CN103012973A - High heat conductivity nanocomposite rubber - Google Patents
High heat conductivity nanocomposite rubber Download PDFInfo
- Publication number
- CN103012973A CN103012973A CN2012105739792A CN201210573979A CN103012973A CN 103012973 A CN103012973 A CN 103012973A CN 2012105739792 A CN2012105739792 A CN 2012105739792A CN 201210573979 A CN201210573979 A CN 201210573979A CN 103012973 A CN103012973 A CN 103012973A
- Authority
- CN
- China
- Prior art keywords
- rubber
- agent
- high heat
- parts
- heat conducting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a high heat conductivity nanocomposite rubber. The raw materials comprise one or more of the following components: ethylene-propylene-diene-terpolymer (EPDM) rubber, anti-aging agents, carbon black, sulfur, accelerants, plasticizers, paraffin oil, an organic active agent PEG4000, inorganic active agents and dispersing agents. The nanocomposite rubber has the beneficial effects that the heat conductivity of the composite material is greatly improved by using the mixed fillers; granules and whiskers with certain length-diameter ratios are utilized to form a continuous heat conduction network chain; the fillers in different grain sizes are selected and combined to achieve higher filling density; a coupling agent is utilized to improve the interfaces of the fillers and the matrix to reduce the heat resistance on the interfaces; the heat conductivity is improved by filling the rubber with nano materials; molecule interaction forces between the thermoplastic rubber and the fillers are improved by utilizing unique molecular design; and a heat channel is formed through efficient contact between the fillers, thus greatly improving the heat conductivity.
Description
Technical field
The present invention relates to the nanometer new material technology field, particularly relate to the high heat conduction compounded rubber of a kind of nanometer.
Background technology
Now, because electronic product more and more is tending towards miniaturization, therefore those easily integrated and miniaturization and the good compounded rubber substrate of snappiness are widely used, but because the multiple stratification of the highly integrated and laminate of unicircuit certainly leads to the heat release problem, so the requirement of the heat conductivility of these materials just become the task of top priority.
Terpolymer EP rubber (EPDM) is the terpolymer of ethene, propylene and dienes monomer, and the introducing of diene is to vulcanize in order to realize, the type of diene has: dicyclopentadiene (DCPD), l, 4 one hexadienes.EPDM is better than common ethylene-propylene rubber(EPR) toughness.
People have tentatively solved this problem with dielectric metal oxide and other compound filled polymers in recent years.The filler of insulated type heat conductive rubber mainly comprises: metal oxide such as BeO, MgO, A1
2O
3, CaO, NIO; Metal nitride such as AlN, BN etc.; Carbide such as SiC, B
4C
3Deng.They have higher thermal conductivity, and what is more important compares with metal powder excellent electrical insulating property is arranged, so they can guarantee that end article has good electrical insulating property, and this is vital in electronic apparatus industry.
For the research of heat conductive rubber with use a lot, can be divided into by the kind of particle filled composite: metal filled type, metal oxide filled-type, metal nitride filled-type, inorganic non-metallic filled-type, fiber filled type heat conductive rubber; Also can divide according to a certain character of heat conductive rubber, such as can be divided into insulated type heat conductive rubber and nonisulated type heat conductive rubber according to its electrical insulation capability.
Because rubber itself has insulativity, the therefore electrical insulation capability of most heat conductive rubbers finally is that the insulating property by particle filled composite determine.The filler that is used for nonisulated type heat conductive rubber usually is metal powder, graphite, carbon black, carbon fiber etc., the characteristics of this class filler are to have good thermal conductivity, can easily make material obtain high heat conductivility, but simultaneously also so that the decreasing insulating of material even become electro-conductive material.Therefore in the less demanding situation, can use above-mentioned filler for electrical insulating property at the Working environment of material.And also necessarily require under certain conditions heat conductive rubber to have low electrical insulating property to meet specific requirement, such as electromagnetic shielding material etc.
Flourish information industry in the last few years, performance to macromolecular material has proposed Secretary, especially the development for heat conductive rubber provides development space, the application of heat conductive rubber on computer fittings will improve the heat dissipation problem of computer and improve its travelling speed and stability, such as CPU, notebook computer shell and various surface-mounted integrated circuit, these materials all require heat conductive insulating.Macromolecular material insulate, but as thermally conductive material, pure macromolecular material generally is inefficient, because macromolecular material is the poor conductor of heat mostly, the macromolecular material thermal conductivity is about the 1/500-1/600 of metal.Must carry out modification to macromolecular material.The thermal conductivity of metal and metal oxide sees Table 1-1, table 1-2.
The thermal conductivity of table 1-1 metal and metal oxide
Can substantially have following several as metal and the mineral filler of heat conduction particle:
(l) metal powder filler: copper powder, aluminium powder, bronze, silver powder.
(2) metal oxide: aluminum oxide, oxidation is secret, barium oxide, magnesium oxide, zinc oxide.
(3) metal nitride: aluminium nitride, boron nitride.
(4) inorganic non-metallic: graphite, silicon carbide.
Ceramic is during as heat conductive filler filled high polymer material matrix, and the quality of filling effect depends primarily on following factor: (l) kind of polymeric matrix, characteristic; (2) shape of filler, particle diameter, distribution of sizes; (3) interaction of the interface binding characteristic of filler and matrix and two-phase.
The thermal conductivity of some packing materials of table 1-2
Because the adding of filler descends the mechanical property of material.Therefore, the conductivity that in the design of matrix material, not only will consider, and require that stability of material is good, nontoxic, satisfactory mechanical property and inexpensive.Another selection with respect to filled polymer is the polymkeric substance that use itself has the good heat conductive performance, but materials is expensive and performance on deficient in stability, become their main drawback in the use.Rubber is the material of output maximum in the macromolecular material.
The market requirement of conductivity macromolecular material is all increasing every year, and wherein the market demand of heat conductive rubber increases faster.Therefore the research of rubber heat conductivility is caused various countries investigator's interest, and done good work.The at present research of fillibility heat conductive rubber, most of method that adopts physics to fill, heat conductivility is poor, and mechanical property descends serious, and production cost is high.But along with the market of expanding day and going deep into of research, heat conductive rubber will have a large development, especially the research and development of nano heat-conductive material, high heat conduction mass polymer material preparation, the discussion of polymkeric substance thermal conduction mechanism should become the developing direction of heat-conducting polymer material.
Summary of the invention
Technical problem to be solved by this invention is to be, electric packaged material requires heat conduction, insulate and have lower specific inductivity, good heat-conductive characteristic and low thermal expansivity.Materials is the larger application market of heat-conducting polymer material.The present invention is inorganic particulate filler superfine, even during to nano-scale, the variation of matter can occur because of the variation of interatomic distance in the particle and structure the thermal conductivity of itself.Thermal conductivity such as aluminium nitride is about 36w/ (m.K), and the thermal conductivity of nano level aluminium nitride can reach 320w/ (m.K).The trickle magnesium oxide of high purity, its thermal conductivity are not less than 50w/ (m.K), are equivalent to 4 times of silicon oxide, 3 times of aluminum oxide.
For solving the problems of the technologies described above, obtain the matrix material of high thermal conductivity, the invention provides a kind of high heat conducting nano compounded rubber, its raw material comprises one or more in the following component: terpolymer EP rubber, anti-aging agent, carbon black, sulphur, promotor, softening agent, paraffin oil, organic active agent PEG4000, the inorganic active agent, dispersion agent.
Described material content proportioning is preferably by weight:
Terpolymer EP rubber 150-200 part,
Anti-aging agent 1-4 part,
Carbon black 40-80 part,
Sulphur 1-3 part,
Promotor 1-3 part,
Softening agent 6-10 part,
Paraffin oil 40-80 part,
Organic active agent PEG4000,3-8 part
Inorganic active agent 6-12 part,
Dispersion agent 1-4 part.
Described anti-aging agent is preferably one or more in the following reagent: 6-oxyethyl group-2,2,4-trimethylammonium-1,2-dihyaroquinoline; 2,2,4-trimethylammonium 1,2-dihydro quinoline polymer; N-phenyl-α-aniline; The N-Phenyl beta naphthylamine; N-phenyl-N`-cyclohexyl Ursol D; N-phenyl-N`-sec.-propyl-Ursol D.N-N`-phenylbenzene-Ursol D.
Described promotor is preferably one or more in the following reagent: promotor T; N, the two thiamides of N-tetramethyl-two sulphur; Tetramethyl-thiuram disulfide; Thiram; Vulcanization accelerator TMTD; Tetramethyl-dithio thiuram; Vulcanization accelerator TMTD; Vulcanization accelerator TMTD-II; Promotor TT; Curing two (thiocarbonyl group dimethylamine); Curing tetramethyl-TMTD; Tetramethyl-sulfo-peroxy dicarbonate diamide; Tetramethyl thiuram disulfide; TMTD; Altax; Accelerant B Z.
Described softening agent is preferably one or more in the following reagent:: o-phthalic acid dibutyl ester; DEDB; Octyl adipate; Di-n-hexyl adipate; Butyl benzyl phthalate; Sebacic acid two (2-ethyl hexyl) ester.
Described promoting agent is preferably PEG4000; Described dispersion agent is preferably one or more in the following reagent: triethyl hexyl phosphoric acid, sodium lauryl sulphate, methyl amyl alcohol, derivatived cellulose, polyacrylamide, guar gum, fatty acid polyglycol ester.
Described inorganic active agent is preferably one or more in the following reagent: MgO, Al
2O
3, Si
3N
4, BN, AlN, ZnO, KAl (SO
4)
212H
2O, Al
2O
3-2SiO
2-2H
2O.
Described AlN is preferably: AlN whisker and AlN particle.
Described Si
3N
4Be preferably highly heat-conductive silicon nitride; Described BN is the nano silicon nitride boron particles, satisfies following index:
Described high heat conducting nano compounded rubber preferably prepares by following steps:
The first step, synthetic rubber: by Banbury mixer with described raw material synthetic rubber;
Second step, moulding: by mill with the synthetic rubber moulding;
In the 3rd step, sulfuration: moulding rubber is put into the mould of vulcanizer, the pressurization scope is 150-210kgf/ ㎝
2, being warmed up to 220-230 ℃, the time is 80-100 second, vulcanizes.
The present invention mixes the thermal conduction capability that uses the raising polymer-based carbon by the filler to various different shapeies and size and has carried out the experiment contrast, and filler comprises MgO, Al
2O
3, Si
3N
4, BN, AlN, ZnO, KAl (SO
4)
212H
2O(alum), Al
2O
3-2SiO
2-2H
2O(kaolin) etc.The present invention significantly improves the thermal conductivity of matrix material with mixed fillers.Utilization of the present invention has particle, the whisker of certain length-to-diameter ratio to form continuous heat conduction network chain; Select the filler combination of different particle diameters, reach higher filling density: the interface that utilizes coupling agent to improve filler and matrix, to reduce thermal resistance at the interface; Improve thermal conductivity with nanomaterial-filled rubber.The high heat conduction compounded rubber of nanometer of the present invention is that thermal conductivity is up to the material of 22.25 ~ 35.56w/mK.The technology of the present invention is utilized unique molecular designing, has improved the interaction force of molecule between thermoplastic elastomer and the filler, and filler high-level efficiency contact has each other formed the heat passage, has increased substantially thermal conductivity.
Embodiment
Describe embodiments of the present invention in detail below with reference to embodiment, how the utilisation technology means solve technical problem to the present invention whereby, and the implementation procedure of reaching technique effect can fully understand and implements according to this.
Embodiment 1: the compound terpolymer EP rubber of the present embodiment high heat conducting nano high-speed vulcanization, and each material component content proportioning is by weight:
Terpolymer EP rubber 150-200 part,
Anti-aging agent 1-4 part,
Carbon black 40-80 part,
Sulphur 1-3 part,
Promotor 1-3 part,
Softening agent 6-10 part,
Paraffin oil 40-80 part,
Organic active agent PEG4000,3-8 part
Inorganic active agent 6-12 part,
Dispersion agent 1-4 part,
And it prepares by following steps:
The first step, synthetic rubber: by Banbury mixer with the above-mentioned raw materials synthetic rubber;
Second step, moulding: by mill with the synthetic rubber moulding;
In the 3rd step, sulfuration: moulding rubber is put into the mould of vulcanizer, the pressurization scope is 150-210kgf/ ㎝
2, being warmed up to 220-230 ℃, the time is 80-100 second, vulcanizes.
Embodiment 2: the rubber dispersion agent is to impel material particles to be dispersed in the Rubber Media, forms the reagent of stable suspension.The rubber dispersion agent that uses in the embodiment of the invention is one or more in the following reagent: triethyl hexyl phosphoric acid, sodium lauryl sulphate, methyl amyl alcohol, derivatived cellulose, polyacrylamide, guar gum, fatty acid polyglycol ester.
Embodiment 3:
The anti-aging agent that one embodiment of the invention is used is: 6-oxyethyl group-2,2,4-trimethylammonium-1,2-dihyaroquinoline.Its trade name is antioxidant A W.Antioxidant A W is the brown thick liquid, and sterling is light brown sticking cylinder liquid.Nontoxic, proportion is 1.029 ~ 1.030(25 ℃), boiling point is 169 ℃.Can be dissolved in benzene, acetone, two oxidative ethanes, tetracol phenixin, industrial naptha and ethanol; Water insoluble.Shelf-stable.Be special efficacy anti-ozone anti-aging agent, flex crack and thermo-oxidative ageing are also had protective effect.The goods that are specially adapted to use under the dynamic condition.No blooming has contaminative, is unsuitable for light goods.Little on the sulfuration impact during 1 ~ 2 part of consumption, increase to 3 parts and then significantly promote sulfuration, promote during use that consumption should suitably reduce.
The anti-aging agent that another embodiment of the present invention is used is: 2,2,4-trimethylammonium 1,2-dihydro quinoline polymer.Trade name is anti-aging agent RD.Anti-aging agent RD be amber to canescence arborescens powder, nontoxic.Softening temperature is not less than 74 ℃.Can be dissolved in acetone, benzene, chloroform, dithiocarbonic anhydride, be slightly soluble in petroleum hydrocarbon; Water insoluble.The oxidation that the energy rejection condition is harsh, thermal ageing and Weather effect, but relatively poor to the flex crack protection effect.No blooming, light contamination is arranged.General amount ranges is 0.5 ~ 2 part, reaches as high as 3 compositions.
The anti-aging agent that yet another embodiment of the invention is used is: N-phenyl-α-aniline.Trade name is antioxidant A.Antioxidant A be tawny to purple crystal shape material, sterling is colourless plate crystal, and is poisonous because containing a small amount of methyl naphthylamine and aniline, can not with skin contact.Proportion is 1.16 ~ 1.17, and fusing point is not less than 52.0 ℃.Be soluble in acetone, ethyl acetate, benzene, ethanol, chloroform, tetracol phenixin; Dissolve in gasoline; Water insoluble.Gradual change purple in daylight and the air.Inflammable.Antioxidant A to heat, oxygen, subdue and the solarization such as weather all has good protection effect, be the general anti-aging agent of natural rubber, synthetic rubber and reclaimed rubber.In chloroprene rubber, have the performance of anti-ozone ageing concurrently; Solarization and reclaimed rubber to variable valency metal ions also have certain inhibition easily to disperse in dried glue, also easily are scattered in the water; Solubleness in rubber is up to 5%, and is larger than antioxidant D, and consumption is no blooming in the time of 3 ~ 4 parts, therefore can increase consumption to improve protective benefits.Antioxidant A has contaminative and transport property.General amount ranges is 1 ~ 2 part, reaches as high as 5 parts.
The anti-aging agent that further embodiment of this invention is used is: the N-Phenyl beta naphthylamine.Trade name is antioxidant D.Antioxidant D is light grey to light brown powder, and sterling is white powder.Proportion is 1.18, and fusing point is not less than 104 ℃.Easily solvent is in acetone, ethyl acetate, dithiocarbonic anhydride, chloroform; Dissolve in ethanol, tetracol phenixin; Be insoluble to gasoline and water.Under air and daylight, gradually become grey black, but do not affect protection effect.Inflammable.Antioxidant D is the universal anti-aging agent of natural rubber, synthetic rubber and latex.Heat, oxygen, flex crack and general aging action all there are good protective effect, and slightly are better than antioxidant A.Ion to poisonous metal also has protective effect, but poor than antioxidant A.If with anti-aging agent 4040 or 4010NA and usefulness, heat resistanceheat resistant, oxygen, flex crack and anti-ozone ageing performance all have remarkable increase.In dried glue, easily be scattered in the water.Solubleness in rubber is lower than antioxidant A, is about 1.5%.Meeting bloom when consumption surpasses 2 parts is with antioxidant A and with then avoiding.The tool contaminative is unsuitable for light goods.Amount ranges is generally 0.5 ~ 2 part.This class anti-aging agent is simple, cheap because raw material is easy to get, makes, therefore also occupy at home certain status at present.
The anti-aging agent that further embodiment of this invention is used is: N-phenyl-N`-cyclohexyl Ursol D.Trade name is antioxidant 4010 (or anti-aging agent CPPD).Antioxidant 4010 is pale powder, and sterling is white powder.Skin there is pungency.Proportion is 1.29, and fusing point very easily is dissolved in methyl chloride for being lower than 110 ℃, is soluble in benzene, ethyl acetate, acetone, is insoluble in industrial naptha, and is water insoluble.In air or the daylight end deepen look, but protection is renderd a service and not to be subtracted.Antioxidant 4010 is one of good universal anti-aging agent of natural rubber and synthetic rubber, is particularly useful for natural rubber and styrene-butadiene rubber(SBR).Good to aging action protective benefitses such as heat, oxygen, ozone, light, also be the be full of cracks of good lasting mechanical stress formation and the inhibitor of flex crack.The solarization of high-energy radiation and cupric ion also had necessarily protective effect.Protection effect than antioxidant A T and antioxidant D is all good, existing goodish protective benefits when alone, but with its anti-aging agent such as AW, crystallinity and use ozone-induced cracking and weather aging protective benefits higher.Also can and use with antioxidant A, D or other universal anti-aging agent.Antioxidant 4010 easily disperses, and consumption can produce bloom when surpassing 1 part, and it is serious that goods are met phototropic.Also can migration stain other sizing material that contacts with it or material.0.15 ~ 1 part of general amount ranges.
The anti-aging agent that further embodiment of this invention is used is: N-phenyl-N`-sec.-propyl-Ursol D.Trade name is antioxidant 4010NA (or anti-aging agent IPPD).Antioxidant 4010NA is the purple plate crystal.Little toxic, can cause allergic anti-hydraulic pressure.Fusing point is not less than 70 ℃.Dissolve in oils, benzene, ethyl acetate, tetracol phenixin, methylene dichloride, chloroform, dithiocarbonic anhydride, acetone, ethanol, be insoluble in gasoline, water insoluble.Shelf-stable.Meeting variable color under the daylight, but do not affect usefulness.Antioxidant 4010NA is the universal anti-aging agent of natural rubber, synthetic rubber latex glue.Good to ozone-induced cracking, flex crack barrier propterty spy; Also be heat, oxygen, light and general aging good protective agent.The solarization that also can suppress variable valency metal ions, protection natural rubber performance than 4010 more comprehensively.Antioxidant 4010NA can be alone, produces with not only reducing consumption but also can improving protective benefits with antioxidant A W or wax.Especially with wax and with staying the anti-static ozone-induced cracking performance of improving the standard.Fusing point is lower, easily disperses, and the solubleness in rubber is larger than 4010, and bloom is less, therefore can improve consumption.Contaminative is large.Be usually used in dynamically and condition that static stress is higher under the goods that use.General amount ranges is 1 ~ 4 part.
The anti-aging agent that further embodiment of this invention is used is: N-N`-phenylbenzene-Ursol D.Trade name is antioxidant H.(having another name called antioxidant DPPD or anti-aging agent PPD).Antioxidant H is that the beige powder is lumped together, and sterling is silvery white plate crystal.Proportion is 1.18 ~ 1.22.Fusing point is not less than 140 ℃.Dissolve in benzene, toluene, acetone, ether, ethylene dichloride, dithiocarbonic anhydride, be slightly soluble in ethanol and gasoline; Water insoluble.Storage-stable.In air, reach under the daylight easy to change.Inflammable.Antioxidant H is natural rubber, elastomeric universal anti-aging agent, has good flex cracking resistance performance, and is excellent to the aging protective effect of heat, oxygen, ozone, light, particularly copper, mn ion.Especially be applicable to natural rubber and elastomeric paralled system.But variable color and seriously polluted.Solubleness in rubber is low; Being up to 0.7% in styrene-butadiene rubber(SBR), is 0.35% in natural rubber, and solubleness is lower in polybutadiene rubber.The bloom phenomenon appears in consumption when surpassing its solubleness, when with other anti-aging agent such as antioxidant A and time spent, can reduce its consumption and can improve protection effect again.Amount ranges is generalized to 0.2 ~ 0.3 part when alone.
Embodiment 4: the promotor that the embodiment of the invention is used is one or more in the following product: promotor T, N, the two thiamides of N-tetramethyl-two sulphur, tetramethyl-thiuram disulfide, thiram, vulcanization accelerator TMTD, tetramethyl-dithio thiuram, Vulcanization accelerator TMTD, Vulcanization accelerator TMTD-II, promotor TT, curing two (thiocarbonyl group dimethylamine), curing tetramethyl-TMTDs, tetramethyl-sulfo-peroxy dicarbonate diamide, tetramethyl thiuram disulfide, TMTD, rubber accelerator DM, accelerant B Z.
Embodiment 5:
The softening agent that one embodiment of the invention is used is: o-phthalic acid dibutyl ester (DOP).Plasticizer DOP is colourless oil liquid, proportion 0.9861 (20/20), fusing point-55, boiling point 370(normal pressure), water insoluble, be dissolved in ethanol, ether, the most of organic solvents of mineral wet goods.General purpose grade DOP is widely used in the industry such as plastics, rubber, paint and emulsifying agent.DOP is universal softening agent, be mainly used in the processing of polyvinyl chloride fat, the also processing of the superpolymer such as can be used for ground resin, acetate resin, ABS resin and rubber, the PVC that also can be used for making lacquer, dyestuff, dispersion agent etc., DOP plasticising can be used for manufacturer's fabricate-leather, agricultural film, wrapping material, cable etc.
The softening agent that another embodiment of the present invention is used is: DEDB.DEDB and polyvinyl chloride and the rare multipolymer of vinyl chloride acetic acid second, the poly-rare good intermiscibility of acetic acid second, also and polyvinyl chloride, polymethyl acrylate, polyvinyl alcohol butyral, Nitrocellulose, N-BUTYL ACETATE Mierocrystalline cellulose and ethyl cellulose etc. mix.The DEDB lighter color, plasticizing efficiency is high, intermiscibility good, volatility is low, exudative low, thermally-stabilised index is high, cold-resistant water-fast extraction, be difficult for oxidation and volatilization, excellent electrical properties, the weighting agent capacity is large, goods luminance brightness high.Be widely used in PVC plastic grain, non-filling calendered film, leatheroid, CABLE MATERIALS, sheet material, sheet material, soft or hard tubing, sole material, rubber-plastic strip, foamed material, film, paint, rubber, synthetic glass, printing-ink, plastipaste, acetate emulsion tackiness agent etc.Be minimum a kind of of softening agent industry price, can significantly reduce the rubber product cost.
The softening agent that yet another embodiment of the invention is used is: Octyl adipate.Its chemistry is by name: hexanodioic acid 2121 ethylhexyls, molecular formula are C
22H
42O
4, Octyl adipate is the colorless and odorless transparent oily liquid, can be dissolved in most of organic solvents such as ethanol, ether, acetone, acetic acid, is slightly soluble in ethylene glycol, and is water insoluble.But the volatility of Octyl adipate is large, and there is certain deficiency the aspects such as water tolerance, transport property, insulativity.Octyl adipate is normal and phthalate is composite, is applied to cold-resistant agricultural film, cable coating layer, leatheroid, sheet material, outdoor water pipe and Frozen Food Packaging film etc.Octyl adipate can also be as the low temperature of the various synthetic rubber cold resistant plasticizer with resins such as softening agent and Nitrocellulose, ethyl cellulose, polystyrene, vinylchlorid one acetic acid butylene copolymers.At present, di-n-hexyl adipate also is widely used in the polyvinyl butyral resin film.In addition, in many countries, legal its can be used as the softening agent of food, medical packaging plastics.
The softening agent that further embodiment of this invention is used is: di-n-hexyl adipate.Di-n-hexyl adipate is the cold resisting type softening agent of in the world consumption maximum.N-octyl-n-decyl adipate, colourless transparent liquid is n-Octanol, the synthetic straight chain type binary acid mixed ester of nonylcarbinol esterification by hexanodioic acid and straight chain; N-octyl-n-decyl adipate is dissolved in mineral oil, gasoline and most of organic solvent, and is insoluble or be slightly soluble in glycerine, glycols and some amine, is the straight chain type cold-resistant plasticizer of excellent property.Compare with the hexanodioic acid branched-chain alcoho and to have better resistance to low temperature, and volatilization loss, thermotolerance and photostabilization, water-fast extractable etc. are also good than the side chain alcohol ester.When itself and phthalic ester share, can improve polyvinyl chloride Vinyl Acetate Copolymer Emulsion performance, be widely used for the cold resistant plasticizer of polyvinyl acetate (PVA), polystyrene, polymethylmethacrylate, nitrocellulose, ethyl cellulose and rubber.
The softening agent that further embodiment of this invention is used is: butyl benzyl phthalate (Butyl benzyl phthalate) molecular weight 312.40.Character: colourless transparent oil liquid.Relative density (25 ℃/4 ℃) 1.116, zero pour-35 ℃, 370 ℃ of boiling points. 199 ℃ of flash-points (opening). specific refractory power 1.535. viscosity (25 ℃) 41.5mPas is dissolved in organic solvent and hydro carbons.Water insoluble.Flammable.Little poison.Good with most of rubber and resin compatible. solvation is strong, as the softening agent of heat-resisting, the oil resistant extractable of water tolerance.
The softening agent that further embodiment of this invention is used is: cold resistant plasticizer DOS.Dioctyl sebacate (DOS), formal name used at school: sebacic acid two (2-ethyl hexyl) ester molecule formula: C
26H
50O
4Cold resistant plasticizer DOS is colourless or faint yellow transparent oily liquid, zero pour-48 ° C, boiling point: 256 ° of C (0.67Kpa), point of ignition 257-263 ° C, viscosity 25mPa.s (20 ° of C), refractive index 1.449-1.451 (25 ° of C) can be dissolved in the organic solvents such as hydro carbons, alcohols, ketone, ester class, chlorinated hydrocarbon, is insoluble to di-alcohols and water.Cold resistant plasticizer DOS is the good cold resistant plasticizer of a kind of polyvinyl chloride, and plasticizing efficiency is high, and volatility is low, therefore except having good low temperature cold tolerance, preferably thermotolerance is arranged again, can use under higher temperature.The weathering resistance of this product is better, and electrical insulation properties is also more excellent, and normal and phthalate and usefulness are specially adapted to the goods such as cold-resistant electric wire and CABLE MATERIALS, leatheroid, film, sheet material, sheet material.Cold resistant plasticizer DOS can be as the low temperature of the various synthetic rubber cold resistant plasticizer with resins such as softening agent and Nitrocellulose, ethyl cellulose, polymethylmethacrylate, polystyrene, vinyl chloride copolymers.
Embodiment 6: the inorganic active agent that comprises in the raw materials is one or more in the following compounds (or mixture): MgO, Al
2O
3, Si
3N
4, BN, high purity carbon dust, AlN, ZnO, KAl (SO
4)
212H
2O(alum), Al
2O
3-2SiO
2-2H
2O(kaolin).
Embodiment 7: the MgO that the embodiment of the invention is used is the nano-MgO particle.
The nano-powder material industrialized producing technology requires the preparation method simple, and production cost is suitable, good reproducibility, and powder granularity is even, product purity is high, the reunion degree is low.A lot of about the synthetic method of nano magnesia in the prior art, but in fact can be applied to industrial less.The one, because problems such as equipment, cost, raw material, scale, investments; The 2nd, some technique still is in the laboratory study stage, and the realization suitability for industrialized production is had any problem, even some may not realize suitability for industrialized production.
The present embodiment adopts indoor temperature solid phase method to prepare the MgO particle.
Solid-phase reaction of the present invention has overcome conventional wet and has prepared the agglomeration traits that the bitter earth nano particle exists, and has reaction and need not the advantages such as solvent, productive rate is high, reaction conditions is easy; And overcome that the efficient that exists in original solid-phase reaction is low, the shortcoming of the easy oxidation distortion of particle.
The concrete grammar that the present embodiment indoor temperature solid phase method prepares the MgO particle is: with MgCI solution and Na
2CO
3(raw material mass mixture ratio 1:1.2) solution, take PVA solution (polyvinyl alcohol solution) as properties-correcting agent, reaction produces precipitation MgCO
3Precipitation, then under 75 ~ 85 ℃ of constant temperature, the mode that transforms by precipitation has obtained alkali formula carbon formula magnesium presoma.50 ~ 60 ℃ left standstill alkali formula carbon formula magnesium presoma precipitation 24-30 hour.Pass at the Ar air-flow at last, temperature is calcination under 600 ~ 650 ℃ the condition, has obtained the nano-MgO particle.Adopt PVA as polymeric surface active agent, controlled the reunion of particle, prepared nano-MgO particle dispersion is better, is cubic structure, and is substantially spherical in shape, and its particle diameter is 25-35nm.
Embodiment 8-1: the Si that the embodiment of the invention is used
3N
4Be the nano silicon nitride silicon grain, satisfy following index:
Embodiment 8-2: the Si that the embodiment of the invention is used
3N
4Can also be highly heat-conductive silicon nitride.Common silicon nitride has randomly-oriented sintering structure.Highly heat-conductive silicon nitride is to add kind of crystal grain (diameter 1um, long 3-4um) at material powder (below the particle diameter 1um), makes the sub-orientations of this all crystal grain, forms the fibrous silicon nitride structure that reaches 100um with orientation.Because the formation of filamentary structure, thermal conductivity presents each diversity, and thermal conductivity is 120w/ (mK) on the oriented structure direction, is 3 times of common silicon nitride, is equivalent to the thermal conductivity of steel.
Embodiment 9: the BN that the embodiment of the invention is used is the nano silicon nitride boron particles, satisfies following index:
Embodiment 10: the high purity carbon dust that the embodiment of the invention is used is: the 10000 high pure carbon powder of pulling together to produce in the Dongguan.Performance index are:
| Fixed carbon: | 99.99% | Specification: | 10000 orders |
| The trade mark: | 18925457433 | Moisture: | 0.015% |
| Turgidity: | 1-2 doubly | The screen overflow granularity: | 0.0006% |
| Ash content: | 0.85 | Volatile matter: | 0.01％ |
| The screen underflow granularity: | 0.0005% |
Embodiment 11: the AlN filler that the embodiment of the invention is used is: AlN whisker and AlN particle are done filler.In the embodiment of the invention, as matrix, AlN whisker and AlN particle (6um is following) are filled, and obtain the matrix material of the highest thermal conductivity 28.2W/ (m.K) with ABS, and AlN whisker and AlN particle ratio (mass ratio) are l:40 ~ 60.What the present invention had further studied filler mixes effect and coupling agent to the impact of matrix material heat conductivility.With AlN whisker and the AlN mix particles of adequate rate, give matrix material higher heat-conductivity and lower thermal expansivity than independent with whisker and particle.By using the coupling agent silane treatment, the thermal conductivity of the ABS matrix material of AlN particulate reinforcement improves 98%, and it is because by improving the interface of matrix and particle, the contact resistance of filler-matrix reduces that thermal conductivity improves.
Embodiment 12: the ZnO that the embodiment of the invention is used is: nano granular of zinc oxide.Its performance index are:
The nano zine oxide that the embodiment of the invention is used, for above-mentioned: 1 class nano-ZnO, 2 class nano-ZnOs, 3 class nano-ZnOs, in a kind of.
Embodiment 13: performance test and sign experiment contrast.
Experimental installation
This experiment adopts flash of light heat transfer analysis instrument LFA447N ano flashTM that thermal diffusivity is measured.This conductometer uses xenon lamp as heating source heated sample surface, uses infrared eye to read the sample temperature rise, has reduced potential surface resistance of heat transfer.
Experimental principle
Under certain design temperature T (constant temperature), launch the light beam pulse by laser source (or photoflash lamp) in moment, uniform irradiation is at the sample lower surface, use the corresponding temperature rise process in infrared detector measurement sample upper surface centre, obtain temperature and raise to the relation curve of time.By half heating-up time (sample upper surface temperature is elevated to peaked half required time after receiving optical pulse irradiation) t50 (or claiming t1/2), by following formula:
α＝01388×d
2/t
50 (1)
Can obtain the thermal diffusivity α of sample under temperature T.In the formula, d is the thickness of sample.Thermal conductivity λ is tried to achieve by following formula:
λ＝α×C
p×ρ (2)
In the formula, Cp is the specific heat of rubber; ρ is the density of rubber.Specific heat is relatively tried to achieve by sample and reference sample.Density is recorded than heavy material balance by micro computer.
The sample preparation
During test sizing material is cut into the thin rounded flakes that diameter is 12.5 ~ 12.7mm, and guarantees that the sample upper and lower surface is smooth, smooth.
Experimental procedure
(1) half an hour before the experiment, pour an amount of liquid nitrogen in instrument, regulate external recirculated water controller, set temperature makes it be higher than 2 ~ 3 degrees centigrade of room temperatures, pre-thermal instrument.
(2) be that the vernier callipers of 0.02mm carries out three times to the thickness of test specimen and measures with precision, get its mean value as the thickness of sample.
(3) with alcohol with the sample wiped clean, dry.Upper and lower surface at sample is carried out uniform graphite coating.
(4) sample is put into sample well, open Survey Software, parameters begins test.
Fill with a liquid nitrogen every 3.5h in the experimentation.Experiment is closed all power supplys after finishing.
Various prescription heat conductivilitys and mechanical property
Filler 1: 150 parts of terpolymer EP rubbers, anti-aging agent [6-oxyethyl group-2,2,4-trimethylammonium-1, the 2-dihyaroquinoline] 2 parts, 40 parts of carbon blacks, 1 part in sulphur, promotor [N, the two thiamides of N-tetramethyl-two sulphur] 1 part, 6 parts in softening agent [o-phthalic acid dibutyl ester], 40 parts of paraffin oils, organic active agent [PEG4000] 3-8 part, inorganic active agent [MgO, Al
2O
3, (high thermal conductivity) Si
3N
4, BN, AlN, (1 class nanometer) ZnO] each 1 part, 1 part of dispersion agent [triethyl hexyl phosphoric acid].
Filler 2: 160 parts of terpolymer EP rubbers, 2 parts in anti-aging agent [2-dihyaroquinoline], 50 parts of carbon blacks, 2 parts in sulphur, 2 parts of promotor [tetramethyl-thiuram disulfide], 7 parts in softening agent [DEDB], 50 parts of paraffin oils, 4 parts of organic active agent [PEG4000], inorganic active agent [MgO2 part, Al
2O
31 part, (nano particle) Si
3N
41 part, BN1 part, AlN1 part, (2 class nanometer) ZnO1 part, KAl (SO
4)
212H
2O1 part], 2 parts of dispersion agents [sodium lauryl sulphate].
Filler 3: 170 parts of terpolymer EP rubbers, 3 parts in anti-aging agent [2,2,4-trimethylammonium 1], 60 parts of carbon blacks, 3 parts in sulphur, 3 parts of promotor [thiram], 8 parts in softening agent [sebacic acid two (2-ethyl hexyl) ester], 60 parts of paraffin oils, organic active agent [PEG4000], 5 parts, inorganic active agent [MgO, Al
2O
3, BN, AlN, Al
2O
3-2SiO
2-2H
2O] each 2 parts, 3 parts of dispersion agents [methyl amyl alcohol].
Filler 4: 180 parts of terpolymer EP rubbers, 4 parts in anti-aging agent [N-phenyl-N`-cyclohexyl Ursol D], 70 parts of carbon blacks, 3 parts in sulphur, 3 parts of promotor [vulcanization accelerator TMTD], 9 parts in softening agent [butyl benzyl phthalate], 70 parts of paraffin oils, organic active agent [PEG4000], 6 parts, inorganic active agent [MgO, Al
2O
3, (nano particle) Si
3N
4, KAl (SO
4)
212H
2O, Al
2O
3-2SiO
2-2H
2O] each 2 parts, 4 parts of dispersion agents [derivatived cellulose].
Filler 5: 190 parts of terpolymer EP rubbers, 4 parts in anti-aging agent [N-phenyl-N`-cyclohexyl Ursol D], 80 parts of carbon blacks, 3 parts in sulphur, 3 parts of promotor [vulcanization accelerator TMTD], 10 parts in softening agent [butyl benzyl phthalate], 80 parts of paraffin oils, 7 parts of organic active agent [PEG4000], inorganic active agent [Al
2O
3, (high thermal conductivity) Si
3N
4, BN, AlN, (2 class nanometer) ZnO, KAl (SO
4)
212H
2O, Al
2O
3-2SiO
2-2H
2O] each 1 part, 4 parts of dispersion agents [polyacrylamide].
Filler 6: 200 parts of terpolymer EP rubbers, 4 parts in anti-aging agent [N-phenyl-N`-sec.-propyl-Ursol D], 80 parts of carbon blacks, 3 parts in sulphur, 3 parts of promotor [Vulcanization accelerator TMTD], 10 parts in softening agent [sebacic acid two (2-ethyl hexyl) ester], 80 parts of paraffin oils, 8 parts of organic active agent [PEG4000], inorganic active agent [MgO, Si
3N
4(nano particle), BN, AlN, (1 class nanometer) ZnO, KAl (SO
4)
212H
2O, Al
2O
3-2SiO
2-2H
2O] each 1.5 parts, 4 parts of dispersion agents [fatty acid polyglycol ester].
Filler 7: 200 parts of terpolymer EP rubbers, anti-aging agent [6-oxyethyl group-2,2,4-trimethylammonium-1,2-dihyaroquinoline; N-N`-phenylbenzene-Ursol D] each 2 parts, 60 parts of carbon blacks, 2 parts in sulphur, promotor [Vulcanization accelerator TMTD-II; Altax; Accelerant B Z] each 1 part, softening agent [Octyl adipate; Di-n-hexyl adipate; Butyl benzyl phthalate; Sebacic acid two (2-ethyl hexyl) ester] each 1 part, 40 parts of paraffin oils, 3 parts of organic active agent [PEG4000], inorganic active agent [MgO, Al
2O
3, Si
3N
4(nano particle), BN, AlN, (1 class nanometer) ZnO ,] each 2 parts, each 1 part of dispersion agent [triethyl hexyl phosphoric acid, sodium lauryl sulphate, methyl amyl alcohol].
Filler 8: 180 parts of terpolymer EP rubbers, anti-aging agent [2,2,4-trimethylammonium 1,2-dihydro quinoline polymer; N-phenyl-N`-sec.-propyl-Ursol D] each 1 part, 50 parts of carbon blacks, 2 parts in sulphur, promotor [promotor T tetramethyl-dithio thiuram; Vulcanization accelerator TMTD; ] each 1 part, softening agent [di-n-hexyl adipate; Butyl benzyl phthalate; Sebacic acid two (2-ethyl hexyl) ester] each 3 parts, 50 parts of paraffin oils, 6 parts of organic active agent [PEG4000], inorganic active agent [MgO, Al
2O
3, Si
3N
4(nano particle), BN, AlN, (2 class nanometer) ZnO, KAl (SO
4)
212H
2O, Al
2O
3-2SiO
2-2H
2O] each 1 part, each 1 part of dispersion agent [derivatived cellulose, polyacrylamide, guar gum, fatty acid polyglycol ester].
Filler 9: 170 parts of terpolymer EP rubbers, anti-aging agent [6-oxyethyl group-2,2,4-trimethylammonium-1,2-dihyaroquinoline; N-N`-phenylbenzene-Ursol D] each 1 part, 70 parts of carbon blacks, 3 parts in sulphur, promotor [promotor T; Vulcanization accelerator TMTD; Vulcanization accelerator TMTD-II; ] each 1 part, softening agent [di-n-hexyl adipate; Butyl benzyl phthalate] each 4 parts, 70 parts of paraffin oils, 4 parts of organic active agent [PEG4000], inorganic active agent [MgO, Al
2O
3, Si
3N
4(high thermal conductivity), BN, AlN, (1 class nanometer) ZnO, KAl (SO
4)
212H
2O, Al
2O
3-2SiO
2-2H
2O] each 1 part, each 1 part of dispersion agent [triethyl hexyl phosphoric acid, methyl amyl alcohol, polyacrylamide].
Filler 10: 160 parts of terpolymer EP rubbers, anti-aging agent [N-phenyl-N`-cyclohexyl Ursol D; N-phenyl-N`-sec.-propyl-Ursol D.N-N`-phenylbenzene-Ursol D] each 1 part, 40 parts of carbon blacks, 3 parts in sulphur, promotor [TMTD; Altax] each 1 part, softening agent [o-phthalic acid dibutyl ester; Octyl adipate; Butyl benzyl phthalate] each 3 parts, 80 parts of paraffin oils, 3 parts of organic active agent [PEG4000], inorganic active agent [MgO, Al
2O
3, Si
3N
4(nano particle), BN, AlN, ZnO ,] each 2 parts, each 1 part of dispersion agent [triethyl hexyl phosphoric acid, methyl amyl alcohol, derivatived cellulose, guar gum].
Filler 11: 200 parts of terpolymer EP rubbers, anti-aging agent [N-phenyl-α-aniline; The N-Phenyl beta naphthylamine; N-phenyl-N`-sec.-propyl-Ursol D] each 1 part, 40 parts of carbon blacks, 1 part in sulphur, promotor [Vulcanization accelerator TMTD; Promotor TT; Curing tetramethyl-TMTD] each 1 part, softening agent [butyl benzyl phthalate; Sebacic acid two (2-ethyl hexyl) ester] each 5 parts, 80 parts of paraffin oils, 4 parts of organic active agent [PEG4000], inorganic active agent [MgO, Al
2O
3, Si
3N
4(high thermal conductivity), BN, AlN, (2 class nanometer) ZnO, KAl (SO
4)
212H
2O, Al
2O
3-2SiO
2-2H
2O] each 1 part, 2 parts of dispersion agents [fatty acid polyglycol ester].
Filler 12: 150 parts of terpolymer EP rubbers, anti-aging agent [N-phenyl-N`-sec.-propyl-Ursol D; N-N`-phenylbenzene-Ursol D] each 1 part, 50 parts of carbon blacks, 2 parts in sulphur, promotor [promotor T; ] 2 parts, 9 parts in softening agent [sebacic acid two (2-ethyl hexyl) ester], 70 parts of paraffin oils, 6 parts of organic active agent [PEG4000], inorganic active agent [MgO, Si
3N
4(high thermal conductivity), AlN, (1 class nanometer) ZnO, Al
2O
3-2SiO
2-2H
2O] each 2 parts, each 1 part of dispersion agent [sodium lauryl sulphate, derivatived cellulose, fatty acid polyglycol ester].
High heat conducting nano compounded rubber of the present invention is that thermal conductivity can be up to the thermoplastic composite resin of 22.25 ~ 35.56w/mK.The technology of the present invention is utilized unique molecular designing, has improved the interaction force of molecule between thermoplastic elastomer and the filler, and filler high-level efficiency contact has each other formed the heat passage, has increased substantially thermal conductivity.
This intellecture property of primary enforcement that all are above-mentioned is not set restriction this product innovation of other forms of enforcement and/or novel method.Those skilled in the art will utilize this important information, and foregoing is revised, to realize similar implementation status.But all modifications or transformation belong to the right of reservation based on product innovation of the present invention.
The above only is preferred embodiment of the present invention, is not to be the restriction of invention being made other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not break away to any simple modification, equivalent variations and remodeling that above embodiment does, still belongs to the protection domain of technical solution of the present invention according to technical spirit of the present invention.
Claims (10)
1. a high heat conducting nano compounded rubber is characterized in that, its raw material comprises one or more in the following component: terpolymer EP rubber, anti-aging agent, carbon black, sulphur, promotor, softening agent, paraffin oil, organic active agent PEG4000, inorganic active agent, dispersion agent.
2. described high heat conducting nano compounded rubber according to claim 1 is characterized in that, described material content proportioning is by weight:
Terpolymer EP rubber 150-200 part,
Anti-aging agent 1-4 part,
Carbon black 40-80 part,
Sulphur 1-3 part,
Promotor 1-3 part,
Softening agent 6-10 part,
Paraffin oil 40-80 part,
Organic active agent PEG4000,3-8 part
Inorganic active agent 6-12 part,
Dispersion agent 1-4 part.
3. described high heat conducting nano compounded rubber according to claim 1 is characterized in that, described anti-aging agent is one or more in the following reagent: 6-oxyethyl group-2,2,4-trimethylammonium-1,2-dihyaroquinoline; 2,2,4-trimethylammonium 1,2-dihydro quinoline polymer; N-phenyl-α-aniline; The N-Phenyl beta naphthylamine; N-phenyl-N`-cyclohexyl Ursol D; N-phenyl-N`-sec.-propyl-Ursol D.N-N`-phenylbenzene-Ursol D.
4. described high heat conducting nano compounded rubber according to claim 1 is characterized in that, described promotor is one or more in the following reagent: promotor T; N, the two thiamides of N-tetramethyl-two sulphur; Tetramethyl-thiuram disulfide; Thiram; Vulcanization accelerator TMTD; Tetramethyl-dithio thiuram; Vulcanization accelerator TMTD; Vulcanization accelerator TMTD-II; Promotor TT; Curing two (thiocarbonyl group dimethylamine); Curing tetramethyl-TMTD; Tetramethyl-sulfo-peroxy dicarbonate diamide; Tetramethyl thiuram disulfide; TMTD; Altax; Accelerant B Z.
5. described high heat conducting nano compounded rubber according to claim 1 is characterized in that, described softening agent is one or more in the following reagent:: o-phthalic acid dibutyl ester; DEDB; Octyl adipate; Di-n-hexyl adipate; Butyl benzyl phthalate; Sebacic acid two (2-ethyl hexyl) ester.
6. described high heat conducting nano compounded rubber according to claim 1 is characterized in that, described promoting agent is PEG4000; Described dispersion agent is one or more in the following reagent: triethyl hexyl phosphoric acid, sodium lauryl sulphate, methyl amyl alcohol, derivatived cellulose, polyacrylamide, guar gum, fatty acid polyglycol ester.
7. described high heat conducting nano compounded rubber according to claim 1 is characterized in that, described inorganic active agent is one or more in the following reagent: MgO, Al
2O
3, Si
3N
4, BN, AlN, ZnO, KAl (SO
4)
212H
2O, Al
2O
3-2SiO
2-2H
2O.
8. described high heat conducting nano compounded rubber according to claim 7 is characterized in that, described AlN is: AlN whisker and AlN particle.
9. described high heat conducting nano compounded rubber according to claim 7 is characterized in that described Si
3N
4Be highly heat-conductive silicon nitride; Described BN is the nano silicon nitride boron particles, satisfies following index:
10. each described high heat conducting nano compounded rubber is characterized in that according to claim 1-9, described high heat conducting nano compounded rubber, and it prepares by following steps:
The first step, synthetic rubber: by Banbury mixer with described raw material synthetic rubber;
Second step, moulding: by mill with the synthetic rubber moulding;
In the 3rd step, sulfuration: moulding rubber is put into the mould of vulcanizer, the pressurization scope is 150-210kgf/ ㎝
2, being warmed up to 220-230 ℃, the time is 80-100 second, vulcanizes.
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| JP2021128940A (en) * | 2015-08-06 | 2021-09-02 | 国立大学法人豊橋技術科学大学 | Composite insulation sheet and manufacturing method of composite insulation sheet |
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| CN109180412B (en) * | 2018-09-29 | 2021-09-03 | 安徽昊源化工集团有限公司 | Chemical product production process optimization method |
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