CN107936916A - A kind of preparation method of modified carbon fiber friction particles - Google Patents
A kind of preparation method of modified carbon fiber friction particles Download PDFInfo
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- CN107936916A CN107936916A CN201711094986.3A CN201711094986A CN107936916A CN 107936916 A CN107936916 A CN 107936916A CN 201711094986 A CN201711094986 A CN 201711094986A CN 107936916 A CN107936916 A CN 107936916A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1436—Composite particles, e.g. coated particles
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/02—Copolymers with acrylonitrile
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
- D01F9/17—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate from lignin
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/55—Epoxy resins
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
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Abstract
The invention discloses a kind of preparation method of modified carbon fiber friction particles, by asphalt powder, epoxy resin, butadiene-styrene rubber, nitrile rubber, coconut husk, phenol, the raw materials such as polyvinyl alcohol are made, the present invention prepares porous carbon fiber with coconut husk, handled through multiple modified technique, obtain high mechanical properties, the porous carbon fiber of high wear resistance, again with kneading after nitrile rubber starching, inside has stable hollow structure, higher elasticity is taken into account, the higher porosity and the stability of high-temperature behavior, possess wider application range compared with conventional friction material, raw material sources of the present invention are wide at the same time, preparation method is simple, obtained friction particles are wear-resistant, high temperature resistant, have good market prospects.
Description
Technical field
The present invention relates to friction resistance material technical field, more particularly to a kind of preparation method of modified carbon fiber friction particles.
Background technology
Product of the friction resistance material as modern industry, plays more and more important in national economy and people's social life
Effect.With auto industry high speed development, application of the friction resistance material in automobile making is also more and more extensive, continuous improvement
Safe, the comfortable and environmentally friendly exploitation needed also to Automotive Friction Materials proposes new demand.Automobile brake sheet passes through at work
Extraneous pressure is born, brake drag effect is produced, so that vehicle achievees the purpose that braking.
Friction material is fabricated to after various raw materials are weighed in the dry state and is mixed to get mixture at present, wherein add
Particulate matter divides three classes：First kind class is mostly the material such as the coke of 1-3mm or so, graphite, tyre talc, waste paper pulverized particles, this kind of
Material basic performance is single, the overall performance of friction material is influenced limited；Second class is through liquid resin and conventional friction material
The particulate matter that material mixture high-speed stirred forms, this kind of material are solid after high temperature is suppressed during friction material following process
Change lacks flexibility；Three classes are common compounding rubber things, and compounding rubber thing has enough elasticity, but the porosity is low, high temperatures
Can be poor.The above particulate matter suffers from the limitation of material or technique, causes performance single, can not take into account the porosity,
The stable friction performance of elasticity and high temperature.
Porous carbon fiber is a kind of new porous fibrous sorbing material, is had because of its unique pore structure and form
There are the specific surface area of more general porous charcoal bigger, the pore volume of higher, the faster rate of adsorption and stronger power of regeneration.Since upper
Since century the seventies appearance, air purification, exhaust gas wastewater treatment, military protection, metal recovery, electricity just it have been widely used in
Sub- equipment etc., and it also shows excellent performance in terms of friction resistance material preparation.At present, the porous carbon of in the market
Fiber mainly has polyacrylonitrile-radical porous carbon fiber, asphaltic base porous carbon fiber, viscose glue base porous carbon fiber and phenolic aldehyde Quito hole
Carbon fiber etc., toughness of the different carbon fibers after carbonization speed, production carbon rate, porosity and carbonization are different.Therefore, it is necessary to
With reference to traditional carbon fibres preparation method, pass through Optimal improvements technique, there is provided aperture is small, porosity is high, fiber homogeneity is good and
With reference to the strong porous carbon fiber of power.
At the same time, since the preparation process of carbon fiber includes carbonization or graphitization so that the carbon atom of carbon fiber surface
Stack orientation is more consistent, atom interlamellar spacing smaller, so fiber surface shows as nonpolar and chemical inertness, other carbon fiber surface
There are the shortcomings such as hydrophobic, smooth, absorption property is low in face, and the storeroom interface adhesion for causing carbon fiber compound with it is poor.Therefore, need
Carbon fiber surface is modified, improve its interface binding intensity with composite material.
The content of the invention
A kind of the defects of the object of the invention is exactly to make up prior art, there is provided preparation of modified carbon fiber friction particles
Method.
The present invention is achieved by the following technical solutions：
A kind of preparation method of modified carbon fiber friction particles, comprises the following steps：
（1）Spinning solution is placed in electrostatic spinning machine, receiver is wrapped up using aluminium-foil paper, as-spun fibre is collected in aluminium-foil paper
On, spinning process technological parameter is positive pressure 15-16kV, negative pressure 1.5-2kV, promotes speed 0.04-0.05mm/min, receiving velocity
30-32r/min, distance is 15-18cm between syringe needle and receiver, and 30-40 DEG C of environment temperature is quiet at room temperature after the completion of spinning
Put one day, obtain as-spun fibre, then be placed in baking oven, be warming up to 160-170 DEG C and cure 60-70 minutes, sent again after taking-up
Enter in tube furnace, rise to 750-850 DEG C, when insulation 1-2 is small from room temperature in a nitrogen atmosphere with the heating rate of 5-10 DEG C/min,
It is spare that carbon fiber is obtained after natural cooling；
（2）Using step 1 gained carbon fiber as anode, graphite is cathode, in the ammonium phosphate electrolyte that mass fraction is 8-10%
In, it is 0.3-0.35A/m to control current density2, anodized 1.5-2 minutes, collects carbon fiber and is rinsed only with clear water, obtained
It is spare to modified carbon fiber；
（3）Step 2 gained modified carbon fiber is sent into cutter and is chopped to 2-5mm, places into and 30- is impregnated in coupling agent solution
Taking-up is dried spare after forty minutes；
（4）The epoxy resin for being 15-20% to the uniform spray concentration of step 3 gained coupling agent pretreatment carbon fiber, wherein asphalt mixtures modified by epoxy resin
Fat dosage pre-processes the 20-40% of carbon fiber quality for coupling agent, after epoxy resin absorption completely, adds the drip of 160-200 mesh
Blue or green powder, it is spare when curing 5-6 is small at 180-220 DEG C after mixing；
（5）Step 4 products therefrom is sent in liquid nitrile rubber and is beaten, wherein liquid nitrile rubber dosage is fine for carbon modified
The 15-25% of dimension, beating consistency 6-8%, beating degree are 40-42 ° of SR, after the completion of stirring to the uniform slurry of material dispersion；
（6）By step 5 gained slurry and liquid styrene butadiene rubber in mass ratio（5-7）：Kneading is carried out in 1 common input masticator,
After the completion of will gained mixture put into comminutor in be granulated, screening granularity be 40-60 mesh particle, up to the present invention friction
Particle.
The preparation method of spinning solution is that coconut husk crushed 100-120 mesh sieves in the step 1, after drying with phenol, dense
Sulfuric acid is in mass ratio（5-7）：（20-25）：（0.6-0.9）It is mixed and stirred for uniformly, being placed in 140-160 DEG C of oil bath pan and reacting
100-120 minutes, room temperature is down to afterwards, adds in sodium hydroxide and pH is to neutrality, product and 80% dioxanes aqueous solution are pressed into body
Product ratio 1：（9-11）It is mixed 60-80 minutes, centrifuges and filter, by the rotated evaporimeter of filtrate in 60-70 after removing residue
Concentrated at DEG C, remove dioxanes, obtain pure liquefied substance, then with polyvinyl alcohol in mass ratio（45-46）：（4-5）Hydrogen-oxygen is used after mixing
Change sodium and adjust pH to 10-11, add formalin afterwards, be warming up to 80-85 DEG C, postcooling is obtained to room temperature when reaction 2-3 is small
Spinning solution.
Coupling agent solution is the aqueous solution for the aluminium titanium composite coupler that mass fraction is 20-30% in the step 3.
Coupling agent pretreatment carbon fiber, epoxy resin, the mass ratio of asphalt powder are 100 in the step 4：（20-40）：
（0.5-2）.
Kneading temperature is 35-45 DEG C in the step 6, and the kneading time is 7-8 minutes.
The preparation method of the spinning solution, the ratio between the formaldehyde of addition and the amount of phenol material are n（Formaldehyde）：n（Phenol）=
（1.4-1.5）：1.
It is an advantage of the invention that：
The method that the present invention uses Liquefaction Products in Phenol, is more active small moleculars by coconut husk liquefaction, avoids conventional wooden procatarxis structure from answering
It is miscellaneous and contain a large amount of impurity, the defects of spinning effect is undesirable is directly used in, then high polymer is connected as by unit of phenolic aldehyde, have more
The production carbon rate and porosity of fast carbonization speed, higher, and phenolic resin due to formed cross-linked structure, so carbonization after still may be used
Certain toughness is kept, is handled in conjunction with the technological parameter of electrostatic spinning optimization, more traditional melt spinning, makes fibre diameter more
Carefully, nanoscale is reached, so that the specific surface area with bigger and stronger wear resistance, obtained carbon fiber passes through and butyronitrile rubber
Kneading after glue starching, inside have stable hollow structure, have taken into account higher elasticity, the higher porosity and high-temperature behavior
Stability, possesses wider application range compared with conventional friction material, while raw material sources of the present invention are wide, and preparation method is simple,
Obtained friction particles are wear-resistant, high temperature resistant, have good market prospects.
Embodiment
A kind of preparation method of modified carbon fiber friction particles, comprises the following steps：
（1）Spinning solution is placed in electrostatic spinning machine, receiver is wrapped up using aluminium-foil paper, as-spun fibre is collected in aluminium-foil paper
On, spinning process technological parameter is positive pressure 15kV, negative pressure 1.5kV, promotes speed 0.04mm/min, receiving velocity 30r/min, pin
Distance is 15cm between head and receiver, and 30 DEG C of environment temperature, stands one day at room temperature after the completion of spinning, obtains just spinning fine
Dimension, then is placed in baking oven, is warming up to 160 DEG C and cures 60 minutes, is re-fed into after taking-up in tube furnace, in a nitrogen atmosphere with
The heating rate of 5 DEG C/min rises to 750 DEG C, when insulation 1 is small from room temperature, and it is spare to obtain carbon fiber after natural cooling；
（2）Using step 1 gained carbon fiber as anode, graphite is cathode, in the ammonium phosphate electrolyte that mass fraction is 8%, control
Current density processed is 0.3A/m2, anodized 1.5 minutes, collects carbon fiber and is rinsed only with clear water, obtain modified carbon fiber
It is spare；
（3）Step 2 gained modified carbon fiber is sent into cutter and is chopped to 2mm, places into and 30 points is impregnated in coupling agent solution
Taking-up is dried spare after clock, and wherein coupling agent solution is the aqueous solution for the aluminium titanium composite coupler that mass fraction is 20%；
（4）The epoxy resin for being 15% to the uniform spray concentration of step 3 gained coupling agent pretreatment carbon fiber, its epoxy resin
Dosage pre-processes the 20% of carbon fiber quality for coupling agent, after epoxy resin absorption completely, adds 160 mesh asphalt powders, mixes
Spare when curing 5 is small at 180 DEG C afterwards, wherein coupling agent pretreatment carbon fiber, epoxy resin, the mass ratio of asphalt powder are 100：
30：1；
（5）Step 4 products therefrom is sent in liquid nitrile rubber and is beaten, wherein liquid nitrile rubber dosage is fine for carbon modified
The 15% of dimension, beating consistency 6%, beating degree be 40 ° of SR, after the completion of stir to the uniform slurry of material dispersion；
（6）By step 5 gained slurry and liquid styrene butadiene rubber in mass ratio 6：Kneading, kneading are carried out in 1 common input masticator
Temperature be 35 DEG C, the kneading time be 7 minutes, after the completion of will gained mixture put into comminutor in be granulated, screening granularity be
The particle of 40 mesh, up to friction particles of the present invention.
The preparation method of the spinning solution is that coconut husk crushed 100 mesh sieves, after drying with phenol, the concentrated sulfuric acid in mass ratio
6：22：0.8 is mixed and stirred for uniformly, being placed in 140 DEG C of oil bath pans and reacting 100 minutes, is down to room temperature afterwards, adds sodium hydroxide
PH is neutralized to neutrality, by product and 80% dioxanes aqueous solution by volume 1：10 are mixed 60 minutes, centrifuge and filter, remove
The rotated evaporimeter of filtrate is concentrated at 60 DEG C after removing residue, dioxanes is removed, obtains pure liquefied substance, then matter is pressed with polyvinyl alcohol
Measure ratio 45：PH to 10 is adjusted with sodium hydroxide after 4 mixing, adds formalin, the formaldehyde of addition and the amount of phenol material afterwards
The ratio between be n（Formaldehyde）：n（Phenol）=1.5：1,80 DEG C are warming up to, postcooling obtains spinning solution to room temperature when reaction 2 is small.
Claims (6)
1. a kind of preparation method of modified carbon fiber friction particles, it is characterised in that comprise the following steps：
（1）Spinning solution is placed in electrostatic spinning machine, receiver is wrapped up using aluminium-foil paper, as-spun fibre is collected in aluminium-foil paper
On, spinning process technological parameter is positive pressure 15-16kV, negative pressure 1.5-2kV, promotes speed 0.04-0.05mm/min, receiving velocity
30-32r/min, distance is 15-18cm between syringe needle and receiver, and 30-40 DEG C of environment temperature is quiet at room temperature after the completion of spinning
Put one day, obtain as-spun fibre, then be placed in baking oven, be warming up to 160-170 DEG C and cure 60-70 minutes, sent again after taking-up
Enter in tube furnace, rise to 750-850 DEG C, when insulation 1-2 is small from room temperature in a nitrogen atmosphere with the heating rate of 5-10 DEG C/min,
It is spare that carbon fiber is obtained after natural cooling；
（2）Using step 1 gained carbon fiber as anode, graphite is cathode, in the ammonium phosphate electrolyte that mass fraction is 8-10%
In, it is 0.3-0.35A/m to control current density2, anodized 1.5-2 minutes, collects carbon fiber and is rinsed only with clear water, obtained
It is spare to modified carbon fiber；
（3）Step 2 gained modified carbon fiber is sent into cutter and is chopped to 2-5mm, places into and 30- is impregnated in coupling agent solution
Taking-up is dried spare after forty minutes；
（4）The epoxy resin for being 15-20% to the uniform spray concentration of step 3 gained coupling agent pretreatment carbon fiber, wherein asphalt mixtures modified by epoxy resin
Fat dosage pre-processes the 20-40% of carbon fiber quality for coupling agent, after epoxy resin absorption completely, adds the drip of 160-200 mesh
Blue or green powder, it is spare when curing 5-6 is small at 180-220 DEG C after mixing；
（5）Step 4 products therefrom is sent in liquid nitrile rubber and is beaten, wherein liquid nitrile rubber dosage is fine for carbon modified
The 15-25% of dimension, beating consistency 6-8%, beating degree are 40-42 ° of SR, after the completion of stirring to the uniform slurry of material dispersion；
（6）By step 5 gained slurry and liquid styrene butadiene rubber in mass ratio（5-7）：Kneading is carried out in 1 common input masticator,
After the completion of will gained mixture put into comminutor in be granulated, screening granularity be 40-60 mesh particle, up to the present invention friction
Particle.
2. the preparation method of modified carbon fiber friction particles according to claim 1, it is characterised in that in the step 1
The preparation method of spinning solution is that coconut husk crushed 100-120 mesh sieves, after drying with phenol, the concentrated sulfuric acid in mass ratio（5-7）：
（20-25）：（0.6-0.9）It is mixed and stirred for uniformly, being placed in 140-160 DEG C of oil bath pan and reacting 100-120 minutes, be down to afterwards
Room temperature, adds in sodium hydroxide and pH is to neutrality, by product and 80% dioxanes aqueous solution by volume 1：（9-11）It is mixed
60-80 minutes, centrifuge and filter, concentrate the rotated evaporimeter of filtrate at 60-70 DEG C after removing residue, remove dioxanes,
Pure liquefied substance is obtained, then with polyvinyl alcohol in mass ratio（45-46）：（4-5）PH to 10-11 is adjusted with sodium hydroxide after mixing, it
After add formalin, be warming up to 80-85 DEG C, postcooling obtains spinning solution to room temperature when reaction 2-3 is small.
3. the preparation method of modified carbon fiber friction particles according to claim 1, it is characterised in that in the step 3
Coupling agent solution is the aqueous solution for the aluminium titanium composite coupler that mass fraction is 20-30%.
4. the preparation method of modified carbon fiber friction particles according to claim 1, it is characterised in that in the step 4
Coupling agent pretreatment carbon fiber, epoxy resin, the mass ratio of asphalt powder are 100：（20-40）：（0.5-2）.
5. the preparation method of modified carbon fiber friction particles according to claim 1, it is characterised in that in the step 6
Kneading temperature is 35-45 DEG C, and the kneading time is 7-8 minutes.
6. the preparation method of spinning solution according to claim 3, it is characterised in that the formaldehyde of addition and the amount of phenol material
The ratio between be n（Formaldehyde）：n（Phenol）=（1.4-1.5）：1.
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| CN111426734A (en) * | 2020-04-30 | 2020-07-17 | 榆林学院 | Nano Cu/graphene composite material modified electrode, preparation method thereof and application of nano Cu/graphene composite material modified electrode in detection of hydroquinone |
| CN112124256A (en) * | 2020-09-08 | 2020-12-25 | 上海国由复合材料科技有限公司 | Tread cleaning device grinder for high-speed motor train and preparation process |
| CN117088360A (en) * | 2023-10-19 | 2023-11-21 | 河北省科学院能源研究所 | Preparation method of nano porous carbon additive for rubber engineering equipment |
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| CN107936916B (en) | 2020-03-10 |
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