CN102627860A - Flame-retardant, high-heat-conductivity, high-temperature-resistant and low-temperature-resistant addition organic silicon rubber and preparation method thereof - Google Patents
Flame-retardant, high-heat-conductivity, high-temperature-resistant and low-temperature-resistant addition organic silicon rubber and preparation method thereof Download PDFInfo
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Abstract
The invention discloses organic silicon rubber, which has flame retardance, high heat conductivity, high temperature resistance and low temperature resistance and can be used for replacing the conventional organic silicon rubber. The organic silicon rubber comprises alpha,omega-divinyl polydimethylsiloxane, methyl hydrogen-containing polysiloxane, cerium oxide, zinc oxide, ferric oxide, alumina, hydroxyl ferric oxide, white carbon black, a catalyst and an aid in the weight ratio of (10-18):(1-6):(1-1.25):(5-25):(1-3):(10-12.5):(1-2.5):(10-25):(1-2.5):(0.003-1.25):(0.003-1.25).
Description
[technical field]
The present invention relates to a kind of organo-silicone rubber and working method thereof; Refer in particular to have fire-retardant, high heat conduction simultaneously, the add-on type organo-silicone rubber and its preparation method of high temperature resistant and resistance to low temperature; The alternative traditional organo-silicone rubber of organo-silicone rubber of the present invention belongs to the organic silicon chemical technical field.
[background technology]
In recent years, silastic material has obtained using widely in electronic enterprises, but because of it is a polymer materials, inflammable, the amount of being fuming is big, but is the direct wick of fire sometimes; Therefore flame retardant type Zylox slowly become silastic material in the electronic enterprises main strength along with industrial production and science and technology development, people constantly propose new requirement to material.In field of electronics; Because developing rapidly of integrated technology and package technique; Electronic component, logical circuit develop to light, thin, little direction, and thermal value also increases thereupon, thereby need the insulating material of high heat conduction; Effectively remove the heat that electronics produces, this is related to the work-ing life of product and the safety of quality.The method of traditional solution electronic equipment dissipating heat; Be that pad one deck insulating medium is as thermally conductive material between heating element and radiator, like mica, tetrafluoroethylene and beryllium oxide ceramics or the like, this method has certain effect; But exist heat conductivility poor, shortcomings such as mechanical property is low, price height.At present, solving electronic equipment dissipating heat is to solve through various forms of scatterers a bit, but great majority must solve through thermally conductive material, and the heat-conducting silicon rubber material is most important a member in the thermally conductive material.Development along with electronics, electrical apparatus technology; Strong functions is integrated in the littler assembly to require various electronic devices and components, electronic product, electrical equipment to incite somebody to action more; For do product saferly, performance is more optimized, more perfect; Many designers exhaust thought for this reason, think most method, but because existing machine Zylox physicals is more single, for example the flame retardant resistance organic silica gel does not but have thermal conductivity; And heat-conductive silicone rubber does not have flame retardant resistance, and the reasonable organo-silicone rubber of weathering resistance does not have thermal conductivity, flame retardant resistance again.
We know; Not fire-retardant organo-silicone rubber can cause very big potential safety hazard; And athermanous organo-silicone rubber can cause equipment slow-downs, equipment work can break down midway; And the organo-silicone rubber of high-low temperature resistant can not cause the product life place short, so current organo-silicone rubber can not satisfy the needs of electronics today, the development of electrical equipment product technology far away.Along with the needs of integrated, miniaturized, ultra-thinization product, if can develop a kind of organo-silicone rubber possess simultaneously flame retardant resistance is arranged, high thermal conductivity, high temperature resistant, low temperature resistant organo-silicone rubber product the applicant's purpose just.
[summary of the invention]
The objective of the invention is to overcome the deficiency of present technology, a kind of have simultaneously fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber, alternative traditional organo-silicone rubber are provided.
Another object of the present invention has provided the preparation method of fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber.
In order to solve the technical problem of above-mentioned existence, the present invention adopts following technical proposals:
A kind of fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber; It is characterized in that comprising a; ω-divinyl polydimethylsiloxane, methylhydrogenpolysi,oxane, cerium oxide, zinc oxide, red oxide of iron, titanium oxide, aluminum oxide, hydrous iron oxide, WHITE CARBON BLACK, catalyzer, auxiliary agent; Their weight ratio is: 10-18:1-6:1-1.25:5-25:1-3:10-12.5:1-2.5:10-25:1-2.5:0.00 3-1.25:0.003-1.25; Wherein: said a, the contents of ethylene of ω-divinyl polydimethylsiloxane is at 0.0013-2.1, and viscosity is at 100mm
2/ s-200000 mm
2In/s the scope; The viscosity of said methylhydrogenpolysi,oxane is at 5 mm
2/ s-1500 mm
2In/s the scope, hydrogen content is at 0.1-1.6%; The median size of said cerium oxide is at 1～8000 μ m, TIO
2Purity is more than 98%; The median size of said zinc oxide is at 1～2000 μ m, TIO
2Purity is more than 90%; The median size of said red oxide of iron is at 1～5000 μ m, TIO
2In purity more than 95%; The median size of said titanium oxide is at 2～4000 μ m, TIO
2In purity more than 99%; The median size of said aluminum oxide is at 1～3000 μ m, TIO
2In purity more than 98%; The median size of said hydrous iron oxide is at 10～5000 μ m, TIO
2In purity more than 96%; The median size of said WHITE CARBON BLACK in 1～3000 μ m, specific surface area at 10～1000m
2/ g; Said catalyzer is the catalyzer that contains the various title complexs of platinum.
In improvement project to above-mentioned fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber; Described a; ω-divinyl polydimethylsiloxane comprises a of two kinds of different viscosity and contents of ethylene; ω-divinyl polydimethylsiloxane mixes, this a of two kinds, and the viscosity of ω-divinyl polydimethylsiloxane is greater than 1000mm
2/ s is smaller or equal to 50000 mm
2/ s, its weight ratio is 1:50-50:1.
In the improvement project to above-mentioned fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber, the viscosity of said methylhydrogenpolysi,oxane is at 50-500 mm
2/ s, hydrogen content are 0.3-1%.
In the improvement project to above-mentioned fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber, said cerium oxide is the powder that comprises two kinds of different-grain diameters, median size 1～800 μ m of every kind of powder.
In the improvement project to above-mentioned fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber, said zinc oxide comprises the powder of two kinds of different-grain diameters, median size 1～200 μ m of every kind of powder.
In the improvement project to above-mentioned fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber, said red oxide of iron comprises the powder of two kinds of different-grain diameters, median size 1～500 μ m of every kind of powder.
In the improvement project to above-mentioned fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber, said titanium oxide comprises the powder of two kinds of different-grain diameters, and the median size of every kind of powder is at 100～2500 μ m.
In the improvement project to above-mentioned fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber, said aluminum oxide comprises the powder of two kinds of different-grain diameters, and the median size of every kind of powder is at 50～2500 μ m.
In the improvement project to above-mentioned fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber, said hydrous iron oxide comprises the powder of two kinds of different-grain diameters, and the median size of every kind of powder is at 100～4000 μ m.
In the improvement project to above-mentioned fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber, said WHITE CARBON BLACK comprises the powder that comprises two kinds of different-grain diameters, median size 50～2500 μ m of every kind of powder.
In improvement project to above-mentioned fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber; Said catalyzer is a kind of in platinum-vinyl siloxane complex, pure modification Platinic chloride title complex, the platinum-alkynes basigamy compound; Its consumption is with a, and ω-divinyl polydimethylsiloxane and methylhydrogenpolysi,oxane content sum are that benchmark is counted 100-10000ppm by pt.
In improvement project to above-mentioned fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber; Said auxiliary agent is a kind of in 3-methyl isophthalic acid-butine-3-alcohol, methylpentynol, the 1-ethynyl-1-hexalin; Its consumption is with a, and ω-divinyl polydimethylsiloxane and methylhydrogenpolysi,oxane content sum are that benchmark is counted 100-10000ppm by pt.
The preparation method of a kind of fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber is characterized in that comprising the steps:
1), in Banbury mixer, add a, ω-divinyl polydimethylsiloxane adds titanium oxide, cerium oxide, aluminum oxide, zinc oxide, hydrous iron oxide, red oxide of iron again, and WHITE CARBON BLACK, adds at unsteady briquetting and depresses mixingly, and mixture is uniformly dispersed,
2), make mixture temperature rise to 100-110 ℃ again; And with 2-8m
3/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-1～-0.7amp, 170～190 ℃ of mixing 2～5h promptly get the mixture base-material;
3), the mixture base-material is moved in the stirrer of prior preheating, with 2-8m
5/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-1～-0.7amp;
4), in the mixture base-material, add methylhydrogenpolysi,oxane, catalyzer and auxiliary agent, mix back decompression down row's bubble promptly be made into the high temperature resistant low temperature resistant addition-type silicon rubber of the fire-retardant high heat conduction of single-component high-viscosity organosilicon.
Compared with prior art, the invention has the beneficial effects as follows:
Organo-silicone rubber thermostability of the present invention is high; The chemical bond of (or radiation irradiation) molecule does not rupture, does not decompose under the high temperature; Therefore be difficult for being decomposed, have, can reach decades in work-ing life under physical environment than the better thermostability of other macromolecular materials and anti-irradiation and weather-proof ability by UV-light and ozone; Not only can be high temperature resistant, and low temperature resistant; Can in a very wide TR, use and have excellent electric insulating can; Its dielectric loss, proof voltage, anti-electric arc, anti-corona, volume resistivity and surface resistivity etc. all come out at the top in insulating material; And their electric property receives the influence of temperature and frequency very little; Therefore, they are a kind of stable electrically insulating materials, are widely used on electronics, the electrical industry; The present invention is except having good thermotolerance; Also have excellent water repellency, this is that electricinstallation uses the guarantee with higher reliability under hygrometric state condition, in a word; Organosilicon Zylox of the present invention not only has good heat-conducting, over-all properties and use characteristics and also has the not available performance of a lot of other materials; Like weather resisteant, cohesiveness or the like, so its DEVELOPMENT PROSPECT is considerable, using also will be more and more widely; Because range of application of the present invention is very extensive, its economic outlook, value are very considerable.
Following embodiment is made further detailed description to the present invention:
[embodiment]
The present invention is fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber; Comprise a; ω-divinyl polydimethylsiloxane, methylhydrogenpolysi,oxane, cerium oxide, zinc oxide, red oxide of iron, titanium oxide, aluminum oxide, hydrous iron oxide, WHITE CARBON BLACK, catalyzer, auxiliary agent; Their weight ratio is: 10-18:1-6:1-1.25:5-25:1-3:10-12.5:1-2.5:10-25:1-2.5:0.00 3-1.25:0.003-1.25, wherein:
Said a, the contents of ethylene of ω-divinyl polydimethylsiloxane is at 0.0013-2.1, and viscosity is at 100mm
2/ s-200000 mm
2In/s the scope; The viscosity of said methylhydrogenpolysi,oxane is at 5 mm
2/ s-1500 mm
2In/s the scope, hydrogen content is at 0.1-1.6%; The median size of said cerium oxide is at 1～8000 μ m, TIO
2Purity is more than 98%; The median size of said zinc oxide is at 1～2000 μ m, TIO
2Purity is more than 90%; The median size of said red oxide of iron is at 1～5000 μ m, TIO
2In purity more than 95%; The median size of said titanium oxide is at 2～4000 μ m, TIO
2In purity more than 99%; The median size of said aluminum oxide is at 1～3000 μ m, TIO
2In purity more than 98%; The median size of said hydrous iron oxide is at 10～5000 μ m, TIO
2In purity more than 96%; The median size of said WHITE CARBON BLACK in 1～3000 μ m, specific surface area at 10～1000m
2/ g; Said catalyzer is the catalyzer that contains the various title complexs of platinum; Said auxiliary agent should have not volatile, and is good with the sizing material consistency.
As the comparative optimization scheme, a that is selected for use, the viscosity of ω-divinyl polydimethylsiloxane is greater than 1000mm
2/ s is smaller or equal to 50000 mm
2/ s; And at whole a, in ω-divinyl polydimethylsiloxane, its viscosity can be identical with contents of ethylene; Also can be viscosity two kind or the above a different with contents of ethylene; ω-divinyl polydimethylsiloxane mixes, and more preferably two kinds of differences (viscosity and contents of ethylene are directly proportional) are mixed, and its weight ratio is 1:50-50:1.
The preferred viscosity of said methylhydrogenpolysi,oxane is at 50-500 mm
2/ s, hydrogen content are 0.3-1% (quality).
Usually, said cerium oxide is median size 1～800 μ m, TIO
2The inorganic powder of purity more than 98%; As the comparative optimization scheme, it generally includes the powder that is no less than two kinds of different-grain diameters, and any two kinds of particle diameter forms have a difference at least.
Usually, said zinc oxide is median size 1～200 μ m, TIO
2The inorganic powder of purity more than 90%; As the comparative optimization scheme, it generally includes the powder that is no less than two kinds of different-grain diameters, and any two kinds of particle diameter forms have a difference at least.
Under comparative optimization, said red oxide of iron comprises median size 1～500 μ m, TIO
2The inorganic powder of purity more than 95%, and comprise that normally the powder that is no less than two kinds of different-grain diameters, these powders have two kinds of median sizes at least, and the form between any two kinds of particle diameters has a difference at least.
Under comparative optimization, the median size of said titanium oxide is at 100～2500 μ m, TIO
2At the inorganic powder of purity more than 99%, and normally comprise the powder that is no less than two kinds of different-grain diameters, and the particle shape between any two kinds of particle diameters has a difference at least.
The median size of said aluminum oxide is at 50～2500 μ m, TIO
2At the inorganic powder of purity more than 98%, and normally comprise the powder that is no less than two kinds of different-grain diameters, the particle shape between any two kinds of particle diameters of these powders has a difference at least.
The median size of said hydrous iron oxide is at 100～4000 μ m, TIO
2At the inorganic powder of purity more than 96%, and normally comprise the powder that is no less than two kinds of particle diameters, the particle shape between any two kinds of particle diameters of these powders has a difference at least.
Generally speaking, said WHITE CARBON BLACK comprises median size 50～2500 μ m, specific surface area 50～800m
2The inorganic powder of/g, and comprise the powder that is no less than two kinds of different-grain diameters, these powders are two kinds of median sizes of tool at least, and the particle shape between any two kinds of powders has a difference at least.
Said catalyst pack contains the catalysis of Platinic chloride title complex; Requirement to catalyst performance; Storage stability, consistency is good, catalytic activity is high; Usually its consumption is with a, and ω-divinyl polydimethylsiloxane and methylhydrogenpolysi,oxane content sum are that benchmark is counted 100-10000ppm by pt, more preferably 500-5000ppm.Said catalyzer is a kind of in platinum-vinyl siloxane complex, pure modification Platinic chloride title complex, the platinum-alkynes basigamy compound normally.
Said auxiliary agent should have not volatile, the characteristic good with the sizing material consistency, and its consumption is with a, and ω-divinyl polydimethylsiloxane and methylhydrogenpolysi,oxane content sum are that benchmark is counted more preferably 500-5000ppm of 100-10000ppm by pt.Said auxiliary agent can be a kind of in 3-methyl isophthalic acid-butine-3-alcohol, methylpentynol, the 1-ethynyl-1-hexalin.
For example also different median size 1～800 μ m of the different flame retardant ratings of first kind of cerium oxide dosage, TIO
2The inorganic powder of purity more than 98% be 100～500 μ m more preferably; Also different median size 1～200 μ m of the different thermal conductivitys of second kind of zinc oxide addition, TIO
2The inorganic powder of purity more than 90%, more preferably 50～150 μ m; The different thermal conductivitys of the third red oxide of iron addition are also different, median size 1～500 μ m, TIO
2The inorganic powder of purity more than 95% more preferably is 50～250 μ m.The 4th kind of titanium oxide addition different physical characteristics is also different, median size 1～500 μ m, TIO
2The inorganic powder of purity more than 95% more preferably is 50～250 μ m.The 5th kind of aluminum oxide addition different physical characteristics is also different, median size 1～500 μ m, TIO
2The inorganic powder of purity more than 95%, more preferably 50～250 μ m.The 6th kind of hydrous iron oxide addition different physical characteristics is also different, median size 1～500 μ m, TIO
2The inorganic powder of purity more than 99%, more preferably 50～250 μ m.
The pre-treatment preferable methods is to use structurizing control, a for example, and alpha, omega-dihydroxy polydimethyl siloxane, a, handle powder alpha, omega-dihydroxy dimethyl diphenyl siloxanes, hexamethyldisilazane.Treatment process can adopt following method: reinforced filling is added the stir mixing vacuum apparatus carry out high-speed stirring (1000-1400 rev/min); Simultaneously to add antistructurizing agent; Stirred 30～180 minutes, and got final product in dry 3～8 hours down at 160-180 ℃ then.
The preparation of flame-retarded heat-conducting high-low temperature resistant add-on type organo-silicone rubber of the present invention comprises a, ω-divinyl polydimethylsiloxane, methylhydrogenpolysi,oxane, cerium oxide, zinc oxide, red oxide of iron, titanium oxide, aluminum oxide, hydrous iron oxide, WHITE CARBON BLACK, catalyzer, auxiliary agent; Preferred ingredients content (weight ratio) per-cent is: a, the content of ω-divinyl polydimethylsiloxane are 10%-18%, and the content of methylhydrogenpolysi,oxane is 1%-6%; The content of cerium oxide is 1%-1.25%, and the content of zinc oxide is 5%-25%, and ferric oxide content is 1%-3%; The content of titanium oxide is 10%-12.5%; The content of aluminum oxide is 1%-2.5%, and the content of hydrous iron oxide is 10%-25%, and the content of WHITE CARBON BLACK is 1%-2.5%; The content of catalyzer is 0.003%-1.25%, and the content of auxiliary agent is 0.003%-1.25%.
Organic silicon flame-retardant heat conduction high-low temperature resistant addition-type silicon rubber of the present invention can also add some singularity auxiliary agents according to different application needs.For example; Add vinyl trichloro silane, vinyltriethoxysilane, vinyltrimethoxy silane, vinyltrimethoxy silane, vinyl three ('beta '-methoxy oxyethyl group) silane to improve the sticking power that cured article solidifies back and surface of base, preferred consumption is the 0.1-8% of organic silicon flame-retardant heat conduction high-low temperature resistant addition-type silicon rubber total amount; Add thinner in the prescription in order to reduce compound viscosity, increase mobile or to reduce sulfuration back Zylox hardness; Preferable absorbent such as a; ω-dimethoxysiloxane, MDT type silicone oil, alkane footpath mixture, alkyl aromatic compound; Their preferred consumptions are the 0.1-3% of organic silicon flame-retardant heat conduction high-low temperature resistant addition-type silicon rubber total amount; Can also in prescription, add wetting agent, dispersion agent, skimmer, rheological agent, anti-settling agent, flow agent, stain control agent, antimildew disinfectant, static eliminator, matting agent, glossing agent, slip(ping)agent, photostabilizer, coupling agent, surface of pigments treatment agent, agent toughener; To satisfy variant prodn to the different denseness (rheological, thixotropy) of organic silica gel, sulfuration back different modulus (high, medium and low) and various property (fire-retardant, high heat conduction, high temperature resistant, low temperature resistant, conduction, delustring, anti-solvent, hydrophilic, low thermal coefficient of expansion etc.) performance requriements, add-on is the 0.1-3% of flame-retarded heat-conducting high-low temperature resistant add-on type organo-silicone rubber gross weight; And the mineral dye that can add different colours is to satisfy the needs to the organic silica gel different colours.
With the packed state of the high temperature resistant low temperature resistant add-on type organo-silicone rubber of fire-retardant high heat conduction of the present invention can be single-component or two component; Condition of cure room temperature or heat; Solidifying the back form is rubber-like and gel; Preferred ambient cure condition is: 25 ℃/24h, preferred heating cure condition is: 40～60 ℃/30～120min or 80～150 ℃/15min.
The characteristics of the high temperature resistant low temperature resistant add-on type organo-silicone rubber of the fire-retardant high heat conduction of the present invention are that flame retardant rating can reach the UL-94V-0 level, and thermal conductivity can arrive 8.0w/m ﹒ k, and heatproof can reach-100～350 ℃, and electrical insulation capability is good.Use this invention organosilicon Zylox can make a kind of good flame resistance, thermal conductivity high, again can high temperature resistant, low temperature resistant and superior isolation property, water tolerance, weathering resistance, the bonding that can be widely used in universe aviation, aircraft manufacturing, electronic industry, mechanical workout, automobile making and building and medical aspect and sealing, be applicable to that also semi-conductor combines the position to make the waterproof sealing of heat derived materials, heating rubber roll material, LED display unit, high-power electronic component, modular power source, wiring board, LED display, Shui nationality submersible pump, photodiode (LED), charactron, lattice module, infrared emission tube, electrical condenser etc.
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Single-component organic silicon glue embodiment 1
Adding viscosity in the 5L Banbury mixer is 100 mm
2The a of/s, ω-divinyl polydimethylsiloxane 750g, viscosity is 300 mm
2The a of/s; In the mixture of ω-divinyl polydimethylsiloxane 250g; Titanium oxide 1000g, the median size that adds median size again and be 2 μ m is that 1 μ m cerium oxide 100g, median size are that 1 μ m aluminum oxide 100g, median size are that zinc oxide 500g, the median size of 1 μ m is that hydrous iron oxide 1000g, the median size of 10 μ m is the red oxide of iron 100g of 1 μ m, and median size 1 μ m, specific surface area 500m
2The WHITE CARBON BLACK 100g of/g adds at unsteady briquetting and to depress mixing about 15min, and mixture is uniformly dispersed, and mixture temperature rises to 105 ℃; With 5m
3/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-0.85amp, and 170～190 ℃ of mixing 3h (TRT 3h) promptly get the mixture base-material; The mixture base-material is moved in the planetary mixer of prior preheating, with 5m
5/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-0.85amp.Then, in the mixture base-material, adding viscosity is 5 mm
2/ s, hydrogen content are the methylhydrogenpolysi,oxane 100g of 1% (quality), quite the massfraction of Pt is 1.0 * 10
-6～5.0 * 10
-5Pure modification chloroplatinic acid catalyst 0.3g, 3-methyl isophthalic acid-butine-3-alcohol 0.3g, mix the back decompression down row's bubble promptly be made into the high temperature resistant low temperature resistant addition-type silicon rubber of the fire-retardant high heat conduction of single-component.Preferred ambient cure condition is: 25 ℃/24h, preferred heating cure condition is: 40～60 ℃/30～120min or 80～150 ℃/15min are solidified into elastomerics.Through detecting, its flame retardant rating can reach the UL-94V-0 level, and thermal conductivity can arrive 8.0w/m ﹒ k, and heatproof can reach-100～300 ℃, and electrical insulation capability is good.
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Single-component organic silicon glue embodiment 2
Adding viscosity in the 5L Banbury mixer is: 1100 mm
2The a of/s, ω-divinyl polydimethylsiloxane 750g, viscosity is: 1300 mm
2/ s and a; In the mixture of ω-divinyl polydimethylsiloxane 250g; Titanium oxide 1000g, the median size that adds median size again and be 100 μ m is that cerium oxide 100g, the median size of 50 μ m is that aluminum oxide 150g, the median size of 50 μ m is that zinc oxide 1500g, the median size of 50 μ m is that hydrous iron oxide 1000g, the median size of 100 μ m is the red oxide of iron 100g of 100 μ m, and median size is 50 μ m, specific surface area 500m
2The WHITE CARBON BLACK 160g of/g adds at unsteady briquetting and to depress mixing about 15min, and mixture is uniformly dispersed, and mixture temperature rises to 105 ℃; With 5m
3/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-0.85amp, and 170～190 ℃ of mixing 3h (TRT 3h) promptly get the mixture base-material; The mixture base-material is moved in the planetary mixer of prior preheating, with 5m
5/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-0.85amp.Then, in the mixture base-material, adding viscosity is 50 mm
2/ s, hydrogen content are the methylhydrogenpolysi,oxane 150g of 1% (quality), quite the massfraction of Pt is 1.0 * 10
-6～5.0 * 10
-5Pure modification chloroplatinic acid catalyst 50g, 3-methyl isophthalic acid-butine-3-alcohol 50g, mix the back decompression down row's bubble promptly be made into the high temperature resistant low temperature resistant addition-type silicon rubber of the fire-retardant high heat conduction of single-component high-viscosity organosilicon.Preferred ambient cure condition is: 25 ℃/24h; Preferred heating cure condition is: 40～60 ℃/30～120min or 80～150 ℃/15min are solidified into elastomerics, through detecting; Its flame retardant rating can reach the UL-94V-0 level; Thermal conductivity can arrive 8.0w/m ﹒ k, and heatproof can reach-100～300 ℃, and electrical insulation capability is good.
Bi-component organic silicon glue (10:1) embodiment 3
In the 5L Banbury mixer, adding viscosity is 10000 mm
2The a of/s, ω-divinyl polydimethylsiloxane 750g, viscosity is 11000 mm
2The a of/s; In the mixture of ω-divinyl polydimethylsiloxane 250g; Cerium oxide 100g, the median size that adds median size again and be 1300 μ m titanium oxide 1000g, median size and be 400 μ m is that aluminum oxide 100g, the median size of 1300 μ m is that zinc oxide 1000g, the median size of 100 μ m is that hydrous iron oxide 1000g, the median size of 2000 μ m is the red oxide of iron 150g of 250 μ m, and median size is that 1000 μ m, specific surface area are 500m
2The WHITE CARBON BLACK 250g of/g adds at unsteady briquetting and to depress mixing about 15min, and mixture is uniformly dispersed, and mixture temperature rises to 105 ℃; With 5m
5/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-0.85amp, and 170～190 ℃ of mixing 3h (TRT 3h) promptly get the mixture base-material; The mixture base-material is moved in the planetary mixer of prior preheating, with 5m
5/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-0.85amp.Then, in the mixture base-material, adding viscosity is 100 mm
2/ s, hydrogen content be 1% (quality) methylhydrogenpolysi,oxane 150g, mix back decompression down row's bubble promptly be made into the A component.To move in the planetary mixer of prior preheating, with the same mixture base-material of A component with 5m
5/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-0.85amp.Then, the massfraction of the suitable Pt of adding is 1.0 * 10 in the mixture base-material
-6～5.0 * 10
-5Pure modification chloroplatinic acid catalyst 10g, 3-methyl isophthalic acid-butine-3-alcohol 15g, mix the back decompression down row's bubble promptly be made into the B component.A:B component proportioning is that 10:1 (quality, volume) mixes back decompression row's bubble down; Preferred ambient cure condition is: 25 ℃/24h; Preferred heating cure condition is: 40～60 ℃/30～120min or 80～150 ℃/15min are solidified into elastomerics.Through detecting, the flame retardant rating of present embodiment can reach the UL-94V-0 level, and thermal conductivity can arrive 8.0w/m ﹒ k, and heatproof can reach-100～300 ℃, and electrical insulation capability is good.
Bi-component organic silicon glue (10:1) embodiment 4
In the 5L Banbury mixer, adding viscosity is 25000 mm
2The a of/s, ω-divinyl polydimethylsiloxane 750g, viscosity is 28000 mm
2The a of/s; In the mixture of ω-divinyl polydimethylsiloxane 250g; Titanium oxide 1000g, the median size that adds median size again and be 1900 μ m is that cerium oxide 125g, the median size of 800 μ m is that aluminum oxide 250g, the median size of 1900 μ m is that zinc oxide 1500g, the median size of 200 μ m is that hydrous iron oxide 1000g, the median size of 3000 μ m is the red oxide of iron 150g of 500 μ m, and median size 1900 μ m, specific surface area 500m
2The WHITE CARBON BLACK 200g of/g adds at unsteady briquetting and to depress mixing about 15min, and mixture is uniformly dispersed, and mixture temperature rises to 105 ℃; With 5m
5/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-0.85amp, and 170～190 ℃ of mixing 3h (TRT 3h) promptly get the mixture base-material; The mixture base-material is moved in the planetary mixer of prior preheating, with 5m
5/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-0.85amp.Then, in the mixture base-material, adding viscosity is 250mm
2/ s, hydrogen content are the methylhydrogenpolysi,oxane 150g of 1% (quality), mix to arrange to steep under the decompression of back promptly to be made into the A component.To move in the planetary mixer of prior preheating, with the same mixture base-material of A component with 5m
5/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-0.85amp.Then, the massfraction of the suitable Pt of adding is 1.0 * 10 in the mixture base-material
-6～5.0 * 10
-5Platinum-vinyl siloxane complex catalyzer 10g, methylpentynol 15g, mix back decompression down row's bubble promptly be made into the B component.A:B component proportioning is that 10:1 (quality, volume) mixes back decompression row's bubble down, and viscosity is 50000 mm
2/ sa, the ambient cure condition is: preferred ambient cure condition is: 25 ℃/24h, preferred heating cure condition is: 40～60 ℃/30～120min or 80～150 ℃/15min are solidified into elastomerics.Through detecting, the flame retardant rating of present embodiment can reach the UL-94V-0 level, and thermal conductivity can arrive 8.0w/m ﹒ k, and heatproof can reach-100～300 ℃, and electrical insulation capability is good.
Two component (1:1) embodiment 5 of bi-component organic silicon glue
In the 5L Banbury mixer, adding viscosity is 50000 mm
2The a of/s, ω-divinyl polydimethylsiloxane 750g, viscosity is 45000 mm
2The a of/s; In the mixture of ω-divinyl polydimethylsiloxane 250g; Titanium oxide 1250g, the median size that adds median size again and be 2500 μ m is that cerium oxide 100g, the median size of 4000 μ m is that aluminum oxide 250g, the median size of 2500 μ m is that zinc oxide 1000g, the median size of 1000 μ m is that hydrous iron oxide 100g, the median size of 4000 μ m is the red oxide of iron 150g of 2500 μ m, and median size is 2500 μ m, specific surface area 500m
2The WHITE CARBON BLACK 250g of/g adds at unsteady briquetting and to depress mixing about 15min, and mixture is uniformly dispersed, and mixture temperature rises to 105 ℃; With 5m
3/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-0.85amp, and 170～190 ℃ of mixing 3h (TRT 3h) promptly get the mixture base-material; The mixture base-material is moved in the planetary mixer of prior preheating, with 5m
3/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-0.85amp.Then, in the mixture base-material, adding viscosity is 500mm
2/ s, hydrogen content be 1% (quality) methylhydrogenpolysi,oxane 600g, mix back decompression down row's bubble promptly be made into the A component.To move in the planetary mixer of prior preheating, with the same mixture base-material of A component with 5m
3/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-0.85amp.Then, the massfraction of the suitable Pt of adding is 1.0 * 10 in the mixture base-material
-6～5.0 * 10
-5Pure modification chloroplatinic acid catalyst 25g, 3-methyl isophthalic acid-butine-3-alcohol 5g mix the back decompression down row's bubble promptly be made into the B component.A:B component proportioning is that 1:1 (quality, volume) mixes back decompression row's bubble down; Preferred ambient cure condition is: 25 ℃/24h; Preferred heating cure condition is: 40～60 ℃/30～120min or 80～150 ℃/15min are solidified into elastomerics.Through detecting, the flame retardant rating of present embodiment can reach the UL-94V-0 level, and thermal conductivity can arrive 8.0w/m ﹒ k, and heatproof can reach-100～300 ℃, and electrical insulation capability is good.
Two component (1:1) embodiment 6 of bi-component organic silicon glue
In the 5L Banbury mixer, adding viscosity is 200000 mm
2The a of/s, ω-divinyl polydimethylsiloxane 750g, viscosity is 190000 mm
2The a of/s; In the mixture of ω-divinyl polydimethylsiloxane 250g; Titanium oxide 1250g, the median size that adds median size again and be 4000 μ m is that cerium oxide 100g, the median size of 8000 μ m is that aluminum oxide 150g, the median size of 3000 μ m is that zinc oxide 1500g, the median size of 2000 μ m is that hydrous iron oxide 2000g, the median size of 5000 μ m is the red oxide of iron 150g of 5000 μ m, and median size 3000 μ m, specific surface area 500m
2The WHITE CARBON BLACK 200g of/g adds at unsteady briquetting and to depress mixing about 15min, and mixture is uniformly dispersed, and mixture temperature rises to 105 ℃; With 5m
3/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-0.85amp, and 170～190 ℃ of mixing 3h (TRT 3h) promptly get the mixture base-material; The mixture base-material is moved in the planetary mixer of prior preheating, with 5m
3/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-0.85amp.Then, in the mixture base-material, adding viscosity is 1500mm
2/ s, hydrogen content are the methylhydrogenpolysi,oxane 100g of 1% (quality), mix to arrange to steep under the decompression of back promptly to be made into the A component.To move in the planetary mixer of prior preheating, with the same mixture base-material of A component with 5m
3/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-0.85amp.Then, the massfraction of the suitable Pt of adding is 1.0 * 10 in the mixture base-material
-6～5.0 * 10
-5Platinum-alkynes basigamy mixture catalyst 25g, 1-ethynyl-1-hexalin 5g, mix back decompression down row's bubble promptly be made into the B component.A:B component proportioning is that 1:1 (quality, volume) mixes back decompression row's bubble down, and viscosity is 50000 mm
2/ sa, preferred ambient cure condition is: 25 ℃/24h, preferred heating cure condition is: 40～60 ℃/30～120min or 80～150 ℃/15min are solidified into elastomerics.Through detecting, the flame retardant rating of present embodiment can reach the UL-94V-0 level, and thermal conductivity can arrive 8.0w/m ﹒ k, and heatproof can reach-100～300 ℃, and electrical insulation capability is good.
Organo-silicone rubber thermostability of the present invention is high; The chemical bond of (or radiation irradiation) molecule does not rupture, does not decompose under the high temperature; Therefore be difficult for being decomposed by UV-light and ozone, have than the better thermostability of other macromolecular materials and anti-irradiation and weather-proof ability, can reach decades the work-ing life under physical environment; Not only can be high temperature resistant, and low temperature resistant; Can in a very wide TR, use and have the excellent electric insulating ability; Its dielectric loss, proof voltage, anti-electric arc, anti-corona, volume resistivity and surface resistivity etc. all come out at the top in insulating material; And their electric property receives the influence of temperature and frequency very little; Therefore, they are a kind of stable electrically insulating materials, are widely used on electronics, the electrical industry; The present invention also has excellent water repellency except having good thermotolerance, this is that electricinstallation uses the guarantee with higher reliability under hygrometric state condition; Because range of application of the present invention is very extensive, its economic outlook, value are very considerable.
It can be single-component or two components 10 that the present invention can process different denseness (rheological, thixotropy), sulfuration back different modulus (high, medium and low) and various property (fire-retardant, heat conduction, high temperature resistant, low temperature resistant etc.) packed state through formulating of recipe
:1, two components 1
:1, condition of cure room temperature and heating is solidified back form rubber-like and gel, and cured article possesses simultaneously flame retardant resistance is arranged, high thermal conductivity, comprehensive physicals such as high temperature resistant, low temperature resistant.
Claims (13)
1. one kind fire-retardant, high heat conduction, high temperature resistant, low temperature resistant add-on type organo-silicone rubber; It is characterized in that comprising a; ω-divinyl polydimethylsiloxane, methylhydrogenpolysi,oxane, cerium oxide, zinc oxide, red oxide of iron, titanium oxide, aluminum oxide, hydrous iron oxide, WHITE CARBON BLACK, catalyzer, auxiliary agent; Their weight ratio is: 10-18:1-6:1-1.25:5-25:1-3:10-12.5:1-2.5:10-25:1-2.5:0.00 3-1.25:0.003-1.25, wherein:
Said a, the contents of ethylene of ω-divinyl polydimethylsiloxane is at 0.0013-2.1, and viscosity is at 100mm
2/ s-200000 mm
2In/s the scope; The viscosity of said methylhydrogenpolysi,oxane is at 5 mm
2/ s-1500 mm
2In/s the scope, hydrogen content is at 0.1-1.6%; The median size of said cerium oxide is at 1～8000 μ m, TIO
2Purity is more than 98%; The median size of said zinc oxide is at 1～2000 μ m, TIO
2Purity is more than 90%; The median size of said red oxide of iron is at 1～5000 μ m, TIO
2In purity more than 95%; The median size of said titanium oxide is at 2～4000 μ m, TIO
2In purity more than 99%; The median size of said aluminum oxide is at 1～3000 μ m, TIO
2In purity more than 98%; The median size of said hydrous iron oxide is at 10～5000 μ m, TIO
2In purity more than 96%; The median size of said WHITE CARBON BLACK in 1～3000 μ m, specific surface area at 10～1000m
2/ g; Said catalyzer is the catalyzer that contains the various title complexs of platinum.
2. fire-retardant, high heat conduction according to claim 1, high temperature resistant, low temperature resistant add-on type organo-silicone rubber; It is characterized in that: described a; ω-divinyl polydimethylsiloxane comprises a of two kinds of different viscosity and contents of ethylene; ω-divinyl polydimethylsiloxane mixes, this a of two kinds, and the viscosity of ω-divinyl polydimethylsiloxane is greater than 1000mm
2/ s is smaller or equal to 50000 mm
2/ s, its weight ratio is 1:50-50:1.
3. fire-retardant, high heat conduction according to claim 1, high temperature resistant, low temperature resistant add-on type organo-silicone rubber, it is characterized in that: the viscosity of said methylhydrogenpolysi,oxane is at 50-500 mm
2/ s, hydrogen content are 0.3-1%.
4. fire-retardant, high heat conduction according to claim 1, high temperature resistant, low temperature resistant add-on type organo-silicone rubber is characterized in that: said cerium oxide is the powder that comprises two kinds of different-grain diameters, median size 1～800 μ m of every kind of powder.
5. fire-retardant, high heat conduction according to claim 1, high temperature resistant, low temperature resistant add-on type organo-silicone rubber, it is characterized in that: said zinc oxide comprises the powder of two kinds of different-grain diameters, median size 1～200 μ m of every kind of powder.
6. fire-retardant, high heat conduction according to claim 1, high temperature resistant, low temperature resistant add-on type organo-silicone rubber, it is characterized in that: said red oxide of iron comprises the powder of two kinds of different-grain diameters, median size 1～500 μ m of every kind of powder.
7. fire-retardant, high heat conduction according to claim 1, high temperature resistant, low temperature resistant add-on type organo-silicone rubber, it is characterized in that: said titanium oxide comprises the powder of two kinds of different-grain diameters, the median size of every kind of powder is at 100～2500 μ m.
8. fire-retardant, high heat conduction according to claim 1, high temperature resistant, low temperature resistant add-on type organo-silicone rubber, it is characterized in that: said aluminum oxide comprises the powder of two kinds of different-grain diameters, the median size of every kind of powder is at 50～2500 μ m.
9. fire-retardant, high heat conduction according to claim 1, high temperature resistant, low temperature resistant add-on type organo-silicone rubber, it is characterized in that: said hydrous iron oxide comprises the powder of two kinds of different-grain diameters, the median size of every kind of powder is at 100～4000 μ m.
10. fire-retardant, high heat conduction according to claim 1, high temperature resistant, low temperature resistant add-on type organo-silicone rubber, it is characterized in that: said WHITE CARBON BLACK comprises the powder that comprises two kinds of different-grain diameters, median size 50～2500 μ m of every kind of powder.
11. fire-retardant, high heat conduction according to claim 1, high temperature resistant, low temperature resistant add-on type organo-silicone rubber; It is characterized in that: said catalyzer is a kind of in platinum-vinyl siloxane complex, pure modification Platinic chloride title complex, the platinum-alkynes basigamy compound; Its consumption is with a, and ω-divinyl polydimethylsiloxane and methylhydrogenpolysi,oxane content sum are that benchmark is counted 100-10000ppm by pt.
12. fire-retardant, high heat conduction according to claim 1, high temperature resistant, low temperature resistant add-on type organo-silicone rubber; It is characterized in that: said auxiliary agent is a kind of in 3-methyl isophthalic acid-butine-3-alcohol, methylpentynol, the 1-ethynyl-1-hexalin; Its consumption is with a, and ω-divinyl polydimethylsiloxane and methylhydrogenpolysi,oxane content sum are that benchmark is counted 100-10000ppm by pt.
13. the preparation method of fire-retardant, a high heat conduction as claimed in claim 1, high temperature resistant, low temperature resistant add-on type organo-silicone rubber is characterized in that comprising the steps:
1), in Banbury mixer, add a, ω-divinyl polydimethylsiloxane adds titanium oxide, cerium oxide, aluminum oxide, zinc oxide, hydrous iron oxide, red oxide of iron again, and WHITE CARBON BLACK, adds at unsteady briquetting and depresses mixingly, and mixture is uniformly dispersed,
2), make mixture temperature rise to 100-110 ℃ again; And with 2-8m
3/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-1～-0.7amp, 170～190 ℃ of mixing 2～5h promptly get the mixture base-material;
3), the mixture base-material is moved in the stirrer of prior preheating, with 2-8m
5/ h flow feeds nitrogen, keeps vacuum state vacuum tightness to be :-1～-0.7amp;
4), in the mixture base-material, add methylhydrogenpolysi,oxane, catalyzer and auxiliary agent, mix back decompression down row's bubble get final product.
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| CN1840599A (en) * | 2005-04-01 | 2006-10-04 | 信越化学工业株式会社 | Hot-compressing adhesive sheet |
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