CN113416418B - Preparation method of high-temperature-resistant heat-conducting organic silicon composition - Google Patents
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Abstract
The invention provides a preparation method of a high-temperature-resistant heat-conducting organic silicon composition, which is composed of A, B double groups, wherein the A component is as follows: 100 parts of vinyl silicone oil, 400 parts of heat-conducting powder and 1800 parts of heat-resisting agent, 5-10 parts of color paste, 0.5-5 parts of platinum catalyst; the component B is as follows: 100 parts of vinyl silicone oil, 400 parts of heat-conducting powder and 1800 parts of heat-resistant agent, 4 parts to 10 parts of hydrogen-containing silicone oil and 0.04 part to 0.2 part of inhibitor. According to the invention, a cerium-zinc solid solution is used as a heat-resistant agent, so that the stability of the heat-conducting organic silicon composition at high temperature is effectively improved, the service life of the heat-conducting organic silicon composition is prolonged, and the application range of the heat-conducting organic silicon composition is widened.
Description
Technical Field
The invention belongs to the technical field of polymer composite materials, and particularly relates to a preparation method of a high-temperature-resistant heat-conducting organic silicon composition.
Background
At present, the integration level and power of electronic components are higher and higher, the size is continuously reduced, and the overflow phenomenon of heat generated during the operation of the components is more serious, so that the temperature is increased rapidly, and the stability and the service life of the product are influenced. In order to solve the problem, the heat-conducting interface material is produced at the same time, and heat generated during the operation of the components is quickly transferred to the outside, so that the safe and stable operation of the electronic components is guaranteed.
The room temperature vulcanized silicone rubber system has excellent weather resistance and electrical insulation performance, is convenient to use, has no by-product and has extremely small shrinkage rate, thereby being widely applied to heat-conducting interface materials (such as heat-conducting pouring sealant, gaskets, extrusion glue and the like). Because the thermal conductivity of the room temperature vulcanized silicone rubber system is relatively low and is only 0.2W/(m.K), a large amount of heat-conducting powder is often required to be filled to improve the heat-conducting property of the material when the heat-conducting interface material is prepared, and the surfaces of the powder often have certain polar groups and are alkaline, so that silicone oil molecules are easier to oxidize at high temperature, and macroscopically, the problems of increased hardness and reduced toughness of the heat-conducting room temperature vulcanized silicone rubber system are shown, so that the stability of the heat-conducting effect of the heat-conducting room temperature vulcanized silicone rubber system is damaged.
At present, the silicone oil formula system can be improved to improve the high temperature resistance, for example, the invention patent of publication No. CN 109880545A introduces an epoxy resin system to effectively improve the heat resistance of the colloid, so that the high temperature resistant heat conductive adhesive tape prepared by the invention can work at a higher temperature for a long time, and the bonding performance is not obviously weakened. Secondly, the high temperature resistance of an organic silicon system is often improved by adding a heat-resistant auxiliary agent, for example, an organic silicon metal complex is added as the heat-resistant auxiliary agent in the patent of the invention with the publication number of CN 109535722A, so that the high temperature resistance is obviously improved, the prepared high temperature-resistant organic silicon material can be used at high temperature for a long time, the problems of cracking, pulverization and the like are avoided, and the long-term heat dissipation stability under the high temperature condition is effectively ensured; patent No. CN 103275491A discloses a silicone rubber heat-resistant additive, wherein the heat-resistant additive is prepared by reacting phosphate, borate, acetic acid ketone and the like at a certain molar ratio at 110-170 ℃ for 3-6 hours, the silicone rubber heat-resistant additive has good compatibility with silicone rubber and can also improve the maximum use temperature of the silicone rubber, but the heat-resistant additive has a complex formula and high manufacturing cost, and is not beneficial to popularization and application.
In conclusion, the invention adopts the cerium-zinc solid solution as the heat-resistant agent, provides the preparation method of the high-temperature-resistant heat-conducting organic silicon composition, and improves the stability of the room-temperature vulcanized silicone rubber system at high temperature so as to prolong the service life and widen the application range of the room-temperature vulcanized silicone rubber system.
Disclosure of Invention
The invention provides a preparation method of a high-temperature-resistant heat-conducting organic silicon composition, which is characterized in that a cerium-zinc solid solution is adopted as a heat-resistant agent, and the prepared composition has good high-temperature resistance after being uniformly mixed in equal amount and cured, thereby having very important significance for widening the application range and prolonging the service life of the organic silicon composition. The composition can be applied to the fields of double-component heat-conducting pouring sealant, heat-conducting extrusion glue, heat-conducting gaskets and the like.
A preparation method of a high-temperature-resistant heat-conducting organic silicon composition comprises the following components of A, B (in parts by mass):
the preparation process of the component A is as follows: dispersing vinyl silicone oil, heat-conducting powder, color paste and a cerium-zinc solid solution heat-resistant auxiliary agent at 130-150 ℃, cooling to room temperature, adding a platinum catalyst, and further dispersing until the mixture is uniformly mixed;
the preparation process of the component B is as follows: dispersing vinyl silicone oil, hydrogen-containing silicone oil, heat-conducting powder and a cerium-zinc solid solution heat-resistant assistant at 130-150 ℃, cooling to room temperature, adding an inhibitor, and further dispersing until the mixture is uniformly mixed.
The preparation process of the cerium-zinc solid solution adopted by the invention is as follows:
(1) dissolving soluble cerium salt and zinc salt in deionized water, fully dissolving and uniformly mixing, adding hydrogen peroxide with the concentration 2 times that of the cerium salt, and stirring for 30min to oxidize trivalent cerium ions into tetravalent cerium ions.
(2) And slowly adding an alkaline solution serving as a precipitating agent into the solution, adjusting the pH value to 10-12, continuously dispersing for 2 hours to ensure that the precipitation reaction is complete, and then filtering and drying the obtained precipitate to obtain the solid solution precursor.
(3) And calcining the precursor at 450-750 ℃ for 3-6 h to obtain the cerium oxide and zinc oxide composite solid solution powder.
(4) And (3) putting the solid solution into a ball mill for ball milling for 2-4 h, sieving, and collecting for later use.
Preferably, the soluble cerium salt is one or a plurality of cerium chloride and cerium nitrate for composite use;
preferably, the soluble zinc salt is one or a plurality of zinc chloride, zinc nitrate and zinc sulfate for composite use;
preferably, the molar ratio of the soluble cerium salt to the zinc salt is 10: 1-3: 1.
Preferably, the mass ratio of the cerium-zinc solid solution heat-resistant agent to the vinyl silicone oil is 5-10%.
Preferably, the precipitator is one or a plurality of sodium hydroxide, ammonia water and sodium carbonate solution.
Preferably, the heat-conducting powder is one or more of aluminum oxide, zinc oxide, boron nitride, aluminum nitride, silicon carbide and silicon nitride, and the median diameter of the powder is 0.5-100 μm.
The technical method of the invention has the advantages that: compared with the common heat-resistant agent cerium oxide, the cerium-zinc solid solution improves the dispersibility of the cerium oxide due to the introduction of the zinc oxide, and the cerium oxide and the zinc oxide have a certain synergistic effect on the improvement of the heat resistance of the organic silicon, so that the heat resistance of the organic silicon composition is effectively improved.
Detailed Description
Example 1
(1) Preparation of cerium-zinc solid solution heat-resistant agent: 740g of cerium chloride and 41g of zinc chloride are weighed and added into 1000mL of deionized water, after full dissolution and uniform mixing, 153g of 30% hydrogen peroxide solution is added, dispersion is continued for 1h, then sodium hydroxide solution is slowly added, the pH value is adjusted to 12, after continuous dispersion is continued for 2h, the obtained precipitate in the solution is filtered, drying is carried out to obtain a precursor, and the precursor is calcined for 3h at 750 ℃ to obtain the cerium oxide and zinc oxide composite solid solution powder. And putting the powder into a ball mill for ball milling for 2 hours, sieving, and collecting for later use.
(2) Preparation of the high-temperature resistant heat-conducting silicone composition: dispersing 600g of vinyl silicone oil, 2400g of heat-conducting powder and 30g of the heat-resistant agent at a high speed at 150 ℃, cooling to room temperature, adding 3g of color paste and 3g of platinum catalyst, and further completely dispersing to obtain a component A of the composition; and (2) dispersing 600g of vinyl silicone oil, 60g of hydrogen-containing silicone oil, 2400g of heat-conducting powder and 30g of the heat-resistant agent at a high speed at 150 ℃, cooling to room temperature, adding 0.24g of inhibitor, and further completely dispersing to obtain the component B of the composition.
Example 2
(1) Preparation of cerium-zinc solid solution heat-resistant agent: weighing 326g of cerium nitrate and 61g of zinc nitrate, adding the weighed cerium nitrate and 61g of zinc nitrate into 1000mL of deionized water, fully dissolving and uniformly mixing, adding 51g of 30% hydrogen peroxide solution, continuously dispersing for 1h, then slowly adding an ammonia solution, adjusting the pH value to 10, continuously dispersing for 2h, filtering a precipitate obtained in the solution, drying to obtain a precursor, and calcining the precursor at 450 ℃ for 6h to obtain the cerium oxide and zinc oxide composite solid solution powder. And putting the powder into a ball mill for ball milling for 4 hours, sieving, and collecting for later use.
(2) Preparation of the high-temperature resistant heat-conducting silicone composition: dispersing 200g of vinyl silicone oil, 3600g of heat-conducting powder and 20g of the heat-resistant agent at a high speed at 130 ℃, cooling to room temperature, adding 10g of color paste and 10g of platinum catalyst, and further completely dispersing to obtain a component A of the composition; and (2) dispersing 600g of vinyl silicone oil, 40g of hydrogen-containing silicone oil, 2400g of heat-conducting powder and 20g of the heat-resistant agent at a high speed at 130 ℃, cooling to room temperature, adding 0.2g of inhibitor, and further completely dispersing to obtain a component B of the composition.
Example 3
(1) Preparation of cerium-zinc solid solution heat-resistant agent: weighing 370g of cerium chloride and 81g of zinc sulfate, adding the cerium chloride and the zinc sulfate into 1000mL of deionized water, fully dissolving and uniformly mixing, adding 77g of 30% hydrogen peroxide solution, continuously dispersing for 1h, then slowly adding a sodium carbonate solution, adjusting the pH value to 10, continuously dispersing for 2h, filtering a precipitate obtained in the solution, drying to obtain a precursor, and calcining the precursor at 600 ℃ for 3h to obtain the cerium oxide and zinc oxide composite solid solution powder. And putting the powder into a ball mill for ball milling for 3 hours, sieving, and collecting for later use.
(2) Preparation of the high-temperature resistant heat-conducting silicone composition: dispersing 300g of vinyl silicone oil, 3000g of heat-conducting powder and 21g of the heat-resistant agent at a high speed at 130 ℃, cooling to room temperature, adding 5g of color paste and 9g of platinum catalyst, and further completely dispersing to obtain a component A of the composition; and (2) dispersing 300g of vinyl silicone oil, 50g of hydrogen-containing silicone oil, 3000g of heat-conducting powder and 21g of the heat-resistant agent at a high speed at 130 ℃, cooling to room temperature, adding 0.25g of inhibitor, and further completely dispersing to obtain the component B of the composition.
Comparative example 1
Dispersing 600g of vinyl silicone oil and 2400g of heat-conducting powder at a high speed at 150 ℃, cooling to room temperature, adding 3g of color paste and 3g of platinum catalyst, and further completely dispersing to obtain a component A of the composition; and (3) dispersing 600g of vinyl silicone oil, 60g of hydrogen-containing silicone oil and 2400g of heat-conducting powder at a high speed at 150 ℃, cooling to room temperature, adding 0.24g of inhibitor, and further completely dispersing to obtain the component B of the composition.
Comparative example 2
Dispersing 600g of vinyl silicone oil, 2400g of heat-conducting powder and 30g of cerium oxide at a high speed at 150 ℃, cooling to room temperature, adding 3g of color paste and 3g of platinum catalyst, and further completely dispersing to obtain a component A of the composition; and (2) dispersing 600g of vinyl silicone oil, 60g of hydrogen-containing silicone oil, 2400g of heat-conducting powder and 30g of cerium oxide at a high speed at 150 ℃, cooling to room temperature, adding 0.24g of inhibitor, and further completely dispersing to obtain the component B of the composition.
Comparative example 3
Dispersing 200g of vinyl silicone oil and 3600g of heat-conducting powder at a high speed at 130 ℃, cooling to room temperature, adding 10g of color paste and 10g of platinum catalyst, and further completely dispersing to obtain a component A of the composition; and (3) dispersing 600g of vinyl silicone oil, 40g of hydrogen-containing silicone oil and 2400g of heat-conducting powder at a high speed at 130 ℃, cooling to room temperature, adding 0.2g of inhibitor, and further completely dispersing to obtain the component B of the composition.
Comparative example 4
Dispersing 200g of vinyl silicone oil, 3600g of heat-conducting powder and 20g of cerium oxide at a high speed at 130 ℃, cooling to room temperature, adding 10g of color paste and 10g of platinum catalyst, and further completely dispersing to obtain a component A of the composition; 600g of vinyl silicone oil, 40g of hydrogen-containing silicone oil, 2400g of heat-conducting powder and 20g of cerium oxide are dispersed at a high speed at 130 ℃, cooled to room temperature, added with 0.2g of inhibitor and further dispersed completely to obtain the component B of the composition.
Comparative example 5
Preparation of the high-temperature resistant heat-conducting silicone composition: dispersing 300g of vinyl silicone oil and 3000g of heat-conducting powder at a high speed at 130 ℃, cooling to room temperature, adding 5g of color paste and 9g of platinum catalyst, and further completely dispersing to obtain a component A of the composition; and (3) dispersing 300g of vinyl silicone oil, 50g of hydrogen-containing silicone oil and 3000g of heat-conducting powder at a high speed at 130 ℃, cooling to room temperature, adding 0.25g of inhibitor, and further completely dispersing to obtain the component B of the composition.
Comparative example 6
Preparation of the high-temperature resistant heat-conducting silicone composition: dispersing 300g of vinyl silicone oil, 3000g of heat-conducting powder and 21g of cerium oxide at a high speed at 130 ℃, cooling to room temperature, adding 5g of color paste and 9g of platinum catalyst, and further completely dispersing to obtain a component A of the composition; and (3) dispersing 300g of vinyl silicone oil, 50g of hydrogen-containing silicone oil, 3000g of heat-conducting powder and 21g of cerium oxide at a high speed at 130 ℃, cooling to room temperature, adding 0.25g of inhibitor, and further completely dispersing to obtain the component B of the composition.
The composition A, B prepared in each of the above examples and comparative examples was mixed at a ratio of 1:1, followed by vacuum application, and was pressed into 2mm sheets on a calender line and cured by baking at 125 ℃ and half of each cured sheet was baked at 200 ℃ for 168 hours for aging test. And the mechanical properties of the high-temperature aging sample and the control sample are tested, and the test results are shown in table 1.
Table 1: mechanical property test results before and after high-temperature aging of examples 1 to 3 and comparative examples 1 to 6
The mechanical property testing method comprises the following steps: testing the structural adhesive with tensile strength and elongation at break by referring to a GB/T1040.1-2006 method, and taking an average value for 3 times; the hardness is tested according to the method GB/T531-1999, and 3 times of average values are taken.
As can be seen from the data in the table, the mechanical properties after aging of examples 1, 2 and 3, in which the cerium-zinc solid solution is added as the heat-resistant agent, are very little changed compared with the blank control comparative examples 1, 3 and 5, respectively, which indicates that the cerium-zinc solid solution can effectively improve the high-temperature resistance of the heat-conductive silicone composition; in addition, as compared with comparative example 2 in which cerium-zinc solid solution is added as a heat-resistant agent, example 1 in which the hardness change is increased by only 4 and the hardness change is increased by 17 in comparison with comparative example 2 in which cerium oxide is added as a heat-resistant agent shows that the cerium-zinc solid solution has improved high-temperature resistance of the silicone composition as compared with cerium oxide, which is also demonstrated by the data of example 2 and comparative example 4, and example 3 and comparative example 6. Meanwhile, because the cerium-zinc solid solution is better in dispersibility than cerium oxide, the hardness of the heat-conducting sheet after the organosilicon compositions of examples 1, 2 and 3 are cured is respectively lower than that of a comparative example added with cerium oxide under the same formula.
The above examples are preferred embodiments of the present invention, but the method of the present invention is not limited thereto, and any other modifications, combinations, and simplifications made by the spirit or principle of the present invention are considered to be equivalent implementations, and are included in the scope of the present invention.
Claims (4)
1. The preparation method of the high-temperature-resistant heat-conducting organic silicon composition is characterized in that A, B components are as follows in parts by mass:
the preparation process of the component A is as follows: dispersing vinyl silicone oil, heat-conducting powder, color paste and a cerium-zinc solid solution heat-resistant auxiliary agent at 130-150 ℃, cooling to room temperature, adding a platinum catalyst, and further dispersing until the mixture is uniformly mixed;
the preparation process of the component B is as follows: dispersing vinyl silicone oil, hydrogen-containing silicone oil, heat-conducting powder and a cerium-zinc solid solution heat-resistant auxiliary agent at 130-150 ℃, cooling to room temperature, adding an inhibitor, and further dispersing until the mixture is uniformly mixed;
the preparation method of the cerium-zinc solid solution heat-resistant agent comprises the following steps:
(1) dissolving soluble cerium salt and zinc salt in deionized water, fully dissolving and uniformly mixing, adding hydrogen peroxide with the concentration 2 times that of the cerium salt, and stirring for 30min to oxidize trivalent cerium ions into tetravalent cerium ions;
(2) slowly adding an alkaline solution serving as a precipitator into the solution, adjusting the pH value to 10-12, continuously dispersing for 2 hours to ensure that the precipitation reaction is complete, and then filtering and drying the obtained precipitate to obtain a solid solution precursor;
(3) calcining the precursor at 450-750 ℃ for 3-6 h to obtain a cerium oxide and zinc oxide composite solid solution;
(4) and (3) putting the solid solution into a ball mill for ball milling for 2-4 h, sieving, and collecting for later use.
2. The preparation method of the high-temperature-resistant heat-conducting silicone composition according to claim 1, wherein the molar ratio of cerium to zinc is 10: 1-3: 1.
3. The preparation method of the high temperature resistant heat conductive silicone composition according to claim 1, characterized in that the mass ratio of the cerium-zinc solid solution heat-resistant agent to the vinyl silicone oil is 5% -10%.
4. The preparation method of the high-temperature-resistant heat-conducting organosilicon composition according to claim 1, characterized in that the heat-conducting powder is one or more of alumina, zinc oxide, boron nitride, aluminum nitride, silicon carbide and silicon nitride, and the median diameter of the powder is 0.5 μm-100 μm.
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CN1775692B (en) * | 2005-12-09 | 2010-06-09 | 天津理工大学 | Nano light-screen zinc-cerium composite oxide and its preparing method |
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Address after: No. 12, Yinzhou Road, Zhou Village, Baini Town, Sanshui District, Foshan, Guangdong 528131 Patentee after: Guangdong Jinge New Materials Co.,Ltd. Address before: No.12, Yinzhou Road, Baini Town, Sanshui District, Foshan City, Guangdong Province Patentee before: Foshan Jinge New Material Co.,Ltd. |