CN109135294A - A kind of silicon rubber modified white carbon black composite material - Google Patents

A kind of silicon rubber modified white carbon black composite material Download PDF

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Publication number
CN109135294A
CN109135294A CN201810879020.9A CN201810879020A CN109135294A CN 109135294 A CN109135294 A CN 109135294A CN 201810879020 A CN201810879020 A CN 201810879020A CN 109135294 A CN109135294 A CN 109135294A
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carbon black
white carbon
silicon rubber
modified
parts
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陈君华
杨万科
周丽
李启明
郭雨
杨妍
杨河
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Bengbu Wanke Silicon Material Technology Co Ltd
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Bengbu Wanke Silicon Material Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

The present invention relates to field of material technology, specifically, it is related to a kind of silicon rubber modified white carbon black composite material, by weight, including following component: 100~120 parts of methyl vinyl phenyl silicon rubber, 2~8 parts of modified ceramic powder, 10~12 parts of modified white carbon black, 1~2 part of coupling agent, 1~2 part of vulcanizing agent, 0.1~0.2 part of hydroxy silicon oil, 4~8 parts of nano-cellulose, so, so that polymer can not only be with silicon rubber, and it can be reacted with modified ceramic powder, to effectively prevent white carbon black and reunion of the ceramic powder in silicon rubber, substantially improve white carbon black, the interfacial adhesion of ceramic powder and silicon rubber, applied in tire, tire tearing strength and tensile strength can be enhanced.

Description

A kind of silicon rubber modified white carbon black composite material
Technical field:
The present invention relates to field of material technology, and in particular, to a kind of silicon rubber modified white carbon black composite material.
Background technique:
Silicon rubber is a kind of special synthetic rubber, and using silicon oxygen bond as main chain, special structure determines that it has resistance to height It is low temperature, resistance to ozone, radiation hardness, weather-proof and the media such as lubricating oil are shown with excellent chemical inertness.In addition, it also have- 50 DEG C to the 300 DEG C wide scope of applications, elasticity is good, but the silicon rubber heating conduction as filling is very poor, is led by filling Its heating conduction can be improved in hot filler.Heat Conduction Material is widely used in needing in the fields such as Aeronautics and Astronautics, electronics, electrical, automobile The position radiated and conducted heat, with science and technology and industrial progress, electronic component increasingly levels off to densification And miniaturization, to be put forward new requirements to Heat Conduction Material, it is desirable to which Heat Conduction Material can provide reliable dissipate for electronic component Hot approach, and insulation, damping can be played the role of.This respect heat-conducting silicon rubber has special advantage, as thermal interfacial material Heat-conducting silicon rubber not only thermal conductivity with higher, good elasticity, also there is good electrical insulating property and good airproof performance The features such as, radiating efficiency is improved in gap that can effectively between filling interface.Heat-conducting silicon rubber refers on the basis of silicon rubber It adds specific conductive filler material and is formed by a kind of silica gel, existing heat filling includes aluminium oxide, silicon carbide, nitridation Aluminium, silicon nitride, magnesia, boron nitride, zinc oxide and graphite, thermally conductive carbon nanotube etc..
White carbon black is the general name of white powder X-ray amorphous silicic acid and silicate product, is primarily referred to as precipitating dioxy SiClx, fumed silica and superfine silicon dioxide gel also include powdered synthetic aluminium silicate and calcium silicates etc..White carbon black is Porous material, composition can indicate that wherein nH2O is existed in the form of surface hydroxyl with SiO2nH2O.Causticity can be dissolved in Alkali and hydrofluoric acid, not soluble in water, solvent and acid.High temperature resistant, it is non-ignitable, tasteless, odorless, have good electrical insulating property.
White carbon black industry is more early in the starting of the developed countries such as America and Europe, starts to realize industrialization during World War II Production.Since 20th century middle nineteen seventies, as western countries deepen continuously to white carbon black research, production and application neck It has obtained developing on a large scale very much in terms of domain.To 2006, about 1,300,000 tons of the production capacity of whole world white carbon black (was free of China), wherein The production capacity of German Degussa, France Luo Na and the big trans-corporation of U.S. PPG tri- is more than the half of world's total capacity.Chinese white Carbon black industry is started in 1958, is originally developed slowly, and output of white carbon black in 1984 is 2,600 tons, nineteen ninety output of white carbon black It is increased to 20,000 tons.Recently as the development of rubber industry, yield rapidly increases, and Chinese output of white carbon black has reached within 2008 71.2 ten thousand tons, yield ranks first in the world, and has become the net exporter of white carbon black.Currently, Chinese white carbon black industry forms Foreign capitals (joint) company and domestic corporation and the market competition structure deposited, market competition are abundant.
White carbon black have special surface texture (with surface hydroxyl and absorption water), special particle shape (particle is small, Large specific surface area etc.) and unique physical and chemical performance.Thus white carbon black has porosity, polymolecularity, light, chemical stabilization The good, high temperature resistant of property is not burnt, the important inorganic silicon compound for the excellent properties such as electrical insulating property is good.Such characteristic makes hard charcoal It is black to be widely used in the numerous areas such as rubber, plastics, coating, medicine, daily-use chemical industry.However, inside due to traditional white carbon black Poly- silicon oxygen and outer surface existing for activated silica alcohol radical and its absorption water characteristic, make it that white carbon black are added into rubber in hydrophily After the materials such as glue, white carbon black is difficult to moisten and disperse in organic phase.Moreover, because there are hydroxyl, surface energy on white carbon black surface Larger, aggregation always tends to agglomerate, thus the application performance of product is affected.It therefore, is raising white carbon black in polymer In dispersibility, it is necessary to it is modified that surface is carried out to it.
Summary of the invention:
The present invention overcomes the deficiencies of existing technologies, and provides a kind of silicon rubber modified white carbon black composite material.
The following technical solution is employed for the technical problems to be solved by the invention to realize: a kind of silicon rubber modified white carbon black Composite material, by weight, including following component:
100~120 parts of methyl vinyl phenyl silicon rubber, 2~8 parts of modified ceramic powder, 10~12 parts of modified white carbon black, 1~2 part of coupling agent, 1~2 part of vulcanizing agent, 0.1~0.2 part of hydroxy silicon oil, 4~8 parts of nano-cellulose;
Above-mentioned material is prepared by the following steps to form the silicon rubber modified white carbon black composite material:
(1) 2~8 parts of modified ceramic powder are dried until its own water content is lower than 2%, and will be after drying Modified ceramic powder is put into batch mixer, and 1~2 part of coupling agent is gradually added dropwise, and 1~2h of stirring is spare;
(2) 100~120 parts of methyl vinyl phenyl silicon rubber are thrown into roller, and after raw rubber packet roller be added 0.1~ 0.2 part of hydroxy silicon oil, 10~12 parts of modified white carbon blacks and step (1) treated modified ceramic powder are thin after being kneaded uniformly It is 10~12 times logical, 1~2 part of vulcanizing agent and 4~8 parts of nano-celluloses are then added, then be kneaded uniform thin logical bottom sheet, obtains silicon It is rubber mixed;
(3) silicon rubber being kneaded is put into mold, carries out one step cure on vulcanizing press after being cold-pressed mold filling;
(4) sample after one step cure carries out post vulcanization in an oven, and it is compound to obtain heat-conducting silicon rubber after natural cooling Material.
Preferably, the vulcanizing agent is organic peroxide, is selected from peroxidating phenyl-diformyl, dilauroyl peroxide or 2, 5 one dimethyl 1, the mixture of one or more of 5- di-t-butyl hexane peroxide.
Preferably, the coupling agent is γ-methyclyloxypropyl trimethoxy silane or bis- [3- (triethoxy first Silylation) propyl]-tetrasulfide.
Preferably, for the length of the nano-cellulose fiber in the range of 5~15 μm, lateral dimension is in 10~30nm In the range of.
Preferably, the modified white carbon black is through being prepared by the following steps:
Include the following steps,
(1) selection mesh number is 1100~1200 white carbon blacks, the carbon source that partial size is 6~15nm is dried respectively, point White carbon black, carbon source are not placed in vacuum desiccator and are dried, drying temperature be 20~40 DEG C, drying time with white carbon black, Carbon source itself water content is lower than subject to 0.2%, and above-mentioned white carbon black, carbon source are then carried out attached charge processing, form Board Lot Lower white carbon black and carbon source form that carrying capacity is identical and polarity on the contrary, then respectively by white carbon black, carbon source using injection tube into Row modification;
(2) modification is to use injection tube respectively by white carbon black, carbon source with 100~160ml/min and in inertia It is blown in high temperature furnace in gas or anoxybiotic environment, reaction temperature keeps the temperature 1~12 hour, carbon source is in hard charcoal at 400~600 DEG C It is 1~2nm clad that black surface, which cracks and to form amorphous carbon and form uniform thickness, obtains A;
(3) A in step (2) is mixed with ethanol solution, mixed mass ratio is 1:100~160, mixing Heating treatment is carried out using heating water bath mode in the process, heating rate is 20 DEG C/h, until being heated to 80 DEG C, is then adjusted molten The pH value of liquid is spare after drying to 4~5, obtains B;
(4) it will disperse in the B investment ethanol solution in step (3), obtain the dispersion liquid of B, then put into dispersion liquid 3-aminopropyltriethoxysilane is modified processing, the mass ratio of B and 3-aminopropyltriethoxysilane in dispersion liquid For 40~60:1, C is obtained;
(5) C in step (4) is washed, after drying and processing again with di-isopropyl peroxydicarbonate, ethyl acetate Be blended, wherein C: di-isopropyl peroxydicarbonate: the mass ratio of ethyl acetate is 1:(0.02~0.06): 40~60, then Heating water bath is to 60 DEG C, and washing is dried to obtain the modified white carbon black after being cooled to room temperature.
Preferably, carbon source includes that starch, oligosaccharide, glycerol, polyethylene glycol or lignin are a kind of or several in the step (1) Kind.
Preferably, the inert gas in the step (3) includes one kind of nitrogen or argon gas.
Preferably, the modified ceramic powder is through being prepared by the following steps:
(1) ethanol solution that volume fraction is 90% is placed in reaction kettle, and is handled using hydrochloric acid solution, until reaction The pH value of solution is 6 3.5 milliliters of vinyltriethoxysilane to be then added dropwise in kettle, stands 2h after mixing evenly, then to 20 grams of ceramic powder is added in reaction kettle, heating in water bath for reaction kettle is used after fully dispersed, heating temperature is 85 DEG C, is centrifuged Pretreatment ceramic powder is obtained after filter, drying;
(2) the pretreatment ceramic powder in step (1) is placed in reaction kettle, it is fully dispersed, wherein pretreatment ceramic powder and steaming The mass ratio of distilled water is 1:3~6, the acrylamide monomer that mass fraction is solution 20% is then added, extremely using heating water bath 40 DEG C, until the acrylamide monomer dissolves, then adds the ammonium persulfate that mass fraction is liquid quality fraction 1%, 2% Sodium hydrogensulfite is gradually heated to 85 DEG C and magnetic agitation 43h, be centrifuged to solution after reaction and be gone with acetone washing Except homopolymer, then be centrifuged, washed, dry after obtain modified ceramic powder.
Compared with prior art, the beneficial effects of the present invention are:
1, silicon rubber modified white carbon black composite material of the invention can effectively transmit heat, and reduce material The thermal expansion coefficient of material, and nano-cellulose is added and not only greatly enhances the thermal coefficient of silicon rubber, even more increase silicon The tensile strength of rubber, and having selected the ceramic powder with high rigidity and wearability is enhancing to improve the friction of silicon rubber Performance, and the dispersibility of ceramic powder is improved using graft polymers method modified ceramic powder and enhances itself and silicon rubber interface In conjunction with the mutual supplement with each other's advantages both preferably realized, the modified white carbon black of use can not only increase its point in silicon rubber Property is dissipated, by using di-isopropyl peroxydicarbonate, after ethyl acetate is modified, formation to carbon coating white carbon black surface There are active groups for decorative layer, make it have reactivity, so that polymer and can not only can make pottery with silicon rubber with modified Vitrified powder reaction, to effectively prevent white carbon black and reunion of the ceramic powder in silicon rubber, substantially improves white carbon black, ceramic The interfacial adhesion of powder and silicon rubber is applied in tire, can enhance the tearing strength of tire 46.8% and 32.6% stretching Intensity.
2, the method for modified white carbon black provided by the invention is formed by the way that white carbon black, carbon source are carried out attached charge processing The lower white carbon black of Board Lot is identical as carbon source formation carrying capacity and then polarity is on the contrary, respectively use white carbon black, carbon source Injection tube is modified processing, and in high temperature furnace, white carbon black adsorbs one with corresponding carbon source and handles via high temperature furnace, carbon source Cracking forms unformed carbon and is coated on white carbon black surface, in the application, can also pass through the unit charge number of adjusting carbon source The thickness size of cladding carbon-coating is adjusted, integrated white carbon black is adsorbed, carbon source complex is in neutrality, during blowing, is convenient for Realize the combination between white carbon black and carbon source, since carbon source or white carbon black have charge, also further avoid carbon source, Agglomeration of the white carbon black in modification solves and white carbon black and carbon source exists in the prior art during being evaporated, white Agglomeration can occur for carbon black itself, and the agraphitic carbon coverage degree after leading to cracking is low, be carbon coating hard charcoal black and white after processing The problem of mixture of carbon black;
It 3, during dialogue is carbon black modified, is connect again after dialogue carbon blacksurface carries out modification first in the application Branch polymer, constructs the coarse structure on twice-modified white carbon black surface, so that the surface formation thickness of white carbon black is uniform, The good white carbon black of dispersion effect, so that white carbon black has hydrophobic performance, the tearing strength of tire can be enhanced by being used to prepare tire With tensile strength.
Specific embodiment:
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below Specific embodiment is closed, the present invention is further explained.
Embodiment 1
A kind of silicon rubber modified white carbon black composite material, including,
Methyl vinyl phenyl silicon rubber 100g, modified ceramic powder 2g, modified white carbon black 10g, coupling agent 1g, vulcanizing agent 1g, hydroxy silicon oil 0.1g, nano-cellulose 4g;
Above-mentioned material is prepared by the following steps to form the silicon rubber modified white carbon black composite material:
(1) modified ceramic powder is dried until its own water content is lower than 2%, and being modified after drying is made pottery Vitrified powder is put into batch mixer, and coupling agent is gradually added dropwise, and 1~2h of stirring is spare;
(2) methyl vinyl phenyl silicon rubber is thrown into roller, and hydroxy silicon oil is added after raw rubber packet roller, modified hard charcoal Black and step (1) treated modified ceramic powder, it is thin 10~12 times logical after being kneaded uniformly, then add 1~2 part of vulcanization Agent and 4~8 parts of nano-celluloses, then it is kneaded uniform thin logical bottom sheet, obtain silicon rubber gross rubber;
(3) silicon rubber being kneaded is put into mold, carries out one step cure on vulcanizing press after being cold-pressed mold filling;
(4) sample after one step cure carries out post vulcanization in an oven, and it is compound to obtain heat-conducting silicon rubber after natural cooling Material.
Vulcanizing agent is organic peroxide, specially peroxidating phenyl-diformyl, and coupling agent is γ-methyclyloxypropyl Trimethoxy silane, for the length of nano-cellulose fiber in the range of 10 μm, lateral dimension is in the range of 20nm.
Modified white carbon black is through being prepared by the following steps:
Include the following steps,
(1) selection mesh number is 1100~1200 white carbon blacks, the carbon source that partial size is 6~15nm is dried respectively, point White carbon black, carbon source are not placed in vacuum desiccator and are dried, drying temperature be 20~40 DEG C, drying time with white carbon black, Carbon source itself water content is lower than subject to 0.2%, and above-mentioned white carbon black, carbon source are then carried out attached charge processing, form Board Lot Lower white carbon black and carbon source form that carrying capacity is identical and polarity on the contrary, then respectively by white carbon black, carbon source using injection tube into Row modification;
(2) modification is to use injection tube respectively by white carbon black, carbon source with 100~160ml/min and in inertia It is blown in high temperature furnace in gas or anoxybiotic environment, reaction temperature keeps the temperature 1~12 hour, carbon source is in hard charcoal at 400~600 DEG C It is 1~2nm clad that black surface, which cracks and to form amorphous carbon and form uniform thickness, obtains A;
(3) A in step (2) is mixed with ethanol solution, mixed mass ratio is 1:100~160, mixing Heating treatment is carried out using heating water bath mode in the process, heating rate is 20 DEG C/h, until being heated to 80 DEG C, is then adjusted molten The pH value of liquid is spare after drying to 4~5, obtains B;
(4) it will disperse in the B investment ethanol solution in step (3), obtain the dispersion liquid of B, then put into dispersion liquid 3-aminopropyltriethoxysilane is modified processing, the mass ratio of B and 3-aminopropyltriethoxysilane in dispersion liquid For 40~60:1, C is obtained;
(5) C in step (4) is washed, after drying and processing again with di-isopropyl peroxydicarbonate, ethyl acetate Be blended, wherein C: di-isopropyl peroxydicarbonate: the mass ratio of ethyl acetate is 1:(0.02~0.06): 40~60, then Heating water bath is to 60 DEG C, and washing is dried to obtain the modified white carbon black after being cooled to room temperature, and carbon source is starch, step in step (1) Suddenly the inert gas in (3) is nitrogen;
Modified ceramic powder is through being prepared by the following steps:
(1) ethanol solution that volume fraction is 90% is placed in reaction kettle, and is handled using hydrochloric acid solution, until reaction The pH value of solution is 6 3.5 milliliters of vinyltriethoxysilane to be then added dropwise in kettle, stands 2h after mixing evenly, then to 20 grams of ceramic powder is added in reaction kettle, heating in water bath for reaction kettle is used after fully dispersed, heating temperature is 85 DEG C, is centrifuged Pretreatment ceramic powder is obtained after filter, drying;
(2) the pretreatment ceramic powder in step (1) is placed in reaction kettle, it is fully dispersed, wherein pretreatment ceramic powder and steaming The mass ratio of distilled water is 1:3~6, the acrylamide monomer that mass fraction is solution 20% is then added, extremely using heating water bath 40 DEG C, until the acrylamide monomer dissolves, then adds the ammonium persulfate that mass fraction is liquid quality fraction 1%, 2% Sodium hydrogensulfite is gradually heated to 85 DEG C and magnetic agitation 43h, be centrifuged to solution after reaction and be gone with acetone washing Except homopolymer, then be centrifuged, washed, dry after obtain modified ceramic powder.
Embodiment 2
The present embodiment content and 1 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that:
A kind of silicon rubber modified white carbon black composite material, including,
Methyl vinyl phenyl silicon rubber 110g, modified ceramic powder 5g, modified white carbon black 11g, coupling agent 1.5g, vulcanization Agent 1.5g, hydroxy silicon oil 0.15g, nano-cellulose 6g.
Embodiment 3
The present embodiment content and 1 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that:
A kind of silicon rubber modified white carbon black composite material, comprising:
Methyl vinyl phenyl silicon rubber 120g, modified ceramic powder 8g, modified white carbon black 12g, coupling agent 2g, vulcanizing agent 2g, hydroxy silicon oil 0.2g, nano-cellulose 8g.
Embodiment 4
The present embodiment content and 2 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that:
Modified white carbon black is through being prepared by the following steps: includes the following steps,
(1) selection mesh number is 1100~1200 white carbon blacks, the carbon source that partial size is 6~15nm is dried respectively, point White carbon black, carbon source are not placed in vacuum desiccator and are dried, drying temperature be 20~40 DEG C, drying time with white carbon black, Carbon source itself water content is lower than subject to 0.2%, and above-mentioned white carbon black, carbon source are then carried out attached charge processing, form Board Lot It is 2:1 that lower white carbon black and carbon source, which forms the ratio between carrying capacity, and polarity is on the contrary, then respectively by white carbon black, carbon source using spray Blowpipe is modified processing;
(2) modification is to use injection tube respectively by white carbon black, carbon source with 100~160ml/min and in inertia It is blown in high temperature furnace in gas or anoxybiotic environment, reaction temperature keeps the temperature 1~12 hour, carbon source is in hard charcoal at 400~600 DEG C It is 1~2nm clad that black surface, which cracks and to form amorphous carbon and form uniform thickness, obtains A;
(3) A in step (2) is mixed with ethanol solution, mixed mass ratio is 1:100~160, mixing Heating treatment is carried out using heating water bath mode in the process, heating rate is 20 DEG C/h, until being heated to 80 DEG C, is then adjusted molten The pH value of liquid is spare after drying to 4~5, obtains B;
(4) it will disperse in the B investment ethanol solution in step (3), obtain the dispersion liquid of B, then put into dispersion liquid 3-aminopropyltriethoxysilane is modified processing, the mass ratio of B and 3-aminopropyltriethoxysilane in dispersion liquid For 40~60:1, C is obtained;
(5) C in step (4) is washed, after drying and processing again with di-isopropyl peroxydicarbonate, ethyl acetate Be blended, wherein C: di-isopropyl peroxydicarbonate: the mass ratio of ethyl acetate is 1:(0.02~0.06): 40~60, then Heating water bath is to 60 DEG C, and washing is dried to obtain the modified white carbon black after being cooled to room temperature, and carbon source is starch, step in step (1) Suddenly the inert gas in (3) is nitrogen.
Embodiment 5
The present embodiment content and 2 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that:
Modified white carbon black is through being prepared by the following steps: includes the following steps,
(1) selection mesh number is 1100~1200 white carbon blacks, the carbon source that partial size is 6~15nm is dried respectively, point White carbon black, carbon source are not placed in vacuum desiccator and are dried, drying temperature be 20~40 DEG C, drying time with white carbon black, Carbon source itself water content is lower than subject to 0.2%, and above-mentioned white carbon black, carbon source are then carried out attached charge processing, form Board Lot It is 1:2 that lower white carbon black and carbon source, which forms the ratio between carrying capacity, and polarity is on the contrary, then respectively by white carbon black, carbon source using spray Blowpipe is modified processing;
(2) modification is to use injection tube respectively by white carbon black, carbon source with 100~160ml/min and in inertia It is blown in high temperature furnace in gas or anoxybiotic environment, reaction temperature keeps the temperature 1~12 hour, carbon source is in hard charcoal at 400~600 DEG C It is 1~2nm clad that black surface, which cracks and to form amorphous carbon and form uniform thickness, obtains A;
(3) A in step (2) is mixed with ethanol solution, mixed mass ratio is 1:100~160, mixing Heating treatment is carried out using heating water bath mode in the process, heating rate is 20 DEG C/h, until being heated to 80 DEG C, is then adjusted molten The pH value of liquid is spare after drying to 4~5, obtains B;
(4) it will disperse in the B investment ethanol solution in step (3), obtain the dispersion liquid of B, then put into dispersion liquid 3-aminopropyltriethoxysilane is modified processing, the mass ratio of B and 3-aminopropyltriethoxysilane in dispersion liquid For 40~60:1, C is obtained;
(5) C in step (4) is washed, after drying and processing again with di-isopropyl peroxydicarbonate, ethyl acetate Be blended, wherein C: di-isopropyl peroxydicarbonate: the mass ratio of ethyl acetate is 1:(0.02~0.06): 40~60, then Heating water bath is to 60 DEG C, and washing is dried to obtain the modified white carbon black after being cooled to room temperature, and carbon source is starch, step in step (1) Suddenly the inert gas in (3) is nitrogen.
Control group 1
This control group content and 2 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that, this is right It is not modified using the present processes according to the white carbon black in group.
Control group 2
This control group content and 2 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that, this is right It is not modified using the present processes according to the ceramic powder in group.
Control group 3
This control group content and 2 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that, this is right It is not modified using the present processes according to white carbon black, the ceramic powder in group.
Performance test:
GB/T1764-1979 standard testing coating thickness is used to embodiment 2,4,5, and is recorded in table 1:
Table 1
Group Thickness (nu)
Embodiment 1 1.6
Embodiment 2 2.3
Embodiment 3 0.5
The silicon rubber that embodiment 1,2,3 and the preparation of control group 1,2,3 are formed is tested, test result such as table 2:
It tests coefficient of friction directly to read from test software, wear rate (ω) is calculated as follows:
ω=△ V/ (π 2rRF)
△ V=14bh/3
H=r- (r2-b2/4) 0.5
In formula: △ V is the wear volume (mm3) of sample;R is antithesis ring radius (mm);R is antithesis ring real-turn circle number;F is Test force (N);B is wear scar width (mm).
Table 2
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its Equivalent thereof.

Claims (3)

1. a kind of silicon rubber modified white carbon black composite material, which is characterized in that by weight, including following component:
100~120 parts of methyl vinyl phenyl silicon rubber, 2~8 parts of modified ceramic powder, 10~12 parts of modified white carbon black, coupling 1~2 part of agent, 1~2 part of vulcanizing agent, 0.1~0.2 part of hydroxy silicon oil, 4~8 parts of nano-cellulose;
Above-mentioned material is prepared by the following steps to form the silicon rubber modified white carbon black composite material:
(1) 2~8 parts of modified ceramic powder are dried to its own water content lower than until 2%, and by the modification after drying Ceramic powder is put into batch mixer, and 1~2 part of coupling agent is gradually added dropwise, and 1~2h of stirring is spare;
(2) 100~120 parts of methyl vinyl phenyl silicon rubber are thrown into roller, and 0.1~0.2 part is added after raw rubber packet roller Hydroxy silicon oil, 10~12 parts of modified white carbon blacks and step (1) treated modified ceramic powder, thin by logical 10 after being kneaded uniformly~ 12 times, 1~2 part of vulcanizing agent and 4~8 parts of nano-celluloses are then added, then is kneaded uniform thin logical bottom sheet, it is mixed to obtain silicon rubber Refining glue;
(3) silicon rubber being kneaded is put into mold, carries out one step cure on vulcanizing press after being cold-pressed mold filling;
(4) sample after one step cure carries out post vulcanization in an oven, obtains thermally conductive silicone rubber composite material after natural cooling.
2. silicon rubber modified white carbon black composite material according to claim 1, which is characterized in that the vulcanizing agent is to have Machine peroxide, be selected from peroxidating phenyl-diformyl, dilauroyl peroxide or 2,5 one dimethyl 1,5- di-tert-butyl peroxide oneself The mixture of one or more of alkane.
3. silicon rubber modified white carbon black composite material according to claim 1, which is characterized in that the coupling agent is γ- Methyclyloxypropyl trimethoxy silane or bis- [3- (triethoxysilyl) propyl]-tetrasulfides.
CN201810879020.9A 2018-08-03 2018-08-03 A kind of silicon rubber modified white carbon black composite material Pending CN109135294A (en)

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CN114231041A (en) * 2021-12-31 2022-03-25 上海电缆研究所有限公司 B1-grade flame-retardant ceramic low-smoke silicone rubber cable material and preparation method thereof

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Application publication date: 20190104