CN105038251A - Preparation method of heat conductive rubber composite - Google Patents
Preparation method of heat conductive rubber composite Download PDFInfo
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Abstract
The invention discloses a preparation method of heat conductive rubber composite. The method comprises the steps that carbon black is dissolved in an ethanol solution by weight, ultrasound is conducted at the temperature ranging from 25 DEG C to 35 DEG C, and packing is obtained after drying is conducted; the packing, polybutylene terephthalate, stainless steel staple fibers, silicone rubber raw rubber, iron oxide red, calcium stearate, polyvinyl butyral are put into a rubber mixing mill for mixing, and after the temperature is raised, mixing is conducted continuously; a vulcanizing agent is added, after vulcanization is conducted, heat preservation is conducted, and the heat conductive rubber composite is obtained after cooling is conducted. According to the preparation method of the heat conductive rubber composite, the prepared heat conductive rubber composite can improve heat conductivity, tensile strength and bending strength and has a better mechanical property.
Description
Technical field
The present invention relates to field of rubber technology, particularly a kind of preparation method of heat-conductivity rubber composite material.
Background technology
Along with industrial production and scientific and technical development, in the field such as heat transmission medium, friction materials of electronic devices and components, heat conductive rubber is good due to its thermal conductivity, has good market outlook.
But in process of production, due to factors such as duration of service are long, the friction between machine parts, the mechanical property of elastomeric material and heat conductivility reduce, and are not enough to meet service requirements, thus accelerate the aging of machine, add production cost.CN102504358A discloses a kind of high heat-conductivity rubber composite material and preparation method thereof.Its composition is counted by mass parts: rubber 100, zinc oxide 4 ~ 6, stearic acid 1 ~ 3, anti-aging agent 1 ~ 2, carbon black 40 ~ 60, promotor 1 ~ 1.5, sulphur 1 ~ 3, thermal conducting agent 50 ~ 170.Described making method comprises following processing step: added by rubber in mill, adds zinc oxide, stearic acid, anti-aging agent, promotor, carbon black, thermal conducting agent successively, finally add Sulfur after bag roller.After sizing material mixes, then thin-pass also plays each 5 times of triangle bag, clot, adjusts roll spacing to 1.5mm slice.Tablet is put into mould, sulfuration on vulcanizing press, curing time is 15 ~ 20 minutes, and curing temperature is 160 ~ 165 DEG C, sulfide stress 10 ~ 12Mpa.CN104693523A relates to a kind of preparation method of heat conductive rubber, belongs to rubber materials.The preparation method of heat conductive rubber of the present invention, the method comprises following processing step: I. by the vitriol oil, potassium permanganate and graphite by H
2sO
4: KMnO
4: C processes 30 ~ 150min under 3.5 ~ 4.5:0.2 ~ 0.8:1 room temperature; Mixture after process is dissolved in 0.5 ~ 2% phosphoric acid, mixes rear dry modified expanded graphite after adding Zinc oxide nanoparticle, modified expanded graphite is prepared rubber as raw material.The heat conductive rubber that aforesaid method prepares also exists the not high problem of physical strength.
Summary of the invention
The technical problem that the present invention solves provides a kind of preparation method of heat-conductivity rubber composite material, can improve the thermal conductivity of matrix material, tensile strength and flexural strength, have good mechanical property.
The technical solution used in the present invention is:
A preparation method for heat-conductivity rubber composite material, comprises the following steps:
(1) by weight, it is in the ethanolic soln of 10% that 1-11 part carbon black is dissolved in 20-80 part volumetric concentration, ultrasonic at 25-35 DEG C of temperature, obtains filler after drying;
(2) rubber mixing machine is placed in step (1) gained filler and 26-43 part polybutylene terephthalate, 12-18 part stainless steel short fiber, 42-65 part raw-silastic continuously, 2-8 part red iron oxide, 4-15 part calcium stearate, 9-17 part polyvinyl butyral acetal, mixing 0.8-1.5 hour at 120-160 DEG C, 170-210 DEG C is warming up in 1-3min, continue mixing 0.8-1.5 hour, obtain rubber unvulcanizate;
(3) add 12-22 part vulcanizing agent by step (2) gained rubber unvulcanizate, sulfuration 15-40min at 150-185 DEG C, insulation, after furnace cooling and get final product.
In above-mentioned steps (1), ultrasonic time is 25-35min.
Temperature dry in above-mentioned steps (1) is 30-35 DEG C.
In above-mentioned steps (2), stainless steel short fiber filament diameter is between 2-20 μm.
In above-mentioned steps (3), vulcanizing agent is the one in di-t-butyl peroxide, t-butylperoxyl benzoate, the different phenylpropyl alcohol of peroxidation two.
In above-mentioned steps (3), in sulfidation, pressure is 12.5-14MPa.
In above-mentioned steps (3), soaking time is 1-2h.
Modified organic silicone resin 3-5 part is also added in above-mentioned steps (3), the preparation method of described modified organic silicone resin is: get Union carbide A-162 60g, be added in 700g water, be hydrolyzed under the effect of hydrolyst formic acid 0.1g, the time of hydrolysis reaction is 1 hour, hydrolysis temperature 1 DEG C; After being hydrolyzed, heating up and carry out polyreaction, carry out underpressure distillation after reaction terminates, obtain silicone resin; M-phthalic acid 10g, neopentyl glycol 10g are mixed, heat up, under the protection of argon gas, carry out condensation reaction, the temperature of condensation reaction is 180 DEG C, and under the condition of termination reaction, the acid number of reaction system reaches 4KOHmg/g, obtains vibrin; Silicone resin, vibrin, titanate catalyst 0.4g, ethyl acetate 15g are mixed, under the protection of argon gas, heating carries out dehydration condensation, temperature of reaction 110 DEG C, in 1 hour reaction times, obtains modified organic silicone resin.
Beneficial effect: the heat conductivity that the present invention obtains is between 1.45-1.68W/m*K, tensile strength is between 105-132MPa, tensile strength is between 189-213MPa, due to the synergy between component, improve the thermal conductivity of matrix material, tensile strength and flexural strength, there is good mechanical property, to the control of temperature in preparation process, more can strengthen its performance.
Embodiment
Embodiment 1
A preparation method for heat-conductivity rubber composite material, comprises the following steps:
(1) by weight, it is in the ethanolic soln of 10% that 1 part of carbon black is dissolved in 20 parts of volumetric concentrations, and at 25 DEG C of temperature, ultrasonic 25min, obtains filler after drying, and wherein dry temperature is 30 DEG C;
(2) rubber mixing machine is placed in step (1) gained filler and 26 parts of polybutylene terephthalates, 12 parts of stainless steel short fibers (filament diameter is 2 μm), 42 parts of raw-silastic continuouslies, 2 parts of red iron oxides, 4 parts of calcium stearates, 9 parts of polyvinyl butyral acetals, at 120 DEG C mixing 0.8 hour, 170 DEG C are warming up in 1min, continue mixing 0.8 hour, obtain rubber unvulcanizate;
(3) add 12 parts of di-t-butyl peroxides by step (2) gained rubber unvulcanizate, sulfuration 15min at 150 DEG C, sulfide stress is 12.5MPa, and insulation 1h, after furnace cooling and get final product.
Embodiment 2
A preparation method for heat-conductivity rubber composite material, comprises the following steps:
(1) by weight, it is in the ethanolic soln of 10% that 11 parts of carbon blacks are dissolved in 80 parts of volumetric concentrations, and at 35 DEG C of temperature, ultrasonic 35min, obtains filler after drying, and wherein dry temperature is 35 DEG C;
(2) rubber mixing machine is placed in step (1) gained filler and 43 parts of polybutylene terephthalates, 18 parts of stainless steel short fibers (filament diameter is 20 μm), 65 parts of raw-silastic continuouslies, 8 parts of red iron oxides, 15 parts of calcium stearates, 17 parts of polyvinyl butyral acetals, at 160 DEG C mixing 1.5 hours, 210 DEG C are warming up in 3min, continue mixing 1.5 hours, obtain rubber unvulcanizate;
(3) add 22 parts of t-butylperoxyl benzoates by step (2) gained rubber unvulcanizate, sulfuration 40min at 185 DEG C, sulfide stress is 14MPa, and insulation 2h, after furnace cooling and get final product.
Embodiment 3
A preparation method for heat-conductivity rubber composite material, comprises the following steps:
(1) by weight, it is in the ethanolic soln of 10% that 3 parts of carbon blacks are dissolved in 22 parts of volumetric concentrations, and at 30 DEG C of temperature, ultrasonic 30min, obtains filler after drying, and wherein dry temperature is 32 DEG C;
(2) rubber mixing machine is placed in step (1) gained filler and 28 parts of polybutylene terephthalates, 13 parts of stainless steel short fibers (filament diameter is 5 μm), 47 parts of raw-silastic continuouslies, 3 parts of red iron oxides, 5 parts of calcium stearates, 11 parts of polyvinyl butyral acetals, at 130 DEG C mixing 1 hour, 180 DEG C are warming up in 1.5min, continue mixing 1 hour, obtain rubber unvulcanizate;
(3) will add 14 parts of different phenylpropyl alcohols of peroxidation two in step (2) gained rubber unvulcanizate, sulfuration 20min at 155 DEG C, sulfide stress is 13MPa, and insulation 1.2h, after furnace cooling and get final product.
Embodiment 4
A preparation method for heat-conductivity rubber composite material, comprises the following steps:
(1) by weight, it is in the ethanolic soln of 10% that 9 parts of carbon blacks are dissolved in 70 parts of volumetric concentrations, and at 30 DEG C of temperature, ultrasonic 30min, obtains filler after drying, and wherein dry temperature is 34 DEG C;
(2) rubber mixing machine is placed in step (1) gained filler and 41 parts of polybutylene terephthalates, 17 parts of stainless steel short fibers (filament diameter is 18 μm), 60 parts of raw-silastic continuouslies, 6 parts of red iron oxides, 12 parts of calcium stearates, 15 parts of polyvinyl butyral acetals, at 150 DEG C mixing 1.2 hours, 195 DEG C are warming up in 2.5min, continue mixing 1.2 hours, obtain rubber unvulcanizate;
(3) add 19 parts of t-butylperoxyl benzoates by step (2) gained rubber unvulcanizate, sulfuration 35min at 175 DEG C, sulfide stress is 13.5MPa, and insulation 1.5h, after furnace cooling and get final product.
Embodiment 5
A preparation method for heat-conductivity rubber composite material, comprises the following steps:
(1) by weight, it is in the ethanolic soln of 10% that 7 parts of carbon blacks are dissolved in 50 parts of volumetric concentrations, and at 30 DEG C of temperature, ultrasonic 30min, obtains filler after drying, and wherein dry temperature is 35 DEG C;
(2) rubber mixing machine is placed in step (1) gained filler and 37 parts of polybutylene terephthalates, 15 parts of stainless steel short fibers (filament diameter is 10 μm), 54 parts of raw-silastic continuouslies, 6 parts of red iron oxides, 12 parts of calcium stearates, 12 parts of polyvinyl butyral acetals, at 140 DEG C mixing 1 hour, 180 DEG C are warming up in 2min, continue mixing 1 hour, obtain rubber unvulcanizate;
(3) add 18 parts of di-t-butyl peroxides by step (2) gained rubber unvulcanizate, sulfuration 30min at 165 DEG C, sulfide stress is 13MPa, and insulation 1.5h, after furnace cooling and get final product.
Embodiment 6
Be with the difference of embodiment 5: in the 3rd step, also add modified organic silicone resin, the preparation method of described modified organic silicone resin is: get Union carbide A-162 60g, be added in 700g water, be hydrolyzed under the effect of hydrolyst formic acid 0.1g, the time of hydrolysis reaction is 1 hour, hydrolysis temperature 1 DEG C; After being hydrolyzed, heating up and carry out polyreaction, carry out underpressure distillation after reaction terminates, obtain silicone resin; M-phthalic acid 10g, neopentyl glycol 10g are mixed, heat up, under the protection of argon gas, carry out condensation reaction, the temperature of condensation reaction is 180 DEG C, and under the condition of termination reaction, the acid number of reaction system reaches 4KOHmg/g, obtains vibrin; Silicone resin, vibrin, titanate catalyst 0.4g, ethyl acetate 15g are mixed, under the protection of argon gas, heating carries out dehydration condensation, temperature of reaction 110 DEG C, in 1 hour reaction times, obtains modified organic silicone resin;
A preparation method for heat-conductivity rubber composite material, comprises the following steps:
(1) by weight, it is in the ethanolic soln of 10% that 7 parts of carbon blacks are dissolved in 50 parts of volumetric concentrations, and at 30 DEG C of temperature, ultrasonic 30min, obtains filler after drying, and wherein dry temperature is 35 DEG C;
(2) rubber mixing machine is placed in step (1) gained filler and 37 parts of polybutylene terephthalates, 15 parts of stainless steel short fibers (filament diameter is 10 μm), 54 parts of raw-silastic continuouslies, 6 parts of red iron oxides, 12 parts of calcium stearates, 12 parts of polyvinyl butyral acetals, at 140 DEG C mixing 1 hour, 180 DEG C are warming up in 2min, continue mixing 1 hour, obtain rubber unvulcanizate;
(3) will add 18 parts of di-t-butyl peroxides and 5 parts of modified organic silicone resins in step (2) gained rubber unvulcanizate, sulfuration 30min at 165 DEG C, sulfide stress is 13MPa, and insulation 1.5h, after furnace cooling and get final product.
Comparative example 1
That the silicone resin that do not add in the preparation process of modified organic silicone resin is without vibrin modification with the difference of embodiment 6, step is as follows: get Union carbide A-162 60g, be added in 700g water, be hydrolyzed under the effect of hydrolyst formic acid 0.1g, the time of hydrolysis reaction is 1 hour, hydrolysis temperature 1 DEG C; After being hydrolyzed, heating up and carry out polyreaction, carry out underpressure distillation after reaction terminates, obtain silicone resin.
A preparation method for heat-conductivity rubber composite material, comprises the following steps:
(1) by weight, it is in the ethanolic soln of 10% that 7 parts of carbon blacks are dissolved in 50 parts of volumetric concentrations, and at 30 DEG C of temperature, ultrasonic 30min, obtains filler after drying, and wherein dry temperature is 35 DEG C;
(2) rubber mixing machine is placed in step (1) gained filler and 37 parts of polybutylene terephthalates, 15 parts of stainless steel short fibers (filament diameter is 10 μm), 54 parts of raw-silastic continuouslies, 6 parts of red iron oxides, 12 parts of calcium stearates, 12 parts of polyvinyl butyral acetals, at 140 DEG C mixing 1 hour, 180 DEG C are warming up in 2min, continue mixing 1 hour, obtain rubber unvulcanizate;
(3) will add 18 parts of di-t-butyl peroxides and 5 parts of silicone resins in step (2) gained rubber unvulcanizate, sulfuration 30min at 165 DEG C, sulfide stress is 13MPa, and insulation 1.5h, after furnace cooling and get final product.
Comparative example 2
Do not add polyvinyl butyral acetal with the difference of embodiment 5.
A preparation method for heat-conductivity rubber composite material, comprises the following steps:
(1) by weight, it is in the ethanolic soln of 10% that 7 parts of carbon blacks are dissolved in 50 parts of volumetric concentrations, and at 30 DEG C of temperature, ultrasonic 30min, obtains filler after drying, and wherein dry temperature is 35 DEG C;
(2) rubber mixing machine is placed in step (1) gained filler and 37 parts of polybutylene terephthalates, 15 parts of stainless steel short fibers (filament diameter is 10 μm), 54 parts of raw-silastic continuouslies, 6 parts of red iron oxides, 12 parts of calcium stearates, at 140 DEG C mixing 1 hour, 180 DEG C are warming up in 2min, continue mixing 1 hour, obtain rubber unvulcanizate;
(3) add 18 parts of di-t-butyl peroxides by step (2) gained rubber unvulcanizate, sulfuration 30min at 165 DEG C, sulfide stress is 13MPa, and insulation 1.5h, after furnace cooling and get final product.
Performance test:
The material of embodiment 1-5 and comparative example 1-2 gained is carried out Performance Detection, and result is as following table:
As can be seen from the above table: the heat conductivity that embodiment 1-5 obtains is between 1.45-1.68W/m*K, and tensile strength is between 105-132MPa, and tensile strength is between 189-213MPa; By adding modified organic silicone resin in embodiment 6, the thermal conductivity of thermally conductive material effectively can be improved.Having there is decline relative to embodiment 6 tensile strength in the matrix material prepared in comparative example 1, which illustrates and adopt vibrin to carry out modification to silicone resin, effectively can improve the tensile strength of material; Do not add polyvinyl butyral acetal in comparative example 2, heat conductivity is 1.15W/m*K, and tensile strength is 72MPa, and flexural strength is 127MPa.It can thus be appreciated that, the matrix material that the present invention obtains be due to component between synergy, improve the thermal conductivity of matrix material, tensile strength and flexural strength, there is good mechanical property, to the control of temperature in preparation process, more can strengthen above-mentioned performance.
Claims (8)
1. a preparation method for heat-conductivity rubber composite material, is characterized in that, comprises the following steps:
(1) by weight, it is in the ethanolic soln of 10% that 1-11 part carbon black is dissolved in 20-80 part volumetric concentration, ultrasonic at 25-35 DEG C of temperature, obtains filler after drying;
(2) rubber mixing machine is placed in step (1) gained filler and 26-43 part polybutylene terephthalate, 12-18 part stainless steel short fiber, 42-65 part raw-silastic continuously, 2-8 part red iron oxide, 4-15 part calcium stearate, 9-17 part polyvinyl butyral acetal, mixing 0.8-1.5 hour at 120-160 DEG C, 170-210 DEG C is warming up in 1-3min, continue mixing 0.8-1.5 hour, obtain rubber unvulcanizate;
(3) add 12-22 part vulcanizing agent by step (2) gained rubber unvulcanizate, sulfuration 15-40min at 150-185 DEG C, insulation, after furnace cooling and get final product.
2. the preparation method of heat-conductivity rubber composite material according to claim 1, is characterized in that: in described step (1), ultrasonic time is 25-35min.
3. the preparation method of heat-conductivity rubber composite material according to claim 1, is characterized in that: temperature dry in described step (1) is 30-35 DEG C.
4. the preparation method of heat-conductivity rubber composite material according to claim 1, is characterized in that: in described step (2), stainless steel short fiber filament diameter is between 2-20 μm.
5. the preparation method of heat-conductivity rubber composite material according to claim 1, is characterized in that: in described step (3), vulcanizing agent is the one in di-t-butyl peroxide, t-butylperoxyl benzoate, the different phenylpropyl alcohol of peroxidation two.
6. the preparation method of heat-conductivity rubber composite material according to claim 1, is characterized in that: in described step (3), in sulfidation, pressure is 12.5-14MPa.
7. the preparation method of heat-conductivity rubber composite material according to claim 1, is characterized in that: in institute's above-mentioned steps (3), soaking time is 1-2h.
8. the preparation method of heat-conductivity rubber composite material according to claim 1, it is characterized in that: in above-mentioned steps (3), also add modified organic silicone resin 3-5 part, the preparation method of described modified organic silicone resin is: get Union carbide A-162 60g, be added in 700g water, be hydrolyzed under the effect of hydrolyst formic acid 0.1g, the time of hydrolysis reaction is 1 hour, hydrolysis temperature 1 DEG C; After being hydrolyzed, heating up and carry out polyreaction, carry out underpressure distillation after reaction terminates, obtain silicone resin; M-phthalic acid 10g, neopentyl glycol 10g are mixed, heat up, under the protection of argon gas, carry out condensation reaction, the temperature of condensation reaction is 180 DEG C, and under the condition of termination reaction, the acid number of reaction system reaches 4KOHmg/g, obtains vibrin; Silicone resin, vibrin, titanate catalyst 0.4g, ethyl acetate 15g are mixed, under the protection of argon gas, heating carries out dehydration condensation, temperature of reaction 110 DEG C, in 1 hour reaction times, obtains modified organic silicone resin.
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