CN114410118A - Preparation method of insulating compound heat-conducting powder filled silicone resin with ultralow thermal resistance - Google Patents
Preparation method of insulating compound heat-conducting powder filled silicone resin with ultralow thermal resistance Download PDFInfo
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- CN114410118A CN114410118A CN202210095016.XA CN202210095016A CN114410118A CN 114410118 A CN114410118 A CN 114410118A CN 202210095016 A CN202210095016 A CN 202210095016A CN 114410118 A CN114410118 A CN 114410118A
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K3/22—Oxides; Hydroxides of metals
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Abstract
The application relates to the technical field of preparation of heat-conducting silicone resin, and particularly discloses a preparation method of insulating compound heat-conducting powder filled silicone resin with ultralow thermal resistance. The method comprises the following steps: grinding and sieving 150-200 parts of heat-conducting powder, adding a surfactant, vibrating, standing, precipitating and drying to obtain modified heat-conducting powder; stirring and mixing vinyl silicone resin and hydroxyl silicone resin, adding a cross-linking agent, stirring, and taking out to obtain a silicone resin base material; adding a thickening agent, a platinum catalyst and an enhancer into a silicone base material, and stirring to obtain a silicone mixture; stirring and mixing the modified heat-conducting powder, the insulating filler and sodium chloride, placing the mixture in a ball mill for ball milling, washing, filtering and drying to obtain a powder mixture; and stirring and mixing the powder mixture and the silicon resin mixture, taking out and cooling to room temperature to obtain the heat-conducting silicon resin. This application can improve heat conduction silicone grease when long-term the use, the heat conduction material and silicone resin's the compactness of being connected to make heat conduction silicone grease keep the low thermal resistance state when long-term the use.
Description
Technical Field
The application relates to the technical field of preparation of heat-conducting silicone resin, in particular to a preparation method of insulating compound heat-conducting powder filled silicone resin with ultralow thermal resistance.
Background
The heat-conducting interface material is widely applied to the fields of electronics and new energy automobile power batteries, and is commonly provided with four types of heat-conducting structure adhesives, heat-conducting gaskets, heat-conducting silicone grease and heat-conducting silicone gel grease. The adhesive of the heat-conducting structure has over-high bonding strength and is not easy to disassemble and repair; the heat-conducting gasket can not achieve good filling effect in a complex structure, and has high interface heat resistance and low heat-conducting efficiency when applied.
When the heat conduction silicone grease is prepared, the heat conduction materials and the silicone resin are mixed, stirring is carried out to enable the heat conduction materials to be dispersed in the silicone resin, the silicone resin plays a role in supporting and wrapping the heat conduction materials, the heat conduction materials are uniformly distributed in the silicone resin and are mutually connected, so that a heat conduction network is formed, however, if the heat conduction materials and the silicone resin are not tightly combined, the heat conduction materials can be gradually separated in the silicone resin when the heat conduction silicone grease is used for a long time, and the overall heat resistance of the heat conduction silicone grease is improved.
Disclosure of Invention
In order to improve the connection tightness of the heat conduction silicone grease and the silicone resin when the heat conduction silicone grease is used for a long time, so that the heat conduction silicone grease is kept in a low-thermal-resistance state when the heat conduction silicone grease is used for a long time, the application provides a preparation method of the insulation compound heat conduction powder filled silicone resin with ultralow thermal resistance.
The application provides a preparation method of insulating compound heat-conducting powder filled silicone resin with ultralow thermal resistance, which adopts the following technical scheme:
a preparation method of insulating compound heat-conducting powder filled silicone resin with ultra-low thermal resistance comprises the following steps:
placing 150-200 parts by weight of heat-conducting powder in an environment of 130-150 ℃ and grinding the powder through a 300-mesh screen, adding the powder into an ethanol solution, performing ultrasonic oscillation to enable the solution to become turbid liquid, adding 15-20 parts by weight of surfactant, continuing oscillation for 30min, standing, precipitating and drying to obtain modified heat-conducting powder;
stirring and mixing 25-30 parts by weight of vinyl silicone resin and 15-20 parts by weight of hydroxyl silicone resin, adjusting to an acidic environment, adding a cross-linking agent, stirring at 70-80 ℃ for 1h, and taking out to obtain a silicone resin base material; adding 3-5 parts of thickening agent, 1-3 parts of platinum catalyst and 1-2 parts of reinforcing agent into a silicone base material, adjusting to a weak acid environment, and stirring for 0.5h at 80-90 ℃ to obtain a silicone mixture;
according to parts by weight, stirring and mixing modified heat-conducting powder, 10-15 parts of insulating filler and 1-2 parts of sodium chloride, placing the mixture into a ball mill for ball milling until the mixture passes through a 500-mesh screen, and then washing, filtering and drying the mixture to obtain a powder mixture; and stirring and mixing the powder mixture and the silicon resin mixture at the rotating speed of 200-250r/min, and taking out and cooling to room temperature to obtain the heat-conducting silicon resin.
By adopting the technical scheme, after the heat conduction powder is ground in a high-temperature environment, the particle size of the heat conduction powder is more uniform and is convenient to disperse, the heat conduction powder can be activated in the high-temperature environment, the heat conduction powder is added into an ethanol solution, impurities on the surface of the heat conduction powder can be cleaned, and meanwhile, the heat conduction powder is ultrasonically vibrated in the ethanol solution, so that the heat conduction powder is uniformly dispersed in the ethanol solution, and after the surfactant is added, the contact area and the contact efficiency of the surfactant and the heat conduction powder can be improved; after stirring and mixing vinyl silicon resin and carboxyl silicon resin, premixing the vinyl silicon resin and the carboxyl silicon resin, and adding a cross-linking agent in an acidic environment high-temperature environment to improve the cross-linking activity of the cross-linking agent, so that the cross-linking agent has a cross-linking effect on the vinyl silicon resin and the carboxyl silicon resin, and long-chain vinyl silicon resin and carboxyl silicon resin form a net-shaped structure; after a thickening agent, a platinum catalyst and an enhancer are added into the silicone base material, stirring and mixing are carried out, so that various index parameters of the silicone resin can be enhanced; ball-milling and sieving the modified heat-conducting powder, the insulating filler and the sodium chloride to uniformly mix the three particles, and then stirring and mixing the powder mixture and the silicone resin mixture to obtain the heat-conducting silicone resin; after the sodium chloride is added into the heat-conducting silicone resin, the heat-conducting capacity of the silicone resin can be improved, and the thermal resistance is reduced.
Preferably, by weight, 25-30 parts of vinyl silicone resin, 15-20 parts of hydroxyl silicone resin and 5-10 parts of polyurethane acrylic resin are stirred and mixed, the mixture is adjusted to an acidic environment, a cross-linking agent is added, the mixture is stirred for 1 hour at 70-80 ℃, and then the mixture is taken out to obtain the silicone resin base material.
Preferably, the powder mixture and 2-3 parts of Irgacure-184 are stirred and mixed according to the parts by weight to obtain a secondary mixture, the secondary mixture and the silicone resin mixture are stirred and mixed in a dark environment at the rotating speed of 200-250r/min, and then the mixture is placed into a mold to be irradiated by ultraviolet light, and the heat-conducting silicone resin is obtained through calendaring molding.
Preferably, overlapping and feeding the 1/N amount of silicone resin mixture and the 1/M amount of powder mixture until the feeding is finished, standing and settling for 20min, stirring and mixing at the rotating speed of 200-250r/min, taking out and cooling to room temperature to obtain the heat-conducting silicone resin; wherein M and N are any natural number between 1 and 10, and M and N are independent of each other.
Through adopting above-mentioned technical scheme, throw the material with silicone resin mixture and powder mixture with above-mentioned mode, can be at the settlement in-process for the powder mixture is along with the action of gravity, carries out preliminary dispersion in the silicone resin mixture, thereby improves the dispersion homogeneity to the powder mixture in the silicone resin mixture.
Preferably, the heat conducting powder is spherical aluminum hydroxide.
Preferably, the surfactant is a silane coupling agent.
Preferably, the thickener is inorganic bentonite.
Preferably, the reinforcing agent is fumed silica.
Preferably, the insulating filler is silica.
In summary, the present application has the following beneficial effects: overlapping and feeding 1/N amount of silicone resin mixture and 1/M amount of powder mixture until the feeding is finished, standing and settling for 20min, stirring and mixing at the rotating speed of 200-250r/min, taking out and cooling to room temperature to obtain heat-conducting silicone resin; the silicone resin mixture and the powder mixture are fed in the above mode, so that the powder mixture can be preliminarily dispersed in the silicone resin mixture along with the action of gravity in the sedimentation process, and the dispersion uniformity of the powder mixture in the silicone resin mixture is improved.
Drawings
FIG. 1 is a schematic diagram of the overlapping feeding of silicone compound and secondary compound in example 6 of the present application.
Description of reference numerals: 1. a silicone resin mixture; 2. and (5) mixing the materials for the second time.
Detailed Description
The present application is described in further detail below with reference to examples 1 to 6 and comparative example 1.
Examples
Example 1
The weight parts of the raw materials of the thermally conductive silicone resins in examples 1 to 5 are shown in table 1.
TABLE 1 weight parts of the thermally conductive Silicone materials of examples 1-5
In examples 1 to 5, the heat conductive powder was aluminum hydroxide of sphero-star; the surfactant is a silane coupling agent; the thickening agent is inorganic bentonite; the reinforcing agent is fumed silica; the insulating filler is silicon dioxide.
In examples 1 to 3, the method for preparing the thermally conductive silicone resin comprises the steps of:
grinding the heat-conducting powder in an environment of 130-150 ℃ and passing through a 300-mesh screen, adding the ground heat-conducting powder into an ethanol solution, performing ultrasonic oscillation to enable the solution to become turbid liquid, adding a surfactant, continuing oscillation for 30min, standing, precipitating and drying to obtain modified heat-conducting powder;
stirring and mixing vinyl silicone resin and hydroxyl silicone resin, adjusting to an acidic environment, adding a cross-linking agent, stirring for 1h at 70-80 ℃, and taking out to obtain a silicone resin base material; adding a thickening agent, a platinum catalyst and an enhancer into a silicone base material, adjusting to a weak acid environment, and stirring for 0.5h at 80-90 ℃ to obtain a silicone mixture;
stirring and mixing the modified heat-conducting powder, the insulating filler and sodium chloride, placing the mixture into a ball mill for ball milling until the mixture passes through a 500-mesh screen, washing, filtering and drying to obtain a powder mixture; and stirring and mixing the powder mixture and the silicon resin mixture at the rotating speed of 200-250r/min, and taking out and cooling to room temperature to obtain the heat-conducting silicon resin.
In examples 4 to 5, the method for producing the thermally conductive silicone resin includes the steps of:
grinding the heat-conducting powder in an environment of 130-150 ℃ and passing through a 300-mesh screen, adding the ground heat-conducting powder into an ethanol solution, performing ultrasonic oscillation to enable the solution to become turbid liquid, adding a surfactant, continuing oscillation for 30min, standing, precipitating and drying to obtain modified heat-conducting powder;
stirring and mixing vinyl silicone resin, hydroxyl silicone resin and polyurethane acrylic resin, adjusting to an acidic environment, adding a cross-linking agent, stirring at 70-80 ℃ for 1h, and taking out to obtain a silicone resin base material; adding a thickening agent, a platinum catalyst and an enhancer into a silicone base material, adjusting to a weak acid environment, and stirring for 0.5h at 80-90 ℃ to obtain a silicone mixture;
and stirring and mixing the powder mixture and the Irgacure-184 to obtain a secondary mixture, stirring and mixing the secondary mixture and the silicone resin mixture at the rotating speed of 200-250r/min in a dark environment, placing the mixture into a mold, irradiating the mixture by ultraviolet light, and performing calendaring molding to obtain the heat-conducting silicone resin.
Example 6
The present embodiment 6 differs from embodiment 5 in that the method for preparing the thermally conductive silicone resin in embodiment 6 includes the following steps:
grinding the heat-conducting powder in an environment of 130-150 ℃ and passing through a 300-mesh screen, adding the ground heat-conducting powder into an ethanol solution, performing ultrasonic oscillation to enable the solution to become turbid liquid, adding a surfactant, continuing oscillation for 30min, standing, precipitating and drying to obtain modified heat-conducting powder;
stirring and mixing vinyl silicone resin, hydroxyl silicone resin and polyurethane acrylic resin, adjusting to an acidic environment, adding a cross-linking agent, stirring at 70-80 ℃ for 1h, and taking out to obtain a silicone resin base material; adding a thickening agent, a platinum catalyst and an enhancer into a silicone base material, adjusting to a weak acid environment, and stirring for 0.5h at 80-90 ℃ to obtain a silicone mixture;
stirring and mixing the powder mixture and Irgacure-184 to obtain a secondary mixture; overlapping and feeding the silicone resin mixture in an amount of 1/3 and the powder mixture in an amount of 1/4, wherein the feeding amounts of the silicone resin mixture and the powder mixture are sequentially increased during multiple feeding until the feeding is finished, standing and settling for 20min, stirring and mixing at a rotation speed of 200-250r/min, and taking out and cooling to room temperature to obtain the heat-conducting silicone resin.
Comparative example
Comparative example 1
Comparative example 1 differs from example 2 in that sodium chloride is not added to the thermally conductive silicone resin in comparative example 1.
Performance test
Test method
The thermally conductive silicone resins of examples 1-6 and comparative example 1 were calendered and cut into circular gaskets 2mm thick and 3cm in diameter. After the gaskets of examples 1 to 6 and comparative example 1 were subjected to heat aging in an atmospheric environment at 150 ℃ and an oxygen content of 21% for 30 days, the thermal resistances of the gaskets before and after the heat aging were measured by the method described in ASTM D5470, and the rate of increase in the thermal resistance was calculated, and the results are shown in Table 2.
TABLE 2 thermal resistance of the gaskets of examples 1-6 and comparative example 1
| Thermal resistance before thermal aging ℃/W | Thermal resistance after thermal aging ℃/W | Increase in thermal resistance% | |
| Example 1 | 0.442 | 0.539 | 21.95 |
| Example 2 | 0.439 | 0.534 | 21.64 |
| Example 3 | 0.445 | 0.545 | 22.47 |
| Example 4 | 0.458 | 0.518 | 13.10 |
| Example 5 | 0.461 | 0.522 | 13.23 |
| Example 6 | 0.452 | 0.486 | 7.52 |
| Comparative example 1 | 0.567 | 0.693 | 22.22 |
By combining examples 1-3 and table 2, it can be seen that the thermally conductive silicone resin prepared in the present application has a low thermal resistance and an excellent thermal aging capability, and the increase rate of the thermal resistance is less than 23% after thermal aging.
In the present application, it can be seen that the addition of sodium chloride to the preparation of the thermally conductive silicone resin can reduce the thermal resistance of the thermally conductive silicone resin, as seen by combining examples 1 to 3 with comparative example 1, and by combining table 2.
Combining examples 1-3 and examples 4-5, and combining table 2, it can be seen that adding urethane acrylic resin and Irgacure-184, and adding the step of ultraviolet irradiation, when preparing the thermally conductive silicone, can reduce the rate of increase in thermal resistance of the thermally conductive silicone after thermal aging.
It can be seen from the combination of examples 5 and 6 that, when the heat-conductive silicone resin is prepared, the secondary mixture and the silicone resin mixture are overlapped and put, so that the dispersion rate can be improved, and the thermal resistance increase rate of the heat-conductive silicone resin after thermal aging can be greatly reduced.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (9)
1. A preparation method of insulating compound heat-conducting powder filled silicone resin with ultralow thermal resistance is characterized by comprising the following steps:
placing 150-200 parts by weight of heat-conducting powder in an environment of 130-150 ℃ and grinding the powder through a 300-mesh screen, adding the powder into an ethanol solution, performing ultrasonic oscillation to enable the solution to become turbid liquid, adding 15-20 parts by weight of surfactant, continuing oscillation for 30min, standing, precipitating and drying to obtain modified heat-conducting powder;
stirring and mixing 25-30 parts by weight of vinyl silicone resin and 15-20 parts by weight of hydroxyl silicone resin, adjusting to an acidic environment, adding a cross-linking agent, stirring at 70-80 ℃ for 1h, and taking out to obtain a silicone resin base material; adding 3-5 parts of thickening agent, 1-3 parts of platinum catalyst and 1-2 parts of reinforcing agent into a silicone base material, adjusting to a weak acid environment, and stirring for 0.5h at 80-90 ℃ to obtain a silicone mixture;
according to parts by weight, stirring and mixing modified heat-conducting powder, 10-15 parts of insulating filler and 1-2 parts of sodium chloride, placing the mixture into a ball mill for ball milling until the mixture passes through a 500-mesh screen, and then washing, filtering and drying the mixture to obtain a powder mixture; and stirring and mixing the powder mixture and the silicon resin mixture at the rotating speed of 200-250r/min, and taking out and cooling to room temperature to obtain the heat-conducting silicon resin.
2. The preparation method of the insulating compound heat-conducting powder filled silicone resin with ultralow thermal resistance according to claim 1, characterized in that: according to the weight parts, 25-30 parts of vinyl silicone resin, 15-20 parts of hydroxyl silicone resin and 5-10 parts of polyurethane acrylic resin are stirred and mixed, the mixture is adjusted to an acid environment, a cross-linking agent is added, the mixture is stirred for 1 hour at 70-80 ℃, and then the silicon resin base material is obtained after the mixture is taken out.
3. The preparation method of the insulating compound heat-conducting powder filled silicone resin with ultralow thermal resistance according to claim 2, characterized in that: the powder mixture and 2-3 parts of Irgacure-184 are stirred and mixed according to the parts by weight to obtain a secondary mixture, the secondary mixture and the silicone resin mixture are stirred and mixed in a dark environment at the rotating speed of 200-250r/min, and then the mixture is placed into a die to be irradiated by ultraviolet light, and the heat-conducting silicone resin is obtained through calendaring molding.
4. The preparation method of the insulating compound heat-conducting powder filled silicone resin with ultralow thermal resistance according to claim 1, characterized in that: overlapping and feeding the 1/N amount of silicone resin mixture and the 1/M amount of powder mixture until the feeding is finished, standing and settling for 20min, stirring and mixing at the rotating speed of 200-250r/min, taking out and cooling to room temperature to obtain the heat-conducting silicone resin; wherein M and N are any natural number between 1 and 10, and M and N are independent of each other.
5. The preparation method of the insulating compound heat-conducting powder filled silicone resin with ultralow thermal resistance according to claim 1, characterized in that: the heat conducting powder is spherical aluminum hydroxide.
6. The preparation method of the insulating compound heat-conducting powder filled silicone resin with ultralow thermal resistance according to claim 1, characterized in that: the surfactant is a silane coupling agent.
7. The preparation method of the insulating compound heat-conducting powder filled silicone resin with ultralow thermal resistance according to claim 1, characterized in that: the thickening agent is inorganic bentonite.
8. The preparation method of the insulating compound heat-conducting powder filled silicone resin with ultralow thermal resistance according to claim 1, characterized in that: the reinforcing agent is fumed silica.
9. The preparation method of the insulating compound heat-conducting powder filled silicone resin with ultralow thermal resistance according to claim 1, characterized in that: the insulating filler is silicon dioxide.
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| CN104530707A (en) * | 2014-12-16 | 2015-04-22 | 惠州力王佐信科技有限公司 | Crystal whisker reinforced organic silicon heat conducting material and preparation method thereof |
| CN105331255A (en) * | 2015-12-10 | 2016-02-17 | 展辰新材料集团股份有限公司 | Ultraviolet curing coating and preparation method thereof |
| WO2017041454A1 (en) * | 2015-09-09 | 2017-03-16 | 中兴通讯股份有限公司 | High thermal conductivity composite interface material and preparation method therefor |
| CN107573474A (en) * | 2017-08-22 | 2018-01-12 | 广东省石油与精细化工研究院 | A kind of silicone-modified water-soluble polyurethane acrylic resin emulsion and preparation method thereof |
| CN110027127A (en) * | 2019-04-27 | 2019-07-19 | 北京化工大学 | Mixed refining process equipment is laminated in polymer filler differential 3D printing |
| CN112409791A (en) * | 2020-11-23 | 2021-02-26 | 中国科学院深圳先进技术研究院 | Heat-conducting composite material and preparation method thereof |
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- 2022-01-26 CN CN202210095016.XA patent/CN114410118B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104530707A (en) * | 2014-12-16 | 2015-04-22 | 惠州力王佐信科技有限公司 | Crystal whisker reinforced organic silicon heat conducting material and preparation method thereof |
| WO2017041454A1 (en) * | 2015-09-09 | 2017-03-16 | 中兴通讯股份有限公司 | High thermal conductivity composite interface material and preparation method therefor |
| CN105331255A (en) * | 2015-12-10 | 2016-02-17 | 展辰新材料集团股份有限公司 | Ultraviolet curing coating and preparation method thereof |
| CN107573474A (en) * | 2017-08-22 | 2018-01-12 | 广东省石油与精细化工研究院 | A kind of silicone-modified water-soluble polyurethane acrylic resin emulsion and preparation method thereof |
| CN110027127A (en) * | 2019-04-27 | 2019-07-19 | 北京化工大学 | Mixed refining process equipment is laminated in polymer filler differential 3D printing |
| CN112409791A (en) * | 2020-11-23 | 2021-02-26 | 中国科学院深圳先进技术研究院 | Heat-conducting composite material and preparation method thereof |
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