CN103319898B - Micro-nano lamellar boron nitride/rubber composite material and preparation method thereof - Google Patents
Micro-nano lamellar boron nitride/rubber composite material and preparation method thereof Download PDFInfo
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- CN103319898B CN103319898B CN201310253733.1A CN201310253733A CN103319898B CN 103319898 B CN103319898 B CN 103319898B CN 201310253733 A CN201310253733 A CN 201310253733A CN 103319898 B CN103319898 B CN 103319898B
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 238
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- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 22
- 239000000725 suspension Substances 0.000 claims description 20
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 14
- 235000021355 Stearic acid Nutrition 0.000 claims description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 11
- 239000005864 Sulphur Substances 0.000 claims description 11
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 11
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 11
- 239000008117 stearic acid Substances 0.000 claims description 11
- 239000011787 zinc oxide Substances 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 9
- 239000013543 active substance Substances 0.000 claims description 9
- BQFCCCIRTOLPEF-UHFFFAOYSA-N chembl1976978 Chemical compound CC1=CC=CC=C1N=NC1=C(O)C=CC2=CC=CC=C12 BQFCCCIRTOLPEF-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- NRHMKIHPTBHXPF-TUJRSCDTSA-M sodium cholate Chemical compound [Na+].C([C@H]1C[C@H]2O)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC([O-])=O)C)[C@@]2(C)[C@@H](O)C1 NRHMKIHPTBHXPF-TUJRSCDTSA-M 0.000 claims description 9
- 235000011149 sulphuric acid Nutrition 0.000 claims description 9
- 239000001117 sulphuric acid Substances 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 7
- 238000000975 co-precipitation Methods 0.000 claims description 6
- 229920000126 latex Polymers 0.000 claims description 6
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- 238000005987 sulfurization reaction Methods 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 230000003712 anti-aging effect Effects 0.000 claims description 2
- 239000000839 emulsion Substances 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 238000011049 filling Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 2
- 230000017525 heat dissipation Effects 0.000 abstract 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 52
- 239000000523 sample Substances 0.000 description 34
- 239000011159 matrix material Substances 0.000 description 26
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- 238000000748 compression moulding Methods 0.000 description 18
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- 229920006173 natural rubber latex Polymers 0.000 description 10
- OWRCNXZUPFZXOS-UHFFFAOYSA-N 1,3-diphenylguanidine Chemical compound C=1C=CC=CC=1NC(=N)NC1=CC=CC=C1 OWRCNXZUPFZXOS-UHFFFAOYSA-N 0.000 description 9
- AFZSMODLJJCVPP-UHFFFAOYSA-N dibenzothiazol-2-yl disulfide Chemical compound C1=CC=C2SC(SSC=3SC4=CC=CC=C4N=3)=NC2=C1 AFZSMODLJJCVPP-UHFFFAOYSA-N 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 9
- ZRMMVODKVLXCBB-UHFFFAOYSA-N 1-n-cyclohexyl-4-n-phenylbenzene-1,4-diamine Chemical compound C1CCCCC1NC(C=C1)=CC=C1NC1=CC=CC=C1 ZRMMVODKVLXCBB-UHFFFAOYSA-N 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
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- 229920002449 FKM Polymers 0.000 description 5
- 244000043261 Hevea brasiliensis Species 0.000 description 5
- 229920000459 Nitrile rubber Polymers 0.000 description 5
- 229920013649 Paracril Polymers 0.000 description 5
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- 229920003048 styrene butadiene rubber Polymers 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
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- Processes Of Treating Macromolecular Substances (AREA)
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Abstract
The invention provides a micro-nano lamellar boron nitride/rubber composite material and a preparation method thereof. The preparation method comprises the following steps of: 1, placing a micrometer lamellar boron nitride raw material into a solvent, and ultrasonically stripping to prepare nanometer lamellar boron nitride; 2, mixing obtained nanometer lamellar boron nitride and the micrometer lamellar boron nitride raw material with rubber in proportion, adding a vulcanizing agent, and uniformly mixing to prepare a rubber compound; 3, vulcanizing the boron nitride/rubber rubber compound to obtain a high heat-conducting silicon rubber product. The micrometer lamellar boron nitride is difficult to aggregate and mainly plays a bridge overlapping role in the rubber, and the prepared boron nitride in a nanometer lamellar structure theoretically achieves the heat conductivity far more than that of common boron nitride. The boron nitride heat-conducting rubber prepared through the method provided by the invention has higher heat-conducting property under less filling parts and can be widely applied to positions which need heat dissipation and heat transfer in the fields of spaceflight, avigation, electron and electric appliances.
Description
Technical field
The present invention proposes a kind of preparation method and application of hexagonal nano lamella boron nitride, it mixes matrix material prepared by filled rubber matrix and possesses higher heat conductivility with micron boron nitride, can be widely used in for needing in space flight, aviation, electronics, appliance field to dispel the heat and the position of heat transfer.
Background technology
After twentieth century, the elastomeric material as the fourth-largest strategic resource enters the great development stage, compares the materials such as traditional metal, pottery, and elastomeric material has the features such as light weight, high visco-elasticity, resistance to chemical attack, easily machine-shaping, anti-fatigue performance be excellent.But elastomeric material mostly is the poor conductor of heat, its application on the product needing thermal conductivity good is restricted.
At present, the filler improving elastomeric material thermal conductivity mostly is metal, metal oxide, and it is nonmetal as graphite, carbon black etc., the matrix material made thus does not have good electrical insulation capability, or due to the filling number of filler larger, make other degradation of matrix material, product performance are undesirable.Hexagonal boron nitride (h-BN) is referred to as white graphite, belongs to III-V, hexagonal system, has the laminate structure of similar graphite.Its lattice parameter is a=0.2504nm, c=0.6652nm.In addition, the same with graphite, every one deck of h-BN forms plane hexagonal ring shape structure by B atom and atom N, and along C direction of principal axis, each layer atom presses ABAB ... mode arranges.The interlayer of h-BN combines by Van der Waals force, and the B atom in layer, the covalent bonds of atom N are together.Although the layer inner structure of h-BN is very stable, but easily slide between layers, peel off, the boron nitride of monolithic layer or several lamella can be peeled off into, in theory, the plane thermal rate of nm-class boron nitride sheet layer material can reach 2000W/mk, has exceeded the thermal conductivity of 300W/mk in common boron nitride plane far away.And, compared with traditional heat conductive filler, the characteristic that h-BN also has many excellences as anti-oxidant, high temperature resistant, thermal conductivity is high and chemical stability is high, the coefficient of expansion is low and frictional coefficient is low, processability is good, it has clear superiority improving in the mechanical behavior under high temperature of rubber-base composite material, thermostability, oxidation-resistance etc.
That the present invention relates to is a kind of preparation method of simple boron nitride/rubber composite newly, be by the large nanoscale twins boron nitride of flakiness ratio of preparation and micron lamella boron nitride blending dispersion in rubber matrix, the consumption of boron nitride filler can be reduced, form good heat conduction network, greatly improve the thermal conductivity of elastomeric material.
Summary of the invention
Object of the present invention: prepare the nanoscale twins boron nitride that flakiness ratio is large, and by its filled rubber material together with micron lamella boron nitride.Compared with conventional thermal conductive filler, select micron and nanoscale twins boron nitride mixed fillers, because micron lamella boron nitride is not easily reunited, a main bridge snap action in rubber matrix, and the boron nitride of obtained nano-lamellar structure has the thermal conductivity far exceeding common boron nitride, and there is larger flakiness ratio compared with micron lamella boron nitride, under identical filling number, more effective heat conduction network can be obtained, thus prepare the silicon rubber composite material of high heat conduction.The method with less heat conductive filler number, can improve the heat conductivility of elastomeric material.
The preparation method of a kind of micron and nanoscale twins boron nitride mixing filled rubber, it is characterized in that: rubber raw materials is dry glue or emulsion form, rubber weight number is 100 parts, and total boron nitride parts by weight are 50-100 part, and wherein the mass ratio of micron boron nitride and nm-class boron nitride is 1:9-9:1;
The dry glue of raw material choose:
Micron lamella boron nitride is placed in solvent orange 2 A, being made into concentration is 1mg/ml-6mg/ml suspension, the ultrasonic thickness that obtains is at below 10nm, flakiness ratio is the nanoscale twins boron nitride of 50-300, obtain rubber solutions with solvent orange 2 A dissolving rubber, micron lamella boron nitride, nanoscale twins boron nitride and rubber solutions are mixed; Then evaporating solvent A; Or pouring in solvent B, this solvent B is 5-15 times of solvent orange 2 A volume, dissolves each other with solvent orange 2 A, and not sol rubber and boron nitride, make rubber and boron nitride coprecipitation out; Again by mixing in mill, Banbury mixer or screw extrusion press, add the vulcanizing agent DCP of 1wt% wherein, obtained micro-nano lamella boron nitride/silicon rubber composite material after sulfuration;
Raw material choose latex:
Being placed in containing tensio-active agent Sodium cholic acid by micron lamella boron nitride is the deionized water of 0.05wt%-1wt%, being made into concentration is 1mg/ml-6mg/ml suspension, the ultrasonic thickness that obtains is at below 10nm, flakiness ratio is the nanoscale twins boron nitride of 50-300, after mixing with micron lamella boron nitride, rubber latex again, flocculate with the dilute sulphuric acid of 1wt%, dry, add in mixing roll at least comprise zinc oxide, stearic acid, promotor, anti-aging agent, sulphur Synergist S-421 95 evenly mixing, obtain Micro-nano lamellar boron nitride/rubber composite material after sulfuration.
Further, used solvent is alcohol, ketone, alkane or tetrahydrofuran (THF).
Further, ultrasonic power is 200-1500W, and ultrasonic time is 2-12h, and the flakiness ratio of the nanoscale twins boron nitride of acquisition is 50-250.
Further, the mass ratio of micron lamella boron nitride and prepared nanoscale twins boron nitride is 3:7-5:5.
Further, the mass ratio of micron lamella boron nitride and prepared nanoscale twins boron nitride is 3:7.
Micro-nano boron nitride/rubber composite prepared by the present invention can select different elastomeric materials to do matrix according to the difference of purposes.Goods can select different rubber matrixs according to the difference of environment for use (as temperature, pressure, the solvent etc. contacted).Film, sheet material, sheet material etc. are made according to using the difference needed.
Micro-nano lamellar boron nitride/rubber composite material prepared by the present invention may be used for the position needing in space flight, aviation, electronics, appliance field to dispel the heat and conduct heat, can reach and reduce thermal contact resistance between interface, and there is good processing characteristics, toughness and higher mechanical property, so that the requirement of minim gap between filling interface.
Accompanying drawing explanation
Fig. 1: the SEM of raw material six square piece layer boron nitride
Fig. 2: the TEM of nanoscale twins boron nitride
Fig. 3: it is 3.6nm that the AFM(of nm-class boron nitride characterizes thickness, and flakiness ratio is 287)
Fig. 4 a: the HR-TEM (embodiment 1) of micro-nano lamella boron nitride/silicon rubber composite material section; Fig. 4 b: the HR-TEM (embodiment 11) of micro-nano lamella boron nitride/native rubber composite material section
Below in conjunction with embodiment, effect of the present invention is described further.
Embodiment
Embodiment 1: 100 parts, silicon rubber, micron lamella boron nitride 1 part, nanoscale twins boron nitride 9 parts, prepares micro-nano lamella boron nitride/silicon rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 1g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 1000ml propanol solution, carry out ultrasonic with ultrasonic instrument, ultrasonic power 200W, ultrasonic time is 12h, obtains thickness at below 10nm, and flakiness ratio is the nanoscale twins boron nitride/propanol suspension between 50-300.
The preparation of matrix material: take 10g silicon rubber and join in 400ml propanol solution, heating in water bath 75 DEG C of stirring and dissolving.Join in the propanol solution of having dissolved silicon rubber together with taking 0.1g micron lamella boron nitride and containing the propanol solution of 0.9g nanoscale twins boron nitride and mix, after evaporating solvent, 0.1g vulcanizing agent (DCP) is added in mixing roll, evenly mixing, be positioned over again in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm
2, temperature is 150 DEG C, suppresses after 10 minutes, mould is taken out taking-up sample, obtains the heat-conducting silicon rubber finished product that micro-nano (mass ratio=1:9) boron nitride mass percent is 9.1wt%.
Embodiment 2: 100 parts, silicon rubber, micron lamella boron nitride 90 parts, nanoscale twins boron nitride 10 parts, prepares micro-nano lamella boron nitride/silicon rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 10g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 2500ml propanol solution, carry out ultrasonic with ultrasonic instrument, ultrasonic power 1000W, ultrasonic time is 3h, obtains thickness at below 10nm, and flakiness ratio is the nanoscale twins boron nitride/propanol suspension between 50-300.
The preparation of matrix material: take 10g silicon rubber and join in 400ml propanol solution, heating in water bath 75 DEG C of stirring and dissolving.Join in the propanol solution of having dissolved silicon rubber together with taking 9g micron lamella boron nitride and containing the propanol solution of 1g nanoscale twins boron nitride and mix, after evaporating solvent, 0.1g vulcanizing agent (DCP) is added in mixing roll, evenly mixing, be positioned over again in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm
2, temperature is 150 DEG C, suppresses after 10 minutes, mould is taken out taking-up sample, and obtaining micro-nano (mass ratio=9:1) boron nitride mass percent is 50wt% heat-conducting silicon rubber finished product.
Embodiment 3: 100 parts, silicon rubber, micron lamella boron nitride 20 parts, nanoscale twins boron nitride 80 parts, prepares micro-nano lamella boron nitride/silicon rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 10g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 2000ml acetone soln, carry out ultrasonic with ultrasound probe, ultrasonic power 1500W, ultrasonic time is 2h, obtains thickness at below 10nm, and flakiness ratio is the nanoscale twins boron nitride/acetone suspension between 50-300.
The preparation of matrix material: take 10g silicon rubber and join in 400ml acetone soln, heating in water bath 35 DEG C of stirring and dissolving.Join in the acetone soln having dissolved silicon rubber together with taking 2g micron lamella boron nitride and containing the acetone soln of 8g nanoscale twins boron nitride and mix, after evaporating solvent, 0.1g vulcanizing agent (DCP) is added in mixing roll, evenly mixing, be positioned over again in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm2, temperature is 150 DEG C, suppress after 10 minutes, mould is taken out taking-up sample, obtain the heat-conducting silicon rubber finished product that micro-nano (mass ratio=2:8) boron nitride mass percent is 50wt%.
Embodiment 4: 100 parts, silicon rubber, micron lamella boron nitride 40 parts, nanoscale twins boron nitride 60 parts, prepares micro-nano boron nitride/silicon rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 10g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 1800ml tetrahydrofuran solution, carry out ultrasonic with ultrasound probe, ultrasonic power 800W, ultrasonic time is 6h, obtains thickness at below 10nm, and flakiness ratio is the nanoscale twins boron nitride/tetrahydrofuran (THF) suspension between 50-300.
The preparation of matrix material: take 10g silicon rubber and join in 400ml tetrahydrofuran solution, heating in water bath 75 DEG C of stirring and dissolving.Join after mixing in the tetrahydrofuran solution having dissolved silicon rubber together with taking 4g micron lamella boron nitride and containing the tetrahydrofuran solution of 6g nanoscale twins boron nitride, mixture is poured in 8L water, at the uniform velocity stir, because tetrahydrofuran (THF) and water dissolve each other, and silicon rubber and boron nitride are all water insoluble, when the ratio of water is considerably beyond the ratio of tetrahydrofuran (THF), silicon rubber and boron nitride coprecipitation are out, obtain boron nitride/silicon rubber composite material, after to be dried, 0.1g vulcanizing agent (DCP) is added in mixing roll, evenly mixing, be positioned over again in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm
2, temperature is 150 DEG C, suppresses after 10 minutes, mould is taken out taking-up sample, obtains the heat-conducting silicon rubber finished product that micro-nano (mass ratio=4:6) boron nitride mass percent is 50wt%.
Embodiment 5: 100 parts, silicon rubber, micron lamella boron nitride 12 parts, nanoscale twins boron nitride nitrogen boron 28 parts, prepares micro-nano boron nitride/silicon rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 10g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 1800ml acetone soln, carry out ultrasonic with ultrasound probe, ultrasonic power 900W, ultrasonic time is 7h, obtains thickness at below 10nm, and flakiness ratio is the nanoscale twins boron nitride/acetone suspension between 50-300.
The preparation of matrix material: take 10g silicon rubber and join in 400ml acetone soln, heating in water bath 75 DEG C of stirring and dissolving.Join in the acetone soln having dissolved silicon rubber together with taking 1.2 microns of boron nitride and containing the acetone soln of 2.8g nm-class boron nitride and mix, mixture is poured in 8L water, at the uniform velocity stir, because acetone and water dissolve each other, and silicon rubber and boron nitride are all water insoluble, when the ratio of water is considerably beyond the ratio of acetone, silicon rubber and boron nitride coprecipitation are out, obtain boron nitride/silicon rubber composite material, after to be dried, 0.1g vulcanizing agent (DCP) is added in mixing roll, evenly mixing, be positioned over again in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm
2, temperature is 150 DEG C, suppresses after 10 minutes, mould is taken out taking-up sample, obtains the heat-conducting silicon rubber finished product that micro-nano (mass ratio=3:7) boron nitride mass percent is 28.6wt%.
Embodiment 6: 100 parts, silicon rubber, micron lamella 15 parts, nanoscale twins boron nitride 35 parts, prepares micro-nano boron nitride/silicon rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 10g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 1800ml acetone soln, carry out ultrasonic with ultrasound probe, ultrasonic power 1400W, ultrasonic time is 2.5h, obtains thickness at below 10nm, and flakiness ratio is the nanoscale twins boron nitride/acetone suspension between 50-300.
The preparation of matrix material: take 10g silicon rubber and join in 400ml acetone soln, heating in water bath 75 DEG C of stirring and dissolving.Join in the acetone soln having dissolved silicon rubber together with taking 1.5g micron lamella boron nitride and containing the acetone soln of 3.5g nanoscale twins boron nitride and mix, mixture is poured in 10L water, at the uniform velocity stir, because acetone and water dissolve each other, and silicon rubber and boron nitride are all water insoluble, when the ratio of water is considerably beyond the ratio of acetone, silicon rubber and boron nitride coprecipitation are out, obtain boron nitride/silicon rubber composite material, after to be dried, 0.1g vulcanizing agent (DCP) is added in mixing roll, evenly mixing, be positioned over again in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm
2, temperature is 150 DEG C, suppresses after 10 minutes, mould is taken out taking-up sample, obtains the heat-conducting silicon rubber finished product that micro-nano (mass ratio=3:7) boron nitride mass percent is 33.3wt%.
Embodiment 7: 100 parts, silicon rubber, micron lamella boron nitride 18 parts, nanoscale twins boron nitride 42 parts, prepares micro-nano boron nitride/silicon rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 10g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 1900ml propanol solution, carry out ultrasonic with ultrasound probe, ultrasonic power 1000W, ultrasonic time is 5h, obtains thickness at below 10nm, and flakiness ratio is the nanoscale twins boron nitride/propanol suspension between 50-300.
The preparation of matrix material: take 10g silicon rubber and join in 400ml propanol solution, heating in water bath 75 DEG C of stirring and dissolving.Join in the propanol solution of having dissolved silicon rubber together with taking 1.8g micron lamella boron nitride and containing the propanol solution of 4.2g nanoscale twins boron nitride and mix, after evaporating solvent, 0.1g vulcanizing agent (DCP) is added in mixing roll, evenly mixing, be positioned over again in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm
2, temperature is 150 DEG C, suppresses after 10 minutes, mould is taken out taking-up sample, obtains the heat-conducting silicon rubber finished product that micro-nano (mass ratio=3:7) boron nitride mass percent is 37.5wt%.
Embodiment 8: 100 parts, silicon rubber, micron lamella boron nitride 24 parts, nanoscale twins boron nitride 56 parts, prepares micro-nano boron nitride/silicon rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 10g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 1800ml propanol solution, carry out ultrasonic with ultrasound probe, ultrasonic power 1200W, ultrasonic time is 3h, obtains thickness at below 10nm, and flakiness ratio is the nanoscale twins boron nitride/propanol suspension between 50-300.
The preparation of matrix material: take 10g silicon rubber and join in 400ml propanol solution, heating in water bath 75 DEG C of stirring and dissolving.Join in the propanol solution of having dissolved silicon rubber together with taking 2.4g micron lamella boron nitride and containing the propanol solution of 5.6g nanoscale twins boron nitride and mix, after evaporating solvent, 0.1g vulcanizing agent (DCP) is added in mixing roll, evenly mixing, be positioned over again in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm
2, temperature is 150 DEG C, suppresses after 10 minutes, mould is taken out taking-up sample, obtains the heat-conducting silicon rubber finished product that micro-nano (mass ratio=3:7) boron nitride mass percent is 44.4wt%.
Embodiment 9: 100 parts, silicon rubber, micron lamella boron nitride 30 parts, nanoscale twins boron nitride 70 parts, prepares micro-nano boron nitride/silicon rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 10g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 1800ml acetone soln, carry out ultrasonic with ultrasound probe, ultrasonic power 600W, ultrasonic time is 10h, obtains thickness at below 10nm, and flakiness ratio is the nanoscale twins boron nitride/acetone suspension between 50-300.
The preparation of matrix material: take 10g silicon rubber and join in 400ml acetone soln, heating in water bath 75 DEG C of stirring and dissolving.Join in the acetone soln having dissolved silicon rubber together with taking 3g micron lamella boron nitride and containing the acetone soln of 7g nanoscale twins boron nitride and mix, mixture is poured in 10L water, at the uniform velocity stir, because acetone and water dissolve each other, and silicon rubber and boron nitride are all water insoluble, when the ratio of water is considerably beyond the ratio of acetone, silicon rubber and boron nitride coprecipitation are out, obtain boron nitride/silicon rubber composite material, after to be dried, 0.1g vulcanizing agent (DCP) is added in mixing roll, evenly mixing, be positioned over again in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm
2, temperature is 150 DEG C, suppresses after 10 minutes, mould is taken out taking-up sample, obtains the heat-conducting silicon rubber finished product that micro-nano (mass ratio=3:7) boron nitride per-cent is 50wt%.
Embodiment 10: natural rubber 100 parts, micron lamella boron nitride 4 parts, nanoscale twins boron nitride 36 parts, prepares micro-nano boron nitride/native rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 10g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 1800ml deionized water (containing 0.1wt% tensio-active agent Sodium cholic acid), carry out ultrasonic with ultrasound probe, ultrasonic power 1000W, ultrasonic time is 3h, obtains thickness at below 10nm, and flakiness ratio is the suspension of the nanoscale twins boron nitride/water between 50-300.
The preparation of matrix material: take 24.19g natural rubber latex (solid content 0.62, actual in natural gum 15g).By 0.6g micron lamella boron nitride with after mixing with natural rubber latex containing the aqueous solution of 5.4g nanoscale twins boron nitride, be poured into (dilute sulphuric acid of 1wt%) in flocculation agent, boron nitride/natural gum flocculates, put into baking oven and dry (60 DEG C), Synergist S-421 95 (5 parts, zinc oxide is added in mixing roll, stearic acid 2 parts, vulkacit D 0.5 part, altax 0.5 part, promotor TT0.1 part, antioxidant 4010 1 part, 2 parts, sulphur) place 24h afterwards, back mixing in mill again, be positioned in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm
2, temperature is 143 DEG C, suppresses after 7 minutes, mould is taken out taking-up sample, obtains the heat conduction natural gum finished product that micro-nano (mass ratio=1:9) boron nitride mass percent is 28.6wt%.
Embodiment 11: natural rubber 100 parts, micron lamella boron nitride 4 parts, nanoscale twins boron nitride 36 parts, prepares micro-nano boron nitride/native rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 10g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 1800ml deionized water (containing 0.1wt% tensio-active agent Sodium cholic acid), carry out ultrasonic with ultrasound probe, ultrasonic power 1000W, ultrasonic time is 3h, obtains thickness at below 10nm, and flakiness ratio is the suspension of the nanoscale twins boron nitride/water between 50-300.
The preparation of matrix material: take 24.19g natural rubber latex (solid content 0.62, actual in natural gum 15g).By 0.6g micron lamella boron nitride with after mixing with natural rubber latex containing the aqueous solution of 5.4g nanoscale twins boron nitride, be poured into (dilute sulphuric acid of 1wt%) in flocculation agent, micro-nano boron nitride/natural gum flocculates, put into baking oven and dry (60 DEG C), Synergist S-421 95 (5 parts, zinc oxide is added in mixing roll, stearic acid 2 parts, vulkacit D 0.5 part, altax 0.5 part, promotor TT0.1 part, antioxidant 4010 1 part, 2 parts, sulphur) place 24h afterwards, back mixing in mill again, be positioned in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm
2, temperature is 143 DEG C, suppresses after 7 minutes, mould is taken out taking-up sample, obtains the heat conduction natural gum finished product that micro-nano (mass ratio=1:9) boron nitride mass percent is 28.6wt%.
Embodiment 12: natural rubber 100 parts, micron lamella boron nitride 18 parts, nanoscale twins boron nitride 42 parts, prepares micro-nano boron nitride/native rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 10g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 1800ml deionized water (containing 0.05wt% tensio-active agent Sodium cholic acid), carry out ultrasonic with ultrasound probe, ultrasonic power 1500W, ultrasonic time is 2h, obtains thickness at below 10nm, and flakiness ratio is the suspension of the nanoscale twins boron nitride/water between 50-300.
The preparation of matrix material: take 24.19g natural rubber latex (solid content 0.62, actual in natural gum 15g).By 2.7g micron lamella boron nitride with after mixing with natural rubber latex containing the aqueous solution of 6.3g nanoscale twins boron nitride, be poured into (dilute sulphuric acid of 1wt%) in flocculation agent, micro-nano boron nitride/natural gum flocculates, put into baking oven and dry (60 DEG C), Synergist S-421 95 (5 parts, zinc oxide is added in mixing roll, stearic acid 2 parts, vulkacit D 0.5 part, altax 0.5 part, promotor TT0.1 part, antioxidant 4010 1 part, 2 parts, sulphur) place 24h afterwards, back mixing in mill again, be positioned in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm
2, temperature is 143 DEG C, suppresses after 7 minutes, mould is taken out taking-up sample, obtains the heat conduction natural gum finished product that micro-nano (mass ratio=3:7) boron nitride mass percent is 37.5wt%.
Embodiment 13: natural rubber 100 parts, micron lamella boron nitride 24 parts, nanoscale twins boron nitride 56 parts, prepares micro-nano boron nitride/native rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 20g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 3800ml deionized water (containing 0.5wt% tensio-active agent Sodium cholic acid), carry out ultrasonic with ultrasound probe, ultrasonic power 1200W, ultrasonic time is 2.5h, obtains thickness at below 10nm, and flakiness ratio is the suspension of the nanoscale twins boron nitride/water between 50-300.
The preparation of matrix material: take 16.12g natural rubber latex (solid content 0.62, actual in natural gum 10g).By 2.4g micron lamella boron nitride with after mixing with natural rubber latex containing the aqueous solution of 5.6g nanoscale twins boron nitride, be poured into (dilute sulphuric acid of 1wt%) in flocculation agent, micro-nano boron nitride/natural gum flocculates, put into baking oven and dry (60 DEG C), Synergist S-421 95 (5 parts of zinc oxide are added in mixing roll, 2 parts of stearic acid, 0.5 part of vulkacit D, 0.5 part of altax, 0.1 part of promotor TT, 1 part of antioxidant 4010, 2 parts of sulphur) place 24h afterwards, back mixing in mill again, be positioned in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm2, temperature is 143 DEG C, suppress after 7 minutes, mould is taken out taking-up sample, obtain the heat conduction natural gum finished product that micro-nano (mass ratio=3:7) boron nitride mass percent is 44.4wt%.
Embodiment 14: natural rubber 100 parts, micron lamella boron nitride 30 parts, nanoscale twins boron nitride 70 parts, prepares micro-nano boron nitride/native rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 20g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 4000ml deionized water (containing 0.1wt% tensio-active agent Sodium cholic acid), carry out ultrasonic with ultrasound probe, ultrasonic power 600W, ultrasonic time is 8h, obtains thickness at below 10nm, and flakiness ratio is the suspension of the nanoscale twins boron nitride/water between 50-300.
The preparation of matrix material: take 16.12g natural rubber latex (solid content 0.62, actual in natural gum 10g).By 3g micron lamella boron nitride with after mixing with natural rubber latex containing the aqueous solution of 7g nanoscale twins boron nitride, be poured into (dilute sulphuric acid of 1wt%) in flocculation agent, micro-nano boron nitride/natural gum flocculates, put into baking oven and dry (60 DEG C), Synergist S-421 95 (5 parts of zinc oxide are added in mixing roll, 2 parts of stearic acid, 0.5 part of vulkacit D, 0.5 part of altax, 0.1 part of promotor TT, 1 part of antioxidant 4010, 2 parts of sulphur) place 24h afterwards, instead in mill again to refine, be positioned in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm
2, temperature is 143 DEG C, suppresses after 7 minutes, mould is taken out taking-up sample, obtains the heat conduction natural gum finished product that micro-nano (mass ratio=3:7) boron nitride mass percent is 50wt%.
Embodiment 15: paracril 100 parts, micron lamella boron nitride 10 parts, nanoscale twins boron nitride 40 parts, prepares micro-nano boron nitride/nitile-butadiene rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 10g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 2000ml deionized water (containing 0.8wt% tensio-active agent Sodium cholic acid), carry out ultrasonic with ultrasound probe, ultrasonic power 1000W, ultrasonic time is 3.5h, obtains thickness at below 10nm, and flakiness ratio is the suspension of the nanoscale twins boron nitride/water between 50-300.
The preparation of matrix material: take 33.33g nitrile rubber (solid content 0.45, actual in paracril 15g).By 1.5g micron lamella boron nitride with after mixing with nitrile rubber containing the aqueous solution of 6g nanoscale twins boron nitride, be poured into (dilute sulphuric acid of 1wt%) in flocculation agent, micro-nano boron nitride/butadiene-acrylonitrile rubber flocculates, put into baking oven and dry (60 DEG C), Synergist S-421 95 (5 parts of zinc oxide are added in mixing roll, 2 parts of stearic acid, 0.5 part of vulkacit D, 0.5 part of altax, 0.1 part of promotor TT, 1 part of antioxidant 4010, 2 parts of sulphur) place 24h afterwards, back mixing in mill again, be positioned in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm
2, temperature is 170 DEG C, suppresses after 16 minutes, mould is taken out taking-up sample, obtains the heat conduction butadiene-acrylonitrile rubber finished product that micro-nano (mass ratio=2:8) boron nitride mass percent is 33.3wt%.
Embodiment 16: 100 parts, styrene-butadiene rubber(SBR), micron lamella boron nitride 7 parts, nanoscale twins boron nitride 63 parts, prepares micro-nano boron nitride/styrene-butadiene rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 10g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 2000ml deionized water (containing 1wt% tensio-active agent Sodium cholic acid), carry out ultrasonic with ultrasound probe, ultrasonic power 1000W, ultrasonic time is 3h, obtains thickness at below 10nm, and chi flakiness ratio is the suspension of the nanoscale twins boron nitride/water between 50-300.
The preparation of matrix material: take 52.63g styrene-butadiene latex (solid content 0.19, actual in styrene-butadiene rubber(SBR) 10g).By 0.7g micron lamella boron nitride with after mixing with styrene-butadiene latex containing the aqueous solution of 6.3g nanoscale twins boron nitride, be poured into (dilute sulphuric acid of 1wt%) in flocculation agent, micro-nano boron nitride/butadiene-styrene rubber flocculates, put into baking oven and dry (60 DEG C), Synergist S-421 95 (5 parts of zinc oxide are added in mixing roll, 2 parts of stearic acid, 0.5 part of vulkacit D, 0.5 part of altax, 0.1 part of promotor TT, 1 part of antioxidant 4010, 2 parts of sulphur) place 24h afterwards, instead in mill again to refine, be positioned in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm
2, temperature is 150 DEG C, suppresses after 17 minutes, mould is taken out taking-up sample, obtains the heat conduction butadiene-styrene rubber finished product that micro-nano (mass ratio=1:9) boron nitride mass percent is 41.2wt%.
Embodiment 17: viton 100 parts, micron lamella boron nitride 20 parts, nanoscale twins boron nitride 30 parts, prepares micro-nano boron nitride/viton matrix material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 10g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 2000ml propyl alcohol, carry out ultrasonic with ultrasound probe, ultrasonic power 1100W, ultrasonic time is 3.5h, obtains thickness at below 10nm after drying, and flakiness ratio is the nanoscale twins boron nitride between 50-300.
The preparation of matrix material: take 15g viton, 3g micron lamella boron nitride and 4.5g nanoscale twins boron nitride are mixed in mixing roll with viton, then 3 parts of MgO are added, 6 parts of gCa (OH) 2 and all kinds of Synergist S-421 95 (5 parts of zinc oxide, 2 parts of stearic acid, 0.5 part of vulkacit D, 0.5 part of altax, 0.1 part of promotor TT, 1 part of antioxidant 4010, 2 parts of sulphur), add 0.15g two-25 as linking agent, mix rear placement 24h, back mixing in mill again, be positioned in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm
2, temperature is 170 DEG C, suppresses after 10 minutes, mould is taken out taking-up sample, obtains the heat conduction viton finished product that micro-nano (mass ratio=4:6) boron nitride mass percent is 33.3wt%.
Embodiment 18: paracril 100 parts, micron lamella boron nitride 25 parts, nanoscale twins boron nitride 25 parts, prepares micro-nano boron nitride/nitile-butadiene rubber composite material.
First nanoscale twins boron nitride is prepared: (thickness is about 1.5 μm to take 10g feedstock boron nitride, lateral dimension is about 20 μm, flakiness ratio is about 13) in 2000ml propyl alcohol, carry out ultrasonic with ultrasound probe, ultrasonic power 1100W, ultrasonic time is 3.5h, obtains thickness at below 10nm after drying, and flakiness ratio is the nanoscale twins boron nitride between 50-300.
The preparation of matrix material: take 15g paracril, 3.75g micron lamella boron nitride and 3.75g nanoscale twins boron nitride are mixed in mixing roll with paracril, then Synergist S-421 95 (5 parts of zinc oxide, 2 parts of stearic acid, 0.5 part of vulkacit D, 0.5 part of altax, 0.1 part of promotor TT, 1 part of antioxidant 4010,2 parts of sulphur) is added, mix rear placement 24h, back mixing in mill again, be positioned in rubber mold, pressure exhaust in compression molding instrument, pressure is 100kg/cm
2, temperature is 170 DEG C, suppresses after 15 minutes, mould is taken out taking-up sample, obtains the heat conduction butadiene-acrylonitrile rubber finished product that micro-nano (mass ratio=5:5) boron nitride mass percent is 33.3wt%.
The performance data of embodiment is in table one.
Claims (4)
1. the preparation method of a micron and nanoscale twins boron nitride mixing filled rubber, it is characterized in that: rubber raw materials is dry glue or emulsion form, rubber weight number is 100 parts, total boron nitride parts by weight are 50-100 part, and wherein the mass ratio of micron boron nitride and nm-class boron nitride is 1:9-9:1;
The dry glue of raw material choose:
Micron lamella boron nitride is placed in solvent orange 2 A, being made into concentration is 1mg/ml-6mg/ml suspension, the ultrasonic thickness that obtains is at below 10nm, flakiness ratio is the nanoscale twins boron nitride of 50-300, obtain rubber solutions with solvent orange 2 A dissolving rubber, micron lamella boron nitride, nanoscale twins boron nitride and rubber solutions are mixed; Then evaporating solvent A; Or pouring in solvent B, this solvent B is 5-15 times of solvent orange 2 A volume, dissolves each other with solvent orange 2 A, and not sol rubber and boron nitride, make rubber and boron nitride coprecipitation out; Again by mixing in mill, Banbury mixer or screw extrusion press, add the vulcanizing agent DCP of 1wt% wherein, obtained micro-nano lamella boron nitride/silicon rubber composite material after sulfuration;
Raw material choose latex:
Being placed in containing tensio-active agent Sodium cholic acid by micron lamella boron nitride is the deionized water of 0.05wt%-1wt%, being made into concentration is 1mg/ml-6mg/ml suspension, the ultrasonic thickness that obtains is at below 10nm, flakiness ratio is the nanoscale twins boron nitride of 50-300, after mixing with micron lamella boron nitride, rubber latex again, flocculate with the dilute sulphuric acid of 1wt%, dry, add in mixing roll at least comprise zinc oxide, stearic acid, promotor, anti-aging agent, sulphur Synergist S-421 95 evenly mixing, obtain Micro-nano lamellar boron nitride/rubber composite material after sulfuration;
Used solvent orange 2 A or B are alcohol, ketone, alkane or tetrahydrofuran (THF).
2. the preparation method of micron according to claim 1 and nanoscale twins boron nitride mixing filled rubber, it is characterized in that: ultrasonic power is 200-1500W, ultrasonic time is 2-12h, and the flakiness ratio of the nanoscale twins boron nitride of acquisition is 50-250.
3. the preparation method of micron according to claim 1 and nanoscale twins boron nitride mixing filled rubber, is characterized in that: the mass ratio of micron lamella boron nitride and prepared nanoscale twins boron nitride is 3:7-5:5.
4. the preparation method of micron according to claim 3 and nanoscale twins boron nitride mixing filled rubber, is characterized in that: the mass ratio of micron lamella boron nitride and prepared nanoscale twins boron nitride is 3:7.
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