filter, with deionized water repetitive scrubbing chloride ion-containing not to the elutant, the vermiculite that to handle mixes with 100 parts of deionized waters again, add 3 parts of cetyl trimethylammonium bromides or octadecyl dimethyl benzyl brometo de amonio, stir 12h down in 80 ℃ of constant temperatures, centrifugation afterwards, filter, with the deionized water repetitive scrubbing to there not being bromide anion, with the vermiculite cleaned under 120 ℃ of conditions dry 2 hours, grind 200 mesh sieves, promptly made the vermiculite that organises;
(2) preparation of melting intercalation method resol/vermiculite nano composite material: get above-mentioned 3 parts of the vermiculites of organising by mass fraction, even with the blend of 100 parts of powdery thermoplastic resol, be heated to 160~170 ℃, powerful mechanical stirring 2h, grind 200 mesh sieves after the cooling, promptly made resol/vermiculite nano composite material.
The preparation of described resol/vermiculite nano composite material:
(1) processing that organises of vermiculite: the mass fraction by each raw material is: 10 part of 200~300 order expanded vermiculite and 3 parts of sodium-chlor, 100 parts of deionized water centrifugations after stirring 5h under 50 ℃ of constant temperatures, filtration, with deionized water repetitive scrubbing chloride ion-containing not to the elutant; The expanded vermiculite that to handle mixes with 100 parts of deionized waters again, add 3 parts of cetyl trimethylammonium bromides or octadecyl dimethyl benzyl brometo de amonio, stir 12h down in 80 ℃ of constant temperatures, centrifugation afterwards, filtration, with the deionized water repetitive scrubbing to there not being bromide anion, with the vermiculite cleaned under 120 ℃ of conditions dry 2 hours, ground 200 mesh sieves, promptly make the vermiculite that organises;
(2) preparation of in-situ inserted method resol/vermiculite nano composite material: get above-mentioned 8 parts of the vermiculites of organising by mass fraction, 400 parts of phenol, mass concentration is 292 parts in 37% a formaldehyde, 2 parts of oxalic acid, mass concentration is 4 parts of the hydrochloric acid of 36-38%, to organise vermiculite, phenol, formaldehyde joins in the reactor simultaneously, and violent stirring 3 hours makes mixed solution be transparence; Use heating in water bath again, when temperature is increased to 65 ℃, add oxalic acid, controlled temperature is at 95 ℃, reacts to stop after 3 hours; Decompression dehydration is 3 hours in 100 ℃ of water-baths, takes out product then, 110 ℃ of baking oven inner dryings 2 hours, grinds 200 mesh sieves after the cooling, promptly makes resol/vermiculite nano composite material.
Beneficial effect of the present invention is as follows: organise vermiculite and resol through hydrochloric acid and sodium-chlor mixing solutions or sodium chloride solution structural modification and organic cation exchange preparation form exfoliated nano composite structure by melt or original position are compound, this nano composite structure significantly improves the thermotolerance of resol and wear resistance, and toughness also is improved simultaneously.Adopt this resol/vermiculite nano composite material to have advantages such as resistance toheat is good, stable friction factor, character of heat-fading is little, wear rate is low as the friction resistance material of adhesive preparation.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1:
(1) processing that organises of vermiculite: 10 parts of (mass fractions, below identical) the common vermiculite of 200 orders and 3 parts of hydrochloric acid are (commercially available, its mass concentration is 36~38%), 3 parts of sodium-chlor, 100 parts of deionized water centrifugations after stirring 5h under 50 ℃ of constant temperatures, filter, with deionized water repetitive scrubbing chloride ion-containing not to the elutant, the vermiculite that to handle mixes with 100 parts of deionized waters again, add 3 parts of cetyl trimethylammonium bromides, stir 12h down in 80 ℃ of constant temperatures, centrifugation afterwards, filter, with the deionized water repetitive scrubbing to there not being bromide anion, with the vermiculite cleaned under 120 ℃ of conditions dry 2 hours, grind 200 mesh sieves, promptly made the vermiculite that organises.
(2) preparation of melting intercalation method resol/vermiculite nano composite material: get above-mentioned 3 parts of the vermiculites of organising, even with the blend of 100 parts of powdery thermoplastic resol, be heated to 160-170 ℃, powerful mechanical stirring 2h, grind 200 mesh sieves after the cooling, promptly made resol/vermiculite nano composite material.
(3) 10 parts of the resol/vermiculite nano composite materials of above-mentioned melting intercalation method preparation (mass fraction, below identical), 2 parts on carbon fiber, 3 parts of steel fibers, 18 parts in barium sulfate, 3 parts of kaolin, 5 parts of silicon-dioxide, 8 parts of wollastonites, 10 parts in lime carbonate, 3 parts in graphite, 2 parts of molybdenumdisulphide, 5 parts of paracrils, 1 part of hexamethylenetetramine; By the quality of above-mentioned each raw material than weighing after, pour stirrer into, pour in the mould after mixing, compression molding, forming pressure is 20MPa, molding temperature is under 160~170 ℃, behind the 30s venting once, heat-insulation pressure keeping 20min then.The goods that the demoulding makes are put into baking oven, rise to 120 ℃, insulation 1h from room temperature; Be warmed up to 130 ℃, insulation 1h; Be warmed up to 140 ℃, insulation 1h; Be warmed up to 155 ℃, insulation 1h; Be warmed up to 165 ℃, insulation 2h; Be warmed up to 175 ℃, insulation 2h; Be warmed up to 180 ℃, insulation 1h; Then, take out goods and be cooled to room temperature, promptly obtain product.The coefficientoffriction of made friction resistance material can be stabilized in 0.35~0.45,350 ℃ of wear rate Δ W less than 5.0 * 10 at 100~350 ℃
-8Cm
3/ Nm, shock strength is greater than 4.8dJ/m
2
Embodiment 2:
(1) processing that organises of vermiculite: 10 part of 300 order expanded vermiculite and 3 parts of sodium-chlor, 100 parts of deionized water centrifugations after stirring 5h under 50 ℃ of constant temperatures, filtration, with deionized water repetitive scrubbing chloride ion-containing not to the elutant.The expanded vermiculite that to handle mixes with 100 parts of deionized waters again, add 3 parts of octadecyl dimethyl benzyl brometo de amonios, stir 12h down in 80 ℃ of constant temperatures, centrifugation afterwards, filtration, with the deionized water repetitive scrubbing to there not being bromide anion, with the vermiculite cleaned under 120 ℃ of conditions dry 2 hours, ground 200 mesh sieves, promptly make the vermiculite that organises.
(2) preparation of in-situ inserted method resol/vermiculite nano composite material: get above-mentioned 8 parts of the vermiculites of organising, 400 parts of phenol, formaldehyde is (commercially available, its mass concentration is 37%) 292 parts, 2 parts of oxalic acid, to organise vermiculite, phenol, formaldehyde joins in the reactor simultaneously, and violent stirring 3 hours makes mixed solution be transparence.Use heating in water bath again, when temperature is increased to 65 ℃, add oxalic acid, controlled temperature is at 95 ℃, reacts to stop after 3 hours.Decompression dehydration is 3 hours in 100 ℃ of water-baths, takes out product then, 110 ℃ of baking oven inner dryings 2 hours, grinds 200 mesh sieves after the cooling, promptly makes resol/vermiculite nano composite material.
(3) resol/vermiculite nano composite material of above-mentioned in-situ inserted method preparation is 15 parts, 4 parts on carbon fiber, 5 parts of steel fibers, 15 parts in barium sulfate, 4 parts of kaolin, 6 parts of silicon-dioxide, 10 parts of wollastonites, 13 parts in lime carbonate, 5 parts in graphite, 3 parts of molybdenumdisulphide, 8 parts of paracrils, 1.6 parts of hexamethylenetetramines.The preparation method is with embodiment 1.
With the friction resistance material of method preparation, its coefficientoffriction can be stabilized in 0.38~0.45,350 ℃ of wear rate Δ W less than 5.0 * 10 at 100~350 ℃ according to the above ratio
-8Cm
3/ Nm, shock strength is greater than 5.0dJ/m
2
Embodiment 3:
The preparation method of the compound base frictional drag material of a kind of resol/vermiculite nano, carry out as follows:
(1) processing that organises of vermiculite: 10 part of 200 common vermiculite of order and 3 parts of hydrochloric acid are (commercially available, mass concentration is 36~38%), 3 parts of sodium-chlor, 100 parts of deionized water centrifugations after stirring 5h under 50 ℃ of constant temperatures, filter, with deionized water repetitive scrubbing chloride ion-containing not to the elutant, the vermiculite that to handle mixes with 100 parts of deionized waters again, add 3 parts of cetyl trimethylammonium bromides, stir 12h down in 80 ℃ of constant temperatures, centrifugation afterwards, filter, with the deionized water repetitive scrubbing to there not being bromide anion, with the vermiculite cleaned under 120 ℃ of conditions dry 2 hours, grind 200 mesh sieves, promptly made the vermiculite that organises.
(2) preparation of melting intercalation method resol/vermiculite nano composite material: get above-mentioned 3 parts of the vermiculites of organising, even with the blend of 100 parts of powdery thermoplastic resol, be heated to 160~170 ℃, powerful mechanical stirring 2h, grind 200 mesh sieves after the cooling, promptly made resol/vermiculite nano composite material.
(3) mass fraction by each raw material is: 10 parts of resol/vermiculite nano composite materials, 1 part on carbon fiber, 2 parts of steel fibers, 15 parts in barium sulfate, 1 part of kaolin, silica 1 part, 1 part of wollastonite, 1 part in lime carbonate, 3 parts in graphite, 2 parts of molybdenumdisulphide, 2 parts of paracrils, hexamethylenetetramine are chosen resol/vermiculite nano composite material, carbon fiber, steel fiber, barium sulfate, kaolin, silicon-dioxide, wollastonite, lime carbonate, graphite, molybdenumdisulphide, paracril and hexamethylenetetramine raw material for 1 part, pour stirrer into, mix; Organise vermiculite and resol of described resol/vermiculite nano composite material prepares by melting intercalation method.
(4) with above-mentioned compound in mould, compression molding, forming pressure is 20MPa, molding temperature is under 160 ℃, behind the 30s venting once, heat-insulation pressure keeping 15min then.
(5) goods that the demoulding is made are put into baking oven, rise to 120 ℃ from room temperature, insulation 1h; Be warmed up to 130 ℃, insulation 1h; Be warmed up to 140 ℃, insulation 1h; Be warmed up to 155 ℃, insulation 1h; Be warmed up to 165 ℃, insulation 2h; Be warmed up to 175 ℃, insulation 2h; Be warmed up to 180 ℃, insulation 1h; Then, take out goods and be cooled to room temperature, promptly obtain product.
Embodiment 4:
The preparation method of the compound base frictional drag material of a kind of resol/vermiculite nano, carry out as follows:
(1) processing that organises of vermiculite: 10 part of 200 order expanded vermiculite and 3 parts of sodium-chlor, 100 parts of deionized water centrifugations after stirring 5h under 50 ℃ of constant temperatures, filtration, with deionized water repetitive scrubbing chloride ion-containing not to the elutant.The expanded vermiculite that to handle mixes with 100 parts of deionized waters again, add 3 parts of octadecyl dimethyl benzyl brometo de amonios, stir 12h down in 80 ℃ of constant temperatures, centrifugation afterwards, filtration, with the deionized water repetitive scrubbing to there not being bromide anion, with the vermiculite cleaned under 120 ℃ of conditions dry 2 hours, ground 200 mesh sieves, promptly make the vermiculite that organises.
(2) preparation of in-situ inserted method resol/vermiculite nano composite material: get above-mentioned 8 parts of the vermiculites of organising, 400 parts of phenol, formaldehyde is (commercially available, mass concentration is 37%) 292 parts, 2 parts of oxalic acid, to organise vermiculite, phenol, formaldehyde joins in the reactor simultaneously, and violent stirring 3 hours makes mixed solution be transparence.Use heating in water bath again, when temperature is increased to 65 ℃, add acid catalyst, controlled temperature is at 95 ℃, reacts to stop after 3 hours.Decompression dehydration is 3 hours in 100 ℃ of water-baths, takes out product then, 110 ℃ of baking oven inner dryings 2 hours, grinds 200 mesh sieves after the cooling, promptly makes resol/vermiculite nano composite material.
(3) mass fraction by each raw material is: 20 parts of resol/vermiculite nano composite materials, 5 parts on carbon fiber, 5 parts of steel fibers, 20 parts in barium sulfate, 5 parts of kaolin, 8 parts of silicon-dioxide, 15 parts of wollastonites, 15 parts in lime carbonate, 10 parts in graphite, 5 parts of molybdenumdisulphide, 12 parts of paracrils, hexamethylenetetramine are chosen resol/vermiculite nano composite material, carbon fiber, steel fiber, barium sulfate, kaolin, silicon-dioxide, wollastonite, lime carbonate, graphite, molybdenumdisulphide, paracril and hexamethylenetetramine raw material for 2 parts, pour stirrer into, mix; Organise vermiculite and phenol, formaldehyde and hydrochloric acid catalyst of described resol/vermiculite nano composite material prepares by in-situ inserted method.
(4) with above-mentioned compound in mould, compression molding, forming pressure is 30MPa, molding temperature is under 180 ℃, behind the 30s venting once, heat-insulation pressure keeping 30min then.
(5) goods that the demoulding is made are put into baking oven, rise to 120 ℃ from room temperature, insulation 1h; Be warmed up to 130 ℃, insulation 1h; Be warmed up to 140 ℃, insulation 1h; Be warmed up to 155 ℃, insulation 1h; Be warmed up to 165 ℃, insulation 2h; Be warmed up to 175 ℃, insulation 2h; Be warmed up to 180 ℃, insulation 1h; Then, take out goods and be cooled to room temperature, promptly obtain product.
The bound value and the interval value of each raw material of the present invention can both be realized the present invention, do not enumerate embodiment one by one at this.
Claims (2)
1. compound base frictional drag material of resol/vermiculite nano, it is characterized in that it is by resol/vermiculite nano composite material, carbon fiber, steel fiber, barium sulfate, kaolin, silicon-dioxide, wollastonite, lime carbonate, graphite, molybdenumdisulphide, paracril and hexamethylenetetramine feedstock production form, the shared mass fraction of each raw material is: resol/vermiculite nano composite material 10~20, carbon fiber 1~5, steel fiber 2~5, barium sulfate 15~20, kaolin 1~5, silica 1~8, wollastonite 1~15, lime carbonate 1~15, graphite 3~10, molybdenumdisulphide 2~5, paracril 2~12, hexamethylenetetramine 0.8~2;
One of following two kinds of methods are adopted in the preparation of described resol/vermiculite nano composite material:
1) first method:
(1) processing that organises of vermiculite: the mass fraction by each raw material is: 10 part of 200~300 common vermiculite of order and 3 parts of mass concentrations are 36~38% hydrochloric acid, 3 parts of sodium-chlor, 100 parts of deionized water centrifugations after stirring 5h under 50 ℃ of constant temperatures, filter, with deionized water repetitive scrubbing chloride ion-containing not to the elutant, the vermiculite that to handle mixes with 100 parts of deionized waters again, add 3 parts of cetyl trimethylammonium bromides or octadecyl dimethyl benzyl brometo de amonio, stir 12h down in 80 ℃ of constant temperatures, centrifugation afterwards, filter, with the deionized water repetitive scrubbing to there not being bromide anion, with the vermiculite cleaned under 120 ℃ of conditions dry 2 hours, grind 200 mesh sieves, promptly made the vermiculite that organises;
(2) preparation of melting intercalation method resol/vermiculite nano composite material: get above-mentioned 3 parts of the vermiculites of organising by mass fraction, even with the blend of 100 parts of powdery thermoplastic resol, be heated to 160~170 ℃, powerful mechanical stirring 2h, grind 200 mesh sieves after the cooling, promptly made resol/vermiculite nano composite material;
2) second method:
(1) processing that organises of vermiculite: the mass fraction by each raw material is: 10 part of 200~300 order expanded vermiculite and 3 parts of sodium-chlor, 100 parts of deionized water centrifugations after stirring 5h under 50 ℃ of constant temperatures, filtration, with deionized water repetitive scrubbing chloride ion-containing not to the elutant; The expanded vermiculite that to handle mixes with 100 parts of deionized waters again, add 3 parts of cetyl trimethylammonium bromides or octadecyl dimethyl benzyl brometo de amonio, stir 12h down in 80 ℃ of constant temperatures, centrifugation afterwards, filtration, with the deionized water repetitive scrubbing to there not being bromide anion, with the vermiculite cleaned under 120 ℃ of conditions dry 2 hours, ground 200 mesh sieves, promptly make the vermiculite that organises;
(2) preparation of in-situ inserted method resol/vermiculite nano composite material: get above-mentioned 8 parts of the vermiculites of organising by mass fraction, 400 parts of phenol, mass concentration is 292 parts in 37% a formaldehyde, 2 parts of oxalic acid, mass concentration is 4 parts of the hydrochloric acid of 36-38%, to organise vermiculite, phenol, formaldehyde joins in the reactor simultaneously, and violent stirring 3 hours makes mixed solution be transparence; Use heating in water bath again, when temperature is increased to 65 ℃, add oxalic acid, controlled temperature is at 95 ℃, reacts to stop after 3 hours; Decompression dehydration is 3 hours in 100 ℃ of water-baths, takes out product then, 110 ℃ of baking oven inner dryings 2 hours, grinds 200 mesh sieves after the cooling, promptly makes resol/vermiculite nano composite material.
2. the preparation method of the compound base frictional drag material of a kind of resol/vermiculite nano as claimed in claim 1 is characterized in that carrying out as follows:
(1) mass fraction by each raw material is: resol/vermiculite nano composite material 10~20, carbon fiber 1~5, steel fiber 2~5, barium sulfate 15~20, kaolin 1~5, silica 1~8, wollastonite 1~15, lime carbonate 1~15, graphite 3~10, molybdenumdisulphide 2~5, paracril 2~12, hexamethylenetetramine 0.8~2, choose resol/vermiculite nano composite material, carbon fiber, steel fiber, barium sulfate, kaolin, silicon-dioxide, wollastonite, lime carbonate, graphite, molybdenumdisulphide, paracril and hexamethylenetetramine raw material, pour stirrer into, mix;
(2) with above-mentioned compound in mould, compression molding, forming pressure is 20~30MPa, molding temperature is under 160~180 ℃, behind the 30s venting once, heat-insulation pressure keeping 15~30min then;
(3) goods that the demoulding is made are put into baking oven, rise to 120 ℃ from room temperature, insulation 1h; Be warmed up to 130 ℃, insulation 1h; Be warmed up to 140 ℃, insulation 1h; Be warmed up to 155 ℃, insulation 1h; Be warmed up to 165 ℃, insulation 2h; Be warmed up to 175 ℃, insulation 2h; Be warmed up to 180 ℃, insulation 1h; Then, take out goods and be cooled to room temperature, promptly obtain product;
One of following two kinds of methods are adopted in the preparation of described resol/vermiculite nano composite material:
1) first method:
(1) processing that organises of vermiculite: the mass fraction by each raw material is: 10 part of 200~300 common vermiculite of order and 3 parts of mass concentrations are 36~38% hydrochloric acid, 3 parts of sodium-chlor, 100 parts of deionized water centrifugations after stirring 5h under 50 ℃ of constant temperatures, filter, with deionized water repetitive scrubbing chloride ion-containing not to the elutant, the vermiculite that to handle mixes with 100 parts of deionized waters again, add 3 parts of cetyl trimethylammonium bromides or octadecyl dimethyl benzyl brometo de amonio, stir 12h down in 80 ℃ of constant temperatures, centrifugation afterwards, filter, with the deionized water repetitive scrubbing to there not being bromide anion, with the vermiculite cleaned under 120 ℃ of conditions dry 2 hours, grind 200 mesh sieves, promptly made the vermiculite that organises;
(2) preparation of melting intercalation method resol/vermiculite nano composite material: get above-mentioned 3 parts of the vermiculites of organising by mass fraction, even with the blend of 100 parts of powdery thermoplastic resol, be heated to 160~170 ℃, powerful mechanical stirring 2h, grind 200 mesh sieves after the cooling, promptly made resol/vermiculite nano composite material;
2) second method:
(1) processing that organises of vermiculite: the mass fraction by each raw material is: 10 part of 200~300 order expanded vermiculite and 3 parts of sodium-chlor, 100 parts of deionized water centrifugations after stirring 5h under 50 ℃ of constant temperatures, filtration, with deionized water repetitive scrubbing chloride ion-containing not to the elutant; The expanded vermiculite that to handle mixes with 100 parts of deionized waters again, add 3 parts of cetyl trimethylammonium bromides or octadecyl dimethyl benzyl brometo de amonio, stir 12h down in 80 ℃ of constant temperatures, centrifugation afterwards, filtration, with the deionized water repetitive scrubbing to there not being bromide anion, with the vermiculite cleaned under 120 ℃ of conditions dry 2 hours, ground 200 mesh sieves, promptly make the vermiculite that organises;
(2) preparation of in-situ inserted method resol/vermiculite nano composite material: get above-mentioned 8 parts of the vermiculites of organising by mass fraction, 400 parts of phenol, mass concentration is 292 parts in 37% a formaldehyde, 2 parts of oxalic acid, mass concentration is 4 parts of the hydrochloric acid of 36-38%, to organise vermiculite, phenol, formaldehyde joins in the reactor simultaneously, and violent stirring 3 hours makes mixed solution be transparence; Use heating in water bath again, when temperature is increased to 65 ℃, add oxalic acid, controlled temperature is at 95 ℃, reacts to stop after 3 hours; Decompression dehydration is 3 hours in 100 ℃ of water-baths, takes out product then, 110 ℃ of baking oven inner dryings 2 hours, grinds 200 mesh sieves after the cooling, promptly makes resol/vermiculite nano composite material.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2008100471428A CN101250272B (en) | 2008-03-25 | 2008-03-25 | Formaldehyde-phenol resin/vermiculite nano composite friction material and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2008100471428A CN101250272B (en) | 2008-03-25 | 2008-03-25 | Formaldehyde-phenol resin/vermiculite nano composite friction material and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN101250272A CN101250272A (en) | 2008-08-27 |
CN101250272B true CN101250272B (en) | 2010-11-03 |
Family
ID=39953886
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN2008100471428A Expired - Fee Related CN101250272B (en) | 2008-03-25 | 2008-03-25 | Formaldehyde-phenol resin/vermiculite nano composite friction material and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN101250272B (en) |
Families Citing this family (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102432785B (en) * | 2011-09-14 | 2013-06-12 | 武汉理工大学 | Method for preparing in-situ dispersion nano polybasic graft modified phenolic resin |
CN103185095B (en) * | 2011-12-29 | 2015-11-18 | 上海壬丰复合材料有限公司 | A kind of for friction sheet for wind energy generator yaw device and manufacture method thereof |
CN103665746B (en) * | 2012-08-30 | 2015-07-01 | 上海壬丰复合材料有限公司 | Micropore friction material with low abrasion and high stability coefficient and manufacturing method thereof |
CN103059809A (en) * | 2012-12-14 | 2013-04-24 | 青岛四方车辆研究所有限公司 | Handmade motor friction ring and preparing method thereof |
CN104194259A (en) * | 2014-08-29 | 2014-12-10 | 宁国飞鹰汽车零部件股份有限公司 | Inorganic nano modified phenolic resin brake pad and preparation process thereof |
CN104565136A (en) * | 2014-12-23 | 2015-04-29 | 江西科技学院 | Composite nanometer brake block manufacturing method |
CN104893230B (en) * | 2015-05-06 | 2018-02-16 | 辽宁航宇星物联仪表科技有限公司 | A kind of diaphragm gas meter bonnet valve seat material |
CN104804440B (en) * | 2015-06-02 | 2018-06-05 | 郑州轻工业学院 | The preparation method of silicon rubber/vermiculite Composite and its silicon rubber/vermiculite Composite obtained |
CN105647482B (en) * | 2016-01-20 | 2018-10-30 | 福州大学 | A kind of ternary aliphatic acid/modified expanded vermiculite composite phase-change energy storage material |
CN105623275A (en) * | 2016-03-16 | 2016-06-01 | 王社兵 | Tear-resistant and heat-resistant silicone rubber cable |
CN107383762A (en) * | 2017-07-04 | 2017-11-24 | 东莞市佳乾新材料科技有限公司 | A kind of preparation method of enhanced phenolic aldehyde friction resistance material for automobile |
CN108752862A (en) * | 2018-06-27 | 2018-11-06 | 巩义市泛锐熠辉复合材料有限公司 | A kind of supercritical CO2The method that auxiliary prepares carbon fiber/phenolic resin composite |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2000319409A (en) * | 1999-05-14 | 2000-11-21 | Hitachi Chem Co Ltd | Friction material |
EP1081406A2 (en) * | 1999-07-30 | 2001-03-07 | Nisshinbo Industries, Inc. | Non-asbestos friction materials |
US6284815B1 (en) * | 1996-06-27 | 2001-09-04 | Akebono Brake Industry Co. Ltd. | Non-asbestos friction material |
CN1377916A (en) * | 2001-03-29 | 2002-11-06 | 中国科学院化学研究所 | Water soluble phenolic resin/nano clay composition and its preparing method |
CN101113204A (en) * | 2007-07-17 | 2008-01-30 | 李军魂 | Formula of ceramic radical friction material for automobile braking friction facing |
-
2008
- 2008-03-25 CN CN2008100471428A patent/CN101250272B/en not_active Expired - Fee Related
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6284815B1 (en) * | 1996-06-27 | 2001-09-04 | Akebono Brake Industry Co. Ltd. | Non-asbestos friction material |
JP2000319409A (en) * | 1999-05-14 | 2000-11-21 | Hitachi Chem Co Ltd | Friction material |
EP1081406A2 (en) * | 1999-07-30 | 2001-03-07 | Nisshinbo Industries, Inc. | Non-asbestos friction materials |
CN1377916A (en) * | 2001-03-29 | 2002-11-06 | 中国科学院化学研究所 | Water soluble phenolic resin/nano clay composition and its preparing method |
CN101113204A (en) * | 2007-07-17 | 2008-01-30 | 李军魂 | Formula of ceramic radical friction material for automobile braking friction facing |
Non-Patent Citations (3)
Title |
---|
JP特开平10-8036A 1998.01.13 |
魏连启.酚醛树脂纳米复合材料及其在摩阻材料中的应用研究.中国优秀博硕士论文全文数据库(硕士)工程科技I辑 2004年第03期.2004,(2004年第03期),26-74. |
魏连启.酚醛树脂纳米复合材料及其在摩阻材料中的应用研究.中国优秀博硕士论文全文数据库(硕士)工程科技I辑 2004年第03期.2004,(2004年第03期),26-74. * |
Also Published As
Publication number | Publication date |
---|---|
CN101250272A (en) | 2008-08-27 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101250272B (en) | Formaldehyde-phenol resin/vermiculite nano composite friction material and preparation method thereof | |
CN105114498B (en) | PPTA composite fibre dry clutch dough sheet and preparation method thereof | |
CN104693678B (en) | Phenolic resin-base composite containing Graphene and preparation method thereof | |
CN104405807B (en) | A kind of preparation method of automobile brake sheet | |
CN103059504B (en) | A kind of wear resistant automobile braking composite material and preparation method thereof that strengthens | |
CN102758870B (en) | A kind of brake for cars friction facing and preparation method thereof | |
CN105111675B (en) | A kind of calcium carbonate crystal whisker reinforced resin-Rubber base friction material and preparation method thereof | |
CN104262622B (en) | The preparation method of the in-situ inserted solution of carboxylated graphene oxide Benzoxazine nanocomposite | |
CN104292409A (en) | Modified phenolic resin and friction material containing same | |
CN103396650B (en) | A kind of modified alkyd resin based friction material | |
CN101956776A (en) | High strength car braking friction plate containing nanomaterial and production method thereof | |
CN101928457A (en) | Carbon-based nano cast nylon composite material and in-situ polymerization preparation method thereof | |
CN102391834A (en) | Preparation method for high temperature-resistant automobile brake lining | |
CN101948608A (en) | Boron, nano-montmorillonite and nitrile-butadiene rubber modified phenolic resin and preparation method thereof | |
CN102977850A (en) | Bamboo charcoal composite fiber friction material and brake pad fabricated therefrom, and method for preparing same | |
Zhao et al. | Wood-plastic materials with organic–inorganic hybrid phase change thermal storage as novel green energy storage composites for building energy conservation | |
CN101270791A (en) | Abrasive dust recycling method in brake disc production | |
CN108050184A (en) | A kind of preparation method of wear-resisting type friction material | |
CN104086947A (en) | Phenol aldehyde molding compound for commutators | |
CN102206482A (en) | Preparation method of carbon fiber brake block | |
CN104194259A (en) | Inorganic nano modified phenolic resin brake pad and preparation process thereof | |
CN102432785A (en) | Method for preparing in-situ dispersion nano polybasic graft modified phenolic resin | |
CN101058678B (en) | Large interlamellar spacing and high activity modified calcium-base montmorillonite and preparation method thereof | |
CN103396651A (en) | Preparation method of modified phenolic resin-base friction material | |
CN102643517B (en) | Method for preparing composite material by blending PHQEP/montmorillonite and modified epoxy resin |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
C17 | Cessation of patent right | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20101103 Termination date: 20130325 |