CN102942895B - A kind of heat conductive electronic pouring sealant and preparation method thereof - Google Patents
A kind of heat conductive electronic pouring sealant and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to embedding adhesive area, in particular to a kind of low viscosity heat conductive electronic pouring sealant being applicable to various electronic devices and components and preparation method thereof, described heat conductive flame-retarding electron pouring sealant forms by by weight for the component A of 100:90 ~ 100:110 and B component, described component A comprises the raw material of following weight percent: heat conductive flame-retarding powder 39.20% ~ 79.60%, toning agent 0.80 ~ 2.00%, silane coupling agent 0.40 ~ 1.00%, liquid silicone oil 16.20% ~ 43.80%, silane crosslinker 3.00% ~ 14.50%; Described B component comprises the raw material of following weight percent: heat conductive flame-retarding powder 39.20% ~ 79.60%, liquid silicone oil 18.00% ~ 57.80%, silane coupling agent 0.20 ~ 1.00%, toning agent 1.00 ~ 1.96%, catalyzer 0.04% ~ 1.00%.Viscosity of the present invention is lower, and have excellent mobility, good heat conductivity, fire-retardant rank is high, can meet the embedding requirement in the gap being less than 0.2mm, easy construction; Cured strength is high, dust-proof, moistureproof, against shock performance is good, effectively can protect electronic devices and components, improves the work-ing life of electronic devices and components.
Description
Technical field
The present invention relates to embedding adhesive area, particularly a kind of low viscosity heat conductive electronic pouring sealant being applicable to various electronic devices and components and preparation method thereof.
Background technology
Organic silicon potting material has that operating temperature range is wide, high-low temperature resistant impact property excellent, solidification time do not absorb heat, heat release, do not shrink after solidification, electric property and chemical stability excellent, corrosion-resistant, good weatherability, the advantage of excellent thermal conductivity.As electronic encapsulation material, the effect of dust-proof, moistureproof, against shock, heat conduction can be played, improve the stability of electronic devices and components.Compared with traditional condensed type electron pouring sealant, add-on type electron pouring sealant has does not release the advantages such as low molecule by product, corrosion-free, crosslinking structure is easy to control, and vulcanizate shrinking percentage is little.There is simple process, quick, energy-efficient advantage in addition.Therefore, be the extremely rising used in electronic industry type material of generally acknowledging both at home and abroad.
And along with the development of electronic industry, electronic devices and components are tending towards densification and miniaturization, and the raising of its power it is also proposed higher requirement to the thermal conductivity of joint sealant and flame retardant resistance.In order to realize this requirement, need when preparing joint sealant to add a large amount of heat conduction and flame-retardant inorganic filler, due to filler and base glue poor compatibility, be easy to cause that the viscosity of joint sealant increases, intensity reduces, finally cause poor fluidity, intensity low, effectively cannot meet the embedding requirement of electronic devices and components.Application Ball-type packing can address this problem to a certain extent, but due to Ball-type packing expensive, finally cause the terminal price of product high, thus limit the Application Areas of joint sealant.
Summary of the invention
The present invention avoid adding expensive spherical or class Ball-type packing, viscosity lower, there is excellent mobility, low viscous heat conductive flame-retarding electron pouring sealant of a kind of low cost and preparation method thereof is provided.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: described heat conductive flame-retarding electron pouring sealant forms by by weight for the component A of 100:90 ~ 100:110 and B component,
Described component A comprises the raw material of following weight percent: heat conductive flame-retarding powder 39.20% ~ 79.60%, toning agent 0.80 ~ 2.00%, silane coupling agent 0.40 ~ 1.00%, liquid silicone oil 16.20% ~ 43.80%, silane crosslinker 3.00% ~ 14.50%;
Described B component comprises the raw material of following weight percent: heat conductive flame-retarding powder 39.20% ~ 79.60%, liquid silicone oil 18.00% ~ 57.80%, silane coupling agent 0.20 ~ 1.00%, toning agent 1.00 ~ 1.96%, catalyzer 0.04% ~ 1.00%.
The invention has the beneficial effects as follows: viscosity is lower to there is excellent mobility, the embedding requirement in the gap being less than 0.2mm can be met, easy construction.Cured strength is high, dust-proof, moistureproof, against shock performance is good, effectively can protect electronic devices and components.Good heat conductivity, is beneficial to the conduct heat away of electronic devices and components, effective work-ing life of improving electronic devices and components; Fire-retardant rank is high, ensure that the reliability of electronic devices and components.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described heat conductive flame-retarding powder is silicon oxide, aluminum oxide, a kind of or several arbitrarily mixture in aluminium nitride, boron nitride, silicon nitride, titanium oxide, aluminium hydroxide, magnesium hydroxide.The shape characteristic of described heat conductive flame-retarding powder is irregular aciculiform, threadiness, and regularity is lower.
Adopt the beneficial effect of above-mentioned further scheme to be, due to the shape characteristic of irregular powder, directly contact and to form the probability of thermal conducting path comparatively large, reduces thermal resistance, thus is conducive to the raising of thermal conductivity mutually.
Further, the particle diameter of described heat conductive flame-retarding powder is 0.10 ~ 60.00 μm.
Adopt the beneficial effect of above-mentioned further scheme to be, sized particles with the use of, effectively can improve thermal conductivity, and viscosity increases not obvious.
Further, described liquid silicone oil is the silicone oil that vinyl-terminated silicone fluid or side chain contain vinyl.
Adopt the beneficial effect of above-mentioned further scheme to be that the solidification of vinyl silicone oil belongs to addition curing, and solidification process is overflowed without small molecules, corrosion device surface can not be polluted; Heat resistance is good, can use within the scope of-50 DEG C ~ 260 DEG C.The silicone oil that vinyl-terminated silicone fluid and side chain contain vinyl is co-vulcanized, raising cross-linking density that can be suitable, thus reaches the object improving intensity.
Further, the silicon oil viscosity that described vinyl-terminated silicone fluid and/or side chain contain vinyl is 40 ~ 5000mPas, and described in ethene fiduciary point, the molar ratio of liquid silicone oil is 0.20% ~ 0.80%.
Adopt the beneficial effect of above-mentioned further scheme to be that the vinyl silicone oil of different viscosity, with the use of falling low viscous while, can form Concentrative crosslinking point, thus raising intensity, particularly tear strength can be greatly improved.
Further, in described silane crosslinker, the mass content of reactive hydrogen is 0.05% ~ 1.00%, and described silane crosslinker is terminal methyl hydrogen polysiloxanes or pending methyl group hydrogen polysiloxanes.
Adopting the beneficial effect of above-mentioned further scheme to be select low viscous low hydrogeneous methylhydrogenpolysi,oxane, can system viscosity be reduced, simultaneously by regulating the kind of crosslinking component and consumption, the intensity of product after sulfuration can be regulated.
Further, described catalyzer is highly active platinum catalyst, comprise in Platinic chloride isopropanol complex, Platinic chloride divinyl tetramethyl-silicone complex or Platinic chloride diethyl phthalate complex compound any one, in described catalyzer, the mass content of platinum is 1000 ~ 5000ppm.
Adopting the beneficial effect of above-mentioned further scheme to be, by adopting highly active platinum catalyst, can catalytic efficiency be improved, shortening curing time.
Further, described toning agent is any one in carbon black, barba hispanica or titanium dioxide.
The beneficial effect of above-mentioned further scheme is adopted to be to regulate the color of joint sealant as requested, with suitable with the colour match of embedding device.And can judge whether two components mix.
Further, described silane coupling agent be γ-aminopropyl triethoxysilane, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane any one or a few.
The beneficial effect of above-mentioned further scheme is adopted to be, silane coupling agent is utilized to carry out surface modification treatment to heat conductive flame-retarding powder, surface energy and the surface polarity of filler can be reduced, increase loading level, improve the degree of scatter of filler, while guaranteeing that the silica gel after sulfuration has good heat conductive flame-retarding performance, possesses good mobility and intensity.
The another technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of preparation method of heat conductive flame-retarding electron pouring sealant comprises the following steps:
1) heat conductive flame-retarding powder is placed in ball grinder, silane coupling agent (consumption is 0.20% ~ 1.00% of heat conductive flame-retarding powder weight) dehydrated alcohol is added in ball grinder after the dilution proportion for 1:20, after stirring, put into ball mill and carry out ball milling modification.Grind to take out after 2 hours and dry, then continue grinding and after 1 hour, obtain modified heat conductive flame-retarding powder.
2) vinyl silicone oil of system total mass number 16.20% ~ 43.80% will be accounted for, heat conductive flame-retarding powder through the system that the accounts for total mass mark 39.20% ~ 79.60% of ball milling modification adds (by weight ratio for the modified heat conductive flame-retarding powder described in 39.20:16.20 ~ 79.60:43.80 and liquid silicone oil add in kneader) in kneader successively, at 120-130 DEG C, vacuum kneading 2-4 hour, obtains base-material.
3) successively by a certain amount of base-material, silane crosslinker 3.00% ~ 14.50%, toning agent 0.80 ~ 2.00% adds in 5L double-planet dynamic mixing stirrer, rotational velocity is 200-2000 rev/min, revolution speed is 8-30 rev/min, mechanical stirring 2 ~ 3 hours obtained component A under the condition of vacuum tightness-0.08MP ~-0.1MPa;
4) successively by a certain amount of base-material, low-viscosity (mobile) liquid silicone oil 1.80% ~ 14.00%, catalyzer 0.04% ~ 1.00%, toning agent 1.00 ~ 1.96% adds in 5L double-planet dynamic mixing stirrer, rotational velocity is 200-2000 rev/min, revolution speed is 8-30 rev/min, mechanical stirring 2 ~ 3 hours obtained B component under the condition of vacuum tightness-0.08MP ~-0.1MPa;
5) when using, A, B component are mixed with the weight ratio of 100:90 ~ 100:110, self-vulcanizing 24 hours, namely described heat conductive flame-retarding electron pouring sealant.
Further, step 1) described in kneader be vacuum kneader.
Embodiment
Be described principle of the present invention and feature below, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
Be 10 μm of irregular silica powder 2560.00g successively by median size, median size is the irregular alumina powder jointed 6400.00g of 60 μm, median size is that the aluminium hydroxide powder 3840.00g of 20 μm is placed in container, add in heat conductive flame-retarding powder after 25.60g silane coupling agent γ-aminopropyl triethoxysilane 512.00g dehydrated alcohol is diluted, stir and be placed in ball grinder.Put into ball mill and carry out ball milling modification.Grind to take out after 2 hours and dry, then continue grinding and after 1 hour, obtain modified heat conductive flame-retarding powder.
Accurately take vinyl-terminated silicone fluid 2592.00g, modified heat conductive flame-retarding powder 12825.60g, adds in vacuum kneader successively, and at 120 ~ 130 DEG C, vacuum kneading 4 hours, obtains base-material.
Accurately take base-material 6156.80g, silane crosslinker terminal methyl hydrogen polysiloxanes 192.00g, carbon black 51.20g, add in 10L double-planet dynamic mixing stirrer, rotational velocity is 2000 revs/min, revolution speed is 30 revs/min, and under the condition of vacuum tightness-0.1MPa, mechanical stirring obtains component A in 3 hours;
Accurately take base-material 6156.80g, low viscosity vinyl-terminated silicone fluid 115.20g, catalyzer Platinic chloride isopropanol complex 2.56g, titanium dioxide 125.44g, add in 10L double-planet dynamic mixing stirrer, rotational velocity is 2000 revs/min, and revolution speed is 30 revs/min, and under the condition of vacuum tightness-0.1MPa, mechanical stirring obtains B component in 2 ~ 3 hours;
During use, A, B component are mixed with the weight ratio of 100:90 ~ 100:110, self-vulcanizing 24 hours, to obtain final product.
Wherein, the viscosity of described vinyl-terminated silicone fluid is 50mPas; Described silane crosslinker to be hydrogen content be 1.00% silicon oil of low hydrogen content terminal methyl hydrogen polysiloxanes; In described catalyzer, the concentration of platinum is 5000ppm.
Embodiment 2
Be 5 μm of irregular silica powder 2305.00g successively by median size, median size is the irregular silica powder 3455.00g of 13 μm, median size is that the magnesium hydrate powder 3840.00g of 40 μm is placed in container, by 48.00g silane coupling agent γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane 960.00g dehydrated alcohol dilution after add in heat conductive flame-retarding powder, stir and be placed in ball grinder.Put into ball mill and carry out ball milling modification.Grind to take out after 2 hours and dry, then continue grinding and after 1 hour, obtain modified heat conductive flame-retarding powder.
Accurately take vinyl silicone oil 4800.00g, modified heat conductive flame-retarding powder 9648.00g, adds in vacuum kneader successively, and at 120-130 DEG C, vacuum kneading 3 hours, obtains base-material.
Accurately take base-material 5760.00g, silane crosslinker pending methyl group hydrogen polysiloxanes 512.00g, carbon black 128.00g, add in 10L double-planet dynamic mixing stirrer, rotational velocity is 1500 revs/min, revolution speed is 28 revs/min, and under the condition of vacuum tightness-0.1MPa, mechanical stirring obtains component A in 3 hours;
Accurately take base-material 5760.00g, low viscosity side chain is containing vinyl silicone oil 499.20g, catalyzer Platinic chloride divinyl tetramethyl-silicone complex 32g, titanium dioxide 108.80g, add in 10L double-planet dynamic mixing stirrer, rotational velocity is 1500 revs/min, and revolution speed is 28 revs/min, and under the condition of vacuum tightness-0.1MPa, mechanical stirring obtains B component in 3 hours;
During use, A, B component are mixed with the weight ratio of 100:90 ~ 100:110, self-vulcanizing 24 hours, to obtain final product.
Wherein, described side chain is 200mPas containing the viscosity of vinyl silicone oil; Described silane crosslinker pending methyl group hydrogen polysiloxanes to be hydrogen content be 0.50% silicon oil of low hydrogen content; In described catalyzer Platinic chloride divinyl tetramethyl-silicone complex, the concentration of platinum is 3000ppm.
Embodiment 3
Be 2 μm of irregular silica powder 1920.00g successively by median size, median size is the irregular alumina powder jointed 3200.00g of 20 μm, median size is that the titanium oxide powder 1280.00g of 13 μm is placed in container, by 64.00g silane coupling agent γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane 1280.00g dehydrated alcohol dilution after add in heat conductive flame-retarding powder, stir and be placed in ball grinder.Put into ball mill and carry out ball milling modification.Grind to take out after 2 hours and dry, then continue grinding and after 1 hour, obtain modified heat conductive flame-retarding powder.
Accurately take vinyl-terminated silicone fluid 7040.00g, modified heat conductive flame-retarding powder 6464.00g, adds in vacuum kneader successively, and at 120-130 DEG C, vacuum kneading 3 hours, obtains base-material.
Accurately take base-material 5376.00g, silane crosslinker pending methyl group hydrogen polysiloxanes 928.00g, carbon black 96.00g, add in 10L double-planet dynamic mixing stirrer, rotational velocity is 1800 revs/min, revolution speed is 28 revs/min, and under the condition of vacuum tightness-0.1MPa, mechanical stirring obtains component A in 3 hours;
Accurately take base-material 5376.00g, low viscosity vinyl-terminated silicone fluid 896.00g, catalyzer Platinic chloride diethyl phthalate complex compound 64g, titanium dioxide 64.00g, add in 10L double-planet dynamic mixing stirrer, rotational velocity is 1800 revs/min, and revolution speed is 28 revs/min, and under the condition of vacuum tightness-0.1MPa, mechanical stirring obtains B component in 3 hours;
During use, A, B component are mixed with the weight ratio of 100:90 ~ 100:110, self-vulcanizing 24 hours, to obtain final product.
Wherein, the viscosity of described vinyl-terminated silicone fluid is 500mPas; Described silane crosslinker pending methyl group hydrogen polysiloxanes to be hydrogen content be 0.25% silicon oil of low hydrogen content; In described catalyzer Platinic chloride diethyl phthalate complex compound, the concentration of platinum is 1000ppm.
Comparative example 1
Accurately take following various raw material, viscosity is the vinyl silicone oil 2816.00g of 500mPas, silane crosslinker 928.00g, median size is 5 μm of aluminium hydroxide 512.00g, and median size is 50 μm of alumina powder jointed 1280.00g, median size is the silica powder 768.00g of 25 μm, carbon black 96.00g, adds in 10L double-planet dynamic mixing stirrer, mixing and stirring successively, obtain component A, packaging is placed stand-by; Viscosity is the vinyl silicone oil 2816.00g of 500mPas, concentration is 1000ppm platinum catalyst 64.00g, median size is 5 μm of aluminium hydroxide 512.00g, and median size is 50 μm of alumina powder jointed 1280.00g, and median size is the silica powder 768.00g of 25 μm, titanium dioxide 64.00g, viscosity is the vinyl silicone oil 896.00g of 200mPas, adds in 10L double-planet dynamic mixing stirrer successively, mixing and stirring, obtain B component, packaging is placed stand-by;
During use, by obtained component A and B component, mix with the weight proportion of 100:100, in 25 DEG C of solidifications 24 hours, carry out polyreaction.
Wherein, described silane crosslinker is the silicon oil of low hydrogen content of 0.25% reactive hydrogen content.
Comparative example 2
Accurately take following various raw material, viscosity is the vinyl silicone oil 1036.80g of 200mPas, silane crosslinker 192.00g, median size is the ball-aluminium oxide 1024.00g of 5 μm, and median size is the ball-aluminium oxide powder 2560.00g of 50 μm, median size is the aluminium hydroxide powder 1536.00g of 25 μm, carbon black 51.20g, adds in 10L double-planet dynamic mixing stirrer, mixing and stirring successively, obtain component A, packaging is placed stand-by; Accurately take following various raw material, viscosity is the vinyl silicone oil 1036.80g of 200mPas, viscosity is the vinyl silicone oil 115.20g of 40mPas, median size is the ball-aluminium oxide 1024.00g of 5 μm, median size is the ball-aluminium oxide powder 2560.00g of 50 μm, median size is the aluminium hydroxide powder 1536.00g of 25 μm, titanium dioxide 125.44g, concentration is that 1000ppm platinum catalyst 64.00g adds in 10L double-planet dynamic mixing stirrer successively, mixing and stirring, obtain component A, packaging is placed stand-by; During use, by obtained component A and B component, mix with the weight proportion of 100:100, in 25 DEG C of solidifications 24 hours, carry out polyreaction.
Wherein, described silane crosslinker is the silicon oil of low hydrogen content of 0.50% reactive hydrogen content.
Concrete test example
By the performance of the two-pack embedding of the present invention of experimental test below silica gel.
Testing method:
The A, the B component that contrast case and case study on implementation are mixed final vacuum deaeration, according to standard GB/T2794-1995 tested viscosity; A, B component mix final vacuum deaeration, are evenly coated on mould that thickness is 2mm, press the tensile strength of GB/T528-1998 test sample, elongation at break after solidification 72h; Thermal conductivity is tested according to ASTMD5470.
Acquired results tested by table one
From table, can find out, when filler number comparision contents height, thermal conductivity, the tensile strength of heat conduction joint sealant of the present invention and the joint sealant containing Ball-type packing are suitable with elongation at break, viscosity is slightly high, but because Ball-type packing is expensive, therefore heat conduction joint sealant cost performance of the present invention is higher.When filler number content is lower, heat conduction joint sealant of the present invention has the thermal conductivity of lower viscosity, better intensity and Geng Gao.Effectively can meet the embedding requirement of electronic devices and components.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. a heat conductive flame-retarding electron pouring sealant, is characterized in that, adopts and prepares with the following method:
Be 10 μm of irregular silica powder 2560.00g successively by median size, median size is the irregular alumina powder jointed 6400.00g of 60 μm, median size is that the aluminium hydroxide powder 3840.00g of 20 μm is placed in container, add in heat conductive flame-retarding powder after 25.60g silane coupling agent γ-aminopropyl triethoxysilane 512.00g dehydrated alcohol is diluted, stir and be placed in ball grinder, put into ball mill and carry out ball milling modification, grind after 2 hours and take out oven dry, continue grinding again and after 1 hour, obtain modified heat conductive flame-retarding powder
Accurately take vinyl-terminated silicone fluid 2592.00g, modified heat conductive flame-retarding powder 12825.60g, adds in vacuum kneader successively, and at 120 ~ 130 DEG C, vacuum kneading 4 hours, obtains base-material,
Accurately take base-material 6156.80g, silane crosslinker terminal methyl hydrogen polysiloxanes 192.00g, carbon black 51.20g, add in 10L double-planet dynamic mixing stirrer, rotational velocity is 2000 revs/min, revolution speed is 30 revs/min, and under the condition of vacuum tightness-0.1MPa, mechanical stirring obtains component A in 3 hours;
Accurately take base-material 6156.80g, low viscosity vinyl-terminated silicone fluid 115.20g, catalyzer Platinic chloride isopropanol complex 2.56g, titanium dioxide 125.44g, add in 10L double-planet dynamic mixing stirrer, rotational velocity is 2000 revs/min, and revolution speed is 30 revs/min, and under the condition of vacuum tightness-0.1MPa, mechanical stirring obtains B component in 2 ~ 3 hours;
During use, A, B component are mixed with the weight ratio of 100:90 ~ 100:110, self-vulcanizing 24 hours, to obtain final product,
Wherein, the viscosity of described vinyl-terminated silicone fluid is 50mPas; Described silane crosslinker to be hydrogen content be 1.00% silicon oil of low hydrogen content terminal methyl hydrogen polysiloxanes; In described catalyzer, the concentration of platinum is 5000ppm.
2. a heat conductive flame-retarding electron pouring sealant, is characterized in that, adopts and prepares with the following method:
Be 5 μm of irregular silica powder 2305.00g successively by median size, median size is the irregular silica powder 3455.00g of 13 μm, median size is that the magnesium hydrate powder 3840.00g of 40 μm is placed in container, by 48.00g silane coupling agent γ-(2, 3-epoxy third oxygen) propyl trimethoxy silicane 960.00g dehydrated alcohol dilution after add in heat conductive flame-retarding powder, stir and be placed in ball grinder, put into ball mill and carry out ball milling modification, grind after 2 hours and take out oven dry, continue grinding again and after 1 hour, obtain modified heat conductive flame-retarding powder,
Accurately take vinyl silicone oil 4800.00g, modified heat conductive flame-retarding powder 9648.00g, adds in vacuum kneader successively, and at 120-130 DEG C, vacuum kneading 3 hours, obtains base-material,
Accurately take base-material 5760.00g, silane crosslinker pending methyl group hydrogen polysiloxanes 512.00g, carbon black 128.00g, add in 10L double-planet dynamic mixing stirrer, rotational velocity is 1500 revs/min, revolution speed is 28 revs/min, and under the condition of vacuum tightness-0.1MPa, mechanical stirring obtains component A in 3 hours;
Accurately take base-material 5760.00g, low viscosity side chain is containing vinyl silicone oil 499.20g, catalyzer Platinic chloride divinyl tetramethyl-silicone complex 32g, titanium dioxide 108.80g, add in 10L double-planet dynamic mixing stirrer, rotational velocity is 1500 revs/min, and revolution speed is 28 revs/min, and under the condition of vacuum tightness-0.1MPa, mechanical stirring obtains B component in 3 hours;
During use, A, B component are mixed with the weight ratio of 100:90 ~ 100:110, self-vulcanizing 24 hours, to obtain final product,
Wherein, described side chain is 200mPas containing the viscosity of vinyl silicone oil; Described silane crosslinker pending methyl group hydrogen polysiloxanes to be hydrogen content be 0.50% silicon oil of low hydrogen content; In described catalyzer Platinic chloride divinyl tetramethyl-silicone complex, the concentration of platinum is 3000ppm.
3. a heat conductive flame-retarding electron pouring sealant, is characterized in that, adopts and prepares with the following method:
Be 2 μm of irregular silica powder 1920.00g successively by median size, median size is the irregular alumina powder jointed 3200.00g of 20 μm, median size is that the titanium oxide powder 1280.00g of 13 μm is placed in container, by 64.00g silane coupling agent γ-(2, 3-epoxy third oxygen) propyl trimethoxy silicane 1280.00g dehydrated alcohol dilution after add in heat conductive flame-retarding powder, stir and be placed in ball grinder, put into ball mill and carry out ball milling modification, grind after 2 hours and take out oven dry, continue grinding again and after 1 hour, obtain modified heat conductive flame-retarding powder,
Accurately take vinyl-terminated silicone fluid 7040.00g, modified heat conductive flame-retarding powder 6464.00g, adds in vacuum kneader successively, and at 120-130 DEG C, vacuum kneading 3 hours, obtains base-material,
Accurately take base-material 5376.00g, silane crosslinker pending methyl group hydrogen polysiloxanes 928.00g, carbon black 96.00g, add in 10L double-planet dynamic mixing stirrer, rotational velocity is 1800 revs/min, revolution speed is 28 revs/min, and under the condition of vacuum tightness-0.1MPa, mechanical stirring obtains component A in 3 hours;
Accurately take base-material 5376.00g, low viscosity vinyl-terminated silicone fluid 896.00g, catalyzer Platinic chloride diethyl phthalate complex compound 64g, titanium dioxide 64.00g, add in 10L double-planet dynamic mixing stirrer, rotational velocity is 1800 revs/min, and revolution speed is 28 revs/min, and under the condition of vacuum tightness-0.1MPa, mechanical stirring obtains B component in 3 hours;
During use, A, B component are mixed with the weight ratio of 100:90 ~ 100:110, self-vulcanizing 24 hours, to obtain final product,
Wherein, the viscosity of described vinyl-terminated silicone fluid is 500mPas; Described silane crosslinker pending methyl group hydrogen polysiloxanes to be hydrogen content be 0.25% silicon oil of low hydrogen content; In described catalyzer Platinic chloride diethyl phthalate complex compound, the concentration of platinum is 1000ppm.
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| CN115895277B (en) * | 2022-12-22 | 2023-10-20 | 广州市白云化工实业有限公司 | Pre-cured single-component heat-conducting gel and preparation method thereof |
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