CN111334049A - Method for preparing heat-conducting silicone rubber gasket from waste artificially-synthesized graphite film - Google Patents
Method for preparing heat-conducting silicone rubber gasket from waste artificially-synthesized graphite film Download PDFInfo
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Abstract
The invention provides a method for preparing a heat-conducting silicone rubber gasket by using a waste artificially synthesized graphite film, which comprises the following steps: (1) crushing and sieving the artificially synthesized graphite film to obtain artificially synthesized graphite powder; (2) grafting oxygen-containing groups on the surface of the artificially synthesized graphite powder to prepare surface activated graphite powder; (3) and uniformly mixing the surface activated graphite powder with reactive silicone oil, a filler, an inhibitor, a catalyst, a coupling agent and a vulcanizing agent, and then carrying out oriented extrusion molding and frozen slicing to obtain the heat-conducting silicone rubber gasket. The method for preparing the heat-conducting silicone rubber gasket by using the waste artificially-synthesized graphite film not only solves the problems of high recovery and treatment cost, easy generation of secondary pollution and the like of the existing waste artificially-synthesized graphite film material, but also develops the preparation of the heat-conducting silicone rubber gasket by using the waste artificially-synthesized graphite film as a raw material, so that the utilization value of waste materials is fully improved, and the method for preparing the heat-conducting silicone rubber gasket is simple and easy for industrial production.
Description
Technical Field
The invention relates to the technical field of preparation of heat-conducting silicone rubber gaskets, in particular to a method for preparing a heat-conducting silicone rubber gasket from a waste artificially synthesized graphite film.
Background
The artificially synthesized graphite film is a high-crystalline and high-thermal conductivity (thermal conductivity greater than 1500W/(m.K)) graphite film which is formed by taking a polyimide film as a raw material and carrying out processes such as carbonization, high-temperature graphitization, calendaring, die cutting and the like. The artificially synthesized graphite film provides excellent heat conduction and heat dissipation effects for various terminal electronic products, such as smart phones, notebook computers, tablet computers and the like. However, a large amount of graphite film scraps are generated during the processing processes such as calendaring, die cutting and the like. These wastes having high thermal conductivity are not easily combustible, are difficult to handle, and have high recycling costs. Therefore, the development of an environment-friendly and high-quality technology for recycling waste artificially-synthesized graphite films is still an urgent problem to be solved in the industry development. At present, the technology of recycling waste artificially synthesized graphite films and using the waste artificially synthesized graphite films in high-performance and high-added-value products is rarely reported at home and abroad.
On the other hand, with the gradual development of integration, miniaturization and high speed of various high-power devices, such as 5G base stations, LED displays, automotive LED lamps, etc., the heat generated by internal electronic components is also increasing. Generally, heat dissipation of a heating component is realized by filling an interface gap with a heat-conducting silicone rubber gasket and connecting the heat-conducting silicone rubber gasket with a radiator. The traditional heat-conducting silicone rubber gasket is obtained by adding ceramic heat-conducting filler into a silicone matrix, but the heat conductivity coefficient of the gasket (< 9W/(m.K)) is difficult to satisfy the heat conduction and heat dissipation of a high-power device. Therefore, the development of a novel high-thermal-conductivity and low-cost heat-conducting silicone rubber gasket is a difficult problem to be solved urgently in the industry of heat-conducting interface materials.
Therefore, it is necessary to provide a method for preparing a heat conductive silicone rubber gasket from waste synthetic graphite film to solve the above-mentioned drawbacks.
Disclosure of Invention
The invention aims to provide a method for preparing a heat-conducting silicone rubber gasket by using a waste artificially-synthesized graphite film, which not only solves the problems of high recovery and treatment cost, easy generation of secondary pollution and the like of the existing waste artificially-synthesized graphite film material, but also develops the preparation of the heat-conducting silicone rubber gasket by using the waste artificially-synthesized graphite film as a raw material, so that the utilization value of waste materials is fully improved, and the heat-conducting silicone rubber gasket is simple in manufacturing method and easy for industrial production.
In order to achieve the above object, the present invention provides a method for preparing a heat conductive silicone rubber gasket from a waste artificially synthesized graphite film, comprising the steps of:
(1) crushing and sieving the artificially synthesized graphite film to obtain artificially synthesized graphite powder;
(2) grafting oxygen-containing groups on the surface of the artificially synthesized graphite powder to prepare surface activated graphite powder;
(3) and uniformly mixing the surface activated graphite powder with reactive silicone oil, a filler, an inhibitor, a catalyst, a coupling agent and a vulcanizing agent, and then carrying out oriented extrusion molding and frozen slicing to obtain the heat-conducting silicone rubber gasket.
Further, in the step (2), the artificially synthesized graphite powder is subjected to heat treatment at 300-900 ℃ under the condition of containing oxygen, so that oxygen-containing groups are grafted on the surface of the artificially synthesized graphite powder. Wherein the oxygen-containing condition can be at least one of air, oxygen and ozone.
Further, in the step (2), the artificially synthesized graphite powder is immersed in at least one liquid of fuming sulfuric acid, nitric acid and hydrogen peroxide, so that oxygen-containing groups are grafted on the surface of the artificially synthesized graphite powder, and the artificially synthesized graphite powder is washed to be neutral by deionized water and then dried for later use.
Further, in the step (1), crushing is carried out by adopting a winnowing type crusher, the rotating speed is 1000-2500 rpm, the blade interval is 1-3 mm, and the cycle time is 3-10 times.
Further, in the step (1), the sieving is carried out by adopting a vibrating screen, and the vibrating screen is connected with a material outlet of the winnowing type pulverizer. Preferably, the mesh number of the vibrating screen is 60-2000 meshes.
Further, in the step (1), the particle size of the artificially synthesized graphite powder is 2-250 μm. The shape of the synthetic graphite powder can be, but is not limited to, one or more of a circle, a square, a regular polygon and an irregular polygon.
Further, in the step (3), the orientation extrusion molding is carried out by using a funnel-shaped screw extrusion device, and pressure is applied to enable the material to flow from a large-caliber position to a small-caliber position.
Further, in the step (3), the oriented extruded and molded heat-conducting silicone rubber is cured for a certain time at a certain temperature, so that a crosslinking reaction is generated inside the heat-conducting silicone rubber.
Further, the cured heat-conducting silicone rubber is hardened at low temperature, and frozen cutting is performed by adopting an ultrasonic knife along the direction perpendicular to the extrusion direction, so that frozen slicing is realized. The low temperature range can be-10 to-150 ℃, and the low temperature is realized by adopting a liquid nitrogen technology.
Further, the heat-conducting silicone rubber gasket comprises the following raw materials in parts by weight:
further, the reactive silicone oil is selected from vinyl silicone oil.
Further, the vulcanizing agent is selected from hydrogen-containing silicone oil vulcanizing agents.
Further, the filler may be selected from, but not limited to, one of alumina powder and carbon fiber.
Further, the inhibitor may be selected from, but not limited to, alkynols.
Further, the catalyst may be selected from, but is not limited to, platinum catalysts.
Further, the coupling agent may be selected from, but is not limited to, silane coupling agents.
Compared with the prior art, the method for preparing the heat-conducting silicone rubber gasket by using the waste artificially synthesized graphite film comprises the steps of crushing and sieving the waste artificially synthesized graphite film to obtain artificially synthesized graphite powder, grafting oxygen-containing groups on the surface of the artificially synthesized graphite powder to increase active sites, mixing the surface activated graphite powder with reactive silicone oil, a filler, an inhibitor, a catalyst, a coupling agent and a vulcanizing agent, extruding the mixture into a mold by using an oriented extrusion device, heating and curing, and performing freezing slicing along the direction perpendicular to the extrusion direction to obtain the heat-conducting silicone rubber gasket. The heat conduction coefficient of the heat conduction silicon rubber gasket is 9-40W/(m.K). Therefore, the method for preparing the heat-conducting silicone rubber gasket by using the waste artificially synthesized graphite film not only solves the problems of high recovery and treatment cost, easy generation of secondary pollution and the like of the existing waste artificially synthesized graphite film material, but also develops the preparation of the heat-conducting silicone rubber gasket by using the waste artificially synthesized graphite film as a raw material, fully improves the utilization value of waste materials, and is simple in manufacturing method and easy for industrial production.
Drawings
Fig. 1 is a flow chart of a manufacturing process of a thermally conductive silicone rubber gasket according to the present application.
Fig. 2 is an ultra-depth of field microscope image of the synthetic graphite powder of the present application.
Detailed Description
The technical solutions of the present invention are further illustrated by the following specific embodiments, but the present invention is not limited thereto.
Referring to fig. 1, a flow chart of a manufacturing process of a heat conductive silicone rubber gasket according to the present application includes:
s1: crushing and sieving the waste artificially synthesized graphite film to obtain artificially synthesized graphite powder;
s2: grafting oxygen-containing groups on the surface of the artificially synthesized graphite powder to prepare surface activated graphite powder;
s3: the surface activated graphite powder is uniformly mixed with reactive silicone oil, filler, inhibitor, catalyst, coupling agent and vulcanizing agent, and then is subjected to mixing, oriented extrusion molding and frozen slicing to obtain the heat-conducting silicone rubber gasket.
Example 1
(1) Putting 1kg of artificially synthesized graphite film into a winnowing type pulverizer for crushing, connecting a material outlet of the winnowing type pulverizer with a vibrating screen, setting the rotating speed to be 1000rpm, setting the blade spacing to be 1mm, and the cycle number to be 3 times, screening the material on the vibrating screen (the mesh number of the screen is 60 meshes) after discharging to obtain artificially synthesized graphite powder, wherein the particle size is 250 mu m, the shape is square and irregular polygon, and the super depth of field microscopic picture is shown in figure 2;
(2) placing the artificially synthesized graphite powder in a muffle furnace, introducing oxygen, heating to 300 ℃ for heat treatment, and grafting oxygen-containing groups on the surface of the powder to obtain surface activated graphite powder;
(3) mechanically stirring 850 parts of surface-activated graphite powder, 100 parts of vinyl silicone oil, 30 parts of carbon fiber, 0.02 part of inhibitor, 0.1 part of platinum catalyst, 0.1 part of silane coupling agent and 0.1 part of hydrogen-containing silicone oil vulcanizing agent for 20 minutes, and defoaming in vacuum for 20 minutes to obtain uniformly mixed slurry;
placing the mixed slurry in a funnel-shaped screw extrusion device, applying pressure to enable the materials to flow from a large-caliber position to a small-caliber position until the materials are extruded into a die, enabling the materials to be arranged along the extrusion direction in an oriented mode, and curing the materials for 20 minutes at 120 ℃;
and (3) hardening the cured heat-conducting silicone rubber at low temperature (liquid nitrogen), and performing freezing cutting along the direction vertical to the extrusion direction by using an ultrasonic knife to realize freezing slicing to obtain the heat-conducting silicone rubber gasket with the thickness of 1 mm.
The heat conductivity coefficient of the heat-conducting silicon rubber gasket is measured to be 40W/(m.K) by a thermal stability method, and the heat-conducting silicon rubber gasket has high heat conductivity and can meet the requirements of practical application.
Example 2
(1) Putting 1kg of artificially synthesized graphite film into a winnowing type pulverizer for crushing, connecting a material outlet of the winnowing type pulverizer with a vibrating screen, setting the rotating speed to be 1500rpm, the blade spacing to be 2mm, and the cycle number to be 5 times, and screening on the vibrating screen (the mesh number of the screen is 200 meshes) after discharging to obtain artificially synthesized graphite powder, wherein the particle size is 75 microns, and the shape is square or irregular polygon;
(2) placing the artificially synthesized graphite powder in a muffle furnace, introducing oxygen, heating to 500 ℃ for heat treatment, and grafting oxygen-containing groups on the surface of the powder to obtain surface activated graphite powder;
(3) mechanically stirring 750 parts of surface-activated graphite powder, 80 parts of vinyl silicone oil, 20 parts of alumina powder, 0.3 part of inhibitor, 0.3 part of platinum catalyst, 0.8 part of silane coupling agent and 0.6 part of hydrogen-containing silicone oil vulcanizing agent for 40 minutes, and defoaming in vacuum for 40 minutes to obtain uniformly mixed slurry;
placing the mixed slurry in a funnel-shaped screw extrusion device, applying pressure to enable the materials to flow from a large-caliber position to a small-caliber position until the materials are extruded into a die, enabling the materials to be arranged along the extrusion direction in an oriented mode, and curing the materials for 30 minutes at the temperature of 140 ℃;
and (3) hardening the cured heat-conducting silicone rubber at low temperature (liquid nitrogen), and performing freezing cutting along the direction vertical to the extrusion direction by using an ultrasonic knife to realize freezing slicing to obtain the heat-conducting silicone rubber gasket with the thickness of 1 mm.
The heat-conducting silicone rubber gasket has a heat conductivity coefficient of 25W/(m.K) measured by a thermal stability method, has high heat conductivity, and can meet the requirements of practical application.
Example 3
(1) Putting 1kg of artificially synthesized graphite film into a winnowing type pulverizer for crushing, connecting a material outlet of the winnowing type pulverizer with a vibrating screen, setting the rotating speed to be 2000rpm, setting the blade spacing to be 3mm, setting the cycle number to be 10 times, and screening the discharged material on the vibrating screen (the mesh number of the screen is 1200 meshes) to obtain artificially synthesized graphite powder, wherein the particle size is 15 mu m, and the shape is square or irregular polygon;
(2) dipping the artificially synthesized graphite powder in hydrogen peroxide to graft oxygen-containing groups on the surface of the artificially synthesized graphite powder, washing the artificially synthesized graphite powder to be neutral by using deionized water, and drying the artificially synthesized graphite powder for later use to prepare surface activated graphite powder;
(3) mechanically stirring 550 parts of surface activated graphite powder, 120 parts of vinyl silicone oil, 300 parts of alumina powder, 0.5 part of inhibitor, 0.4 part of platinum catalyst, 1.2 parts of silane coupling agent and 1.3 parts of hydrogen-containing silicone oil vulcanizing agent for 50 minutes, and defoaming in vacuum for 30 minutes to obtain uniformly mixed slurry;
placing the mixed slurry in a funnel-shaped screw extrusion device, applying pressure to enable the materials to flow from a large-caliber position to a small-caliber position until the materials are extruded into a die, enabling the materials to be arranged along the extrusion direction in an oriented mode, and curing the materials for 30 minutes at the temperature of 140 ℃;
and (3) hardening the cured heat-conducting silicone rubber at low temperature (liquid nitrogen), and performing freezing cutting along the direction vertical to the extrusion direction by using an ultrasonic knife to realize freezing slicing to obtain the heat-conducting silicone rubber gasket with the thickness of 1 mm.
The heat-conducting silicone rubber gasket has a heat conductivity coefficient of 18W/(m.K) measured by a thermal stability method, has high heat conductivity, and can meet the requirements of practical application.
Example 4
(1) Putting 1kg of artificially synthesized graphite film into a winnowing type pulverizer for crushing, connecting a material outlet of the winnowing type pulverizer with a vibrating screen, setting the rotating speed to be 2400rpm, setting the blade spacing to be 2mm, and setting the cycle number to be 6 times, and screening the materials on the vibrating screen (the mesh number of the screen is 1800 meshes) after discharging to obtain artificially synthesized graphite powder, wherein the particle size is 10 mu m, and the shape is circular or irregular polygon;
(2) dipping the artificially synthesized graphite powder in fuming sulfuric acid to graft oxygen-containing groups on the surface of the artificially synthesized graphite powder, washing the artificially synthesized graphite powder to be neutral by using deionized water, and drying the artificially synthesized graphite powder for later use to prepare surface activated graphite powder;
(3) mechanically stirring 600 parts of surface activated graphite powder with 100 parts of vinyl silicone oil, 400 parts of alumina powder, 0.3 part of inhibitor, 0.5 part of platinum catalyst, 1.5 parts of silane coupling agent and 1.3 parts of hydrogen-containing silicone oil vulcanizing agent for 50 minutes, and defoaming in vacuum for 30 minutes to obtain uniformly mixed slurry;
placing the mixed slurry in a funnel-shaped screw extrusion device, applying pressure to enable the materials to flow from a large-caliber position to a small-caliber position until the materials are extruded into a die, enabling the materials to be arranged along the extrusion direction in an oriented mode, and curing the materials for 30 minutes at the temperature of 140 ℃;
and (3) hardening the cured heat-conducting silicone rubber at low temperature (liquid nitrogen), and performing freezing cutting along the direction vertical to the extrusion direction by using an ultrasonic knife to realize freezing slicing to obtain the heat-conducting silicone rubber gasket with the thickness of 1 mm.
The heat-conducting silicone rubber gasket has a heat conductivity coefficient of 13W/(m.K) measured by a thermal stability method, has high heat conductivity, and can meet the requirements of practical application.
Example 5
Example 5 was prepared in substantially the same manner as example 4, except that in step (2):
step (2) in example 5: soaking the artificially synthesized graphite powder in hydrogen peroxide to graft oxygen-containing groups on the surface of the artificially synthesized graphite powder, washing the artificially synthesized graphite powder to be neutral by using deionized water, and drying the artificially synthesized graphite powder for later use to prepare the surface activated graphite powder.
And step (2) in example 4: dipping the artificially synthesized graphite powder in fuming sulfuric acid to graft oxygen-containing groups on the surface of the artificially synthesized graphite powder, washing the artificially synthesized graphite powder to be neutral by adopting deionized water, and drying the artificially synthesized graphite powder for later use to prepare the surface activated graphite powder.
The heat-conducting silicone rubber gasket has a heat conductivity coefficient of 19W/(m.K) measured by a thermal stability method, has high heat conductivity, and can meet the requirements of practical application.
Comparative example 1
(1) Putting 1kg of artificially synthesized graphite film into a winnowing type pulverizer for crushing, connecting a material outlet of the winnowing type pulverizer with a vibrating screen, setting the rotating speed to be 1000rpm, setting the blade interval to be 1mm, and the cycle number to be 3 times, and screening on the vibrating screen (the mesh number of the screen is 60 meshes) after discharging to obtain artificially synthesized graphite powder, wherein the particle size is 250 mu m, and the shape is square or irregular polygon;
(2) mechanically stirring 250 parts of artificially synthesized graphite powder with 100 parts of vinyl silicone oil, 30 parts of carbon fiber, 0.02 part of inhibitor, 0.1 part of platinum catalyst, 0.1 part of silane coupling agent and 0.1 part of hydrogen-containing silicone oil vulcanizing agent for 20 minutes, and defoaming in vacuum for 20 minutes to obtain uniformly mixed slurry;
placing the mixed slurry in a funnel-shaped screw extrusion device, applying pressure to enable the materials to flow from a large-caliber position to a small-caliber position until the materials are extruded into a die, enabling the materials to be arranged along the extrusion direction in an oriented mode, and curing the materials for 20 minutes at 120 ℃;
and (3) hardening the cured heat-conducting silicone rubber at low temperature (liquid nitrogen), and performing freezing cutting along the direction vertical to the extrusion direction by using an ultrasonic knife to realize freezing slicing to obtain the heat-conducting silicone rubber gasket with the thickness of 1 mm. The heat conductivity of the heat-conducting silicone rubber gasket is 5.3W/(m.K) measured by a thermal stability method. Therefore, the surface of the artificially synthesized graphite powder is grafted with the oxygen-containing group without the step (2), and the high-heat-conductivity silicone rubber gasket is difficult to obtain due to poor compatibility of the powder and the silicone rubber matrix.
It should be noted that the above-mentioned embodiments illustrate rather than limit the scope of the invention, and that those skilled in the art will be able to modify the invention in its various equivalent forms after reading the present invention and to fall within the scope of the invention as defined in the appended claims.
Claims (10)
1. A method for preparing a heat-conducting silicone rubber gasket by using a waste artificially synthesized graphite film is characterized by comprising the following steps:
(1) crushing and sieving the artificially synthesized graphite film to obtain artificially synthesized graphite powder;
(2) grafting oxygen-containing groups on the surface of the artificially synthesized graphite powder to prepare surface activated graphite powder;
(3) and uniformly mixing the surface activated graphite powder with reactive silicone oil, a filler, an inhibitor, a catalyst, a coupling agent and a vulcanizing agent, and then carrying out oriented extrusion molding and frozen slicing to obtain the heat-conducting silicone rubber gasket.
2. The method for preparing the heat-conducting silicone rubber gasket from the waste synthetic graphite film according to claim 1, wherein in the step (2), the synthetic graphite powder is subjected to heat treatment at 300-900 ℃ under the condition of containing oxygen, so that oxygen-containing groups are grafted on the surface of the synthetic graphite powder.
3. The method for preparing the heat-conducting silicone rubber gasket from the waste synthetic graphite film according to claim 1, wherein in the step (2), the synthetic graphite powder is immersed in at least one liquid of fuming sulfuric acid, nitric acid and hydrogen peroxide, so that oxygen-containing groups are grafted on the surface of the synthetic graphite powder, and the synthetic graphite powder is washed to be neutral by deionized water and then dried for later use.
4. The method for preparing a heat conductive silicone rubber gasket from the waste synthetic graphite film according to claim 1, wherein in the step (1), the crushing is performed by using an air separation type crusher at a rotation speed of 1000 to 2500rpm with a blade pitch of 1 to 3mm and a cycle number of 3 to 10.
5. The method for preparing the heat-conducting silicone rubber gasket from the waste artificially synthesized graphite film as claimed in claim 4, wherein the sieving is performed by using a vibrating screen, the vibrating screen is connected to a material outlet of the air separation type pulverizer, and the mesh number of the vibrating screen is 60-2000 meshes.
6. The method for preparing a heat conductive silicone rubber gasket using waste synthetic graphite film as claimed in claim 1, wherein in the step (3), the orientation extrusion molding is performed by using a funnel-shaped screw extrusion device, and the material is forced to flow from the large diameter portion to the small diameter portion.
7. The method of preparing the heat conductive silicone rubber gasket using the waste synthetic graphite film as claimed in claim 6, wherein in the step (3), the oriented extruded heat conductive silicone rubber is cured at a certain temperature for a certain time.
8. The method of preparing the heat conductive silicone rubber gasket using the waste synthetic graphite film as set forth in claim 7, wherein the cured heat conductive silicone rubber is hardened at a low temperature, and is subjected to the freezing cutting in a direction perpendicular to the extrusion direction using an ultrasonic blade to realize the freezing slicing.
9. The method for preparing a heat conductive silicone rubber gasket from waste synthetic graphite film according to claim 1, wherein said reactive silicone oil is selected from vinyl silicone oil.
10. The method for producing a heat conductive silicone rubber gasket from waste synthetic graphite film according to claim 1, wherein said vulcanizing agent is selected from hydrogen-containing silicone oil vulcanizing agents.
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